N-叔丁基-2-苯骈噻唑次磺酰胺制备及其光谱分析  

Study on the Preparation of N-Tert-Butylbenzothiazole-2-Sulphenamide and Its Spectral Analysis

作　　者：贾太轩[1] 宋国全 郭尧[1] 赵凌[1] 田大勇[1] 侯绍刚[1] 

机构地区：[1]安阳工学院化学与环境工程学院,河南安阳455000 [2]迈奇化学股份有限公司,河南濮阳457000

出　　处：《光谱学与光谱分析》2016年第7期2213-2216,共4页Spectroscopy and Spectral Analysis

基　　金：国家自然科学基金项目(U1404217);河南省高等学校重点科研项目(16B530001)资助

摘　　要：采用双氧水为氧化剂,一步法制备出N-叔丁基-2-苯骈噻唑次磺酰胺（TBBS）,通过FTIR,UVVis,XRD,TG-DSC对其进行检测和表征,揭示出TBBS的微观结构和内在规律性。FTIR揭示了TBBS分子内部的各元素之间的化学键键型,确定最终产物为TBBS。UV-Vis检测出TBBS在228.3,281.5,298.3nm有三个吸收峰,分别由n→σ^＊,π→π^＊,n→π^＊电子跃迁产生的,为企业TBBS产品质量检测,推测TBBS的结构提供实验依据。XRD从晶胞参数、晶面指数等晶体学数据,变换出TBBS晶体微观结构,完成TBBS物相组成和结构的定性鉴定。TG-DSC检测出TBBS的质量变化与热效应两种信息,TBBS的DSC曲线很复杂,53.3℃有一个很小的放热峰,由TBBS中所含少量叔丁胺的氧化产生;117.4,269.2,373.7℃存在三个吸热峰,分别是TBBS的相变峰和分解峰,TBBS分解温度偏高,为采用硫化仪研究TBBS的橡胶硫化性能提供参考。本研究为企业选定工作标准品,对TBBS工业化生产进行跟踪检测,评判TBBS的产品性能指标,填报立项TBBS化工行业标准的申报,撰写标准草案提供基础实验数据。In the study ,N-tert-butylbenzothiazole-2-sulphenamide （TBBS） was synthesized with one-step method with hydrogen peroxide as the oxidant .TBBS was detected and characterized with FTIR ,UV-Vis ,XRD and TG-DSC .Its micro-structure and intrinsic regularity were revealed .Chemical bond types into TBBS molecule were revealed with FTIR .The final product was de-termined TBBS .Three absorption peaks were detected by UV-Vis at 228 .3 ,281 .5 ,298 .3 nm respectively ,due to n→σ^＊ ,π→π^＊ ,n→π^＊ electronic transitions .It could provide experimental basis with enterprise to test TBBS product quality and speculate its structure .The phase composition and structure of TBBS were revealed by crystallographic data from XRD detecting such as cell parameters ,crystal face index .The phase composition and qualitative identification of TBBS structure were completed .Two kinds of information were detected by TG-DSC as quality change and thermal effect .The DSC curve of TBBS was very complex . There were a small absorption peak of 53.3 ℃ as a small amount of tert-butylamine containing in TBBS was oxidized .Three ex-othermic peaks of 117.4 ,269.2 ,373.7 ℃ ,due to transition peak and decomposition phase of TBBS respectively .The decompo-sition temperature of TBBS was very high .It could provide reference for research on rubber vulcanizing properties by TBBS on rubber vulcanizing machine .This study could provide the basis experimental data on the enterprises to designate the working standard tracing detection of TBBS industrialized production .The performance index of TBBS was judged .The project of TBBS industry standard could be declared by the enterprises ,written a draft standard .

关 键 词：N-叔丁基-2-苯骈噻唑次磺酰胺 FTIR UV-VIS XRD TG-DSC 

分 类 号：O657.3[理学—分析化学]