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Sample records for solvent-free aza-michael addition

  1. Solvent-free, catalyst-free aza-Michael addition of cyclohexylamine to diethyl maleate: reaction mechanism and kinetics

    Czech Academy of Sciences Publication Activity Database

    Bláha, Michal; Trhlíková, Olga; Podešva, Jiří; Abbrent, Sabina; Steinhart, Miloš; Dybal, Jiří; Dušková-Smrčková, Miroslava

    2018-01-01

    Roč. 74, č. 1 (2018), s. 58-67 ISSN 0040-4020 Institutional support: RVO:61389013 Keywords : Aza-Michael addition * solvent-free * catalyst-free Subject RIV: CD - Macromolecular Chemistry OBOR OECD: Polymer science Impact factor: 2.651, year: 2016

  2. Tetrabutylammonium Bromide Media Aza-Michael Addition of 1,2,3,6-Tetrahydrophthalimide to Symmetrical Fumaric Esters and Acrylic Esters under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Mohammadreza Zamanloo

    2010-10-01

    Full Text Available The aza-Michael addition of 1,2,3,6-tetrahydrophthalimide with symmetrical fumaric esters has been performed efficiently in a solvent-free system at 100 °C and using 1,4-diazabicyclo[2.2.2]octane (DABCO as a base in the presence of tetrabutylammonium bromide (TBAB. The products were obtained in good to high yields within 2.5-7.0 h. This reaction worked well on linear alkyl fumarates and was not effective with nonlinear alkyl fumarates. Although the reaction was also applicable to acrylates such as n-butyl acrylate, methacrylates and crotonates were not suitable Michael acceptors for this reaction.

  3. Organocatalytic aza-Michael/retro-aza-Michael reaction: pronounced chirality amplification in aza-Michael reaction and racemization via retro-aza-Michael reaction.

    Science.gov (United States)

    Cai, Yong-Feng; Li, Li; Luo, Meng-Xian; Yang, Ke-Fang; Lai, Guo-Qiao; Jiang, Jian-Xiong; Xu, Li-Wen

    2011-05-01

    A detailed experimental investigation of an aza-Michael reaction of aniline and chalcone is presented. A series of Cinchona alkaloid-derived organocatalysts with different functional groups were prepared and used in the aza-Michael and retro-aza-Michael reaction. There was an interesting finding that a complete reversal of stereoselectivity when a benzoyl group was introduced to the cinchonine and cinchonidine. The chirality amplification vs. time proceeds in the quinine-derived organocatalyst containing silicon-based bulky group, QN-TBS, -catalyzed aza-Michael reaction under solvent-free conditions. In addition, we have demonstrated for the first time that racemization was occurred in suitable solvents under mild conditions due to retro-aza-Michael reaction of the Michael adduct of aniline with chalcone. These indicate the equilibrium of retro-aza-Michael reaction and aza-Michael reaction produce the happening of chirality amplification in aza-Michael reaction and racemization via retro-aza-Michael reaction under different conditions, which would be beneficial to the development of novel chiral catalysts for the aza-Michael reactions. Copyright © 2011 Wiley-Liss, Inc.

  4. Aza-Michael Mono-addition Using Acidic Alumina under Solventless Conditions

    Directory of Open Access Journals (Sweden)

    Giovanna Bosica

    2016-06-01

    Full Text Available Aza-Michael reactions between primary aliphatic and aromatic amines and various Michael acceptors have been performed under environmentally-friendly solventless conditions using acidic alumina as a heterogeneous catalyst to selectively obtain the corresponding mono-adducts in high yields. Ethyl acrylate was the main acceptor used, although others such as acrylonitrile, methyl acrylate and acrylamide were also utilized successfully. Bi-functional amines also gave the mono-adducts in good to excellent yields. Such compounds can serve as intermediates for the synthesis of anti-cancer and antibiotic drugs.

  5. Asymmetric Domino Aza-Michael Addition/[3+2] Cycloaddition Reactions as a Versatile Approach to alpha,beta,gamma,-Triamino Acid Derivatives

    Czech Academy of Sciences Publication Activity Database

    Kapras, Vojtěch; Pohl, Radek; Císařová, I.; Jahn, Ullrich

    2014-01-01

    Roč. 16, č. 4 (2014), s. 1088-1091 ISSN 1523-7060 Institutional support: RVO:61388963 Keywords : 1,3-dipolar cycloaddition * lithium amides * aza-Michael addition * amino acids * pyrazoles Subject RIV: CC - Organic Chemistry Impact factor: 6.364, year: 2014

  6. Nano-organocatalyst: magnetically retrievable ferrite-anchored glutathione for microwave-assisted Paal–Knorr reaction, aza-Michael addition, and pyrazole synthesis

    KAUST Repository

    Polshettiwar, Vivek; Varma, Rajender S.

    2010-01-01

    Postsynthetic Surface modification of magnetic nanoparticles by glutathione imparts desirable chemical functionality and enables the generation of catalytic sites on the surfaces of ensuing organocatalysts. In this article, we discuss the developments, unique activity, and high selectivity of nano-organocatalysts for microwave-assisted Paal-Knorr reaction, aza-Michael addition, and pyrazole synthesis. Their insoluble character Coupled with paramagnetic nature enables easy separation of these nano-catalysts from the reaction mixture using external magnet, which eliminates the requirement of catalyst filtration. Published by Elsevier Ltd.

  7. Aza-Michael Reaction for an Undergraduate Organic Chemistry Laboratory

    Science.gov (United States)

    Nigam, Manisha; Rush, Brittney; Patel, Jay; Castillo, Raul; Dhar, Preeti

    2016-01-01

    A green, aza-Michael reaction is described that can be used to teach undergraduate students conjugate addition of nitrogen nucleophile to an a,ß-unsaturated ester. Students analyze spectral data of the product obtained from the assigned reaction to determine product structure and propose the mechanism of its formation. The experiment requires…

  8. Aza-Michael reaction: achievements and prospects

    International Nuclear Information System (INIS)

    Rulev, Alexander Yu

    2011-01-01

    Data published in the last 10 years on the use of the aza-Michael reaction in organic synthesis are described systematically. The attention is focused on environmentally friendly processes following green chemistry principles and on methods for the synthesis of compounds that are difficult to access by other routes.

  9. Solvent-free microwave-mediated Michael addition reactions

    Indian Academy of Sciences (India)

    Unknown

    obviously difficult to scale up. In this context ... eco-friendly features such as, (i) no solvent is required to conduct the ... water soluble, addition of reaction mixture after com- ..... Yield: 855 mg (89%; viscous liquid). 3.4 Ethyl .... Jung M E 1993 Comprehensive organic synthesis ... Leshcheva I F and Bundel Y G 1997 Mendeleev.

  10. New eco-friendly animal bone meal catalysts for preparation of chalcones and aza-Michael adducts

    Directory of Open Access Journals (Sweden)

    Riadi Yassine

    2012-06-01

    Full Text Available Abstract Two efficient reactions were successfully carried out using Animal Bone Meal (ABM and potassium fluoride or sodium nitrate doped ABMs as new heterogeneous catalysts under very mild conditions. After preparation and characterization of the catalysts, we first report their use in a simple and convenient synthesis of various chalcones by Claisen–Schmidt condensation and then in an aza-Michael addition involving several synthesized chalcones with aromatic amines. All the reactions were carried out at room temperature in methanol; the chalcone synthesis was also achieved in water environment under microwave irradiation. Doping ABM enhances the rate and yield at each reaction. Catalytic activities are discussed and the ability to re-use the ABM is demonstrated. Results For Claisen–Schmidt the use of ABM alone, yields never exceeded 17%. In each entry, KF/ABM and NaNO3/ABM (79-97% gave higher yields than using ABM alone under thermic condition. Also the reaction proceeded under microwave irradiation in good yields (72-94% for KF/ABM and 81-97% for NaNO3/ABM and high purity. For aza-Michael addition the use of ABM doped with KF or NaNO3 increased the catalytic activity remarkably. The very high yields could be noted (84-95% for KF/ABM and 81-94% for NaNO3/ABM. Conclusion The present method is an efficient and selective procedure for the synthesis of chalcones an aza-Michael adducts. The ABM and doped ABMs are a new, inexpensive and attractive solid supports which can contribute to the development of catalytic processes and reduced environmental problems.

  11. Solvent-Free Synthesis of Silver-Nanoparticles and their Use as Additive in Poly (Dicyclopentadiene)

    International Nuclear Information System (INIS)

    Abbas, M.; Kienberger, J.

    2013-01-01

    A solvent-free environmentally benign synthesis of oleylamine capped silver nanoparticles is presented. Upon heating 10 equivalents of oleylamine and silver nitrate at 165 degree C for 30 min followed by a precipitation step using ethanol as the precipitant particles characterized by an Z-average diameter of 63 nm were obtained. Dried particles can be easily redispersed in unpolar solvents or monomers, which pave the way for using them as an antimicrobial additive in polymeric materials. In particular, newly prepared Ag-particles were dispersed in dicyclopentadiene and the mixture was cured using ring opening metathesis polymerization yielding an antimicrobially equipped duroplastic material. (author)

  12. Green Michael addition of thiols to electron deficient alkenes using KF/alumina and recyclable solvent or solvent-free conditions

    Energy Technology Data Exchange (ETDEWEB)

    Lenardao, Eder J.; Trecha, Danusia O.; Ferreira, Patricia da C.; Jacob, Raquel G.; Perin, Gelson [Universidade Federal de Pelotas (UFPEL), Pelotas, RS (Brazil). Inst. de Quimica e Geociencias. Lab. de Sintese Organica Limpa (LASOL)]. E-mail: lenardao@ufpel.edu.br

    2009-07-01

    A general, clean and easy method for the conjugated addition of thiols to citral promoted by KF/Al{sub 2}O{sub 3} under solvent-free or using glycerin as recyclable solvent at room temperature is described. It was found that the solvent-free protocol is applicable to the direct reaction of thiophenol with the essential oil of lemon grass (Cymbopogon citratus) to afford directly 3,7-dimethyl-3-(phenylthio)oct-6-enal, a potential bactericide agent. The method was extended to other electron-poor alkenes with excellent results. For the solvent-free protocol, the use of microwave irradiation facilitated the procedure and accelerates the reaction. The catalytic system and glycerin can be reused up to three times without previous treatment with comparable activity. (author)

  13. Catalyst-free and solvent-free Michael addition of 1,3-dicarbonyl compounds to nitroalkenes by a grinding method

    Science.gov (United States)

    Xie, Zong-Bo; Wu, Ming-Yu; He, Ting; Le, Zhang-Gao

    2012-01-01

    Summary An environmentally benign, fast and convenient protocol has been developed for the Michael addition of 1,3-dicarbonyl compounds to β-nitroalkenes in good to excellent yields by a grinding method under catalyst- and solvent-free conditions. PMID:22563352

  14. Domino Aza-Michael-ih-Diels-Alder Reaction to Various 3-Vinyl-1,2,4-triazines: Access to Polysubstituted Tetrahydro-1,6-naphthyridines.

    Science.gov (United States)

    Jouha, Jabrane; Buttard, Floris; Lorion, Magali; Berthonneau, Clément; Khouili, Mostafa; Hiebel, Marie-Aude; Guillaumet, Gérald; Brière, Jean-François; Suzenet, Franck

    2017-09-15

    A straightforward domino aza-Michael-inverse-electron-demand-hetero-Diels-Alder/retro-Diels-Alder reaction between primary and secondary propargylamine derivatives and 3-vinyl-1,2,4-triazines is developed highlighting not only the uniqueness of this dual-heterocyclic platform but also a novel and unprecedented path to polysubstituted tetrahydro-1,6-naphthyridine scaffolds.

  15. On the addition of conducting ceramic nanoparticles in solvent-free ionic liquid electrolyte for dye-sensitized solar cells

    KAUST Repository

    Lee, Chuan-Pei

    2009-08-01

    Titanium carbide (TiC) is an extremely hard conducting ceramic material often used as a coating for titanium alloys as well as steel and aluminum components to improve their surface properties. In this study, conducting ceramic nanoparticles (CCNPs) have been used, for the first time, in dye-sensitized solar cells (DSSCs), and the incorporation of TiC nanoparticles in a binary ionic liquid electrolyte on the cell performance has been investigated. Cell conversion efficiency with 0.6 wt% TiC reached 1.68%, which was higher than that without adding TiC (1.18%); however, cell efficiency decreased when the TiC content reached 1.0 wt%. The electrochemical impedance spectroscopy (EIS) technique was employed to analyze the interfacial resistance in DSSCs, and it was found that the resistance of the charge-transfer process at the Pt counter electrode (Rct1) decreased when up to 1.0 wt% TiC was added. Presumably, this was due to the formation of the extended electron transfer surface (EETS) which facilitates electron transfer to the bulk electrolyte, resulting in a decrease of the dark current, whereby the open-circuit potential (VOC) could be improved. Furthermore, a significant increase in the fill factor (FF) for all TiC additions was related to the decrease in the series resistance (RS) of the DSSCs. However, at 1.0 wt% TiC, the largest charge-transfer resistance at the TiO2/dye/electrolyte interface was observed and resulted from the poor penetration of the electrolyte into the porous TiO2. The long-term stability of DSSCs with a binary ionic liquid electrolyte, which is superior to that of an organic solvent-based electrolyte, was also studied. © 2009 Elsevier B.V. All rights reserved.

  16. SHORT COMMUNICATION SOLVENT FREE PREPARATION OF N ...

    African Journals Online (AJOL)

    Preferred Customer

    KEYWORDS: Solvent free, Maleanilic acids, Maleic anhydride, Aniline derivatives ... associated with the carboxylic group between 3275-2877 cm-1, the weak –NH .... Chemical shifts (σ/ppm) relative to TMS*. O-H N-H Ha. Hb. Hc. Hd. He. Hf.

  17. Dynamics of solvent-free grafted nanoparticles

    KAUST Repository

    Chremos, Alexandros

    2012-01-01

    The diffusivity and structural relaxation characteristics of oligomer-grafted nanoparticles have been investigated with simulations of a previously proposed coarse-grained model at atmospheric pressure. Solvent-free, polymer-grafted nanoparticles as well as grafted nanoparticles in a melt were compared to a reference system of bare (ungrafted) particles in a melt. Whereas longer chains lead to a larger hydrodynamic radius and lower relative diffusivity for grafted particles in a melt, bulk solvent-free nanoparticles with longer chains have higher relative diffusivities than their short chain counterparts. Solvent-free nanoparticles with short chains undergo a glass transition as indicated by a vanishing diffusivity, diverging structural relaxation time and the formation of body-centered-cubic-like order. Nanoparticles with longer chains exhibit a more gradual increase in the structural relaxation time with decreasing temperature and concomitantly increasing particle volume fraction. The diffusivity of the long chain nanoparticles exhibits a minimum at an intermediate temperature and volume fraction where the polymer brushes of neighboring particles overlap, but must stretch to fill the interparticle space. © 2012 American Institute of Physics.

  18. Oligoquinolines under Solvent-free Microwave Irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Park, Kwi-Jeon; Kwon, Tae-Woo [Kyungsung University, Busan (Korea, Republic of)

    2015-01-15

    Quinolines are thermally stable and can be used as an excellent n-type semiconducting materials. Since quinolines are also known to be electron acceptor molecules, combination of various electron donor building blocks can be utilized in photonic and electronic organic light-emitting diode (OLED) applications. For example, donor.acceptor systems with phenothiazine (or carbazole) molecules as electron donors and the phenylquinoline group as an electron acceptor provide an efficient approach for the design of new materials exhibiting highly efficient charge-transfer photophysics and electroluminescence in OLEDs. We have described the Friedlander quinoline synthesis between aminobenzophenones and symmetrical diacetyl compounds having phenothiazine, carbazole, biphenyl, and phenyl moieties under solvent-free microwave irradiation in 12.98% isolated yields.

  19. SOLVENT-FREE TETRAHYDROPYRANYLATION (THP) OF ALCOHOLS AND PHENOLS AND THEIR REGENERATION BY CATALYTIC ALUMINUM CHLORIDE HEXAHYDRATE

    Science.gov (United States)

    Catalytic amount of aluminum chloride hexahydrate enables solvent-free tetrahydropyranylation (THP) of alcohols and phenols at moderate temperatures. A simple addition of methanol helps to regenerate the corresponding alcohols and phenols thus rendering these protection and depro...

  20. Structural Transitions of Solvent-Free Oligomer-Grafted Nanoparticles

    KAUST Repository

    Chremos, Alexandros; Panagiotopoulos, Athanassios Z.

    2011-01-01

    that of simple liquids. The reversible nature of these transitions in solvent-free conditions offers new ways to control self-assembly of nanoparticles at experimentally accessible conditions. © 2011 American Physical Society.

  1. Synthesis, characterisation and non-isothermal degradation kinetics ...

    Indian Academy of Sciences (India)

    Synthesis of a novel co-polymer made by the addition polymerisation between MEGDMA and 4-AB by aza-Michael addition (AMA) polymerisation method is a fascinating field of research. The present investigationyielded a hazardous metal catalyst-free and toxic solvent-free methodology. The AMA polymerisation was ...

  2. Structural Transitions of Solvent-Free Oligomer-Grafted Nanoparticles

    KAUST Repository

    Chremos, Alexandros

    2011-09-01

    Novel structural transitions of solvent-free oligomer-grafted nanoparticles are investigated by using molecular dynamics simulations of a coarse-grained bead-spring model. Variations in core size and grafting density lead to self-assembly of the nanoparticles into a variety of distinct structures. At the boundaries between different structures, the nanoparticle systems undergo thermoreversible transitions. This structural behavior, which has not been previously reported, deviates significantly from that of simple liquids. The reversible nature of these transitions in solvent-free conditions offers new ways to control self-assembly of nanoparticles at experimentally accessible conditions. © 2011 American Physical Society.

  3. An efficient synthesis of quinolines under solvent-free conditions

    Indian Academy of Sciences (India)

    Unknown

    An efficient synthesis of quinolines under solvent-free conditions. 201 was then irradiated with microwaves in a microwave oven (Samsung model# CE118KF) at 1050W (70% of total power) for 5 minutes (3 + 2 with an inter- mission of 5 minutes). The reaction mixture was cooled at room temperature and rendered basic (pH.

  4. GRINDING SOLVENT-FREE PAAL-KNORR PYRROLE SYNTHESIS ...

    African Journals Online (AJOL)

    Paal-Knorr pyrrole synthesis on smectites as recyclable and green catalysts. Bull. Chem. Soc. .... 1-Propyl-2,5-dimethyl-1H-pyrrole (8a). Oil (reported as oil .... of pyrroles catalyzed by zirconium chloride under solvent-free conditions . Ultrason.

  5. Efficient synthesis of sulfonamide derivatives on solid supports catalyzed using solvent-free and microwave-assisted methods

    Energy Technology Data Exchange (ETDEWEB)

    Camargo-Ordonez, Argelia; Moreno-Reyes, Christian; Olazaran-Santibanez, Fabian; Martinez-Hernandez, Sheila; Bocanegra-Garcia, Virgilio; Rivera, Gildardo [Universidad Autonoma de Tamaulipas, Reynosa (Mexico). Dep. de Farmacia y Quimica Medicinal

    2011-07-01

    In this work we report the synthesis of sulfonamide derivatives using a conventional procedure and with solid supports, such as silica gel, florisil, alumina, 4A molecular sieves, montmorillonite KSF, and montmorillonite K10 using solvent-free and microwave-assisted methods. Our results show that solid supports have a catalytic activity in the formation of sulfonamide derivatives. We found that florisil, montmorillonite KSF, and K10 could be used as inexpensive alternative catalysts that are easily separated from the reaction media. Additionally, solvent-free and microwave-assisted methods were more efficient in reducing reaction time and in increasing yield. (author)

  6. Efficient synthesis of sulfonamide derivatives on solid supports catalyzed using solvent-free and microwave-assisted methods

    International Nuclear Information System (INIS)

    Camargo-Ordonez, Argelia; Moreno-Reyes, Christian; Olazaran-Santibanez, Fabian; Martinez-Hernandez, Sheila; Bocanegra-Garcia, Virgilio; Rivera, Gildardo

    2011-01-01

    In this work we report the synthesis of sulfonamide derivatives using a conventional procedure and with solid supports, such as silica gel, florisil, alumina, 4A molecular sieves, montmorillonite KSF, and montmorillonite K10 using solvent-free and microwave-assisted methods. Our results show that solid supports have a catalytic activity in the formation of sulfonamide derivatives. We found that florisil, montmorillonite KSF, and K10 could be used as inexpensive alternative catalysts that are easily separated from the reaction media. Additionally, solvent-free and microwave-assisted methods were more efficient in reducing reaction time and in increasing yield. (author)

  7. Liquid Quinones for Solvent-Free Redox Flow Batteries.

    Science.gov (United States)

    Shimizu, Akihiro; Takenaka, Keisuke; Handa, Naoyuki; Nokami, Toshiki; Itoh, Toshiyuki; Yoshida, Jun-Ichi

    2017-11-01

    Liquid benzoquinone and naphthoquinone having diethylene glycol monomethyl ether groups are designed and synthesized as redox active materials that dissolve supporting electrolytes. The Li-ion batteries based on the liquid quinones using LiBF 4 /PC show good performance in terms of voltage, capacity, energy efficiency, and cyclability in both static and flow modes. A battery is constructed without using intentionally added organic solvent, and its high energy density (264 W h L -1 ) demonstrates the potential of solvent-free organic redox flow batteries using liquid active materials. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Synthesis of halide- and solvent free metal borohydrides

    DEFF Research Database (Denmark)

    Grinderslev, Jakob; Møller, Kasper Trans; Richter, Bo

    have challenges due to their high desorption kinetics and limited reversibility at moderate conditions.[2],[3],[4] In this work, we present a new approach to synthesize halide- and solvent free metal borohydrides starting from the respective metal hydride. The synthetic strategy ensures that no metal...... to the metal. Hence, the powdered M(BH4)3∙DMS is heated to 140 °C for 4 hours to obtain pure M(BH4)3. The rare-earth metal borohydrides have been investigated by infrared spectroscopy and thermal analysis (TGA-DSC-MS). Furthermore, the structural trends are investigated by synchrotron radiation powder X...

  9. Microwave-Assisted Solvent-Free Synthesis of Zeolitic Imidazolate Framework-67

    Directory of Open Access Journals (Sweden)

    Heng Zhang

    2016-01-01

    Full Text Available A microporous metal-organic framework (MOF, cobalt-based zeolitic imidazolate framework-67 (ZIF-67, was synthesized by the combination of solvent-free hand-mill and microwave irradiation, without any organic solvent and within 30 minutes. The hand-milling process can mix the reactants well by the virtue of high moisture/water absorption capacity of reactants. In addition, the outstanding electromagnetic wave absorption capability of cobalt leads to efficient conversion to MOF structures before carbonization. The obtained ZIF-67 possesses high surface area and micropore volume.

  10. Photo-triggered solvent-free metamorphosis of polymeric materials.

    Science.gov (United States)

    Honda, Satoshi; Toyota, Taro

    2017-09-11

    Liquefaction and solidification of materials are the most fundamental changes observed during thermal phase transitions, yet the design of organic and polymeric soft materials showing isothermal reversible liquid-nonliquid conversion remains challenging. Here, we demonstrate that solvent-free repeatable molecular architectural transformation between liquid-star and nonliquid-network polymers that relies on cleavage and reformation of a covalent bond in hexaarylbiimidazole. Liquid four-armed star-shaped poly(n-butyl acrylate) and poly(dimethyl siloxane) with 2,4,5-triphenylimidazole end groups were first synthesized. Subsequent oxidation of the 2,4,5-triphenylimidazoles into 2,4,5-triphenylimidazoryl radicals and their coupling with these liquid star polymers to form hexaarylbiimidazoles afforded the corresponding nonliquid network polymers. The resulting nonliquid network polymers liquefied upon UV irradiation and produced liquid star-shaped polymers with 2,4,5-triphenylimidazoryl radical end groups that reverted to nonliquid network polymers again by recoupling of the generated 2,4,5-triphenylimidazoryl radicals immediately after terminating UV irradiation.The design of organic and polymeric soft materials showing isothermal reversible liquid-nonliquid conversion is challenging. Here, the authors show solvent-free repeatable molecular architectural transformation between liquid-star and non-liquid-network polymers by the cleavage and reformation of covalent bonds in the polymer chain.

  11. Development of solvent-free ambient mass spectrometry for green chemistry applications.

    Science.gov (United States)

    Liu, Pengyuan; Forni, Amanda; Chen, Hao

    2014-04-15

    Green chemistry minimizes chemical process hazards in many ways, including eliminating traditional solvents or using alternative recyclable solvents such as ionic liquids. This concept is now adopted in this study for monitoring solvent-free reactions and analysis of ionic liquids, solids, and catalysts by mass spectrometry (MS), without using any solvent. In our approach, probe electrospray ionization (PESI), an ambient ionization method, was employed for this purpose. Neat viscous room-temperature ionic liquids (RTILs) in trace amounts (e.g., 25 nL) could be directly analyzed without sample carryover effect, thereby enabling high-throughput analysis. With the probe being heated, it can also ionize ionic solid compounds such as organometallic complexes as well as a variety of neat neutral solid chemicals (e.g., amines). More importantly, moisture-sensitive samples (e.g., [bmim][AlCl4]) can be successfully ionized. Furthermore, detection of organometallic catalysts (including air-sensitive [Rh-MeDuPHOS][OTf]) in ionic liquids, a traditionally challenging task due to strong ion suppression effect from ionic liquids, can be enabled using PESI. In addition, PESI can be an ideal approach for monitoring solvent-free reactions. Using PESI-MS, we successfully examined the alkylation of amines by alcohols, the conversion of pyrylium into pyridinium, and the condensation of aldehydes with indoles as well as air- and moisture-sensitive reactions such as the oxidation of ferrocene and the condensation of pyrazoles with borohydride. Interestingly, besides the expected reaction products, the reaction intermediates such as the monopyrazolylborate ion were also observed, providing insightful information for reaction mechanisms. We believe that the presented solvent-free PESI-MS method would impact the green chemistry field.

  12. Towards room temperature, direct, solvent free synthesis of tetraborohydrides

    International Nuclear Information System (INIS)

    Remhof, A; Yan, Y; Friedrichs, O; Kim, J W; Mauron, Ph; Borgschulte, A; Züttel, A; Wallacher, D; Buchsteiner, A; Hoser, A; Oh, K H; Cho, Y W

    2012-01-01

    Due to their high hydrogen content, tetraborohydrides are discussed as potential synthetic energy carriers. On the example of lithium borohydride LiBH 4 , we discuss current approaches of direct, solvent free synthesis based on gas solid reactions of the elements or binary hydrides and/or borides with gaseous H 2 or B 2 H 6 . The direct synthesis from the elements requires high temperature and high pressure (700°C, 150bar D 2 ). Using LiB or AlB 2 as boron source reduces the required temperature by more than 300 K. Reactive milling of LiD with B 2 H 6 leads to the formation of LiBD 4 already at room temperature. The reactive milling technique can also be applied to synthesize other borohydrides from their respective metal hydrides.

  13. Tuning of Activated Carbon for Solvent-Free Oxidation of Cyclohexane

    Directory of Open Access Journals (Sweden)

    Mohammad Sadiq

    2017-01-01

    Full Text Available Activated carbon (AC was prepared from carbonization of phosphoric acid soaked peanut shell at 380°C under inert atmosphere followed by activation with hydrogen peroxide. The AC was characterized by SEM, EDX, FTIR, TGA, and BET surface area and pore size analyzer. The potential of AC as a catalyst for solvent-free oxidation of cyclohexane to cyclohexanol and cyclohexanone (the mixture is known as KA oil in the presence of molecular oxygen at moderate temperature was investigated in a self-designed double-walled three-necked batch reactor. The effect of different reaction parameters/additive was optimized. The maximum productivity value (2.14 mmolg−1 h−1, without base, and 4.85 mmolg−1 h−1, with 0.2 mmol NaOH of the desired product was achieved under optimal reaction parameters: vol 12.5 mL, cat 0.4 g, time 14 h, oxygen flow 40 mL/min (pO2 760 Torr, stirring 1100 rpm, and temp 75°C. The AC shows recyclability for multiple runs without any significant loss in activity. Thus, the AC can be an efficient catalyst, due to low cost, ease of synthesis, easy recovery, nonleaching, and recyclability for multiple uses for the solvent-free oxidation of cyclohexane.

  14. Solvent-free functionalization of carbon nanotube buckypaper with amines

    International Nuclear Information System (INIS)

    Basiuk, Elena V.; Ramírez-Calera, Itzel J.; Meza-Laguna, Victor; Abarca-Morales, Edgar; Pérez-Rey, Luis A.; Re, Marilena; Prete, Paola; Lovergine, Nico

    2015-01-01

    Graphical abstract: - Abstract: We demonstrate the possibility of fast and efficient solvent-free functionalization of buckypaper (BP) mats prefabricated from oxidized multiwalled carbon nanotubes (MWCNTs-ox), by using three representative amines of different structure: one monofunctional aliphatic amine, octadecylamine (ODA), one monofunctional aromatic amine, 1-aminopyrene (AP), and one aromatic diamine, 1,5-diaminonaphthalene (DAN). The functionalization procedure, which relies on the formation of amide bonds with carboxylic groups of MWCNTs-ox, is performed at 150–180 °C under reduced pressure and takes about 4 h including auxiliary degassing. The amine-treated BP samples (BP-ODA, BP-AP and BP-DAN, respectively) were characterized by means of a variety of analytical techniques such as Fourier-transform infrared and Raman spectroscopy, thermogravimetric and differential thermal analysis, scanning and transmission electron microscopy, scanning helium ion microscopy, and atomic force microscopy. The highest amine content was found for BP-ODA, and the lowest one was observed for BP-DAN, with a possible contribution of non-covalently bonded amine molecules in all three cases. Despite of some differences in spectral and morphological characteristics for amine-functionalized BP samples, they have in common a dramatically increased stability in water as compared to pristine BP and, on the other hand, a relatively invariable electrical conductivity.

  15. Solvent-free covalent functionalization of nanodiamond with amines

    International Nuclear Information System (INIS)

    Basiuk, Elena V.; Santamaría-Bonfil, Adriana; Meza-Laguna, Victor; Gromovoy, Taras Yu.; Alvares-Zauco, Edgar; Contreras-Torres, Flavio F.; Rizo, Juan; Zavala, Guadalupe; Basiuk, Vladimir A.

    2013-01-01

    Covalent functionalization of pristine nanodiamond (ND) with 1,12-diaminododecane (DAD), 1,5-diaminonaphthalene (DAN), poly(ethylene glycol) diamine (PEGDA), and polyethylenimine (PEI) was carried out by employing solvent-free methodology, which is based on thermal instead of chemical activation of carboxylic groups at ND surface. A simple solubility/dispersibility test in water and isopropanol showed an increased lipophilicity of the functionalized samples. The conversion of intrinsic carboxylic groups into the corresponding amide derivatives was characterized by means of Fourier-transform infrared spectroscopy. Thermogravimetric analysis found the highest organic content of about 18% for ND-PEI, followed by ND-DAD, for which the contribution of covalently bonded diamine was estimated to be of ca. 10%. In temperature programmed desorption measurements with mass spectrometric detection, the presence of organic functionalizing groups changed both mass spectra and thermodesorption curves of ND. The changes in morphology of primary and secondary ND aggregates were characterized by scanning and transmission electron microscopy, as well as by atomic force microscopy. The current–voltage measurements under atmospheric pressure found an increased conductivity for ND-DAN, as compared to that of pristine ND, whereas for ND-DAD, ND-PEGDA and ND-PEI a dramatic decrease in conductivity due to functionalization was observed.

  16. Solvent-free covalent functionalization of nanodiamond with amines

    Energy Technology Data Exchange (ETDEWEB)

    Basiuk, Elena V., E-mail: elenagd@unam.mx [Centro de Ciencias Aplicadas y Desarrollo Tecnológico, Universidad Nacional Autónoma de México, Circuito Exterior, Ciudad Universitaria, 04510 México D.F. (Mexico); Santamaría-Bonfil, Adriana; Meza-Laguna, Victor [Centro de Ciencias Aplicadas y Desarrollo Tecnológico, Universidad Nacional Autónoma de México, Circuito Exterior, Ciudad Universitaria, 04510 México D.F. (Mexico); Gromovoy, Taras Yu. [Institute of Surface Chemistry, National Academy of Sciences of the Ukraine, Gen. Naumova 17, 03164 Kiev (Ukraine); Alvares-Zauco, Edgar [Facultad de Ciencias, Universidad Nacional Autónoma de México, Circuito Exterior, Ciudad Universitaria, 04510 México D.F. (Mexico); Contreras-Torres, Flavio F.; Rizo, Juan [Centro de Ciencias Aplicadas y Desarrollo Tecnológico, Universidad Nacional Autónoma de México, Circuito Exterior, Ciudad Universitaria, 04510 México D.F. (Mexico); Zavala, Guadalupe [Instituto de Biotecnología, Universidad Nacional Autónoma de México, Av. Universidad 2001, Col. Chamilpa, 62210, Cuernavaca, Morelos (Mexico); Basiuk, Vladimir A. [Instituto de Ciencias Nucleares, Universidad Nacional Autónoma de México, Circuito Exterior, Ciudad Universitaria, 04510 México, D.F. (Mexico)

    2013-06-15

    Covalent functionalization of pristine nanodiamond (ND) with 1,12-diaminododecane (DAD), 1,5-diaminonaphthalene (DAN), poly(ethylene glycol) diamine (PEGDA), and polyethylenimine (PEI) was carried out by employing solvent-free methodology, which is based on thermal instead of chemical activation of carboxylic groups at ND surface. A simple solubility/dispersibility test in water and isopropanol showed an increased lipophilicity of the functionalized samples. The conversion of intrinsic carboxylic groups into the corresponding amide derivatives was characterized by means of Fourier-transform infrared spectroscopy. Thermogravimetric analysis found the highest organic content of about 18% for ND-PEI, followed by ND-DAD, for which the contribution of covalently bonded diamine was estimated to be of ca. 10%. In temperature programmed desorption measurements with mass spectrometric detection, the presence of organic functionalizing groups changed both mass spectra and thermodesorption curves of ND. The changes in morphology of primary and secondary ND aggregates were characterized by scanning and transmission electron microscopy, as well as by atomic force microscopy. The current–voltage measurements under atmospheric pressure found an increased conductivity for ND-DAN, as compared to that of pristine ND, whereas for ND-DAD, ND-PEGDA and ND-PEI a dramatic decrease in conductivity due to functionalization was observed.

  17. Solvent-free ZnO dye-sensitised solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Guillen, E.; Anta, J.A. [Departamento de Sistemas Fisicos, Quimicos y Naturales, Universidad Pablo de Olavide, 41013 Sevilla (Spain); Fernandez-Lorenzo, C.; Alcantara, R.; Martin-Calleja, J. [Departamento de Quimica Fisica, Universidad de Cadiz, Cadiz (Spain)

    2009-10-15

    Dye-sensitised solar cells (DSSC) based on commercial nanostructured zinc oxide combined with imidazolium-based room temperature ionic-liquid electrolytes are characterized. The electrolytes are based on a binary mixture of two ionic liquids, one of them used as source of iodide ions. The composition of this solvent-free electrolyte is optimized with respect to the concentration of iodine and iodide and the effect of additives such as lithium and tert-butylpyridine (TBP) on the photovoltaic performance and the recombination rate is analyzed and discussed. A maximum photoconversion efficiency of 3.4% at 1 sun illumination has been obtained for cells of 0.64 cm{sup 2} active area with the best performing compositions. Diffusion limitations due to slow transport processes are analyzed and discussed. (author)

  18. Synthesis of quinoxaline 1,4-di-n-oxide derivatives on solid support using room temperature and microwave-assisted solvent-free procedures

    International Nuclear Information System (INIS)

    Gomez-Caro, Lilia C.; Sanchez-Sanchez, Mario; Bocanegra-Garcia, Virgilio; Rivera, Gildardo; Monge, Antonio

    2011-01-01

    We describe the synthesis of 12 new ethyl and methyl quinoxaline-7-carboxylate 1,4-di-N-oxide derivatives on solid supports with room temperature and microwave-assisted solvent-free procedures. Results show that solid supports have good catalytic activity in the formation of quinoxaline 1,4-di-N-oxide derivatives. We found that florisil and montmorillonite KSF and K10 could be used as new, easily available, inexpensive alternatives of catalysts. Additionally, room temperature and microwave-irradiation solvent-free synthesis was more efficient than a conventional procedure (Beirut reaction), reducing reaction time and increasing yield. (author)

  19. Synthesis of quinoxaline 1,4-di-n-oxide derivatives on solid support using room temperature and microwave-assisted solvent-free procedures

    Energy Technology Data Exchange (ETDEWEB)

    Gomez-Caro, Lilia C.; Sanchez-Sanchez, Mario; Bocanegra-Garcia, Virgilio; Rivera, Gildardo [Universidad Autonoma de Tamaulipas, Reynosa (Mexico). Dept. de Farmacia y Quimica Medicinal; Monge, Antonio [Universidad de Navarra, Pamplona (Spain). Centro de Investigacion en Farmacobiologia Aplicada. Unidad de Investigacion y Desarrollo de Medicamentos

    2011-07-01

    We describe the synthesis of 12 new ethyl and methyl quinoxaline-7-carboxylate 1,4-di-N-oxide derivatives on solid supports with room temperature and microwave-assisted solvent-free procedures. Results show that solid supports have good catalytic activity in the formation of quinoxaline 1,4-di-N-oxide derivatives. We found that florisil and montmorillonite KSF and K10 could be used as new, easily available, inexpensive alternatives of catalysts. Additionally, room temperature and microwave-irradiation solvent-free synthesis was more efficient than a conventional procedure (Beirut reaction), reducing reaction time and increasing yield. (author)

  20. Solvent-free Oxidation of Alcohols and Mild Catalytic Deprotection of ...

    African Journals Online (AJOL)

    tetrabromobenzene- 1,3-disulphonamide (TBBDA) can be used for solvent-free oxidation of primary and secondary alcohols to the corresponding carbonyl compounds without over-oxidation, and efficient catalytic deprotection of various silyl ...

  1. Grinding solvent-free Paal-Knorr pyrrole synthesis on smectites as ...

    African Journals Online (AJOL)

    Journal Home > Vol 32, No 1 (2018) > ... An environmentally benign method for the synthesis of N-substituted pyrroles from one-pot solvent-free ... conditions make this protocol practical, environmentally friendly and economically attractive.

  2. Multicomponent One-Pot Synthesis of Substituted Hantzsch Thiazole Derivatives Under Solvent Free Conditions

    Directory of Open Access Journals (Sweden)

    Bhaskar S. Dawane

    2009-01-01

    Full Text Available Thiazole derivatives were prepared by one-pot procedure by the reaction of α-haloketones, thiourea and substituted o-hydroxybenzaldehyde under environmentally solvent free conditions.

  3. Solvent-free synthesis of nanosized hierarchical sodalite zeolite with a multi-hollow polycrystalline structure

    KAUST Repository

    Zeng, Shangjing; Wang, Runwei; Li, Ang; Huang, Weiwei; Zhang, Zongtao; Qiu, Shilun

    2016-01-01

    A solvent-free route is developed for preparing nanoscale sodalite zeolite with a multi-hollow structure. Furthermore, the synthesis of nanosized hollow sodalite polycrystalline aggregates with a mesoporous structure and high crystallinity

  4. Microwave-assisted silica-promoted solvent-free synthesis of ...

    Indian Academy of Sciences (India)

    method using microwave irradiation with an excellent yield. The newly ... Table 1. Silica promoted microwave-assisted solvent-free synthesis of quinazolinone ... Time (min). Yield (%)a ..... thanks SC/ST cell of Bangalore University for research.

  5. Multicomponent Synthesis of Isoindolinone Frameworks via RhIII -Catalysed in situ Directing Group-Assisted Tandem Oxidative Olefination/Michael Addition.

    Science.gov (United States)

    Wang, Liang; Liu, Xi; Liu, Jian-Biao; Shen, Jun; Chen, Qun; He, Ming-Yang

    2018-04-04

    A Rh III -catalysed three-component synthesis of isoindolinone frameworks via direct assembly of benzoyl chlorides, o-aminophenols and activated alkenes has been developed. The process involves in situ generation of o-aminophenol (OAP)-based bidentate directing group (DG), Rh III -catalysed tandem ortho C-H olefination and subsequent cyclization via aza-Michael addition. This protocol exhibits good chemoselectivity and functional group tolerance. Computational studies showed that the presence of hydroxyl group on the N-aryl ring could enhance the chemoselectivity of the reaction. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Solvent Free Preparation of p-Cymene from Limonene Using Vietnamese Montmorillonite

    DEFF Research Database (Denmark)

    Nguyen, Thao-Tran Thi; Duus, Fritz; Le, Thach Ngoc

    2013-01-01

    p-Cymene, an important intermediate in industrial chemistry, has been prepared in good yields by thermally induced dehydrogenation of limonene under solvent-free reaction conditions using Vietnamese montmorillonite as an efficient green catalyst.......p-Cymene, an important intermediate in industrial chemistry, has been prepared in good yields by thermally induced dehydrogenation of limonene under solvent-free reaction conditions using Vietnamese montmorillonite as an efficient green catalyst....

  7. Surface functionalization of SBA-15 by the solvent-free method

    International Nuclear Information System (INIS)

    Wang Yimeng; Zheng Yingwu; Zhu Jianhua

    2004-01-01

    A solvent-free technique was employed for fast modification of mesoporous materials. Copper, chromium and iron oxide species could be highly dispersed in SBA-15 by manually grinding the corresponding precursor salts and the host, followed by calcinations for the first time. This method is more effective to spontaneously disperse oxide species onto SBA-15 than impregnation, probably forming monolayer or submonolayer dispersion of salts or oxides. Besides, Cr(VI) species dominate in the mixing sample while Cr(III) species dominate in the impregnation one. In the temperature programmed surface reaction of nitrosamines, the sample prepared by solvent-free method showed a higher catalytic activity than the impregnation one

  8. Preparation of Ultra-fine Calcium Carbonate by a Solvent-free ...

    African Journals Online (AJOL)

    The treatment of calcium chloride with sodium carbonate under solvent-free conditions with a supersonic airflow and at a low heating temperature leads to the synthesis of ultra-fine calcium carbonate. The reaction not only involves mild conditions, a simple operation, and high yields but also gives a high conversion rate.

  9. Solvent-free synthesis of nanosized hierarchical sodalite zeolite with a multi-hollow polycrystalline structure

    KAUST Repository

    Zeng, Shangjing

    2016-08-03

    A solvent-free route is developed for preparing nanoscale sodalite zeolite with a multi-hollow structure. Furthermore, the synthesis of nanosized hollow sodalite polycrystalline aggregates with a mesoporous structure and high crystallinity is investigated by adding an organosilane surfactant as a mesopore-generating agent.

  10. A Highly Efficient Solvent-Free Acetalization of Aldehydes to 1,1 ...

    African Journals Online (AJOL)

    1,1-Diacetates are prepared in excellent yields from aldehydes and acetic anhydride under solvent-free conditions at room temperature in short reaction times using catalytic amount of sulfonic acid functionalized silica (SiO2-Pr-SO3H) which could be easily handled and removed from the mixture of reaction. Keywords: 1 ...

  11. Predicting the Disorder–Order Transition of Solvent-Free Nanoparticle–Organic Hybrid Materials

    KAUST Repository

    Yu, Hsiu-Yu; Koch, Donald L.

    2013-01-01

    in the ordered phase, the cooperation of the oligomers in filling the space is hindered. Therefore, shorter oligomers feel a stronger entropic penalty in the ordered solid and favor the disordered phase. Strikingly, we found that the solvent-free system has a

  12. Solvent-free porous framework resulted from 3D entanglement of 1D zigzag coordination polymer

    KAUST Repository

    Kole, Goutam Kumar Umar

    2010-01-01

    A solvent-free porous metal organic framework is constructed by the 3D entanglement of 1D zigzag coordination polymeric chains. The role of solvents and the effect of reaction conditions on such unique entanglement are addressed. © 2010 The Royal Society of Chemistry and the Centre National de la Recherche Scientifique.

  13. An Expedient Method for the Synthesis of Thiosemicarbazones under Microwave Irradiation in Solvent-free Medium

    Institute of Scientific and Technical Information of China (English)

    LI, Jian-Ping; ZHENG, Peng-Zhi; ZHU, Jun-Ge; LIU, Rui-Jie; QU, Gui-Rong

    2006-01-01

    A simple, efficient and eco-friendly method for the synthesis of thiosemicarbazones from thiosemicarbazides and aldehyde under microwave irradiation has been reported, and no solvent and catalyst were used. And the technique of microwave irradiation coupled with solvent-free condition proved to be a quite valuable method in the organic synthesis.

  14. Solvent-Free Wittig Reaction: A Green Organic Chemistry Laboratory Experiment

    Science.gov (United States)

    Leung, Sam H.; Angel, Stephen A.

    2004-01-01

    Some Wittig reactions can be carried out by grinding the reactants in a mortar with a pestle for about 20 minutes, as per investigation. A laboratory experiment involving a solvent-free Wittig reaction that can be completed in a three-hour sophomore organic chemistry laboratory class period, are developed.

  15. Solvent-free microwave extraction of essential oil from Melaleuca leucadendra L.

    Directory of Open Access Journals (Sweden)

    Widya Ismanto Aviarina

    2018-01-01

    Full Text Available Cajuput (Melaleuca leucadendra L. oil is one of potential commodity that provides an important role for the country’s foreign exchange but the extraction of these essential oil is still using conventional method such as hydrodistillation which takes a long time to produce essential oil with good quality. Therefore it is necessary to optimize the extraction process using a more effective and efficient method. So in this study the extraction is done using solvent-free microwave extraction method that are considered more effective and efficient than conventional methods. The optimum yield in the extraction of cajuput oil using solvent-free microwave extraction method is 1.0674%. The optimum yield is obtained on the feed to distiller (F/D ratio of 0.12 g/mL with microwave power of 400 W. In the extraction of cajuput oil using solvent-free microwave extraction method is performed first-order and second-order kinetics modelling. Based on kinetics modelling that has been done, it can be said that the second-order kinetic model (R2 = 0.9901 can be better represent experimental results of extraction of cajuput oil that using solvent-free microwave extraction method when compared with the first-order kinetic model (R2 = 0.9854.

  16. Solvent-free porous framework resulted from 3D entanglement of 1D zigzag coordination polymer

    KAUST Repository

    Kole, Goutam Kumar Umar; Cairns, Amy J.; Eddaoudi, Mohamed; Vittal, Jagadese J.

    2010-01-01

    A solvent-free porous metal organic framework is constructed by the 3D entanglement of 1D zigzag coordination polymeric chains. The role of solvents and the effect of reaction conditions on such unique entanglement are addressed. © 2010 The Royal

  17. Solvent free amorphisation for pediatric formulations (minitablets) using mesoporous silica

    DEFF Research Database (Denmark)

    Monsuur, Fred; Choudhari, Yogesh; Reddy, Upendra

    2016-01-01

    Introduction: Most silica based amorphisation strategies are using organic solvent loading methods. Towards pediatric formulations this is creating concerns. With this in mind the development of a dry amorphisation strategy was the focus of this study. The high internal surface area of mesoporous...... silica gel is densely crowded with silanol groups, which can provide hydrogen-bonding possibilities with a drug, potentially resulting in amorphisation. Purpose: Amorphous drugs provide an advantage in solubility; however, their low physical stability always remained concern. Additional there was a need...... to understand the mechanism and variables of dry amorphisation. Method: Ibuprofen (IBU) and Syloid® silica at different ratios were co-milled at variable milling times between 1 and 90 min. The interaction with; and amorphisation of IBU; on Syloid® silica was analyzed using SEM, FTIR, DSC and XRD. The co...

  18. Solvent-free functionalization of fullerene C{sub 60} and pristine multi-walled carbon nanotubes with aromatic amines

    Energy Technology Data Exchange (ETDEWEB)

    Ramírez-Calera, Itzel J. [Centro de Ciencias Aplicadas y Desarrollo Tecnológico, Universidad Nacional Autónoma de México, Circuito Exterior C. U., 04510, México, D.F. (Mexico); Meza-Laguna, Victor [Instituto de Ciencias Nucleares, Universidad Nacional Autónoma de México, Circuito Exterior C. U., 04510 México, D.F. (Mexico); Gromovoy, Taras Yu. [O.O. Chuiko Institute of Surface Chemistry, National Academy of Sciences of the Ukraine, Gen. Naumova 17, 03164 Kiev (Ukraine); Chávez-Uribe, Ma. Isabel [Instituto de Química, Universidad Nacional Autónoma de México, Circuito Exterior C. U., 04510 México, D.F. (Mexico); Basiuk, Vladimir A., E-mail: basiuk@nucleares.unam.mx [Instituto de Ciencias Nucleares, Universidad Nacional Autónoma de México, Circuito Exterior C. U., 04510 México, D.F. (Mexico); Basiuk, Elena V., E-mail: elbg1111@gmail.com [Centro de Ciencias Aplicadas y Desarrollo Tecnológico, Universidad Nacional Autónoma de México, Circuito Exterior C. U., 04510, México, D.F. (Mexico)

    2015-02-15

    Highlights: • Pristine multi-walled carbon nanotubes were functionalized with aromatic amines. • The amines add onto nanotube defects, likewise they add onto fullerene C{sub 60}. • The addition takes place at elevated temperature and without organic solvents. • Functionalized nanotubes were characterized by a number of instrumental techniques. - Abstract: We employed a direct one-step solvent-free covalent functionalization of solid fullerene C{sub 60} and pristine multi-walled carbon nanotubes (MWCNTs) with aromatic amines 1-aminopyrene (AP), 2-aminofluorene (AF) and 1,5-diaminonaphthalene (DAN). The reactions were carried out under moderate vacuum, in a wide temperature range of 180–250 °C, during relatively short time of about 2 h. To confirm successful amine attachment, a large number of analytical techniques were used (depending on the nanomaterial functionalized) such as Fourier transform infrared, Raman, X-ray photoelectron, {sup 13}C cross-polarization magic angle spinning NMR spectroscopy, thermogravimetric analysis, laser-desorption ionization time-of-flight mass spectrometry, temperature-programmed desorption with mass spectrometric detection, as well as scanning and transmission electron microscopy. The nucleophilic addition of the aromatic amines to C{sub 60} molecule was studied theoretically by using density functional theory (PBE GGA functional with Grimme dispersion correction in conjunction with the DNP basis set). In the case of crystalline C{sub 60}, the solvent-free technique has a limited applicability due to poor diffusion of vaporous aromatic amines into the bulk. Nevertheless, the approach proposed allows for a facile preparation of aromatic amine-functionalized pristine MWCNTs without contamination with other chemical reagents, detergents and solvents, which is especially important for a vast variety of nanotube applications spanning from nanoelectronics to nanomedicine.

  19. Predicting the Disorder–Order Transition of Solvent-Free Nanoparticle–Organic Hybrid Materials

    KAUST Repository

    Yu, Hsiu-Yu

    2013-07-02

    The transition from a disordered to a face-centered-cubic phase in solvent-free oligomer-tethered nanoparticles is predicted using a density-functional theory for model hard spheres with tethered bead-spring oligomers. The transition occurs without a difference of volume fraction for the two phases, and the phase boundary is influenced by the loss of oligomer configurational entropy relative to an ideal random system in one phase compared with the other. When the particles are localized in the ordered phase, the cooperation of the oligomers in filling the space is hindered. Therefore, shorter oligomers feel a stronger entropic penalty in the ordered solid and favor the disordered phase. Strikingly, we found that the solvent-free system has a later transition than hard spheres for all investigated ratios of oligomer radius of gyration to particle radius. © 2013 American Chemical Society.

  20. Solvent-free preparation of co-crystals of phenazine and acridine with vanillin

    Energy Technology Data Exchange (ETDEWEB)

    Braga, Dario, E-mail: dario.braga@unibo.it [Dipartimento di Chimica ' G.Ciamician' , Universita degli studi di Bologna, Via Selmi 2, 40126 Bologna (Italy); Grepioni, Fabrizia; Maini, Lucia; Mazzeo, Paolo P.; Rubini, Katia [Dipartimento di Chimica ' G.Ciamician' , Universita degli studi di Bologna, Via Selmi 2, 40126 Bologna (Italy)

    2010-08-10

    Co-crystals of phenazine and acridine with vanillin have been obtained by solvent-free reaction or thermal treatment of the solid reactants: their structures, thermal behaviour and eutectic formation have been investigated via single crystal X-ray diffraction, differential scanning calorimetry (DSC), variable temperature X-ray powder diffraction and hot-stage microscopy (HSM). Polymorph screening of the reagents has also been carried out.

  1. An Efficient, Mild and Solvent-Free Synthesis of Benzene Ring Acylated Harmalines

    Directory of Open Access Journals (Sweden)

    Sabira Begum

    2009-12-01

    Full Text Available A facile synthesis of a series of benzene ring acylated analogues of harmaline has been achieved by Friedel-Crafts acylation under solvent-free conditions at room temperature using acyl halides/acid anhydrides and AlCl3. The reaction afforded 10- and 12-acyl analogues of harmaline in good yield, along with minor quantities of N-acyl-tryptamines and 8-acyl analogues of N-acyltryptamines.

  2. Fe–Al/clay as an efficient heterogeneous catalyst for solvent-free ...

    Indian Academy of Sciences (India)

    SiO2,27 amberlyst-15,28 etc. ... tometer, using Ni-filtered Cu Ka (0.15418 nm) radia- ... The spectral data of some ... C).29 1H NMR ... 3.99(q, j = 7.1 Hz, 2H), 5.12 (s,1H), 7.23 (d, j = 8.35 .... Recyclability was studied in both solvent-free and.

  3. Acid catalyzed solvent free synthesis of new 1-acyl-4-benzhydryl substituted pyrazoles

    International Nuclear Information System (INIS)

    Sher, M.; Kausar, T.; Riaz, N.; Sharif, A.

    2016-01-01

    A convenient, cost effective and environmentally benign methodology has been developed, which delivered fourteen new 1-acyl-4-benzhyrdyl substituted pyrazole derivatives under solvent free conditions. Target compounds were synthesized in good to excellent yields simply by grinding reactants in a pestle and mortar with catalytic amount of conc. H/sub 2/SO/sub 4/. All the newly formed compounds were fully characterized with the help of detailed spectroscopic techniques including FTIR, NMR and GC-MS. (author)

  4. Solvent-free, visible-light photocatalytic alcohol oxidations applying an organic photocatalyst

    Directory of Open Access Journals (Sweden)

    Martin Obst

    2016-11-01

    Full Text Available A method for the solvent-free photocatalytic conversion of solid and liquid substrates was developed, using a novel rod mill apparatus. In this setup, thin liquid films are realized which is crucial for an effective photocatalytic conversion due to the low penetration depth of light in heterogeneous systems. Several benzylic alcohols were oxidized with riboflavin tetraacetate as photocatalyst under blue light irradiation of the reaction mixture. The corresponding carbonyl compounds were obtained in moderate to good yields.

