Sample records for ammonolysis

  1. The Influence of the Ammonolysis Temperature on the Photocatalytic Activity of β-TaON

    Directory of Open Access Journals (Sweden)

    Songhak Yoon


    Full Text Available Phase-pure tantalum oxynitride (β-TaON powders were synthesized by thermal ammonolysis of Ta2O5 powders. X-ray diffraction revealed an enlargement of the unit cell and an increase of the crystallite size with increasing ammonolysis temperature. Scanning electron microscopy showed reduced particle sizes for β-TaON synthesized at 800 and compared to the precursor oxide. With increasing nitridation temperature the Brunauer-Emmett-Teller surface area was reduced and the nitrogen content increased. UV-Vis spectroscopy showed a bandgap energy of 2.6–2.4 eV. The highest oxygen evolution rate of 220 μmol·g−1·h−1 was achieved for β-TaON synthesized at . The factors determining the photocatalytic activity of β-TaON powders were found to be the specific surface area and defects in the β-TaON.

  2. Thermal Ammonolysis Study of the Rare-Earth Tantalates RTaO4


    Maillard, Pascal; Tessier, Franck; Orhan, Emmanuelle; Cheviré, François; Marchand, Roger


    International audience Reaction between rare-earth tantalates RTaO4 and ammonia flow at 900−950 °C forms oxynitrides belonging to different structure types, perovskites RTaON2, pyrochlores R2Ta2O5N2, and defect fluorites RTa(O,N,□)4, depending on the size of the R element. The nature of the oxide precursor is a crucial parameter affecting the ammonolysis reaction. A comparative study has been carried out between oxide powders prepared by a ceramic route and a chimie douce process. The pyro...

  3. Magnetic properties of the ammonolysis product of α-Fe powder containing a small amount of aluminum

    Energy Technology Data Exchange (ETDEWEB)

    Tsugawa, Yuta; Maubuchi, Yuji; Motohashi, Teruki; Kikkawa, Shinichi, E-mail:


    Magnetite was prepared containing a small amount of aluminum and its nitride was generated through low temperature ammonolysis following reduction under hydrogen. The nitrided product was determined by XRD to be a mixture of “α″-Fe{sub 16}N{sub 2}” having a slightly deformed crystal structure from α″-Fe{sub 16}N{sub 2} and the residual α-Fe. Magnetic coercivity of the mixture was decreased from the value of 150 mT obtained for the nitride product made without aluminum, due to the precipitation of nonmagnetic amorphous alumina in the low temperature nitrided bcc (Fe{sub 1−x}Al{sub x}) with x≤0.03. The aluminum-doped nitride product in which the “α″-Fe{sub 16}N{sub 2}” fraction was 30 at% exhibited magnetization at 1.5 T of approximately 200 Am{sup 2}kg{sup −1} at room temperature and its magnetic coercivity was 20 mT. - Graphical abstract: Magnetic iron nitride particles were separated by nonmagnetic amorphous γ-alumina. Magnetic coercivity was decreased by reducing the magnetic interaction between the particles. - Highlights: • Magnetic coercivity decreased in α”-Fe{sub 16}N{sub 2} like compound as a soft magnet. • Small amount of Al addition was effective in its preparation. • Magnetic interaction decreased between the “α”-Fe{sub 16}N{sub 2}” particles.

  4. Synthesis of uranium fluorides from uranium dioxide with ammonium bifluoride and ammonolysis of uranium fluorides to uranium nitrides (United States)

    Yeamans, Charles Burnett

    This work presents the chemical conversion of uranium oxides to uranium fluorides, and their subsequent conversion to uranium nitrides. Uranium dioxide reacts with ammonium bifluoride at 20°C to form compound in the ammonium-uranium fluoride chemical system. This reaction occurs between solid uranium dioxide at the surface of the particles and ammonium fluoride vapor. A shrinking-sphere model demonstrated surface reaction kinetics, not mass transport by diffusion through the product layer, limit the reaction rate when the starting material consists of 100 mum uranium dioxide particles. Powder x-ray diffraction showed the reaction to be complete within 8 hours, with (NH4) 4UF8 the reaction product. High-resolution electron microcopy revealed the product is largely amorphous on a micrometer-scale, but contains well-formed crystal domains on the order of 10x10 nm. X-ray diffraction showed the reaction progresses though beta-NH4UF5, delta-(NH 4)2UF6, and gamma-(NH4)2UF6 intermediate phases before finally forming (NH4)4UF 8. Modeling the system as a series of first-order reaction suggested a fourth intermediate, possibly UF4, is likely to occur. The reaction of (NH4)4UF8 with ammonia gas at 800°C forms alpha-U2N3/UN2 solid solution products with a composition of UN1.83. The x-ray powder diffraction pattern of this product is the fcc pattern commonly referenced as that of UN2 and the lattice parameter was 0.53050 nm. Surface area increased by a factor of ten during ammonolysis, consistent with the action of a hydriding agent. The alpha-U2N 3/UN2 solid solution system formed contained 1 wt% UO 2 as an impurity. Upon subsequent heating to 1150°C for 4.5 hours under argon, the nitride sample formed UN with a UO2 impurity of 9 wt%. Based on the HRTEM images, oxidation in the UN product appears to be limited to within 20 nm of particle surfaces and grain boundaries.

  5. Research on Synthesis of Ammonolysis Derivative of Arctigenin and Antitumor Bioactivity%牛蒡苷元氨解衍生物的合成及其抗肿瘤活性研究

    Institute of Scientific and Technical Information of China (English)

    陈桂荣; 徐煜彬; 窦德强; 姜洪帅


    Objective:For the lower water solubility,arctigenin was used as a lead compound for structure modification to improve the water solubility and the bioavailability and convenient preparation and expand the range of clinical application.Methods:Arctigenin was treated with propylamine aqueous solutions at the room temperature and the ammonolysis derivative was obtained by recrystallization.The five cancer lines were used to examine the bioactivity of arctigenin and ammonolysis derivative.Results:The ammonolysisi derivative was yield and the experiment was easy treatment and simple operation and high yield.The bioactivity result was indicated that the ammonolysis derivative had lower antitumor activity than arctigenin.Conclusion:The optimal synthesized art was that the ration of arctigenin and propylamine was 1:0.05 and the reaction was carried out at room temperature for 24 hours and the yield was 64%.The bioactivity results showed that lactone ring of arctigenin was the important agent in antitumor activity.%目的:牛蒡苷元属于木脂素类化合物,水溶性差,故以牛蒡苷元为先导化合物进行结构修饰,改善其水溶性,进而提高生物度,方便制剂、扩大牛蒡苷元的临床应用范围.方法:采用丙胺与牛蒡苷元在室温下发生氨解反应,通过重结晶方法制备氨解衍生物.采用5种人癌细胞株对氨解衍生物进行抗肿瘤活性研究.结果:合成得到牛蒡苷元氨解衍生物,操作简单,后处理容易,收率较高,并且衍生物的溶解性高于牛蒡苷元.对牛蒡苷元与氨解衍生物进行抗肿瘤活性研究表明氨解衍生物的活性低于牛蒡苷元.结论:牛蒡苷元氨解衍生物的最佳合成条件为:牛蒡苷元与丙胺的质量体积比为1∶0.05,室温反应24 h,收率为64%.经活性研究表明牛蒡苷元的内酯环是抗肿瘤活性关键基团.

  6. Biocatalytic ammonolysis of (5S)-4,5-dihydro-1H-pyrrole-1,5-dicarboxylic acid, 1-(1,1-dimethylethyl)-5-ethyl ester: preparation of an intermediate to the dipeptidyl peptidase IV inhibitor Saxagliptin. (United States)

    Gill, Iqbal; Patel, Ramesh


    An efficient biocatalytic method has been developed for the conversion of (5S)-4,5-dihydro-1H-pyrrole-1,5-dicarboxylic acid, 1-(1,1-dimethylethyl)-5-ethyl ester (1) into the corresponding amide (5S)-5-aminocarbonyl-4,5-dihydro-1H-pyrrole-1-carboxylic acid, 1-(1,1-dimethylethyl)ester (2), which is a critical intermediate in the synthesis of the dipeptidyl peptidase IV (DPP4) inhibitor Saxagliptin (3). Candida antartica lipase B mediates ammonolysis of the ester with ammonium carbamate as ammonia donor to yield up to 71% of the amide. The inclusion of Ascarite and calcium chloride as adsorbents for carbon dioxide and ethanol byproducts, respectively, increases the yield to 98%, thereby offering an efficient and practical alternative to chemical routes which yield 57-64%.

