期刊文献+
任意字段
题名或关键词
题名
关键词
文摘
作者
第一作者
机构
刊名
分类号
参考文献
作者简介
基金资助
栏目信息

三氧化硫脲制备中纯度分析及其表征 被引量：1

Purity Detection and Characterization During Preparating of Thiourea Trioxide
下载PDF
导出
摘要 以H2O2为氧化剂氧化二氧化硫脲制备三氧化硫脲.运用HPLC对产物进行纯度分析,考查了反应物配比、温度、时间和酸浓度以及重结晶方法对产物收率和纯度的影响.得出最佳反应条件:使用12 mol/L浓硫酸的酸性环境,二氧化硫脲与双氧水的摩尔比是1:1.5,在50～60℃反应100 min.产品用无水乙醇重结晶3次得到最终产物,其收率为85.83%,纯度为98.03%.用FTIR,V-Vis,S对产品进行了表征. Thiourea trioxide was synthesized by oxidation of thiourea dioxide with H2O2. Effects of mole ratio of reactants, reaction temperature, reaction time, concentration of acids and methods of re-crystallining on yield and purity of product were discussed with high performance liquid chromatography （HPLC）. The optimal reaction conditions are mole ratio of H2O2 to thiourea dioxide of 1.5, temperature of 50-60 C, time of 100 min and concentration of acids of 12 mol/L. After re-crystallining three times with anhydrous ethanol, the product＇s yield and purity is 85.83% and 98. 03%, respectively. Structure of product was confirmed by fourier transform infrared spectrophotometer （FTIR）, ultraviolet and visible spectrophotometry （UV-Vis） and mass spectrometry （MS）.
作者 吕小丽 高庆宇 陆永超 韦芳芳 刘兵
机构地区 中国矿业大学化工学院
出处 《中国矿业大学学报》 EI CAS CSCD 北大核心 2005年第6期784-788,共5页 Journal of China University of Mining & Technology
基金 国家自然科学基金项目(20103010) 教育部优秀青年教师资助计划(2002-2117)
关键词 三氧化硫脲 制备 PLC 纯度检测 thiourea trioxide preparation HPLC purity detection
分类号 O612.6 [理学—无机化学]
  • 相关文献

参考文献11

  • 1Kim K,Lin Y T,Mosher H S. Monosubstituted guanidines from primary amines and aminoiminom ethanesulfonic acid[J]. Tetrahedron Lett,1988,29:3183-3186.
  • 2王舜,高庆宇,林娟娟,尹文萱,刘兵,程勇.硫脲氧化反应的热效应[J].中国矿业大学学报,2004,33(4):375-378. 被引量：4
  • 3Morei A,Cohen B D,Lowenthal A. Historical,bi-ological,biochemical,and clinical aspects of thenaturally occurring guanidino compounds[M]. New York:Plenum,1983.
  • 4Greenhill J L,Lue P. Progress in medicinal chemi-stry[M]. NewYork:Elsevier Science,1993.
  • 5Thompson A,Schaefer J,Kuhn K,et al. Tandem mass tags:A novel quantification strategy for comparative analysis of complex protein mixtures by MS/MS[J]. Analytical Chemistry,2003,75(18):4942-4947.
  • 6Miller A E;ischoff J J. Chemistry of metabolites of thioureas[J]. Advances in Experimental Medicine and Biology,1986,197:925-929.
  • 7Sergei V,Makarov C M,John H P,et al. Structure and stability of aminoiminomethanesulfonic acid[J]. Inorganic Chemica Acta,1999,286:149-154.
  • 8Schaefer A,Kuhn J,Kienle K,et al. Synthesis hy-groscopicity and moisture retention of chitosguanidine sulfate[J]. Analytical Chemistry 2001,35(18):465-471.
  • 9Miller A E,Bischoff J J,Chemistry of metabolites of thioureas[J]. Advances in Experimental Medicine and Biology,1986,197:925-929.
  • 10Simoyi R H. New bromate oscillator:the bromateth-iourea reaction in a CSTR[J]. Journal of Physical Chemistry,1986,90(13):2802-2804.