  5. Solvent free oxidation of primary alcohols and diols using thymine iron(III) catalyst.

    Science.gov (United States)

    Al-Hunaiti, Afnan; Niemi, Teemu; Sibaouih, Ahlam; Pihko, Petri; Leskelä, Markku; Repo, Timo

    2010-12-28

    In this study, we developed an efficient and selective iron-based catalyst system for the synthesis of ketones from secondary alcohols and carboxylic acids from primary alcohol. In situ generated iron catalyst of thymine-1-acetate (THA) and FeCl(3) under solvent-free condition exhibits high activity. As an example, 1-octanol and 2-octanol were oxidized to 1-octanoic acid and 2-octanone with 89% and 98% yields respectively.

  6. Solvent-free preparation of co-crystals of phenazine and acridine with vanillin

    International Nuclear Information System (INIS)

    Braga, Dario; Grepioni, Fabrizia; Maini, Lucia; Mazzeo, Paolo P.; Rubini, Katia

    2010-01-01

    Co-crystals of phenazine and acridine with vanillin have been obtained by solvent-free reaction or thermal treatment of the solid reactants: their structures, thermal behaviour and eutectic formation have been investigated via single crystal X-ray diffraction, differential scanning calorimetry (DSC), variable temperature X-ray powder diffraction and hot-stage microscopy (HSM). Polymorph screening of the reagents has also been carried out.

  7. Innovative polymeric system (IPS) for solvent-free lipophilic drug transdermal delivery via dissolving microneedles.

    Science.gov (United States)

    Dangol, Manita; Yang, Huisuk; Li, Cheng Guo; Lahiji, Shayan Fakhraei; Kim, Suyong; Ma, Yonghao; Jung, Hyungil

    2016-02-10

    Lipophilic drugs are potential drug candidates during drug development. However, due to the need for hazardous organic solvents for their solubilization, these drugs often fail to reach the pharmaceutical market, and in doing so highlight the importance of solvent free systems. Although transdermal drug delivery systems (TDDSs) are considered prospective safe drug delivery routes, a system involving lipophilic drugs in solvent free or powder form has not yet been described. Here, we report, for the first time, a novel approach for the delivery of every kind of lipophilic drug in powder form based on an innovative polymeric system (IPS). The phase transition of powder form of lipophilic drugs due to interior chemical bonds between drugs and biodegradable polymers and formation of nano-sized colloidal structures allowed the fabrication of dissolving microneedles (DMNs) to generate a powerful TDDS. We showed that IPS based DMN with powder capsaicin enhances the therapeutic effect for treatment of the rheumatic arthritis in a DBA/1 mouse model compared to a solvent-based system, indicating the promising potential of this new solvent-free platform for lipophilic drug delivery. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. In-Vitro Characterization and Oral Bioavailability of Organic Solvent-free Solid Dispersions Containing Telmisartan

    DEFF Research Database (Denmark)

    Cao, Yue; Shi, Li-Li; Cao, Qing-Ri

    2016-01-01

    Poorly water-soluble drugs often suffer from limited or irreproducible clinical response due to their low solubility and dissolution rate. In this study, organic solvent-free solid dispersions (OSF-SDs) containing telmisartan (TEL) were prepared using polyvinylpyrrolidone K30 (PVP K30....... The results from DSC, XRD showed that TEL was molecularly dispersed in the OSF-SDs as an amorphous form. The FT-IR results suggested that intermolecular hydrogen bonding had formed between TEL and its carriers. The OSF-SDs exhibited significantly higher AUC0-24 h and Cmax, but similar Tmax as compared...

  9. Silica Gel-Mediated Organic Reactions under Organic Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Satoaki Onitsuka

    2012-09-01

    Full Text Available Silica gel was found to be an excellent medium for some useful organic transformations under organic solvent-free conditions, such as (1 the Friedel-Crafts-type nitration of arenes using commercial aqueous 69% nitric acid alone at room temperature, (2 one-pot Wittig-type olefination of aldehydes with activated organic halides in the presence of tributyl- or triphenylphosphine and Hunig’s base, and (3 the Morita-Baylis-Hillman reaction of aldehydes with methyl acrylate. After the reactions, the desired products were easily obtained in good to excellent yields through simple manipulation.

  10. Synthesis and characterization of solvent-free ionic molybdenum disulphide (MoS2) nanofluids

    International Nuclear Information System (INIS)

    Gu, Shu-Ying; Gao, Xie-Feng; Zhang, Yi-Han

    2015-01-01

    A development of the novel and stable solvent-free ionic MoS 2 nanofluids by a facile and scalable hydrothermal method is presented. The nanofluids were synthesized by surface functionalizing nanoscale MoS 2 from hydrothermal synthesis with a charged corona, and ionically tethering with oligomeric chains as a canopy. The structures and properties of the nanofluids were characterized by Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR, 1 H), differential scanning calorimeter (DSC), thermogravimetric analysis (TGA) and ARES rheometer. The obtained solvent-free nanofluids are homogeneous, stable amber-like fluids with no evidence of phase separation. The nanofluids could be easily dispersed in both aqueous and organic solvents to form transparent and stable liquids due to the ionic nature and the presence of oligomeric polymer chains. It was found that the solvent-free nanofluids with up to 32 wt% inorganic content show Newtonian rheological behaviors due to the high graft density and uniform dispersion of inorganic cores, indicating that the nanofluids would have a stable lubricating performance. As reported in our previous communication, the nanofluids showing lower, more stable friction coefficients of less than 0.1 with self-healing lubricating behaviors. For deeper understanding of the nanofluids, the details of synthesis, chemical structures, rheological behaviors and molecular dynamics of the nanofluids were investigated in details. The rheological behaviors can be tailored by varying the grafting density of the canopy. Dynamic results of the canopy of the MoS 2 nanofluids show that inorganic MoS 2 cores have hindrance effect on the canopy segmental motions above 253 K due to their effect to the mobility of anions and the departing-recombining motions between the paired cations and anions. - Highlights: • A development of the novel synthesis of solvent-free MoS 2 nanofluids is presented. • The rheological behaviors can be tailored by

  11. A Solvent-Free Base Liberation of a Tertiary Aminoalkyl Halide by Flow Chemistry

    DEFF Research Database (Denmark)

    Pedersen, Michael Jønch; Skovby, Tommy; Mealy, Michael J.

    2016-01-01

    A flow setup for base liberation of 3-(N,N-dimethylamino)propyl chloride hydrochloride and solvent-free separation of the resulting free base has been developed. Production in flow profits from an on-demand approach, useful for labile aminoalkyl halides. The requirement for obtaining a dry product...... has been fulfilled by the simple use of a saturated NaOH solution, followed by isolation of the liquid phases by gravimetric separation. The flow setup has an E factor reduction of nearly 50%, and a distillation step has been avoided. The method exemplifies how flow chemistry can be exploited...

  12. Synthesis and characterization of solvent-free ionic molybdenum disulphide (MoS{sub 2}) nanofluids

    Energy Technology Data Exchange (ETDEWEB)

    Gu, Shu-Ying, E-mail: gushuying@tongji.edu.cn [School of Materials Science and Engineering, Tongji University, Shanghai 201804 (China); Key Laboratory of Advanced Civil Engineering Materials, Ministry of Education, School of Materials Science and Engineering, Tongji University, Shanghai 201804 (China); Gao, Xie-Feng; Zhang, Yi-Han [School of Materials Science and Engineering, Tongji University, Shanghai 201804 (China)

    2015-01-15

    A development of the novel and stable solvent-free ionic MoS{sub 2} nanofluids by a facile and scalable hydrothermal method is presented. The nanofluids were synthesized by surface functionalizing nanoscale MoS{sub 2} from hydrothermal synthesis with a charged corona, and ionically tethering with oligomeric chains as a canopy. The structures and properties of the nanofluids were characterized by Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR, {sup 1}H), differential scanning calorimeter (DSC), thermogravimetric analysis (TGA) and ARES rheometer. The obtained solvent-free nanofluids are homogeneous, stable amber-like fluids with no evidence of phase separation. The nanofluids could be easily dispersed in both aqueous and organic solvents to form transparent and stable liquids due to the ionic nature and the presence of oligomeric polymer chains. It was found that the solvent-free nanofluids with up to 32 wt% inorganic content show Newtonian rheological behaviors due to the high graft density and uniform dispersion of inorganic cores, indicating that the nanofluids would have a stable lubricating performance. As reported in our previous communication, the nanofluids showing lower, more stable friction coefficients of less than 0.1 with self-healing lubricating behaviors. For deeper understanding of the nanofluids, the details of synthesis, chemical structures, rheological behaviors and molecular dynamics of the nanofluids were investigated in details. The rheological behaviors can be tailored by varying the grafting density of the canopy. Dynamic results of the canopy of the MoS{sub 2} nanofluids show that inorganic MoS{sub 2} cores have hindrance effect on the canopy segmental motions above 253 K due to their effect to the mobility of anions and the departing-recombining motions between the paired cations and anions. - Highlights: • A development of the novel synthesis of solvent-free MoS{sub 2} nanofluids is presented. • The rheological

  13. Solvent free one pot synthesis of amidoalkyl naphthols over phosphotungstic acid

    Directory of Open Access Journals (Sweden)

    Divya P. Narayanan

    2017-07-01

    Full Text Available Montmorillonite KSF clay was effectively modified by the encapsulation of phosphotungstic acid into the clay layers via sonication followed by incipient wet impregnation method. The prepared catalysts were characterized by X-ray diffraction (XRD, Fourier-transform infrared spectroscopy (FTIR and scanning electron microscopy (SEM techniques. The catalytic activities of the prepared systems were investigated in the solvent free synthesis of amidoalkyl naphthols by the multicomponent one-pot condensation of an aldehyde, β-naphthol and an amide or urea. Excellent yield, shorter reaction time, easy work-up, and reusability of the catalyst are the main attractions of this green procedure.

  14. A three-dimensional graphene aerogel containing solvent-free polyaniline fluid for high performance supercapacitors.

    Science.gov (United States)

    Gao, Zhaodongfang; Yang, Junwei; Huang, Jing; Xiong, Chuanxi; Yang, Quanling

    2017-11-23

    Conducting polymer based supercapacitors usually suffer from the difficulty of achieving high specific capacitance and good long-term stability simultaneously. In this communication, a long-chain protonic acid doped solvent-free self-suspended polyaniline (S-PANI) fluid and reduced graphene oxide (RGO) were used to fabricate a three-dimensional RGO/S-PANI aerogel via a simple self-assembled hydrothermal method, which was then applied as a supercapacitor electrode. This 3D RGO/S-PANI composite exhibited a high specific capacitance of up to 480 F g -1 at a current density of 1 A g -1 and 334 F g -1 even at a high discharge rate of 40 A g -1 . An outstanding cycling performance, with 96.14% of the initial capacitance remaining after 10 000 charging/discharging cycles at a rate of 10 A g -1 , was also achieved. Compared with the conventional conducting polymer materials, the 3D RGO/S-PANI composite presented more reliable rate capability and cycling stability. Moreover, S-PANI possesses excellent processability, thereby revealing its enormous potential in large scale production. We anticipate that the solvent-free fluid technique is also applicable to the preparation of other 3D graphene/polymer materials for energy storage.

  15. Antimicrobial nanocapsules: from new solvent-free process to in vitro efficiency

    Directory of Open Access Journals (Sweden)

    Steelandt J

    2014-09-01

    Full Text Available Julie Steelandt,1 Damien Salmon,1,2 Elodie Gilbert,1 Eyad Almouazen,3 François NR Renaud,4 Laurène Roussel,1 Marek Haftek,5 Fabrice Pirot1,2 1University Claude Bernard Lyon 1, Faculty of Pharmacy, Fundamental, Clinical and Therapeutic Aspects of Skin Barrier Function, FRIPharm, Laboratoire de Pharmacie Galénique Industrielle, 2Hospital Pharmacy, FRIPharm, Hospital Edouard Herriot, Hospices Civils de Lyon, 3Laboratoire d’Automatique et de Génie des Procédés, University Claude Bernard Lyon 1, 4University Claude Bernard Lyon 1, UMR CNRS 5510/MATEIS, 5University Claude Bernard Lyon 1, Faculty of Pharmacy, Fundamental, Clinical and Therapeutic Aspects of Skin Barrier Function, FRIPharm, Laboratoire de Dermatologie, Lyon, France Abstract: Skin and mucosal infections constitute recurrent pathologies resulting from either inappropriate antiseptic procedures or a lack of efficacy of antimicrobial products. In this field, nanomaterials offer interesting antimicrobial properties (eg, long-lasting activity; intracellular and tissular penetration as compared to conventional products. The aim of this work was to produce, by a new solvent-free process, a stable and easily freeze-dryable chlorhexidine-loaded polymeric nanocapsule (CHX-NC suspension, and then to assess the antimicrobial properties of nanomaterials. The relevance of the process and the physicochemical properties of the CHX-NCs were examined by the assessment of encapsulation efficiency, stability of the nanomaterial suspension after 1 month of storage, and by analysis of granulometry and surface electric charge of nanocapsules. In vitro antimicrobial activities of the CHX-NCs and chlorhexidine digluconate solution were compared by measuring the inhibition diameters of two bacterial strains (Escherichia coli and Staphylococcus aureus and one fungal strain (Candida albicans cultured onto appropriate media. Based on the findings of this study, we report a new solvent-free process for the

  16. PLLA-PHB fiber membranes obtained by solvent-free electrospinning for short-time drug delivery.

    Science.gov (United States)

    Cao, K; Liu, Y; Olkhov, A A; Siracusa, V; Iordanskii, A L

    2018-02-01

    Fibers of poly(L-lactic acid) (PLLA)/polyhydroxybutyrate (PHB) with different concentrations of the drug dipyridamole (DPD) were prepared using solvent-free melt electrospinning to obtain a polymeric drug delivery system. The electrospun fibers were morphologically, structurally, thermally, and dynamically characterized. Crazes that resemble lotus root crevices were interestingly observed in the 7:3 PLLA/PHB fibers with 1% DPD. The crystallinity of PLLA slightly decreased as PHB was incorporated, and the addition of DPD significantly reduced the melting temperature of the composite. The interactions between PLLA and PHB mainly occurred at a proportion of 7:3, and drug encapsulation in the fibers was verified. The kinetic profiles of drug release demonstrated the predominant multiple patterns involving a diffusional stage in the short-term mode of release and kinetic process related to the hydrolysis of the biopolymers. Furthermore, the dynamic behavior of the polymer molecules was evaluated based on the segmental mobility using probe electron spin resonance spectroscopy. The segmental mobility in the amorphous fraction of PLLA decreased with increasing PLLA content. The 9:1 PLLA/PHB system was more resistant to polymer hydrolysis than to the 7:3 system and the rate of diffusion transport was approximately two times higher for the 7:3 PLLA/PHB fibers than for the 9:1 PLLA/PHB fibers.

  17. Development of a new solvent-free flow efficiency coating for natural gas pipelines

    Energy Technology Data Exchange (ETDEWEB)

    Fogg, Graham A.; Morse, Jennifer [Bredero Shaw, Houston, TX (United States)

    2005-07-01

    Pipeline design engineers have traditionally considered external anti-corrosion coatings for the protection of gas transmission pipelines, with less consideration given to the benefits of internal flow efficiency coatings. This paper reviews the benefits of using a traditional solvent-based flow efficiency coating, and the relationship between the internal surface roughness of a pipe, the pressure drop across the pipeline, and the maximum flow rate of gas through the pipeline. To improve upon existing solvent-based flow efficiency coatings, a research program was undertaken to develop a solvent-free coating. The stages in the development of this coating are discussed, resulting in the plant application of the coating and final qualification to API RP 5L2. (author)

  18. Structure of solvent-free grafted nanoparticles: Molecular dynamics and density-functional theory

    KAUST Repository

    Chremos, Alexandros

    2011-01-01

    The structure of solvent-free oligomer-grafted nanoparticles has been investigated using molecular dynamics simulations and density-functional theory. At low temperatures and moderate to high oligomer lengths, the qualitative features of the core particle pair probability, structure factor, and the oligomer brush configuration obtained from the simulations can be explained by a density-functional theory that incorporates the configurational entropy of the space-filling oligomers. In particular, the structure factor at small wave numbers attains a value much smaller than the corresponding hard-sphere suspension, the first peak of the pair distribution function is enhanced due to entropic attractions among the particles, and the oligomer brush expands with decreasing particle volume fraction to fill the interstitial space. At higher temperatures, the simulations reveal effects that differ from the theory and are likely caused by steric repulsions of the expanded corona chains. © 2011 American Institute of Physics.

  19. Solvent-Free Patterning of Colloidal Quantum Dot Films Utilizing Shape Memory Polymers

    Directory of Open Access Journals (Sweden)

    Hohyun Keum

    2017-01-01

    Full Text Available Colloidal quantum dots (QDs with properties that can be tuned by size, shape, and composition are promising for the next generation of photonic and electronic devices. However, utilization of these materials in such devices is hindered by the limited compatibility of established semiconductor processing techniques. In this context, patterning of QD films formed from colloidal solutions is a critical challenge and alternative methods are currently being developed for the broader adoption of colloidal QDs in functional devices. Here, we present a solvent-free approach to patterning QD films by utilizing a shape memory polymer (SMP. The high pull-off force of the SMP below glass transition temperature (Tg in conjunction with the conformal contact at elevated temperatures (above Tg enables large-area, rate-independent, fine patterning while preserving desired properties of QDs.

  20. Olive oil glycero lysis with the immobilized lipase Candida antarctica in a solvent free system

    Energy Technology Data Exchange (ETDEWEB)

    Singh, A. K.; Mukhopadhyay, M.

    2012-11-01

    In the present work, the solvent free lipase glycerolysis of olive oil for the production of monoglyceride (MG) and diglyceride (DG) with an immobilized Lipase B Candida antarctica was studied. The experiments were performed in batch mode by varying different process parameters. The Results showed that the MG and DG yields were dependent on operating conditions such as time, temperature, glycerol/ oil molar ratio, enzyme concentration and the water content in glycerol. The optimum operating time for maximum MG, 26 wt% and DG, 30 wt% production was 3h. The initial reaction rate was studied by varying different process parameters for 1h. The initial reaction rate increased at 30 degree centigrade temperature, 2:1 glycerol/oil molar ratio, 3.5% (w/w) water content in glycerol and 0.015g of enzyme loading. Comparative data for MG and DG yields for different oils and enzyme combinations were presented.

  1. Solvent free low-melt viscosity imide oligomers and thermosetting polymide composites

    Science.gov (United States)

    Chuang, Chun-Hua (Inventor)

    2012-01-01

    .[.This invention relates to the composition and a solvent-free process for preparing novel imide oligomers and polymers specifically formulated with effective amounts of a dianhydride such as 2,3,3',4-biphenyltetra carboxylic dianydride (a-BPDA), at least one aromatic diamine and an endcapped of 4-phenylethynylphthalic anhydride (PEPA) or nadic anhydride to produce imide oligomers that possess a low-melt viscosity of 1-60 poise at 260-280.degree. C. When the imide oligomer melt is cured at about 371.degree. C. in a press or autoclave under 100-500 psi, the melt resulted in a thermoset polyimide having a glass transition temperature (T.sub.g) equal to and above 310.degree. C. A novel feature of this process is that the monomers; namely the dianhydrides, diamines and the endcaps, are melt processable to form imide oligomers at temperatures ranging between 232-280.degree. C. (450-535.degree. F.) without any solvent. These low-melt imide oligomers can be easily processed by resin transfer molding (RTM), vacuum-assisted resin transfer molding (VARTM) or the resin infusion process with fiber preforms e.g. carbon, glass or quartz preforms to produce polyimide matrix composites with 288-343.degree. C. (550-650.degree. F.) high temperature performance capability..]. .Iadd.This invention relates to compositions and a solvent-free reaction process for preparing imide oligomers and polymers specifically derived from effective amounts of dianhydrides such as 2,3,3',4'-biphenyltetracarboxylic dianhydride (a-BPDA), at least one aromatic polyamine and an end-cap such as 4-phenylethynyphthalic anhydride (PEPA) or nadic anhydride to produce imide oligomers that possess a low-melt viscosity of 1-60 poise at 260.degree. C.-280.degree. C..Iaddend.

  2. Solvent-Free Synthesis of Aryl Iodide Using Nano SiO2/HIO4 as a Reusable Acid Catalyst

    Directory of Open Access Journals (Sweden)

    A. Bamoniri

    2014-07-01

    Full Text Available An efficient and environmentally benign   method for the synthesis of aryl iodides have been developed by diazotization of aromatic amines with NaNO2 and nanosilica periodic acid (nano-SPIA as a green catalyst via grinding followed by a sandmeyer iodination by KI under solvent-free conditions at room temperature. The ensuing aryl diazonium salts supported on nano-SPIA were sufficiently stable to be kept at room temperature in the dry state. This method is a novel, efficient, eco-friendly route for solvent-free synthesis of aryl iodides.

  3. Comparison of microwave hydrodistillation and solvent-free microwave extraction of essential oil from Melaleuca leucadendra Linn

    Science.gov (United States)

    Ismanto, A. W.; Kusuma, H. S.; Mahfud, M.

    2017-12-01

    The comparison of solvent-free microwave extraction (SFME) and microwave hydrodistillation (MHD) in the extraction of essential oil from Melaleuca leucadendra Linn. was examined. Dry cajuput leaves were used in this study. The purpose of this study is also to determine optimal condition (microwave power). The relative electric consumption of SFME and MHD methods are both showing 0,1627 kWh/g and 0,3279 kWh/g. The results showed that solvent-free microwave extraction methods able to reduce energy consumption and can be regarded as a green technique for extraction of cajuput oil.

  4. 21 CFR 182.40 - Natural extractives (solvent-free) used in conjunction with spices, seasonings, and flavorings.

    Science.gov (United States)

    2010-04-01

    ... conjunction with spices, seasonings, and flavorings. 182.40 Section 182.40 Food and Drugs FOOD AND DRUG... in conjunction with spices, seasonings, and flavorings. Natural extractives (solvent-free) used in conjunction with spices, seasonings, and flavorings that are generally recognized as safe for their intended...

  5. 21 CFR 582.40 - Natural extractives (solvent-free) used in conjunction with spices, seasonings, and flavorings.

    Science.gov (United States)

    2010-04-01

    ... conjunction with spices, seasonings, and flavorings. 582.40 Section 582.40 Food and Drugs FOOD AND DRUG... in conjunction with spices, seasonings, and flavorings. Natural extractives (solvent-free) used in conjunction with spices, seasonings, and flavorings that are generally recognized as safe for their intended...

  6. Microwave-assisted clean synthesis of amides via aza-wittig reaction under solvent-free condition

    Energy Technology Data Exchange (ETDEWEB)

    Sathishkumar, Murugan; Nagarajan, Sangaraiah; Velan, Poovan Shanmuga; Dinesh, Murugan; Ponnuswamy, Alagusundaram [Department of Organic Chemistry, School of Chemistry, Madurai Kamaraj University, Tamilnadu (India)

    2011-09-15

    A solvent-free microwave-assisted coupling of phosphazenes with acyl chlorides or carboxylic anhydrides in presence of triethylphosphite has been accomplished resulting in a clean synthesis of amides in good yields. Unlike the prevailing time-consuming solution phase methodologies employing chlorinated solvents, benzene (carcinogenic), etc, the present protocol is an eco friendly, rapid and simple approach. (author)

  7. Nafion®-catalyzed microwave-assisted Ritter reaction: An atom-economic solvent-free synthesis of amides

    Science.gov (United States)

    An atom-economic solvent-free synthesis of amides by the Ritter reaction of alcohols and nitriles under microwave irradiation is reported. This green protocol is catalyzed by solid supported Nafion®NR50 with improved efficiency and reduced waste production.

  8. Three Component Synthesis of Substituted 4H-[1,3]Dioxin Derivatives Under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Hosseini-Tabatabaei

    2012-01-01

    Full Text Available Reaction between aryl aldehydes, acetylacetone and alkyl isocyanides in solvent-free conditions provided a simple and efficient one-pot route for the synthesis of 1-(2-alkylamino-6-methyl-4-aryl-4H-[1,3]dioxin-5-ylethanone derivatives in excellent yields.

  9. Preparation of ultra-fine calcium carbonate by a solvent-free reaction using supersonic airflow and low temperatures

    OpenAIRE

    Cai, Yan-Hua; Ma, Dong-Mei; Peng, Ru-Fang; Chu, Shi-Jin

    2008-01-01

    The treatment of calcium chloride with sodium carbonate under solvent-free conditions with a supersonic airflow and at a low heating temperature leads to the synthesis of ultra-fine calcium carbonate. The reaction not only involves mild conditions, a simple operation, and high yields but also gives a high conversion rate.

  10. An efficient solvent-free synthesis of imidazolines and benzimidazoles using K 4[Fe(CN 6] catalysis

    Directory of Open Access Journals (Sweden)

    Kabeer A. Shaikh

    2012-01-01

    Full Text Available Imidazolines and Benzimidazoles have been efficiently synthesized in high yields by treatment of 1,2-diamine with aldehydes using the metal co-ordinate complex K 4[Fe(CN 6] as a catalysis. The method was carried out under solvent free condition via oxidation of carbon-nitrogen bond. The process is green, mild and inexpensive.

  11. A Diazonium Salt-Based Ionic Liquid for Solvent-FreeModification of Carbon.

    Energy Technology Data Exchange (ETDEWEB)

    Liang, Chengdu [ORNL; Huang, Jing-Fang [ORNL; Li, Zuojiang [ORNL; Luo, Huimin [ORNL; Dai, Sheng [ORNL

    2006-01-01

    A novel ionic liquid that consists of p-butylbenzenediazonium ions and bis(trifluoromethanesulfonyl)amidates (Tf{sub 2}N{sup -}) has been synthesized as a task-specific ionic liquid for the solvent-free modification of carbon materials. The use of anions Tf{sub 2}N{sup =} is the key to rendering the hydrophobicity, low liquidus temperature, and ionicity to this novel molten salt. This diazonium salt has a melting point of 7.2 C and a moderate electric conductivity of 527 {micro} s/cm at 25 C. The thermal stability of this diazonium ionic liquid has been investigated by high-resolution thermogravimetric analysis (HRTGA). The compound is stable up to about 90 C in nitrogen, which is only 10 C less than its solid tetrafluoroborate counterpart. The modification of carbon materials has been carried out through both thermal and electrochemical activations of diazonium ions to generate free radical intermediates without the use of any solvent. The surface-coverage loadings of 3.38 {micro} mol/m{sup 2} and 6.07 {micro} mol/m{sup 2} for covalently attached organic functionalities have been achieved by the thermally induced functionalization and electrochemically assisted reaction, respectively.

  12. An insight on acyl migration in solvent-free ethanolysis of model triglycerides using Novozym 435.

    Science.gov (United States)

    Sánchez, Daniel Alberto; Tonetto, Gabriela Marta; Ferreira, María Luján

    2016-02-20

    In this work, the ethanolysis of triglycerides catalyzed by immobilized lipase was studied, focusing on the secondary reaction of acyl migration. The catalytic tests were performed in a solvent-free reaction medium using Novozym 435 as biocatalyst. The selected experimental variables were biocatalyst loading (5-20mg), reaction time (30-90min), and chain length of the fatty acids in triglycerides with and without unsaturation (short (triacetin), medium (tricaprylin) and long (tripalmitin/triolein)). The formation of 2-monoglyceride by ethanolysis of triglycerides was favored by long reaction times and large biocatalyst loading with saturated short- to medium-chain triglycerides. In the case of long-chain triglycerides, the formation of this monoglyceride was widely limited by acyl migration. In turn, acyl migration increased the yield of ethyl esters and minimized the content of monoglycerides and diglycerides. Thus, the enzymatic synthesis of biodiesel was favored by long-chain triglycerides (which favor the acyl migration), long reaction times and large biocatalyst loading. The conversion of acylglycerides made from long-chain fatty acids with unsaturation was relatively low due to limitations in their access to the active site of the lipase. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Solvent Free Low-Melt Viscosity Imide Oligomers And Thermosetting Polyimide Composites

    Science.gov (United States)

    Chuang, CHun-Hua (Inventor)

    2006-01-01

    This invention relates to the composition and a solvent-free process for preparing novel imide oligomers and polymers specifically formulated with effective amounts of a dianhydride such as 2,3,3',4-biphenyltetra carboxylic dianydride (a-BPDA), at least one aromatic diamine' and an endcapped of 4-phenylethynylphthalic anhydride (PEPA) or nadic anhydride to produce imide oligomers that possess a low-melt viscosity of 1-60 poise at 260-280" C. When the imide oligomer melt is cured at about 371 C. in a press or autoclave under 100-500 psi, the melt resulted in a thermoset polyimide having a glass transition temperature (T(sub g)) equal to and above 310 C. A novel feature of this process is that the monomers; namely the dianhydrides, diamines and the endcaps, are melt processable to form imide oligomers at temperatures ranging between 232-280 C. (450-535 F) without any solvent. These low-melt imide oligomers can be easily processed by resin transfer molding (RTM), vacuum-assisted resin transfer molding (VARTM) or the resin infusion process with fiber preforms e.g. carbon, glass or quartz preforms to produce polyimide matrix composites with 288-343C (550-650 F) high temperature performance capability.

  14. An Efficient, Solvent-Free Process for Synthesizing Anhydrous MgCl2

    Energy Technology Data Exchange (ETDEWEB)

    Motkuri, Radha K.; Vemuri, Venkata Rama S.; Barpaga, Dushyant; Schaef, Herbert T.; Loring, John S.; Martin, Paul F.; Lao, David; Nune, Satish K.; McGrail, Bernard P.

    2018-01-02

    A new efficient and solvent-free method for the synthesis of anhydrous MgCl2 from its hexahydrate is proposed. Fluidized dehydration of MgCl2·6H2O feedstock at 200 °C in a porous bed reactor yields MgCl2·nH2O (0 < n < 1), which has a similar diffraction pattern as activated MgCl2. The MgCl2·nH2O is then ammoniated directly using liquefied NH3 in the absence of solvent to form MgCl2·6NH3. Calcination of the hexammoniate complex at 300 °C then yields anhydrous MgCl2. Both dehydration and deammoniation were thoroughly studied using in situ as well as ex situ characterization techniques. Specifically, a detailed understanding of the dehydration process was monitored by in situ PXRD and in situ FTIR techniques where formation of salt with nH2O (n = 4, 2, 1, <1) was characterized. Given the reduction in thermal energy required to produce dehydrated feedstock with this method compared with current strategies, significant cost benefits are expected. Overall, the combined effect of activation, macroporosity, and coordinated water depletion allows the formation of hexammoniate without using solvent, thus minimizing waste formation.

  15. Eco-friendly all-carbon paper electronics fabricated by a solvent-free drawing method

    International Nuclear Information System (INIS)

    Kanaparthi, Srinivasulu; Badhulika, Sushmee

    2016-01-01

    Here we report the fabrication of high-performance all-carbon temperature and infrared (IR) sensors with a solvent-free multiwalled carbon nanotube (MWCNT) trace as the sensing element and commercial graphite pencil trace as the electrical contact on recyclable and biodegradable cellulose filter paper without using any toxic materials or complex procedures. The temperature sensor shows a large negative temperature coefficient of resistance (TCR) in the range of −3100 ppm K −1 to −4900 ppm K −1 , which is comparable to available commercial temperature sensors, and an activation energy of 34.85 meV. The IR sensor shows a high responsivity of 58.5 V W −1 , which is greater than reported IR sensors with similar dimensions. A detailed study of the conduction mechanism in MWCNTs with temperature and the photo response with IR illumination was done and it was found that the conduction is due to thermally assisted hopping in band tails and the photo response is bolometric in nature. The successful fabrication of these sensors on cellulose filter paper with a comparable performance to existing components indicates that it is possible to fabricate high-performance electronics using low-cost, eco-friendly materials without the need for expensive clean-room processing techniques or harmful chemicals. (paper)

  16. Efficient and Highly Selective Solvent-Free Oxidation of Primary Alcohols to Aldehydes Using Bucky Nanodiamond.

    Science.gov (United States)

    Lin, Yangming; Wu, Kuang-Hsu Tim; Yu, Linhui; Heumann, Saskia; Su, Dang Sheng

    2017-09-11

    Selective oxidation of alcohols to aldehydes is widely applicable to the synthesis of various green chemicals. The poor chemoselectivity for complicated primary aldehydes over state-of-the-art metal-free or metal-based catalysts represents a major obstacle for industrial application. Bucky nanodiamond is a potential green catalyst that exhibits excellent chemoselectivity and cycling stability for the selective oxidation of primary alcohols in diverse structures (22 examples, including aromatic, substituted aromatic, unsaturated, heterocyclic, and linear chain alcohols) to their corresponding aldehydes. The results are comparable to reported transition-metal catalysts including conventional Pt/C and Ru/C catalysts for certain substrates under solvent-free conditions. The possible activation process of the oxidant and substrates by the surface oxygen groups and defect species are revealed with model catalysts, ex situ electrochemical measurements, and ex situ attenuated total reflectance. The zigzag edges of sp 2 carbon planes are shown to play a key role in these reactions. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Diffusivities, viscosities, and conductivities of solvent-free ionically grafted nanoparticles

    KAUST Repository

    Hong, Bingbing; Panagiotopoulos, Athanassios Z.

    2013-01-01

    A new class of conductive composite materials, solvent-free ionically grafted nanoparticles, were modeled by coarse-grained molecular dynamics methods. The grafted oligomeric counterions were observed to migrate between different cores, contributing to the unique properties of the materials. We investigated the dynamics by analyzing the dependence on temperature and structural parameters of the transport properties (self-diffusion coefficients, viscosities and conductivities) and counterion migration kinetics. Temperature dependence of all properties follows the Arrhenius equation, but chain length and grafting density have distinct effects on different properties. In particular, structural effects on the diffusion coefficients are described by the Rouse model and the theory of nanoparticles diffusing in polymer solutions, viscosities are strongly influenced by clustering of cores, and conductivities are dominated by the motions of oligomeric counterions. We analyzed the migration kinetics of oligomeric counterions in a manner analogous to unimer exchange between micellar aggregates. The counterion migrations follow the "double-core" mechanism and are kinetically controlled by neighboring-core collisions. © 2013 The Royal Society of Chemistry.

  18. Solvent-free optical recording of structural colours on pre-imprinted photocrosslinkable nanostructures

    Science.gov (United States)

    Jiang, Hao; Rezaei, Mohamad; Abdolahi, Mahssa; Kaminska, Bozena

    2017-09-01

    Optical digital information storage media, despite their ever-increasing storage capacity and data transfer rate, are vulnerable to the potential risk of turning inaccessible. For this reason, long-term eye-readable full-colour optical archival storage is in high demand for preserving valuable information from cultural, intellectual, and scholarly resources. However, the concurrent requirements in recording colours inexpensively and precisely, and preserving colours for the very long term (for at least 100 years), have not yet been met by existing storage techniques. Structural colours hold the promise to overcome such challenges. However, there is still the lack of an inexpensive, rapid, reliable, and solvent-free optical patterning technique for recording structural colours. In this paper, we introduce an enabling technique based on optical and thermal patterning of nanoimprinted SU-8 nanocone arrays. Using photocrosslinking and thermoplastic flow of SU-8, diffractive structural colours of nanocone arrays are recorded using ultra-violet (UV) exposure followed by the thermal development and reshaping of nanocones. Different thermal treatment procedures in reshaping nanocones are investigated and compared, and two-step progressive baking is found to allow the controllable reshaping of nanocones. The height of the nanocones and brightness of diffractive colours are modulated by varying the UV exposure dose to enable grey-scale patterning. An example of recorded full-colour image through half-tone patterning is also demonstrated. The presented technique requires only low-power continuous-wave UV light and is very promising to be adopted for professional and consumer archival storage applications.

  19. Application of 2k Full Factorial Design in Optimization of Solvent-Free Microwave Extraction of Ginger Essential Oil

    Directory of Open Access Journals (Sweden)

    Mumtaj Shah

    2014-01-01

    Full Text Available The solvent-free microwave extraction of essential oil from ginger was optimized using a 23 full factorial design in terms of oil yield to determine the optimum extraction conditions. Sixteen experiments were carried out with three varying parameters, extraction time, microwave power, and type of sample for two levels of each. A first order regression equation best fits the experimental data. The predicted values calculated by the regression model were in good agreement with the experimental values. The results showed that the extraction time is the most prominent factor followed by microwave power level and sample type for extraction process. An average of 0.25% of ginger oil can be extracted using current setup. The optimum conditions for the ginger oil extraction using SFME were the extraction time 30 minutes, microwave power level 640 watts, and sample type, crushed sample. Solvent-free microwave extraction proves a green and promising technique for essential oil extraction.

  20. Hot Melt Extrusion as Solvent-Free Technique for a Continuous Manufacturing of Drug-Loaded Mesoporous Silica

    DEFF Research Database (Denmark)

    Genina, Natalja; Hadi, Batol; Löbmann, Korbinian

    2018-01-01

    The aim of this study is to explore hot melt extrusion (HME) as a solvent-free drug loading technique for preparation of stable amorphous solid dispersions using mesoporous silica (PSi). Ibuprofen and carvedilol were used as poorly soluble active pharmaceutical ingredients (APIs). Due to the high...... friction of an API:PSi mixture below the loading limit of the API, it was necessary to add the polymer Soluplus(®) (SOL) in order to enable the extrusion process. As a result, the APIs were distributed between the PSi and SOL phase after HME. Due to its higher affinity to PSi, ibuprofen was mainly adsorbed...... into the PSi, whereas carvedilol was mainly found in the SOL phase. Intrinsic dissolution rate was highest for HME formulations, containing PSi, compared to pure crystalline (amorphous) APIs and HME formulations without PSi. HME is a feasible solvent-free drug loading technique for preparation of PSi...

  1. Nanocrystalline copper(II oxide-catalyzed one-pot four- component synthesis of polyhydroquinoline derivativesunder solvent-free conditions

    Directory of Open Access Journals (Sweden)

    J. Safaei-Ghomi

    2011-07-01

    Full Text Available The efficient and environmentally friendly method for the one-pot synthesis of polyhydroquinolines has been developed in the presence of CuO nanoparticles. The multi-component reactions of aldehydes, dimedone, ethyl acetoacetate andammonium acetate were carried out under solvent-free conditions to afford some polyhydroquinoline derivatives. This method provides several advantages including high yields, low reaction times and little catalyst loading.

  2. Solvent-free synthesis of C10 and C11 branched alkanes from furfural and methyl isobutyl ketone.

    Science.gov (United States)

    Yang, Jinfan; Li, Ning; Li, Guangyi; Wang, Wentao; Wang, Aiqin; Wang, Xiaodong; Cong, Yu; Zhang, Tao

    2013-07-01

    Our best results jet: C10 and C11 branched alkanes, with low freezing points, are synthesized through the aldol condensation of furfural and methyl isobutyl ketone from lignocellulose, which is then followed by hydrodeoxygenation. These jet-fuel-range alkanes are obtained in high overall yields (≈90%) under solvent-free conditions. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. An Organocatalyzed and Ultrasound Accelerated Expeditious Synthetic Route to 1,5-Benzodiazepines under Solvent-Free Conditions

    Energy Technology Data Exchange (ETDEWEB)

    Shinde, Pravin V.; Shingate, Bapurao B.; Shingare, Murlidhar S. [Babasaheb Ambedkar Marathwada University, Aurngabad (India)

    2011-04-15

    In the present work, successful implementation of ultrasound irradiations for the rapid synthesis of 1,5- benzodiazepine derivatives under solvent-free conditions is demonstrated. Use of a novel catalyst i.e. camphor sulphonic acid in combination with ultrasound technique is reported for the first time. Comparative study for the synthesis of 1,5-benzodiazepines using conventional as well as ultrasonication method is discussed.

  4. NaHSO4-SiO2-Promoted Solvent-Free Synthesis of Benzoxazoles, Benzimidazoles, and Benzothiazole Derivatives

    Directory of Open Access Journals (Sweden)

    K. Ravi Kumar

    2013-01-01

    Full Text Available An efficient protocol has been developed for the preparation of a library of benzoxazole, benzimidazole, and benzothiazole derivatives from reactions of acyl chlorides with o-substituted aminoaromatics in the presence of catalytic amount of silica-supported sodium hydrogen sulphate under solvent-free conditions. Simple workup procedure, high yield, easy availability, reusability, and use of ecofriendly catalyst are some of the striking features of the present protocol.

  5. On the addition of conducting ceramic nanoparticles in solvent-free ionic liquid electrolyte for dye-sensitized solar cells

    KAUST Repository

    Lee, Chuan-Pei; Lee, Kun-Mu; Chen, Po-Yen; Ho, Kuo-Chuan

    2009-01-01

    ) have been used, for the first time, in dye-sensitized solar cells (DSSCs), and the incorporation of TiC nanoparticles in a binary ionic liquid electrolyte on the cell performance has been investigated. Cell conversion efficiency with 0.6 wt% TiC reached

  6. YCl3-Catalyzed Highly Selective Ring Opening of Epoxides by Amines at Room Temperature and under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Wuttichai Natongchai

    2017-11-01

    Full Text Available A simple, efficient, and environmentally benign approach for the synthesis of β-amino alcohols is herein described. YCl3 efficiently carried out the ring opening of epoxides by amines to produce β-amino alcohols under solvent-free conditions at room temperature. This catalytic approach is very effective, with several aromatic and aliphatic oxiranes and amines. A mere 1 mol % concentration of YCl3 is enough to deliver β-amino alcohols in good to excellent yields with high regioselectivity.

  7. Synthesis of β-phenylchalcogeno-α, β-unsaturated esters, ketones and nitriles using microwave and solvent-free conditions

    International Nuclear Information System (INIS)

    Lenardao, Eder J.; Silva, Marcio S.; Mendes, Samuel R.; Azambuja, Francisco de; Jacob, Raquel G.; Perin, Gelson; Santos, Paulo Cesar Silva dos

    2007-01-01

    A simple, clean and efficient solvent-free protocol was developed for hydrochalcogenation of alkynes containing a Michael acceptor (ester, ketone and nitrile) with phenylchalcogenolate anions generated in situ from the respective diphenyl dichalcogenide (Se, Te, S), using alumina supported sodium borohydride. This efficient and improved method is general and furnishes the respective (Z)-β-phenylchalcogeno-α,β-unsaturated esters, ketones and nitriles, in good yield and higher selectivity, compared with those that use organic solvent and inert atmosphere. The use of microwave (MW) irradiation facilitates the procedure and accelerates the reaction. (author)

  8. An Efficient Solvent-Free Protocol for the Synthesis of 1-Amidoalkyl-2-naphthols using Silica-Supported Molybdatophosphoric Acid

    Directory of Open Access Journals (Sweden)

    Abdolkarim Zare

    2010-01-01

    Full Text Available A highly efficient, green and simple solvent-free method for the synthesis of 1-amidoalkyl-2-naphthols via one-pot multi-components condensation of 2-naphthol, aromatic aldehydes and amides in the presence of catalytic amount of silica-supported molybdatophosphoric acid (H3PMo12O40.xH2O/SiO2, 3.17 mol% is described. The reactions proceed rapidly and the title compounds are produced in high to excellent yields.

  9. Chemoselective Synthesis of Dithioacetals from Bio-aldehydes with Zeolites under Ambient and Solvent-free Conditions

    DEFF Research Database (Denmark)

    Li, Hu; Yang, Tingting; Riisager, Anders

    2017-01-01

    of commercial and modified zeolites are excellent catalysts for thioacetalization of different thiols with carbonyl compounds, including biomass-derived aldehydes, at room temperature under solvent-free conditions. A near quantitative yield of dithioacetal was obtained over H-beta(19) at room temperature......Dithioacetals are an important class of versatile compounds extensively applied in pharmaceuticals, separations, electrochemistry, and organic synthesis, but few heterogeneous catalytic systems are reported to be generally applicable for their synthesis from a wide range of substrates. A series...

  10. B2O3/Al2O3 as a new, highly efficient and reusable heterogeneous catalyst for the selective synthesis of β-enamino ketones and esters under solvent-free conditions

    International Nuclear Information System (INIS)

    Chen, Jiu-Xi; Gao, Wen-Xia; Jin, Hui-Le; Ding, Jin-Chang; Wu, Hua-Yue

    2010-01-01

    Boron oxide adsorbed on alumina (B 2 O 3 /Al 2 O 3 ) has been found to be a new and highly efficient heterogeneous catalyst for the synthesis of β-enamino ketones and esters by the enamination of various primary and secondary amines with β-dicarbonyl compounds under solvent-free conditions. The important features of this methodology are broad substrate scope, high yield, no requirement of metal catalysts, high regio- and chemoselectivity and environmental friendliness. In addition, the catalyst could be recovered easily after the reactions and reused without evident loss of reactivity. (author)

  11. Molecular interactions and redox effects of carvacrol and thymol on myofibrillar proteins using a non-destructive and solvent-free methodological approach.

    Science.gov (United States)

    Lahmar, Aida; Akcan, Tolga; Chekir-Ghedira, Leila; Estévez, Mario

    2018-04-01

    The present study provides molecular insight into the effect of thymol and carvacrol on the oxidative damage caused to myofibrillar proteins by a hydroxyl-radical generating system (HRGS). An innovative model system was designed, in which gels, prepared with increasing levels of myofibrillar proteins, were oxidized by a HRGS (Fe 3+ /H 2 O 2 , 60 °C and 7 days) in the presence of lipids. The molecular affinity between myofibrillar proteins and both terpenes, as well as their effect on the oxidative stability of the gel systems, were studied using a non-destructive and solvent-free procedure based on fluorescence spectroscopy. Carvacrol displayed more affinity than thymol for establishing chemical interactions with protein residues. Both terpenes exhibited a significant antioxidant potential against the generation of lipid-derived volatile carbonyls and against the formation of protein crosslinking. This procedure may be applied to meat products to assess the effectiveness of a given antioxidant additive without size reduction or sample processing. Copyright © 2018 Elsevier Ltd. All rights reserved.

  12. Solvent-free covalent functionalization of multi-walled carbon nanotubes and nanodiamond with diamines: Looking for cross-linking effects

    International Nuclear Information System (INIS)

    Basiuk, Elena V.; Basiuk, Vladimir A.; Meza-Laguna, Víctor; Contreras-Torres, Flavio F.; Martínez, Melchor; Rojas-Aguilar, Aarón; Salerno, Marco

    2012-01-01

    Highlights: ► Diamines were used for one-step functionalization of nanotubes and nanodiamond. ► We found experimental evidences of cross-linking effects in these nanomaterials. ► We found a strong orientation effect in the functionalized carbon nanotubes. - Abstract: The covalent functionalization of carbon nanomaterials with diamines is a way to enhance the mechanical strength of nanocomposites due to cross-linking effects, to form complex networks for nanotube-based electronic circuits, as well as is important for a number of biomedical applications. The main goal of the present work was to covalently functionalize pristine multi-walled carbon nanotubes and nanodiamond with three aliphatic diamines (1,8-diaminooctane, 1,10-diaminodecane and 1,12-diaminododecane) and one aromatic diamine (1,5-diaminonaphthalene), by employing a simple one-step solvent-free methodology, which is based on thermal instead of chemical activation. We looked for experimental evidences of cross-linking effects in the carbon nanomaterials synthesized by using solubility/dispersibility tests, atomic force microscopy, scanning and transmission electron microscopy, as well as Fourier-transform infrared spectroscopy and thermogravimetric analysis for additional characterization.

  13. Solvent-free microwave-assisted synthesis of novel pyrazolo[4′,3′:5,6]pyrido[2,3-d]pyrimidines with potential antifungal activity

    Directory of Open Access Journals (Sweden)

    Paola Acosta

    2016-05-01

    Full Text Available Novel fused pyrazolo[4′,3′:5,6]pyrido[2,3-d]pyrimidines 5 were prepared by a solvent-free microwave assisted reaction of heterocyclic o-aminonitriles 3 and cyanopyridines 4 in the presence of tBuOK as catalyst. This protocol provides a versatile procedure for the synthesis of the title compounds with the advantages of easy work-up, mild reaction conditions and good yields. All compounds were also tested for antifungal properties against two clinically important fungi; Candida albicans and Cryptococcus neoformans. Several compounds showed moderate activity against both fungi, being 5a the most active compound. Analysis of the antifungal behavior of properly grouped compounds allowed to determine that the position of the N in the pyrimidyl moiety per se does not play a role in the activity. In turn, the type of 4-R substituent appears to influence the activity. In addition to the above considerations, the lipophilicity of compounds measured as logP showed to be not related to the activity and regarding the dipole moment (D, no net correlation was observed, although it is the most active compounds (% inhibition >50% that have a D ⩾ 7.5, mainly against C. albicans.

  14. Sustained Release of Lidocaine from Solvent-Free Biodegradable Poly[(d,l)-Lactide-co-Glycolide] (PLGA): In Vitro and In Vivo Study.

    Science.gov (United States)

    Kau, Yi-Chuan; Liao, Chia-Chih; Chen, Ying-Chi; Liu, Shih-Jung

    2014-09-16

    Local anesthetics are commonly used for pain relief by regional nerve blocking. In this study, we fabricated solvent-free biodegradable pellets to extend the duration of lidocaine release without any significant local or systemic toxicity levels. To manufacture the pellets, poly[(d,l)-lactide-co-glycolide] (PLGA) was first pre-mixed with lidocaine powder into different ratios. The powder mixture was then compressed with a mold (diameter of 1, 5, 8 or 10 mm) and sintered at 65 °C to form pellets. The in vitro release study showed that the lidocaine/PLGA pellets exhibited a tri-phase release behavior (a burst, a diffusion-controlled release and a degradation-dominated release) and reached completion around day 28. Scanning electron microscope (SEM) photos show that small channels could be found on the surfaces of the pellets on day 2. Furthermore, the polymer matrix swelled and fell apart on day 7, while the pellets became viscous after 10 days of in vitro elution. Perineural administration of the lidocaine/PLGA pellets produced anti-hypersensitivity effects lasting for at least 24 h in rats, significant when compared to the control group (a pure PLGA was pellet administered). In addition, no inflammation was detected within the nerve and in the neighboring muscle by histopathology.

  15. Sustained Release of Lidocaine from Solvent-Free Biodegradable Poly[(d,l-Lactide-co-Glycolide] (PLGA: In Vitro and In Vivo Study

    Directory of Open Access Journals (Sweden)

    Yi-Chuan Kau

    2014-09-01

    Full Text Available Local anesthetics are commonly used for pain relief by regional nerve blocking. In this study, we fabricated solvent-free biodegradable pellets to extend the duration of lidocaine release without any significant local or systemic toxicity levels. To manufacture the pellets, poly[(d,l-lactide-co-glycolide] (PLGA was first pre-mixed with lidocaine powder into different ratios. The powder mixture was then compressed with a mold (diameter of 1, 5, 8 or 10 mm and sintered at 65 °C to form pellets. The in vitro release study showed that the lidocaine/PLGA pellets exhibited a tri-phase release behavior (a burst, a diffusion-controlled release and a degradation-dominated release and reached completion around day 28. Scanning electron microscope (SEM photos show that small channels could be found on the surfaces of the pellets on day 2. Furthermore, the polymer matrix swelled and fell apart on day 7, while the pellets became viscous after 10 days of in vitro elution. Perineural administration of the lidocaine/PLGA pellets produced anti-hypersensitivity effects lasting for at least 24 h in rats, significant when compared to the control group (a pure PLGA was pellet administered. In addition, no inflammation was detected within the nerve and in the neighboring muscle by histopathology.

  16. Preparation of a Nanoemulsion with Carapa guianensis Aublet (Meliaceae Oil by a Low-Energy/Solvent-Free Method and Evaluation of Its Preliminary Residual Larvicidal Activity

    Directory of Open Access Journals (Sweden)

    Flávia L. M. Jesus

    2017-01-01

    Full Text Available Andiroba (Carapa guianensis seeds are the source of an oil with a wide range of biological activities and ethnopharmacological uses. However, few studies have devoted attention to innovative formulations, including nanoemulsions. The present study aimed to obtain a colloidal system with the andiroba oil using a low-energy and organic-solvent-free method. Moreover, the preliminary residual larvicidal activity of the nanoemulsion against Aedes aegypti was evaluated. Oleic and palmitic acids were the major fatty acids, in addition to the phytosterol β-sitosterol and limonoids (tetranortriterpenoids. The required hydrophile-lipophile was around 11.0 and the optimal nanoemulsion was obtained using polysorbate 85. The particle size distribution suggested the presence of small droplets (mean diameter around 150 nm and low polydispersity index (around 0.150. The effect of temperature on particle size distribution revealed that no major droplet size increase occurred. The preliminary residual larvicidal assay suggested that the mortality increased as a function of time. The present study allowed achievement of a potential bioactive oil in water nanoemulsion that may be a promising controlled release system. Moreover, the ecofriendly approach involved in the preparation associated with the great bioactive potential of C. guianensis makes this nanoemulsion very promising for valorization of this Amazon raw material.

  17. Solvent-free covalent functionalization of multi-walled carbon nanotubes and nanodiamond with diamines: Looking for cross-linking effects

    Energy Technology Data Exchange (ETDEWEB)

    Basiuk, Elena V., E-mail: elenagd@unam.mx [Centro de Ciencias Aplicadas y Desarrollo Tecnologico, Universidad Nacional Autonoma de Mexico, Circuito Exterior, Ciudad Universitaria, 04510 Mexico, D.F. (Mexico); Nanophysics Department, Italian Institute of Technology, via Morego 30, 16163 Genova, Liguria (Italy); Basiuk, Vladimir A. [Nanophysics Department, Italian Institute of Technology, via Morego 30, 16163 Genova, Liguria (Italy); Instituto de Ciencias Nucleares, Universidad Nacional Autonoma de Mexico, Circuito Exterior, Ciudad Universitaria, 04510 Mexico, D.F. (Mexico); Facultad de Ciencias, Universidad Autonoma del Estado de Morelos, Av. Universidad 1001, Col. Chamilpa, 62209 Cuernavaca, Morelos (Mexico); Meza-Laguna, Victor; Contreras-Torres, Flavio F.; Martinez, Melchor [Centro de Ciencias Aplicadas y Desarrollo Tecnologico, Universidad Nacional Autonoma de Mexico, Circuito Exterior, Ciudad Universitaria, 04510 Mexico, D.F. (Mexico); Rojas-Aguilar, Aaron [Centro de Investigacion y de Estudios Avanzados, Instituto Politecnico Nacional, Av. Instituto Politecnico Nacional 2508, Col. San Pedro Zacatenco, 07360 Mexico, D.F. (Mexico); Salerno, Marco [Nanophysics Department, Italian Institute of Technology, via Morego 30, 16163 Genova, Liguria (Italy); and others

    2012-10-15

    Highlights: Black-Right-Pointing-Pointer Diamines were used for one-step functionalization of nanotubes and nanodiamond. Black-Right-Pointing-Pointer We found experimental evidences of cross-linking effects in these nanomaterials. Black-Right-Pointing-Pointer We found a strong orientation effect in the functionalized carbon nanotubes. - Abstract: The covalent functionalization of carbon nanomaterials with diamines is a way to enhance the mechanical strength of nanocomposites due to cross-linking effects, to form complex networks for nanotube-based electronic circuits, as well as is important for a number of biomedical applications. The main goal of the present work was to covalently functionalize pristine multi-walled carbon nanotubes and nanodiamond with three aliphatic diamines (1,8-diaminooctane, 1,10-diaminodecane and 1,12-diaminododecane) and one aromatic diamine (1,5-diaminonaphthalene), by employing a simple one-step solvent-free methodology, which is based on thermal instead of chemical activation. We looked for experimental evidences of cross-linking effects in the carbon nanomaterials synthesized by using solubility/dispersibility tests, atomic force microscopy, scanning and transmission electron microscopy, as well as Fourier-transform infrared spectroscopy and thermogravimetric analysis for additional characterization.