  7. Synthesis of Arcitgenin Ammonolysis Derivative%牛蒡苷元氨解衍生物的合成

    Institute of Scientific and Technical Information of China (English)

    张辉; 陈桂荣; 窦德强; 康廷国


    目的:合成牛蒡苷元的氨解衍生物N-苯甲基-2-(4'-羟基-3'-甲氧基苯甲基)-3-(3",4"-二甲氧基苯甲基)丁酰胺.方法:本实验采用氨解的方法对牛蒡苷元的内酯环进行结构修饰,牛蒡苷元和苄胺溶液反应合成氨解衍生物.结论:通过对合成工艺条件进行较为详细的考察,确定最佳工艺条件.%Objective: N-benzyl-3- ( 3",4"-dimethoxybenzyl ) -4-hydroxyl-2- ( 3'-hydroxoy-4'-methoxybenzyl )butanamide, ammonoylsis derivative of arctigenin was yielded. Method: Structure modification in y -lactone ring of arctigenin was carried out. The ammonolysia derivative was synthesized by treating arctigenin and henzylamine solution. Conclusion : The art of the synthesis process was investigated in detail to determine the optimum process conditions.

  8. Lipase-catalyzed synthesis of fatty acid amide (erucamide) using fatty acid and urea. (United States)

    Awasthi, Neeraj Praphulla; Singh, R P


    Ammonolysis of fatty acids to the corresponding fatty acid amides is efficiently catalysed by Candida antartica lipase (Novozym 435). In the present paper lipase-catalysed synthesis of erucamide by ammonolysis of erucic acid and urea in organic solvent medium was studied and optimal conditions for fatty amides synthesis were established. In this process erucic acid gave 88.74 % pure erucamide after 48 hour and 250 rpm at 60 degrees C with 1:4 molar ratio of erucic acid and urea, the organic solvent media is 50 ml tert-butyl alcohol (2-methyl-2-propanol). This process for synthesis is economical as we used urea in place of ammonia or other amidation reactant at atmospheric pressure. The amount of catalyst used is 3 %.

  9. Synthesis and Ceramic Conversion of Polysiloxazane to Silicon Oxynitride

    Institute of Scientific and Technical Information of China (English)


    Amorphous silicon oxynitride powders have been obtained by pyrolysis of polysiloxazane in a stream of anhydrous NH3 at the temperature up to 1000°C. The polysiloxazane is fabricated from ammonolysis of chloropolysiloxane that is produced by the hydrolysis of silicon tetrachloride. The conversion of polysiloxazane to silicon oxynitride and the structural features of the final powders have also been studied by infrared spectra, elemental composition and X-ray diffraction analysis and SEM observation.

  10. Convenient synthesis of (4R,5R)-4,5-bis(aminomethyl)-2-isopropyl- 1,3-dioxolane

    Institute of Scientific and Technical Information of China (English)


    A convenient approach for the preparation of (4R,5R)-4,5-bis(aminomethyl)-2-isopropyl-l,3-dioxolane is described. The target compound via two steps is synthesized from diethyl-2,3-O-isobutylidene-D-tartrate, through ammonolysis and reduction.(C) 2007 De Cai Wang. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.

  11. Research progress of ammoniation reaction of carbon dioxide%二氧化碳的氨化反应研究进展

    Institute of Scientific and Technical Information of China (English)

    王付燕; 孙洪志; 宋名秀; 阿不都拉江·那斯尔; 王倩; 朱维群


    论述了减排CO2的重要性,概述了CO2化学利用的主要方法,综述了CO2的3种氨化反应,即氨化反应生成碳酸氢铵、尿素和三聚氰酸,重点介绍了 CO2氨化反应生成三聚氰酸,对该反应进行了热力学分析,叙述了其反应的特点,得出 CO2氨化合成三聚氰酸等固体产品是一条比较可行的 CO2化学利用路线。氨化合成三聚氰酸不仅可以实现CO2的封存,而且能够实现CO2的高值有效利用,对解决CO2减排具有重要意义。认为将氨化反应与煤化工产业相结合,可以有效减少二氧化碳的排放强度,具有广阔的发展前景。%The importance of CO2 emission reduction is discussed,and the main methods of chemical utilization of CO2 is outlined. Three ways of ammonolysis reaction of carbon dioxide are reviewed. Ammonolysis reaction produces ammonium bicarbonate , urea and cyanuric acid. Production of cyanuric acid by ammonolysis of carbon dioxide is highlighted,and the thermodynamics is analyzed. The reaction characteristics are described,and ammonolysis of carbon dioxide to produce cyanuric acid and other solid products is a feasible way for chemicalutulization of carbon dioxide. Not only carbon dioxide can be sealed up,but also high added value products can be obtained. Combination of ammonolysis reaction and coal chemical industry will reduce emission of carbon dioxide effectively, and has a broad prospect.

  12. Preparation of niobium based oxynitride nanosheets by exfoliation of Ruddlesden-Popper phase precursor.


    Maia, Ary da Silva; Cheviré, François; Demange, Valerie; Bouquet, Valérie; Pasturel, Mathieu; Députier, Stéphanie; Lebullenger, Ronan; Guilloux-Viry, Marylline; Tessier, Franck


    International audience; A new oxynitride Ruddlesden-Popper phase K1.6Ca2Nb3O9.4N0.6 .1.1H2 O was synthesized by the topochemical ammonolysis reaction at 700 °C from the oxide Dion-Jacobson phase KCa2Nb3O10 in the presence of K2CO3. The oxynitride showed good stability with a little loss of nitrogen, even after a few months of exposure to air. Its crystal structure was solved by Rietveld refinement of X-ray powder diffraction data in space group P4/mmm and considering a two-phase mixture, due ...

  13. (-)-Arctigenin as a lead compound for anticancer agent. (United States)

    Chen, Gui-Rong; Li, Hong-Fu; Dou, De-Qiang; Xu, Yu-Bin; Jiang, Hong-Shuai; Li, Fu-Rui; Kang, Ting-Guo


    (-)-Arctigenin, an important active constituent of the traditional Chinese herb Fructus Arctii, was found to exhibit various bioactivities, so it can be used as a good lead compound for further structure modification in order to find a safer and more potent medicine. (-)-Arctigenin derivatives 1-5 of (-)-arctingen were obtained by modifying with ammonolysis at the lactone ring and sulphonylation at C (6') and C (6″) and O-demethylation at CH3O-C (3'), CH3O-C (3″) and CH3O-C (4″), and their anticancer bioactivities were examined. PMID:23962054

  14. Syntheses and metal ions recognition of dendritic calix[n]arenes(n=6,8)amide derivative

    Institute of Scientific and Technical Information of China (English)

    WANG Yunyan; CAI Yahua; YAN Chaoguo


    Dendritic p-t'butylcalix[n]arene amide derivatives with terminal amino groups of the first and second generations were synthesized by using divergent methods from ammonolysis of ethyl calixarylacetate with 1,6-diaminohexane and Michael addition of methyl acrylate.Their structures were confirmed by IR,1H NMR.The recognition properties of these amide derivatives for several kinds of metal ions were studied with UV-Vis spectroscopy.The results showed a great affinity for soft Ag+ and UO22+ ions and formed 1:2 or 1:3 stoichiometric complexes.

  15. Study of sorptive ability of nitrogen-containing wood derivatives with respect to ions of diverse metals

    International Nuclear Information System (INIS)

    Sorptive ability of wood oxidating ammonolysis products towards Fe3+, Cu2+, Cd2+ and Ca2+ ions was studied under equilibrium conditions. It was ascertained that exchange capacity of modified wood depends on the content of carboxylic groups and nitrogen compounds in it; for Cd2+ ions its value makes up 5.22 and 5.41 g-eq./g at cadmium concentration in the initial solution 0.01 and 0.1 g-eq./l respectively. It is shown that the high sorptive ability of nitrogen-containing wood derivatives towards multi-charged cations stems from their chelating properties

  16. Amino acid analogs IV:4-fluoroisoleucine. (United States)

    Gershon, H; Shanks, L; Clarke, D D


    4-Fluoroisoleucine was produced by ammonolysis of 2-bromo-4-fluoro-3-methylpentanoic acid, which resulted from the bromofluorination of 4-methyl-2-pentenoic acid. It did not inhibit Plasmodium berghei in mice at 640 mg/kg and was not toxic to the animals. The fluoroamino acid inhibited Aspergillus niger, Trichoderma viride, Myrothecium verrucaria, Trichophyton mentagrophytes, and Mucor mucedo in Czapek solution agar at a concentration between 10(4) and 10(3) microgram/ml. Growth of Escherichia coli was inhibited 25% at 900 microgram/ml in a defined medium.

  17. Basic research with view to the development of new techniques of wood chemistry

    Energy Technology Data Exchange (ETDEWEB)

    Wienhaus, O.; Koch, H.; Schiene, R.; Fischer, F.


    The paper provides an overview of research in the areas wood pyrolysis (smoldering behaviour of the components of tree material, production of activated coal from coke from mixed chipwood of pine, process for drying, smoldering, and partial gasification of wood in a reactor, wood tar analyses, phenolic-resin glues on the basis of wood tar), utilization of lignin (Knowledge of material composition, utilization as a coking auxiliary, chemical conversion by hydrogenolysis and oxydative ammonolysis) and substances extracted from wood (tall oil production and upgrading, manufacture of paper glues from tall oil resin, production of ..beta..-sitosterol).