二级参考文献17

  • 1张国政,郑淑娴,卢冠忠.硫脲与过氧化氢合成二氧化硫脲过程的热效应[J].华东理工大学学报（自然科学版）,1996,22(2):206-210. 被引量：4
  • 2Gherrou A, Kerdjoudj H. Cyanide as a copper leach-ing agent for the remediation of fouling of a supported liquid membrance by formamidine disulphide in thiourea medium[J]. Desalination, 2003, 158: 195-200.
  • 3Ferreira J T B,De Oliveira A R M,Comasseto J V. A convenient method of synthesis of diakyltellurides and dialkylditelluides[J]. Synth Commun, 1989, 1(1): 239-244.
  • 4Comasseto J V, Long E S, Ferreira J T B, et al. The use of aminoiminomethanesulfinic acid (thiourea dioxide) under phase transfer conditions for generating organochalcogcnate anions: Synthesis of sulfides selenides and tellurides[J]. J Organo-metal, Chem., 1987, 334: 329-340.
  • 5Robertson J G, Sparvero L J, Villafranca J J. Inactiv-ation and covalent modification of CTP synthetase by thiourea dioxide[J]. Protein Sci, 1992, 1: 1298-1307.
  • 6Robertson J G. Determination of subunit dissociation constants in native and inactivated CTP synthetase by sedimentation equilibrium[J]. Biochemistry, 1995, 34: 7533-7541.
  • 7Arifoglu M, Marmer W N, Dudley R L. Investig-ation of the reaction of thiourea with hydrogen peroxide using 13C NMR spectroscopy. Insights into an oxidative/reductive bleaching process[J]. Text Res J, 1992, 62: 94-100.
  • 8Maryanoff C A, Stanzione R C, Plampin J N, et al. convenient synthesis of guanidines from thioureas[J]. J Org Chem, 1986, 51(10): 1882-1884.
  • 9Morei A, Cohen B D, Lowenthal A. Historical, biological, biochemical, and clinical aspects of the naturally occurring guanidino compounds[M]. New York: Plenum,1983.
  • 10Greenhill J L, Lue P. In progress in medicinal chem-istry[M]. Ellis G P, Luscombe D K, Eds. New York: Elsevier Science,1993.

共引文献3

同被引文献16

  • 1Omer B P, Hamilton A D. The guanidinium group in molecular recognition: design and synthetic approaches [J]. Journal of Inclusion Ph enomena and Macrocyclic Chemistry, 2001, 41 : 141 - 147.
  • 2Kane J M. Newer antipsyehotic drugs: A review of their pharmacology and therapeutic potential [J]. Drug 1993, 46(4) : 585 - 589.
  • 3Hiroyuki A, Takeshi I. Preparation of sparingly water soluble salts of dodecylguanidine as antifouling agents against marine organisms [P]. JP: 04225945, 1992-08-14.
  • 4Mitamura J. Hair preparations containing guanidine derivatives and higher alcohols [P]. JP: 05194150, 1993-08-03.
  • 5Matthias P. Use of alkyl guanidine compounds for the treatment and after-treatment of hair [P]. US: 2004258651, 2004-12-23.
  • 6Lepain A, Bronchart R. Compositions and method for eliminating fdms of oil on the surface of water [P]. BE: 895 840,1982- 09-19.
  • 7Boemer Horst, Rieder Georg, Solle Alfred. Guanidine fungicides [P]. DE:3 606 294,1986.
  • 8Mitamura, J. Hair preparations containing guanidine derivatives and higher alcohols [P]. JP: 05 194 150, 1993.
  • 9Srivastaca S K. Smith T A. The inhibition of growth in higher plants by a homologous series of guanidines and its reversal by sper-mine [J]. Ann Bot, 1982,50 (2):265- 275.
  • 10Schuchardt U. Vargas Rogerio Matheus, Gelbard Georges: Alkylguanidine as catalysts for the lransesterification of rapeseed oil[j]. Jnd Catal A: Chem, 1995,99 (2):65- 70.

引证文献1

二级引证文献1

中国矿业大学学报
2005年 第6期

相关作者

内容加载中请稍等...

相关机构

内容加载中请稍等...

相关主题

内容加载中请稍等...

浏览历史

内容加载中请稍等...
;
使用帮助 返回顶部