  18. Solvent-free synthesis of azomethines, spectral correlations and antimicrobial activities of some E-benzylidene-4-chlorobenzenamines

    Directory of Open Access Journals (Sweden)

    R. Suresh

    2015-07-01

    Full Text Available Some azomethines including substituted benzylidene-4-chlorobenzenamines (E-imines have been synthesized by fly-ash: PTS catalyzed microwave assisted condensation of 4-chloroaniline and substituted benzaldehydes under solvent-free conditions. The yield of the imines has been found to be more than 85%. The purity of all imines has been checked using their physical constants and UV, IR and NMR spectral data. These spectral data have been correlated with Hammett substituent constants and F and R parameters using single and multi-linear regression analysis. From the results of statistical analysis, the effect of substituents on the above spectral data has been studied. The antimicrobial activities of all imines have been studied using standard methods.

  19. Solvent free hydroxylation of the methyl esters of Blighia unijugata seed oil in the presence of cetyltrimethylammonium permanganate

    Directory of Open Access Journals (Sweden)

    Adewuyi Adewale

    2011-12-01

    Full Text Available Abstract Extraction of oil from the seed of Blighia unijugata gave a yield of 50.82 ± 1.20% using hexane in a soxhlet extractor. The iodine and saponification values were 67.60 ± 0.80 g iodine/100 g and 239.20 ± 1.00 mg KOH/g respectively with C18:1 being the dominant fatty acid. Unsaturated methyl esters of Blighia unijugata which had been previously subjected to urea adduct complexation was used to synthesize methyl 9, 10-dihydroxyoctadecanoate via hydroxylation in the presence of cetyltrimethylammonium permanganate (CTAP. The reaction was monitored and confirmed using FTIR and GC-MS. This study has revealed that oxidation reaction of mono unsaturated bonds using CTAP could be achieved under solvent free condition.

  20. Solvent-Free Biginelli Condensation using Tungstate Sulfuric Acid: a Powerful and Reusable Catalyst for Selective Synthesis

    Directory of Open Access Journals (Sweden)

    Rezvan Rezaee Nasab

    2014-07-01

    Full Text Available Tungstate sulfuric acid (TSA has been prepared and used as a recyclable catalyst for the Biginelli syn-thesis of some biologically active quinazolinones/thiones under solvent-free conditions. This method has advantages such as the avoidance of organic solvents, high yield of pure products, short reaction times, and operational simplicity.  © 2014 BCREC UNDIP. All rightsReceived: 28th April 2014; Revised: 15th May 2014; Accepted: 26th May 2014[ How to Cite: Nasab, R.R., Karami, B., Khodabakhshi, S. (2014. Selective Solvent‐free Biginelli Condensation using Tungstate Sulfuric Acid as Powerful and Reusable Catalyst. Bulletin of Chemical Reaction Engineering & Catalysis, 9 (2: 142-154. (doi:10.9767/bcrec.9.2.6794.148-154][ Permalink/DOI: http://dx.doi.org/10.9767/bcrec.9.2.6794.148-154

  1. Facile synthesis of 1-naphthol azo dyes with nano SiO2/HIO4 under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    A.R. Pourali

    2013-09-01

    Full Text Available Nano-silica supported periodic acid (nano-SPIA has been utilized as a heterogeneous reagent for a highly efficient and one pot synthesis of azo dyes based on 1-naphthol under solvent-free conditions at room temperature. This method has some advantages, the reaction workup is very easy and the catalyst can be easily separated from the reaction mixture and one-pot procedure. The related products have been obtained in good to excellent yields, high purity and short reaction times. The structures of the products have been characterized by several techniques using UV-Vis, FT-IR, 1H NMR, 13C NMR and mass spectra.DOI: http://dx.doi.org/10.4314/bcse.v27i3.13

  2. Solvent-free enzymatic synthesis of feruloylated structured lipids by the transesterification of ethyl ferulate with castor oil.

    Science.gov (United States)

    Sun, Shangde; Zhu, Sha; Bi, Yanlan

    2014-09-01

    A novel enzymatic route of feruloylated structured lipids synthesis by the transesterification of ethyl ferulate (EF) with castor oil, in solvent-free system, was investigated. The transesterification reactions were catalysed by Novozym 435, Lipozyme RMIM, and Lipozyme TLIM, among which Novozym 435 showed the best catalysis performance. Effects of feruloyl donors, reaction variables, and ethanol removal on the transesterification were also studied. High EF conversion (∼100%) was obtained under the following conditions: enzyme load 20% (w/w, relative to the weight of substrates), reaction temperature 90 °C, substrate molar ratio 1:1 (EF/castor oil), 72 h, vacuum pressure 10 mmHg, and 200 rpm. Under these conditions, the transesterification product consisted of 62.6% lipophilic feruloylated structured lipids and 37.3% hydrophilic feruloylated lipids. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. Polar-solvent-free colloidal synthesis of highly luminescent alkylammonium lead halide perovskite nanocrystals

    Science.gov (United States)

    Vybornyi, Oleh; Yakunin, Sergii; Kovalenko, Maksym V.

    2016-03-01

    A novel synthesis of hybrid organic-inorganic lead halide perovskite nanocrystals (CH3NH3PbX3, X = Br or I) that does not involve the use of dimethylformamide or other polar solvents is presented. The reaction between methylamine and PbX2 salts is conducted in a high-boiling nonpolar solvent (1-octadecene) in the presence of oleylamine and oleic acid as coordinating ligands. The resulting nanocrystals are characterized by high photoluminescence quantum efficiencies of 15-50%, outstanding phase purity and tunable shapes (nanocubes, nanowires, and nanoplatelets). Nanoplatelets spontaneously assemble into micrometer-length wires by face-to-face stacking. In addition, we demonstrate amplified spontaneous emission from thin films of green-emitting CH3NH3PbBr3 nanowires with low pumping thresholds of 3 μJ cm-2.A novel synthesis of hybrid organic-inorganic lead halide perovskite nanocrystals (CH3NH3PbX3, X = Br or I) that does not involve the use of dimethylformamide or other polar solvents is presented. The reaction between methylamine and PbX2 salts is conducted in a high-boiling nonpolar solvent (1-octadecene) in the presence of oleylamine and oleic acid as coordinating ligands. The resulting nanocrystals are characterized by high photoluminescence quantum efficiencies of 15-50%, outstanding phase purity and tunable shapes (nanocubes, nanowires, and nanoplatelets). Nanoplatelets spontaneously assemble into micrometer-length wires by face-to-face stacking. In addition, we demonstrate amplified spontaneous emission from thin films of green-emitting CH3NH3PbBr3 nanowires with low pumping thresholds of 3 μJ cm-2. Electronic supplementary information (ESI) available: Materials and methods, additional figures. See DOI: 10.1039/c5nr06890h

  4. Solvent-free functionalization of silicone rubber and efficacy of PAAm brushes grafted from an amino-PPX layer against bacterial adhesion

    NARCIS (Netherlands)

    Fundeanu, Irina; Klee, Doris; Schouten, Arend J.; Busscher, Henk J.; van der Mei, Henny C.

    Silicone rubber is a frequently employed biomaterial that is prone to bacterial adhesion and biofilm formation. In this study, the surface of silicone rubber was solvent-free functionalized by chemical vapor deposition (CVD) of poly(o-amino-p-xylylene-co-p-xylylene (amino-PPX). Subsequently, the

  5. A Facile Solvent Free Microwave Induced Synthesis and Antibacterial Activity of Some 3-(2’-Hydroxyphenyl-5-(Substituted Aryl-2-Pyrazoline-N1-Caboxaldehydes

    Directory of Open Access Journals (Sweden)

    Birbal Bajia

    2007-01-01

    Full Text Available A novel one pot formylation of 3-(2’-hydroxyphenyl-5-(substituted 2-pyrazolines has been carried out using microwave irradiation with formic acid. solvent free reaction afforded title compounds in 80-90% yield with high purity.synthesized compounds were tested for their antibacterial activity using standard drug.

  6. Solvent-free Hydrodeoxygenation of Bio-oil Model Compounds Cyclopentanone and Acetophenone over Flame-made Bimetallic Pt-Pd/ZrO2 Catalysts

    Science.gov (United States)

    Jiang, Yijiao; Büchel, Robert; Huang, Jun; Krumeich, Frank; Pratsinis, Sotiris E.; Baiker, Alfons

    2013-01-01

    Bimetallic Pt-Pd/ZrO2 catalysts with different Pt/Pd atomic ratio and homogeneous dispersion of the metal nanoparticles were prepared in a single step by flame-spray pyrolysis. The catalysts show high activity and tuneable product selectivity for the solvent-free hydrodeoxygenation of the bio-oil model compounds cyclopentanone and acetophenone. PMID:22674738

  7. Using Pd-salen complex as an efficient catalyst for the copper- and solvent-free coupling of acyl chlorides with terminal alkynes under aerobic conditions

    Institute of Scientific and Technical Information of China (English)

    Mohammad

    2010-01-01

    The palladium-salen complex palladium(Ⅱ) N,N'-bis{[5-(triphenylphosphonium)-methyl]salicylidene}-l,2-ethanediamine chloride was found to be a highly active catalyst for the copper- and solvent-free coupling reaction of terminal alkynes with different acyl chlorides in the presence of triethylamine as base, giving excellent ynones under aerobic conditions.

  8. Microwave-Enhanced Sulphated Zirconia and SZ/MCM-41 Catalyzed Regioselective Synthesis of β-Amino Alcohols Under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Eduardo González-Zamora

    2008-04-01

    Full Text Available A solvent-free approach for the regioselective synthesis of β-amino alcohols inshorter reaction times and higher yields, compared to conventional heating is described. Itinvolves microwave (MW exposure of undiluted reactants in the presence of sulphatedzirconia (SZ or sulphated zirconia over MCM-41 (SZM as catalyst. Both acid materialscan be easily recovered and reused.

  9. The extraction of essential oil from patchouli leaves (Pogostemon cablin Benth) using microwave hydrodistillation and solvent-free microwave extraction methods

    Science.gov (United States)

    Putri, D. K. Y.; Kusuma, H. S.; Syahputra, M. E.; Parasandi, D.; Mahfud, M.

    2017-12-01

    Patchouli plant (Pogostemon cablin Benth) is one of the important essential oil-producing plant, contributes more than 50% of total exports of Indonesia’s essential oil. However, the extraction of patchouli oil that has been done in Indonesia is generally still used conventional methods that require enormous amount of energy, high solvent usage, and long time of extraction. Therefore, in this study, patchouli oil extraction was carried out by using microwave hydrodistillation and solvent-free microwave extraction methods. Based on this research, it is known that the extraction of patchouli oil using microwave hydrodistillation method with longer extraction time (240 min) only produced patchouli oil’s yield 1.2 times greater than solvent-free microwave extraction method which require faster extraction time (120 min). Otherwise the analysis of electric consumption and the environmental impact, the solvent-free microwave extraction method showed a smaller amount when compared with microwave hydrodistillation method. It is conclude that the use of solvent-free microwave extraction method for patchouli oil extraction is suitably method as a new green technique.

  10. Synthesis of 1-amidoalkyl-2-naphthols based on a three-component reaction catalyzed by boric acid as a solid heterogeneous catalyst under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Zahed Karimi-Jaberi

    2012-12-01

    Full Text Available An efficient method for the preparation of 1-amidoalkyl-2-naphthols has been described using a multi-component, one-pot condensation reaction of 2-naphthol, aldehydes and amides in the presence of boric acid under solvent-free conditions.DOI: http://dx.doi.org/10.4314/bcse.v26i3.18

  11. Chemoselective Preparation of 1,1-Diacetates from Aldehydes, Mediated by a Keggin Heteropolyacid Under Solvent Free Conditions at Room Temperature

    Directory of Open Access Journals (Sweden)

    G. Romanelli

    2007-01-01

    Full Text Available A simple, general and efficient method has been developed for the conversion of aldehydes to 1,1-diacetates using acetic anhydride, a catalytic amount of non commercial Keggin heteropolyacid (H6 PalMo11O40 (1% mol in solvent free conditions at room temperature. Aromatic and aliphatic, simple and conjugated aldehydes were protected with excellent yields.

  12. Natrolite zeolite: A natural and reusable catalyst for one-pot synthesis of α-aminophosphonates under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Siavash Bahari

    2017-02-01

    Full Text Available α-Aminophosphonates are synthesized efficiently by one-pot reaction of aldehydes or ketones, amines, trialkyl phosphites in the presence of Natrolite zeolite as a natural catalyst under solvent-free conditions. Furthermore, the catalyst can be reused several times without any significant loss of catalytic activity.

  13. An efficient solvent-free synthesis of meso-substituted dipyrromethanes using SnCl2•2H2O catalysis

    Directory of Open Access Journals (Sweden)

    Kabeer Ahmed Shaikh

    2012-07-01

    Full Text Available Highly rapid and simple methodology has been developed for the quantitative synthesis of meso-substituted dipyrromethanes from lowest pyrrole/aldehyde ratio. The method was carried out by using SnCl2•2H2O as a catalyst under solvent free condition. The method is environmentally friendly, easy to workup, and gives excellent yield of the products.

  14. Synthesis and catalytic activity of Birnessite-Type Manganese Oxide synthesized by solvent-free method

    Science.gov (United States)

    Siregar, S. S.; Awaluddin, A.

    2018-04-01

    Redox reaction between KMnO4 and glucose usingsolvent-free method produces the octahedral layer birnessite-type manganese oxide. The effects of mole ratios, temperatures, and calcinations time on the structures and crystallinity of the oxides were studied throughthe X-ray powder diffraction analysis. The mole ratio of KMnO4/glucose (1:3) produces the purebirnessite with low crystallinity, whereas the mole ratio of KMnO4/glucose (3:1) yields high crystalline birnessite with minor components of hausmannite-type manganese oxide.The increasing of the temperature and calcinations times (300-700 °C and 3-7 h, respectively) willimprove the crystallinity and the purity of the as-synthesized oxide. Further experiments also showed that the as-syntesized octahedral layer birnessite-type manganese oxides have catalytic activity on the degradation of methylene blue (MB) dye with H2O2 as oxidant. The results revealed that the effective degradation could be achieved only in the presence of both the birnessite and H2O2, whereas without the addition of catalyst (H2O2only) or addition of H2O2 (catalyst only), the 3.5% and 15.5% of MB removal were obtained, respectively.

  15. Clean synthesis of biolubricant range esters using novel liquid lipase enzyme in solvent free medium.

    Science.gov (United States)

    Trivedi, Jayati; Aila, Mounika; Sharma, Chandra Dutt; Gupta, Piyush; Kaul, Savita

    2015-01-01

    In view of the rising global problems of environment pollution and degradation, the present process provides a 'green solution' to the synthesis of higher esters of lubricant range, more specifically in the range C12-C36, using different combinations of acids and alcohols, in a single step reaction. The esters produced are biodegradable in nature and have a plethora of uses, such as in additives, as lubricating oils and other hydraulic fluids. The enzymatic esterification was performed using liquid (non-immobilized or free) lipase enzyme, without any additional organic solvent. Soluble lipase proves to be superior to immobilized enzymes as it is more cost effective and provides a faster process for the production of higher esters of lubricant range. An interesting finding was, that the lipase enzyme showed higher conversion rates with increasing carbon number of straight chain alcohols and acids. Reactions were carried out for the optimization of initial water concentration, temperature, pH of the substrate mixture and the chain length of the substrates. Under optimized conditions, the method was suitable to achieve ~ 99% conversion. Thus, the process provides an environment friendly, enzymatic alternative to the chemical route which is currently used in the industrial synthesis of lubricant components.

  16. Solvent-free lipase catalysed synthesis of diacylgycerols as low-calorie food ingredients

    Directory of Open Access Journals (Sweden)

    Luis eVazquez

    2016-02-01

    Full Text Available Problems derived from obesity and overweight have recently promoted the development of fat substitutes and other low-calorie foods. On the one hand, fats with short and medium chain fatty acids are a source of quick energy, easily hydrolyzable and hardly stored as fat. Furthermore, 1,3-diacylglycerols are not hydrolyzed to 2-monoacylglycerols in the gastrointestinal tract, reducing the formation of chylomicron and lowers the serum level of triacylglycerols by decreasing its re-synthesis in the enterocyte and its metabolism and absorption by the enterocyte are limited in comparison with the TAG, reducing chylomicron formation. In this work these two effects were combined to synthesize short and medium chain 1,3 diacylglycerols, leading to a product with great potential as for their low-calorie properties. Lipase catalysed transesterification reactions were performed between short and medium chain fatty acid ethyl esters and glycerol. Different variables were investigated such as the type of biocatalyst, the molar ratio FAEE:glycerol, the adsorption of glycerol on silica gel or the addition of lecithin. Best reaction conditions were evaluated considering the conversion intopercentage of 1,3-DAG produced and the reaction rate. Except Novozym 435 (Candida antarctica, other lipases required the adsorption of glycerol on silica gel to form acylglycerols. Lipases that gave the best results with adsorption were Novozym 435 and Lipozyme RM IM (Rhizomucor miehei with 52% and 60.7% of DAG at 32 h, respectively. Because of its specificity for sn-1 and sn-3 positions, lipases leading to a higher proportion of 1,3-DAG vs 1,2-DAG were Lipozyme RM IM (39.8% and 20.9%, respectively and Lipase PLG (Alcaligenes sp. (35.9% and 19.3%, respectively. By adding 1% (w/w of lecithin to the reaction with Novozym 435 and raw glycerol the reaction rate was considerably increased from 41.7% to 52.8% DAG at 24 h.

  17. Solvent-Free Lipase-Catalyzed Synthesis of Diacylgycerols as Low-Calorie Food Ingredients.

    Science.gov (United States)

    Vázquez, Luis; González, Noemí; Reglero, Guillermo; Torres, Carlos

    2016-01-01

    Problems derived from obesity and overweight have recently promoted the development of fat substitutes and other low-calorie foods. On the one hand, fats with short- and medium-chain fatty acids are a source of quick energy, easily hydrolyzable and hardly stored as fat. Furthermore, 1,3-diacylglycerols are not hydrolyzed to 2-monoacylglycerols in the gastrointestinal tract, reducing the formation of chylomicron and lowers the serum level of triacylglycerols by decreasing its resynthesis in the enterocyte. In this work, these two effects were combined to synthesize short- and medium-chain 1,3-diacylglycerols, leading to a product with great potential as for their low-calorie properties. Lipase-catalyzed transesterification reactions were performed between short- and medium-chain fatty acid ethyl esters and glycerol. Different variables were investigated, such as the type of biocatalyst, the molar ratio FAEE:glycerol, the adsorption of glycerol on silica gel, or the addition of lecithin. Best reaction conditions were evaluated considering the percentage of 1,3-DAG produced and the reaction rate. Except Novozym 435 (Candida antarctica), other lipases required the adsorption of glycerol on silica gel to form acylglycerols. Lipases that gave the best results with adsorption were Novozym 435 and Lipozyme RM IM (Rhizomucor miehei) with 52 and 60.7% DAG at 32 h, respectively. Because of its specificity for sn-1 and sn-3 positions, lipases leading to a higher proportion of 1,3-DAG vs. 1,2-DAG were Lipozyme RM IM (39.8 and 20.9%, respectively) and Lipase PLG (Alcaligenes sp.) (35.9 and 19.3%, respectively). By adding 1% (w/w) of lecithin to the reaction with Novozym 435 and raw glycerol, the reaction rate was considerably increased from 41.7 to 52.8% DAG at 24 h.

  18. Optimization of 2-ethylhexyl palmitate production using lipozyme RM IM as catalyst in a solvent-free system.

    Science.gov (United States)

    Richetti, Aline; Leite, Selma G F; Antunes, Octávio A C; de Souza, Andrea L F; Lerin, Lindomar A; Dallago, Rogério M; Paroul, Natalia; Di Luccio, Marco; Oliveira, J Vladimir; Treichel, Helen; de Oliveira, Débora

    2010-04-01

    This work reports the application of a lipase in the 2-ethylhexyl palmitate esterification in a solvent-free system with an immobilized lipase (Lipozyme RM IM). A sequential strategy was used applying two experimental designs to optimize the 2-ethylhexyl palmitate production. An empirical model was then built so as to assess the effects of process variables on the reaction conversion. Afterwards, the operating conditions that optimized 2-ethylhexyl palmitate production were established as being acid/alcohol molar ratio 1:3, temperature of 70 degrees C, stirring rate of 150 rpm, 10 wt.% of enzyme, leading to a reaction conversion as high as 95%. From this point, a kinetic study was carried out evaluating the effect of acid:alcohol molar ratio, the enzyme concentration and the temperature on product conversion. The results obtained in this step permit to verify that an excess of alcohol (acid to alcohol molar ratio of 1:6), relatively low enzyme concentration (10 wt.%) and temperature of 70 degrees C, led to conversions next to 100%.

  19. A Solvent-Free Surface Suspension Melt Technique for Making Biodegradable PCL Membrane Scaffolds for Tissue Engineering Applications

    Directory of Open Access Journals (Sweden)

    Ratima Suntornnond

    2016-03-01

    Full Text Available In tissue engineering, there is limited availability of a simple, fast and solvent-free process for fabricating micro-porous thin membrane scaffolds. This paper presents the first report of a novel surface suspension melt technique to fabricate a micro-porous thin membrane scaffolds without using any organic solvent. Briefly, a layer of polycaprolactone (PCL particles is directly spread on top of water in the form of a suspension. After that, with the use of heat, the powder layer is transformed into a melted layer, and following cooling, a thin membrane is obtained. Two different sizes of PCL powder particles (100 µm and 500 µm are used. Results show that membranes made from 100 µm powders have lower thickness, smaller pore size, smoother surface, higher value of stiffness but lower ultimate tensile load compared to membranes made from 500 µm powder. C2C12 cell culture results indicate that the membrane supports cell growth and differentiation. Thus, this novel membrane generation method holds great promise for tissue engineering.

  20. Development of solvent-free offset ink using vegetable oil esters and high molecular-weight resin.

    Science.gov (United States)

    Park, Jung Min; Kim, Young Han; Kim, Sung Bin

    2013-01-01

    In the development of solvent-free offset ink, the roles of resin molecular weight and used solvent on the ink performance were evaluated by examining the relationship between the various properties of resin and solvent and print quality. To find the best performing resin, the soy-oil fatty acid methyl ester (FAME) was applied to the five modified-phenolic resins having different molecular weights. It is found from the experimental results that the ink made of higher molecular weight and better solubility resin gives better printability and print quality. It is because larger molecular weight resin with better solubility gives higher rate of ink transfer. From the ink application of different esters to high molecular weight resin, the best printing performance was yielded from the soy-oil fatty acid butyl ester (FABE). It is due to its high kinematic viscosity resulting in the smallest change of ink transfer weight upon multiple number of printing, which improves the stability of ink quality.

  1. Solvent-Free Microwave-Assisted Extraction of Polyphenols from Olive Tree Leaves: Antioxidant and Antimicrobial Properties.

    Science.gov (United States)

    Şahin, Selin; Samli, Ruya; Tan, Ayşe Seher Birteksöz; Barba, Francisco J; Chemat, Farid; Cravotto, Giancarlo; Lorenzo, José M

    2017-06-24

    Response surface methodology (RSM) and artificial neural networks (ANN) were evaluated and compared in order to decide which method was the most appropriate to predict and optimize total phenolic content (TPC) and oleuropein yields in olive tree leaf ( Olea europaea ) extracts, obtained after solvent-free microwave-assisted extraction (SFMAE). The SFMAE processing conditions were: microwave irradiation power 250-350 W, extraction time 2-3 min, and the amount of sample 5-10 g. Furthermore, the antioxidant and antimicrobial activities of the olive leaf extracts, obtained under optimal extraction conditions, were assessed by several in vitro assays. ANN had better prediction performance for TPC and oleuropein yields compared to RSM. The optimum extraction conditions to recover both TPC and oleuropein were: irradiation power 250 W, extraction time 2 min, and amount of sample 5 g, independent of the method used for prediction. Under these conditions, the maximal yield of oleuropein (0.060 ± 0.012 ppm) was obtained and the amount of TPC was 2.480 ± 0.060 ppm. Moreover, olive leaf extracts obtained under optimum SFMAE conditions showed antibacterial activity against S. aureus and S. epidermidis , with a minimum inhibitory concentration (MIC) value of 1.25 mg/mL.

  2. Improved interfacial adhesion in carbon fiber/polyether sulfone composites through an organic solvent-free polyamic acid sizing

    International Nuclear Information System (INIS)

    Yuan, Haojie; Zhang, Shouchun; Lu, Chunxiang; He, Shuqing; An, Feng

    2013-01-01

    An organic solvent-free polyamic acid (PAA) nanoemulsion was obtained by direct ionization of the solid PAA in deionized water, with the average particle size of 261 nm and Zeta potential of −55.1 mV, and used as a carbon fiber sizing to improve the interfacial adhesion between the carbon fiber and polyether sulfone (PES). The surface characteristics of PAA coated carbon fibers were investigated using Fourier transform infrared spectroscopy, scanning electron microscopy, atomic force microscopy and dynamic contact angle measurement. The results demonstrated that a continuous and uniform PAA sizing layer was formed on the surface of carbon fibers, and the surface energy of carbon fibers increased from 42.91 to 54.55 mN/m after sizing treatment. The single fiber pull-out testing was also performed, which showed the increased interfacial shear strength (IFSS) of carbon fiber/PES composites from 33.6 to 49.7 MPa by 47.9%. The major reasons for the improved interfacial adhesion were the increased van der Waals forces between the PES matrix and sizing layer as well as the chemical bonding between the sizing layer and carbon fiber surface. Furthermore, the PAA sizing also presented a positive effect on the interfacial adhesion of carbon fiber/PES composites under hydrothermal condition.

  3. Improved interfacial adhesion in carbon fiber/polyether sulfone composites through an organic solvent-free polyamic acid sizing

    Energy Technology Data Exchange (ETDEWEB)

    Yuan, Haojie [National Engineering Laboratory for carbon fiber technology, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Zhang, Shouchun, E-mail: zschun@sxicc.ac.cn [National Engineering Laboratory for carbon fiber technology, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001 (China); Lu, Chunxiang, E-mail: chunxl@sxicc.ac.cn [National Engineering Laboratory for carbon fiber technology, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001 (China); He, Shuqing [National Engineering Laboratory for carbon fiber technology, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); An, Feng [National Engineering Laboratory for carbon fiber technology, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001 (China)

    2013-08-15

    An organic solvent-free polyamic acid (PAA) nanoemulsion was obtained by direct ionization of the solid PAA in deionized water, with the average particle size of 261 nm and Zeta potential of −55.1 mV, and used as a carbon fiber sizing to improve the interfacial adhesion between the carbon fiber and polyether sulfone (PES). The surface characteristics of PAA coated carbon fibers were investigated using Fourier transform infrared spectroscopy, scanning electron microscopy, atomic force microscopy and dynamic contact angle measurement. The results demonstrated that a continuous and uniform PAA sizing layer was formed on the surface of carbon fibers, and the surface energy of carbon fibers increased from 42.91 to 54.55 mN/m after sizing treatment. The single fiber pull-out testing was also performed, which showed the increased interfacial shear strength (IFSS) of carbon fiber/PES composites from 33.6 to 49.7 MPa by 47.9%. The major reasons for the improved interfacial adhesion were the increased van der Waals forces between the PES matrix and sizing layer as well as the chemical bonding between the sizing layer and carbon fiber surface. Furthermore, the PAA sizing also presented a positive effect on the interfacial adhesion of carbon fiber/PES composites under hydrothermal condition.

  4. Solvent-Free Microwave-Assisted Extraction of Polyphenols from Olive Tree Leaves: Antioxidant and Antimicrobial Properties

    Directory of Open Access Journals (Sweden)

    Selin Şahin

    2017-06-01

    Full Text Available Response surface methodology (RSM and artificial neural networks (ANN were evaluated and compared in order to decide which method was the most appropriate to predict and optimize total phenolic content (TPC and oleuropein yields in olive tree leaf (Olea europaea extracts, obtained after solvent-free microwave-assisted extraction (SFMAE. The SFMAE processing conditions were: microwave irradiation power 250–350 W, extraction time 2–3 min, and the amount of sample 5–10 g. Furthermore, the antioxidant and antimicrobial activities of the olive leaf extracts, obtained under optimal extraction conditions, were assessed by several in vitro assays. ANN had better prediction performance for TPC and oleuropein yields compared to RSM. The optimum extraction conditions to recover both TPC and oleuropein were: irradiation power 250 W, extraction time 2 min, and amount of sample 5 g, independent of the method used for prediction. Under these conditions, the maximal yield of oleuropein (0.060 ± 0.012 ppm was obtained and the amount of TPC was 2.480 ± 0.060 ppm. Moreover, olive leaf extracts obtained under optimum SFMAE conditions showed antibacterial activity against S. aureus and S. epidermidis, with a minimum inhibitory concentration (MIC value of 1.25 mg/mL.

  5. Conversion of glycerol to polyglycerol over waste duck-bones as a catalyst in solvent free etherification process

    Science.gov (United States)

    Ayoub, Muhammad; Sufian, Suriati; Mekuria Hailegiorgis, Sintayehu; Ullah, Sami; Uemura, Yoshimitsu

    2017-08-01

    The alkaline catalyst derived from the duck-bones was used for conversion of glycerol to polyglycerol via solvent free etherification process. The physicochemical properties of prepared materials were duck-bones were systematically investigated as a catalyst by latest techniques of Thermo gravimetric analysis (TGA), X-ray diffraction (XRD), and Brunauer-Emmett-Teller (BET) surface properties. TGA showed different trends of duck-bones decomposition from room temperature to 1000C. XRD pattern showed a clear and sharp peaks of a crystalline phase of CaO. The activity of the catalysts was in line with the basic amount of the strong base sites, surface area, and crystalline phase in the catalysts. The prepared catalyst derived from duck-bones provided high activity (99 %) for glycerol conversion and around 68 % yield for polyglycerol production. These ample wastes of duck-bones have good potential to be used as polyglycerol production catalysts due to have high quantity of Ca compare to other types of bones like cow, chicken and fish bones.

  6. Orthogonal protection of saccharide polyols through solvent-free one-pot sequences based on regioselective silylations

    Directory of Open Access Journals (Sweden)

    Serena Traboni

    2016-12-01

    Full Text Available tert-Butyldimethylsilyl (TBDMS and tert-butyldiphenylsilyl (TBDPS are alcohol protecting groups widely employed in organic synthesis in view of their compatibility with a wide range of conditions. Their regioselective installation on polyols generally requires lengthy reactions and the use of high boiling solvents. In the first part of this paper we demonstrate that regioselective silylation of sugar polyols can be conducted in short times with the requisite silyl chloride and a very limited excess of pyridine (2–3 equivalents. Under these conditions, that can be regarded as solvent-free conditions in view of the insolubility of the polyol substrates, the reactions are faster than in most examples reported in the literature, and can even be further accelerated with a catalytic amount of tetrabutylammonium bromide (TBAB. The strategy proved also useful for either the selective TBDMS protection of secondary alcohols or the fast per-O-trimethylsilylation of saccharide polyols. In the second part of the paper the scope of the silylation approach was significantly extended with the development of unprecedented “one-pot” and “solvent-free” sequences allowing the regioselective silylation/alkylation (or the reverse sequence of saccharide polyols in short times. The developed methodologies represent a very useful and experimentally simple tool for the straightforward access to saccharide building-blocks useful in organic synthesis.

  7. New Trend for Acceleration Solid Phase Extraction Process Based on Using Magnetic Nano-adsorbents along with Surface Functionalization through Microwave Assisted Solvent-free Technique.

    Science.gov (United States)

    Ahmed, Salwa A; Soliman, Ezzat M

    2015-01-01

    The use of a microwave assisted solvent-free technique for silica coating of iron magnetic nanoparticles (Fe3O4-MNPs) and their functionalization with three aliphatic diamines: 1,2-ethylenediamine (1,2EDA), 1,5-pentanediamine (1,5PDA) and 1.8-octanediamine (1,8-ODA), were successfully achieved in a very short time. Only 60 min were needed for the nano-adsorbent modification as compared with more than 1000 min using conventional methods under reflux conditions. Their surface characteristics (observed by TEM, XRD and FT-IR), in addition to Cu(II) adsorption capacities (1.805, 1.928 and 2.116 mmol g(-1)) and time of equilibration (5 s) were almost the same. Thus, the time required to accomplish the solid phase extraction process is greatly reduced. On the other hand, the phenomenon of the fast equilibration kinetics was successfully extended on using the functionalized aliphatic diamines magnetic nano-adsorbents as precursors for further microwave treatment. Three selective magnetic nano-adsorbents (Fe3O4-MNPs-SiO2-1,2EDA-3FSA, Fe3O4-MNPs-SiO2-1,5PDA-3FSA and Fe3O4-MNPs-SiO2-1,8ODA-3FSA) were obtained via the reaction with 3-formayl salicylic acid (3FSA) as a selective reagent for Fe(III). At 5 s contact time, they exhibited maximum Fe(III) uptake equal to 4.512, 4.987 and 5.367 mmol g(-1), respectively. Furthermore, modeling of values of metal uptake capacity obtained at different shaking time intervals supports pseudo-second order kinetics.

  8. Structure factor of blends of solvent-free nanoparticle–organic hybrid materials: density-functional theory and small angle X-ray scattering

    KAUST Repository

    Yu, Hsiu-Yu

    2014-09-15

    © the Partner Organisations 2014. We investigate the static structure factor S(q) of solvent-free nanoparticle-organic hybrid materials consisting of silica nanocores and space-filling polyethylene glycol coronas using a density-functional theory and small angle X-ray scattering measurements. The theory considers a bidisperse suspension of hard spheres with different radii and tethered bead-spring oligomers with different grafting densities to approximate the polydispersity effects in experiments. The experimental systems studied include pure samples with different silica core volume fractions and the associated mean corona grafting densities, and blends with different mixing ratios of the pure samples, in order to introduce varying polydispersity of corona grafting density. Our scattering experiments and theory show that, compared to the hard-sphere suspension with the same core volume fraction, S(q) for pure samples exhibit both substantially smaller values at small q and stronger particle correlations corresponding to a larger effective hard core at large q, indicating that the tethered incompressible oligomers enforce a more uniform particle distribution, and the densely grafted brush gives rise to an additional exclusionary effect between the nanoparticles. According to the theory, polydispersity in the oligomer grafting density controls the deviation of S(q) from the monodisperse system at smaller q, and the interplay of the enhanced effective core size and the entropic attraction among the particles is responsible for complex variations in the particle correlations at larger q. The successful comparison between the predictions and the measurements for the blends further suggests that S(q) can be used to assess the uniformity of grafting density in polymer-grafted nanoparticle materials. This journal is

  9. Structure factor of blends of solvent-free nanoparticle-organic hybrid materials: density-functional theory and small angle X-ray scattering.

    Science.gov (United States)

    Yu, Hsiu-Yu; Srivastava, Samanvaya; Archer, Lynden A; Koch, Donald L

    2014-12-07

    We investigate the static structure factor S(q) of solvent-free nanoparticle-organic hybrid materials consisting of silica nanocores and space-filling polyethylene glycol coronas using a density-functional theory and small angle X-ray scattering measurements. The theory considers a bidisperse suspension of hard spheres with different radii and tethered bead-spring oligomers with different grafting densities to approximate the polydispersity effects in experiments. The experimental systems studied include pure samples with different silica core volume fractions and the associated mean corona grafting densities, and blends with different mixing ratios of the pure samples, in order to introduce varying polydispersity of corona grafting density. Our scattering experiments and theory show that, compared to the hard-sphere suspension with the same core volume fraction, S(q) for pure samples exhibit both substantially smaller values at small q and stronger particle correlations corresponding to a larger effective hard core at large q, indicating that the tethered incompressible oligomers enforce a more uniform particle distribution, and the densely grafted brush gives rise to an additional exclusionary effect between the nanoparticles. According to the theory, polydispersity in the oligomer grafting density controls the deviation of S(q) from the monodisperse system at smaller q, and the interplay of the enhanced effective core size and the entropic attraction among the particles is responsible for complex variations in the particle correlations at larger q. The successful comparison between the predictions and the measurements for the blends further suggests that S(q) can be used to assess the uniformity of grafting density in polymer-grafted nanoparticle materials.

  10. Silica sulfuric acid: a reusable solid catalyst for one pot synthesis of densely substituted pyrrole-fused isocoumarins under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Sudipta Pathak

    2013-11-01

    Full Text Available A convenient and efficient methodology for the synthesis of densely substituted pyrrole-fused isocoumarins, which employs solid-supported silica sulfuric acid (SSA as catalyst, has been developed. When the mixture of ninhydrin adducts of acetylacetone/ethyl acetoacetate and primary amines was heated on the solid surface of SSA under solvent-free conditions, the pyrrole-fused isocoumarins were formed in good yields. This synthetic method has several advantages such as the employment of solvent-free reaction conditions without the use of any toxic reagents and metal catalysts, the ease of product isolation, the use of a recyclable catalyst, the low cost, the easy availability of the starting materials, and the excellent yields of products.

  11. Solvent-free directed patterning of a highly ordered liquid crystalline organic semiconductor via template-assisted self-assembly for organic transistors.

    Science.gov (United States)

    Kim, Aryeon; Jang, Kwang-Suk; Kim, Jinsoo; Won, Jong Chan; Yi, Mi Hye; Kim, Hanim; Yoon, Dong Ki; Shin, Tae Joo; Lee, Myong-Hoon; Ka, Jae-Won; Kim, Yun Ho

    2013-11-20

    Highly ordered organic semiconductor micropatterns of the liquid-crystalline small molecule 2,7-didecylbenzothienobenzothiophene (C10 -BTBT) are fabricated using a simple method based on template-assisted self-assembly (TASA). The liquid crystallinity of C10 -BTBT allows solvent-free fabrication of high-performance printed organic field-effect transistors (OFETs). © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. A facile solvent-free Synthesis Route for the Assembly of Highly CO2 Selective and H2S tolerant NiSIFSIX Metal-Organic Framework

    KAUST Repository

    Eddaoudi, Mohamed; Shekhah, Osama; Belmabkhout, Youssef; Adil, Karim; Cairns, Amy J.; Bhatt, Prashant

    2015-01-01

    The development of materials for CO2 capture with high selectivity and high tolerance to H2S is of prime importance for various industrially relevant gas streams (e.g. natural gas and biogas upgrading as well as pre-combustion capture). Here, we report the successful fabrication of a MOF with combined exceptional CO2 capture properties and H2S tolerance, namely Ni SIFSIX based-MOF using both solvothermal and solvent-free methodologies.

  13. One-pot solvent-free rapid and green synthesis of 3,4-dihydropyrano[c]chromenes using grindstone chemistry

    Directory of Open Access Journals (Sweden)

    Devji S. Patel

    2016-09-01

    Full Text Available An easy solvent-free method is described for the synthesis of 3,4-dihydropyrano[c]chromenes by a one pot three component coupling reaction of aromatic aldehydes, malononitrile, and 4-hydroxycoumarin using basic ionic liquid as the catalyst by grindstone chemistry. The salient features of this one pot protocol are short reaction times, cleaner reaction profiles and simple workup.

  14. A facile solvent-free Synthesis Route for the Assembly of Highly CO2 Selective and H2S tolerant NiSIFSIX Metal-Organic Framework

    KAUST Repository

    Eddaoudi, Mohamed

    2015-07-06

    The development of materials for CO2 capture with high selectivity and high tolerance to H2S is of prime importance for various industrially relevant gas streams (e.g. natural gas and biogas upgrading as well as pre-combustion capture). Here, we report the successful fabrication of a MOF with combined exceptional CO2 capture properties and H2S tolerance, namely Ni SIFSIX based-MOF using both solvothermal and solvent-free methodologies.

  15. Fast and efficient method for reduction of carbonyl compounds with NaBH{sub 4} /wet SiO{sub 2} under solvent free condition

    Energy Technology Data Exchange (ETDEWEB)

    Zeynizadeh, Behzad; Bahyar, Tarifeh [Urmia University, Urmia (Iran, Islamic Republic of). Faculty of Sciences. Dept. of Chemistry]. E-mail: b.zeynizadeh@mail.urmia.ac.ir

    2005-11-15

    Reduction of structurally different carbonyl compounds such as aldehydes, ketones, {alpha},{beta}-unsaturated enals and enones, {alpha}-diketones and acyloins were accomplished efficiently by sodium borohydride in the presence of wet SiO{sub 2} (30% m/m) under solvent free condition. The reactions were performed at room tempere or 75-80 deg C with high to excellent yields of the corresponding products. The chemoselective reduction of aldehydes over ketones was achieved successfully with this reducing system. (author)

  16. Fast and efficient method for reduction of carbonyl compounds with NaBH4 /wet SiO2 under solvent free condition

    International Nuclear Information System (INIS)

    Zeynizadeh, Behzad; Bahyar, Tarifeh

    2005-01-01

    Reduction of structurally different carbonyl compounds such as aldehydes, ketones, α,β-unsaturated enals and enones, α-diketones and acyloins were accomplished efficiently by sodium borohydride in the presence of wet SiO 2 (30% m/m) under solvent free condition. The reactions were performed at room temperature or 75-80 deg C with high to excellent yields of the corresponding products. The chemoselective reduction of aldehydes over ketones was achieved successfully with this reducing system. (author)

  17. Solvent-Free Lipase-Catalyzed Synthesis of Technical-Grade Sugar Esters and Evaluation of Their Physicochemical and Bioactive Properties

    Directory of Open Access Journals (Sweden)

    Ran Ye

    2016-05-01

    Full Text Available Technical-grade oleic acid esters of sucrose and fructose were prepared using solvent-free biocatalysis at 65 °C, without any downstream purification applied, and their physicochemical and bioactivity-related properties were evaluated and compared to a commercially available sucrose laurate emulsifier. To increase the conversion of sucrose and fructose oleate, prepared previously using solvent-free lipase-catalyzed esterification catalyzed by Rhizomucor miehei lipase (81% and 83% ester, respectively, the enzymatic reaction conditions was continued using CaSO4 to control the reactor’s air headspace and a lipase (from Candida antarctica B with a hydrophobic immobilization matrix to provide an ultralow water activity, and high-pressure homogenation, to form metastable suspensions of 2.0–3.3 micron sized saccharide particles in liquid-phase reaction media. These measures led to increased ester content of 89% and 96% for reactions involving sucrose and fructose, respectively. The monoester content among the esters decreased from 90% to <70% due to differences in regioselectivity between the lipases. The resultant technical-grade sucrose and fructose lowered the surface tension to <30 mN/m, and possessed excellent emulsification capability and stability over 36 h using hexadecane and dodecane as oils, comparable to that of sucrose laurate and Tween® 80. The technical-grade sugar esters, particularly fructose oleate, more effectively inhibited gram-positive foodborne pathogens (Lactobacillus plantarum, Pediococcus pentosaceus and Bacillus subtilis. Furthermore, all three sugar esters displayed antitumor activity, particularly the two sucrose esters. This study demonstrates the importance of controlling the biocatalysts’ water activity to achieve high conversion, the impact of a lipase’s regioselectivity in dictating product distribution, and the use of solvent-free biocatalysis to important biobased surfactants useful in foods, cosmetics

  18. FeF(3) catalyzed cascade C-C and C-N bond formation: synthesis of differentially substituted triheterocyclic benzothiazole functionalities under solvent-free condition.

    Science.gov (United States)

    Atar, Amol B; Jeong, Yeon Tae

    2014-05-01

    A series of diverse polyfunctionalized triheterocyclic benzothiazoles were easily prepared in excellent yields via the Biginelli reaction of 2-aminobenzothiazole with substituted benzaldehydes and α-methylene ketones using FeF(3) as an expeditious catalyst under solvent-free conditions. The protocol provides a practical and straightforward approach toward highly functionalized triheterocyclic benzothiazole derivatives in excellent yields. The reaction was conveniently promoted by FeF(3) and the catalyst could be recovered easily after the reaction and reused without any loss of its catalytic activity. The advantageous features of this methodology are high atom economy, operational simplicity, shorter reaction time, convergence, and facile automation.

  19. Parameters affecting incorporation and by-product formation during the production of structured phospholipids by lipase-catalyzed acidolysis in solvent free system

    DEFF Research Database (Denmark)

    Vikbjerg, Anders Falk; Mu, Huiling; Xu, Xuebing

    2005-01-01

    By-product formation is a serious problem in the lipase-catalyzed acyl exchange of phospholipids (PL). By-products are formed due to parallel hydrolysis reactions and acyl migration in the reaction system. A clear elucidation of these side reactions is important for practical operation in order...... to minimize by-products during reaction. In the present study we examined the Lipozyme RM IM-catalyzed acidolysis for the production of structured phospholipids between phosphatidylcholine (PC) and caprylic acid in the solvent free system. A five-factor response surface design was used to evaluate...

  20. Benign and efficient preparation of thioethers by solvent-free S-alkylation of thiols with alkyl halides catalyzed by potassium fluoride on alumina

    DEFF Research Database (Denmark)

    Nguyen, Kha Ngoc; Duus, Fritz; Luu, Thi Xuan Thi

    2016-01-01

    The preparation of thioethers by S-alkylation of various thiols with alkyl halides under solvent-free reaction conditions using potassium fluoride on alumina (KF/Al2O3) as a solid catalyst has been investigated in detail with respect to three different modes of reaction activation (ultrasound...... irradiation, microwave irradiation, and conventional heating) for obtaining maximum yield of the thioether. The importance of KF/Al2O3 as a particularly efficient catalyst was corroborated for all three modes of reaction activation, although the reaction time was found to be strongly dependent on the mode...

  1. Traceable atomic force microscopy of high-quality solvent-free crystals of [6,6]-phenyl-C61-butyric acid methyl ester

    OpenAIRE

    Lazzerini, GM; Paterno, GM; Tregnago, G; Treat, N; Stingelin, N; Yacoot, A; Cacialli, F

    2016-01-01

    We report high-resolution, traceable atomic force microscopymeasurements of high-quality, solvent-free single crystals of [6,6]-phenyl-C61-butyric acid methyl ester (PCBM). These were grown by drop-casting PCBM solutions onto the spectrosil substrates and by removing the residual solvent in a vacuum. A home-built atomic force microscope featuring a plane mirror differential optical interferometer, fiber-fed from a frequency-stabilized laser (emitting at 632.8???nm), was used to measure the cr...

  2. Traceable atomic force microscopy of high-quality solvent-free crystals of [6,6]-phenyl-C-61-butyric acid methyl ester

    OpenAIRE

    Lazzerini, G. M.; Paterno, G. M.; Tregnago, G.; Treat, N.; Stingelin, N.; Yacoot, A.; Cacialli, F.

    2016-01-01

    We report high-resolution, traceable atomic force microscopymeasurements of high-quality, solvent-free single crystals of [6,6]-phenyl-C61-butyric acid methyl ester (PCBM). These were grown by drop-casting PCBM solutions onto the spectrosil substrates and by removing the residual solvent in a vacuum. A home-built atomic force microscope featuring a plane mirror differential optical interferometer, fiber-fed from a frequency-stabilized laser (emitting at 632.8 nm), was used to measure the crys...

  3. “Flash” Solvent-free Synthesis of Triazoles Using a Supported Catalyst

    Directory of Open Access Journals (Sweden)

    Ibtissem Jlalia

    2009-01-01

    Full Text Available A solvent-free synthesis of 1,4-disubstituted-1,2,3-triazoles using neat azides and alkynes and a copper(I polymer supported catalyst (Amberlyst® A21•CuI is presented herein. As it provides the products in high yields and purities within minutes, this method thus being characterized as a "flash" synthesis, and was exemplified through the synthesis of a 24-compound library on a small scale.

  4. A Simple, Rapid and Mild One Pot Synthesis of Benzene Ring Acylated and Demethylated Analogues of Harmine under Solvent-free Conditions

    Directory of Open Access Journals (Sweden)

    Bina S. Siddiqui

    2008-08-01

    Full Text Available A simple, rapid, solvent-free, room temperature one pot synthesis of benzene ring acylated and demethylated analogues of harmine using acyl halides/acid anhydrides and AlCl3 has been developed. Eight different acyl halides/acid anhydrides were used in the synthesis. The resulting mixture of products was separated by column chromatography to afford 10- and 12-monoacyl analogues, along with 10,12-diacyl-11-hydroxy products. In five cases the corresponding 10-acyl-11-hydroxy analogues were also obtained. Yields from the eight syntheses (29 products in total were in the 6-34% range and all compounds were fully characterized.

  5. Lithium-Acetate-Mediated Biginelli One-Pot Multicomponent Synthesis under Solvent-Free Conditions and Cytotoxic Activity against the Human Lung Cancer Cell Line A549 and Breast Cancer Cell Line MCF7

    Directory of Open Access Journals (Sweden)

    Harshita Sachdeva

    2012-01-01

    Full Text Available Various Biginelli compounds (dihydropyrimidinones have been synthesized efficiently and in high yields under mild, solvent-free, and eco-friendly conditions in a one-pot reaction of 1,3-dicarbonyl compounds, aldehydes, and urea/thiourea/acetyl thiourea using lithium-acetate as a novel catalyst without the addition of any proton source. Comparative catalytic efficiency of lithium-acetate and polyphosphoric acid to catalyze Biginelli condensation is also studied under neat conditions. The reaction is carried out in the absence of any solvent and represents an improvement of the classical Biginelli protocol and an advantage in comparison with FeCl3·6H2O, NiCl2·6H2O and CoCl2·6H2O that were used with HCl as a cocatalyst. Compared to classical Biginelli reaction conditions, the present method has advantages of good yields, short reaction times, and experimental simplicity. The obtained products have been identified by spectral (1H NMR and IR data and their melting points. The prepared compounds are evaluated for anticancer activity against two human cancer cell lines (lung cancer cell line A549 and breast cancer cell line MCF7.

  6. Solvent-free oxidation of secondary alcohols to carbonyl compounds by 1, 3-Dibromo-5, 5-Dimethylhydantoin (DBDMH) and 1, 3-Dichloro-5, 5-Dimethylhydantoin (DCDMH)

    Energy Technology Data Exchange (ETDEWEB)

    Khazaei, Ardeshir; Abbasi, Fatemeh, E-mail: Khazaei_1326@yahoo.com, E-mail: fatemehabbasi807@gmail.com [Faculty of Chemistry, Department of Organic Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Kianiborazjani, Maryam [Faculty of Science, Department of Chemistry, Bushehr Payame Noor University (PNU), Bushehr (Iran, Islamic Republic of); Saednia, Shahnaz [Young Researchers Club, Toyserkan Branch, Islamic Azad University, Toyserkan (Iran, Islamic Republic of)

    2014-02-15

    Aldehydes and ketones are important intermediates, especially for the construction of carbon-skeletons. The oxidation of alcohols is so important that a large number of methods and reagents have been reported for this purpose. N-halo reagents are widely used in organic synthesis and as a continuation of our interest in the application of N-halo compounds in organic synthesis, dibromo dimethylhydantoin (DBDMH) and dichloro dimethylhydantoin (DCDMH) were used for the oxidation of alcohols and our ongoing work on development of highly efficient oxidation protocols. We observed the oxidation of secondary alcohols with stoichiometric amounts of DBDMH and DCDMH under solvent-free conditions in the range of temperature 70-80 deg C. (author)

  7. Highly Regio- and Stereoselective Diels-Alder Cycloadditions via Two-Step and Multicomponent Reactions Promoted by Infrared Irradiation under Solvent-Free Conditions

    Science.gov (United States)

    Flores-Conde, Maria Ines; Reyes, Leonor; Herrera, Rafael; Rios, Hulme; Vazquez, Miguel A.; Miranda, Rene; Tamariz, Joaquin; Delgado, Francisco

    2012-01-01

    Infrared irradiation promoted the Diels-Alder cycloadditions of exo-2-oxazolidinone dienes 1–3 with the Knoevenagel adducts 4–6, as dienophiles, leading to the synthesis of new 3,5-diphenyltetrahydrobenzo[d]oxazol-2-one derivatives (7, 9, 11 and 13–17), under solvent-free conditions. These cycloadditions were performed with good regio- and stereoselectivity, favoring the para-endo cycloadducts. We also evaluated the one-pot three-component reaction of active methylene compounds 20, benzaldehydes 21 and exo-2-oxazolidinone diene 2 under the same reaction conditions. A cascade Knoevenagel condensation/Diels-Alder cycloaddition reaction was observed, resulting in the final adducts 13–16 in similar yields. These procedures are environmentally benign, because no solvent and no catalyst were employed in these processes. The regioselectivity of these reactions was rationalized by Frontier Molecular Orbital (FMO) calculations. PMID:22489113

  8. Highly Regio- and Stereoselective Diels-Alder Cycloadditions via Two-Step and Multicomponent Reactions Promoted by Infrared Irradiation under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Francisco Delgado

    2012-02-01

    Full Text Available Infrared irradiation promoted the Diels-Alder cycloadditions of exo-2-oxazolidinone dienes 1–3 with the Knoevenagel adducts 4–6, as dienophiles, leading to the synthesis of new 3,5-diphenyltetrahydrobenzo[d]oxazol-2-one derivatives (7, 9, 11 and 13–17, under solvent-free conditions. These cycloadditions were performed with good regio- and stereoselectivity, favoring the para-endo cycloadducts. We also evaluated the one-pot three-component reaction of active methylene compounds 20, benzaldehydes 21 and exo-2-oxazolidinone diene 2 under the same reaction conditions. A cascade Knoevenagel condensation/Diels-Alder cycloaddition reaction was observed, resulting in the final adducts 13–16 in similar yields. These procedures are environmentally benign, because no solvent and no catalyst were employed in these processes. The regioselectivity of these reactions was rationalized by Frontier Molecular Orbital (FMO calculations.

  9. Sequential Dy(OTf)3 -Catalyzed Solvent-Free Per-O-Acetylation and Regioselective Anomeric De-O-Acetylation of Carbohydrates.