  18. Stepwise conversion of a single source precursor into crystalline AlN by transamination reaction

    International Nuclear Information System (INIS)

    Ammonolysis of the monomeric, base-stabilized trisaminoalane Me3N-Al[N(H)Dipp)]3 (Dipp=2,6-iPr2-C6H3) yielded Al-N oligomers, which were characterized in detail by solid state NMR spectroscopy (1H, 13C, 15N, 27Al) and TGA/DTA. Pyrolysis of as-prepared oligomers at different temperatures in an argon steam yielded carbon-containing black solids, whereas pyrolysis under a steady flow of NH3 produced pure aluminum nitride (AlN). The role of the pyrolysis temperature and the influence of NH3 on the formation of crystalline materials were investigated. As-prepared AlN was characterized by solid state NMR spectroscopy (15N, 27Al), X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron energy loss spectroscopy (EELS). Theoretical calculations were performed in order to identify potential reaction intermediates. - Graphical abstract: Ammonolysis reactions of Me3N-Al(NHDipp)3 in liquid NH3 yielded Al-N oligomers, which can be transformed into nanocrystalline aluminum nitride particles under thermolysis conditions at 1000 deg. C. Theoretical calculations were performed in order to identify potential reaction intermediates

  19. Bandgap tuning in SrTi(N,O,F){sub 3} by anionic-lattice variation

    Energy Technology Data Exchange (ETDEWEB)

    Yoon, Songhak; Maegli, Alexandra E.; Karvonen, Lassi; Matam, Santhosh K.; Shkabko, Andrey [Laboratory for Solid State Chemistry and Catalysis, Empa-Swiss Federal Laboratories for Materials Science and Technology, CH-8600 Dübendorf (Switzerland); Riegg, Stefan [Lehrstuhl für Experimentalphysik 5, EKM, Universität Augsburg, Universitätsstraße 1, 86135 Augsburg (Germany); Großmann, Thomas; Ebbinghaus, Stefan G. [Institut für Chemie, Martin-Luther Universität Halle-Wittenberg, Kurt-Mothes-Straße 2, 06120 Halle/Saale (Germany); Pokrant, Simone [Laboratory for Solid State Chemistry and Catalysis, Empa-Swiss Federal Laboratories for Materials Science and Technology, CH-8600 Dübendorf (Switzerland); Weidenkaff, Anke, E-mail: [Laboratory for Solid State Chemistry and Catalysis, Empa-Swiss Federal Laboratories for Materials Science and Technology, CH-8600 Dübendorf (Switzerland)


    Polycrystalline SrTiO{sub 3} and SrTi(O,F){sub 3} powders were synthesized by a solid-state reaction. A partial substitution of oxygen by nitrogen was subsequently carried out using thermal ammonolysis resulting in SrTi(N,O){sub 3} and SrTi(N,O,F){sub 3}. Powder X-ray diffraction (XRD) revealed a cubic perovskite structure with space group Pm-3m for all samples. The thermal ammonolysis slightly increased the lattice parameters, crystallite sizes and strain. As a result from the co-substitution of oxygen with nitrogen and fluorine for SrTi(N,O,F){sub 3}, highly distorted TiO{sub 6} octahedra were detected using X-ray absorption near edge structure (XANES) spectroscopy. The weakening of all active modes of the Raman spectra after thermal ammonolysis also indicated enhanced distortions in the local crystal structure. SrTi(N,O,F){sub 3} has the largest amount of nitrogen as well as fluorine among all four samples as determined by thermogravimetric analysis (TGA), elemental analysis and X-ray photoelectron spectroscopy (XPS). In the UV–vis spectra a distinctive shift of the absorption-edge energy was observed exclusively for the SrTi(N,O,F){sub 3} sample from 390 to 510 nm corresponding to a bandgap narrowing from 3.18 to 2.43 eV. - Graphical abstract: Figure shows the shift of the absorption-edge energy for the SrTi(N,O,F){sub 3} sample from 390 to 510 nm corresponding to a bandgap narrowing from 3.18 to 2.43 eV. Display Omitted - Highlights: • Synthesis of phase-pure SrTi(N,O,F){sub 3} via solid-state reaction. • The incorporated nitrogen contents increase by the presence of fluorine in SrTi(N,O,F){sub 3}. • Co-substitution with nitrogen and fluorine is beneficial for the bandgap narrowing compared to by only nitrogen or fluorine substitution.

  20. Synthesis of allylamine in ethanol%乙醇中烯丙基胺的合成

    Institute of Scientific and Technical Information of China (English)

    唐炳涛; 张淑芬; 杨锦宗


    Allylamine was prepared from the ammonolysis of allyl chloride or the reaction of allyl chloride with hexamethylenetetramine in ethanol. The selectivity of allylamine was improved from 21.4% to 67.6% when the reaction was carried out in ethanol instead of liquid ammonia. At the same time, the selectivity of allylamine was increased from 13.3% to 67.6% when the molar ratio of NH3 to allyl chloride was increased from 4.5∶1 to 25∶1.However, the reaction of allyl chloride and hexamethylenetetramine in ethanol produced allylamine with high selectivity (100%) and high yield (87%).The synthesis of allylamine from the reaction of allyl chloride and hexamethylenetetramine in ethanol was more straightforward and convenient.

  1. Synthesis and antitumor activity of 2-. beta. -D-ribofuranosylselenazole-4-carboxamide and related derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Srivastava, P.C.; Robins, R.K.


    Treatment of 2,3,5-tri-O-benzoyl-..beta..-D-ribofuranosyl-1-carbonitrile with hydrogen selenide provided 2,5-anhydro-3,4,6-tri-O-benzoyl-D-allonselenoamide (3). Compound 3 was treated with ethyl bromopyruvate to provide ethyl 2-(2,3,5-tri-O-benzoyl-D-ribofuranosyl)selenazole-4-carboxylates, which after ammonolysis were converted to 2-..beta..-D-ribofuranosylselenazole-4-carboxamide (6) and its ..cap alpha..-analogue 7, respectively. Acetylation of nucleoside 6 provided 2-(2,3,5-tri-O-acetyl-..beta..-D-ribofuranosyl)selenazole-4-carboxamide, and phosphorylation of 6 provided the corresponding 5'-phosphate 9. Compounds 6 and 9 were found to be cytotoxic toward P388 and L1210 cells in culture and effective against Lewis lung carcinoma in mice.

  2. 氨基甲酸酯清洁合成技术进展%Progress in clean synthesis of carbamates

    Institute of Scientific and Technical Information of China (English)

    谭学峰; 王越; 胡静; 马飞; 王公应


    综述了氨基甲酸酯清洁合成技术的发展现状和趋势,并对所用催化剂体系做了详细评述,认为碳酸酯胺解法是最具产业化前景的氨基甲酸酯清洁合成路线,高活性催化剂结合适宜的工艺流程是产业化成功的关键.%Recent progress and trends in clean synthesis of carbamates were reviewed, including a detail commentary on the catalyst systems. Ammonolysis of dimethyl carbonate (DMC) was considered to be the most promising industrial route for clean synthesis of carbamates. It was believed that developing high activity catalyst with suitable process would be the key to the industrial success.

  3. Synthesis of 2,3,8,9-Tetrahydropyrido[2,3-d:6,5-d']dipyrimidine-4,6-diones%2,3,8,9-四氢吡啶并[2,3-d:6,5-d]二嘧啶-4,6-二酮衍生物的合成

    Institute of Scientific and Technical Information of China (English)

    杨留攀; 李加荣; 柴洪新; 袁洪; 张奇; 史大昕


    以丙二腈、原羧酸三乙酯、吡啶为起始原料经环化、氨解,然后与酮在甲醇钠催化下反应得到了2,3,8,9-四氢吡啶并[2,3-d:6,5-d']二嘧啶-4,6-二酮衍生物.目标产物的结构经IR,NMR,ESI和元素分析确证.%2,3,8,9-Tetrahydropyrido[2,3-d:6,5-d']dipyrimidine-4,6-diones were synthesized by using malononitrile, or- tho-triethyl and pyridine as starting materials in three steps reaction including cyclization, ammonolysis and reaction with ke- tones under the catalysis of sodium methoxide. The structures of the products were confirmed by NMR, IR, ESI and elemental analysis.

  4. 新型杯[4]芳烃酰肼基羰基羧酸衍生物的合成%Synthesis of Novel Calix [ 4 ] -hydrazinylcarbonyl Carboxylic Acid Derivatives

    Institute of Scientific and Technical Information of China (English)

    刘志强; 洪碧琼; 杨发福; 许冰婷; 谢剑伟


    杯[4]芳烃经醚化引入酯基后再经水合肼肼解,进一步与丁二酸酐或顺丁烯二酸酐氨解开环合成了两个新型的杯[4]芳烃酰肼基羰基羧酸衍生物,产率85%和83%,其结构经1H NMR,IR和ESI-MS表征.%Two novel calix[4]-hydrazinylcarbonyl carboxylic acid derivatives in yields of 85% and 83% were synthesized by introducing ester groups into calix[4]arene, subsequently ammonolysis with hydrazine hydrate, and then ring-opening reaction with succinic anhydride or maleic anhydride. Their structures were characterized by 1H NMR, IR and ESI-MS.

