三氧化硫脲制备中纯度分析及其表征  

Purity Detection and Characterization During Preparating of Thiourea Trioxide

作　　者：吕小丽[1] 高庆宇[1] 陆永超[1] 韦芳芳[1] 刘兵[1] 

机构地区：[1]中国矿业大学化工学院,江苏徐州221008

出　　处：《中国矿业大学学报》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)

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）.

关 键 词：三氧化硫脲 制备 PLC 纯度检测 

分 类 号：O612.6[理学—无机化学]