    Science.gov (United States)

    Yan, Yi-Ling; Guo, Jiun-Rung; Liang, Chien-Fu

    2017-09-19

    Dysprosium(III) trifluoromethanesulfonate-catalyzed per-O-acetylation and regioselective anomeric de-O-acetylation of carbohydrates can be tuned by adjusting the reaction medium. In this study, the per-O-acetylation of unprotected sugars by using a near-stoichiometric amount of acetic anhydride under solvent-free conditions resulted in the exclusive formation of acetylated saccharides as anomeric mixtures, whereas anomeric de-O-acetylation in methanol resulted in a moderate-to-excellent yield. Reactions with various unprotected monosaccharides or disaccharides followed by a semi-one-pot sequential conversion into the corresponding acetylated glycosyl hemiacetal also resulted in high yields. Furthermore, the obtained hemiacetals could be successfully transformed into trichloroimidates after Dy(OTf) 3 -catalyzed glycosylation. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. High-sensitivity green resist material with organic solvent-free spin-coating and tetramethylammonium hydroxide-free water-developable processes for EB and EUV lithography

    Science.gov (United States)

    Takei, Satoshi; Hanabata, Makoto; Oshima, Akihiro; Kashiwakura, Miki; Kozawa, Takahiro; Tagawa, Seiichi

    2015-03-01

    We investigated the eco-friendly electron beam (EB) and extreme-ultraviolet (EUV) lithography using a high-sensitive negative type of green resist material derived from biomass to take advantage of organic solvent-free water spin-coating and tetramethylammonium hydroxide(TMAH)-free water-developable techniques. A water developable, non-chemically amplified, high sensitive, and negative tone resist material in EB lithography was developed for environmental affair, safety, easiness of handling, and health of the working people, instead of the common developable process of TMAH. The material design concept to use the water-soluble resist material with acceptable properties such as pillar patterns with less than 100 nm in high EB sensitivity of 10 μC/cm2 and etch selectivity with a silicon-based middle layer in CF4 plasma treatment was demonstrated for EB and EUV lithography.

  11. Vanadium Hydrogen Sulfate Catalyzed Solvent-Free Synthesis of 3,4-Dihydropyrimidin-2(1H)-ones and Bis-(indolyl) methanes

    Energy Technology Data Exchange (ETDEWEB)

    Shirini, F.; Yahyazadeh, A.; Abedini, M.; Langroodi, D. Imani [Univ. of Guilan, Rasht (Iran, Islamic Republic of)

    2010-06-15

    We have developed a mild, simple and efficient method for the synthesis of 3,4-dihydropyrimidin-2(1H)-ones/thiones and bis-(indolyl) methanes catalyzed by V(HSO{sub 4}){sub 3}. Based on our studies, this method offers several adavantages including mild reaction conditions, good to high yields of the products, short reaction times, solvent-free reaction conditions and simple experimental procedure. 3,4-Dihydropyrimidin-2(1H)-ones and their derivatives have attracted increasing interest due to their wide range of therapeutical and pharmacological properties, such as antiviral, antitumor, antibacterial, and antiinflammatory properties. Some of them have been successfully used as calcium channel blockers, antihypertensive agents, and α1a-antagonists. Moreover, several marine alkaloids whose molecular structures contain the dihydropyrimidinone core also exhibit interesting biological activities. Therefore, synthesis of these type of compounds is still of great importance.

  12. Vanadium Hydrogen Sulfate Catalyzed Solvent-Free Synthesis of 3,4-Dihydropyrimidin-2(1H)-ones and Bis-(indolyl) methanes

    International Nuclear Information System (INIS)

    Shirini, F.; Yahyazadeh, A.; Abedini, M.; Langroodi, D. Imani

    2010-01-01

    We have developed a mild, simple and efficient method for the synthesis of 3,4-dihydropyrimidin-2(1H)-ones/thiones and bis-(indolyl) methanes catalyzed by V(HSO 4 ) 3 . Based on our studies, this method offers several adavantages including mild reaction conditions, good to high yields of the products, short reaction times, solvent-free reaction conditions and simple experimental procedure. 3,4-Dihydropyrimidin-2(1H)-ones and their derivatives have attracted increasing interest due to their wide range of therapeutical and pharmacological properties, such as antiviral, antitumor, antibacterial, and antiinflammatory properties. Some of them have been successfully used as calcium channel blockers, antihypertensive agents, and α1a-antagonists. Moreover, several marine alkaloids whose molecular structures contain the dihydropyrimidinone core also exhibit interesting biological activities. Therefore, synthesis of these type of compounds is still of great importance

  13. Chemical composition and antibacterial activity of Origanum saccatum P.H. Davis essential oil obtained by solvent-free microwave extraction: comparison with hydrodistillation.

    Science.gov (United States)

    Sozmen, Fazli; Uysal, Burcu; Oksal, Birsen S; Kose, Elif Odabas; Deniz, I Gokhan

    2011-01-01

    The components of the essential oils (EOs) obtained by solvent-free microwave extraction (SFME) and hydrodistillation (HD) from endemic Origanum saccatum P.H. Davis were identified by using GC/MS. The main constituents of both EOs obtained by SFME and HD, respectively, from O. saccatum were p-cymene (72.5 and 70.6%), thymol (9.32 and 8.11%), and carvacrol (7.18 and 6.36%). The EO obtained by SFME contained substantially higher amounts of oxygenated compounds and lower amounts of monoterpenes than did the EO obtained by HD. The antibacterial activities of the EOs obtained by SFME and HD were evaluated with the disc diffusion method by comparison with 10 different bacterial strains. The antibacterial activity of the EO extracted by SFME was found to be more effective than that of the EO extracted by HD against seven of the tested bacteria.

  14. One Pot Synthesis of α-Aminophosphonates Containing Bromo and 3,4,5-Trimethoxybenzyl Groups under Solvent-free Conditions

    Directory of Open Access Journals (Sweden)

    Wei Xue

    2007-02-01

    Full Text Available New α-aminophosphonates were synthesized by the Kabachnik-Fields reactionof 3,4,5-trimethoxybenzaldehyde (TMB with p- or m-bromoaniline and a dialkylphosphite under solvent-free conditions. TMB was prepared from gallic acid via a fourstep synthetic sequence involving etherification, esterification, hydrazidation andpotassium ferricyanide oxidation. The structures of all synthesized compounds wereconfirmed by elemental analysis, IR, 1H-, 13C- and 31P-NMR spectral data. Compound 7gwas also characterized by X-ray crystallography. A half-leaf method was used todetermine the in vivo curative efficacy of the eight title products against tobacco mosaicvirus (TMV. It was found that compounds 7g and 7h possess good in vivo curativeeffects against TMV.

  15. Dipyridine cobalt chloride as an efficient and chemoselective catalyst for the synthesis of 1,1-diacetates under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Sobhan Rezayati

    2014-02-01

    Full Text Available 1,1-Diacetates(acylals were prepared by direct condensation of various aldehydes with acetic anhydride using dipyridine cobalt chloride (CoPy2Cl2 as an efficient and green catalyst under solvent-free conditions at room temperature. The important features of this catalyst method are that the catalyst is solid, stable at high temperatures, soluble in water, stable in air, immiscible in common organic solvents, and low toxic and, above all, it is reusable. CoPy2Cl2 can be recycled after a simple work-up and reused at least five runs without appreciable loss of its catalytic activity. High chemo-selectivity toward aldehyde in the presence of ketones is another advantage of the present method which provides selective protection of aldehydes in their mixtures with ketones.

  16. MICROWAVE-ASSISTED CU (I) CATALYZED SOLVENT-FREE THREE COMPONENT COUPLING OF ALDEHYDE, ALKYNE AND AMINE

    Science.gov (United States)

    Direct Grignard type addition of terminal alkynes to in situ generated imines, from aldehydes and amines, occurs under microwave irradiation using CuBr alone in a one-pot operation. This solventless approach provides ready access to propargylamines and is applicable both...

  17. Piper-betle-shaped nano-S-catalyzed synthesis of 1-amidoalkyl-2-naphthols under solvent-free reaction condition: a greener "nanoparticle-catalyzed organic synthesis enhancement" approach.

    Science.gov (United States)

    Das, Vijay K; Borah, Madhurjya; Thakur, Ashim J

    2013-04-05

    Nano-S prepared by an annealing process showed excellent catalytic activity for the synthesis of 1-amidoalkyl-2-naphthols under solvent-free reaction condition at 50 °C. The catalyst could be reused up to the fifth cycle without loss in its action. The green-ness of the present protocol was also measured using green metrics drawing its superiority.

  18. Solvent-free and room temperature synthesis of 3-arylquinolines from different anilines and styrene oxide in the presence of Al2O3/MeSO3H

    Directory of Open Access Journals (Sweden)

    Hashem Sharghi

    2017-09-01

    Full Text Available A highly efficient, simple and environmentally friendly synthesis of 3-arylquinolines has been developed in the presence of Al2O3/MeSO3H via one-pot reaction of anilines and styrene oxide. This methodology provides very rapid access to 3-arylquinolines in good to excellent yields under solvent-free conditions at room temperature in air.

  19. Mechanochemical Solvent-Free and Catalyst-Free One-Pot Synthesis of Pyrano[2,3-d]Pyrimidine-2,4(1H,3H-Diones with Quantitative Yields

    Directory of Open Access Journals (Sweden)

    M. Reza Naimi-Jamal

    2009-01-01

    Full Text Available Solvent-free synthesis of pyrano[2,3-d]pyrimidine-2,4(1H,3H-diones by ball-milling and without any catalyst is described. This method provides several advantages such as being environmentally friendly, using a simple workup procedure, and affording high yields.

  20. Synthesis of Cycloveratrylene Macrocycles and Benzyl Oligomers Catalysed by Bentonite under Microwave/Infrared and Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Manuel Salmón

    2013-10-01

    Full Text Available Tonsil Actisil FF, which is a commercial bentonitic clay, promotes the formation of cycloveratrylene macrocycles and benzyl oligomers from the corresponding benzyl alcohols in good yields under microwave heating and infrared irradiation in the absence of solvent in both cases. The catalytic reaction is sensitive to the type of substituent on the aromatic ring. Thus, when benzyl alcohol was substituted with a methylenedioxy, two methoxy or three methoxy groups, a cyclooligomerisation process was induced. Unsubstituted, methyl and methoxy benzyl alcohols yielded linear oligomers. In addition, computational chemistry calculations were performed to establish a validated mechanistic pathway to explain the growth of the obtained linear oligomers.

  1. Continuous Preparation of 1:1 Haloperidol-Maleic Acid Salt by a Novel Solvent-Free Method Using a Twin Screw Melt Extruder.

    Science.gov (United States)

    Lee, Hung Lin; Vasoya, Jaydip M; Cirqueira, Marilia de Lima; Yeh, Kuan Lin; Lee, Tu; Serajuddin, Abu T M

    2017-04-03

    Salts are generally prepared by acid-base reaction in relatively large volumes of organic solvents, followed by crystallization. In this study, the potential for preparing a pharmaceutical salt between haloperidol and maleic acid by a novel solvent-free method using a twin-screw melt extruder was investigated. The pH-solubility relationship between haloperidol and maleic acid in aqueous medium was first determined, which demonstrated that 1:1 salt formation between them was feasible (pH max 4.8; salt solubility 4.7 mg/mL). Extrusion of a 1:1 mixture of haloperidol and maleic acid at the extruder barrel temperature of 60 °C resulted in the formation of a highly crystalline salt. The effects of operating temperature and screw configuration on salt formation were also investigated, and those two were identified as key processing parameters. Salts were also prepared by solution crystallization from ethyl acetate, liquid-assisted grinding, and heat-assisted grinding and compared with those obtained by melt extrusion by using DSC, PXRD, TGA, and optical microscopy. While similar salts were obtained by all methods, both melt extrusion and solution crystallization yielded highly crystalline materials with identical enthalpies of melting. During the pH-solubility study, a salt hydrate form was also identified, which, upon heating, converted to anhydrate similar to that obtained by other methods. There were previous reports of the formation of cocrystals, but not salts, by melt extrusion. 1 H NMR and single-crystal X-ray diffraction confirmed that a salt was indeed formed in the present study. The haloperidol-maleic acid salt obtained was nonhygroscopic in the moisture sorption study and converted to the hydrate form only upon mixing with water. Thus, we are reporting for the first time a relatively simple and solvent-free twin-screw melt extrusion method for the preparation of a pharmaceutical salt that provides material comparable to that obtained by solution

  2. Solvent-Free Selective Oxidation of Toluene with O2 Catalyzed by Metal Cation Modified LDHs and Mixed Oxides

    Directory of Open Access Journals (Sweden)

    Xiaoli Wang

    2016-01-01

    Full Text Available A series of metal cation modified layered-double hydroxides (LDHs and mixed oxides were prepared and used to be the selective oxidation of toluene with O2. The results revealed that the modified LDHs exhibited much higher catalytic performance than their parent LDH and the modified mixed oxides. Moreover, the metal cations were also found to play important roles in the catalytic performance and stabilities of modified catalysts. Under the optimal reaction conditions, the highest toluene conversion reached 8.7% with 97.5% of the selectivity to benzyldehyde; moreover, the catalytic performance remained after nine catalytic runs. In addition, the reaction probably involved a free-radical mechanism.

  3. Solvent-free biodegradable scleral plugs providing sustained release of vancomycin, amikacin, and dexamethasone--an in vivo study.

    Science.gov (United States)

    Peng, Yi-Jie; Kau, Yi-Chuan; Wen, Chin-Wei; Liu, Kuo-Sheng; Liu, Shih-Jung

    2010-08-01

    Delivering effective drugs at sufficiently high concentrations to the area of infection is a standard treatment for infectious disease, such as endophthalmitis. This is currently done by empirical trans pars plana intravitreal injection of both antibiotics directed against gram-positive and gram-negative microorganisms and steroids. However, injections by needles repeatedly may increase the risks of intraocular infection and hemorrhage, as well as retinal detachment. This article explores the alternative of using biodegradable polymers as scleral plugs for a long-term drug release in vivo. To manufacture plugs, poly(lactide-glycolide) copolymers were first mixed with vancomycin, amikacin, and dexamethasone. The mixture was compressed and sintered at 55 degrees C to form scleral plugs 1.4 mm in diameter. Biodegradable scleral plugs released high concentrations of antibiotics (well above the minimum inhibitory concentrations, MIC) and steroids in vivo for the period of time needed to treat intraocular infection. In addition, no major complications such as infectious or sterile endophthalmitis, retinal detachment, ocular phthisis, or uvea protrusion at sclerotomy site were observed throughout the experiment. The sclerotomy wound healed after total degradation of the scleral implants without leakage or local necrosis. Antibiotic/steroid-impregnated biodegradable scleral plugs may have a potential role in the treatment of various intraocular infections. (c) 2010 Wiley Periodicals, Inc.

  4. CO2-assisted high pressure homogenization: a solvent-free process for polymeric microspheres and drug-polymer composites.

    Science.gov (United States)

    Kluge, Johannes; Mazzotti, Marco

    2012-10-15

    The study explores the enabling role of near-critical CO(2) as a reversible plasticizer in the high pressure homogenization of polymer particles, aiming at their comminution as well as at the formation of drug-polymer composites. First, the effect of near-critical CO(2) on the homogenization of aqueous suspensions of poly lactic-co-glycolic acid (PLGA) was investigated. Applying a pressure drop of 900 bar and up to 150 passes across the homogenizer, it was found that particles processed in the presence of CO(2) were generally of microspherical morphology and at all times significantly smaller than those obtained in the absence of a plasticizer. The smallest particles, exhibiting a median x(50) of 1.3 μm, were obtained by adding a small quantity of ethyl acetate, which exerts on PLGA an additional plasticizing effect during the homogenization step. Further, the study concerns the possibility of forming drug-polymer composites through simultaneous high pressure homogenization of the two relevant solids, and particularly the effect of near-critical CO(2) on this process. Therefore, PLGA was homogenized together with crystalline S-ketoprofen (S-KET), a non-steroidal anti-inflammatory drug, at a drug to polymer ratio of 1:10, a pressure drop of 900 bar and up to 150 passes across the homogenizer. When the process was carried out in the presence of CO(2), an impregnation efficiency of 91% has been reached, corresponding to 8.3 wt.% of S-KET in PLGA; moreover, composite particles were of microspherical morphology and significantly smaller than those obtained in the absence of CO(2). The formation of drug-polymer composites through simultaneous homogenization of the two materials is thus greatly enhanced by the presence of CO(2), which increases the efficiency for both homogenization and impregnation. Copyright © 2012 Elsevier B.V. All rights reserved.

  5. Organic Solvent-Free Fabrication of Durable and Multifunctional Superhydrophobic Paper from Waterborne Fluorinated Cellulose Nanofiber Building Blocks.

    Science.gov (United States)

    Baidya, Avijit; Ganayee, Mohd Azhardin; Jakka Ravindran, Swathy; Tam, Kam Chiu; Das, Sarit Kumar; Ras, Robin H A; Pradeep, Thalappil

    2017-11-28

    In view of a great demand for paper-based technologies, nonwettable fibrous substrates with excellent durability have drawn much attention in recent years. In this context, the use of cellulose nanofibers (CNFs), the smallest unit of cellulosic substrates (5-20 nm wide and 500 nm to several microns in length), to design waterproof paper can be an economical and smart approach. In this study, an eco-friendly and facile methodology to develop a multifunctional waterproof paper via the fabrication of fluoroalkyl functionalized CNFs in the aqueous medium is presented. This strategy avoids the need for organic solvents, thereby minimizing cost as well as reducing safety and environmental concerns. Besides, it widens the applicability of such materials as nanocellulose-based aqueous coatings on hard and soft substrates including paper, in large areas. Water droplets showed a contact angle of 160° (±2°) over these surfaces and rolled off easily. While native CNFs are extremely hydrophilic and can be dispersed in water easily, these waterborne fluorinated CNFs allow the fabrication of a superhydrophobic film that does not redisperse upon submersion in water. Incorporated chemical functionalities provide excellent durability toward mechanochemical damages of relevance to daily use such as knife scratch, sand abrasion, spillage of organic solvents, etc. Mechanical flexibility of the chemically modified CNF composed paper remains intact despite its enhanced mechanical strength, without additives. Superhydrophobicity induced excellent microbial resistance of the waterproof paper which expands its utility in various paper-based technologies. This includes waterproof electronics, currency, books, etc., where the integrity of the fibers, as demonstrated here, is a much-needed criterion.

  6. ZnAl2O4@SiO2 nanocomposite catalyst for the acetylation of alcohols, phenols and amines with acetic anhydride under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    Saeed Farhadi; Kosar Jahanara

    2014-01-01

    A ZnAl2O4@SiO2 nanocomposite was prepared from metal nitrates and tetraethyl orthosilicate by the sol-gel process, and characterized by X-ray diffraction, Fourier transform infrared, transmission electron microscopy, and N2 adsorption-desorption measurements. The nanocomposite was tested as a heterogeneous catalyst for the acetylation of alcohols, phenols, and amines under solvent-free conditions. Under optimized conditions, efficient acetylation of these substrates with acetic anhy-dride over the ZnAl2O4@SiO2 nanocomposite was obtained. Acetylation of anilines and primary aliphatic amines proceeded rapidly at room temperature, while the reaction time was longer for the acetylation of alcohols and phenols, showing that an amine NH2 group can be selectively acetylated in the presence of alcoholic or phenolic OH groups. The catalyst can be reused without obvious loss of catalytic activity. The catalytic activity of the ZnAl2O4@SiO2 nanocomposite was higher than that of pure ZnAl2O4. The method gives high yields, and is clean, cost effective, compatible with sub-strates having other functional groups and it is suitable for practical organic synthesis.

  7. First-Row-Transition Ion Metals(II-EDTA Functionalized Magnetic Nanoparticles as Catalysts for Solvent-Free Microwave-Induced Oxidation of Alcohols

    Directory of Open Access Journals (Sweden)

    Nuno M. R. Martins

    2017-11-01

    Full Text Available A series of first-row transition-metals combined with ethylenediamine tetraacetic acid (EDTA, as metal-based N,O-chelating ligands, at the surface of ferrite magnetic nanoparticles (MNPs was prepared by a co-precipitation method. Those EDTA functionalized MNPs with general formula Fe3O4@EDTA-M2+ [M = Mn2+ (1, Fe2+ (2, Co2+ (3, Ni2+ (4, Cu2+ (5 or Zn2+ (6] were characterized by FTIR (Fourier Transform Infrared spectroscopy, powder XRD (X-ray Diffraction, SEM (Scanning Electron Microscope, EDS (Energy Dispersive Spectrometer, VSM (Vibrating Sample Magnetometer and TGA (Thermal Gravity Analysis. The application of the magnetic NPs towards the microwave-assisted oxidation of several alcohol substrates in a solvent-free medium was evaluated. The influence of reaction parameters such as temperature, time, type of oxidant, and presence of organic radicals was investigated. This study demonstrates that these MNPs can act as efficient catalysts for the conversion of alcohols to the corresponding ketones or aldehydes with high selectivity and yields up to 99% after 2 h of reaction at 110 °C using t-BuOOH as oxidant. Moreover, they have the advantage of being magnetically recoverable catalysts that can be easily recycled in following runs.

  8. Solvent-free functionalization of silicone rubber and efficacy of PAAm brushes grafted from an amino-PPX layer against bacterial adhesion.

    Science.gov (United States)

    Fundeanu, Irina; Klee, Doris; Schouten, Arend J; Busscher, Henk J; van der Mei, Henny C

    2010-11-01

    Silicone rubber is a frequently employed biomaterial that is prone to bacterial adhesion and biofilm formation. In this study, the surface of silicone rubber was solvent-free functionalized by chemical vapor deposition (CVD) of poly(o-amino-p-xylylene-co-p-xylylene (amino-PPX). Subsequently, the amino groups of the amino-PPX layer were used to introduce the initiator from a vapor phase for atom transfer radical polymerization of acrylamide to form polyacrylamide (PAAm) brushes. The modification steps were verified by means of X-ray photoelectron spectroscopy and attenuated total reflection-Fourier transform infrared spectroscopy. Adhesion of Staphylococcus aureus ATCC 12600 and Escherichia coli 3.14 to an amino-PPX-PAAm brush coating in a parallel plate flow chamber was strongly reduced with respect to non-coated silicone rubber - by 93% and 99%, respectively. For E. coli 3.14, this reduction is larger than that obtained for solvent functionalization of γ-aminopropyltriethoxysilane-PAAm brushes due to the higher density of amino groups introduced by the CVD of amino-PPX. Copyright © 2010 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

  9. Comparative Study of Essential Oils Extracted from Egyptian Basil Leaves (Ocimum basilicum L.) Using Hydro-Distillation and Solvent-Free Microwave Extraction.

    Science.gov (United States)

    Chenni, Mohammed; El Abed, Douniazad; Rakotomanomana, Njara; Fernandez, Xavier; Chemat, Farid

    2016-01-19

    Solvent-free microwave extraction (SFME) and conventional hydro-distillation (HD) were used for the extraction of essential oils (EOs) from Egyptian sweet basil (Ocimum basilicum L.) leaves. The two resulting EOs were compared with regards to their chemical composition, antioxidant, and antimicrobial activities. The EO analyzed by GC and GC-MS, presented 65 compounds constituting 99.3% and 99.0% of the total oils obtained by SFME and HD, respectively. The main components of both oils were linalool (43.5% SFME; 48.4% HD), followed by methyl chavicol (13.3% SFME; 14.3% HD) and 1,8-cineole (6.8% SFME; 7.3% HD). Their antioxidant activity were studied with the 2,2-diphenyl-1-picrylhydrazyl (DPPH(•)) radical scavenging method. The heating conditions effect was evaluated by the determination of the Total Polar Materials (TPM) content. The antimicrobial activity was investigated against five microorganisms: two Gram-positive bacteria, Staphylococcus aureus and Bacillus subtilis, two Gram-negative bacteria, Escherichia coli and Pseudomonas aeruginosa, and one yeast, Candida albicans. Both EOs showed high antimicrobial, but weak antioxidant, activities. The results indicated that the SFME method may be a better alternative for the extraction of EO from O. basilicum since it could be considered as providing a richer source of natural antioxidants, as well as strong antimicrobial agents for food preservation.

  10. Performance of an enzymatic packed bed reactor running on babassu oil to yield fatty ethyl esters (FAEE in a solvent-free system

    Directory of Open Access Journals (Sweden)

    Aline Simões

    2015-06-01

    Full Text Available The transesterification reaction of babassu oil with ethanol mediated by Burkholderia cepacia lipase immobilized on SiO2-PVA composite was assessed in a packed bed reactor running in the continuous mode. Experiments were performed in a solvent-free system at 50 °C. The performance of the reactor (14 mm ×210 mm was evaluated using babassu oil and ethanol at two molar ratios of 1:7 and 1:12, respectively, and operational limits in terms of substrate flow rate were determined. The system’s performance was quantified for different flow rates corresponding to space times between 7 and 13 h. Under each condition, the impact of the space time on the ethyl esters formation, the transesterification yield and productivity were determined. The oil to ethanol molar ratio was found as a critical parameter in the conversion of babassu oil into the correspondent ethyl esters. The highest transesterification yield of 96.0 ± 0.9% and productivity of 41.1 ± 1.6 mgester gcatalyst-1h-1 were achieved at the oil to ethanol molar ratio of 1:12 and for space times equal or higher than 11 h. Moreover, the immobilized lipase was found stable with respect to its catalytic characteristics, exhibiting a half-life of 32 d.

  11. Magnetic amine-functionalized graphene oxide as a novel and recyclable bifunctional nanocatalyst for solvent-free synthesis of pyrano[3,2-c]pyridine derivatives

    Directory of Open Access Journals (Sweden)

    Shahnaz Rostamizadeh

    2017-01-01

    Full Text Available The new magnetic amine-functionalized graphene oxide (Fe3O4-GO-NH2 nanocatalyst was prepared through the reaction of 3-aminopropyltriethoxysilane (APTES with magnetic graphene oxide (Fe3O4-GO. It was characterized by XRD, TEM, SEM, FT-IR and EDX techniques. The intrinsic carboxylic acids on the edges of Fe3O4-GO along with the amine groups post grafted to the surface of Fe3O4-GO led to preparation of an acid-base bifunctional magnetically recyclable nanocatalyst. It proved to be efficient nanocatalyst for solvent-free synthesis of pyrano[3,2-c]pyridine derivatives under mild reaction conditions with good to excellent yields. This heterogeneous catalyst also exhibited higher activities than acid or base functionalized mesoporous silica, magnetic GO or basic Al2O3 an even higher than some basic homogeneous catalysts such as triethylamine and piperazine. More importantly, due to the loaded iron oxide nanoparticles, this catalyst could be easily recovered from the reaction mixture using an external magnet and reused without significant decrease in activity even after 7 runs.

  12. Optimization of the production of biodiesel by a commercial immobilized lipase in a solvent-free system using a response surface methodology

    Directory of Open Access Journals (Sweden)

    ZORICA KNEZEVIC

    2008-02-01

    Full Text Available Response surface methodology was used for the evaluation of the effects of various factors on the synthesis of biodiesel catalyzed with immobilized lipase from Rhizomucor miehei in a solvent-free system. The production of biodiesel was optimized and model response equations were obtained, enabling the prediction of biodiesel production from the values of the four main factors. It would seem that the reaction temperature and the amount of water predominantly determined the conversion process while the methanol/oil molar ratio had no significant influence on the reaction rate. The temperature and amount of water showed negative interactive effects on the observed reaction rate per amount of enzyme. However, there were no significant interactions among the other variables according to the test of statistical significance. The highest yield of 10.15 mol kg-1 enzyme was observed at 45 °C with a 6:1 methanol to oil molar ratio and with no added water in the system.

  13. Traceable atomic force microscopy of high-quality solvent-free crystals of [6,6]-phenyl-C61-butyric acid methyl ester

    International Nuclear Information System (INIS)

    Lazzerini, Giovanni Mattia; Yacoot, Andrew; Paternò, Giuseppe Maria; Tregnago, Giulia; Cacialli, Franco; Treat, Neil; Stingelin, Natalie

    2016-01-01

    We report high-resolution, traceable atomic force microscopy measurements of high-quality, solvent-free single crystals of [6,6]-phenyl-C61-butyric acid methyl ester (PCBM). These were grown by drop-casting PCBM solutions onto the spectrosil substrates and by removing the residual solvent in a vacuum. A home-built atomic force microscope featuring a plane mirror differential optical interferometer, fiber-fed from a frequency-stabilized laser (emitting at 632.8 nm), was used to measure the crystals' height. The optical interferometer together with the stabilized laser provides traceability (via the laser wavelength) of the vertical measurements made with the atomic force microscope. We find that the crystals can conform to the surface topography, thanks to their height being significantly smaller compared to their lateral dimensions (namely, heights between about 50 nm and 140 nm, for the crystals analysed, vs. several tens of microns lateral dimensions). The vast majority of the crystals are flat, but an isolated, non-flat crystal provides insights into the growth mechanism and allows identification of “molecular terraces” whose height corresponds to one of the lattice constants of the single PCBM crystal (1.4 nm) as measured with X-ray diffraction

  14. Traceable atomic force microscopy of high-quality solvent-free crystals of [6,6]-phenyl-C61-butyric acid methyl ester

    Science.gov (United States)

    Lazzerini, Giovanni Mattia; Paternò, Giuseppe Maria; Tregnago, Giulia; Treat, Neil; Stingelin, Natalie; Yacoot, Andrew; Cacialli, Franco

    2016-02-01

    We report high-resolution, traceable atomic force microscopy measurements of high-quality, solvent-free single crystals of [6,6]-phenyl-C61-butyric acid methyl ester (PCBM). These were grown by drop-casting PCBM solutions onto the spectrosil substrates and by removing the residual solvent in a vacuum. A home-built atomic force microscope featuring a plane mirror differential optical interferometer, fiber-fed from a frequency-stabilized laser (emitting at 632.8 nm), was used to measure the crystals' height. The optical interferometer together with the stabilized laser provides traceability (via the laser wavelength) of the vertical measurements made with the atomic force microscope. We find that the crystals can conform to the surface topography, thanks to their height being significantly smaller compared to their lateral dimensions (namely, heights between about 50 nm and 140 nm, for the crystals analysed, vs. several tens of microns lateral dimensions). The vast majority of the crystals are flat, but an isolated, non-flat crystal provides insights into the growth mechanism and allows identification of "molecular terraces" whose height corresponds to one of the lattice constants of the single PCBM crystal (1.4 nm) as measured with X-ray diffraction.

  15. Traceable atomic force microscopy of high-quality solvent-free crystals of [6,6]-phenyl-C{sub 61}-butyric acid methyl ester

    Energy Technology Data Exchange (ETDEWEB)

    Lazzerini, Giovanni Mattia; Yacoot, Andrew [National Physical Laboratory, Hampton Road, Teddington, Middlesex TW11 0LW (United Kingdom); Paternò, Giuseppe Maria; Tregnago, Giulia; Cacialli, Franco [Department of Physics and Astronomy and London Centre for Nanotechnology, University College London, Gower Street, London WC1E 6BT (United Kingdom); Treat, Neil; Stingelin, Natalie [Department of Materials Science, Imperial College London, London SW7 2AZ (United Kingdom)

    2016-02-01

    We report high-resolution, traceable atomic force microscopy measurements of high-quality, solvent-free single crystals of [6,6]-phenyl-C61-butyric acid methyl ester (PCBM). These were grown by drop-casting PCBM solutions onto the spectrosil substrates and by removing the residual solvent in a vacuum. A home-built atomic force microscope featuring a plane mirror differential optical interferometer, fiber-fed from a frequency-stabilized laser (emitting at 632.8 nm), was used to measure the crystals' height. The optical interferometer together with the stabilized laser provides traceability (via the laser wavelength) of the vertical measurements made with the atomic force microscope. We find that the crystals can conform to the surface topography, thanks to their height being significantly smaller compared to their lateral dimensions (namely, heights between about 50 nm and 140 nm, for the crystals analysed, vs. several tens of microns lateral dimensions). The vast majority of the crystals are flat, but an isolated, non-flat crystal provides insights into the growth mechanism and allows identification of “molecular terraces” whose height corresponds to one of the lattice constants of the single PCBM crystal (1.4 nm) as measured with X-ray diffraction.

  16. Solvent-free sample preparation by headspace solid-phase microextraction applied to the tracing of n-butyl nitrite abuse.

    Science.gov (United States)

    Tytgat, J; Daenens, P

    1996-01-01

    The most common alkyl nitrites encountered in forensic toxicology are iso-butyl, n-butyl and iso-pentyl(amyl) nitrites. All have become popular as an aphrodisiac, especially among the homosexual population. Alkyl nitrites are a volatile and unstable group of compounds, which hydrolyse in aqueous matrices to the alcohol and nitrite ion. Here we describe a fast, clean and sensitive procedure for the detection of hydrolysed n-butyl nitrite in whole human blood using a new, solvent-free sampling technique, the headspace solid-phase micro-extraction (HSPME), combined with GC/FID analysis. Sample preparation was investigated using two different stationary phases (100 microns polydimethylsiloxane and 85 microns polyacrylate), coating a fused silica fibre. The effect of different sampling times at fixed temperatures was also studied. Our results demonstrate that the HSPME/GC/FID procedure allows tracing of n-butyl nitrite abuse and detects hydrolysed n-butyl nitrite, i.e., released n-butanol, in whole blood at the 1 ng/mL level.

  17. Molecular imaging of banknote and questioned document using solvent-free gold nanoparticle-assisted laser desorption/ionization imaging mass spectrometry.

    Science.gov (United States)

    Tang, Ho-Wai; Wong, Melody Yee-Man; Chan, Sharon Lai-Fung; Che, Chi-Ming; Ng, Kwan-Ming

    2011-01-01

    Direct chemical analysis and molecular imaging of questioned documents in a non/minimal-destructive manner is important in forensic science. Here, we demonstrate that solvent-free gold-nanoparticle-assisted laser desorption/ionization mass spectrometry is a sensitive and minimal destructive method for direct detection and imaging of ink and visible and/or fluorescent dyes printed on banknotes or written on questioned documents. Argon ion sputtering of a gold foil allows homogeneous coating of a thin layer of gold nanoparticles on banknotes and checks in a dry state without delocalizing spatial distributions of the analytes. Upon N(2) laser irradiation of the gold nanoparticle-coated banknotes or checks, abundant ions are desorbed and detected. Recording the spatial distributions of the ions can reveal the molecular images of visible and fluorescent ink printed on banknotes and determine the printing order of different ink which may be useful in differentiating real banknotes from fakes. The method can also be applied to identify forged parts in questioned documents, such as number/writing alteration on a check, by tracing different writing patterns that come from different pens.

  18. Immobilization of Pseudomonas fluorescens lipase on hydrophobic supports and application in biodiesel synthesis by transesterification of vegetable oils in solvent-free systems.

    Science.gov (United States)

    Lima, Lionete N; Oliveira, Gladson C; Rojas, Mayerlenis J; Castro, Heizir F; Da Rós, Patrícia C M; Mendes, Adriano A; Giordano, Raquel L C; Tardioli, Paulo W

    2015-04-01

    This work describes the preparation of biocatalysts for ethanolysis of soybean and babassu oils in solvent-free systems. Polystyrene, Amberlite (XAD-7HP), and octyl-silica were tested as supports for the immobilization of Pseudomonas fluorescens lipase (PFL). The use of octyl-silica resulted in a biocatalyst with high values of hydrolytic activity (650.0 ± 15.5 IU/g), immobilization yield (91.3 ± 0.3 %), and recovered activity (82.1 ± 1.5 %). PFL immobilized on octyl-silica was around 12-fold more stable than soluble PFL, at 45 °C and pH 8.0, in the presence of ethanol at 36 % (v/v). The biocatalyst provided high vegetable oil transesterification yields of around 97.5 % after 24 h of reaction using babassu oil and around 80 % after 48 h of reaction using soybean oil. The PFL-octyl-silica biocatalyst retained around 90 % of its initial activity after five cycles of transesterification of soybean oil. Octyl-silica is a promising support that can be used to immobilize PFL for subsequent application in biodiesel synthesis.

  19. Organic solvent-free air-assisted liquid-liquid microextraction for optimized extraction of illegal azo-based dyes and their main metabolite from spices, cosmetics and human bio-fluid samples in one step.

    Science.gov (United States)

    Barfi, Behruz; Asghari, Alireza; Rajabi, Maryam; Sabzalian, Sedigheh

    2015-08-15

    Air-assisted liquid-liquid microextraction (AALLME) has unique capabilities to develop as an organic solvent-free and one-step microextraction method, applying ionic-liquids as extraction solvent and avoiding centrifugation step. Herein, a novel and simple eco-friendly method, termed one-step air-assisted liquid-liquid microextraction (OS-AALLME), was developed to extract some illegal azo-based dyes (including Sudan I to IV, and Orange G) from food and cosmetic products. A series of experiments were investigated to achieve the most favorable conditions (including extraction solvent: 77μL of 1-Hexyl-3-methylimidazolium hexafluorophosphate; sample pH 6.3, without salt addition; and extraction cycles: 25 during 100s of sonication) using a central composite design strategy. Under these conditions, limits of detection, linear dynamic ranges, enrichment factors and consumptive indices were in the range of 3.9-84.8ngmL(-1), 0.013-3.1μgmL(-1), 33-39, and 0.13-0.15, respectively. The results showed that -as well as its simplicity, fastness, and use of no hazardous disperser and extraction solvents- OS-AALLME is an enough sensitive and efficient method for the extraction of these dyes from complex matrices. After optimization and validation, OS-AALLME was applied to estimate the concentration of 1-amino-2-naphthol in human bio-fluids as a main reductive metabolite of selected dyes. Levels of 1-amino-2-naphthol in plasma and urinary excretion suggested that this compound may be used as a new potential biomarker of these dyes in human body. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Optimisation and Characterisation of Lipase-Catalysed Synthesis of a Kojic Monooleate Ester in a Solvent-Free System by Response Surface Methodology.

    Directory of Open Access Journals (Sweden)

    Khairulazhar Jumbri

    Full Text Available Kojic acid is widely used to inhibit the browning effect of tyrosinase in cosmetic and food industries. In this work, synthesis of kojic monooleate ester (KMO was carried out using lipase-catalysed esterification of kojic acid and oleic acid in a solvent-free system. Response Surface Methodology (RSM based on central composite rotatable design (CCRD was used to optimise the main important reaction variables, such as enzyme amount, reaction temperature, substrate molar ratio, and reaction time along with immobilised lipase from Candida Antarctica (Novozym 435 as a biocatalyst. The RSM data indicated that the reaction temperature was less significant in comparison to other factors for the production of a KMO ester. By using this statistical analysis, a quadratic model was developed in order to correlate the preparation variable to the response (reaction yield. The optimum conditions for the enzymatic synthesis of KMO were as follows: an enzyme amount of 2.0 wt%, reaction temperature of 83.69°C, substrate molar ratio of 1:2.37 (mmole kojic acid:oleic acid and a reaction time of 300.0 min. Under these conditions, the actual yield percentage obtained was 42.09%, which is comparably well with the maximum predicted value of 44.46%. Under the optimal conditions, Novozym 435 could be reused for 5 cycles for KMO production percentage yield of at least 40%. The results demonstrated that statistical analysis using RSM can be used efficiently to optimise the production of a KMO ester. Moreover, the optimum conditions obtained can be applied to scale-up the process and minimise the cost.

  1. Solid-state flurbiprofen and methyl-β-cyclodextrin inclusion complexes prepared using a single-step, organic solvent-free supercritical fluid process.

    Science.gov (United States)

    Rudrangi, Shashi Ravi Suman; Kaialy, Waseem; Ghori, Muhammad U; Trivedi, Vivek; Snowden, Martin J; Alexander, Bruce David

    2016-07-01

    The aim of this study was to enhance the apparent solubility and dissolution properties of flurbiprofen through inclusion complexation with cyclodextrins. Especially, the efficacy of supercritical fluid technology as a preparative technique for the preparation of flurbiprofen-methyl-β-cyclodextrin inclusion complexes was evaluated. The complexes were prepared by supercritical carbon dioxide processing and were evaluated by solubility, differential scanning calorimetry, X-ray powder diffraction, scanning electron microscopy, practical yield, drug content estimation and in vitro dissolution studies. Computational molecular docking studies were conducted to study the possibility of molecular arrangement of inclusion complexes between flurbiprofen and methyl-β-cyclodextrin. The studies support the formation of stable molecular inclusion complexes between the drug and cyclodextrin in a 1:1 stoichiometry. In vitro dissolution studies showed that the dissolution properties of flurbiprofen were significantly enhanced by the binary mixtures prepared by supercritical carbon dioxide processing. The amount of flurbiprofen dissolved into solution alone was very low with 1.11±0.09% dissolving at the end of 60min, while the binary mixtures processed by supercritical carbon dioxide at 45°C and 200bar released 99.39±2.34% of the drug at the end of 30min. All the binary mixtures processed by supercritical carbon dioxide at 45°C exhibited a drug release of more than 80% within the first 10min irrespective of the pressure employed. The study demonstrated the single step, organic solvent-free supercritical carbon dioxide process as a promising approach for the preparation of inclusion complexes between flurbiprofen and methyl-β-cyclodextrin in solid-state. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Optimisation and Characterisation of Lipase-Catalysed Synthesis of a Kojic Monooleate Ester in a Solvent-Free System by Response Surface Methodology.

    Science.gov (United States)

    Jumbri, Khairulazhar; Al-Haniff Rozy, Mohd Fahruddin; Ashari, Siti Efliza; Mohamad, Rosfarizan; Basri, Mahiran; Fard Masoumi, Hamid Reza

    2015-01-01

    Kojic acid is widely used to inhibit the browning effect of tyrosinase in cosmetic and food industries. In this work, synthesis of kojic monooleate ester (KMO) was carried out using lipase-catalysed esterification of kojic acid and oleic acid in a solvent-free system. Response Surface Methodology (RSM) based on central composite rotatable design (CCRD) was used to optimise the main important reaction variables, such as enzyme amount, reaction temperature, substrate molar ratio, and reaction time along with immobilised lipase from Candida Antarctica (Novozym 435) as a biocatalyst. The RSM data indicated that the reaction temperature was less significant in comparison to other factors for the production of a KMO ester. By using this statistical analysis, a quadratic model was developed in order to correlate the preparation variable to the response (reaction yield). The optimum conditions for the enzymatic synthesis of KMO were as follows: an enzyme amount of 2.0 wt%, reaction temperature of 83.69°C, substrate molar ratio of 1:2.37 (mmole kojic acid:oleic acid) and a reaction time of 300.0 min. Under these conditions, the actual yield percentage obtained was 42.09%, which is comparably well with the maximum predicted value of 44.46%. Under the optimal conditions, Novozym 435 could be reused for 5 cycles for KMO production percentage yield of at least 40%. The results demonstrated that statistical analysis using RSM can be used efficiently to optimise the production of a KMO ester. Moreover, the optimum conditions obtained can be applied to scale-up the process and minimise the cost.

  3. Solvent-free thermoplastic-poly(dimethylsiloxane) bonding mediated by UV irradiation followed by gas-phase chemical deposition of an adhesion linker

    Science.gov (United States)

    Ahn, S. Y.; Lee, N. Y.

    2015-07-01

    Here, we introduce a solvent-free strategy for bonding various thermoplastic substrates with poly(dimethylsiloxane) (PDMS) using ultraviolet (UV) irradiation followed by the gas-phase chemical deposition of aminosilane on the UV-irradiated thermoplastic substrates. The thermoplastic substrates were first irradiated with UV for surface hydrophilic treatment and were then grafted with vacuum-evaporated aminosilane, where the alkoxysilane side reacted with the oxidized surface of the thermoplastic substrate. Next, the amine-terminated thermoplastic substrates were treated with corona discharge to oxidize the surface and were bonded with PDMS, which was also oxidized via corona discharge. The two substrates were then hermetically sealed and pressed under atmospheric pressure for 30 min at 60 °C. This process enabled the formation of a robust siloxane bond (Si-O-Si) between the thermoplastic substrate and PDMS under relatively mild conditions using an inexpensive and commercially available UV lamp and Tesla coil. Various thermoplastic substrates were examined for bonding with PDMS, including poly(methylmethacrylate) (PMMA), polycarbonate (PC), poly(ethyleneterephthalate) (PET) and polystyrene (PS). Surface characterizations were performed by measuring the contact angle and performing x-ray photoelectron spectroscopy analysis, and the bond strength was analyzed by conducting various mechanical force measurements such as pull, delamination, leak and burst tests. The average bond strengths for the PMMA-PDMS, PC-PDMS, PET-PDMS and PS-PDMS assemblies were measured at 823.6, 379.3, 291.2 and 229.0 kPa, respectively, confirming the highly reliable performance of the introduced bonding strategy.

  4. Microwave Assisted Convenient One-Pot Synthesis of Coumarin Derivatives via Pechmann Condensation Catalyzed by FeF3 under Solvent-Free Conditions and Antimicrobial Activities of the Products

    Directory of Open Access Journals (Sweden)

    Vahid Vahabi

    2014-08-01

    Full Text Available A rapid and efficient solvent-free one-pot synthesis of coumarin derivatives by Pechmann condensation reactions of phenols with ethyl acetoacetate using FeF3 as a catalyst under microwave irradiation is described. This one-pot synthesis on a solid inorganic support provides the products in good yields. The newly synthesized compounds were systematically characterized by IR, 1H-NMR, 13C-NMR, MS and elemental CHN analyses. The proposed solvent-free microwave irradiation method using the environmentally friendly catalyst FeF3 offers the unique advantages of high yields, shorter reaction times, easy and quick isolation of the products, excellent chemoselectivity, and a one-pot, green synthesis. The products were screened for antimicrobial activity, and the results showed that the compounds reacted against all the tested bacteria.

  5. Potassium Hydroxide Impregnated Alumina (KOH-Alumina) as a Recyclable Catalyst for the Solvent-Free Multicomponent Synthesis of Highly Functionalized Substituted Pyridazines and/or Substituted Pyridazin-3(2H)-ones under Microwave Irradiation.

    Science.gov (United States)

    Mecadon, Hormi; Myrboh, Bekington

    2011-01-01

    The work described herein employs potassium hydroxide impregnated alumina (KOH-alumina) as a mild, efficient, and recyclable catalyst for a one-pot solvent-free and environmentally safer synthesis of 3,4,6-triarylpyridazines and some substituted pyridazines from active methylene carbonyl species, 1,2-dicarbonyls, and hydrazine hydrate by microwave (MW) irradiation. The method offers highly convergent, inexpensive, and functionality-tolerable procedure for rapid access to important pyridazine compounds in good yields.

  6. Two New 1,1,3,3-Tetramethylguanidinium Halochromates (C5H14N3CrO3X (X: Cl, F: Efficient Reagents for Oxidation of Organic Substrates under Solvent-Free Conditions and Microwave Irradiation

    Directory of Open Access Journals (Sweden)

    Kıvılcım Şendıl

    2016-01-01

    Full Text Available Two new mild oxidizing agents 1,1,3,3-tetramethylguanidinium fluorochromate (TMGFC and 1,1,3,3-tetramethylguanidinium chlorochromate (TMGCC were prepared in high yields by reacting tetramethylguanidine with CrO3 and related acid. These reagents are suitable to oxidize various primary and secondary alcohols and oximes to the corresponding carbonyl compounds under solvent-free conditions and microwave irradiation.

  7. An Efficient Synthesis of 3,4-Dihydropyrimidin-2(1H-Ones and Thiones Catalyzed by a Novel Brønsted Acidic Ionic Liquid under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Yonghong Zhang

    2015-02-01

    Full Text Available We report here an efficient and green method for Biginelli condensation reaction of aldehydes, β-ketoesters and urea or thiourea catalyzed by Brønsted acidic ionic liquid [Btto][p-TSA] under solvent-free conditions. Compared to the classical Biginelli reaction conditions, the present method has the advantages of giving good yields, short reaction times, near room temperature conditions and the avoidance of the use of organic solvents and metal catalyst.

  8. An efficient and high-yielding one-pot synthesis of 1H-pyrazolo[1,2-b]phthalazine-5,10-diones catalyzed by sodium hydrogen carbonate under solvent-free conditions

    OpenAIRE

    Asieh Vafaee; Abolghasem Davoodnia; Mehdi Pordel; Mohammad Reza Bozorgmehr

    2015-01-01

    Sodium hydrogen carbonate, NaHCO3, efficiently catalyzes the one-pot, three-component reaction of phthalhydrazide, an aromatic aldehyde, and malononitrile or ethyl cyanoacetate under solvent-free conditions, to afford the corresponding 1H-pyrazolo[1,2-b]phthalazine-5,10-diones in high yields. Easy work‐up, inexpensive and readily available catalyst and avoiding the use of harmful organic solvents are other advantages of this simple procedure.

  9. Hydrophobic lapatinib encapsulated dextran-chitosan nanoparticles using a toxic solvent free method: fabrication, release property & in vitro anti-cancer activity

    Energy Technology Data Exchange (ETDEWEB)

    Mobasseri, Rezvan [Department of Nanobiotechnology, Faculty of Biological Sciences, Tarbiat Modares University, Tehran (Iran, Islamic Republic of); Center for Nanofibers & Nanotechnology, Department of Mechanical Engineering, National University of Singapore, 117576 (Singapore); Karimi, Mahdi [Department of Nanobiotechnology, Faculty of Biological Sciences, Tarbiat Modares University, Tehran (Iran, Islamic Republic of); Tian, Lingling, E-mail: lingling_tian@nus.edu.sg [Center for Nanofibers & Nanotechnology, Department of Mechanical Engineering, National University of Singapore, 117576 (Singapore); Naderi-Manesh, Hossein, E-mail: naderman@modares.ac.ir [Department of Nanobiotechnology, Faculty of Biological Sciences, Tarbiat Modares University, Tehran (Iran, Islamic Republic of); Department of Biophysics, Faculty of Biological Sciences, Tarbiat Modares University, Tehran (Iran, Islamic Republic of); Ramakrishna, Seeram [Center for Nanofibers & Nanotechnology, Department of Mechanical Engineering, National University of Singapore, 117576 (Singapore); Guangdong-Hongkong-Macau Institute of CNS Regeneration (GHMICR), Jinan University, Guangzhou 510632 (China)

    2017-05-01

    Dextran sulfate-chitosan (DS-CS) nanoparticles, which possesses properties such as nontoxicity, biocompatibility and biodegradability have been employed as drug carriers in cancer therapy. In this study, DS-CS nanoparticles were synthesized and their sizes were controlled by a modification of the divalent cations cross-linkers (Ca{sup 2+}, Zn{sup 2+} or Mg{sup 2+}). Based on the optimized processing parameters, lapatinib encapsulated nanoparticles were developed and characterized by Dynamics Light Scattering (DLS) measurements, Fourier Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscopy (SEM). Calcium chloride (CaCl{sub 2}) facilitated the formation of bare (100.3 ± 0.80 nm) and drug-loaded nanoparticles (134.3 ± 1.3 nm) with narrow size distributions being the best cross-linker. The surface potential of drug-loaded nanoparticles was − 16.8 ± 0.47 mV and its entrapment and loading efficiency were 76.74 ± 1.73% and 47.36 ± 1.27%, respectively. Cellular internalization of nanoparticles was observed by fluorescence microscopy and MTT (3-(4, 5-dimethylthiazol-2-yl)-2, 5-diphenyltetrazolium bromide) assay was used to determine cytotoxicity of bare and drug-loaded nanoparticles in comparison to the free drug lapatinib. The MTT assay showed that drug-loaded nanoparticles had comparable anticancer activity to free drug within a duration of 48 h. The aforementioned results showed that the DS-CS nanoparticles were able to entrap, protect and release the hydrophobic drug, lapatinib in a controlled pattern and could further serve as a suitable drug carrier for cancer therapy. - Highlights: • The best condition to prepare best size (about 100 nm) dextran-chitosan nanoparticles is proposed. • Divalent cationic cross-linker can act as hardener and compress the particles. • Drug/dextran mixing in a toxic solvent free method provides hydrophobic drug encapsulation within a hydrophilic system. • High entrapment efficiency of Lapatinib in polymeric

  10. Using solvent-free sample preparation to promote protonation of poly(ethylene oxide)s with labile end-groups in matrix-assisted laser desorption/ionisation.

    Science.gov (United States)

    Mazarin, Michael; Phan, Trang N T; Charles, Laurence

    2008-12-01

    Protonation is usually required to observe intact ions during matrix-assisted laser desorption/ionization (MALDI) of polymers containing fragile end-groups while cation adduction induces chain-end degradation. These polymers, generally obtained via living free radical polymerization techniques, are terminated with a functionality in which a bond is prone to homolytic cleavage, as required by the polymerization process. A solvent-free sample preparation method was used here to avoid salt contaminant from the solvent traditionally used in the dried-droplet MALDI procedure. Solvent-based and solvent-free sample preparations were compared for a series of three poly(ethylene oxide) polymers functionalized with a labile end-group in a nitroxide-mediated polymerization reaction, using 2,4,6-trihydroxyacetophenone (THAP) as the matrix without any added salt. Intact oligomer ions could only be produced as protonated molecules in solvent-free MALDI while sodium adducts of degraded polymers were formed from the dried-droplet samples. Although MALDI analysis was performed at the laser threshold, fragmentation of protonated macromolecules was still observed to occur. However, in contrast to sodiated molecules, dissociation of protonated oligomers does not involve the labile C--ON bond of the end-group. As the macromolecule size increased, protonation appeared to be less efficient and sodium adduction became the dominant ionization process, although no sodium salt was added in the preparation. Formation of sodiated degraded macromolecules would be dictated by increasing cation affinity as the size of the oligomers increases and would reveal the presence of salts at trace levels in the MALDI samples.

  11. Synthesis, characterization and catalytic application of silica supported tin oxide nanoparticles for synthesis of 2,4,5-tri and 1,2,4,5-tetrasubstituted imidazoles under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Ashok V. Borhade

    2017-02-01

    Full Text Available Highly efficient and eco-friendly, one pot synthesis of 1,2,4,5-tetra substituted imidazoles and 2,4,5-trisubstituted imidazoles was reported under solvent free conditions using nanocrystalline silica supported tin oxide (SiO2:SnO2 as a catalyst with excellent yield. The present methodology offers several advantages such as mild reaction conditions, short reaction time, good yield, high purity of product, recyclable catalyst without a noticeable decrease in catalytic activity and can be used for large scale synthesis. The synthesized SiO2:SnO2 nanocrystalline catalyst was characterized by XRD, BET surface area and TEM techniques.