  5. Rapid thermal synthesis of GaN nanocrystals and nanodisks

    Energy Technology Data Exchange (ETDEWEB)

    Sofer, Zdenek, E-mail:; Sedmidubsky, David; Huber, Stepan; Simek, Petr; Sanek, Filip; Jankovsky, Ondrej [Institute of Chemical Technology Prague, Department of Inorganic Chemistry (Czech Republic); Gregorova, Eva [Institute of Chemical Technology Prague, Department of Glass and Ceramics (Czech Republic); Fiala, Roman [Charles University, Faculty of Mathematics and Physics (Czech Republic); Matejkova, Stanislava [Institute of Organic Chemistry and Biochemistry of the ASCR, v.v.i (Czech Republic); Mikulics, Martin [PGI-9, Peter Gruenberg Institute, Forschungszentrum Juelich (Germany)


    Gallium nitride materials are at the forefront of nanoelectronic research due to their importance for UV optoelectronics. In this contribution, we present a facile and well-controlled synthesis of GaN nanodisks by rapid thermal ammonolysis of complex gallium fluoride precursor. We observed the formation of GaN nanodisks in 150 s at 800 Degree-Sign C. The structural properties of GaN were investigated by X-ray diffraction, Raman spectroscopy, and micro-photoluminescence. The morphology of GaN was investigated by scanning electron microscopy and the magnetic properties by superconducting quantum interference device (SQUID) techniques. The morphology of nanodisks was strongly influenced by the temperature of synthesis. The structure characterization shows a high concentration of defects related mainly to the vacancies of N and Ga. The magnetic measurement by SQUID shows paramagnetic behavior induced by structure defects. These findings have a strong implication on the construction of modern optoelectronic nanodevices.

  6. Space-confined preparation of high surface area tungsten oxide and tungsten nitride inside the pores of mesoporous silica SBA-15

    DEFF Research Database (Denmark)

    Meyer, Simon; Beyer, Hans; Köhler, Klaus;


    For the direct preparation of high surface area nitride materials, a lack of suitable precursors exists. Indirect preparation by gas phase nitridation (e.g. by ammonia) requires high temperatures and often results in sintering. The present work demonstrates that the space-confined preparation of W2......N inside the pores of ordered mesoporous silica SBA-15 offers a possibility to reduce sintering phenomena and thus to obtain smaller particles, porous structures and a higher surface area material. The preparation was pursued in a two-step approach. First, WO3 was introduced into the channels of SBA......-15 and second, ammonolysis was conducted for its conversion to W2N. When performed in the presence of the exo-template, SBA-15 acts as a stabilizer and small W2N particles (6-7 nm) with a high specific surface area (40 m(2) g(-1)) are obtained after template removal. When the template is, however...

  7. Nanosized Si3N4/SiC-powders by polysilazane/polycarbosilane-pyrolysis

    International Nuclear Information System (INIS)

    The preparation of the nanosized powders has been realized by gasphase-pyrolysis of volatile precursor compounds at temperatures between 600 and 1200 C. Silicon carbonitride powders have been created from polysilazanes, which have been synthesized by ammonolysis of alkylchlorosilanes. Silicon carbide powders have been prepared from 1,1,3,3-tetramethyl-1,3-disilacyclobutane, gained by the dechlorination- and coupling reaction of chloromethyldimethylchlorosilane with magnesium. The ball-like powder particles have a diameter between 100 and 500 nm and a surface of 10 to 50 m2/g. They are X-ray amorphous and can be crystallized upper 1400 C to α-Si3N4 and β-SiC respectively. (orig.)

  8. Synthesis of ternary nitrides by mechanochemical alloying

    DEFF Research Database (Denmark)

    Jacobsen, C.J.H.; Zhu, J.J.; Lindelov, H.;


    Ternary metal nitrides ( of general formula MxM'N-y(z)) attract considerable interest because of their special mechanical, electrical, magnetic, and catalytic properties. Usually they are prepared by ammonolysis of ternary oxides (MxM'O-y(m)) at elevated temperatures. We show that ternary...... transition metal nitrides are also obtained by nitridation of the corresponding ternary carbide at 823 K. This transformation appears to occur by solid-state diffusion of carbide and nitride ions. To establish more general synthesis schemes for ternary nitrides, we have focused on the preparation of ternary...... nitrides by mechanochemical alloying of a binary transition metal nitride (MxN) with an elemental transition metal. In this way, we have been able to prepare Fe3Mo3N and Co3Mo3N by ball-milling of Mo2N with Fe and Co, respectively. The transformation sequence from the starting materials ( the binary...

  9. Silicon oxynitrides of KCC-1, SBA-15 and MCM-41 for CO 2 capture with excellent stability and regenerability

    KAUST Repository

    Patil, Umesh


    We report the use of silicon oxynitrides as novel adsorbents for CO 2 capture. Three series of functionalized materials based on KCC-1, SBA-15 and MCM-41 with Si-NH 2 groups were prepared using a simple one-step process via thermal ammonolysis using ammonia gas, and they demonstrated excellent CO 2 capture capabilities. These materials overcome several limitations of conventional amine-grafted mesoporous silica. They offer good CO 2 capture capacity, faster adsorption-desorption kinetics, efficient regeneration and reuse, more crucially excellent thermal and mechanical stability even in oxidative environments, and a clean and green synthesis route, which allows the overall CO 2 capture process to be practical and sustainable. This journal is © The Royal Society of Chemistry 2012.

  10. Study on the synthesis of N(2)-L-alanyl-L-glutamine%N(2)-L-丙氨酰-L-谷氨酰胺的合成工艺研究

    Institute of Scientific and Technical Information of China (English)

    陈再新; 夏正君; 蒋龙


    N (2) -L-Alanyl-L-glutamine was synthesized by ammonolysis of N- (D-2-chloropropionyl) -L- glutamine, which was obtained by condensation of D-2-chloropropionic chloride and L-glutamine. The best re- sult of the condensation reaction was obtained in toluene-water two-phase system, at 0~5~C, and by using 2 e- quivalent of NaOH solution, which was added dropwise with D-2-chloropropionic chloride at the same time, the yield was 92 %. The best yield 67.5 % of the ammonolysis reaction was obtained at 60℃ and by using concentrat ed ammonia solution.%以D-2-氯代丙酰氯和L-谷氨酰胺为原料,缩合得到N-(D-2-氯丙酰)-L-谷氨酰胺,再经氨化后得到N(2)-L-丙氨酰-L-谷氨酰胺。缩合反应使用2倍氢氧化钠水溶液并采用与D-2-氯代丙酰氯同时滴加的方式、在两相的甲苯/水体系中、温度在0~5℃结果最佳,收率92%。氨解反应使用浓氨水、在60℃下结果最佳,收率67.5%。

  11. A novel LaFeO{sub 3-X}N{sub X} oxynitride. Synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Sierra Gallego, G., E-mail: [Escuela de Ingenieria de Materiales, Facultad de Minas, Universidad Nacional de Colombia, Calle 75 no. 79A-51, Bloque M17, Medellin (Colombia); Marin Alzate, N.; Arnache, O. [Institute of Physics, University of Antioquia, Calle 67, No. 53-108, A.A. 1226 Medellin (Colombia)


    Highlights: Black-Right-Pointing-Pointer LaFeO{sub 3} perovskite synthesized by auto combustion method. Black-Right-Pointing-Pointer LaFeO{sub 3-X}N{sub X} oxynitride produced by ammonolysis reaction. Black-Right-Pointing-Pointer Oxynitride characterized by XRD, Rietveld, SEM, EDX, BET, Raman, TGA and FTIR. Black-Right-Pointing-Pointer Partial replacement of oxygen by nitrogen increases slightly the cell parameters. Black-Right-Pointing-Pointer TGA shows that oxynitride start to decompose in air above 550 Degree-Sign C. Evolution of N{sub 2} and NO was detected. - Abstract: A perovskite LaFeO{sub 3} was synthesized by auto combustion method and then LaFeO{sub 3-X}N{sub X} oxynitride was produced by ammonolysis reaction. The synthesized LaFeO{sub 3-X}N{sub X} oxynitride was characterized by X-ray diffraction (XRD), Rietveld refinement, scanning electron microscopy (SEM), energy dispersive X-ray (EDX), Brunauer-Emmett-Teller (BET) nitrogen adsorption, particle size distribution, Raman spectroscopy, thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR). Nitrogen effect into the perovskite structure was confirmed by DRX. The structure refinement using the Rietveld method indicates that partial replacement of oxygen by nitrogen increases slightly the cell parameters of the LaFeO{sub 3} perovskite. FTIR analysis show that bands at 995 and 1070 cm{sup -1} in the oxynitrides spectra could be assigned to the stretching vibration modes of Fe-N bonds in the FeO{sub 6-X}N{sub X} octahedral. Thermogravimetric analysis (TGA) showed that LaFeO{sub 3-X}N{sub X} oxynitride series start to decompose in air above 550 Degree-Sign C. During the decomposition it was found that some amount of nitrogen stays retained in the structure forming intermediate compounds. MS analysis of the gaseous products reveals the evolution of N{sub 2} and NO, suggesting a complex reaction mechanism. To our knowledge, there are no reports on the synthesis and characterization

  12. Improvement on Synthesis Process of C. I. Direct Blue 199%C.I.直接蓝199工艺改进

    Institute of Scientific and Technical Information of China (English)

    王雪梅; 郑玉安


    The Synthesis Process of C. I. Direct Blue 199 was improved. The reaction temperature of CuPc and chtorosulfonic acid was raised from 130℃ to 140 ℃, then the reaction temperature of the product with thionyl chloride was raised from 60 - 65 ℃ to 80 ℃ ; the dropping time of thionyl chloride was prolonged from 2 - 2. 5 hours to 4 hours; and ammonia was replaced by organic base in ammonolysis. By this new technology, the difficult problem in membrane filtration before salting out was resolved when the dye was applied in ink.%对C.I.直接蓝199的老工艺进行了改进。使铜酞菁与氯磺酸的反应温度由原来的130℃升至140℃左右,之后与氯化亚砜的反应温度由60~65℃提高到80℃,而且滴加氯化亚砜的时间从2~2.5延长至4小时,同时氨解用的氨水用有机碱替代。新工艺解决了此染料用于墨水时在盐析前膜过滤困难的问题。

  13. Enhanced photocatalytic degradation of rhodamine B under visible light irradiation on mesoporous anatase TiO2 microspheres by codoping with W and N (United States)

    Zheng, Jian; Xiong, Feng-Qiang; Zou, Mingming; Thomas, Tiju; Jiang, Heng; Tian, Ying; Yang, Minghui


    Mesoporous anatase TiO2 microspheres were prepared via solvothermal method. Ammonium tungstate was used as the W source, and ammonia gas flowing in an ammonothermal reactor as the N source for codoping. TiO2:(W,N) mesoporous microspheres, which were prepared from solvothermal treatment at 160 °C for 16 h and thermal ammonolysis at 500 °C for 2 h after calcination, have high specific surface area of 106 m2 g-1. XPS results indicate the presence of NO, Ni and W6+ in the codoped mesoporous TiO2 microspheres. Monodoping with N shifts the absorption band edge of anatase TiO2 from ultraviolet region to visible region. Although codoping with W makes the visible light absorbance decrease a little, the photocatalytic degradation of a cationic dye rhodamine B (RhB) on mesoporous TiO2:(W,N) microspheres is increased to 1.7 times of that on mesoporous TiO2:N microspheres. This may due to decreasing recombination centers by W-doping charge compensation.

  14. A novel solid-state electrochemiluminescence detector for capillary electrophoresis based on tris(2,2'-bipyridyl)ruthenium(II) immobilized in Nafion/PTC-NH2 composite film. (United States)

    Liu, Huijing; Yuan, Ruo; Chai, Yaqing; Mao, Li; Yang, Xia; Zhuo, Ying; Yuan, Yali


    A new electrochemiluminescence (ECL) detector for capillary electrophoresis (CE) based on tris(2,2'-bipyridyl)ruthenium(II) (Ru(bpy)(3)(2+)) immobilized in Nafion/PTC-NH(2) (an ammonolysis product of 3,4,9,10-perylenetetracarboxylic dianhydride (PTCDA)) composite film was presented for the first time. The Nafion/PTC-NH(2) composite film could effectively immobilize tris(2,2'-bipyridyl)ruthenium(II) via ion-exchange and electrostatic interaction. Cyclic voltammetric and ECL behavior of Nafion/PTC-NH(2)/Ru composite film was investigated compared to Nafion/Ru composite. The Nafion/PTC-NH(2)/Ru composite film exhibited good ECL stability and simple operability. Then the CE with solid-state ECL detector system was successfully used to detect sophora - a quinolizidine type - alkaloids as sophoridine (SR) and matrine (MT). The CE-ECL parameters that affected separation and detection were optimized. Under the optimized conditions, the linear range was from 2.5 × 10(-8) to 2 × 10(-6)mol/L for SR, 1.0 × 10(-8) to 1.0 × 10(-6)mol/L for MT. The detection limit (S/N=3) was estimated to be 5 × 10(-9) and 10(-9)mol/L for SR and MT, respectively. It was shown that the CE coupling with solid-state ECL detector system exhibited satisfying sensitivity of analysis. PMID:21376962

  15. Identification of neighbouring protein pairs in the rat liver 40-S ribosomal subunits cross-linked with dimethyl suberimidate. (United States)

    Terao, K; Uchiumi, T; Kobayashi, Y; Ogata, K


    (1) The 40-S ribosomal subunits of rat liver were treated with a bifunctional cross-linking reagent, dimethyl suberimidate. Cross-linked protein-protein dimers were separated by two-dimensional acrylamide gel electrophoresis. The stained cross-linked complexes within the gel were radioiodinated without the elution of proteins from the gel and were cloven into the original monomeric protein constituents by ammonolysis. The proteins in each dimer were finally identified by two-dimensional acrylamide gel electrophoresis of the cloven monomeric proteins, followed by radioautography of the stained gel. (2) The molecular weights of cross-linked complexes were determined by SDS-polyacrylamide gel electrophoresis and were compared with those of their constituent proteins. (3) The following dimers were proposed from these results: S3-S12 (S3 or S3a-S11), S4-S12 (S3b-S11, S5-S7 (S4-S6), S5-S22 (S4-S23 or S24), S6-S8 (S5-S7), S8-S16 (S7-S18), S17-S21 (S16--S19) and S22A-S22B (S23-S24), designated according to our numbering system [1]. The designations according to the proposed uniform nomenclature [2] are described in parentheses.

  16. Thermosensitive tribrachia star-shaped s-P(NIPAM-co-DMAM) random copolymer micelle aggregates: Preparation, characterization, and drug release applications. (United States)

    Luo, Yan-Ling; Wang, Yuan; Wang, Xuan; Xu, Feng; Chen, Ya-Shao


    Tribrachia star-shaped random copolymers with tunable thermosensitive phase transition temperature were designed and synthesized via a simple one-pot ammonolysis reaction approach with trimesic acid as cores. The self-assembly micellization behavior of the copolymers in aqueous solution was examined by surface tension, UV-vis transmittance, transmission electron microscope, and dynamic light scattering measurements, etc. The results indicated that the resultant copolymers formed thermosensitive micelle aggregates through hydrophobic interactions among the isopropyl groups of poly(N-isopropylacrylamide) PNIPAM chains and inter-star association at a polymer concentration above critical aggregation concentrations from 4.06 to 6.55 mg L(-1), with a cloud point range from 36.6℃ to 52.1℃, and homogeneously distributed micelle size below 200 nm. The arm length and the compositional ratios of the two comonomers had effect on physicochemical properties of the polymer micelle aggregates. Particularly, the cloud point values were enhanced as the (N,N-dimethylacrylamide) DMAM monomer was introduced and reached to 36.6℃ and 41.0℃-44.7℃ when the mass ratio of NIPAM to DMAM was 90:10 and 80:20, respectively. The thermo-triggered drug release and cytotoxicity were evaluated to confirm the applicability of the random copolymer micelle aggregates as novel drug targeted release carriers. PMID:25926671

  17. Preparation of niobium based oxynitride nanosheets by exfoliation of Ruddlesden-Popper phase precursor (United States)

    da Silva Maia, Ary; Cheviré, François; Demange, Valérie; Bouquet, Valérie; Pasturel, Mathieu; Députier, Stéphanie; Lebullenger, Ronan; Guilloux-Viry, Marylline; Tessier, Franck


    A new oxynitride Ruddlesden-Popper phase K1.6Ca2Nb3O9.4N0.6.1.1H2O was synthesized by the topochemical ammonolysis reaction at 700 °C from the oxide Dion-Jacobson phase KCa2Nb3O10 in the presence of K2CO3. The oxynitride showed good stability with a little loss of nitrogen, even after a few months of exposure to air. Its crystal structure was solved by Rietveld refinement of X-ray powder diffraction data in space group P4/mmm and considering a two-phase mixture, due to the difference in the degree of hydration, with a = 3.894(2) Å and c = 17.90(8) Å for the most hydrated phase and a = 3.927(6) Å and c = 17.09(2) Å for the less one. Optical band gaps were measured by diffuse reflectance in the UV-Visible range indicating a red shift of Eg to the visible region. The oxynitride layered perovskite was then protonated and exfoliated into nanosheets. TEM images and SAED patterns of the nanosheets proved that exfoliation was successful, showing lattice parameters quite compatible with the Rietveld refinement.