  12. Wet SiO2 As a Suitable Media for Fast and Efficient Reduction of Carbonyl Compounds with NaBH3CN under Solvent-Free and Acid-Free Conditions

    International Nuclear Information System (INIS)

    Kouhkan, Mehri; Zeynizadeh, Behzad

    2010-01-01

    Reduction of carbonyl compounds such as aldehydes, ketones, α,β-unsaturated enals and enones, α-diketones and acyloins was carried out readily with NaBH 3 CN in the presence of wet SiO 2 as a neutral media. The reactions were performed at solvent-free conditions in oil bath (70 - 80 .deg. C) or under microwave irradiation (240 W) to give the product alcohols in high to excellent yields. Regioselective 1,2-reduction of conjugated carbonyl compounds took place in a perfect selectivity without any side product formation

  13. Wet SiO{sub 2} As a Suitable Media for Fast and Efficient Reduction of Carbonyl Compounds with NaBH{sub 3}CN under Solvent-Free and Acid-Free Conditions

    Energy Technology Data Exchange (ETDEWEB)

    Kouhkan, Mehri; Zeynizadeh, Behzad [Urmia University, Urmia (Iran, Islamic Republic of)

    2010-10-15

    Reduction of carbonyl compounds such as aldehydes, ketones, α,β-unsaturated enals and enones, α-diketones and acyloins was carried out readily with NaBH{sub 3}CN in the presence of wet SiO{sub 2} as a neutral media. The reactions were performed at solvent-free conditions in oil bath (70 - 80 .deg. C) or under microwave irradiation (240 W) to give the product alcohols in high to excellent yields. Regioselective 1,2-reduction of conjugated carbonyl compounds took place in a perfect selectivity without any side product formation.

  14. Magnetic Nanoparticle Immobilized N-Propylsulfamic Acid as a Recyclable and Efficient Nanocatalyst for the Synthesis of 2H-indazolo[2,1-b]phthalazine-triones in Solvent-Free Conditions: Comparison with Sulfamic Acid

    Energy Technology Data Exchange (ETDEWEB)

    Rostami, Amin; Tahmasbi, Bahman; Yari, Ako [Univ. of Kurdistan, Sanandaj (Iran, Islamic Republic of)

    2013-05-15

    N-Propylsulfamic acid supported onto magnetic Fe{sub 3}O{sub 4} nanoparticles (MNPs-PSA) was used as an efficient and magnetically recoverable catalyst for synthesis of 2H-Indazolo[2,1-b]phthalazine-1,6,11(13H)-trione derivatives from the three-component, one-pot condensation reaction of phthalhydrazide, aromatic aldehydes and cyclic 1,3-diones, in good to excellent yields at 100 .deg. C under solvent-free conditions. The catalyst was easily separated with the assistance of an external magnetic field from the reaction mixture and reused for several consecutive runs without significant loss of its catalytic efficiency. In order to compare, the synthesis of 2H-Indazolo[2,1-b]phthalazine-1,6,11(13H)-trione derivatives in the presence of catalytic amount of sulfamic acid (SA) under same reaction condition was also reported.

  15. Ni2+ supported on hydroxyapatite-core@shell γ-Fe2O3 nanoparticles as new and green catalyst for the synthesis of 3,4-dihydropyrimidin-2(1H-ones under solvent-free condition

    Directory of Open Access Journals (Sweden)

    Eshagh Rezaee Nezhad

    2013-10-01

    Full Text Available The aim of this research is to study Ni2+ supported on hydroxyapatite-core-shell magnetic γ-Fe2O3 nanoparticles (γ-Fe2O3@HAp-Ni2+ as a green and recyclable catalyst for the Biginelli reaction under solvent-free conditions. One-pot multi-component condensation of 1,3-dicarbonyl compounds, urea and aldehydes at 80 oC affords the corresponding compounds in high yields and in short reaction times using γ-Fe2O3@HAp-Ni2+. The catalyst can be readily isolated using an external magnet and no obvious loss of activity was observed when the catalyst was reused in seven consecutive runs. The mean size and the surface morphology of the nanoparticles were characterized by transmission electron microscopy, scanning electron microscope, vibrating sample magnetometry, X-ray powder diffraction and Fourier transform infrared techniques.

  16. Molybdenum oxide supported on silica (MoO{sub 3}/SiO{sub 2}): an efficient and reusable catalyst for the synthesis of 1,8-dioxodecahydroacridines under solvent-free conditions

    Energy Technology Data Exchange (ETDEWEB)

    Khojastehnezhad, A.; Vafaei, M. [Islamic Azad University, Mashhad Branch, Department of Chemistry, Mashhad (Iran, Islamic Republic of); Moeinpour, F., E-mail: akhojastehnezhad@yahoo.com [Islamic Azad University, Bandar Abbas Branch, Department of Chemistry, Bandar Abbas (Iran, Islamic Republic of)

    2014-07-01

    Silica supported molybdenum oxide (MoO{sub 3}/SiO{sub 2}) was found to be and efficient, eco-friendly and heterogeneous catalyst for the multicomponent reaction of aromatic aldehydes, dimedone and ammonium acetate or aromatic amines under solvent-free conditions to afford the corresponding 1,8-dioxodecahydroacridines in high yields. The catalyst can be easily recovered and reused for several times without considerable loss of activity. Furthermore, the present method offers several advantages, such as an easy experimental and work-up procedures, short reaction times and good to excellent yields. For the characterization were used: Fourier transform infrared spectroscopy (Ft-IR), X-ray diffraction and scanning electron microscopy analyses. (Author)

  17. Molybdenum oxide supported on silica (MoO3/SiO2): an efficient and reusable catalyst for the synthesis of 1,8-dioxodecahydroacridines under solvent-free conditions

    International Nuclear Information System (INIS)

    Khojastehnezhad, A.; Vafaei, M.; Moeinpour, F.

    2014-01-01

    Silica supported molybdenum oxide (MoO 3 /SiO 2 ) was found to be and efficient, eco-friendly and heterogeneous catalyst for the multicomponent reaction of aromatic aldehydes, dimedone and ammonium acetate or aromatic amines under solvent-free conditions to afford the corresponding 1,8-dioxodecahydroacridines in high yields. The catalyst can be easily recovered and reused for several times without considerable loss of activity. Furthermore, the present method offers several advantages, such as an easy experimental and work-up procedures, short reaction times and good to excellent yields. For the characterization were used: Fourier transform infrared spectroscopy (Ft-IR), X-ray diffraction and scanning electron microscopy analyses. (Author)

  18. Nano crystalline ZnO catalyzed one pot three-component synthesis of 7-alkyl-6H,7H- naphtho[1',2':5,6]pyrano[3,2-c] chromen-6-ones under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    M. J. Piltan

    2016-08-01

    Full Text Available In the present paper, an efficient one-pot synthesis of 7-alkyl-6H,7H-naphtho[1',2':5,6]pyrano[3,2-c]chromen-6-ones is described by three-component reaction of β-naphthol, aromatic aldehydes and 4-hydroxycoumarin using ZnO nanoparticles under solvent-free conditions. The present method provides a novel and efficient procedure for the synthesis of chromene derivatives with some advantageous such as short reaction times, easy workup, high yields, wide range of products, reusability of the catalyst, little catalyst loading and green conditions in the presence of ZnO nanoparticles (7 mol% at 110 ºC.

  19. Green synthesis, characterization and catalytic activity of natural bentonite-supported copper nanoparticles for the solvent-free synthesis of 1-substituted 1H-1,2,3,4-tetrazoles and reduction of 4-nitrophenol

    Directory of Open Access Journals (Sweden)

    Akbar Rostami-Vartooni

    2015-12-01

    Full Text Available In this study, Cu nanoparticles were immobilized on the surface of natural bentonite using Thymus vulgaris extract as a reducing and stabilizing agent. The natural bentonite-supported copper nanoparticles (Cu NPs/bentonite were characterized by FTIR spectroscopy, X-ray diffraction (XRD, X-ray fluorescence (XRF, field emission scanning electron microscopy (FE-SEM, energy dispersive X-ray spectroscopy (EDS, transmission electron microscopy (TEM, selected area electron diffraction (SAED and Brunauer–Emmett–Teller (BET analysis. Afterward, the catalytic performance of the prepared catalyst was investigated for the solvent-free synthesis of 1-substituted 1H-1,2,3,4-tetrazoles and reduction of 4-nitrophenol (4-NP in water. It was found that the Cu NPs/bentonite is a highly active and recyclable catalyst for related reactions.

  20. Journal of Chemical Sciences | Indian Academy of Sciences

    Indian Academy of Sciences (India)

    Synthesis of 7-arylethyl-5-arylpyrazolo[1,5-a]pyrimidines through an aza-Michael addition/nucleophilic addition/1,3-hydrogen transfer cascade · ZHENG LI DEMENG XIE ... REGULAR ARTICLE. Resolution of the Identity and Cholesky Representation of EOM-MP2 Approximation: Implementation, Accuracy and Efficiency.

  1. Comment on "An unexpected formation of the novel 7-oxa-2-azabicyclo[2.2.1]hept-5-ene skeleton during the reaction of furfurylamine with maleimides and their bioprospection using a zebrafish embryo model" by C. E. Puerto Galvis and V. V. Kouznetsov, Org. Biomol. Chem., 2013, 11, 407.

    Science.gov (United States)

    Zubkov, F I; Kvyatkovskaya, E A; Nikitina, E V; Amoyaw, P N-A; Kouznetsov, V V; Lazarenko, V A; Khrustalev, V N

    2017-08-02

    It has been proved that the reaction between furfuryl amines and N-R-maleimides leads to the formation of aza-Michael addition products - 3-(furylmethylamino)-N-R-pyrrolidine-2,5-diones, instead of 7-oxa-2-azabicyclo[2.2.1]hept-5-enes, as this journal reported previously.

  2. Expedient Access to an N-phenylpyrrolidin-2-yl Heterocycle via a ...

    African Journals Online (AJOL)

    NICO

    Milder bases were employed catalytically for the 1,4-conjugate addition of ... using 2-bromoaniline given that it was available in our labora- tory and ... Scheme 3. Base-catalysed intramolecular aza-Michael reaction of indoles containing pendant-conjugated esters. Scheme 4. Synthesis of pyran-2-ol. Scheme 5. Synthesis of ...

  3. Solvent-free nanofluid with three structure models based on the composition of a MWCNT/SiO2 core and its adsorption capacity of CO2.

    Science.gov (United States)

    Yang, R L; Zheng, Y P; Wang, T Y; Li, P P; Wang, Y D; Yao, D D; Chen, L X

    2017-12-15

    A series of core/shell nanoparticle organic/inorganic hybrid materials (NOHMs) with different weight ratios of two components, consisting of multi-walled carbon nanotubes (MWCNTs) and silicon dioxide (SiO 2 ) as the core were synthesized. The NOHMs display a liquid-like state in the absence of solvent at room temperature. Five NOHMs were categorized into three kinds of structure states based on different weight ratio of two components in the core, named the power strip model, the critical model and the collapse model. The capture capacities of these NOHMs for CO 2 were investigated at 298 K and CO 2 pressures ranging from 0 to 5 MPa. Compared with NOHMs having a neat MWCNT core, it was revealed that NOHMs with the power strip model show better adsorption capacity toward CO 2 due to its lower viscosity and more reactive groups that can react with CO 2 . In addition, the capture capacities of NOHMs with the critical model were relatively worse than the neat MWCNT-based NOHM. The result is attributed to the aggregation of SiO 2 in these samples, which may cause the consumption and hindrance of reactive groups. However, the capture capacity of NOHMs with the collapse model was the worst of all the NOHMs, owing to its lowest content of reactive groups and hollow structure in MWCNTs. In addition, they presented non-interference of MWCNTs and SiO 2 without aggregation state.

  4. Solvent-free nanofluid with three structure models based on the composition of MWCNTs/SiO2 core and its adsorption capacity of CO2.

    Science.gov (United States)

    Yang, Ruilu; Zheng, Yaping; Wang, Tianyu; Li, Peipei; Wang, Yudeng; Yao, Dongdong; Chen, Lixin

    2017-11-26

    A series of core/shell nanoparticle organic/inorganic hybrid materials (NOHMs) with different weight ratios of two components, consisting of multi-walled carbon nanotubes (MWCNTs) and silicon dioxide (SiO2) as the core had been synthesized. The NOHMs displays a liquid-like state in the absence of solvent at room temperature. Five NOHMs were categorized into three kinds of structure states based on different weight ratio of two components in core, named power strip model, critical model and collapse model. The capture capacities of these NOHMs for CO2 were investigated at 298 K and CO2 pressures ranging from 0 to 5 MPa. Compared with NOHM having neat MWCNTs core, it had been revealed that NOHMs with power strip model show better adsorption capacity toward CO2, due to its lower viscosity and more reactive groups that can react with CO2. In addition, the capture capacities of NOHMs with critical model were relatively worse than neat MWCNTs-based NOHM. The result is attributed to the aggregation of SiO2 in these samples, which may cause the consumption and hindrance of reactive groups. However, the capture capacity of NOHM with collapse model was the worst in all NOHMs, owing to its lowest content of reactive groups and hollow structure in MWCNTs. Besides, it presented non-interference of MWCNTs and SiO2 without aggregation state. © 2017 IOP Publishing Ltd.

  5. SHORT COMMUNICATION A SOLVENT FREE AND SELECTIVE ...

    African Journals Online (AJOL)

    Preferred Customer

    Selective protection of 1,2-propanediol (1n) with dimethoxytrityl chloride and triethylamine under microwave irradiation. In a beaker, a mixture of dimethoxytrityl chloride (4.06 g, 12 mmol) and triethylamine (3.5 mL, 25 mmol) was taken and 1,2-propanediol 1n (0.76 g, 10 mmol) was added to this mixture and was irradiated ...

  6. Enantioselective solvent-free Robinson annulation reactions

    Indian Academy of Sciences (India)

    Unknown

    solvents to effect an asymmetric synthesis is an important step forward towards ... In continuation of our preliminary communication 2, we wish to ..... formation of chiral enamine 74 from the reaction of S-proline with pro-R carbonyl group.

  7. Dynamics of solvent-free grafted nanoparticles

    KAUST Repository

    Chremos, Alexandros; Panagiotopoulos, Athanassios Z.; Koch, Donald L.

    2012-01-01

    as well as grafted nanoparticles in a melt were compared to a reference system of bare (ungrafted) particles in a melt. Whereas longer chains lead to a larger hydrodynamic radius and lower relative diffusivity for grafted particles in a melt, bulk solvent

  8. SHORT COMMUNICATION A SOLVENT FREE AND SELECTIVE ...

    African Journals Online (AJOL)

    Preferred Customer

    1Department of Chemistry and Chemical Engineering, Faculty of Material ... A very simple and efficient method is described for protection of alcohols and ... Hydroxyl group protection is important in the synthesis of some organic molecules. ..... applied this method for the protection of hydroxyl groups in these compounds.

  9. Use of the co-grinding method to enhance the dissolution behavior of a poorly water-soluble drug: generation of solvent-free drug-polymer solid dispersions.

    Science.gov (United States)

    Yang, Caiqin; Xu, Xiujuan; Wang, Jing; An, Zhiqian

    2012-01-01

    The solid dispersion (SD) technique is the most effective method for improving the dissolution rate of poorly water-soluble drugs. In the present work, SDs of the Ca2+ channel blocker dipfluzine (DF) with polyvinylpyrrolidone K30 (PVP) and poloxamer 188 (PLXM) were prepared by the powder solid co-grinding method under a solvent-free condition. The properties of all SDs and physical mixtures were investigated by X-ray diffraction, Fourier-transform infrared, differential scanning calorimetry, scanning electron microscopy, dissolution test, and particles size determination. Eutectic compounds were produced between the DF and PLXM matrix during the co-grinding process, whereas glass suspension formed in the SDs with PVP carrier. Hydrogen bond formation was not observed between DF and carriers and DF was microcrystalline state in the PVP and PLXM matrices. The solubility of DF in different concentration of carriers at 25, 31, and 37°C was investigated; the values obtained were used to calculate the thermodynamic parameters of interaction between DF and carriers. The Gibbs free energy (ΔrGθ) values were negative, indicating the spontaneous nature of dispersing DF into the carriers. Moreover, entropy is the drive force when DF disperses into the matrix of PVP, while, enthalpy-driven dispersing encounters in the PLXM carrier. All the SDs of DF/carriers showed a considerably higher dissolution rate than pure DF and the corresponding physical mixtures. The cumulative dissolution rate at 10 min of the SD with a 1 : 3 DF/carrier ratio increased 5.1-fold for PVP and 5.5-fold for PLXM.

  10. Defect-rich Ni-Ti layered double hydroxide as a highly efficient support for Au nanoparticles in base-free and solvent-free selective oxidation of benzyl alcohol.

    Science.gov (United States)

    Liu, Mengran; Fan, Guoli; Yu, Jiaying; Yang, Lan; Li, Feng

    2018-04-17

    Tuning the surface properties of supported metal catalysts is of vital importance for governing their catalytic performances in nanocatalysis. Here, we report highly dispersed nanometric gold nanoparticles (NPs) supported on Ni-Ti layered double hydroxides (NiTi-LDHs), which were employed in solvent-free and base-free selective oxidation of benzyl alcohol. A series of characterization techniques demonstrated that defect-rich NiTi-LDHs could efficiently stabilize Au NPs and decrease surface electron density of Au NPs. The as-formed Au/NiTi-LDH catalyst with a Ni/Ti molar ratio of 3 : 1 and an Au loading of 0.71 wt% yielded the highest turnover frequency value of ∼4981 h-1 at 120 °C among tested Au/NiTi-LDH catalysts with different Ni/Ti molar ratios, along with a high benzaldehyde selectivity of 98%. High catalytic efficiency of the catalyst was mainly correlated with surface cooperation between unique defects (i.e. defective Ti3+ species and oxygen vacancies) and abundant hydroxyl groups on the brucite-like layers of the NiTi-LDH support, which could lead to the preferential adsorption and activation of an alcohol hydroxyl moiety in benzyl alcohol and oxygen molecule, as well as the formation of more electron-deficient Ni3+ and Au0 species on the catalyst surface. Furthermore, the present Au/NiTi-LDH catalyst tolerated the oxidation of a wide variety of substrate structures into the corresponding aldehydes, acids or ketones. Our primary results illustrate that defect-rich NiTi-LDHs are promising supports which can efficiently modify surface structure and electronic properties of supported metal catalysts and consequently improve their catalytic performances.

  11. Perlite-SO3H nanoparticles as an efficient and reusable catalyst for one-pot three-component synthesis of 1,2-dihydro-1-aryl-naphtho[1,2-e][1,3]oxazine-3-one derivatives under both microwave-assisted and thermal solvent-free conditions: Single crystal X-ray structure analysis and theoretical study

    Directory of Open Access Journals (Sweden)

    Ali Ramazani

    2016-01-01

    Full Text Available A general synthetic route for the synthesis of 1,2-dihydro-1-aryl-naphtho[1,2-e][1,3]oxazine-3-one derivatives has been developed using perlite-SO3H nanoparticles as efficient catalyst under both microwave-assisted and thermal solvent-free conditions. The combination of 2-naphthol, aldehyde and urea enabled the synthesis of 1,2-dihydro-1-aryl-naphtho[1,2-e][1,3]oxazine-3-one derivatives in the presence of perlite-SO3H nanoparticles in good to excellent yields. This method provides several advantages like simple work-up, environmentally benign, and shorter reaction times along with high yields. In order to explore the recyclability of the catalyst, the perlite-SO3H nanoparticles in solvent-free conditions were used as catalyst for the same reaction repeatedly and the change in their catalytic activity was studied. It was found that perlite-SO3H nanoparticles could be reused for four cycles with negligible loss of their activity. Single crystal X-ray structure analysis and theoretical studies also were investigated for 4i product. The electronic properties of the compound have been analyzed using DFT calculations (B3LYP/6-311+G*. The FMO analysis suggests that charge transfer takes place within the molecule and the HOMO is localized mainly on naphthalene and oxazinone rings whereas the LUMO resides on the naphthalene ring.

  12. Nano Fe{sub 2}O{sub 3,} clinoptilolite and H{sub 3}PW{sub 12}O{sub 40} as efficient catalysts for solvent-free synthesis of 5(4H)-isoxazolone under microwave irradiation conditions

    Energy Technology Data Exchange (ETDEWEB)

    Fozooni, Samieh, E-mail: samieh.fozooni@uk.ac.ir, E-mail: s_fozooni@yahoo.com [Shahid Bahonar University, Kerman (Iran, Islamic Republic of). Mining Engineering Department. Zarand High Education Center; Hosseinzadeh, Nasrin Gholam; Akhgar, Mohammad Reza [Islamic Azad University, Kerman (Iran, Islamic Republic of). Department of Chemistry; Hamidian, Hooshang [Payame Noor University (PNU), Tehran (Iran, Islamic Republic of). Department of Chemistry

    2013-10-15

    A quick and solvent-free approach involving the exposure of neat reactants to microwave irradiation in conjunction with the use of clinoptilolite, H{sub 3}PW{sub 12}O{sub 40} and Fe{sub 2}O{sub 3} nanoparticle catalysts is described. In this work, condensation of hydroxylamine hydrochloride, sodium acetate, acetoacetic or benzoyl acetic ethyl ester and appropriate aldehydes by employing catalysts gave 5(4H)-isoxazolone only in one step. Catalyst amount, temperature effects and catalysts reusability were monitored. Among the catalysts, Fe{sub 2}O{sub 3} nanoparticles had better performance than other catalysts from viewpoint of yield and reaction time. The present protocol offers several advantages, such as short reaction time, reasonable yield, mild reaction condition and recycling catalysts with a very easy workup. (author)

  13. Expedient Access to an N -phenylpyrrolidin-2-yl Heterocycle via a ...

    African Journals Online (AJOL)

    Expedient Access to an N -phenylpyrrolidin-2-yl Heterocycle via a Base-Induced Intramolecular aza -Michael Reaction. ... in good overall yield when employing a stoichiometric amount of base to facilitate the intramolecular aza-Michael reaction. Keywords: aza Michael, intramolecular, catalysed, piperidine, pyrrolidine, base ...

  14. Ultrasensitive, simple and solvent-free micro-assay for determining sulphite preservatives (E220-228) in foods by HS-SDME and UV-vis micro-spectrophotometry.

    Science.gov (United States)

    Gómez-Otero, E; Costas, M; Lavilla, I; Bendicho, C

    2014-03-01

    A new method based on headspace single-drop microextraction in combination with UV-vis micro-spectrophotometry has been developed for the ultrasensitive determination of banned sulphite preservatives (E220-228) in fruits and vegetables. Sample acidification was used for SO2 generation, which is collected onto a 5,5'-dithiobis-(2-nitrobenzoic acid) microdrop for spectrophotometric measurement. A careful study of this reaction was necessary, including conditions for SO2 generation from different sulphating salts, drop pH, 5,5'-dithiobis-(2-nitrobenzoic acid) concentration and potential interference effects. Variables influencing mass transfer (stirring, sample volume and addition of salt) and microextraction time were also studied. A simple sulphite extraction was carried out, and problems caused by oxidation during the extraction process were addressed. A high enrichment factor (380) allows the determination of low levels of free SO2 in fruits and vegetables (limit of detection 0.06 μg g(-1), limit of quantification 0.2 μg g(-1)) with an adequate precision (repeatability, relative standard deviation 5 %). In addition, the sulphiting process was studied through the monitoring of residual SO2 in a vegetal sample, thus showing the importance of a sensitive tool for SO2 detection at low levels.

  15. H-ferrierite zeolite: As an effective and reusable heterogeneous catalyst for synthesis of 1,5-benzothiazepine under solvent free condition and 1,3-dipolar cycloaddition in water

    Directory of Open Access Journals (Sweden)

    Thoraya A. Farghaly

    2017-05-01

    Full Text Available An efficient synthesis of new derivatives of 1,5-benzothiazepine has been developed by the reaction of various chalcones (1,3-diaryl-2-propenones with 2-amino-thiophenol in the presence of H-ferrierite zeolite as acidic catalyst without solvent. In addition, 1,3-dipolar cycloaddition of hydrazonoyl chlorides on CN bond of 1,5-benzothiazepines in water in the presence of Na2CO3/THAC as a base catalyst afforded 1,2,4-triazolo[3,4-d][1,5]benzothiazepines. The structure of all the newly synthesized compounds was established on the basis of spectral data (Mass, IR, 1H NMR, 13C NMR and elemental analysis.

  16. Ultrasound-assisted phase-transfer catalysis method in an aqueous medium to promote the Knoevenagel reaction: advantages over the conventional and microwave-assisted solvent-free/catalyst-free method.

    Science.gov (United States)

    De-la-Torre, Pedro; Osorio, Edison; Alzate-Morales, Jans H; Caballero, Julio; Trilleras, Jorge; Astudillo-Saavedra, Luis; Brito, Iván; Cárdenas, Alejandro; Quiroga, Jairo; Gutiérrez, Margarita

    2014-09-01

    Given the broad spectrum of uses of acrylonitrile derivatives as fluorescent probes, AChE inhibitors, and others, it is necessary to find easy, efficient and simple methods to synthesize and diversify these compounds. We report the results of a comparative study of the effects of three techniques on the reactions between heterocyclic aldehydes and 2-(benzo[d]thiazol-2-yl)acetonitrile: stirring; ultrasound coupled to PTC conditions (US-PTC); and MW irradiation (MWI) under solvent and catalyst-free conditions. The effects of conditions on reaction parameters were evaluated and compared in terms of reaction time, yield, purity and outcomes. The US-PTC method is more efficient than the MWI and conventional methods. The reaction times were considerably shorter, with high yields (>90%) and good levels of purity. In addition, X-ray diffraction analysis and quantum mechanical calculations, at the level of density functional theory (DFT), ratify obtaining acrylonitrile isomers with E configurations. The crystal structure of 3c is stabilized by weak C-Ho⋯N intermolecular interactions (Ho⋯NC=2.45 Å, Co⋯NC=3.348(3) Å, Ho⋯NC=162°), forming centrosymmetric ring R2(2) (20) along the crystallographic a axis. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Solvent-free one-pot cyclization and acetylation of chalcones: Synthesis of some 1-acetyl pyrazoles and spectral correlations of 1-(3-(3,4-dimethylphenyl-5-(substituted phenyl-4,5-dihydro-1H-pyrazole-1-yl ethanones

    Directory of Open Access Journals (Sweden)

    G. Thirunarayanan

    2016-11-01

    Full Text Available One-pot synthesis of some 1N-acetyl pyrazoles including 1-(3-(3,4-dimethylphenyl-5-(substituted phenyl-4,5-dihydro-1H-pyrazole-1-yl ethanones has been achieved via solvent-free microwave irradiation using substituted chalcones, hydrazine hydrate and acetic anhydride in the presence of catalytic amount of fly-ash: PTS catalyst. The yield of these 1N-acetyl pyrazole derivatives is more than 75%. The synthesized 1N-acetyl pyrazoline derivatives were characterized by their physical constants and spectral data. The infrared spectral νCN and CO (cm−1 frequencies, NMR chemical shifts (δ, ppm of Ha, Hb, Hc, CH3 protons, CN, CO and CH3 carbons of 1-(3-(3,4-dimethylphenyl-5-(substituted phenyl-4,5-dihydro-1H-pyrazole-1-yl ethanones have been assigned and correlated with Hammett substituent constants and Swain-Lupton’s parameters using single and multi-regression analysis. From the results of statistical analyses, the effect of substituents on the above group frequencies and chemical shifts of the acetylated pyrazoles were discussed.

  18. Structure of Solvent-Free Nanoparticle−Organic Hybrid Materials

    KAUST Repository

    Yu, Hsiu-Yu; Koch, Donald L.

    2010-01-01

    that the constraint that each particle carries its own share of the fluid attached to itself yields a static structure factor that approaches zero as the wavenumber approaches zero. This result indicates that each particle excludes exactly one other particle from its

  19. dichlorodiazene dioxides using levulinic acid under solvent-free

    Indian Academy of Sciences (India)

    Administrator

    43 599; (b) Tchou- bar B and Sackur O ... Bremeyer N, Smith S C, Ley S V and Gaunt M J. 2004 Angew. ... Bellesia F, Ghelfi F, Pagnoni U M and Pinetti A 1990. J. Chem. Res. ... Kronenthal D, Huang M H and Nugent W A 2004 J. Org. Chem.

  20. Highly Efficient Method for Solvent-Free Synthesis of Diarylmethane ...

    African Journals Online (AJOL)

    NICO

    2011-02-25

    Feb 25, 2011 ... aFaculty of Chemistry, Bu-Ali Sina University, P.O. Box 651783868, Hamedan, Iran. ... Arylmethanes are useful compounds in organic synthesis and industry1 ... ketones,9,10 catalytic condensation of the Grignard reagent with.

  1. Solvent-free microwave-assisted synthesis of oxadiazoles ...

    Indian Academy of Sciences (India)

    TECS

    tion mixture was refluxed for 4–5 h on an oil bath, the contents were cooled to room temperature and poured onto crushed ice. It was then neutralized by. 5% sodium bicarbonate solution. The solid that separated was collected by filtration through a. Büchner funnel and dried. Further purification was done by recrystallization ...

  2. Synthesis of Halide- and Solvent free metal borohydrides

    DEFF Research Database (Denmark)

    Grinderslev, Jakob; Møller, Kasper Trans; Jensen, Torben René

    chloride or LiBH4 is present in the sample. The synthesis pathway has been shown to work for most of the already known metal borohydrides, M = Na, Ca, Sr, Ba, Y, La, Eu, Gd, Tb, Dy, Ho, Er, Tm, and Yb, but also new borohydrides are formed, M = Pr, Nd and Lu. Besides new compounds, new polymorphs...

  3. INVESTIGATION OF THE SOLVENT FREE ISOMERISATION OF cis ...

    African Journals Online (AJOL)

    Preferred Customer

    The rate of the solid state isomerisation of cis-Mo(CO)4(PPh3)2 was .... R = reflectance, k = absorption coefficient, s = scattering coefficient, c = concentration of the .... total loss of 75 % mass, which is assumed to be due to loss of the two PPh3 ...

  4. Novel, Solvent-Free, Single Ion Conductive Polymer Electrolytes

    Science.gov (United States)

    2008-01-20

    liquid oligomeric analogue PEODME (ε = 8, dioxane:CH3CN mass ratio 48:7). The choice of the solvent mixture was a compromise between the...trifluoride – a derivative of Lewis acid properties. An increase in the degree of dissociation, decrease in the share of ionic associates and increase in...diphenylphosphinate this product is a solid, and in reaction with lithium diphenylphosphate the second fraction is a viscous, light-brown liquid , and

  5. Structure of Solvent-Free Nanoparticle−Organic Hybrid Materials

    KAUST Repository

    Yu, Hsiu-Yu

    2010-11-16

    We derive the radial distribution function and the static structure factor for the particles in model nanoparticleorganic hybrid materials composed of nanoparticles and attached oligomeric chains in the absence of an intervening solvent. The assumption that the oligomers form an incompressible fluid of bead-chains attached to the particles that is at equilibrium for a given particle configuration allows us to apply a density functional theory for determining the equilibrium configuration of oligomers as well as the distribution function of the particles. A quasi-analytic solution is facilitated by a regular perturbation analysis valid when the oligomer radius of gyration R g is much greater than the particle radius a. The results show that the constraint that each particle carries its own share of the fluid attached to itself yields a static structure factor that approaches zero as the wavenumber approaches zero. This result indicates that each particle excludes exactly one other particle from its neighborhood. © 2010 American Chemical Society.

  6. Complex phase behavior in solvent-free nonionic surfactants

    DEFF Research Database (Denmark)

    Hillmyer, M.A.; Bates, F.S.; Almdal, K.

    1996-01-01

    Unsolvated block copolymers and surfactant solutions are ''soft materials'' that share a common set of ordered microstructures, A set of polyethyleneoxide-polyethylethylene (PEG-PEE) block copolymers that are chemically similar to the well-known alkane-oxyethylene (C(n)EO(m)) nonionic surfactants...... was synthesized here. The general phase behavior in these materials resembles that of both higher molecular weight block copolymers and lower molecular weight nonionic surfactant solutions. Two of the block copolymers exhibited thermally induced order-order transitions and were studied in detail by small...

  7. Organic Synthesis under Solvent-free Condition. An Environmentally ...

    Indian Academy of Sciences (India)

    Though it is a common practice to run the organic reactions in solvent media, the ... this concept is simple. That is, the ... to vigorous research activity and reinvestigation of known reac- tions to achieve ... experimental procedure, work up technique and saving in labour. These would be ... This is true not only of the crystals of ...

  8. A Solvent-free Synthesis of Polyhydroquinolines via Hantzsch ...

    African Journals Online (AJOL)

    NICO

    ABSTRACT. A simple and efficient procedure for the synthesis of polyhydroquinolines was developed, involving a one-pot four-component ... inhibition and most importantly as calcium channel blockers.8–15 ..... to magnetic nanoparticles.

  9. Novel, Solvent-Free, Single Ion Conductive Polymer Electrolytes

    National Research Council Canada - National Science Library

    Florjanczyk, Zbigniew

    2008-01-01

    This project report concerns studies on the synthesis of new polymer electrolytes for application in lithium and lithium-ion batteries characterized by limited participation of anions in the transport...

  10. SOLVENT FREE OXIDATION OF ALCOHOLS USING IRON (III) NITRATE NONAHYDRATE

    Science.gov (United States)

    Oxidation of alcohols have been conducted with metal nitrate reagents on various mineral supports such as clay, silica and zeolite etc. To circumvent the limitations of these supported reagents namely their preparation using solvents and short shelf-life, we explored the use of i...

  11. Highly efficient solvent-free synthesis of pyranopyrazoles by a ...

    Indian Academy of Sciences (India)

    bDepartment of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, P.O. Box 91775, ... key advantages of this process are high yields, shorter reaction times, easy work-up, ... ing pyran derivatives and hydrazine hydrate,9 use of.

  12. Solvent free lipase catalyzed synthesis of butyl caprylate

    Indian Academy of Sciences (India)

    MEERA T SOSE

    2017-11-10

    Nov 10, 2017 ... Department of Chemical Engineering, Institute of Chemical Technology, Matunga (E), ... study for the synthesis of butyl caprylate in presence of bio-catalyst. ..... −1 with Thermomyces lanuginosus lipase.26 The relation.

  13. solvent-free synthesis of azomethines, spectral correlations

    African Journals Online (AJOL)

    B. S. Chandravanshi

    attention of organic and medicinal chemists [2, 3]. ... Spectroscopic data is very useful for studying the ground state equilibrium of ... determines the structure of unsaturated systems, such as E- or Z, s-cis and .... The IR and NMR spectra of selective ... The proposed mechanism for the synthesis of E- imines in presence of ...

  14. Additive manufacturing.

    Science.gov (United States)

    Mumith, A; Thomas, M; Shah, Z; Coathup, M; Blunn, G

    2018-04-01

    Increasing innovation in rapid prototyping (RP) and additive manufacturing (AM), also known as 3D printing, is bringing about major changes in translational surgical research. This review describes the current position in the use of additive manufacturing in orthopaedic surgery. Cite this article: Bone Joint J 2018;100-B:455-60.

  15. Food additives

    Science.gov (United States)

    ... GO About MedlinePlus Site Map FAQs Customer Support Health Topics Drugs & Supplements Videos & Tools Español You Are Here: Home → Medical Encyclopedia → Food additives URL of this page: //medlineplus.gov/ency/article/ ...

  16. Cobalt/N-Hydroxyphthalimide(NHPI)-Catalyzed Aerobic Oxidation of Hydrocarbons with Ionic Liquid Additive

    DEFF Research Database (Denmark)

    Mahmood, Sajid; Xu, Bao Hua; Ren, Tian Lu

    2018-01-01

    A highly efficient and solvent-free system of cobalt/NHPI-catalyzed aerobic oxidation of hydrocarbons was developed using imidazolium-based ionic liquid (IL) as an additive. These amphipathic ILs were found self-assemble at the interface between the organic hydrocarbons and the aqueous phase...... the optimum reactivity. Besides, the interfacial boundary between aqueous and organic phase composed by C2-alkylated imidazolium ILs, such as [bdmim]SbF6 and [C12dmim]SbF6, not only has ternary aggregates (hydrocarbons/IL/H2O) of higher stability but renders O2 a faster diffusion rate and higher concentration......, thereby offering a high reactivity of the protocol towards hydrocarbon oxidation....

  17. Synthesis by extrusion: continuous, large-scale preparation of MOFs using little or no solvent† †Electronic supplementary information (ESI) available. See DOI: 10.1039/c4sc03217a Click here for additional data file.

    Science.gov (United States)

    Crawford, Deborah; Casaban, José; Haydon, Robert; Giri, Nicola; McNally, Tony

    2015-01-01

    Grinding solid reagents under solvent-free or low-solvent conditions (mechanochemistry) is emerging as a general synthetic technique which is an alternative to conventional solvent-intensive methods. However, it is essential to find ways to scale-up this type of synthesis if its promise of cleaner manufacturing is to be realised. Here, we demonstrate the use of twin screw and single screw extruders for the continuous synthesis of various metal complexes, including Ni(salen), Ni(NCS)2(PPh3)2 as well as the commercially important metal organic frameworks (MOFs) Cu3(BTC)2 (HKUST-1), Zn(2-methylimidazolate)2 (ZIF-8, MAF-4) and Al(fumarate)(OH). Notably, Al(fumarate)(OH) has not previously been synthesised mechanochemically. Quantitative conversions occur to give products at kg h–1 rates which, after activation, exhibit surface areas and pore volumes equivalent to those of materials produced by conventional solvent-based methods. Some reactions can be performed either under completely solvent-free conditions whereas others require the addition of small amounts of solvent (typically 3–4 mol equivalents). Continuous neat melt phase synthesis is also successfully demonstrated by both twin screw and single screw extrusion for ZIF-8. The latter technique provided ZIF-8 at 4 kg h–1. The space time yields (STYs) for these methods of up to 144 × 103 kg per m3 per day are orders of magnitude greater than STYs for other methods of making MOFs. Extrusion methods clearly enable scaling of mechanochemical and melt phase synthesis under solvent-free or low-solvent conditions, and may also be applied in synthesis more generally. PMID:29308131

  18. Effect of Addition of Fennel (Foeniculum vulgare L. on the Quality of Protein Bread

    Directory of Open Access Journals (Sweden)

    Sayed-Ahmad Bouchra

    2017-12-01

    Full Text Available Fennel (Foeniculum vulgare L. is an aromatic plant belonging to Apiaceae family widely cultivated elsewhere for its strongly flavoured leaves and seeds. Fennel seeds are of particular interest as a rich source of both vegetable and essential oils with high amounts of valuable components. However, residual cakes after oil extraction were typically considered as byproducts, in the present framework, the potential added value of these cakes was studied. The aim of this study was to investigate the effect of addition of fennel cake and seeds to protein bread quality. In the current research, a single-screw extruder, which is a solvent-free technique, was used for fennel seed oil extraction. For the protein bread making, fennel seed and cake flour in concentrations from 1 to 6% were used. Moisture, colour L*a*b*, hardness, total phenolic concentration, DPPH radical scavenging activity, and nutritional value of protein bread were determined. The addition of fennel cake and seeds had significant (p < 0.05 effect on bread crumb colour and hardness attribute, whereby the bread became darker and harder in texture than the control. Moreover, higher antioxidant activity and total phenolic concentration were observed for both protein breads enriched with fennel cake and seed flour. The overall results showed that addition of fennel cake and seed had beneficial effects on phenolic concentration, antioxidant activity and quality of protein bread. This result suggests also that added value of fennel seeds oil by-products could be increased by their utilisation in bread production.

  19. Additive Manufacturing Infrared Inspection

    Science.gov (United States)

    Gaddy, Darrell; Nettles, Mindy

    2015-01-01

    The Additive Manufacturing Infrared Inspection Task started the development of a real-time dimensional inspection technique and digital quality record for the additive manufacturing process using infrared camera imaging and processing techniques. This project will benefit additive manufacturing by providing real-time inspection of internal geometry that is not currently possible and reduce the time and cost of additive manufactured parts with automated real-time dimensional inspections which deletes post-production inspections.

  20. [Food additives and healthiness].

    Science.gov (United States)

    Heinonen, Marina

    2014-01-01

    Additives are used for improving food structure or preventing its spoilage, for example. Many substances used as additives are also naturally present in food. The safety of additives is evaluated according to commonly agreed principles. If high concentrations of an additive cause adverse health effects for humans, a limit of acceptable daily intake (ADI) is set for it. An additive is a risk only when ADI is exceeded. The healthiness of food is measured on the basis of nutrient density and scientifically proven effects.

  1. Additives in yoghurt production

    Directory of Open Access Journals (Sweden)

    Milna Tudor

    2008-02-01

    Full Text Available In yoghurt production, mainly because of sensory characteristics, different types of additives are used. Each group, and also each substance from the same group has different characteristics and properties. For that reason, for improvement of yoghurt sensory characteristics apart from addition selection, the quantity of the additive is very important. The same substance added in optimal amount improves yoghurt sensory attributes, but too small or too big addition can reduce yoghurt sensory attributes. In this paper, characteristics and properties of mostly used additives in yoghurt production are described; skimmed milk powder, whey powder, concentrated whey powder, sugars and artificial sweeteners, fruits, stabilizers, casein powder, inulin and vitamins. Also the impact of each additive on sensory and physical properties of yoghurt, syneresis and viscosity, are described, depending on used amount added in yoghurt production.

  2. Polylactides in additive biomanufacturing.

    Science.gov (United States)

    Poh, Patrina S P; Chhaya, Mohit P; Wunner, Felix M; De-Juan-Pardo, Elena M; Schilling, Arndt F; Schantz, Jan-Thorsten; van Griensven, Martijn; Hutmacher, Dietmar W

    2016-12-15

    New advanced manufacturing technologies under the alias of additive biomanufacturing allow the design and fabrication of a range of products from pre-operative models, cutting guides and medical devices to scaffolds. The process of printing in 3 dimensions of cells, extracellular matrix (ECM) and biomaterials (bioinks, powders, etc.) to generate in vitro and/or in vivo tissue analogue structures has been termed bioprinting. To further advance in additive biomanufacturing, there are many aspects that we can learn from the wider additive manufacturing (AM) industry, which have progressed tremendously since its introduction into the manufacturing sector. First, this review gives an overview of additive manufacturing and both industry and academia efforts in addressing specific challenges in the AM technologies to drive toward AM-enabled industrial revolution. After which, considerations of poly(lactides) as a biomaterial in additive biomanufacturing are discussed. Challenges in wider additive biomanufacturing field are discussed in terms of (a) biomaterials; (b) computer-aided design, engineering and manufacturing; (c) AM and additive biomanufacturing printers hardware; and (d) system integration. Finally, the outlook for additive biomanufacturing was discussed. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Additive and polynomial representations

    CERN Document Server

    Krantz, David H; Suppes, Patrick

    1971-01-01

    Additive and Polynomial Representations deals with major representation theorems in which the qualitative structure is reflected as some polynomial function of one or more numerical functions defined on the basic entities. Examples are additive expressions of a single measure (such as the probability of disjoint events being the sum of their probabilities), and additive expressions of two measures (such as the logarithm of momentum being the sum of log mass and log velocity terms). The book describes the three basic procedures of fundamental measurement as the mathematical pivot, as the utiliz

  4. Food Additives and Hyperkinesis

    Science.gov (United States)

    Wender, Ester H.

    1977-01-01

    The hypothesis that food additives are causally associated with hyperkinesis and learning disabilities in children is reviewed, and available data are summarized. Available from: American Medical Association 535 North Dearborn Street Chicago, Illinois 60610. (JG)

  5. Groups – Additive Notation

    Directory of Open Access Journals (Sweden)

    Coghetto Roland

    2015-06-01

    Full Text Available We translate the articles covering group theory already available in the Mizar Mathematical Library from multiplicative into additive notation. We adapt the works of Wojciech A. Trybulec [41, 42, 43] and Artur Korniłowicz [25].

  6. Groups – Additive Notation

    OpenAIRE

    Coghetto Roland

    2015-01-01

    We translate the articles covering group theory already available in the Mizar Mathematical Library from multiplicative into additive notation. We adapt the works of Wojciech A. Trybulec [41, 42, 43] and Artur Korniłowicz [25].

  7. Highly efficient cobalt-doped carbon nitride polymers for solvent-free selective oxidation of cyclohexane

    Directory of Open Access Journals (Sweden)

    Yu Fu

    2017-04-01

    Full Text Available Selective oxidation of saturated hydrocarbons with molecular oxygen has been of great interest in catalysis, and the development of highly efficient catalysts for this process is a crucial challenge. A new kind of heterogeneous catalyst, cobalt-doped carbon nitride polymer (g-C3N4, was harnessed for the selective oxidation of cyclohexane. X-ray diffraction, Fourier transform infrared spectra and high resolution transmission electron microscope revealed that Co species were highly dispersed in g-C3N4 matrix and the characteristic structure of polymeric g-C3N4 can be retained after Co-doping, although Co-doping caused the incomplete polymerization to some extent. Ultraviolet–visible, Raman and X-ray photoelectron spectroscopy further proved the successful Co doping in g-C3N4 matrix as the form of Co(IIN bonds. For the selective oxidation of cyclohexane, Co-doping can markedly promote the catalytic performance of g-C3N4 catalyst due to the synergistic effect of Co species and g-C3N4 hybrid. Furthermore, the content of Co largely affected the activity of Co-doped g-C3N4 catalysts, among which the catalyst with 9.0 wt% Co content exhibited the highest yield (9.0% of cyclohexanone and cyclohexanol, as well as a high stability. Meanwhile, the reaction mechanism over Co-doped g-C3N4 catalysts was elaborated. Keywords: Selective oxidation of cyclohexane, Oxygen oxidant, Carbon nitride, Co-doping

  8. 21 CFR 182.20 - Essential oils, oleoresins (solvent-free), and natural extractives (including distillates).

    Science.gov (United States)

    2010-04-01

    ... (clary sage) Salvia sclarea L. Clover Trifolium spp. Coca (decocainized) Erythroxylum coca Lam. and other spp. of Erythroxylum. Coffee Coffea spp. Cola nut Cola acuminata Schott and Endl., and other spp. of Cola. Coriander Coriandrum sativum L. Cumin (cummin) Cuminum cyminum L. Curacao orange peel (orange...

  9. 21 CFR 582.20 - Essential oils, oleoresins (solvent-free), and natural extractives (including distillates).

    Science.gov (United States)

    2010-04-01

    .... Clover Trifolium spp. Coca (decocainized) Erythroxylum coca Lam. and other spp. of Erythroxylum. Coffee Coffea spp. Cola nut Cola acuminata Schott and Endl., and other spp. of Cola. Coriander Coriandrum... Cola acuminata Schott and Endl., and other spp. of Cola. Laurel berries Laurus nobilis L. Laurel leaves...

  10. Enzymatic preparation of "functional oil" rich in feruloylated structured lipids with solvent-free ultrasound pretreatment.

    Science.gov (United States)

    Zhang, Haiping; Zheng, Mingming; Shi, Jie; Tang, Hu; Deng, Qianchun; Huang, Fenghong; Luo, Dan

    2018-05-15

    In this study, a series of functional oils rich in feruloylated structured lipids (FSLs) was prepared by enzymatic transesterification of ethyl ferulate (EF) with triglycerides under ultrasound pretreatment. A conversion of more than 92.7% and controllable FSLs (3.1%-26.3%) can be obtained under the following conditions: 16% enzyme, substrate ratio 1:5 (oil/EF, mol/mol), 85 °C, ultrasound 1 h, pulse mode 3 s/3s (working/waiting), and 17.0 W/mL. Compared to conventional mechanical stirring, the activation energy decreased from 50.0 kJ/mol to 40.7 kJ/mol. The apparent kinetic constant increased by more than 13 times, and the time required for the maximum conversion reduced sharply from 20-60 h to 4-6h, which was the fastest rate for enzymatic synthesis of FSLs. The antioxidant activities of the functional oil significantly increased 1.0- to 8.1-fold more than that of the raw oil. The functional oil could be widely applied in various fields of functional foods. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Solvent-free formation of hydroxyapatite coated biodegradable particles via nanoparticle-stabilized emulsion route

    International Nuclear Information System (INIS)

    Okada, Masahiro; Fujii, Syuji; Nishimura, Taiki; Nakamura, Yoshinobu; Takeda, Shoji; Furuzono, Tsutomu

    2012-01-01

    Highlights: ► Hydroxyapatite (HAp) nanoparticles stabilized polymer melt-in-water emulsions without any molecular surfactants. ► Interaction between polymer and HAp played a crucial role. ► HAp-coated polymer particles were obtained from the emulsions without any organic solvents. - Abstract: Hydroxyapatite (HAp) nanoparticle-coated biodegradable polymer particles were fabricated from a nanoparticle-stabilized emulsion in the absence of any molecular surfactants or organic solvents. First, a polymer melt-in-water emulsion was prepared by mixing a water phase containing nanosized HAp particles as a particulate emulsifier and an oil phase consisting of poly(ε-caprolactone) (PCL) or poly(L-lactide-co-ε-caprolactone) (P(LLA-CL)) above its melting point. It was clarified that the interaction between ester/carboxyl groups of the polymers and the HAp nanoparticles at the polymer–water interface played a crucial role to prepare the nanoparticle-stabilized emulsion. The HAp nanoparticle-coated biodegradable polymer particle (a polymer solid-in-water emulsion) was fabricated by cooling the emulsion. The particle morphology and particle size were evaluated using scanning electron microscope.

  12. Rapid, efficient and solvent free microwave mediated synthesis of aldo- and ketonitrones

    Directory of Open Access Journals (Sweden)

    Loredana Maiuolo

    2016-01-01

    Full Text Available A library of C-alkyl and C-aryl nitrones has been obtained by direct condensation of primary N-substituted hydroxylamine hydrochlorides with various aldehydes and ketones without catalysts or base. The synthetic procedure, performed under MW irradiation in the absence of solvent, does not require the presence of a base, is fast, clean, high-yielding and characterized by simple work-up.

  13. Microwave Assisted Solvent Free Synthesis of Azomethines from Aryl Aldehydes on Melamin Formaldehyde as Solid Support

    Directory of Open Access Journals (Sweden)

    Ramin Rezaei

    2011-01-01

    Full Text Available Various aryl aldehydes underwent prompt one pot conversion into the corresponding azomethines in high yields by reacting with hydroxylamine hydrochloride supported on melamine formaldehyde under microwave irradiation.

  14. Vacuum-and-solvent-free fabrication of organic semiconductor layers for field-effect transistors

    Science.gov (United States)

    Matsushima, Toshinori; Sandanayaka, Atula S. D.; Esaki, Yu; Adachi, Chihaya

    2015-09-01

    We demonstrate that cold and hot isostatic pressing (CIP and HIP) is a novel, alternative method for organic semiconductor layer fabrication, where organic powder is compressed into a layer shape directly on a substrate with 200 MPa pressure. Spatial gaps between powder particles and the other particles, substrates, or electrodes are crushed after CIP and HIP, making it possible to operate organic field-effect transistors (OFETs) containing the compressed powder as the semiconductor. The CIP-compressed powder of 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C8-BTBT) had a hole mobility of (1.6 ± 0.4) × 10-2 cm2/Vs. HIP of C8-BTBT powder increased the hole mobility to an amorphous silicon-like value (0.22 ± 0.07 cm2/Vs) because of the growth of the C8-BTBT crystallites and the improved continuity between the powder particles. The vacuum and solution processes are not involved in our CIP and HIP techniques, offering a possibility of manufacturing OFETs at low cost.

  15. The development of a solvent-free approach for the determination of petroleum hydrocarbons in water

    International Nuclear Information System (INIS)

    Ehntholt, D.J.; Bodek, I.; Miseo, E.V.

    1995-01-01

    Current analytical methods for analysis of total petroleum hydrocarbons or oil and grease in water use extraction of 1.5 liters of the aqueous sample with three aliquots of Freon 113, drying with silica gel and subsequent analysis by infrared spectroscopy at 2,930 cm -1 . The use of chlorofluorocarbons is unacceptable based on environmental concerns regarding the degradation of the ozone layer by photochemical reactions of halocarbons. Due to these environmental concerns, various international agreements have resulted in a plan to eliminate CFCs by the year 2000. A new approach relies on a solid/liquid extraction with thermal desorption of the analytes into a gas stream. The gas stream is analyzed by infrared spectroscopy and the analytes quantified. The steps in the analysis are presented. A known volume of aqueous sample (typically between 10 and 50 ml) is passed through a selectively absorbent resin such as XAD-16. The analytes are absorbed onto the resin, while the water passes through. The analytes are thermally desorbed using a stream of IR transparent gas such as N 2 , At or He which flushes the analytes into a suitable gas cell. The spectrum of the sample is either collected using a Fourier transform spectrometer and commercially available GC/IR or kinetic data collection software or a single wavelength measurement is made using a filter or prism instrument. By integrating the area under the curve for the infrared response versus desorption time, the concentration of the analytes can be calculated

  16. SOLVENT FREE ONE POT SYNTHESIS OF NOVEL NAPHTHO[1,8 ...

    African Journals Online (AJOL)

    KEY WORDS: Synthesis, Naphtho[1,8-gh]quinazoline-7,10-diones, One pot, ... In this regard, development of novel compounds and especially diverse small ..... catalysed by lithium bromide: An improved procedure for the Biginelli reaction.

  17. Structure of solvent-free grafted nanoparticles: Molecular dynamics and density-functional theory

    KAUST Repository

    Chremos, Alexandros; Panagiotopoulos, Athanassios Z.; Yu, Hsiu-Yu; Koch, Donald L.

    2011-01-01

    with decreasing particle volume fraction to fill the interstitial space. At higher temperatures, the simulations reveal effects that differ from the theory and are likely caused by steric repulsions of the expanded corona chains. © 2011 American Institute

  18. Cycloadditions of ketene acetals under microwave irradiation in solvent-free conditions

    International Nuclear Information System (INIS)

    Diaz-Ortiz, A.; Diez-Barra, E.; La Hoz, A. De; Prieto, P.; Moreno, A.

    1994-01-01

    When subjected to microwave irradiation ketene acetals undergo 1.3-dipolar and hetero-Diels-Alder cycloadditions within 5-12 min to give excellent yields of easily purified heterocyclic products. This efficient and rapid synthesis has the advantage of employing milder reaction conditions than those of classical thermal heating. (author)

  19. Solvent-free and catalyst-free chemistry: A benign pathway to sustainability

    Science.gov (United States)

    In the past decade, alternative benign organic methodologies have become an imperative part of organic syntheses and novel chemical reactions. The various new and innovative sustainable organic reactions and methodologies using no solvents or catalysts and employing alternative ...

  20. Green production of cocrystals using a new solvent-free approach by spray congealing.

    Science.gov (United States)

    Duarte, Íris; Andrade, Rita; Pinto, João F; Temtem, Márcio

    2016-06-15

    Pharmaceutical cocrystals are used as a strategy to overcome poor physicochemical properties of drugs. The use of cocrystals in the pharmaceutical industry remains to be fully exploited due, in part, to the scarcity of suitable large-scale production methods and lack of robust and cost-effective processes. To overcome these challenges, spray congealing was used for the first time in the preparation of cocrystals. The work considered a feasibility study, followed by a design of experiments to assess the impact of varying atomization and cooling-related process parameters on cocrystal formation, purity, particle size, shape and bulk powder flow properties. It was demonstrated that spray congealing could be used to produce cocrystals. The thermal analysis and X-ray results of the spray-congealed products were different from the pure components or physical mixtures and were aligned with those reported for the same cocrystals systems produced by other techniques. Cocrystal particles were compact and spherical consisting of aggregates of individual cocrystals entangled or adhered with each other. From the design of experiments, the results demonstrated that varying the process parameters did not influence cocrystal formation, but had an impact on cocrystal purity. Moreover, it was demonstrated that cocrystal particle properties can be adjusted, in situ, by varying atomization and cooling efficiency, in order to produce particles more suited for incorporation in final dosage forms such as tablets. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. New thermo-sensitive chelating surfactants for selective solvent-free extraction of uranyl nitrate

    International Nuclear Information System (INIS)

    Prevost, S.; Larpent, C.; Testard, F.; Coulombeau, H.; Baczko, K.; Berthon, L.; Desvaux, H.; Madic, C.; Zemb, T.