  18. Analysis on market demand and production technologies of acetonitrile%乙腈市场需求情况与技术分析

    Institute of Scientific and Technical Information of China (English)

    韩凤义; 白亮; 曹金朋; 张鹏


    The application and market demand of acetonitrile are presented, and the domestic and overseas advances in production technonlgies of acetonitrile are reviewed. Based on comparing with ammonolysis of acetic acid and ammoxidation of eth-anol, the synthesis of acetonitrile by ethanol dehydrogenation ammoniation is analyzed emphatically, owing to easily available and cheap raw materials, slight corrosion to equipment and by-produced hydrogen gas. In the long term, as long as the high efficient catalyst is developed, the industrial prospects of synthesis of acetonitrile by ethanol dehydrogenation amination will be more promising.%介绍了乙腈的用途及市场需求情况,综述了国内外合成乙腈的主要工艺方法,在与乙酸氨化路线、乙醇氨氧化路线对比分析的基础上,着重分析了乙醇脱氢氨化法合成乙腈技术,结果表明,用乙醇作为原料直接合成乙腈,原料相对易得、价格低廉,设备腐蚀性小,并且可以副产氢气.从长远来看,只要开发出高效的催化剂,乙醇脱氢氨化合成乙腈技术更有工业应用前景.

  19. Synthesis of Clofarabine%氯法拉滨的合成

    Institute of Scientific and Technical Information of China (English)

    陈云华; 杨伟强; 白骅


    Clofarabine, an antileukemie agent, was synthesized from guanosine via acetylation, chlorination,Sandmeyer reaction and ammonolysis to afford 2-cholor-2',3',5'-tri- O-acetyladenosine, which was subjected to selective deprotection with NH2OH·HCl-AcONa-pyridine system, followed by sulfonylation, fluorination and deprotection with an overall yield of about 8 %.%以鸟苷为原料,经乙酰化、氯代、重氮化后氯代及氨解反应制得关键中间体2-氯-2-,3',5'-三-O-乙酰基腺苷(6).6在盐酸羟胺-乙酸钠-吡啶体系中选择性脱2'-乙酰基,再经三氟甲磺酰化、氟代及脱保护反应制得抗白血病药氯法拉滨,总收率8%.

  20. Incorporating different vegetable oils into an aqueous dispersion of hybrid organic nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Samyn, Pieter, E-mail: [Albert-Luedwigs-University Freiburg, Institute for Forest Utilization (Germany); Schoukens, Gustaaf [Ghent University, Department of Textiles (Belgium); Stanssens, Dirk; Vonck, Leo; Van den Abbeele, Henk [Topchim N.V. (Belgium)


    Different vegetable oils including soy oil, high-oleic sunflower oil, corn oil, castor oil (CO), rapeseed oil, and hydrogenated CO were added to the imidization reaction of poly(styrene-maleic anhydride) or SMA, with ammonium hydroxide in aqueous medium. The oils favorably reduce viscosity during ammonolysis of the anhydride moieties and increase the maximum solid content of the dispersed imidized SMA to at least 50 wt%, compared to a maximum of 35 wt% for pure imidized SMA. The viscosity of imidized SMA with polyunsaturated oils was generally larger than for monosaturated oils, but it was highest for COs due to high contents of hydroxyl groups. Depending on the oil reactivity, homogeneous or core-shell nanoparticles with 20-60 nm diameters formed. The interactions of oil and organic phase were studied by Fourier-transform infrared spectroscopy, indicating qualitative variances between different oils, the fraction imidized SMA and remaining fraction of ammonolyzed SMA without leakage of oil upon diluting the dispersion and precipitation at low pH. A quantitative analysis with calculation of imide contents, amounts of reacted oil and chemical interactions was made by Fourier-transform-Raman spectroscopy suggesting that most interactions take place around the unsaturated oil moieties and ammonolyzed anhydride.

  1. 聚氨酯泡沫在环境领域的应用及其回收处理%Application of Polyurethane Foams in the Environmental Field and Reuse of the Materials

    Institute of Scientific and Technical Information of China (English)

    耿佳; 冯芳; 王东田


    总结了聚氨酯泡沫在环境领域的应用开发,包括利用聚氨酯泡沫作为水处理金属离子吸附剂、气固废吸附材料基材、废水处理用微生物载体.综述了废旧聚氨酯泡沫回收处理及利用方法,重点阐述了物理回收法、化学回收法中的醇解、水解、氨解、热解法等.最后对各类回收方法进行了总结比较.%The application and development of polyurethane foams in the environmental field, including the use of polyurethane foam as metal ion adsorbent for water treatment, gas and solid waste absorbent substrate, micro-carrier for waste water treatment, were summarized. The waste recycling and reuse methods of polyurethane foam were reviewed, focusing on the physical recycling and chemical recycling methods, such as alcoholysis, hydrolysis, am-monolysis, pyrolysis, etc. Finally, various types of rcycling methods were concluded and compared.

  2. Green House Gas Control and Agricultural Biomass for Sustainable Animal Agriculture in Developing Countries

    Directory of Open Access Journals (Sweden)

    J Takahashi


    Full Text Available Important green house gases (GHG attributed to animal agriculture are methane (CH4 and nitrous oxide (N2O, though carbon dioxide (CO2 contributes almost half of total greenhouse effect. Rumen CH4 production in an enteric fermentation can be accounted as the biggest anthropogenic source. Some of prebiotics and probiotics have been innovated to mitigate rumen CH4 emission. The possible use of agricultural biomass consisted of non-edible parts of crop plants such as cellulose and hemi cellulose and animal wastes was proposed as a renewable energy and nitrogen sources. The ammonia stripping from digested slurry of animal manure in biogas plant applied three options of nitrogen recycling to mitigate nitrous oxide emission. In the first option of the ammonia stripping, the effect of ammonolysis on feed value of cellulose biomass was evaluated on digestibility, energy metabolism and protein utilization. Saccharification of the NH3 treated cellulose biomass was confirmed in strictly anaerobic incubation with rumen cellulolytic bacteria, Ruminoccous flavefaciens, to produce bio-ethanol as the second option of ammonia stripping. In an attempt of NH3 fuel cell, the reformed hydrogen from the NH3 stripped from 20 liter of digested slurry in thermophilic biogas plant could generate 0.12 W electricity with proton exchange membrane fuel cell (PEM as the third option.

  3. A facile method to synthesize magnetic polymer nanospheres with multifunctional groups

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Xiaojuan, E-mail: [School of Material Engineering, Jinling Institute of Technology, Nanjing 211169 (China); Jiang Wei [National Special Superfine Powder Engineering Research Center, Nanjing University of Science and Technology, Nanjing 210094 (China); Ye Yuanfeng; Feng Zhiqiang [School of Material Engineering, Jinling Institute of Technology, Nanjing 211169 (China); Sun Zhendong; Li Fengsheng [National Special Superfine Powder Engineering Research Center, Nanjing University of Science and Technology, Nanjing 210094 (China); Hao Lingyun [School of Material Engineering, Jinling Institute of Technology, Nanjing 211169 (China); Chu Jianjun [Fourth Affiliated Hospital of Soochow University, Wuxi 214062 (China)


    Magnetic poly(styrene methyl methacrylate)/Fe{sub 3}O{sub 4} nanospheres with ester groups were prepared by a modified one-step mini-emulsion polymerization in the presence of Fe{sub 3}O{sub 4} ferrofluids. The effects of monomer dose, surfactant content, ferrofluid concentration and initiator content on the particle characteristics such as the size, morphology and magnetic properties were investigated by Fourier-transform infrared spectroscopy, transmission electron microscopy, thermogravimetric analysis and vibrating sample magnetometer. The results indicated that magnetic nanospheres were superparamagnetic with high saturation magnetization of 51.0 emu/g and corresponding magnetite content of 61.5 wt%. Subsequently, magnetic nanospheres with carboxyl and amino groups were also obtained by hydrolysis and ammonolysis reaction. These magnetic nanospheres with multifunctional groups have biomedical applications. - Research highlights: Facile way of synthesis of ester-functionalized superparamagnetic nanospheres. Wide scope of synthesis for other kinds of functional magnetic polymer nanospheres. The modification bilayer is the key factor controlling the encapsulation of products. Potential application of biomedical field.

  4. Comment on "High-temperature soft magnetic properties of antiperovskite nitrides ZnNFe3 and AlNFe3" by Yankun Fu, Shuai Lin, and Bosen Wang, J. Magn. Magn. Mater. 378 (2015) 54-58 (United States)

    Scholz, T.; Leineweber, A.; Dronskowski, R.


    The authors of the aforementioned manuscript have recently claimed the synthesis of the ternary nitrides ZnNFe3 (=ZnFe3N) and AlNFe3 (=AlFe3N), ordered substituted variants of the binary phase γ'-Fe4N [1]. While soft ferromagnets of such kind are presently attracting lots of attention, their history dates back for more than half a century. In particular, Al-substituted γ'-Fe4N has already been mentioned in 1961 [2], and the existence of AlFe3N has also been claimed in 2009 [3] from a two-step ammonolysis reaction combining a high-temperature sintering step and a low-temperature nitriding reaction [4]. Nonetheless, one of us had to withdraw the latter claim after finding out, by means of scanning-electron microscopy and elemental mapping, that all samples of "AlFe3N" consisted of an intimate solid mixture of γ'-Fe4N and amorphous Al2O3[5]. From what follows, we have strong reasons to believe that the authors of Ref. [1] overlooked our findings [5] and also did not synthesize ZnFe3N and AlFe3N.

  5. The Reaction and Applied Study of the Amide and P2S5

    Institute of Scientific and Technical Information of China (English)

    Guan zuowu; Ma Zhuang; Liu Xing; Cheng Tie-ming


    It is usually reported that reaction between carbonyl and P2S5 produce thiono group compound. The Products from carbonyl after ammonolysis and hydrazinolysis have the very import applied value in the synthesize of heterocyclic compound. Sulfuration reation if a nucleophilic attack,SPS2 anionsid obtained from P2S5 in the organic sovent, rather easier than thereationsof scheeren's reagent. The reation mechanism is as follows:The reation speed has something todo with the electronegative of R1R2 can be aliphatic group or aromatic group. The reaction can take place in the polar solvent or non-polar solent.But it is seldom reported that cyclic amide can be sulfured. In 1964, G.A, Archer et made the 7-chloro-1,3-dihyhro-5-phenyl 2H-1,4-ebnzodiazepin-2-thioue and in the reation of pyridine solent with 7-chloro-1,3-dilydro-5-phenyl-2H-1,4-benzodiazepin-2-one and P2S5. And the yield rate reached 40%. This reaction is very important in the pharmaceutical compound, but has quite low yield rate and high cost with present method. And the application is restricted duo to the pyridine,but it is a feasible way indeed. So we undertook further the deep studyof this, made P2S5 catalytic sulfurization in the proper solvent. And the yield rate of the reation has raised a lot. The quality of this product has been affirmed by UV. IR. 1HMNR.MS chart. This method successfully has been applied for the pharmaceutical compound, such as, Estazolam, Trithlozine Alprazolam, Triazolam Clozapine. This has been applied for manufacturing with obvious economic and social benefit.

  6. Synthesis of Pepper Acid Hexamethylene Diamine%胡椒酸己二胺的合成

    Institute of Scientific and Technical Information of China (English)

    吐尔孙拜克·叶尔达; 赵静; 纳森巴特


    Piperic acid(2) was prepared by reaction of piperine with KOH , and then acidification. Ethyl piperic acid(3) was prepared by reaction of 2 with ethanol.Pepper acid hexanediamine (4) was obtained by ammonolysis of 3 with hexamethylene diamine catalyzed by sodium .The structure was con-firmed by 1 H NMR, 13 C NMR and IR.The optimum reaction conditions for synthesizing 4 were as fol-lowed:The catalyst dosage was 2 wt%, n(3)∶n(hexamethylenediamine ) =0.6, reaction at 65~75℃for 48 h, the yield was 83 .5%.The process was magnified by ten times on the micro experiment , the yield was above 79%.%以胡椒碱为起始原料,与KOH反应生成胡椒酸钾盐,经酸化后制得胡椒酸(2);2与乙醇经酯化反应制得胡椒酸乙酯(3);3与己二胺在金属钠催化下经氨解反应合成了胡椒酸己二胺(4),其结构经1H NMR,13C NMR和IR确证。合成4的最佳反应条件为:催化剂用量2 wt%, n(3)∶n(己二胺)=0.6, m(乙醇)∶m(3)=2.5,于65~75℃反应48 h,收率83.5%。该工艺在微型实验基础上放大十倍,收率大于79%。

  7. 香豆素杯[4]芳烃的合成及其锌(Ⅱ)配合物的光谱%Synthesis of Coumarin- Calix[ 4 ] arene Derivative and Spectral Properties of Its Zn(Ⅱ) Complex

    Institute of Scientific and Technical Information of China (English)

    王飞; 张晓梅; 徐国财


    为探寻对过渡金属离子具有配合作用的新型超分子配体,将杯[4]芳烃经醚化、氨解得到的中间体3与香豆素-3-甲酰氯反应,合成了新的合香豆素片段的杯[4]芳烃配体H2L,用1 HNMR、13CNMR、IR、MS( Maldi - Tof)表征其结构.H2L与醋酸锌反应,获得了相应锌(Ⅱ)配合物(LZn),元素分析及MS( ESI)分析结果表明,LZn的化学组成为L(ZnAc)2·2H2O.研究了锌(Ⅱ)配合物的UV和IR吸收光谱性质,还测定了它的荧光强度.结果表明,与H2L相比,锌(Ⅱ)配合物分子中共轭体系增大且平面刚性增加.%In order to seek a new supramolecular ligand with the capacity for coordination to transition metal I-ons, a new calix[4]arene derivative H2L with coumarin sections was synthesized by the reaction of coumarin -3 -formyl chloride with intermediater 3 prepared by etherification firstly and then ammonolysis of calix[4]arene, and its structure was characterized by 1HNMR, 13C NMR, IR and MS (Maldi -Tof). Reacting H2L with zinc acetate could produce a Zn(II) complex (LZn) , and the chemical composition of LZn was L(ZnAc)2 · 2H2O determined by elementary analysis and MS (ESI). Using IR and UV, the absorption spectra of LZn were studied, and the fluorescence intensity was examined also. Results showed that conjugation system in LZn was enlarged and plane rigidity increased by comparison with those in H2L.

  8. Composition-induced structural, electrical, and magnetic phase transitions in AX-type mixed-valence cobalt oxynitride epitaxial thin films

    Energy Technology Data Exchange (ETDEWEB)

    Takahashi, Jumpei; Oka, Daichi [Department of Chemistry, School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo, Tokyo 113-0033 (Japan); Kanagawa Academy of Science and Technology (KAST), 3-2-1 Sakado, Takatsu, Kawasaki 213-0012 (Japan); Hirose, Yasushi, E-mail:; Yang, Chang; Fukumura, Tomoteru; Hasegawa, Tetsuya [Department of Chemistry, School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo, Tokyo 113-0033 (Japan); Kanagawa Academy of Science and Technology (KAST), 3-2-1 Sakado, Takatsu, Kawasaki 213-0012 (Japan); CREST, Japan Science and Technology Agency, 7-3-1 Hongo, Bunkyo, Tokyo 113-0033 (Japan); Nakao, Shoichiro [Kanagawa Academy of Science and Technology (KAST), 3-2-1 Sakado, Takatsu, Kawasaki 213-0012 (Japan); CREST, Japan Science and Technology Agency, 7-3-1 Hongo, Bunkyo, Tokyo 113-0033 (Japan); Harayama, Isao; Sekiba, Daiichiro [University of Tsukuba Tandem Accelerator Complex (UTTAC), 1-1-1 Tennoudai, Tsukuba, Ibaraki 305-8577 (Japan)


    Synthesis of mid- to late-transition metal oxynitrides is generally difficult by conventional thermal ammonolysis because of thermal instability. In this letter, we synthesized epitaxial thin films of AX-type phase-pure cobalt oxynitrides (CoO{sub x}N{sub y}) by using nitrogen-plasma-assisted pulsed laser deposition and investigated their structural, electrical, and magnetic properties. The CoO{sub x}N{sub y} thin films with 0 ≤ y/(x + y) ≤ 0.63 grown on MgO (100) substrates showed a structural phase transition from rock salt (RS) to zinc blend at the nitrogen content y/(x + y) ∼ 0.5. As the nitrogen content increased, the room-temperature electrical resistivity of the CoO{sub x}N{sub y} thin films monotonically decreased from the order of 10{sup 5} Ω cm to 10{sup −4} Ω cm. Furthermore, we observed an insulator-to-metal transition at y/(x + y) ∼ 0.34 in the RS-CoO{sub x}N{sub y} phase, which has not yet been reported in Co{sup 2+}/Co{sup 3+} mixed-valence cobalt oxides with octahedral coordination. The low resistivity in the RS-CoO{sub x}N{sub y} phase, on the 10{sup −3} Ω cm order, may have originated from the intermediate spin state of Co{sup 3+} stabilized by the lowered crystal field symmetry of the CoO{sub 6−n}N{sub n} octahedra (n = 1, 2,…5). Magnetization measurements suggested that a magnetic phase transition occurred in the RS-CoO{sub x}N{sub y} films during the insulator-to-metal transition. These results demonstrate that low-temperature epitaxial growth is a promising approach for exploring novel electronic functionalities in oxynitrides.