    2004-01-01

    Functional surfactants were synthesised by grafting a chelating group (amino-acid residue) to the tip of a poly-ethoxylated nonionic surfactant chain (C i E j : C i H 2i +1(OCH 2 CH 2 ) j OH)) or in a branched position. C i E j nonionic surfactants are known to be thermo-reversible and to exhibit a clouding phenomenon associated to phase separation of micelles. The functional surfactants retain both surface-active properties, characteristic thermo-reversible behaviour and have efficient complexing properties toward uranyl. In the presence of uranyl nitrate, small micelles are formed at ambient temperature and the de-mixing leads to a separation of the target ion trapped by the functional surfactant (cloud point extraction). Those surfactants are more efficient than mixture of classical C i E j and complexing agent solubilized in the micelles. This reveals a synergistic effect of the covalent bond between the chelating group and the nonionic surfactant C i E j . This paper presents a systematic study of the extraction and aggregation properties and the influence of the nature of the ions. (authors)

  2. Solvent-free one-pot 1,3-dipolar cycloaddition reactions of ...

    Indian Academy of Sciences (India)

    The synthetic utility of microwave irradiation in organic ..... ized by using frontier molecular orbital theory and 1H ... Expected broad signals for N–H proton around δ 3.40 and alco- holic OH groups around δ 5.20 ppm are also obtained.

  3. Acid, silver, and solvent-free gold-catalyzed hydrophenoxylation of internal alkynes

    Directory of Open Access Journals (Sweden)

    Marcia E. Richard

    2013-10-01

    Full Text Available A range of arylgold compounds have been synthesized and investigated as single-component catalysts for the hydrophenoxylation of unactivated internal alkynes. Both carbene and phosphine-ligated compounds were screened as part of this work, and the most efficient catalysts contained either JohnPhos or IPr/SIPr. Phenols bearing either electron-withdrawing or electron-donating groups were efficiently added using these catalysts. No silver salts, acids, or solvents were needed for the catalysis, and either microwave or conventional heating afforded moderate to excellent yields of the vinyl ethers.

  4. Solvent-free production of 1,3-diglyceride of CLA: Strategy consideration and protocol design

    DEFF Research Database (Denmark)

    Guo, Zheng; Sun, Yan

    2007-01-01

    of eliminating mass transfer resistance, creating effective interaction for a multiple-phase reaction system and yielding an efficient water removal and a faster reaction rate. Hence, vacuum-driven N2 stirring was considered as the best choice among the tested strategies for the production of pure 1......Enzymatic production of a homogeneous 1,3-diglyceride of polyunsaturated fatty acids (PUFAs) was carried out using Novozym 435 as biocatalyst and conjugated linoleic acid (CLA) as a model fatty acid. Three different operation modes, namely, magnetic stirring under vacuum, vacuum-driven N2 bubbling...... incubated with 10–12 mmol CLA for about 3 h at 45–55 °C and a pressure less than 10 mbar, with enzyme loading of 40–70 g l−1. Among the operational parameters, temperature and reaction time were found to have profound effects on the acylmigration and yield of 1,3-diglyceride. Moreover, the enzyme showed...

  5. Solvent-Free Synthesis of Quaternary Metal Sulfide Nanoparticles Derived from Thiourea

    KAUST Repository

    Bhunia, Manas Kumar

    2017-08-09

    The synthesis of metal sulfide (MS) materials with sizes in the sub-10 nm regime often requires capping agents with long hydrocarbon chains that affect their structures and properties. Herein, this study presents a molten-state synthesis method for a series of transition-MS nanoparticles using thiourea as a reactive precursor without capping agents. This study also reports the synthesis of MS with single metals (Fe, Co, Ni, Cu, and Zn) and quaternary CuGa2In3S8 using the same synthesis protocol. Thiourea first melts to form a molten-state condition to serve as the reaction medium at a relatively low temperature (<200 °C), followed by its thermal decomposition to induce a reaction with the metal precursor to form different MS. This synthesis protocol, owing to its dynamic characteristics, involves the formation of a variety of organic carbon nitride polymeric complexes around the MS particles. Dynamic nuclear polarization surface-enhanced nuclear magnetic resonance spectroscopy is effective to identify the polymeric compositions and structures as well as their interactions with the MS. These results provided thorough structural descriptions of the MS nanoparticles surrounded by the carbon nitride species derived from thiourea, which may find various applications, including photocatalytic water splitting.

  6. Vacuum-and-solvent-free fabrication of organic semiconductor layers for field-effect transistors

    Science.gov (United States)

    Matsushima, Toshinori; Sandanayaka, Atula S. D.; Esaki, Yu; Adachi, Chihaya

    2015-01-01

    We demonstrate that cold and hot isostatic pressing (CIP and HIP) is a novel, alternative method for organic semiconductor layer fabrication, where organic powder is compressed into a layer shape directly on a substrate with 200 MPa pressure. Spatial gaps between powder particles and the other particles, substrates, or electrodes are crushed after CIP and HIP, making it possible to operate organic field-effect transistors (OFETs) containing the compressed powder as the semiconductor. The CIP-compressed powder of 2,7-dioctyl[1]benzothieno[3,2-b][1]benzothiophene (C8-BTBT) had a hole mobility of (1.6 ± 0.4) × 10–2 cm2/Vs. HIP of C8-BTBT powder increased the hole mobility to an amorphous silicon-like value (0.22 ± 0.07 cm2/Vs) because of the growth of the C8-BTBT crystallites and the improved continuity between the powder particles. The vacuum and solution processes are not involved in our CIP and HIP techniques, offering a possibility of manufacturing OFETs at low cost. PMID:26416434

  7. Green and solvent-free procedure for microwave-assisted synthesis ...

    Indian Academy of Sciences (India)

    tant tool in organic synthesis and therefore microwave chemistry can provide ... silica nanoparticles for preparation of highly substi- tuted pyridines.42 ..... MgO. 30. 60. 9. BaO. 25. 65. 10. NaOEt. 22. 70. 11. L-Alanine. 25. 65. 12. Montmorillonite.

  8. Solvent-free lipase-catalyzed synthesis of diacylgycerols as low-calorie food ingredients

    OpenAIRE

    Vázquez, Luis; González, Noemí; Reglero, Guillermo; Torres, Carlos F.

    2016-01-01

    Problems derived from obesity and overweight have recently promoted the development of fat substitutes and other low-calorie foods. On the one hand, fats with short- and medium-chain fatty acids are a source of quick energy, easily hydrolyzable and hardly stored as fat. Furthermore, 1,3-diacylglycerols are not hydrolyzed to 2-monoacylglycerols in the gastrointestinal tract, reducing the formation of chylomicron and lowers the serum level of triacylglycerols by decreasing its resynthesis in th...

  9. Solvent-free lipase catalysed synthesis of diacylgycerols as low-calorie food ingredients

    OpenAIRE

    Luis eVazquez

    2016-01-01

    Problems derived from obesity and overweight have recently promoted the development of fat substitutes and other low-calorie foods. On the one hand, fats with short and medium chain fatty acids are a source of quick energy, easily hydrolyzable and hardly stored as fat. Furthermore, 1,3-diacylglycerols are not hydrolyzed to 2-monoacylglycerols in the gastrointestinal tract, reducing the formation of chylomicron and lowers the serum level of triacylglycerols by decreasing its re-synthesis in th...

  10. A Green and Solvent-Free Process for Preparation of High- Purity ...

    African Journals Online (AJOL)

    http://dx.doi.org/10.4314/tjpr.v13i1.6 · AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's Partners · Terms and Conditions of Use · Contact AJOL · News. OTHER RESOURCES... for Researchers · for Journals · for Authors · for Policy Makers ...

  11. Solvent-Free Synthesis of Quaternary Metal Sulfide Nanoparticles Derived from Thiourea

    KAUST Repository

    Bhunia, Manas Kumar; Abou-Hamad, Edy; Anjum, Dalaver H.; Gurinov, Andrei; Takanabe, Kazuhiro

    2017-01-01

    The synthesis of metal sulfide (MS) materials with sizes in the sub-10 nm regime often requires capping agents with long hydrocarbon chains that affect their structures and properties. Herein, this study presents a molten-state synthesis method

  12. Scalable organic solvent free supercritical fluid spray drying process for producing dry protein formulations.

    Science.gov (United States)

    Nuchuchua, O; Every, H A; Hofland, G W; Jiskoot, W

    2014-11-01

    In this study, we evaluated the influence of supercritical carbon dioxide (scCO2) spray drying conditions, in the absence of organic solvent, on the ability to produce dry protein/trehalose formulations at 1:10 and 1:4 (w/w) ratios. When using a 4L drying vessel, we found that decreasing the solution flow rate and solution volume, or increasing the scCO2 flow rate resulted in a significant reduction in the residual water content in dried products (Karl Fischer titration). The best conditions were then used to evaluate the ability to scale the scCO2 spray drying process from 4L to 10L chamber. The ratio of scCO2 and solution flow rate was kept constant. The products on both scales exhibited similar residual moisture contents, particle morphologies (SEM), and glass transition temperatures (DSC). After reconstitution, the lysozyme activity (enzymatic assay) and structure (circular dichroism, HP-SEC) were fully preserved, but the sub-visible particle content was slightly increased (flow imaging microscopy, nanoparticle tracking analysis). Furthermore, the drying condition was applicable to other proteins resulting in products of similar quality as the lysozyme formulations. In conclusion, we established scCO2 spray drying processing conditions for protein formulations without an organic solvent that holds promise for the industrial production of dry protein formulations. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. A transparent, solvent-free laminated top electrode for perovskite solar cells.

    Science.gov (United States)

    Makha, Mohammed; Fernandes, Silvia Letícia; Jenatsch, Sandra; Offermans, Ton; Schleuniger, Jürg; Tisserant, Jean-Nicolas; Véron, Anna C; Hany, Roland

    2016-01-01

    A simple lamination process of the top electrode for perovskite solar cells is demonstrated. The laminate electrode consists of a transparent and conductive plastic/metal mesh substrate, coated with an adhesive mixture of poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate), PEDOT:PSS, and sorbitol. The laminate electrode showed a high degree of transparency of 85%. Best cell performance was achieved for laminate electrodes prepared with a sorbitol concentration of ~30 wt% per milliliter PEDOT:PSS dispersion, and using a pre-annealing temperature of 120°C for 10 min before lamination. Thereby, perovskite solar cells with stabilized power conversion efficiencies of (7.6 ± 1.0)% were obtained which corresponds to 80% of the reference devices with reflective opaque gold electrodes.

  14. A transparent, solvent-free laminated top electrode for perovskite solar cells

    OpenAIRE

    Makha, Mohammed; Fernandes, Silvia Let?cia; Jenatsch, Sandra; Offermans, Ton; Schleuniger, J?rg; Tisserant, Jean-Nicolas; V?ron, Anna C.; Hany, Roland

    2016-01-01

    Abstract A simple lamination process of the top electrode for perovskite solar cells is demonstrated. The laminate electrode consists of a transparent and conductive plastic/metal mesh substrate, coated with an adhesive mixture of poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate), PEDOT:PSS, and sorbitol. The laminate electrode showed a high degree of transparency of 85%. Best cell performance was achieved for laminate electrodes prepared with a sorbitol concentration of ~30 wt% per mil...

  15. Solvent-free Oxidation of Alcohols and Mild Catalytic Deprotection of ...

    African Journals Online (AJOL)

    NJD

    and ketones. Although the yields of aldehyde and ketone were high using this method, disadvantages included the need to use dimethyl sulphide, a volatile organic .... 1d. DABCO, CH2Cl2,. 5 h. 97. 1h water. TBBDA. 10 min. 85. –. PBBS. 10 min. 80. TEMPO, CuCl, O2,. 15 h. 72. 1j. (bmim)(PF6), 65°C. (NO3)3CeBrO3, 90°C.

  16. Solvent-Free Manufacturing of Electrodes for Lithium-ion Batteries

    Science.gov (United States)

    Ludwig, Brandon; Zheng, Zhangfeng; Shou, Wan; Wang, Yan; Pan, Heng

    2016-03-01

    Lithium ion battery electrodes were manufactured using a new, completely dry powder painting process. The solvents used for conventional slurry-cast electrodes have been completely removed. Thermal activation time has been greatly reduced due to the time and resource demanding solvent evaporation process needed with slurry-cast electrode manufacturing being replaced by a hot rolling process. It has been found that thermal activation time to induce mechanical bonding of the thermoplastic polymer to the remaining active electrode particles is only a few seconds. Removing the solvent and drying process allows large-scale Li-ion battery production to be more economically viable in markets such as automotive energy storage systems. By understanding the surface energies of various powders which govern the powder mixing and binder distribution, bonding tests of the dry-deposited particles onto the current collector show that the bonding strength is greater than slurry-cast electrodes, 148.8 kPa as compared to 84.3 kPa. Electrochemical tests show that the new electrodes outperform conventional slurry processed electrodes, which is due to different binder distribution.

  17. Alternative additives; Alternative additiver

    Energy Technology Data Exchange (ETDEWEB)

    2007-08-15

    In this project a number of industrial and agricultural waste products have been characterised and evaluated in terms of alkali-getter performance. The intended use is for biomass-fired power stations aiming at reducing corrosion or slagging related problems. The following products have been obtained, characterised and evaluated: 1) Brewery draff 2) Danish de-gassed manure 3) Paper sludge 4) Moulding sand 5) Spent bleaching earth 6) Anorthosite 7) Sand 8) Clay-sludge. Most of the above alternative additive candidates are deemed unsuitable due to insufficient chemical effect and/or expensive requirements for pre-treatment (such as drying and transportation). 3 products were selected for full-scale testing: de-gassed manure, spent bleaching earth and clay slugde. The full scale tests were undertaken at the biomass-fired power stations in Koege, Slagelse and Ensted. Spent bleaching earth (SBE) and clay sludge were the only tested additive candidates that had a proven ability to react with KCl, to thereby reduce Cl-concentrations in deposits, and reduce the deposit flux to superheater tubes. Their performance was shown to nearly as good as commercial additives. De-gassed manure, however, did not evaluate positively due to inhibiting effects of Ca in the manure. Furthermore, de-gassed manure has a high concentration of heavy metals, which imposes a financial burden with regard to proper disposal of the ash by-products. Clay-sludge is a wet clay slurring, and drying and transportation of this product entails substantial costs. Spent bleaching does not require much pre-treatment and is therefore the most promising alternative additive. On the other hand, bleaching earth contains residual plant oil which means that a range of legislation relating to waste combustion comes into play. Not least a waste combustion fee of 330 DKK/tonne. For all alternative (and commercial) additives disposal costs of the increase ash by-products represents a significant cost. This is

  18. Model Additional Protocol

    International Nuclear Information System (INIS)

    Rockwood, Laura

    2001-01-01

    Since the end of the cold war a series of events has changed the circumstances and requirements of the safeguards system. The discovery of a clandestine nuclear weapons program in Iraq, the continuing difficulty in verifying the initial report of Democratic People's Republic of Korea upon entry into force of their safeguards agreement, and the decision of the South African Government to give up its nuclear weapons program and join the Treaty on the Non-Proliferation of Nuclear Weapons have all played a role in an ambitious effort by IAEA Member States and the Secretariat to strengthen the safeguards system. A major milestone in this effort was reached in May 1997 when the IAEA Board of Governors approved a Model Protocol Additional to Safeguards Agreements. The Model Additional Protocol was negotiated over a period of less than a year by an open-ended committee of the Board involving some 70 Member States and two regional inspectorates. The IAEA is now in the process of negotiating additional protocols, State by State, and implementing them. These additional protocols will provide the IAEA with rights of access to information about all activities related to the use of nuclear material in States with comprehensive safeguards agreements and greatly expanded physical access for IAEA inspectors to confirm or verify this information. In conjunction with this, the IAEA is working on the integration of these measures with those provided for in comprehensive safeguards agreements, with a view to maximizing the effectiveness and efficiency, within available resources, the implementation of safeguards. Details concerning the Model Additional Protocol are given. (author)

  19. Additive manufacturing of metals

    International Nuclear Information System (INIS)

    Herzog, Dirk; Seyda, Vanessa; Wycisk, Eric; Emmelmann, Claus

    2016-01-01

    Additive Manufacturing (AM), the layer-by layer build-up of parts, has lately become an option for serial production. Today, several metallic materials including the important engineering materials steel, aluminium and titanium may be processed to full dense parts with outstanding properties. In this context, the present overview article describes the complex relationship between AM processes, microstructure and resulting properties for metals. It explains the fundamentals of Laser Beam Melting, Electron Beam Melting and Laser Metal Deposition, and introduces the commercially available materials for the different processes. Thereafter, typical microstructures for additively manufactured steel, aluminium and titanium are presented. Special attention is paid to AM specific grain structures, resulting from the complex thermal cycle and high cooling rates. The properties evolving as a consequence of the microstructure are elaborated under static and dynamic loading. According to these properties, typical applications are presented for the materials and methods for conclusion.

  20. Additive manufactured serialization

    Science.gov (United States)

    Bobbitt, III, John T.

    2017-04-18

    Methods for forming an identifying mark in a structure are described. The method is used in conjunction with an additive manufacturing method and includes the alteration of a process parameter during the manufacturing process. The method can form in a unique identifying mark within or on the surface of a structure that is virtually impossible to be replicated. Methods can provide a high level of confidence that the identifying mark will remain unaltered on the formed structure.

  1. BWR zinc addition Sourcebook

    International Nuclear Information System (INIS)

    Garcia, Susan E.; Giannelli, Joseph F.; Jarvis, Alfred J.

    2014-01-01

    Boiling Water Reactors (BWRs) have been injecting zinc into the primary coolant via the reactor feedwater system for over 25 years for the purpose of controlling primary system radiation fields. The BWR zinc injection process has evolved since the initial application at the Hope Creek Nuclear Station in 1986. Key transitions were from the original natural zinc oxide (NZO) to depleted zinc oxide (DZO), and from active zinc injection of a powdered zinc oxide slurry (pumped systems) to passive injection systems (zinc pellet beds). Zinc addition has continued through various chemistry regimes changes, from normal water chemistry (NWC) to hydrogen water chemistry (HWC) and HWC with noble metals (NobleChem™) for mitigation of intergranular stress corrosion cracking (IGSCC) of reactor internals and primary system piping. While past reports published by the Electric Power Research Institute (EPRI) document specific industry experience related to these topics, the Zinc Sourcebook was prepared to consolidate all of the experience gained over the past 25 years. The Zinc Sourcebook will benefit experienced BWR Chemistry, Operations, Radiation Protection and Engineering personnel as well as new people entering the nuclear power industry. While all North American BWRs implement feedwater zinc injection, a number of other BWRs do not inject zinc. This Sourcebook will also be a valuable resource to plants considering the benefits of zinc addition process implementation, and to gain insights on industry experience related to zinc process control and best practices. This paper presents some of the highlights from the Sourcebook. (author)

  2. Teardrop bladder: additional considerations

    International Nuclear Information System (INIS)

    Wechsler, R.J.; Brennan, R.E.

    1982-01-01

    Nine cases of teardrop bladder (TDB) seen at excretory urography are presented. In some of these patients, the iliopsoas muscles were at the upper limit of normal in size, and additional evaluation of the perivesical structures with computed tomography (CT) was necessary. CT demonstrated only hypertrophied muscles with or without perivesical fat. The psoas muscles and pelvic width were measured in 8 patients and compared with the measurements of a control group of males without TDB. Patients with TDB had large iliopsoas muscles and narrow pelves compared with the control group. The psoas muscle width/pelvic width ratio was significantly greater (p < 0.0005) in patients with TDB than in the control group, with values of 1.04 + 0.05 and 0.82 + 0.09, respectively. It is concluded that TDB is not an uncommon normal variant in black males. Both iliopsoas muscle hypertrophy and a narrow pelvis are factors that predispose a patient to TDB

  3. Sewage sludge additive

    Science.gov (United States)

    Kalvinskas, J. J.; Mueller, W. A.; Ingham, J. D. (Inventor)

    1980-01-01

    The additive is for a raw sewage treatment process of the type where settling tanks are used for the purpose of permitting the suspended matter in the raw sewage to be settled as well as to permit adsorption of the dissolved contaminants in the water of the sewage. The sludge, which settles down to the bottom of the settling tank is extracted, pyrolyzed and activated to form activated carbon and ash which is mixed with the sewage prior to its introduction into the settling tank. The sludge does not provide all of the activated carbon and ash required for adequate treatment of the raw sewage. It is necessary to add carbon to the process and instead of expensive commercial carbon, coal is used to provide the carbon supplement.

  4. Bio-affinity mediated immobilization of lipase onto magnetic cellulose nanospheres for high yield biodiesel in one time addition of methanol.

    Science.gov (United States)

    Bandikari, Ramesh; Qian, Jiaxin; Baskaran, Ram; Liu, Ziduo; Wu, Gaobing

    2018-02-01

    To synthesis biodiesel from palm oil in one-time addition of methanol and solvent-free medium using CBD fused with C-terminal of lipase from G. stearothermophilus (GSlip-CBD) was immobilized onto magnetic cellulose nanosphere (MCNS). The immobilized matrix traits were preconceived by FT-IR, TEM and XRD. Perceptible biodiesel yield 98 and 73% was synthesized by GSlip-CBD-MCNS in 4 h and GSlip-MCNS in 6 h under the optimized conditions of oil:methanol ratio (1:3.5), temperature (55 and 50 °C) and enzyme loading (15 U). Intriguingly, the operational stability of GSlip-CBD-MCNS was an easily attainable owing to the magnetic properties and could be reused up to 8th and19th cycles with 94 and 45% of biodiesel yield respectively, compared to GSlip-MCNS. Thus GSlip-CBD-MCNS could be a potential biocatalyst for higher yield of biodiesel and reusability in one step addition of methanol. Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. In Situ Monitoring of the Mechanosynthesis of the Archetypal Metal-Organic Framework HKUST-1: Effect of Liquid Additives on the Milling Reactivity.

    Science.gov (United States)

    Stolar, Tomislav; Batzdorf, Lisa; Lukin, Stipe; Žilić, Dijana; Motillo, Cristina; Friščić, Tomislav; Emmerling, Franziska; Halasz, Ivan; Užarević, Krunoslav

    2017-06-05

    We have applied in situ monitoring of mechanochemical reactions by high-energy synchrotron powder X-ray diffraction to study the role of liquid additives on the mechanochemical synthesis of the archetypal metal-organic framework (MOF) HKUST-1, which was one of the first and is still among the most widely investigated MOF materials to be synthesized by solvent-free procedures. It is shown here how the kinetics and mechanisms of the mechanochemical synthesis of HKUST-1 can be influenced by milling conditions and additives, yielding on occasion two new and previously undetected intermediate phases containing a mononuclear copper core, and that finally rearrange to form the HKUST-1 architecture. On the basis of in situ data, we were able to tune and direct the milling reactions toward the formation of these intermediates, which were isolated and characterized by spectroscopic and structural means and their magnetic properties compared to those of HKUST-1. The results have shown that despite the relatively large breadth of analysis available for such widely investigated materials as HKUST-1, in situ monitoring of milling reactions can help in the detection and isolation of new materials and to establish efficient reaction conditions for the mechanochemical synthesis of porous MOFs.

  6. Functional bio-based polyesters by enzymatic polymerization

    DEFF Research Database (Denmark)

    Daugaard, Anders Egede; Hoffmann, Christian; Andersen, Christian

    During recent years enzymatic polymerization has become increasingly popular as an alternative to classical polyesterification processes. The high regioselectivity observed for lipases permits preparation of novel polyesters with a high number of functional groups.1 This is particularly interesting...... polymerization was applied to prepare functional water soluble polyesters based on dimethyl itaconate and poly(ethyleneglycol).2 The monomer permits postfunctionalization using thiol-ene chemistry or aza-michael additions, which was used to illustrate the possibilites of preparing functional hydrogels. Hydrogels...... based on the polyesters were shown to be degradable and could be prepared either from the pure polyester or from prefunctionalized polyesters, though the thiol-ene reactions were found to be less effective. Since then a new monomer, trans-2,5-dihydroxy-3-pentenoic acid methyl ester (DPM) has been...

  7. Stereoselective Synthesis of Functionalized 1,3-Disubstituted Isoindolines via Rh(III)-Catalyzed Tandem Oxidative Olefination-Cyclization of 4-Aryl-cyclic Sulfamidate-5-Carboxylates.

    Science.gov (United States)

    Achary, Raghavendra; Jung, In-A; Son, Se-Mi; Lee, Hyeon-Kyu

    2017-07-21

    A new method for the direct, stereoselective synthesis of highly functionalized 1,3-disubstituted isoindolines 6 from enantiomerically enriched cyclic 4-aryl-sulfamidate-5-carboxylates (5) is described. The process involves sulfamidate directed, Rh(III)-catalyzed tandem ortho C-H olefination of the 4-aryl-sulfamidate-5-carboxylates and subsequent cyclization by aza-Michael addition. In the reaction, which generates trans-1,3-disubstituted isoindolines exclusively, the configurational integrity of the stereogenic center in the starting cyclic sulfamidate is completely retained in the product. Examples are provided which show that the cyclic sulfamidate moiety not only serves as a chiral directing group but also as a versatile handle for further functionalization of the generated isoindoline ring system.

  8. Additive lattice kirigami.

    Science.gov (United States)

    Castle, Toen; Sussman, Daniel M; Tanis, Michael; Kamien, Randall D

    2016-09-01

    Kirigami uses bending, folding, cutting, and pasting to create complex three-dimensional (3D) structures from a flat sheet. In the case of lattice kirigami, this cutting and rejoining introduces defects into an underlying 2D lattice in the form of points of nonzero Gaussian curvature. A set of simple rules was previously used to generate a wide variety of stepped structures; we now pare back these rules to their minimum. This allows us to describe a set of techniques that unify a wide variety of cut-and-paste actions under the rubric of lattice kirigami, including adding new material and rejoining material across arbitrary cuts in the sheet. We also explore the use of more complex lattices and the different structures that consequently arise. Regardless of the choice of lattice, creating complex structures may require multiple overlapping kirigami cuts, where subsequent cuts are not performed on a locally flat lattice. Our additive kirigami method describes such cuts, providing a simple methodology and a set of techniques to build a huge variety of complex 3D shapes.

  9. Additive Manufactured Superconducting Cavities

    Science.gov (United States)

    Holland, Eric; Rosen, Yaniv; Woolleet, Nathan; Materise, Nicholas; Voisin, Thomas; Wang, Morris; Mireles, Jorge; Carosi, Gianpaolo; Dubois, Jonathan

    Superconducting radio frequency cavities provide an ultra-low dissipative environment, which has enabled fundamental investigations in quantum mechanics, materials properties, and the search for new particles in and beyond the standard model. However, resonator designs are constrained by limitations in conventional machining techniques. For example, current through a seam is a limiting factor in performance for many waveguide cavities. Development of highly reproducible methods for metallic parts through additive manufacturing, referred to colloquially as 3D printing\\x9D, opens the possibility for novel cavity designs which cannot be implemented through conventional methods. We present preliminary investigations of superconducting cavities made through a selective laser melting process, which compacts a granular powder via a high-power laser according to a digitally defined geometry. Initial work suggests that assuming a loss model and numerically optimizing a geometry to minimize dissipation results in modest improvements in device performance. Furthermore, a subset of titanium alloys, particularly, a titanium, aluminum, vanadium alloy (Ti - 6Al - 4V) exhibits properties indicative of a high kinetic inductance material. This work is supported by LDRD 16-SI-004.

  10. Green Chemistry Challenge: 2017 Greener Synthetic Pathways Award

    Science.gov (United States)

    Green Chemistry Challenge 2017 award winners, Merck, developed a novel asymmetric aza-Michael cyclization, employing a chemically stable and fully recyclable organocatalyst to make Letermovir, an antiviral drug

  11. effects of sulphur addition on addition on and mechanical properties

    African Journals Online (AJOL)

    User

    234-8034714355. 8034714355. 1. EFFECTS OF SULPHUR ADDITION ON. ADDITION ON. 2. AND MECHANICAL PROPERTIES O. 3. 4. C. W. Onyia. 5. 1DEPT. OF METALLURGICAL AND MATERIALS. 6. 2, 4DEPT. OF METALLURGICAL ...

  12. ADDITIVES USED TO OBTAIN FOOD

    Directory of Open Access Journals (Sweden)

    Dorina Ardelean

    2012-01-01

    Full Text Available Use of food additives in food is determined by the growth of contemporary food needs of the world population. Additives used in food, both natural and artificial ones, contribute to: improving the organoleptic characteristics and to preserve the food longer, but we must not forget that all these additives should not be found naturally in food products. Some of these additives are not harmful and human pests in small quantities, but others may have harmful effects on health.

  13. Color Addition and Subtraction Apps

    Science.gov (United States)

    Ruiz, Frances; Ruiz, Michael J.

    2015-01-01

    Color addition and subtraction apps in HTML5 have been developed for students as an online hands-on experience so that they can more easily master principles introduced through traditional classroom demonstrations. The evolution of the additive RGB color model is traced through the early IBM color adapters so that students can proceed step by step…

  14. How Safe Are Color Additives?

    Science.gov (United States)

    ... Linkedin Pin it Email Print Subscribe: FDA Consumer Health Information Color additives give the red tint to your fruit punch ... in Foods, Drugs, Cosmetics, and Medical Devices Color Additives: FDA's Regulatory Process and Historical Perspectives ... Health Cosmetics Dietary Supplements Drugs Food Medical Devices Nutrition ...

  15. Density measures and additive property

    OpenAIRE

    Kunisada, Ryoichi

    2015-01-01

    We deal with finitely additive measures defined on all subsets of natural numbers which extend the asymptotic density (density measures). We consider a class of density measures which are constructed from free ultrafilters on natural numbers and study a certain additivity property of such density measures.

  16. Prevalence of Food Additive Intolerance

    DEFF Research Database (Denmark)

    Madsen, Charlotte Bernhard

    1994-01-01

    The prevalence estimates vary with a factor 100. As the results vary so do the study populations. 6 If the different study populations are accounted for, a common conclusion can be drawn: Food additive intolerance is found in adults with atopic symptoms from the respiratory tract and skin. The prevalence......1 The existing prevalence estimates of food additive intolerance(1-4) are being reviewed. 2 In the EEC report the estimated frequency of food additive intolerance is 0.03% to 0.15% based on data from patient groups. 3 The British population study results in a prevalence estimate of 0.......026%. The challenged population is 81 children and adults with a history of reproducible clinical symptoms after ingestion of food additives. 4 In the Danish population study a prevalence of 1-2% is found in children age 5-16. In this study a total of 606 children mainly with atopic disease have been challenged. 5...

  17. Topology Optimization for Additive Manufacturing

    DEFF Research Database (Denmark)

    Clausen, Anders

    This PhD thesis deals with the combination of topology optimization and additive man-ufacturing (AM, also known as 3D-printing). In addition to my own works, the thesis contains a broader review and assessment of the literature within the field. The thesis first presents a classification...... of the various AM technologies, a review of relevant manufacturing materials, the properties of these materials in the additively manufactured part, as well as manufacturing constraints with a potential for design optimization. Subsequently, specific topology optimization formulations relevant for the most im...... for scalable manufacturing. In relation to interface problems it is shown how a flexible void area may be included into a standard minimum compliance problem by employing an additional design variable field and a sensitivity filter. Furthermore, it is shown how the design of coated structures may be modeled...

  18. (ICSID) ADDITIONAL FACILITY IN INTERNA

    African Journals Online (AJOL)

    Fr. Ikenga

    ... which is adopted by Article 5 of the Additional Facility Rules to guide the ... B, Barrister at Law, e-mail: kcezeibe@yahoo.com; Phone 08033950631 and .... revision and annulment which are internally available under the Washington ...

  19. Food additives: an ethical evaluation.

    Science.gov (United States)

    Mepham, Ben

    2011-01-01

    Food additives are an integral part of the modern food system, but opinion polls showing most Europeans have worries about them imply an urgent need for ethical analysis of their use. The existing literature on food ethics, safety assessment and animal testing. Food additives provide certain advantages in terms of many people's lifestyles. There are disagreements about the appropriate application of the precautionary principle and of the value and ethical validity of animal tests in assessing human safety. Most consumers have a poor understanding of the relative benefits and risks of additives, but concerns over food safety and animal testing remain high. Examining the impacts of food additives on consumer sovereignty, consumer health and on animals used in safety testing should allow a more informed debate about their appropriate uses.

  20. Wide and High Additive Manufacturing

    Energy Technology Data Exchange (ETDEWEB)

    Post, Brian K. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Roschli, Alex C. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-03-01

    The goal of this project is to develop and demonstrate the enabling technologies for Wide and High Additive Manufacturing (WHAM). WHAM will open up new areas of U.S. manufacturing for very large tooling in support of the transportation and energy industries, significantly reducing cost and lead time. As with Big Area Additive Manufacturing (BAAM), the initial focus is on the deposition of composite materials.

  1. Food additives and preschool children.

    Science.gov (United States)

    Martyn, Danika M; McNulty, Breige A; Nugent, Anne P; Gibney, Michael J

    2013-02-01

    Food additives have been used throughout history to perform specific functions in foods. A comprehensive framework of legislation is in place within Europe to control the use of additives in the food supply and ensure they pose no risk to human health. Further to this, exposure assessments are regularly carried out to monitor population intakes and verify that intakes are not above acceptable levels (acceptable daily intakes). Young children may have a higher dietary exposure to chemicals than adults due to a combination of rapid growth rates and distinct food intake patterns. For this reason, exposure assessments are particularly important in this age group. The paper will review the use of additives and exposure assessment methods and examine factors that affect dietary exposure by young children. One of the most widely investigated unfavourable health effects associated with food additive intake in preschool-aged children are suggested adverse behavioural effects. Research that has examined this relationship has reported a variety of responses, with many noting an increase in hyperactivity as reported by parents but not when assessed using objective examiners. This review has examined the experimental approaches used in such studies and suggests that efforts are needed to standardise objective methods of measuring behaviour in preschool children. Further to this, a more holistic approach to examining food additive intakes by preschool children is advisable, where overall exposure is considered rather than focusing solely on behavioural effects and possibly examining intakes of food additives other than food colours.

  2. Differently-catalyzed silica-based precursors as functional additives for the epoxy-based hybrid materials

    Czech Academy of Sciences Publication Activity Database

    Perchacz, Magdalena; Beneš, Hynek; Zhigunov, Alexander; Serkis, Magdalena; Pavlova, Ewa

    2016-01-01

    Roč. 99, 2 September (2016), s. 434-446 ISSN 0032-3861 R&D Projects: GA ČR(CZ) GA14-05146S; GA MŠk(CZ) LO1507 Institutional support: RVO:61389013 Keywords : epoxy-silica hybrid material * solvent-free sol-gel process * silica-based precursor Subject RIV: CD - Macromolecular Chemistry Impact factor: 3.684, year: 2016

  3. effects of sulphur addition on addition on and mechanical properties

    African Journals Online (AJOL)

    User

    on the microstructure and mechanical properties of sand cast been investigated ... owed that the addition of sulphur to Al-12wt%Si alloy. 12wt%Si alloy .... 28 materials. 29. Element. Aluminum. Silicon. Al. Si. Ca. Fe. Cu. Zn. Mn. Mg. Cr. B. 99.71.

  4. Evaluation of certain food additives.

    Science.gov (United States)

    2017-01-01

    This report represents the conclusions of a Joint FAO/WHO Expert Committee convened to evaluate the safety of various food additives, including flavouring agents, with a view to concluding as to safety concerns and to preparing specifications for identity and purity. The first part of the report contains a general discussion of the principles governing the toxicological evaluation of and assessment of dietary exposure to food additives, including flavouring agents. A summary follows of the Committee’s evaluations of technical, toxicological and dietary exposure data for 10 food additives (Allura Red AC; carob bean gum; lutein esters from Tagetes erecta; octenyl succinic acid (OSA)– modified gum arabic; pectin; Quinoline Yellow; rosemary extract; steviol glycosides; tartrazine; and xanthan gum) and five groups of flavouring agents (alicyclic, alicyclic-fused and aromatic-fused ring lactones; aliphatic and aromatic amines and amides; aliphatic secondary alcohols, ketones and related esters; cinnamyl alcohol and related substances; and tetrahydrofuran and furanone derivatives). Specifications for the following food additives were revised: aspartame; cassia gum; citric and fatty acid esters of glycerol (CITREM); modified starches; octanoic acid; starch sodium octenyl succinate; and total colouring matters. Annexed to the report are tables summarizing the Committee’s recommendations for dietary exposures to and toxicological evaluations of all of the food additives, including flavouring agents, considered at this meeting.

  5. Additive manufacturing of tunable lenses

    Science.gov (United States)

    Schlichting, Katja; Novak, Tobias; Heinrich, Andreas

    2017-02-01

    Individual additive manufacturing of optical systems based on 3D Printing offers varied possibilities in design and usage. In addition to the additive manufacturing procedure, the usage of tunable lenses allows further advantages for intelligent optical systems. Our goal is to bring the advantages of additive manufacturing together with the huge potential of tunable lenses. We produced tunable lenses as a bundle without any further processing steps, like polishing. The lenses were designed and directly printed with a 3D Printer as a package. The design contains the membrane as an optical part as well as the mechanical parts of the lens, like the attachments for the sleeves which contain the oil. The dynamic optical lenses were filled with an oil. The focal length of the lenses changes due to a change of the radius of curvature. This change is caused by changing the pressure in the inside of the lens. In addition to that, we designed lenses with special structures to obtain different areas with an individual optical power. We want to discuss the huge potential of this technology for several applications. Further, an appropriate controlling system is needed. Wéll show the possibilities to control and regulate the optical power of the lenses. The lenses could be used for illumination tasks, and in the future, for individual measurement tasks. The main advantage is the individuality and the possibility to create an individual design which completely fulfills the requirements for any specific application.

  6. Calcium addition in straw gasification

    DEFF Research Database (Denmark)

    Risnes, H.; Fjellerup, Jan Søren; Henriksen, Ulrik Birk

    2003-01-01

    The present work focuses on the influence of calcium addition in gasification. The inorganic¿organic element interaction as well as the detailed inorganic¿inorganic elements interaction has been studied. The effect of calcium addition as calcium sugar/molasses solutions to straw significantly...... affected the ash chemistry and the ash sintering tendency but much less the char reactivity. Thermo balance test are made and high-temperature X-ray diffraction measurements are performed, the experimental results indicate that with calcium addition major inorganic¿inorganic reactions take place very late...... in the char conversion process. Comprehensive global equilibrium calculations predicted important characteristics of the inorganic ash residue. Equilibrium calculations predict the formation of liquid salt if sufficient amounts of Ca are added and according to experiments as well as calculations calcium binds...

  7. Additive interaction in survival analysis

    DEFF Research Database (Denmark)

    Rod, Naja Hulvej; Lange, Theis; Andersen, Ingelise

    2012-01-01

    It is a widely held belief in public health and clinical decision-making that interventions or preventive strategies should be aimed at patients or population subgroups where most cases could potentially be prevented. To identify such subgroups, deviation from additivity of absolute effects...... an empirical example of interaction between education and smoking on risk of lung cancer. We argue that deviations from additivity of effects are important for public health interventions and clinical decision-making, and such estimations should be encouraged in prospective studies on health. A detailed...... is the relevant measure of interest. Multiplicative survival models, such as the Cox proportional hazards model, are often used to estimate the association between exposure and risk of disease in prospective studies. In Cox models, deviations from additivity have usually been assessed by surrogate measures...

  8. Additional disulfide bonds in insulin

    DEFF Research Database (Denmark)

    Vinther, Tine N; Pettersson, Ingrid; Huus, Kasper

    2015-01-01

    The structure of insulin, a glucose homeostasis-controlling hormone, is highly conserved in all vertebrates and stabilized by three disulfide bonds. Recently, we designed a novel insulin analogue containing a fourth disulfide bond located between positions A10-B4. The N-terminus of insulin's B......-chain is flexible and can adapt multiple conformations. We examined how well disulfide bond predictions algorithms could identify disulfide bonds in this region of insulin. In order to identify stable insulin analogues with additional disulfide bonds, which could be expressed, the Cβ cut-off distance had...... in comparison to analogues with additional disulfide bonds that were more difficult to predict. In contrast, addition of the fourth disulfide bond rendered all analogues resistant to fibrillation under stress conditions and all stable analogues bound to the insulin receptor with picomolar affinities. Thus...

  9. Aminodisulfides as additives to lubricants

    Energy Technology Data Exchange (ETDEWEB)

    Balin, A.I.; Tarasevich, V.B.; Veretenova, T.N.

    1980-01-01

    A study was carried out and tehcnology developed for producing sulfur-nitrogen containing additives of the type of aminodisulfide by interaction of beta, beta-dichlordialkyl (aryl) disulfides with diethanolamine in a medium of sulfur-diethanolamine. The 2,2'-bis-(diethanol)-dialkyl(aryl) disulfides obtained do not hydrolyze in aqueous soltuions of alkalis, exhibit rather high antiscoring properties and are recommended for tests as active additives of high pressure to SOZH and technological lubricants of the oil and emulsion types.

  10. Ultrafast Self-Assembly of Sub-10 nm Block Copolymer Nanostructures by Solvent-Free High-Temperature Laser Annealing.

    Science.gov (United States)

    Jiang, Jing; Jacobs, Alan G; Wenning, Brandon; Liedel, Clemens; Thompson, Michael O; Ober, Christopher K

    2017-09-20

    Laser spike annealing was applied to PS-b-PDMS diblock copolymers to induce short-time (millisecond time scale), high-temperature (300 to 700 °C) microphase segregation and directed self-assembly of sub-10 nm features. Conditions were identified that enabled uniform microphase separation in the time frame of tens of milliseconds. Microphase ordering improved with increased temperature and annealing time, whereas phase separation contrast was lost for very short annealing times at high temperature. PMMA brush underlayers aided ordering under otherwise identical laser annealing conditions. Good long-range order for sub-10 nm cylinder morphology was achieved using graphoepitaxy coupled with a 20 ms dwell laser spike anneal above 440 °C.

  11. A clean method for solvent-free nitration of toluene over sulfated titania promoted by ceria catalysts.

    Science.gov (United States)

    Mao, Wei; Ma, Hongzhu; Wang, Bo

    2009-08-15

    A mild simple method for nitration of aromatic compounds, various solid acids as catalysts, the air treated with the corona discharge generator as nitrating agent, the liquid-phase nitration of toluene, at ambient temperature and atmospheric pressure without solvent has been investigated. The results show that SO(4)(2-)/TiO(2) (ST) and SO(4)(2-)/TiO(2) doped with CeO(2) (STC) catalysts displayed good nitration activity in the experiments. It is an attractive method for the environmentally friendly synthesis of nitroaromatic compounds. Moreover, only mononitrotoluenes were detected in the products, and the ratio of para-nitrotoluene and ortho-nitrotoluene was approximately 1:1 with various catalysts. A maximum yield of about 11.4% was achieved for mononitrotoluenes in STC reaction system in 3h.

  12. Ultrasound-assisted catalytic synthesis of acyclic imides in the presence of p-toluenesulfonic acid under solvent free conditions

    Directory of Open Access Journals (Sweden)

    Nasr-Esfahani Masoud

    2012-01-01

    Full Text Available A rapid and convenient preparation of acyclic imides by the reaction of aliphatic and aromatic nitriles with acyclic carboxylic anhydride in the presence of catalytic amounts of p-toluenesulfonic acid under thermal or ultrasonic conditions is reported. The advantages of this procedure are moderate reaction times, good to excellent yields, use of inexpensive and ecofriendly catalyst. The reaction of nitriles with aliphatic anhydrides proceeds in thermal conditions, while by the use of ultrasound irradiations these reactions get accelerated.

  13. A low-cost, environment-friendly and solvent-free route for synthesis of AgBr nanoparticles

    Czech Academy of Sciences Publication Activity Database

    Shahsavani, E.; Khalaji, A.D.; Feizi, N.; Das, D.; Matalobos, J.S.; Kučeráková, Monika; Dušek, Michal

    2015-01-01

    Roč. 82, Jun (2015), s. 18-25 ISSN 0749-6036 R&D Projects: GA ČR(CZ) GA14-03276S Institutional support: RVO:68378271 Keywords : AgBr * nanoparticles * thiosemicarbazone * XRD * SEM * TEM Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.117, year: 2015

  14. Solvent-Free Biginelli Reactions Catalyzed by Hierarchical Zeolite Utilizing a Ball Mill Technique: A Green Sustainable Process

    Directory of Open Access Journals (Sweden)

    Ameen Shahid

    2017-03-01

    Full Text Available A sustainable, green one-pot process for the synthesis of dihydropyrimidinones (DHPMs derivatives by a three-component reaction of β-ketoester derivatives, aldehyde and urea or thiourea over the alkali-treated H-ZSM-5 zeolite under ball-milling was developed. Isolation of the product with ethyl acetate shadowed by vanishing of solvent was applied. The hierachical zeolite catalyst (MFI27_6 showed high yield (86%–96% of DHPMs in a very short time (10–30 min. The recyclability of the catalyst for the subsequent reactions was examined in four subsequent runs. The catalyst was shown to be robust without a detectable reduction in catalytic activity, and high yields of products showed the efficient protocol of the Biginelli reactions.

  15. Complexation of c6-ceramide with cholesteryl phosphocholine - a potent solvent-free ceramide delivery formulation for cells in culture.

    Directory of Open Access Journals (Sweden)

    Pramod Sukumaran

    Full Text Available Ceramides are potent bioactive molecules in cells. However, they are very hydrophobic molecules, and difficult to deliver efficiently to cells. We have made fluid bilayers from a short-chain D-erythro-ceramide (C6-Cer and cholesteryl phosphocholine (CholPC, and have used this as a formulation to deliver ceramide to cells. C6-Cer complexed with CholPC led to much larger biological effects in cultured cells (rat thyroid FRTL-5 and human HeLa cells in culture compared to C6-Cer dissolved in dimethyl sulfoxide (DMSO. Inhibition of cell proliferation and induction of apoptosis was significantly more efficient by C6-Cer/CholPC compared to C6-Cer dissolved in DMSO. C6-Cer/CholPC also permeated cell membranes and caused mitochondrial Ca(2+ influx more efficiently than C6-Cer in DMSO. Even though CholPC was taken up by cells to some extent (from C6-Cer/CholPC bilayers, and was partially hydrolyzed to free cholesterol (about 9%, none of the antiproliferative effects were due to CholPC or excess cholesterol. The ceramide effect was not limited to D-erythro-C6-Cer, since L-erythro-C6-Cer and D-erythro-C6-dihydroCer also inhibited cell priolifereation and affected Ca(2+ homeostasis. We conclude that C6-Cer complexed to CholPC increased the bioavailability of the short-chain ceramide for cells, and potentiated its effects in comparison to solvent-dissolved C6-Cer. This new ceramide formulation appears to be superior to previous solvent delivery approaches, and may even be useful with longer-chain ceramides.

  16. Microwave-assisted one-pot synthesis of ring-fused aminals under catalyst- and solvent-free conditions

    Science.gov (United States)

    Heterocyclic compounds hold a special place in drug discovery and variety of techniques such as combinatorial synthesis, parallel synthesis, and automated library production to increase the output of these entities has been developed. Although most of these techniques are rapid a...

  17. Preparation of Second Generation Ionic Liquids by Efficient Solvent-Free Alkylation of N-Heterocycles with Chloroalkanes

    Directory of Open Access Journals (Sweden)

    Werner Bonrath

    2008-01-01

    Full Text Available Non-conventional techniques, such as microwave (MW and power ultrasound(US as well as combined MW/US irradiation, have been used to promote one-potsynthesis of second-generation ionic liquids (ILs, cutting down reaction times andimproving yields. However, the use of chloroalkanes in the alkylation of N-heterocyclesrequires more drastic conditions if results are to match those obtained with more reactivealkyl halides. The present paper describes a series of MW- or MW/US-promoted ILpreparations starting from chloroalkanes and classic heterocycles (1-methylimidazole,pyridine and 1-methylpyrrolidine. When reactions were carried out under conventionalheating in an oil bath they required longer reaction times and gave poorer yields. 1H-NMRanalysis and ion-exchange chromatography showed that the present solventless procedureafforded ILs of satisfactory purity. The observed high yields (usually 70-98% isolated,and short reaction times showed that a straightforward access to ILs can be also achievedwith the use of alkyl chlorides, resulting in a considerable reduction of costs.

  18. Solvent-Free Esterification of Carboxylic Acids Using Supported Iron Oxide Nanoparticles as an Efficient and Recoverable Catalyst

    Directory of Open Access Journals (Sweden)

    Fatemeh Rajabi

    2016-07-01

    Full Text Available Supported iron oxide nanoparticles on mesoporous materials (FeNP@SBA-15 have been successfully utilized in the esterification of a variety carboxylic acids including aromatic, aliphatic, and long-chain carboxylic acids under convenient reaction conditions. The supported catalyst could be easily recovered after reaction completion and reused several times without any loss in activity after up to 10 runs.

  19. Facile and solvent-free routes for the synthesis of size-controllable Fe3O4 nanoparticles

    International Nuclear Information System (INIS)

    Ngo, Thanh Hieu; Tran, Dai Lam; Do, Hung Manh; Le, Van Hong; Nguyen, Xuan Phuc; Tran, Vinh Hoang

    2010-01-01

    Magnetite nanoparticles are one of the most important materials that are widely used in both medically diagnostic and therapeutic research. In this paper, we present some facile and non-toxic synthetic approaches for size-controllable preparations of magnetite nanoparticles, which are appropriate for biomedical applications, namely (i) co-precipitation; (ii) reduction–precipitation and (iii) oxidation–precipitation. Magnetic characterizations of the obtained nanoparticles have been studied and discussed. The oxidation precipitation route was chosen for investigation of the dependence of kinetic driven activation energy and that of coercive force on particle size (and temperature) during the course of the reaction. The structural–magnetic behavior was also correlated. Being solvent and surfactant-free, these methods are advantageous for synthesis and further functionalization towards biomedical applications

  20. Solvent-Free Synthesis of 2,20'-Dinitrobiphenyl: An Ullmann Coupling in the Introductory Organic Laboratory

    Science.gov (United States)

    Gregor, Richard W.; Goj, Laurel A.

    2011-01-01

    The formation of carbon-carbon bonds is an essential theme throughout organic chemistry. The use of transition-metal catalysts to form carbon-carbon bonds, once relegated to more advanced texts, is now commonly found in introductory organic textbooks. However, commensurate laboratory experiments for first-year organic students are more limited.…

  1. Solvent-free lipase-catalyzed preparation of diglycerides from co-products of vegetable oil refining

    Directory of Open Access Journals (Sweden)

    Tangkam, Kamol

    2008-09-01

    Full Text Available Co-products of vegetable oil refining such as a mixed deodorizer distillate resulting from the refining of various vegetable oils, a crude distillate resulting from the physical refining of coconut oil and commercial mixtures of distilled sunflower and coconut fatty acids were used as starting materials for the enzymatic preparation of diglycerides. Reaction conditions (temperature, pressure, molar ratio for the formation of diglycerides by lipase-catalyzed esterification/transesterification were studied using the mixed deodorizer distillate and glycerol as starting materials. The best results were obtained with the immobilized lipase B from Candida antarctica (Novozym 435 in vacuo at 60 °C leading to moderate proportions (~52% of diglycerides. The proportion of diglycerides increased when residual acylglycerides of the co-products of vegetable oil refining were hydrolyzed prior to esterification. Thus, the esterification of hydrolyzed co-products of vegetable oil refining with glycerol led to high formation (62-72% of diglycerides. Short-path vacuum distillation of the esterification products yielded distillation residues containing from 70% to 94% diglycerides. The proportions of fatty acids and monoglycerides in the distilled residues were quite low (Subproductos del refinado de los aceites vegetales tales como el destilado obtenido en el desodorizador al refinar distintos aceites vegetales, el destilado crudo resultante de la refinación física del aceite de coco, y mezclas comerciales de los ácidos grasos obtenidos en la destilación de aceites de girasol y coco fueron utilizados como materiales de partida para la preparación enzimática de diglicéridos. Se estudiaron las condiciones de reacción (temperatura, presión, relación molar para la formación de diglicéridos mediante esterificación/ transesterificación catalizada por lipasas usando la mezcla obtenida del desodorizador y glicerol como materiales de partida. Los mejores resultados se obtuvieron con lipasa B inmovilizada de Candida antarctica (Novozym 435 a vacío y 60 °C obteniéndose una concentración moderada (~52% de diglicéridos. La proporción de diglicéridos aumentó cuando los aciglicéridos residuales de los subproductos de la refinación de los aceites vegetales fueron hidrolizados como paso previo a la esterificación. Así, la esterificación de subproductos hidrolizados del refinado de aceites vegetales con glicerol produjo una alta (62-72% formación de diglicéridos. La posterior destilación a vacío de los productos de esta esterificación produjo destilados conteniendo del 70 al 94% de diglicéridos. Las proporciones de ácidos grasos y monoglicéridos en estos destilados fueron bastante bajas (Rhizomucor miehei y Thermomyces lanuginosus fueron menos activas como biocatalizadores de esterificación.

  2. H2 O2 –HBr: A metal-free and organic solvent-free reagent system ...

    Indian Academy of Sciences (India)

    Administrator

    Chemistry and Chemical Engineering Research Center of Iran, Pajoohesh Blvd., km 17, Karaj Hwy, ... A novel, practical and environmentally benign approach has been developed for .... pure products was applied; A Fisons instruments gas.

  3. Novel Solvent-free Perovskite Deposition in Fabrication of Normal and Inverted Architectures of Perovskite Solar Cells

    Science.gov (United States)

    Nejand, Bahram Abdollahi; Gharibzadeh, Saba; Ahmadi, Vahid; Shahverdi, H. Reza

    2016-01-01

    We introduced a new approach to deposit perovskite layer with no need for dissolving perovskite precursors. Deposition of Solution-free perovskite (SFP) layer is a key method for deposition of perovskite layer on the hole or electron transport layers that are strongly sensitive to perovskite precursors. Using deposition of SFP layer in the perovskite solar cells would extend possibility of using many electron and hole transport materials in both normal and invert architectures of perovskite solar cells. In the present work, we synthesized crystalline perovskite powder followed by successful deposition on TiO2 and cuprous iodide as the non-sensitve and sensitive charge transport layers to PbI2 and CH3NH3I solution in DMF. The post compressing step enhanced the efficiency of the devices by increasing the interface area between perovskite and charge transport layers. The 9.07% and 7.71% cell efficiencies of the device prepared by SFP layer was achieved in respective normal (using TiO2 as a deposition substrate) and inverted structure (using CuI as deposition substrate) of perovskite solar cell. This method can be efficient in large-scale and low cost fabrication of new generation perovskite solar cells. PMID:27640991

  4. Additive to clay drilling muds

    Energy Technology Data Exchange (ETDEWEB)

    Voytenko, V.S.; Nekrasova, V.B.; Nikitinskiy, E.L.; Ponomarev, V.N.