  9. 丙酮氨氧化制备丙酮肟过程中副反应研究%Study on the Side Reaction in Acetone Oxime Synthesis from Ammoxidation of Actone

    Institute of Scientific and Technical Information of China (English)

    林勇; 张胜建; 罗署; 赵迎宪; 段云凤; 王毅


    Acetone oxime was prepared by catalytic ammoxidation of acetone over TS-1 zeolite. The structure of by-products from this synthetic process were characterization by GC-MS, LC-MS, etc. The types of side reactions were discussed in detail. The results showed that this reaction system mainly included the following side-reactions:(1) ketone condensation catalyzed by base to form skeletal structure of products;(2)nu-cleophilic ammonolysis of hydroxyl to form various organic amines, increase the alkalinity of the system raised, and enhance the side reaction by self-catalysis; (3)dehydration to form olefins, and then epoxidation by H2O2; (4) ketone oximation to form oximes; (5)oxidation-coupling of acetone oxime to form 2,3-dimethly-2,3-dinitro-butane(DMNB);(6) other oxidation processes to form various highly unsaturated by-products;etc.%通过GC-MS、LC-MS等方法表征TS-1催化丙酮氨氧化制备丙酮肟过程中的副产物结构,分析副反应类型。结果表明:在此反应体系中,副反应主要产生途径有:(1)碱催化酮缩合,导致副产物骨架的生成;(2)亲核氨解,生成各种有机胺,导致体系碱性增强,起到自催化的作用;(3)消除脱水生成烯烃,然后烯烃被H2O2环氧化;(4)酮类副产物肟化;(5)酮肟氧化偶联反应生成2,3-二硝基-2,3-二甲基丁烷(DMNB);(6)其它氧化过程生成不饱和度高的副产物等。

  10. Synthesis of oxiracetam derivatives and their nootropic activities%奥拉西坦衍生物的合成及其促智作用的研究

    Institute of Scientific and Technical Information of China (English)

    宋艳玲; 孙乔; 李柏娜; 刘晓娟


    目的:设计并合成一系列奥拉西坦衍生物,并对其促智作用进行研究。方法以氯乙酰乙酸乙酯为起始原料,通过还原、取代、环合、氨解反应得到目标产物。通过Morris水迷宫测试法测定小鼠的逃避潜伏期以评估小鼠的学习记忆能力。结果合成了3个目标化合物1~3,其结构经MS、1H-NMR确证。Morris水迷宫测试表明化合物1~3可明显缩短阿尔茨海默病(AD)小鼠的逃避潜伏期(P<0.01)。结论化合物1~3具有一定的促智活性,对进一步开展奥拉西坦衍生物的结构改造和促智作用研究提供参考。%Objective To design and synthesize a series of oxiracetam derivatives, and to assay their nootropic activities. Methods Chlorine ethylacetoacetate was used as starting material to synthesize the target compounds by reduction, alkylation, condensation, and ammonolysis reactions. To study the nootropic effects of target compounds, the escape latency was used to evaluate the memory ability of mice. Results The target compounds 1—3 were synthesized and characterized by MS and 1H-NMR. Water maze results showed that compounds 1—3 could shorten the escape latency of AD mice (P < 0.01). Conclusion Compounds 1—3 have the property of improving memory ability of mice, and provide some practical reference value for the further development on the structure modification of oxiracetam derivatives and nootropic activity.

  11. Multifaceted metabolomics approaches for characterization of lignocellulosic biomass degradation products formed during ammonia fiber expansion pretreatment (United States)

    Vismeh, Ramin

    Lignocellulosic biomass represents a rather unused resource for production of biofuels, and it offers an alternative to food sources including corn starch. However, structural and compositional impediments limit the digestibility of sugar polymers in biomass cell walls. Thermochemical pretreatments improve accessibility of cellulose and hemicellulose to hydrolytic enzymes. However, most pretreatment methods generate compounds that either inhibit enzymatic hydrolysis or exhibit toxicity to fermentive microorganisms. Characterization and quantification of these products are essential for understanding chemistry of the pretreatment and optimizing the process efficiency to achieve higher ethanol yields. Identification of oligosaccharides released during pretreatment is also critical for choosing hydrolases necessary for cost-effective hydrolysis of cellulose and hemicellulose to fermentable monomeric sugars. Two chapters in this dissertation describe new mass spectrometry-based strategies for characterization and quantification of products that are formed during ammonia fiber expansion (AFEX) pretreatment of corn stover. Comparison of Liquid Chromatography Mass Spectrometry (LC/MS) profiles of AFEX-treated corn stover (AFEXTCS) and untreated corn stover (UTCS) extract shows that ammonolysis of lignin carbohydrate ester linkages generates a suite of nitrogenous compounds that are present only in the AFEXTCS extract and represent a loss of ammonia during processing. Several of these products including acetamide, feruloyl, coumaroyl and diferuloyl amides were characterized and quantified in the AFEXTCS extracts. The total amount of characterized and uncharacterized phenolic amides measured 17.4 mg/g AFEXTCS. Maillard reaction products including pyrazines and imidazoles were also identified and measured in the AFEXTCS extract totaling almost 1 mg/g AFEXTCS. The total of quantified nitrogenous products that are formed during AFEX was 43.4 mg/g AFEXTCS which was equivalent

  12. Synthesis and chemistry of organoimidovanadium(V) compounds and their role in the formation of vanadium nitrides (United States)

    Gipson, Rocky Dean

    A series of vanadium(V) compounds of the formula (eta5-C 5Me5)V(NR)Cl2 (R = 1-adamantyl, tert-butyl, para-tolyl) have been prepared by the reaction of (eta5 -C5Me5)V(O)Cl2 with RNCO or by oxidation of [(eta5-C5Me5)VCl2] 3 with azide. The para-tolylimido compound undergoes chloride metathesis with monoanionic reagents NaOtBu, LiNEt 2, and Mg(CH2SiMe3)2 to produce mono- and disubstituted products. A discussion of ligand strength in this system using 51V NMR is presented. Ammonolysis of the dichloro compounds produces the symmetrically-bridged [(eta5-C5Me5)V(mu-N)Cl]2, in yields consistent with the basicity of the organoimido ligand. A comparison of this reactivity with that of (eta5-C5Me 5)V(NSiMe3)Cl2 is presented. An X-ray structural study of (eta5-C5Me5)V(NtBu)Cl 2 exhibits a 173° V-N-C imido linkage and V-N triple bond. Synthesis of (eta5-tBuC5H 4)V(NR)Cl2 compounds was performed utilizing (t-Bu)C 5H4SiMe3 as the cyclopentadiene reagent with V(NR)Cl 3. In contrast to the metathesis of V(NR)Cl3 compounds with Li(tBu)C5H4, reduction of the vanadium(V) is not observed. An X-ray crystal structure of (eta5- tBuC5H4)V(N-ptol)Cl2 reveals linear V-N-C bonding, and a short N-C bond of 139 pm. This is explained by delocalized bonding, which incorporates the imido carbon atoms as well as nitrogen and vanadium. Details of the structure and valence-bond descriptions are of this compound are presented. Organoimidotrichlorovanadium(V) compounds bind ligands L2 (L2 = 1,2-dimethoxyethane; N,N,N,N-tetramethylethylenediamine) to produce adducts V(NR)Cl3L2. The V(NR)Cl3L 2 compounds thermally react to form terminal nitrides V(N)Cl2L 2 via an unprecedented cleavage of the N-C bond of the organoimido ligand, with reactivity following the order t-butyl > 1-adamantyl > p-tolyl. The downfield 51V NMR shifts of the adducts relative to starting materials is discussed using crystal-field models. X-ray crystal structures of V(NAd)Cl3(DME) and V(N ptol)Cl3(TMEDA) are presented, and details

  13. Theme-Based Bidisciplinary Chemistry Laboratory Modules (United States)

    Leber, Phyllis A.; Szczerbicki, Sandra K.


    methanol to effect transesterification (3) and examining the effect of variations in leaf type and season on lipid composition. A second "Plant Assay" study involves preparing and characterizing analogs of naphthalene-1-acetamide, which is the active growth-promoting ingredient in commercial preparations such as Transplantone® and Rootone®. There are two direct methods for synthesizing the amide from the native plant growth regulator ("auxin") or carboxylic acid: acid-catalyzed hydrolysis of the nitrile or ammonolysis of the acid chloride derivative, prepared in situ from the acid by treatment with thionyl chloride (4). In the spring of 1996, organic chemistry students synthesized the amide derivatives of a number of auxins via the acid chloride intermediate, which is more efficiently prepared using oxalyl chloride (40-60% overall yield) instead of thionyl chloride (20-40% overall yield), or via nitrile hydrolysis (72-99% yield). Plant bioassays, based on measurement of pea stem segment elongation (5) have only been performed on the acetamide derivatives of three auxins, indole-3-acetic acid (IAA), naphthalene-1-acetic acid (1-NAA), and naphthalene-2-acetic acid (2-NAA). In comparison with the control, indole-3-acetamide and naphthalene-1-acetamide promoted growth by 50% and 90%, respectively. The acetamide of 2-NAA impeded growth by 30% relative to the control, an observation consistent with the known antiauxin activity of 2-NAA (6). Acquisition of the necessary imaging system for the teaching laboratory will enable students to extend these quantitative studies to other auxin conjugates. Acknowledgment We are grateful to the NSF for financial support through the Division of Undergraduate Education (DUE-9455693 and DUE-9550890). Literature Cited 1. Mayo, D. W.; Pike, R. M.; Trumper, P. K. Microscale Organic Laboratory, 3rd ed; John Wiley & Sons: New York, 1994; pp 202-203. 2. Browse, J.; McCourt, P. J.; Somerville, C. R. Anal. Biochem. 1986, 152, 141. 3. Rodig, O. R