    1984-01-01

    The purpose of the invention is to improve the lubricating and strengthening properties of clay drilling muds. This goal is achieved because the lubricating and strengthening additive used is waste from the pulp and paper industry at the stage of reprocessing crude sulfate soap into phytosterol.

  5. The selective addition of water

    NARCIS (Netherlands)

    Resch, V.; Hanefeld, U.

    2014-01-01

    Water is omnipresent and essential. Yet at the same time it is a rather unreactive molecule. The direct addition of water to C[double bond, length as m-dash]C double bonds is therefore a challenge not answered convincingly. In this perspective we critically evaluate the selectivity and the

  6. Additive manufacturing in maxillofacial reconstruction

    Directory of Open Access Journals (Sweden)

    Dincă Luciana Laura

    2017-01-01

    Full Text Available In this paper the benefits of using additive manufacturing technologies in maxillofacial reconstruction are highlighted. Based on a real clinical case, the paper describes the manufacture of an implant prototype replacing the right zygomatic bone and a part of maxilla using additive manufacturing technologies. The face is the most expressive part of the human body that makes us unique. It was shown that the maxillofacial prostheses help to improve the psychological state of patients affected by, because low self esteem feeling appears commonly to this patients with the facial defects. The aim of this paper is to show how using additive manufacturing technologies methods within this research, the producing a surgical model will help surgeon to improve the pre-operative planning. For this we used additive manufacturing technologies such as Stereolitography to achieve the biomodel and FDM-fused deposition modelling to obtain a prototype model because these technologies make it possible to obtain prosthesis according to the physical and mechanical requirements of the region of implantation.

  7. Radiation curable Michael addition compounds

    International Nuclear Information System (INIS)

    Gruber, G.W.; Friedlander, C.B.; McDonald, W.H.; Dowbenko, R.

    1979-01-01

    Radiation polymerizable acrylyloxy-containing reaction products are provided from Michael addition reaction of an amide containing at least two acrylate groups with a primary or secondary amine. The resulting amine adducts of the amide, which contain at least one acrylate group per molecule, possesses high cure rates in air and are useful in compositions for forming coatings. (author)

  8. Additively manufactured porous tantalum implants

    NARCIS (Netherlands)

    Wauthle, Ruben; Van Der Stok, Johan; Yavari, Saber Amin; Van Humbeeck, Jan; Kruth, Jean Pierre; Zadpoor, Amir Abbas; Weinans, Harrie; Mulier, Michiel; Schrooten, Jan

    2015-01-01

    The medical device industry's interest in open porous, metallic biomaterials has increased in response to additive manufacturing techniques enabling the production of complex shapes that cannot be produced with conventional techniques. Tantalum is an important metal for medical devices because of

  9. Evaluation of certain food additives.

    Science.gov (United States)

    2012-01-01

    This report represents the conclusions of a Joint FAO/WHO Expert Committee convened to evaluate the safety of various food additives, including flavouring agents, with a view to concluding as to safety concerns and to preparing specifications for identity and purity. The first part of the report contains a general discussion of the principles governing the toxicological evaluation of and assessment of dietary exposure to food additives, including flavouring agents. A summary follows of the Committee's evaluations of technical, toxicological and dietary exposure data for five food additives (magnesium dihydrogen diphosphate; mineral oil (medium and low viscosity) classes II and III; 3-phytase from Aspergillus niger expressed in Aspergillus niger; serine protease (chymotrypsin) from Nocardiopsis prasina expressed in Bacillus licheniformis; and serine protease (trypsin) from Fusarium oxysporum expressed in Fusarium venenatum) and 16 groups of flavouring agents (aliphatic and aromatic amines and amides; aliphatic and aromatic ethers; aliphatic hydrocarbons, alcohols, aldehydes, ketones, carboxylic acids and related esters, sulfides, disulfides and ethers containing furan substitution; aliphatic linear alpha,beta-unsaturated aldehydes, acids and related alcohols, acetals and esters; amino acids and related substances; epoxides; furfuryl alcohol and related substances; linear and branched-chain aliphatic, unsaturated, unconjugated alcohols, aldehydes, acids and related esters; miscellaneous nitrogen-containing substances; phenol and phenol derivatives; pyrazine derivatives; pyridine, pyrrole and quinoline derivatives; saturated aliphatic acyclic branched-chain primary alcohols, aldehydes and acids; simple aliphatic and aromatic sulfides and thiols; sulfur-containing heterocyclic compounds; and sulfur-substituted furan derivatives). Specifications for the following food additives were revised: ethyl cellulose, mineral oil (medium viscosity), modified starches and titanium

  10. Protocol for ADDITION-PRO

    DEFF Research Database (Denmark)

    Johansen, Nanna Borup; Hansen, Anne-Louise Smidt; Jensen, Troels M

    2012-01-01

    disease and microvascular diabetic complications. We also require a better understanding of the mechanisms that underlie and drive early changes in cardiometabolic physiology. The ADDITION-PRO study was designed to address these issues among individuals at different levels of diabetes risk recruited from...... Danish primary care. METHODS/DESIGN: ADDITION-PRO is a population-based, longitudinal cohort study of individuals at high risk for diabetes. 16,136 eligible individuals were identified at high risk following participation in a stepwise screening programme in Danish general practice between 2001 and 2006....... All individuals with impaired glucose regulation at screening, those who developed diabetes following screening, and a random sub-sample of those at lower levels of diabetes risk were invited to attend a follow-up health assessment in 2009-2011 (n=4,188), of whom 2,082 (50%) attended. The health...

  11. Additive theory of prime numbers

    CERN Document Server

    Hua, L K

    2009-01-01

    Loo-Keng Hua was a master mathematician, best known for his work using analytic methods in number theory. In particular, Hua is remembered for his contributions to Waring's Problem and his estimates of trigonometric sums. Additive Theory of Prime Numbers is an exposition of the classic methods as well as Hua's own techniques, many of which have now also become classic. An essential starting point is Vinogradov's mean-value theorem for trigonometric sums, which Hua usefully rephrases and improves. Hua states a generalized version of the Waring-Goldbach problem and gives asymptotic formulas for the number of solutions in Waring's Problem when the monomial x^k is replaced by an arbitrary polynomial of degree k. The book is an excellent entry point for readers interested in additive number theory. It will also be of value to those interested in the development of the now classic methods of the subject.

  12. Dolomitic lime containing hydraulic additive

    International Nuclear Information System (INIS)

    Lagzdina, S.; Sedmalis, U.; Bidermanis, L.; Liepins, J.; Grosvalds, I.

    1997-01-01

    To obtain qualitative dolomitic lime the optimum calcination temperature of dolomite containing about 9 % of clayey substances is 900 deg C. The mechanical strength of dolomitic lime containing 30 % of brick waste additive after 6-9 months of hardening is 1.4-1.5 times higher than that of samples without hydraulic additive, for calcium lime - 2.2-2.6 times higher. Generally the mechanical strength of dolomitic lime is higher than that one of calcium lime. It can be explained by the active role of MgO in the hydration and hardening processes of dolomitic lime. Xray diffraction phase analysis was performed by X-ray diffractometer DPON-3M with Cu-K α emission filter

  13. Decontamination formulation with sorbent additive

    Science.gov (United States)

    Tucker; Mark D. , Comstock; Robert H.

    2007-10-16

    A decontamination formulation and method of making that neutralizes the adverse health effects of both chemical and biological compounds, especially chemical warfare (CW) and biological warfare (BW) agents, and toxic industrial chemicals. The formulation provides solubilizing compounds that serve to effectively render the chemical and biological compounds, particularly CW and BW compounds, susceptible to attack, and at least one reactive compound that serves to attack (and detoxify or kill) the compound. The formulation includes at least one solubilizing agent, a reactive compound, a bleaching activator, a sorbent additive, and water. The highly adsorbent, water-soluble sorbent additive (e.g., sorbitol or mannitol) is used to "dry out" one or more liquid ingredients, such as the liquid bleaching activator (e.g., propylene glycol diacetate or glycerol diacetate) and convert the activator into a dry, free-flowing powder that has an extended shelf life, and is more convenient to handle and mix in the field.

  14. The Frontiers of Additive Manufacturing

    Energy Technology Data Exchange (ETDEWEB)

    Grote, Christopher John [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2016-03-03

    Additive manufacturing, more commonly known as 3-D printing, has become a ubiquitous tool in science for its precise control over mechanical design. For additive manufacturing to work, a 3-D structure is split into thin 2D slices, and then different physical properties, such as photo-polymerization or melting, are used to grow the sequential layers. The level of control allows not only for devices to be made with a variety of materials: e.g. plastics, metals, and quantum dots, but to also have finely controlled structures leading to other novel properties. While 3-D printing is widely used by hobbyists for making models, it also has industrial applications in structural engineering, biological tissue scaffolding, customized electric circuitry, fuel cells, security, and more.

  15. Minimum Additive Waste Stabilization (MAWS)

    International Nuclear Information System (INIS)

    1994-02-01

    In the Minimum Additive Waste Stabilization(MAWS) concept, actual waste streams are utilized as additive resources for vitrification, which may contain the basic components (glass formers and fluxes) for making a suitable glass or glassy slag. If too much glass former is present, then the melt viscosity or temperature will be too high for processing; while if there is too much flux, then the durability may suffer. Therefore, there are optimum combinations of these two important classes of constituents depending on the criteria required. The challenge is to combine these resources in such a way that minimizes the use of non-waste additives yet yields a processable and durable final waste form for disposal. The benefit to this approach is that the volume of the final waste form is minimized (waste loading maximized) since little or no additives are used and vitrification itself results in volume reduction through evaporation of water, combustion of organics, and compaction of the solids into a non-porous glass. This implies a significant reduction in disposal costs due to volume reduction alone, and minimizes future risks/costs due to the long term durability and leach resistance of glass. This is accomplished by using integrated systems that are both cost-effective and produce an environmentally sound waste form for disposal. individual component technologies may include: vitrification; thermal destruction; soil washing; gas scrubbing/filtration; and, ion-exchange wastewater treatment. The particular combination of technologies will depend on the waste streams to be treated. At the heart of MAWS is vitrification technology, which incorporates all primary and secondary waste streams into a final, long-term, stabilized glass wasteform. The integrated technology approach, and view of waste streams as resources, is innovative yet practical to cost effectively treat a broad range of DOE mixed and low-level wastes

  16. Trust Trust Me (The Additivity)

    OpenAIRE

    Mano , Ken; Sakurada , Hideki; Tsukada , Yasuyuki

    2017-01-01

    Part 4: Trust Metrics; International audience; We present a mathematical formulation of a trust metric using a quality and quantity pair. Under a certain assumption, we regard trust as an additive value and define the soundness of a trust computation as not to exceed the total sum. Moreover, we point out the importance of not only soundness of each computed trust but also the stability of the trust computation procedure against changes in trust value assignment. In this setting, we define tru...

  17. A manual on using additives

    International Nuclear Information System (INIS)

    Lee, Bong Hoon

    1991-10-01

    This book consists of five chapters, which describe plasticizer ; summary, synthesis of plasticizer, basic notion, analysis and test on plasticizer, stabilizer ; stabilizer for plastic, an antioxidant, phosphorous acid estelle, ultraviolet ray absorbent, performance of stabilizer, influence on another additives, mix case of PVC production and analysis method for stabilizer, ultraviolet ray absorbent ; basic property and ultraviolet ray absorbent maker, anti-static agent ; basics, anti-static agent of a high molecule and analysis of anti-static agent, flame retardant of plastic.

  18. Additive property of separative power

    International Nuclear Information System (INIS)

    Yamamoto, Ichiro; Kanagawa, Akira

    1980-01-01

    A separative power of a separating element, whose heads and tails separation factors are α and β, is expressed by phi sub(b)(α, β) = [α(β - 1)1n α - (α - 1)1n β]/(αβ - 1) for the unit flow of the desired material and phi sub(a)(α, β) (= phi sub(b)(β, α)) for that of undesired material. The additive properties of the functions phi sub(b) and phi sub(a) were demonstrated by calculations of various types of ideal cascades, but the origin of the property is not obvious. The present study has furnished the mathematical basis of the additivity based on the special functional equation. First, for symmetric processes (α = β), the functional equation which describes the function representing the quality of separation f(α, α) concerning the desired material was obtained and solved to give the functional form of f(α, α). The result was extented to the function f(α, β) representing the quality of asymmetric separation (α not equal β). The derived function f(α, β) was demonstrated to be equal to phi sub(b)(α, β), and it was verified that functions phi sub(b)(α, β) and phi sub(a)(α, β) have the additive property in themselves. (author)

  19. Evaluation of certain food additives.

    Science.gov (United States)

    2009-01-01

    This report represents the conclusions of a Joint FAO/WHO Expert Committee convened to evaluate the safety of various food additives, including flavouring agents, with a view to recommending acceptable daily intakes (ADIs) and to preparing specifications for identity and purity. The first part of the report contains a general discussion of the principles governing the toxicological evaluation and assessment of intake of food additives (in particular, flavouring agents). A summary follows of the Committee's evaluations of technical, toxicological and intake data for certain food additives (asparaginase from Aspergillus niger expressed in A. niger, calcium lignosulfonate (40-65), ethyl lauroyl arginate, paprika extract, phospholipase C expressed in Pichia pastoris, phytosterols, phytostanols and their esters, polydimethylsiloxane, steviol glycosides and sulfites [assessment of dietary exposure]) and 10 groups of related flavouring agents (aliphatic branched-chain saturated and unsaturated alcohols, aldehydes, acids and related esters; aliphatic linear alpha,beta-unsaturated aldehydes, acids and related alcohols, acetals and esters; aliphatic secondary alcohols, ketones and related esters; alkoxy-substituted allylbenzenes present in foods and essential oils and used as flavouring agents; esters of aliphatic acyclic primary alcohols with aliphatic linear saturated carboxylic acids; furan-substituted aliphatic hydrocarbons, alcohols, aldehydes, ketones, carboxylic acids and related esters, sulfides, disulfides and ethers; miscellaneous nitrogen-containing substances; monocyclic and bicyclic secondary alcohols, ketones and related esters; hydroxy- and alkoxy-substituted benzyl derivatives; and substances structurally related to menthol). Specifications for the following food additives were revised: canthaxanthin; carob bean gum and carob bean gum (clarified); chlorophyllin copper complexes, sodium and potassium salts; Fast Green FCF; guar gum and guar gum (clarified

  20. Additive Manufacturing of Porous Metal

    Energy Technology Data Exchange (ETDEWEB)

    Dehoff, Ryan R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Kirka, Michael M. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-06-01

    Currently, helium is obtained through separation from natural gas. The current industrial process incurs significant costs and requires large energy resources to successfully achieve separation. Through utilizing Additive Manufacturing (AM) technologies it is possible to reduce both of these burdens when refining helium gas. The ability to engineer porosity levels within Inconel 718 discs for controlled separation of helium from natural gas was investigated. Arrays of samples fabricated using the electron beam melting process were analyzed for their relative porosity density. Based upon the measurements, full scale discs were fabricated, and subsequently tested to determine their effectiveness in separating helium from liquefied natural gas.

  1. Additive manufacturing of RF absorbers

    Science.gov (United States)

    Mills, Matthew S.

    The ability of additive manufacturing techniques to fabricate integrated electromagnetic absorbers tuned for specific radio frequency bands within structural composites allows for unique combinations of mechanical and electromagnetic properties. These composites and films can be used for RF shielding of sensitive electromagnetic components through in-plane and out-of-plane RF absorption. Structural composites are a common building block of many commercial platforms. These platforms may be placed in situations in which there is a need for embedded RF absorbing properties along with structural properties. Instead of adding radar absorbing treatments to the external surface of existing structures, which adds increased size, weight and cost; it could prove to be advantageous to integrate the microwave absorbing properties directly into the composite during the fabrication process. In this thesis, a method based on additive manufacturing techniques of composites structures with prescribed electromagnetic loss, within the frequency range 1 to 26GHz, is presented. This method utilizes screen printing and nScrypt micro dispensing to pattern a carbon based ink onto low loss substrates. The materials chosen for this study will be presented, and the fabrication technique that these materials went through to create RF absorbing structures will be described. The calibration methods used, the modeling of the RF structures, and the applications in which this technology can be utilized will also be presented.

  2. Mechanics of additively manufactured biomaterials.

    Science.gov (United States)

    Zadpoor, Amir A

    2017-06-01

    Additive manufacturing (3D printing) has found many applications in healthcare including fabrication of biomaterials as well as bioprinting of tissues and organs. Additively manufactured (AM) biomaterials may possess arbitrarily complex micro-architectures that give rise to novel mechanical, physical, and biological properties. The mechanical behavior of such porous biomaterials including their quasi-static mechanical properties and fatigue resistance is not yet well understood. It is particularly important to understand the relationship between the designed micro-architecture (topology) and the resulting mechanical properties. The current special issue is dedicated to understanding the mechanical behavior of AM biomaterials. Although various types of AM biomaterials are represented in the special issue, the primary focus is on AM porous metallic biomaterials. As a prelude to this special issue, this editorial reviews some of the latest findings in the mechanical behavior of AM porous metallic biomaterials so as to describe the current state-of-the-art and set the stage for the other studies appearing in the issue. Some areas that are important for future research are also briefly mentioned. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Additive versus multiplicative muon conservation

    International Nuclear Information System (INIS)

    Nemethy, P.

    1981-01-01

    Experimental elucidation of the question of muon conservation is reviewed. It is shown that neutral-current experiments have not yet yielded information about muonium-antimuonium conversion at the weak-interaction level and that all the charged-current experiments agree that there is no evidence for a multiplicative law. The best limits, from the muon-decay neutrino experiment at LAMPF and from the inverse muon-decay experiment in the CERN neutrino beam, definitely exclude multiplicative law schemes with a branching ratio R approximately 1/2. It is concluded that unless the dynamics conspire to make a multiplicative law with very small R it would appear that muon conservation obeys conserved additive lepton flavor law. (U.K.)

  4. An Additive Manufacturing Test Artifact

    Science.gov (United States)

    Moylan, Shawn; Slotwinski, John; Cooke, April; Jurrens, Kevin; Donmez, M Alkan

    2014-01-01

    A test artifact, intended for standardization, is proposed for the purpose of evaluating the performance of additive manufacturing (AM) systems. A thorough analysis of previously proposed AM test artifacts as well as experience with machining test artifacts have inspired the design of the proposed test artifact. This new artifact is designed to provide a characterization of the capabilities and limitations of an AM system, as well as to allow system improvement by linking specific errors measured in the test artifact to specific sources in the AM system. The proposed test artifact has been built in multiple materials using multiple AM technologies. The results of several of the builds are discussed, demonstrating how the measurement results can be used to characterize and improve a specific AM system. PMID:26601039

  5. Business models for additive manufacturing

    DEFF Research Database (Denmark)

    Hadar, Ronen; Bilberg, Arne; Bogers, Marcel

    2015-01-01

    Digital fabrication — including additive manufacturing (AM), rapid prototyping and 3D printing — has the potential to revolutionize the way in which products are produced and delivered to the customer. Therefore, it challenges companies to reinvent their business model — describing the logic...... of creating and capturing value. In this paper, we explore the implications that AM technologies have for manufacturing systems in the new business models that they enable. In particular, we consider how a consumer goods manufacturer can organize the operations of a more open business model when moving from...... a manufacturer-centric to a consumer-centric value logic. A major shift includes a move from centralized to decentralized supply chains, where consumer goods manufacturers can implement a “hybrid” approach with a focus on localization and accessibility or develop a fully personalized model where the consumer...

  6. Additive manufacturing with polypropylene microfibers.

    Science.gov (United States)

    Haigh, Jodie N; Dargaville, Tim R; Dalton, Paul D

    2017-08-01

    The additive manufacturing of small diameter polypropylene microfibers is described, achieved using a technique termed melt electrospinning writing. Sequential fiber layering, which is important for accurate three-dimensional fabrication, was achieved with the smallest fiber diameter of 16.4±0.2μm obtained. The collector speed, temperature and melt flow rate to the nozzle were optimized for quality and minimal fiber pulsing. Of particular importance to the success of this method is appropriate heating of the collector plate, so that the electrostatically drawn filament adheres during the direct-writing process. By demonstrating the direct-writing of polypropylene, new applications exploiting the favorable mechanical, stability and biocompatible properties of this polymer are envisaged. Copyright © 2017. Published by Elsevier B.V.

  7. Additivity of entropic uncertainty relations

    Directory of Open Access Journals (Sweden)

    René Schwonnek

    2018-03-01

    Full Text Available We consider the uncertainty between two pairs of local projective measurements performed on a multipartite system. We show that the optimal bound in any linear uncertainty relation, formulated in terms of the Shannon entropy, is additive. This directly implies, against naive intuition, that the minimal entropic uncertainty can always be realized by fully separable states. Hence, in contradiction to proposals by other authors, no entanglement witness can be constructed solely by comparing the attainable uncertainties of entangled and separable states. However, our result gives rise to a huge simplification for computing global uncertainty bounds as they now can be deduced from local ones. Furthermore, we provide the natural generalization of the Maassen and Uffink inequality for linear uncertainty relations with arbitrary positive coefficients.

  8. Additional Equipment for Soil Biodegradation

    Science.gov (United States)

    Vondráčková, Terezie; Kraus, Michal; Šál, Jiří

    2017-12-01

    Intensification of industrial production, increasing citizens’ living standards, expanding the consumer assortment mean in the production - consumption cycle a constantly increasing occurrence of waste material, which by its very nature must be considered as a source of useful raw materials in all branches of human activity. In addition to strict legislative requirements, a number of circumstances characterize waste management. It is mainly extensive transport associated with the handling and storage of large volumes of substances with a large assortment of materials (substances of all possible physical and chemical properties) and high demands on reliability and time coordination of follow-up processes. Considerable differences in transport distances, a large number of sources, processors and customers, and not least seasonal fluctuations in waste and strong price pressures cannot be overlooked. This highlights the importance of logistics in waste management. Soils that are contaminated with oil and petroleum products are hazardous industrial waste. Methods of industrial waste disposal are landfilling, biological processes, thermal processes and physical and chemical methods. The paper focuses on the possibilities of degradation of oil pollution, in particular biodegradation by bacteria, which is relatively low-cost among technologies. It is necessary to win the fight with time so that no ground water is contaminated. We have developed two additional devices to help reduce oil accident of smaller ranges. In the case of such an oil accident, it is necessary to carry out the permeability test of contaminated soil in time and, on this basis, to choose the technology appropriate to the accident - either in-sit biodegradation - at the site of the accident, or on-sit - to remove the soil and biodegrade it on the designated deposits. A special injection drill was developed for in-sit biodegradation, tossing and aeration equipment of the extracted soil was developed for

  9. Incommensurate crystallography without additional dimensions.

    Science.gov (United States)

    Kocian, Philippe

    2013-07-01

    It is shown that the Euclidean group of translations, when treated as a Lie group, generates translations not only in Euclidean space but on any space, curved or not. Translations are then not necessarily vectors (straight lines); they can be any curve compatible with the parameterization of the considered space. In particular, attention is drawn to the fact that one and only one finite and free module of the Lie algebra of the group of translations can generate both modulated and non-modulated lattices, the modulated character being given only by the parameterization of the space in which the lattice is generated. Moreover, it is shown that the diffraction pattern of a structure is directly linked to the action of that free and finite module. In the Fourier transform of a whole structure, the Fourier transform of the electron density of one unit cell (i.e. the structure factor) appears concretely, whether the structure is modulated or not. Thus, there exists a neat separation: the geometrical aspect on the one hand and the action of the group on the other, without requiring additional dimensions.

  10. Sustainability Characterization for Additive Manufacturing.

    Science.gov (United States)

    Mani, Mahesh; Lyons, Kevin W; Gupta, S K

    2014-01-01

    Additive manufacturing (AM) has the potential to create geometrically complex parts that require a high degree of customization, using less material and producing less waste. Recent studies have shown that AM can be an economically viable option for use by the industry, yet there are some inherent challenges associated with AM for wider acceptance. The lack of standards in AM impedes its use for parts production since industries primarily depend on established standards in processes and material selection to ensure the consistency and quality. Inability to compare AM performance against traditional manufacturing methods can be a barrier for implementing AM processes. AM process sustainability has become a driver due to growing environmental concerns for manufacturing. This has reinforced the importance to understand and characterize AM processes for sustainability. Process characterization for sustainability will help close the gaps for comparing AM performance to traditional manufacturing methods. Based on a literature review, this paper first examines the potential environmental impacts of AM. A methodology for sustainability characterization of AM is then proposed to serve as a resource for the community to benchmark AM processes for sustainability. Next, research perspectives are discussed along with relevant standardization efforts.

  11. Dynamics of ultrasonic additive manufacturing.

    Science.gov (United States)

    Hehr, Adam; Dapino, Marcelo J

    2017-01-01

    Ultrasonic additive manufacturing (UAM) is a solid-state technology for joining similar and dissimilar metal foils near room temperature by scrubbing them together with ultrasonic vibrations under pressure. Structural dynamics of the welding assembly and work piece influence how energy is transferred during the process and ultimately, part quality. To understand the effect of structural dynamics during UAM, a linear time-invariant model is proposed to relate the inputs of shear force and electric current to resultant welder velocity and voltage. Measured frequency response and operating performance of the welder under no load is used to identify model parameters. Using this model and in-situ measurements, shear force and welder efficiency are estimated to be near 2000N and 80% when welding Al 6061-H18 weld foil, respectively. Shear force and welder efficiency have never been estimated before in UAM. The influence of processing conditions, i.e., welder amplitude, normal force, and weld speed, on shear force and welder efficiency are investigated. Welder velocity was found to strongly influence the shear force magnitude and efficiency while normal force and weld speed showed little to no influence. The proposed model is used to describe high frequency harmonic content in the velocity response of the welder during welding operations and coupling of the UAM build with the welder. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Dimensionless numbers in additive manufacturing

    Science.gov (United States)

    Mukherjee, T.; Manvatkar, V.; De, A.; DebRoy, T.

    2017-02-01

    The effects of many process variables and alloy properties on the structure and properties of additively manufactured parts are examined using four dimensionless numbers. The structure and properties of components made from 316 Stainless steel, Ti-6Al-4V, and Inconel 718 powders for various dimensionless heat inputs, Peclet numbers, Marangoni numbers, and Fourier numbers are studied. Temperature fields, cooling rates, solidification parameters, lack of fusion defects, and thermal strains are examined using a well-tested three-dimensional transient heat transfer and fluid flow model. The results show that lack of fusion defects in the fabricated parts can be minimized by strengthening interlayer bonding using high values of dimensionless heat input. The formation of harmful intermetallics such as laves phases in Inconel 718 can be suppressed using low heat input that results in a small molten pool, a steep temperature gradient, and a fast cooling rate. Improved interlayer bonding can be achieved at high Marangoni numbers, which results in vigorous circulation of liquid metal, larger pool dimensions, and greater depth of penetration. A high Fourier number ensures rapid cooling, low thermal distortion, and a high ratio of temperature gradient to the solidification growth rate with a greater tendency of plane front solidification.

  13. Additive Manufacturing of Fuel Injectors

    Energy Technology Data Exchange (ETDEWEB)

    Sadek Tadros, Dr. Alber Alphonse [Edison Welding Institute, Inc., Columbus, OH (United States); Ritter, Dr. George W. [Edison Welding Institute, Inc., Columbus, OH (United States); Drews, Charles Donald [Edison Welding Institute, Inc., Columbus, OH (United States); Ryan, Daniel [Solar Turbines Inc., San Diego, CA (United States)

    2017-10-24

    Additive manufacturing (AM), also known as 3D-printing, has been shifting from a novelty prototyping paradigm to a legitimate manufacturing tool capable of creating components for highly complex engineered products. An emerging AM technology for producing metal parts is the laser powder bed fusion (L-PBF) process; however, industry manufacturing specifications and component design practices for L-PBF have not yet been established. Solar Turbines Incorporated (Solar), an industrial gas turbine manufacturer, has been evaluating AM technology for development and production applications with the desire to enable accelerated product development cycle times, overall turbine efficiency improvements, and supply chain flexibility relative to conventional manufacturing processes (casting, brazing, welding). Accordingly, Solar teamed with EWI on a joint two-and-a-half-year project with the goal of developing a production L-PBF AM process capable of consistently producing high-nickel alloy material suitable for high temperature gas turbine engine fuel injector components. The project plan tasks were designed to understand the interaction of the process variables and their combined impact on the resultant AM material quality. The composition of the high-nickel alloy powders selected for this program met the conventional cast Hastelloy X compositional limits and were commercially available in different particle size distributions (PSD) from two suppliers. Solar produced all the test articles and both EWI and Solar shared responsibility for analyzing them. The effects of powder metal input stock, laser parameters, heat treatments, and post-finishing methods were evaluated. This process knowledge was then used to generate tensile, fatigue, and creep material properties data curves suitable for component design activities. The key process controls for ensuring consistent material properties were documented in AM powder and process specifications. The basic components of the project

  14. Septic tank additive impacts on microbial populations.

    Science.gov (United States)

    Pradhan, S; Hoover, M T; Clark, G H; Gumpertz, M; Wollum, A G; Cobb, C; Strock, J

    2008-01-01

    Environmental health specialists, other onsite wastewater professionals, scientists, and homeowners have questioned the effectiveness of septic tank additives. This paper describes an independent, third-party, field scale, research study of the effects of three liquid bacterial septic tank additives and a control (no additive) on septic tank microbial populations. Microbial populations were measured quarterly in a field study for 12 months in 48 full-size, functioning septic tanks. Bacterial populations in the 48 septic tanks were statistically analyzed with a mixed linear model. Additive effects were assessed for three septic tank maintenance levels (low, intermediate, and high). Dunnett's t-test for tank bacteria (alpha = .05) indicated that none of the treatments were significantly different, overall, from the control at the statistical level tested. In addition, the additives had no significant effects on septic tank bacterial populations at any of the septic tank maintenance levels. Additional controlled, field-based research iswarranted, however, to address additional additives and experimental conditions.

  15. Additive conjoint measurement for multiattribute utility

    NARCIS (Netherlands)

    Maas, A.; Wakker, P.P.

    1994-01-01

    This paper shows that multiattribute utility can be simplified by methods from additive conjoint measurement. Given additive conjoint measurability under certainty, axiomatizations can be simplified, and implementation and reliability of elicitation can be improved. This also contributes to the

  16. Additive Manufacturing of Aerospace Propulsion Components

    Science.gov (United States)

    Misra, Ajay K.; Grady, Joseph E.; Carter, Robert

    2015-01-01

    The presentation will provide an overview of ongoing activities on additive manufacturing of aerospace propulsion components, which included rocket propulsion and gas turbine engines. Future opportunities on additive manufacturing of hybrid electric propulsion components will be discussed.

  17. The Philosophical Consideration about Food Additives

    OpenAIRE

    Baoyu Ma

    2015-01-01

    This study mainly analyzes the essential features of food additives technology from the angle of philosophy, explaining the essential characteristics of food additives technology. As for the attitude towards the application of food additives, it is influenced by the public's gender, age, educational level, occupation and monthly expenditure for buying non-staple food and other variables, thus, the attitude towards food additives and green food, as well as the attitude towards using artificial...

  18. The dilemma of allergy to food additives.

    Science.gov (United States)

    Bahna, Sami L; Burkhardt, Joshua G

    2018-01-01

    To provide a brief summary on food additives and to outline a practical approach for evaluating subjects suspected of having reactions to food additives. Information was derived from selected reviews and original articles published in peer-reviewed journals, supplemented by the clinical experience of the authors. Priority was given to studies that used blinded, placebo controlled, oral challenges to confirm adverse reactions to food additives. In addition, selected, appropriately evaluated case reports were included. A large number of food additives are widely used in the food industry. Allergic reactions to additives seem to be rare but are very likely underdiagnosed, primarily due to a low index of suspicion. A wide variety of symptoms to food additives have been reported, but a cause-and-effect relationship has not been well documented in the majority of cases. Reactions to food additives should be suspected in patients who report symptoms related to multiple foods or to a certain food when commercially prepared but not when home made. It is also prudent to investigate food additives in subjects considered to have "idiopathic" reactions. Except for a limited number of natural additives, there is a small role for skin tests or in vitro testing. Oral challenge, in stages, with commonly used additives is the definitive procedure for detecting the offending agent. Once the specific additive is identified, management is strict avoidance, which can be difficult.

  19. Enabling Technologies for Medium Additive Manufacturing (MAAM)

    Energy Technology Data Exchange (ETDEWEB)

    Richardson, Bradley S. [ORNL; Love, Lonnie J. [ORNL; Chesser, Phillip C. [ORNL; Miller, Jason [Cosine Additive, Inc.; McCalip, Andrew [Cosine Additive, Inc.

    2018-02-01

    ORNL has worked with Cosine Additive, Inc. on the design of MAAM extrusion components. The objective is to improve the print speed and part quality. A pellet extruder has been procured and integrated into the MAAM printer. Print speed has been greatly enhanced. In addition, ORNL and Cosine Additive have worked on alternative designs for a pellet drying and feed system.

  20. Additive operator-difference schemes splitting schemes

    CERN Document Server

    Vabishchevich, Petr N

    2013-01-01

    Applied mathematical modeling isconcerned with solving unsteady problems. This bookshows how toconstruct additive difference schemes to solve approximately unsteady multi-dimensional problems for PDEs. Two classes of schemes are highlighted: methods of splitting with respect to spatial variables (alternating direction methods) and schemes of splitting into physical processes. Also regionally additive schemes (domain decomposition methods)and unconditionally stable additive schemes of multi-component splitting are considered for evolutionary equations of first and second order as well as for sy

  1. Biocompatibility of photopolymers for additive manufacturing

    OpenAIRE

    Leonhardt Stefan; Klare Martin; Scheer Maurice; Fischer Theresa; Cordes Burghard; Eblenkamp Markus

    2016-01-01

    To establish photopolymers for the production of class II or class III medical products by additive manufacturing it is essential to know which components of photopolymeric systems, consisting of monomers, photoinitiators and additives, are the determining factors on their biocompatible properties. In this study the leachable substances of a cured photopolymeric system were eluted and identified by HPLC-MS detection. In addition the cured photopolymer was testes for cytotoxicity and genotoxic...

  2. Harnessing the Potential of Additive Manufacturing

    Science.gov (United States)

    2016-12-01

    31 Defense AT&L: November-December 2016 Harnessing the Potential of Additive Manufacturing Bill Decker Decker is director of Technology...achieve its goal of competition throughout the acquisition life cycle. When we look at additive manufacturing , we have a much different environment. To...Titanium-6 Aluminum-4 Vanadium with Powder Bed Fusion. This specification covers additively manufactured titanium-6 aluminum-4 vanadium (Ti-6Al-4V

  3. Additives in food and their properties

    OpenAIRE

    TYLOVÁ, Kristýna

    2013-01-01

    The aim of this work is to deepen the knowledge about additives in foods, the importance of technological additives in foods, their properties and effects on human health. The aim of this work is a study of technical and scientific literature on the topic: "additives in foods and their properties" and review of the literature. Also in the practical part, implementation and evaluation of a questionnaire survey of the experimental group related to the topic: "Validation and comparison of knowle...

  4. Merits and Demerits of Food Additives

    OpenAIRE

    YANG, Xuening; ZHAN, Yong

    2014-01-01

    Food additive is a double-edged sword. It has merits and demerits. Food additives have such merits as improving sensory properties of foods, preventing deterioration and extending the shelf life, increasing varieties of foods, enhancing convenience of foods, facilitating food processing, and satisfying other demands. However, excessive and illegal use of food additives will exert adverse influence on food security. Therefore, it is required to take proper measures to bring merits of food addi...

  5. Merits and Demerits of Food Additives

    Institute of Scientific and Technical Information of China (English)

    Xuening; YANG; Yong; ZHAN

    2014-01-01

    Food additive is a double-edged sword. It has merits and demerits. Food additives have such merits as improving sensory properties of foods,preventing deterioration and extending the shelf life,increasing varieties of foods,enhancing convenience of foods,facilitating food processing,and satisfying other demands. However,excessive and illegal use of food additives will exert adverse influence on food security.Therefore,it is required to take proper measures to bring merits of food additives into full play,and get rid of their demerits.

  6. Allergic and immunologic reactions to food additives.

    Science.gov (United States)

    Gultekin, Fatih; Doguc, Duygu Kumbul

    2013-08-01

    For centuries, food additives have been used for flavouring, colouring and extension of the useful shelf life of food, as well as the promotion of food safety. During the last 20 years, the studies implicating the additives contained in foods and medicine as a causative factor of allergic reactions have been proliferated considerably. In this review, we aimed to overview all of the food additives which were approved to consume in EU and find out how common and serious allergic reactions come into existence following the consuming of food additives.

  7. 78 FR 34351 - Procurement List; Additions

    Science.gov (United States)

    2013-06-07

    .... ADDRESSES: Committee for Purchase from People Who are Blind or Severely Disabled, 1401 S. Clark Street... COMMITTEE FOR PURCHASE FROM PEOPLE WHO ARE BLIND OR SEVERELY DISABLED Procurement List; Additions AGENCY: Committee for Purchase from People Who are Blind or Severely Disabled. ACTION: Additions to the...

  8. Additive Manufacturing for Low Volume Bearings

    Energy Technology Data Exchange (ETDEWEB)

    Tate, John G. [Schaeffler Group USA, Spartanburg, SC (United States); Richardson, Bradley S. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Love, Lonnie J. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-09-01

    ORNL worked with the Schaeffler Group USA to explore additive manufacturing techniques that might be appropriate for prototyping of bearing cages. Multiple additive manufacturing techniques were investigated, including e-beam, binder jet and multiple laser based processes. The binder jet process worked best for the thin, detailed cages printed.

  9. 48 CFR 1603.7002 - Additional guidelines.

    Science.gov (United States)

    2010-10-01

    ... 48 Federal Acquisition Regulations System 6 2010-10-01 2010-10-01 true Additional guidelines. 1603.7002 Section 1603.7002 Federal Acquisition Regulations System OFFICE OF PERSONNEL MANAGEMENT FEDERAL... OF INTEREST Misleading, Deceptive, or Unfair Advertising 1603.7002 Additional guidelines. Any...

  10. 18 CFR 33.10 - Additional information.

    Science.gov (United States)

    2010-04-01

    ... 18 Conservation of Power and Water Resources 1 2010-04-01 2010-04-01 false Additional information. 33.10 Section 33.10 Conservation of Power and Water Resources FEDERAL ENERGY REGULATORY COMMISSION... § 33.10 Additional information. The Director of the Office of Energy Market Regulation, or his designee...

  11. Additives In Meat and Poultry Products

    Science.gov (United States)

    ... Fact Sheets / Additives in Meat and Poultry Products / Additives in Meat and Poultry Products Z7_0Q0619C0JGR010IFST1G5B10H3 ... Affairs Recalls and Public Health Alerts Regulatory Compliance Regulations, Directives and Notices Rulemaking ...

  12. Feed Additives for Aquaculture and Aquarium Culture

    OpenAIRE

    Barata, Eduardo N.; Velez, Zélia

    2011-01-01

    The presente invention refers of feed additives for aquaculture and aquarium culture. These additives comprise the amino acid, 1-methyl-L-tryptophane, or its isomers with the objective of improving the attractiveness of feeds used in aquaculture and aquaria for fish, as well as other aquatic organisms, under culture conditions. Therefore, this invention has applications in the agriculture-food industry.

  13. 77 FR 41899 - Indirect Food Additives: Polymers

    Science.gov (United States)

    2012-07-17

    ... DEPARTMENT OF HEALTH AND HUMAN SERVICES Food and Drug Administration 21 CFR Part 177 [Docket No. FDA-2012-F-0031] Indirect Food Additives: Polymers AGENCY: Food and Drug Administration, HHS. ACTION... CFR part 177 is amended as follows: PART 177--INDIRECT FOOD ADDITIVES: POLYMERS 0 1. The authority...

  14. Photoactive devices including porphyrinoids with coordinating additives

    Science.gov (United States)

    Forrest, Stephen R; Zimmerman, Jeramy; Yu, Eric K; Thompson, Mark E; Trinh, Cong; Whited, Matthew; Diev, Vlacheslav

    2015-05-12

    Coordinating additives are included in porphyrinoid-based materials to promote intermolecular organization and improve one or more photoelectric characteristics of the materials. The coordinating additives are selected from fullerene compounds and organic compounds having free electron pairs. Combinations of different coordinating additives can be used to tailor the characteristic properties of such porphyrinoid-based materials, including porphyrin oligomers. Bidentate ligands are one type of coordinating additive that can form coordination bonds with a central metal ion of two different porphyrinoid compounds to promote porphyrinoid alignment and/or pi-stacking. The coordinating additives can shift the absorption spectrum of a photoactive material toward higher wavelengths, increase the external quantum efficiency of the material, or both.

  15. Implementation of the Additional Protocol in Japan

    International Nuclear Information System (INIS)

    Ogawa, T.

    2001-01-01

    The Additional Protocol between Japan and the IAEA entered into force in December 1999. To come into force a series of implementation trials of Additional Protocol was carried out at two Japanese representative nuclear research centers, i.e. Tokai Research Establishment of Japan Atomic Energy Research Institute (JAERI) and Oarai Engineering Center of Japan Nuclear Fuel Cycle Development Institute (JNC). These trials were proposed by Japan and were conducted in cooperation with the IAEA Secretariat. In addition, Japan amended 'the Law for the Regulation of Reactors etc.', to collect adequate information to submit to the IAEA, to arrange the surrounding for the complementary access, etc. In addition, Japan Submitted the Initial Declaration of the Additional Protocol within 180 days of the entry into force of the Protocol, in the middle of June, 2000

  16. [Effect of biochar addition on soil evaporation.

    Science.gov (United States)

    Xu, Jian; Niu, Wen Quan; Zhang, Ming Zhi; Li, Yuan; Lyu, Wang; Li, Kang-Yong; Zou, Xiao-Yang; Liang, Bo-Hui

    2016-11-18

    In order to determine the rational amount of biochar application and its effect on soil hydrological processes in arid area, soil column experiments were conducted in the laboratory using three biochar additions (5%, 10% and 15%) and four different biochar types (devaporation. The results showed that the addition of biochar could change the phreatic water recharge, soil water-holding capacity, capillary water upward movement and soil evaporation obviously. But the effects were different depending on the type of biochar raw material and the size of particle. The phreatic water recharge increased with the increasing amount of biochar addition. The addition of biochar could obviously enlarge the soil water-holding capacity and promote the capillary water upward movement rate. This effect was greater when using the material of bamboo charcoal compared with using wood charcoal, while biochar with small particle size had greater impact than that with big particle size. The biochar could effectively restrain the soil evaporation at a low addition amount (5%). But it definitely promoted the soil evaporation if the addition amount was very high. In arid area, biochar addition in appropriate amount could improve soil water retention capacity.

  17. Synthesis and self-assembly behavior of amphiphilic diblock copolymer dextran-block-poly(ε-caprolactone (DEX-b-PCL in aqueous media

    Directory of Open Access Journals (Sweden)

    2010-10-01

    Full Text Available An amphiphilic diblock copolymer, dextran-block-poly(ε-caprolactone (DEX-b-PCL, with a series of welldefined chain lengths of each block was prepared by conjugating a dextran chain with a PCL block via aza-Michael addition reaction under mild conditions. For the dextran block, samples with relatively uniform molecular weight, 3.5 and 6.0 kDa, were used, and the PCL blocks were prepared via ring-opening polymerization at defined ratios of ε-caprolactone to initiator in order to give copolymers with mass fraction of dextran (fDEX ranging from 0.16 to 0.45. When these copolymers were allowed to self-assemble in aqueous solution, the morphology of assembled aggregates varied as a function of fDEX when characterized by transmission electron microscope (TEM, fluorescence microscope (FM and dynamic laser scattering (DLS. As fDEX decreases gradually from 0.45 to 0.16, the morphology of the copolymer assembly changes from spherical micelles to worm-like micelles and eventually to polymersomes, together with an increase in particle sizes.

  18. Graphite and Hybrid Nanomaterials as Lubricant Additives

    Directory of Open Access Journals (Sweden)

    Zhenyu J. Zhang

    2014-04-01

    Full Text Available Lubricant additives, based on inorganic nanoparticles coated with organic outer layer, can reduce wear and increase load-carrying capacity of base oil remarkably, indicating the great potential of hybrid nanoparticles as anti-wear and extreme-pressure additives with excellent levels of performance. The organic part in the hybrid materials improves their flexibility and stability, while the inorganic part is responsible for hardness. The relationship between the design parameters of the organic coatings, such as molecular architecture and the lubrication performance, however, remains to be fully elucidated. A survey of current understanding of hybrid nanoparticles as lubricant additives is presented in this review.

  19. Additional symmetries of supersymmetric KP hierarchies

    International Nuclear Information System (INIS)

    Stanciu, S.

    1993-09-01

    We investigate the additional symmetries of several supersymmetric KP hierarchies: The SKP hierarchy of Manin and Radul, the SKP 2 hierarchy, and the Jacobian SKP hierarchy. The main technical tool is the supersymmetric generalisation of a map originally due to Radul between the Lie algebra of superdifferential operators and the Lie algebra of vector fields on the space of supersymmetric Lax operators. In the case of the Manin-Radul SKP hierarchy we identify additional symmetries which form an algebra isomorphic to a subalgebra of superdifferential operators; whereas in the case of the Jacobian SKP, the (additional) symmetries are identified with the algebra itself. (orig.)

  20. 78 FR 38953 - Procurement List Additions

    Science.gov (United States)

    2013-06-28

    ... Blind or Severely Disabled published notices of proposed additions to the Procurement List. After... Punch, Paper, Desktop, 3-Hole, Adjustable, 11 sheet capacity, Metallic Base, Black Grip. Coverage: A...

  1. 78 FR 12295 - Procurement List; Additions

    Science.gov (United States)

    2013-02-22

    ... published notices of proposed additions to the Procurement List. After consideration of the material..., 508 Compliant, 12 Digit, Portable, Desktop, Battery Operated NPA: MidWest Enterprises for the Blind...

  2. Laser-based additive manufacturing of metals

    CSIR Research Space (South Africa)

    Kumar, S

    2010-11-01

    Full Text Available For making metallic products through Additive Manufacturing (AM) processes, laser-based systems play very significant roles. Laser-based processes such as Selective Laser Melting (SLM) and Laser Engineered Net Shaping (LENS) are dominating processes...

  3. Additively Manufactured Ceramic Rocket Engine Components

    Data.gov (United States)

    National Aeronautics and Space Administration — HRL Laboratories, LLC, with Vector Space Systems (VSS) as subcontractor, has a 24-month effort to develop additive manufacturing technology for reinforced ceramic...

  4. 7 CFR 955.91 - Additional parties.

    Science.gov (United States)

    2010-01-01

    ... Marketing Agreement § 955.91 Additional parties. After the effective date thereof, any handler may become a... Regulations of the Department of Agriculture (Continued) AGRICULTURAL MARKETING SERVICE (Marketing Agreements... then be effective as to such new contracting party. ...

  5. Non-additive measure and integral

    CERN Document Server

    Denneberg, Dieter

    1994-01-01

    Non-Additive Measure and Integral is the first systematic approach to the subject. Much of the additive theory (convergence theorems, Lebesgue spaces, representation theorems) is generalized, at least for submodular measures which are characterized by having a subadditive integral. The theory is of interest for applications to economic decision theory (decisions under risk and uncertainty), to statistics (including belief functions, fuzzy measures) to cooperative game theory, artificial intelligence, insurance, etc. Non-Additive Measure and Integral collects the results of scattered and often isolated approaches to non-additive measures and their integrals which originate in pure mathematics, potential theory, statistics, game theory, economic decision theory and other fields of application. It unifies, simplifies and generalizes known results and supplements the theory with new results, thus providing a sound basis for applications and further research in this growing field of increasing interest. It also co...

  6. Nonparametric additive regression for repeatedly measured data

    KAUST Repository

    Carroll, R. J.; Maity, A.; Mammen, E.; Yu, K.

    2009-01-01

    We develop an easily computed smooth backfitting algorithm for additive model fitting in repeated measures problems. Our methodology easily copes with various settings, such as when some covariates are the same over repeated response measurements

  7. Caustic addition system operability test procedure

    Energy Technology Data Exchange (ETDEWEB)

    Parazin, R.E.

    1994-11-01

    This test procedure provides instructions for performing operational testing of the major components of the 241-AN-107 Caustic Addition System by WHC and Kaiser personnel at the Rotating Equipment Shop run-in pit (Bldg. 272E).

  8. Caustic addition system operability test procedure

    International Nuclear Information System (INIS)

    Parazin, R.E.

    1994-11-01

    This test procedure provides instructions for performing operational testing of the major components of the 241-AN-107 Caustic Addition System by WHC and Kaiser personnel at the Rotating Equipment Shop run-in pit (Bldg. 272E)

  9. 78 FR 40727 - Procurement List; Proposed Additions

    Science.gov (United States)

    2013-07-08

    ... for addition to the Procurement List for production by the nonprofit agencies listed: Products Towel.... 12/BX Cleaner, Brake Parts NSN: 6850-01-167-0678--17 oz. NPA: The Lighthouse for the Blind, St. Louis...

  10. 78 FR 35874 - Procurement List; Proposed Additions

    Science.gov (United States)

    2013-06-14

    ... proposed for addition to the Procurement List for production by the nonprofit agencies listed: Products... Cleaner NPA: Winston-Salem Industries for the Blind, Inc., Winston-Salem, NC Contracting Activity: Defense...

  11. Characterizing Polymer Powders used in Additive Manufacturing

    Energy Technology Data Exchange (ETDEWEB)

    Bajric, Sendin [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-11-16

    These are a set of slides that give the personal background of the author, information about his LANL organization, and information about his internship project at LANL about additive manufacturing and selective laser sintering (SLS).

  12. Additive Manufacturing of Magnesium (Mg) Alloys

    Data.gov (United States)

    National Aeronautics and Space Administration — The proposed work is to investigate additive manufacturing techniques for Mg alloys.  It will leverage off research being conducted at University of Florida and...

  13. 78 FR 9386 - Procurement List; Addition

    Science.gov (United States)

    2013-02-08

    ... Purchase From People Who Are Blind or Severely Disabled published notice of proposed addition to the...: Enterprise Professional Services, Inc., Austin, TX Contracting Activity: Dept of the Army, W40M USA MEDCOM...

  14. 77 FR 55195 - Procurement List; Additions

    Science.gov (United States)

    2012-09-07

    ... Purchase From People Who Are Blind or Severely Disabled published notice of proposed additions to the... Harmon Avenue, Fort Stewart, GA. NPA: Professional Contract Services, Inc., Austin, TX. Contracting...

  15. Additional symmetries of supersymmetric KP hierarchies

    International Nuclear Information System (INIS)

    Stanciu, S.

    1994-01-01

    We investigate the additional symmetries of several supersymmetric KP hierarchies: the SKP hierarchy of Manin and Radul, the SKP 2 hierarchy, and the Jacobian SKP hierarchy. In all three cases we find that the algebra of symmetries is isomorphic to the algebra of superdifferential operators, or equivalently SW 1+∞ . These results seem to suggest that despite their realization depending on the dynamics, the additional symmetries are kinematical in nature. (orig.)

  16. Additive Manufacturing in the Marine Corps

    Science.gov (United States)

    2015-06-01

    TERMS additive manufacturing, 3D printing, improving logistics 15. NUMBER OF PAGES 123 16. PRICE CODE 17. SECURITY CLASSIFICATION OF REPORT...One such method is ultrasonic agglomeration. The process produces compact snack items that are nutrient-dense and shelf-stable. Currently Army...possess outdated technology. Additionally, prices for the printers are dropping significantly.202 Therefore, the Marine Corps will not only have outdated

  17. Finding phosphorus containing additives in manufactured foods

    OpenAIRE

    Lloyd, Lyn; Gillanders, Lyn

    2012-01-01

    Dietary phosphorous (P) intake is associated with an increased serum phosphate level which is a risk factor for cardiovascular disease and increased mortality for people with chronic kidney disease. Dietary restriction of P is an important nutrition intervention as about 50% of daily intake of P is from P–containing food additives. Educating patients on P additives can effectively reduce serum P values over standard care. Avoidance can be achieved by reading the ingredient list to check for o...

  18. Challenges in Additive Manufacturing of Alumina

    OpenAIRE

    Gonzalez, Hugo

    2016-01-01

    Additive manufacturing is seen by many as the holy grail of manufacturing, the ability to produce parts nearly autonomously. Adding material rather than removing it would eliminate the need for expensive resources and machining. The recent expiration of key 3D printing patents has led to many advances in the field and has dramatically lowered the prices of 3D printers, making them accessible to the average individual. The one area where additive manufacturing is still in its infancy is in cer...

  19. Design and additive manufacture for flow chemistry.

    Science.gov (United States)

    Capel, Andrew J; Edmondson, Steve; Christie, Steven D R; Goodridge, Ruth D; Bibb, Richard J; Thurstans, Matthew

    2013-12-07

    We review the use of additive manufacturing (AM) as a novel manufacturing technique for the production of milli-scale reactor systems. Five well-developed additive manufacturing techniques: stereolithography (SL), multi-jet modelling (MJM), selective laser melting (SLM), laser sintering (LS) and fused deposition modelling (FDM) were used to manufacture a number of miniaturised reactors which were tested using a range of organic and inorganic reactions.

  20. Material Database for Additive Manufacturing Techniques

    Science.gov (United States)

    2017-12-01

    components in the field. II. BACKGROUND Additive manufacturing is a rapidly maturing process by which digital 3-D design data are used to build up...improves readiness by offering on-demand low-rate production [8, 9]. 3-D printing also enables rapid design iterations and complexity, which improve...abundant in additive manufacturing , allowing design freedom that is only limited by the material strength requirements. A set of eight conductive

  1. Evaluation of certain food additives and contaminants.

    Science.gov (United States)

    2013-01-01

    This report represents the conclusions of a Joint FAO/WHO Expert Committee convened to evaluate the safety of various food additives and a food contaminant with a view to concluding as to safety concerns and to preparing specifications for identity and purity. The first part of the report contains a general discussion of the principles governing the toxicological evaluation of and assessment of dietary exposure to food additives. A summary follows of the Committee's evaluations of technical, toxicological and dietary exposure data for seven food additives (advantame; glucoamylase from Trichoderma reesei expressed in Trichoderma reesei; glycerol ester of gum rosin; glycerol ester of tall oil rosin; glycerol ester of wood rosin; nisin; and octenyl succinic acid modified gum arabic) and an assessment of dietary exposure to cadmium from cocoa and cocoa products. Specifications for the following food additives were revised: annatto extracts (solvent-extracted bixin and solvent-extracted norbixin); Benzoe tonkinensis; food additives containing aluminium and/or silicon; mineral oil (medium viscosity); modified starches; paprika extract; phosphates (analytical methods for the determination of phosphorus and revision of specifications); 3-phytase from Aspergillus niger expressed in Aspergillus niger; potassium aluminium silicate; and potassium aluminium silicate-based pearlescent pigments. Annexed to the report are tables summarizing the Committee's recommendations for dietary exposures to and toxicological evaluations of the food additives and contaminant considered.

  2. The Development of Korea Additional Protocol System

    International Nuclear Information System (INIS)

    Shim, Hye Won; Yeo, Jin Kyun

    2008-01-01

    The Agreement between the Republic of Korea (ROK) and the IAEA for the Application of Safeguards in Connection with the Treaty on the Non-Proliferation of Nuclear Weapons (the Safeguards Agreement) entered into force on 14 November 1975. The Additional Protocol to the Safeguards Agreement (the Additional Protocol) was signed on 21 June 1999 and entered into force on 19 February 2004. ROK has been submitting annual updated reports of initial declaration on every May 15th since August 2004. Additional protocol reports were submitted through Protocol Reporter provided by IAEA. Annual declarations were simply uploaded and stored in the Accounting Information Treatment System of KINAC, which did not provide data analysis and management function. There have been demands for improvement to handle ever-increasing information. KAPS (Korea Additional Protocol System) has been developed to assist and administrate the additional protocol related works effectively. The new system enables integrated management including composition of additional protocol report and version control, periodical update of related information, results of IAEA complementary access to each facility

  3. Additive effects in radiation grafting and curing

    International Nuclear Information System (INIS)

    Viengkhou, V.; Ng, L.

    1996-01-01

    Full text: Detailed studies on the accelerative effect of novel additives in radiation grafting and curing using acrylated monomer/oligomer systems have been performed in the presence of ionising radiation and UV as sources. Methyl methacrylate (MMA) is used as typical monomer for these grafting studies in the presence of the additives with model backbone polymers, cellulose and propropylene. Additives which have been found to accelerate these grafting processes are: mineral acid, occlusion compounds like urea, thermal initiators and photoinitiators as well as multifunctional monomers such as multifunctional acrylates. The results from irradiation with gamma rays have also been compared with irradiation from a 90W UV lamp. The role of the above additives in accelerating the analogous process of radiation curing has been investigated. Acrylated urethanes, epoxies and polyesters are used as oligomers together with acrylated monomers in this work with uv lamps of 300 watts/inch as radiation source. In the UV curing process bonding between film and substrate is usually due to physical forces. In the present work the presence of additives are shown to influence the occurrence of concurrent grafting during cure thus affecting the nature of the bonding of the cured film. The conditions under which concurrent grafting with UV can occur will be examined. A mechanism for accelerative effect of these additives in both grafting and curing processes has been proposed involving radiation effects and partitioning phenomena

  4. BFR Electrolyte Additive Safety and Flammability Characterization

    Energy Technology Data Exchange (ETDEWEB)

    Allcorn, Eric [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2017-10-13

    Lithium-ion battery safety is a critical issue in the adoption of the chemistry to larger scale applications such as transportation and stationary storage. One of the critical components impacting the safety of lithium-ion batteries is their use of highly flammable organic electrolytes. In this work, brominated flame retardants (BFR’s) – an existing class of flame retardant materials – are incorporated as additives to lithium-ion battery electrolytes with the intention to reduce the electrolyte flammability and thereby improve safety. There are a few critical needs for a successful electrolyte additive: solubility in the electrolyte, electrochemical stability over the range of battery operation, and minimal detrimental effects on battery performance. Those detrimental effects can take the form of electrolyte specific impacts, such as a reduction in conductivity, or electrode impacts, such as SEI-layer modification or chemical instability to the active material. In addition to these needs, the electrolyte additive also needs to achieve its intended purpose, which in this case is to reduce the flammability of the electrolyte. For the work conducted as part of this SPP agreement three separate BFR materials were provided by Albemarle to be tested by Sandia as additives in a traditional lithium-ion battery electrolyte. The provided BFR materials were tribromo-neopentyl alcohol, tetrabromo bisphenol A, and tribromoethylene. These materials were incorporated as separate 4 wt.% additives into a traditional lithium-ion battery electrolyte and compared to said traditional electrolyte, designated Gen2.

  5. Additive manufacturing in production: challenges and opportunities

    Science.gov (United States)

    Ahuja, Bhrigu; Karg, Michael; Schmidt, Michael

    2015-03-01

    Additive manufacturing, characterized by its inherent layer by layer fabrication methodology has been coined by many as the latest revolution in the manufacturing industry. Due to its diversification of Materials, processes, system technology and applications, Additive Manufacturing has been synonymized with terminology such as Rapid prototyping, 3D printing, free-form fabrication, Additive Layer Manufacturing, etc. A huge media and public interest in the technology has led to an innovative attempt of exploring the technology for applications beyond the scope of the traditional engineering industry. Nevertheless, it is believed that a critical factor for the long-term success of Additive Manufacturing would be its ability to fulfill the requirements defined by the traditional manufacturing industry. A parallel development in market trends and product requirements has also lead to a wider scope of opportunities for Additive Manufacturing. The presented paper discusses some of the key challenges which are critical to ensure that Additive Manufacturing is truly accepted as a mainstream production technology in the industry. These challenges would highlight on various aspects of production such as product requirements, process management, data management, intellectual property, work flow management, quality assurance, resource planning, etc. In Addition, changing market trends such as product life cycle, mass customization, sustainability, environmental impact and localized production will form the foundation for the follow up discussion on the current limitations and the corresponding research opportunities. A discussion on ongoing research to address these challenges would include topics like process monitoring, design complexity, process standardization, multi-material and hybrid fabrication, new material development, etc.

  6. Study of zirconium-addition binary systems

    International Nuclear Information System (INIS)

    Wozniakova, B.; Kuchar, L.

    1975-01-01

    The curves are given of the solid and the liquid of binary zirconium-addition systems. Most additions reduce the melting temperature of zirconium. The only known additions to increase the melting temperature are nitrogen, oxygen and hafnium. Also given are the transformation curves of the systems and the elements are given which reduce or raise the temperature of α-β transformation. From the Mendeleev table into which are plotted the curves of the solid and the liquid of binary systems it is possible to predict the properties of unknown binary systems. For the calculations of the curves of the solid and the liquid, 1860 degC was taken as the temperature of zirconium melting. For the calculations of transformation curves, 865 degC was taken as the temperature of α-β transformation. The equations are given of the curves of the solid and the liquid and of the transformation curves of some Zr-addition systems. Also given are the calculated equilibrium distribution coefficients and the equilibrium distribution coefficients of the transformation of additions in Zr and their limit values for temperatures approximating the melting point or the temperature of the transformation of pure Zr, and the values pertaining to eutectic and peritectic or eutectoid and peritectoid temperatures. (J.B.)

  7. Laser polishing of additive manufactured Ti alloys

    Science.gov (United States)

    Ma, C. P.; Guan, Y. C.; Zhou, W.

    2017-06-01

    Laser-based additive manufacturing has attracted much attention as a promising 3D printing method for metallic components in recent years. However, surface roughness of additive manufactured components has been considered as a challenge to achieve high performance. In this work, we demonstrate the capability of fiber laser in polishing rough surface of additive manufactured Ti-based alloys as Ti-6Al-4V and TC11. Both as-received surface and laser-polished surfaces as well as cross-section subsurfaces were analyzed carefully by White-Light Interference, Confocal Microscope, Focus Ion Beam, Scanning Electron Microscopy, Energy Dispersive Spectrometer, and X-ray Diffraction. Results revealed that as-received Ti-based alloys with surface roughness more than 5 μm could be reduce to less than 1 μm through laser polishing process. Moreover, microstructure, microhardness and wear resistance of laser-polished zone was investigated in order to examine the thermal effect of laser polishing processing on the substrate of additive manufactured Ti alloys. This proof-of-concept process has the potential to effectively improve the surface roughness of additive manufactured metallic alloy by local polishing method without damage to the substrate.

  8. Terminal addition in a cellular world.

    Science.gov (United States)

    Torday, J S; Miller, William B

    2018-07-01

    Recent advances in our understanding of evolutionary development permit a reframed appraisal of Terminal Addition as a continuous historical process of cellular-environmental complementarity. Within this frame of reference, evolutionary terminal additions can be identified as environmental induction of episodic adjustments to cell-cell signaling patterns that yield the cellular-molecular pathways that lead to differing developmental forms. Phenotypes derive, thereby, through cellular mutualistic/competitive niche constructions in reciprocating responsiveness to environmental stresses and epigenetic impacts. In such terms, Terminal Addition flows according to a logic of cellular needs confronting environmental challenges over space-time. A reconciliation of evolutionary development and Terminal Addition can be achieved through a combined focus on cell-cell signaling, molecular phylogenies and a broader understanding of epigenetic phenomena among eukaryotic organisms. When understood in this manner, Terminal Addition has an important role in evolutionary development, and chronic disease might be considered as a form of 'reverse evolution' of the self-same processes. Copyright © 2017. Published by Elsevier Ltd.

  9. Non-additive Effects in Genomic Selection

    Directory of Open Access Journals (Sweden)

    Luis Varona

    2018-03-01

    Full Text Available In the last decade, genomic selection has become a standard in the genetic evaluation of livestock populations. However, most procedures for the implementation of genomic selection only consider the additive effects associated with SNP (Single Nucleotide Polymorphism markers used to calculate the prediction of the breeding values of candidates for selection. Nevertheless, the availability of estimates of non-additive effects is of interest because: (i they contribute to an increase in the accuracy of the prediction of breeding values and the genetic response; (ii they allow the definition of mate allocation procedures between candidates for selection; and (iii they can be used to enhance non-additive genetic variation through the definition of appropriate crossbreeding or purebred breeding schemes. This study presents a review of methods for the incorporation of non-additive genetic effects into genomic selection procedures and their potential applications in the prediction of future performance, mate allocation, crossbreeding, and purebred selection. The work concludes with a brief outline of some ideas for future lines of that may help the standard inclusion of non-additive effects in genomic selection.

  10. Additive Manufacturing of Metastable Beta Titanium Alloys

    Science.gov (United States)

    Yannetta, Christopher J.

    Additive manufacturing processes of many alloys are known to develop texture during the deposition process due to the rapid reheating and the directionality of the dissipation of heat. Titanium alloys and with respect to this study beta titanium alloys are especially susceptible to these effects. This work examines Ti-20wt%V and Ti-12wt%Mo deposited under normal additive manufacturing process parameters to examine the texture of these beta-stabilized alloys. Both microstructures contained columnar prior beta grains 1-2 mm in length beginning at the substrate with no visible equiaxed grains. This microstructure remained constant in the vanadium system throughout the build. The microstructure of the alloy containing molybdenum changed from a columnar to an equiaxed structure as the build height increased. Eighteen additional samples of the Ti-Mo system were created under different processing parameters to identify what role laser power and travel speed have on the microstructure. There appears to be a correlation in alpha lath size and power density. The two binary alloys were again deposited under the same conditions with the addition of 0.5wt% boron to investigate the effects an insoluble interstitial alloying element would have on the microstructure. The size of the prior beta grains in these two alloys were reduced with the addition of boron by approximately 50 (V) and 100 (Mo) times.

  11. Fuel and Additive Characterization for HCCI Combustion

    International Nuclear Information System (INIS)

    Aceves, S M; Flowers, D; Martinez-Frias, J; Espinosa-Loza, F; Pitz, W J; Dibble, R

    2003-01-01

    This paper shows a numerical evaluation of fuels and additives for HCCl combustion. First, a long list of candidate HCCl fuels is selected. For all the fuels in the list, operating conditions (compression ratio, equivalence ratio and intake temperature) are determined that result in optimum performance under typical operation for a heavy-duty engine. Fuels are also characterized by presenting Log(p)-Log(T) maps for multiple fuels under HCCl conditions. Log(p)-Log(T) maps illustrate important processes during HCCl engine operation, including compression, low temperature heat release and ignition. Log(p)-Log(T) diagrams can be used for visualizing these processes and can be used as a tool for detailed analysis of HCCl combustion. The paper also includes a ranking of many potential additives. Experiments and analyses have indicated that small amounts (a few parts per million) of secondary fuels (additives) may considerably affect HCCl combustion and may play a significant role in controlling HCCl combustion. Additives are ranked according to their capability to advance HCCl ignition. The best additives are listed and an explanation of their effect on HCCl combustion is included

  12. Excessive Additive Effect On Engine Oil Viscosity

    Directory of Open Access Journals (Sweden)

    Vojtěch Kumbár

    2014-01-01

    Full Text Available The main goal of this paper is excessive additive (for oil filling effect on engine oil dynamic viscosity. Research is focused to commercially distribute automotive engine oil with viscosity class 15W–40 designed for vans. There were prepared blends of new and used engine oil without and with oil additive in specific ratio according manufacturer’s recommendations. Dynamic viscosity of blends with additive was compared with pure new and pure used engine oil. The temperature dependence dynamic viscosity of samples was evaluated by using rotary viscometer with standard spindle. Concern was that the oil additive can moves engine oil of several viscosity grades up. It is able to lead to failure in the engine. Mathematical models were used for fitting experimental values of dynamic viscosity. Exponential fit function was selected, which was very accurate because the coefficient of determination R2 achieved high values (0.98–0.99. These models are able to predict viscosity behaviour blends of engine oil and additive.

  13. Biocompatibility of photopolymers for additive manufacturing

    Directory of Open Access Journals (Sweden)

    Leonhardt Stefan

    2016-09-01

    Full Text Available To establish photopolymers for the production of class II or class III medical products by additive manufacturing it is essential to know which components of photopolymeric systems, consisting of monomers, photoinitiators and additives, are the determining factors on their biocompatible properties. In this study the leachable substances of a cured photopolymeric system were eluted and identified by HPLC-MS detection. In addition the cured photopolymer was testes for cytotoxicity and genotoxicity according to DIN EN ISO 10993 for long time applications. The results showed that uncured residual monomers are the determining factor on the biocompatible properties of the photopolymeric system. Strategies to reduce these residual monomers in the cured photopolymer are presented.

  14. Non-additive measures theory and applications

    CERN Document Server

    Narukawa, Yasuo; Sugeno, Michio; 9th International Conference on Modeling Decisions for Artificial Intelligence (MDAI 2012)

    2014-01-01

    This book provides a comprehensive and timely report in the area of non-additive measures and integrals. It is based on a panel session on fuzzy measures, fuzzy integrals and aggregation operators held during the 9th International Conference on Modeling Decisions for Artificial Intelligence (MDAI 2012) in Girona, Spain, November 21-23, 2012. The book complements the MDAI 2012 proceedings book, published in Lecture Notes in Computer Science (LNCS) in 2012. The individual chapters, written by key researchers in the field, cover fundamental concepts and important definitions (e.g. the Sugeno integral, definition of entropy for non-additive measures) as well some important applications (e.g. to economics and game theory) of non-additive measures and integrals. The book addresses students, researchers and practitioners working at the forefront of their field.  

  15. Additive Manufacturing of Shape Memory Alloys

    Science.gov (United States)

    Van Humbeeck, Jan

    2018-04-01

    Selective Laser Melting (SLM) is an additive manufacturing production process, also called 3D printing, in which functional, complex parts are produced by selectively melting patterns in consecutive layers of powder with a laser beam. The pattern the laser beam is following is controlled by software that calculates the pattern by slicing a 3D CAD model of the part to be constructed. Apart from SLM, also other additive manufacturing techniques such as EBM (Electron Beam Melting), FDM (Fused Deposition Modelling), WAAM (Wire Arc Additive Manufacturing), LENS (Laser Engineered Net Shaping such as Laser Cladding) and binder jetting allow to construct complete parts layer upon layer. But since more experience of AM of shape memory alloys is collected by SLM, this paper will overview the potentials, limits and problems of producing NiTi parts by SLM.

  16. Effects from additives on deacetylation of chitin

    International Nuclear Information System (INIS)

    Campana Filho, Sergio P.; Signini, Roberta

    2001-01-01

    Deacetylation reactions of commercial chitin were carried out in aqueous sodium hydroxide solution at 115 deg C for 6 hours. The effect from additives (sodium borohydride or anthraquinone) and of bubbling inert gas (nitrogen or argon) on the characteristics of deacetylated samples were evaluated. Average degrees of acetylation and intrinsic viscosity were determined by 1 H NMR spectroscopy and capillary viscometry, respectively. X-ray diffraction was employed to evaluate changes in crystallinity and infrared spectroscopy was used to monitor structural changes due to deacetylation. The bubbling of inert gas during the deacetylation reaction resulted in more crystalline samples of chitosan. Deacetylation carried out without any additive produced slightly more deacetylated chitosan but they were severely depolymerized. The depolymerization process was much less important when sodium borohydride was added to the reaction medium but the addition of anthraquinone and the bubbling of nitrogen, or argon, did not have any effect, this suggests that oxygen is not required for depolymerization. (author)

  17. Additive Construction with Mobile Emplacement (ACME)

    Science.gov (United States)

    Vickers, John

    2015-01-01

    The Additive Construction with Mobile Emplacement (ACME) project is developing technology to build structures on planetary surfaces using in-situ resources. The project focuses on the construction of both 2D (landing pads, roads, and structure foundations) and 3D (habitats, garages, radiation shelters, and other structures) infrastructure needs for planetary surface missions. The ACME project seeks to raise the Technology Readiness Level (TRL) of two components needed for planetary surface habitation and exploration: 3D additive construction (e.g., contour crafting), and excavation and handling technologies (to effectively and continuously produce in-situ feedstock). Additionally, the ACME project supports the research and development of new materials for planetary surface construction, with the goal of reducing the amount of material to be launched from Earth.

  18. Evaluation of Advanced Polymers for Additive Manufacturing

    Energy Technology Data Exchange (ETDEWEB)

    Rios, Orlando [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Carter, William G. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Kutchko, Cindy [PPG Industries, Pittsburgh, PA (United States); Fenn, David [PPG Industries, Pittsburgh, PA (United States); Olson, Kurt [PPG Industries, Pittsburgh, PA (United States)

    2017-09-08

    The goal of this Manufacturing Demonstration Facility (MDF) technical collaboration project between Oak Ridge National Laboratory (ORNL) and PPG Industries, Inc. (PPG) was to evaluate the feasibility of using conventional coatings chemistry and technology to build up material layer-by-layer. The PPG-ORNL study successfully demonstrated that polymeric coatings formulations may overcome many limitations of common thermoplastics used in additive manufacturing (AM), allow lightweight nozzle design for material deposition, and increase build rate. The materials effort focused on layer-by-layer deposition of coatings with each layer fusing together. The combination of materials and deposition results in an additively manufactured build that has sufficient mechanical properties to bear the load of additional layers, yet is capable of bonding across the z-layers to improve build direction strength. The formulation properties were tuned to enable a novel, high-throughput deposition method that is highly scalable, compatible with high loading of reinforcing fillers, and inherently low-cost.

  19. Transfer of Training in Simple Addition.

    Science.gov (United States)

    Chen, Yalin; Campbell, Jamie I D

    2017-04-18

    In recent years several researchers have proposed that skilled adults may solve single-digit addition problems (e.g. 3 + 1 = 4, 4 + 3 = 7) using a fast counting procedure. Practicing a procedure, often leads to transfer of learning and faster performance of unpracticed items. Such transfer has been demonstrated using a counting-based alphabet arithmetic task (e.g., B + 4 = C D E F) that indicated robust generalization of practice (i.e., RT gains) when untrained transfer problems at test had been implicitly practiced (e.g., practice B + 3, test B + 2 or B + 1). Here we constructed analogous simple addition problems (practice 4 + 3, test 4 + 2 or 4 + 1). In each of three experiments (total n = 108) participants received six practice blocks followed by two test blocks of new problems to examine generalization effects. Practice of addition identity-rule problems (i.e., 0 + N = N) showed complete transfer of RT gains made during practice to unpracticed items at test. In contrast, the addition ties (2 + 2, 3 + 3, etc.) presented large RT costs for unpracticed problems at test, but sped up substantially in the second test block. This pattern is consistent with item-specific strengthening of associative memory. The critical items were small non-tie additions (sum ≤ 10) for which the test problems would be implicitly practiced if counting was employed during practice. In all three experiments (and collectively) there was no evidence of generalization for these items in the first test block, but there was robust speed up when the items were repeated in the second test block. Thus, there was no evidence of the generalization of practice that would be expected if counting procedures mediated our participants' performance on small non-tie addition problems.

  20. Studies of alumina additions in zirconia - magnesia

    International Nuclear Information System (INIS)

    Muccillo, R.

    1987-01-01

    Ionic conductivity measurements have been carried out in the 500 0 C - 1000 0 C temperature range in Mg - PSZ (Partially Stabilized Zirconia) with 0.5 to 10 mol % alumina additions. All specimens were prepared by pressing followed by pre - and sintering at 1000 0 C/2h and1450 0 C/4h, respectively. Thermal histerysis of the ionic conductivity have been detected, probably due to phase changes in the Mg-PSZ samples. The results show that alumina additions up to 2.1% enhances densification with no major variations in electrical resistivity values. (Author) [pt

  1. Effusion plate using additive manufacturing methods

    Science.gov (United States)

    Johnson, Thomas Edward; Keener, Christopher Paul; Ostebee, Heath Michael; Wegerif, Daniel Gerritt

    2016-04-12

    Additive manufacturing techniques may be utilized to construct effusion plates. Such additive manufacturing techniques may include defining a configuration for an effusion plate having one or more internal cooling channels. The manufacturing techniques may further include depositing a powder into a chamber, applying an energy source to the deposited powder, and consolidating the powder into a cross-sectional shape corresponding to the defined configuration. Such methods may be implemented to construct an effusion plate having one or more channels with a curved cross-sectional geometry.

  2. Photogrammetry for Repositioning in Additive Manufacturing

    DEFF Research Database (Denmark)

    Jensen, Janus Nørtoft; Lyngby, Rasmus Ahrenkiel; Aanæs, Henrik

    2017-01-01

    In this preliminary work, we present our current status on how to use single camera photogrammetry to determine the orientation of an additively manufactured partly finished object that has been repositioned in the printing chamber, from a single image taken with a calibrated camera, and comparing...... this to the CAD model of the object. We describe how this knowledge can be used to update the machine code of the printer such that printing of the object can be resumed in the new location. This opens possibilities for embedding and assembling foreign parts into the additive manufacturing pipeline, adding...

  3. The structure of additive conservation laws

    International Nuclear Information System (INIS)

    Helmut Reen

    1979-01-01

    All additive conserved quantities are listed for a system with short range central force interaction between the particles: a special case shows up in Boltzmann H-theorem and his derivation of the Maxwell velocity distribution. It is concluded that in classical mechanics of mass points there are no other additive conservation laws besides of energy, momentum, angular momentum and center of mass motion. A generator is considered of a symmetry transformation defined as integral over a conserved local current density where the latter, in general, needs not be covariant under translations

  4. 77 FR 13009 - Regulation of Fuels and Fuel Additives: Identification of Additional Qualifying Renewable Fuel...

    Science.gov (United States)

    2012-03-05

    ... Regulation of Fuels and Fuel Additives: Identification of Additional Qualifying Renewable Fuel Pathways Under the Renewable Fuel Standard Program AGENCY: Environmental Protection Agency (EPA). ACTION: Withdrawal... Renewable Fuel Standard program regulations. Because EPA received adverse comment, we are withdrawing the...

  5. 42 CFR 86.20 - Additional conditions.

    Science.gov (United States)

    2010-10-01

    ... 42 Public Health 1 2010-10-01 2010-10-01 false Additional conditions. 86.20 Section 86.20 Public Health PUBLIC HEALTH SERVICE, DEPARTMENT OF HEALTH AND HUMAN SERVICES OCCUPATIONAL SAFETY AND HEALTH RESEARCH AND RELATED ACTIVITIES GRANTS FOR EDUCATION PROGRAMS IN OCCUPATIONAL SAFETY AND HEALTH Occupational Safety and Health Training Grants § 86.2...

  6. 17 CFR 37.7 - Additional requirements.

    Science.gov (United States)

    2010-04-01

    ... 17 Commodity and Securities Exchanges 1 2010-04-01 2010-04-01 false Additional requirements. 37.7 Section 37.7 Commodity and Securities Exchanges COMMODITY FUTURES TRADING COMMISSION DERIVATIVES... of section 5c(c) of the Act and § 40.2 of this chapter, derivatives transaction execution facilities...

  7. Additional reactor protection system of RBMK-1500

    International Nuclear Information System (INIS)

    1999-01-01

    Analysis of anticipated transients without scram of RBMK-1500 reactor showed that additional reactor protection system is required. Data of accident analysis in the case of loose of external electric power and loose of vacuum in condensers of turbines are provided

  8. Neue Werkstoffe über additive Fertigung

    OpenAIRE

    Günther, Johannes; Niendorf, Thomas

    2016-01-01

    Über die additive Fertigung, oftmals bezeichnet als 3D-Druck, lassen sich Bauteile nahezu beliebiger geometrischer Komplexität herstellen. Gleichzeitig lassen die Prozessrandbedingungen die direkte Einstellung der Mikrostruktur in den verwendeten metallischen Werkstoffen zu. Hieraus ergeben sich weitreichende Möglichkeiten bezüglich der Eigenschaftsoptimierung aktueller Hochleistungswerkstoffe.

  9. Additive Manufacturing of Biomaterials, Tissues, and Organs

    NARCIS (Netherlands)

    Zadpoor, Amir A; Malda, Jos

    2017-01-01

    The introduction of additive manufacturing (AM), often referred to as three-dimensional (3D) printing, has initiated what some believe to be a manufacturing revolution, and has expedited the development of the field of biofabrication. Moreover, recent advances in AM have facilitated further

  10. Additive Manufacturing of Biomaterials, Tissues, and Organs

    NARCIS (Netherlands)

    Zadpoor, Amir A; Malda, Jos|info:eu-repo/dai/nl/412461099

    The introduction of additive manufacturing (AM), often referred to as three-dimensional (3D) printing, has initiated what some believe to be a manufacturing revolution, and has expedited the development of the field of biofabrication. Moreover, recent advances in AM have facilitated further

  11. Probabilistic fuzzy systems as additive fuzzy systems

    NARCIS (Netherlands)

    Almeida, R.J.; Verbeek, N.; Kaymak, U.; Costa Sousa, da J.M.; Laurent, A.; Strauss, O.; Bouchon-Meunier, B.; Yager, R.

    2014-01-01

    Probabilistic fuzzy systems combine a linguistic description of the system behaviour with statistical properties of data. It was originally derived based on Zadeh’s concept of probability of a fuzzy event. Two possible and equivalent additive reasoning schemes were proposed, that lead to the

  12. Leaching of Plastic Additives to Marine Organisms

    NARCIS (Netherlands)

    Koelmans, A.A.; Besseling, E.; Foekema, E.M.

    2014-01-01

    It is often assumed that ingestion of microplastics by aquatic species leads to increased exposure to plastic additives. However, experimental data or model based evidence is lacking. Here we assess the potential of leaching of nonylphenol (NP) and bisphenol A (BPA) in the intestinal tracts of

  13. Overview of Food Ingredients, Additives and Colors

    Science.gov (United States)

    ... In addition to maintaining the quality of the food, they help control contamination that can cause foodborne illness, including life-threatening ... still be considered safe. Regulations known as Good Manufacturing ... limit the amount of food ingredients used in foods to the amount necessary ...

  14. Polymeric additive performance in closed whitewater systems

    Science.gov (United States)

    T. H. Wegner

    1984-01-01

    “With more stringent requirements on discharge water quality and with escalating water treatment costs, water recycling within the paper mill is of growing importance. A serious problem resulting from more white-water recycling is reduced drainage and fiber or fines retention because of diminished polymeric additive performance. To provide better insight for overcoming...

  15. 76 FR 80345 - Procurement List; Additions

    Science.gov (United States)

    2011-12-23

    ... ARMY, W6QL ECC MIAMI DIV, MIAMI, FL. Service Type/Location: Industrial Laundry Service, Bureau of... Procurement List. SUMMARY: This action adds services to the Procurement List that will be provided by... concerning capability of qualified nonprofit agencies to provide the services and impact of the additions on...

  16. 78 FR 48656 - Procurement List; Proposed Additions

    Science.gov (United States)

    2013-08-09

    ... Oceanic and Atmospheric Administration, Boulder, CO. Service Type/Location: Laundry Service, US Coast... Additions to the Procurement List. SUMMARY: The Committee is proposing to add products and services to the... required to procure the products and services listed below from nonprofit agencies employing persons who...

  17. 77 FR 27736 - Procurement List Additions

    Science.gov (United States)

    2012-05-11

    ... Research Laboratory, Washington, DC. Service Type/Location: Laundry, Refurbishment, and Warehouse Services... Procurement List. SUMMARY: This action adds products and services to the Procurement List that will be... products and services and impact of the additions on the current or most recent contractors, the Committee...

  18. 77 FR 29596 - Procurement List Proposed Additions

    Science.gov (United States)

    2012-05-18

    .../Location: Laundry Service, Veterans Administration Medical Center (VAMC), (offsite: 1809 W 2nd Avenue... Additions to the Procurement List. SUMMARY: The Committee is proposing to add products and services to the... identified in this notice will be required to procure the products and services listed below from nonprofit...

  19. 75 FR 14576 - Procurement List Additions

    Science.gov (United States)

    2010-03-26

    ... Inspection Service, Minneapolis, MN. M.R. Laundry Products NSN: MR 1103--Heavy Duty Laundry Bag. NSN: MR 1104... procurement list. SUMMARY: This action adds to the Procurement List products and services to be furnished by... products and services and impact of the additions on the current or most recent contractors, the Committee...

  20. Powder Characterization and Optimization for Additive Manufacturing

    NARCIS (Netherlands)

    Cordova, Laura; Campos, Mónica; Tinga, Tiedo

    2017-01-01

    Achieving the optimal quality for Additive Manufactured (AM) parts does not only depend on setting the right process parameters. Material feedstock also plays an important role when aiming for high performance products. The metal AM processes that are most applicable to industry, Powder Bed Fusion

  1. Augmented Reality Interfaces for Additive Manufacturing

    DEFF Research Database (Denmark)

    Eiríksson, Eyþór Rúnar; Pedersen, David Bue; Frisvad, Jeppe Revall

    2017-01-01

    This paper explores potential use cases for using augmented reality (AR) as a tool to operate industrial machines. As a baseline we use an additive manufacturing system, more commonly known as a 3D printer. We implement novel augmented interfaces and controls using readily available open source...

  2. Designing for Color in Additive Manufacturing

    DEFF Research Database (Denmark)

    Eiríksson, Eyþór Rúnar; Luongo, Andrea; Frisvad, Jeppe Revall

    2016-01-01

    In this paper we present a color design pipeline for 3D printed or additively manufactured parts. We demonstrate how to characterize and calibrate a commercial printer and how to obtain its forward and backward color transformation models. We present results from our assistive color design tool...

  3. Additive Manufacturing: From Rapid Prototyping to Flight

    Science.gov (United States)

    Prater, Tracie

    2015-01-01

    Additive manufacturing (AM) offers tremendous promise for the rocket propulsion community. Foundational work must be performed to ensure the safe performance of AM parts. Government, industry, and academia must collaborate in the characterization, design, modeling, and process control to accelerate the certification of AM parts for human-rated flight.

  4. Predicting Color Output of Additive Manufactured Parts

    DEFF Research Database (Denmark)

    Eiríksson, Eyþór Rúnar; Pedersen, David Bue; Aanæs, Henrik

    2015-01-01

    In this paper we address the colorimetric performance of a multicolor additive manufacturing process. A method on how to measure and characterize color performance of said process is presented. Furthermore, a method on predicting the color output is demonstrated, allowing for previsualization...

  5. 78 FR 53734 - Procurement List; Proposed Additions

    Science.gov (United States)

    2013-08-30

    ...: Committee for Purchase From People Who Are Blind or Severely Disabled, 1401 S Clark Street, Suite 10800... COMMITTEE FOR PURCHASE FROM PEOPLE WHO ARE BLIND OR SEVERELY DISABLED Procurement List; Proposed Additions AGENCY: Committee for Purchase From People Who Are Blind or Severely Disabled. ACTION: Proposed...

  6. 78 FR 77105 - Procurement List; Proposed Addition

    Science.gov (United States)

    2013-12-20

    ... People Who Are Blind or Severely Disabled, 1401 S. Clark Street, Suite 10800, Arlington, Virginia, 22202... COMMITTEE FOR PURCHASE FROM PEOPLE WHO ARE BLIND OR SEVERELY DISABLED Procurement List; Proposed Addition AGENCY: Committee for Purchase From People Who Are Blind or Severely Disabled. ACTION: Proposed...

  7. 78 FR 50040 - Procurement List, Proposed Additions

    Science.gov (United States)

    2013-08-16

    ... People Who Are Blind or Severely Disabled, 1401 S Clark Street, Suite 10800, Arlington, Virginia, 22202... COMMITTEE FOR PURCHASE FROM PEOPLE WHO ARE BLIND OR SEVERELY DISABLED Procurement List, Proposed Additions AGENCY: Committee for Purchase From People Who Are Blind or Severely Disabled. ACTION: Proposed...

  8. 78 FR 19248 - Procurement List; Proposed Addition

    Science.gov (United States)

    2013-03-29

    ... Purchase From People Who Are Blind or Severely Disabled, 1401 S. Clark Street, Suite 10800, Arlington... COMMITTEE FOR PURCHASE FROM PEOPLE WHO ARE BLIND OR SEVERELY DISABLED Procurement List; Proposed Addition AGENCY: Committee for Purchase From People Who Are Blind or Severely Disabled. ACTION: Proposed...

  9. Power transformer additional load losses separation procedure

    Directory of Open Access Journals (Sweden)

    Kostić Miloje M.

    2011-01-01

    Full Text Available The proposed procedure is based on the fact that total transformer losses (PLL1,n, determined by short circuit test, can be separated into two components: the eddy current losses in the windings (PEC1,n and stray flux losses (PSL1,n in iron parts of construction as well as in the transformer tank walls. The total additional load losses, PLLd1 and PLLdh, are determined by short circuit test results, conducted at rated frequency (f1 and at increased harmonic frequency (fh=h*f1. Using so obtained total additional load losses, PLLd1 and PLLdh, which can be expressed in the form PLLdh=PEC1,n*h2 + PSL1,n*h, the corresponding rate additional load losses values PEC1,n and PSL1,n are derived. At the end, for given load with predefined high harmonics content, (Ih/I1n, relative to rated current, the total additional load losses value ΣPLLdh > PLLd1, is found. In such a way all harmonics up to hmax are taken into account.

  10. 19 CFR 191.103 - Additional requirements.

    Science.gov (United States)

    2010-04-01

    ... which the alcohol was withdrawn; (iv) Date of withdrawal; (v) Serial number of the tax-paid stamp or... 19 Customs Duties 2 2010-04-01 2010-04-01 false Additional requirements. 191.103 Section 191.103 Customs Duties U.S. CUSTOMS AND BORDER PROTECTION, DEPARTMENT OF HOMELAND SECURITY; DEPARTMENT OF THE...

  11. Acid Rain Analysis by Standard Addition Titration.

    Science.gov (United States)

    Ophardt, Charles E.

    1985-01-01

    The standard addition titration is a precise and rapid method for the determination of the acidity in rain or snow samples. The method requires use of a standard buret, a pH meter, and Gran's plot to determine the equivalence point. Experimental procedures used and typical results obtained are presented. (JN)

  12. Additivity properties of a Gaussian channel

    International Nuclear Information System (INIS)

    Giovannetti, Vittorio; Lloyd, Seth

    2004-01-01

    The Amosov-Holevo-Werner conjecture implies the additivity of the minimum Renyi entropies at the output of a channel. The conjecture is proven true for all Renyi entropies of integer order greater than two in a class of Gaussian bosonic channel where the input signal is randomly displaced or where it is coupled linearly to an external environment

  13. Finding phosphorus containing additives in manufactured foods

    Directory of Open Access Journals (Sweden)

    Lyn Lloyd

    2012-06-01

    This reflects manufactured foods in NZ and it is likely that these results could be generalized to countries with similar food patterns and supplies. Quantitative data in manufactured foods is unlikely to be available to guide patient choice so qualitative information of where to find P additives can be helpful.

  14. ADHD Diet: Do Food Additives Cause Hyperactivity?

    Science.gov (United States)

    ... 3 fatty acids found in certain types of fish, flaxseed and other foods. With David C. Agerter, M.D Food colours and hyperactivity. NHS Choices. http://www.nhs.uk/conditions/food-additive-intolerance/Pages/Introduction.aspx. Accessed Sept. 18, 2017. ...

  15. Additivity of quark masses in gauge theories

    International Nuclear Information System (INIS)

    Scadron, M.D.

    1987-01-01

    It is shown that, in spite of the confinement of quarks in (color-singlet) hadrons, effective quark masses of all types (dynamically generated, constituent and current masses), naturally form hadron masses in an additivity fashion. For the purposes of brevity, the discussion is limited primarily to the nonstrange flavor sector

  16. 76 FR 57719 - Procurement List; Proposed Additions

    Science.gov (United States)

    2011-09-16

    ... proposed for addition to the Procurement List for production by the nonprofit agencies listed: Products NSN: 7930-00-NIB-0583--Refills, Bathroom Cleaner and Deodorizer, Cartridge Concentrate. NSN: 7930-00-NIB-0584--Starter Kit, Bathroom Cleaner and Deodorizer, Cartridge Concentrate. NSN: 7930-00-NIB-0585...

  17. 78 FR 12296 - Procurement List; Proposed Additions

    Science.gov (United States)

    2013-02-22

    ... services are proposed for addition to the Procurement List for production by the nonprofit agencies listed... and Trailer Wash, 55 GL NSN: 7930-00-NIB-0649--Cleaner/Degreaser, Heavy Duty, Biodegradable, Car and Trucks, 5 GL NSN: 7930-00-NIB-0650--Cleaner/Degreaser, Heavy Duty, Biodegradable, Car and Trucks, 55 GL...

  18. Additive manufacturing: From implants to organs

    African Journals Online (AJOL)

    Additive manufacturing (AM) constructs 3D objects layer by layer under computer control from 3D models. 3D printing is one ... anatomical models for surgery planning, and design and construction ... production of implants, particularly to replace bony structures, is ... Manufactured organs are, however, an elusive goal.

  19. Application of Natural Mineral Additives in Construction

    Science.gov (United States)

    Linek, Malgorzata; Nita, Piotr; Wolka, Paweł; Zebrowski, Wojciech

    2017-12-01

    The article concerns the idea of using selected mineral additives in the pavement quality concrete composition. The basis of the research paper was the modification of cement concrete intended for airfield pavements. The application of the additives: metakaolonite and natural zeolite was suggested. Analyses included the assessment of basic physical properties of modifiers. Screening analysis, assessment of micro structure and chemical microanalysis were conducted in case of these materials. The influence of the applied additives on the change of concrete mix parameters was also presented. The impact of zeolite and metakaolinite on the mix density, oxygen content and consistency class was analysed. The influence of modifiers on physical and mechanical changes of the hardened cement concrete was discussed (concrete density, compressive strength and bending strength during fracturing) in diversified research periods. The impact of the applied additives on the changes of internal structure of cement concrete was discussed. Observation of concrete micro structure was conducted using the scanning electron microscope. According to the obtained lab test results, parameters of the applied modifiers and their influence on changes of internal structure of cement concrete are reflected in the increase of mechanical properties of pavement quality concrete. The increase of compressive and bending strength in case of all analysed research periods was proved.

  20. 76 FR 43988 - Procurement List; Additions

    Science.gov (United States)

    2011-07-22

    ... this work, based on applicable experience. Finally, the purpose of the JWOD Act and the responsibility... COMMITTEE FOR PURCHASE FROM PEOPLE WHO ARE BLIND OR SEVERELY DISABLED Procurement List; Additions... Procurement List. SUMMARY: This action adds products and services to the Procurement List that will be...

  1. 7 CFR 1735.18 - Additional equity.

    Science.gov (United States)

    2010-01-01

    ... AGRICULTURE GENERAL POLICIES, TYPES OF LOANS, LOAN REQUIREMENTS-TELECOMMUNICATIONS PROGRAM Loan Purposes and Basic Policies § 1735.18 Additional equity. If determined by the Administrator to be necessary for loan security, a borrower applying for an initial loan shall increase its net worth as a percentage of assets to...

  2. Sintering of magnesia: effect of additives

    Indian Academy of Sciences (India)

    Effect of different additives, namely Cr2O3, Fe2O3 and TiO2, up to 2 wt% was studied on the sinter- ing and .... mental distribution of the components is shown in figure 7. It shows ... Chiang Y M, Birniand D and Kingery W 1996 Physical ceram-.

  3. 77 FR 34026 - Procurement List; Proposed Additions

    Science.gov (United States)

    2012-06-08

    ... provide interested persons an opportunity to submit comments on the proposed actions. Additions If the..., Department of Homeland Security (DHS), Immigration and Customs Enforcement (ICE), Office of Chief Counsel... Institute, Inc., San Antonio, TX. Contracting Activity: Department of Homeland Security, U.S. Immigration...

  4. (ajst) additive main effects and multiplicative

    African Journals Online (AJOL)

    2013-08-02

    Aug 2, 2013 ... genotypes assessed by biplot analysis showed that the most stable ... biplot is a useful tool for the analysis of multi-environment trial (MET) data. ... multiplicative components, extracting first the additive ... The AMMI analysis of variance of cassava harvest index of the 8 .... wheat mega-environments in Iran.

  5. Stability issues in reconstitution by weapon addition

    Energy Technology Data Exchange (ETDEWEB)

    Canavan, G.H.

    1997-08-01

    Reconstitution of strategic forces by the unilateral uploading of additional weapons from initially symmetric modest force levels reduces first strike stability. These changes are quantified and traced to changes in first and second strike costs in a model of missile exchanges in which both strikes are optimized analytically.

  6. 76 FR 26279 - Procurement List; Proposed Additions

    Science.gov (United States)

    2011-05-06

    ...-service area; clean and sanitize food service equipment, utensil cleaning, and dishwashing; clean pots... additions to the Procurement List. SUMMARY: The Committee is proposing to add services to the Procurement... in this notice will be required to procure the services listed below from nonprofit agencies...

  7. 77 FR 60969 - Procurement List; Additions

    Science.gov (United States)

    2012-10-05

    ... Are Blind or Severely Disabled published a notice for additions to the Procurement List with the... Committee for Purchase From People Who Are Blind or Severely Disabled published notices of proposed..., Phoenix, AZ. Service Type/Location: Custodial and Grounds Maintenance Services, Austin Courthouse, 501...

  8. 27 CFR 5.33 - Additional requirements.

    Science.gov (United States)

    2010-04-01

    ... 27 Alcohol, Tobacco Products and Firearms 1 2010-04-01 2010-04-01 false Additional requirements. 5.33 Section 5.33 Alcohol, Tobacco Products and Firearms ALCOHOL AND TOBACCO TAX AND TRADE BUREAU, DEPARTMENT OF THE TREASURY LIQUORS LABELING AND ADVERTISING OF DISTILLED SPIRITS Labeling Requirements for...

  9. 76 FR 41687 - Food Additives Permitted for Direct Addition to Food for Human Consumption; Hydroxypropyl Cellulose

    Science.gov (United States)

    2011-07-15

    ... Organization and the World Health Organization (FAO/WHO) Expert Committee for Food Additives (JECFA) has... DEPARTMENT OF HEALTH AND HUMAN SERVICES Food and Drug Administration 21 CFR Part 172 [Docket No. FDA-2010-F-0103] Food Additives Permitted for Direct Addition to Food for Human Consumption...

  10. Additional Samples: Where They Should Be Located

    International Nuclear Information System (INIS)

    Pilger, G. G.; Costa, J. F. C. L.; Koppe, J. C.

    2001-01-01

    Information for mine planning requires to be close spaced, if compared to the grid used for exploration and resource assessment. The additional samples collected during quasimining usually are located in the same pattern of the original diamond drillholes net but closer spaced. This procedure is not the best in mathematical sense for selecting a location. The impact of an additional information to reduce the uncertainty about the parameter been modeled is not the same everywhere within the deposit. Some locations are more sensitive in reducing the local and global uncertainty than others. This study introduces a methodology to select additional sample locations based on stochastic simulation. The procedure takes into account data variability and their spatial location. Multiple equally probable models representing a geological attribute are generated via geostatistical simulation. These models share basically the same histogram and the same variogram obtained from the original data set. At each block belonging to the model a value is obtained from the n simulations and their combination allows one to access local variability. Variability is measured using an uncertainty index proposed. This index was used to map zones of high variability. A value extracted from a given simulation is added to the original data set from a zone identified as erratic in the previous maps. The process of adding samples and simulation is repeated and the benefit of the additional sample is evaluated. The benefit in terms of uncertainty reduction is measure locally and globally. The procedure showed to be robust and theoretically sound, mapping zones where the additional information is most beneficial. A case study in a coal mine using coal seam thickness illustrates the method

  11. A convenient synthesis of 3-aryl-1,2,4-oxadiazoles from ethyl acetoacetate and amidoximes under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Juliana L. L. F. Regueira

    2012-06-01

    Full Text Available 1,2,4-Oxadiazole containing compounds have attracted great attention due to their applications in material chemistry and therapeutics. Herein we report a convenient synthesis of 3-aril-[1,2,4-oxadiazol-5yl] propan-2-one (3a-d by heating of b-ceto esters and an amidoximes without any solvent and in the absence of base. The arylamidoximes (1a-f was synthesized in moderate and excellent yields (31- 89% by reaction of nitrile with hydroxylamine hydrochloride in water at 25ºC. In the general synthetic strategy employed in our study is illustrated in scheme 1. The 3-aril-[1,2,4-oxadiazol-5yl] propan-2-one (3a-f were synthesized by treatment of arylamidoxime (1a-f with b-ceto esters for 4 hour without any solvent and in the absence of base. The reaction was monitored  by TLC   (thin layer chromatography. The heterocycles (3a-f were obtained in moderate and good yields (60-88%. The products were identified using both analytical and spectral data (IR, 1H and 13C NMR and all compounds are in full agreement with the proposed structure.

  12. Solvent-free preparation of polylactic acid fibers by melt electrospinning using umbrella-like spray head and alleviation of problematic thermal degradation

    Directory of Open Access Journals (Sweden)

    Liu Yong

    2012-01-01

    Full Text Available Melt electrospinning is an even simpler and safer method compared with the solution electrospinning in the production of ultra-fine fibers. Polylactic acid (PLA is a biodegradable and resorbable aliphatic ester that has received significant attention in recent years. PLA is easily degradable at high temperature in the process of melt electrospinning. High efficient fibers were made using our designed umbrella-like spray head spinning facility in this work. To find how to alleviate the problematic degradation and what factors could be relevant to degradation, temperature, relative molecular mass, Differential Scanning Calorimeter and X-ray Diffraction patterns before and after spinning were investigated and compared with each other. Results showed that fibers were facile shorten and fractured when spun at 245°C while the relative molecular mass of PLA fibers decreased markedly as compared with that spun at 210°C. To hinder the degradation, couple of experimental efforts were implemented with adding antioxidants, raising spinning voltage, lowering temperature, and reducing residence time. After such efforts, it was observed that the relative molecular mass of the PLA fibers was higher than those without inputting any efforts. The effect of antioxidant 1010 was found the most promising on the alleviation of PLA problematic thermal degradation.

  13. Microwave- assisted solvent-free Diels-Alder reaction – a fast and simple route to various 5,6-substituted norbornenes and polychlorinated norbornenes

    Czech Academy of Sciences Publication Activity Database

    Dejmek, Milan; Hřebabecký, Hubert; Šála, Michal; Dračínský, Martin; Nencka, Radim

    -, č. 24 (2011), s. 4077-4083 ISSN 0039-7881 R&D Projects: GA MŠk 1M0508 Institutional research plan: CEZ:AV0Z40550506 Keywords : Diels - Alder reaction * polychlorinated norbornanes * norbornene Subject RIV: CC - Organic Chemistry Impact factor: 2.466, year: 2011

  14. Ionic liquid-silica precursors via solvent-free sol-gel process and their application in epoxy-amine network: a theoretical/experimental study

    Czech Academy of Sciences Publication Activity Database

    Perchacz, Magdalena; Donato, R. K.; Seixas, L.; Zhigunov, Alexander; Konefal, Rafal; Serkis-Rodzen, Magdalena; Beneš, Hynek

    2017-01-01

    Roč. 9, č. 19 (2017), s. 16474-16487 ISSN 1944-8244 R&D Projects: GA ČR(CZ) GA17-08273S; GA MŠk(CZ) LO1507 Institutional support: RVO:61389013 Keywords : 3D POSS structures * epoxy-silica hybrid material * IL-silica precursor Subject RIV: CD - Macromolecular Chemistry OBOR OECD: Polymer science Impact factor: 7.504, year: 2016

  15. Disentangled solid state and metastable polymer melt; a solvent free route to high-modulus high-strength tapes and films of UHMWPE

    Science.gov (United States)

    Rastogi, Sanjay

    2013-03-01

    Ultra High Molecular Weight Polyethylene (UHMWPE) having average molar mass greater than a million g/mol is an engineering polymer. Due to its light-weight, high abrasion resistance and biocompatibility it is used for demanding applications such as body armour, prostheses etc. At present, because of its high melt viscosity to achieve the uniaxial/biaxial properties in the form of fibers/films the polymer is processed via solution route where nearly 95wt% of the solvent is used to process 5wt% of the polymer. In past several attempts have been made to process the polymer without using any solvent. However, compared to the solvent processing route the achieved mechanical properties were rather poor. Here we show that by controlled synthesis it is feasible to obtain UHMWPE that could be processed free of solvent to make uniaxial tapes and biaxial films, having unprecedented mechanical properties, exceeding that of the solution spun fibers. We address some of the fundamental aspects of chemistry, physics, rheology and processing for the development of desired morphological features to achieve the ultimate mechanical properties in tapes and films. The paper will also address the metastable melt state obtained on melting of the disentangled crystals and its implication on rheology in linear and nonlinear viscoelastic region. Solid state NMR studies will be applied to establish disentangled state in solid state to the polymerisation conditions. References: Macromolecules 2011, 44(14), 5558-5568; Nature Materials 2005, 4, 635-641; Phys Rev Lett 2006, 96(21), 218303-218205. The authors acknowledge financial support by the Dutch Polymer Institute.

  16. Field Evaluation of Solvent-Free Sampling with Di-n-butylamine for the Determination of Airborne Monomeric and Oligomeric 1,6-Hexamethylene Diisocyanate

    Science.gov (United States)

    2014-03-27

    ISO Guide 34:2009 and ISO / IEC 17025 :2005) for HDI oligomers. Per the manufacturer, a single ASSETTM sampler may be used for over 8 hours which leads...hexamethylene diisocyanate (HDI). During this study, the Supelco ASSETTM EZ4-NCO Dry Sampler was compared to the Omega Specialty Instrument Company ISO ...detection (HPLC-MS); 2) do ASSETTM and ISO -CHEK® samplers collect equivalent HDI monomer and oligomer concentrations; and 3) what is the relative cost of

  17. Skin penetration and photoprotection of topical formulations containing benzophenone-3 solid lipid microparticles prepared by the solvent-free spray-congealing technique.

    Science.gov (United States)

    Martins, Rodrigo Molina; Siqueira, Silvia; Fonseca, Maria José Vieira; Freitas, Luis Alexandre Pedro

    2014-01-01

    Solid-lipid microparticles loaded with high amounts of the sunscreen UV filter benzophenone-3 were prepared by spray congealing with the objective of decreasing its skin penetration and evaluate whether the sunscreen's photoprotection were impaired by the microencapsulation process. The microparticles were produced using the natural lipids carnauba wax or bees wax and three different concentrations of benzophenone-3 (30, 50 and 70%) using spray congealing technique. The microparticles presented properties suitable for topical application, such as spherical morphology, high encapsulation efficiency (95.53-102.2%), average particle sizes between 28.5 and 60.0 µm with polydispersivities from 1.2 to 2.5. In studies of in vitro skin penetration and preliminary stability, formulations of gel cream containing carnauba wax solid lipid microparticles and 70% benzophenone-3 when compared to the formulation added of bees wax solid-lipid microparticles containing 70% benzophenone-3, was stable considering the several parameters evaluated and were able to decrease the penetration of the UV filter into pig skin. Moreover, the formulations containing solid lipid microparticles with 70% benzophenone-3 increased the photoprotective capacity of benzophenone-3 under UV irradiation. The results show that spray-congealed microparticles are interesting solid forms to decrease the penetration solar filters in the skin without compromising their photoprotection.

  18. Microwave—enhanced Mannich Condensation of Terminal Alkynes,Primary Amines with Paraformaldehyde on cuprous Iodide Doped Alumina under Solvent Free Conditions

    Institute of Scientific and Technical Information of China (English)

    王磊; 李品华

    2003-01-01

    A microwave-enhanced,solventless Mannich condensation of terminal alkynes,primary amines with paraformaldehyde on cuprous iodide doped alumina has been investigated.The structures of products depend on the ratio of alkyne to amine and paraformaldehyde.

  19. RETRACTED: Preliminary study: Kinetics of oil extraction from basil (Ocimum basilicum by microwave-assisted hydrodistillation and solvent-free microwave extraction

    Directory of Open Access Journals (Sweden)

    Heri Septya Kusuma

    2016-07-01

    This manipulation of the peer-review process represents a clear violation of the fundamentals of peer review, our publishing policies, and publishing ethics standards. Apologies are offered to the reviewers whose identities were assumed and to the readers of the journal that this deception was not detected during the submission process.

  20. Synthesis, characterization and application of a nano-manganese-catalyst as an efficient solid catalyst for solvent free selective oxidation of ethylbenzene, cyclohexene, and benzylalcohol

    Science.gov (United States)

    Habibi, Davood; Faraji, Ali Reza

    2013-07-01

    The object of this study is to synthesize the heterogeneous Mn-nano-catalyst (MNC) which has been covalently anchored on a modified nanoscaleSiO2/Al2O3, and characterized by FT-IR, UV-Vis, CHN elemental analysis, EDS, TEM, and EDX. The method is efficient for the highly selective oxidation of ethylbenzene, cyclohexene, and benzylalcohol without the need to any solvents, using tert-butyl hydroperoxide (TBHP) as an oxidant. Oxidation of ethylbenzene, cyclohexene, and benzylalcohol gave acetophenone, 2-cyclohexene-1-one and benzaldehyde, respectively, as major products. Reaction conditions have been optimized by considering the effect of various factors such as reaction time, amounts of substrates and oxidant, Mn-nano-catalyst and application of various solvents.