NS-乙酸酐法制备TBSI及其光谱分析

Preparation of TBSI with NS-Acetic Anhydride Method and Its Spectral Analysis

研究采用乙酸酐为溶剂,NS-乙酸酐法制备N-叔丁基-双(2-苯并噻唑)次磺酰胺(TBSI),通过FTIR,XRD,UV-Vis和TG-DTA对其进行检测和表征,揭示出TBSI的微观结构和内在规律性。FTIR揭示了TBSI分子内部各元素之间的化学键键型。XRD从晶胞参数、晶面指数等晶体学数据,变换出TBSI晶体微观结构,完成TBSI物相组成和结构的定性鉴定。UV-Vis检测出了TBSI在228.3,281.3和298.3nm有三个吸收峰,分别为TBSI分子中的n→σ*,π→π*,n→π*的电子跃迁产生的,为企业TBSI产品质量检测,提供了基础数据。TG-DTA检测出TBSI的质量变化与热效应两种信息,DSC曲线在46.5,188.9和368.5℃分别出现了吸收峰,46.5℃吸收峰是样品残留少许溶剂的挥发产生的,188.9和368.5℃分别为相变峰和分解峰,TBSI分解温度偏高,为采用硫化仪研究TBSI的橡胶硫化性能提供参考。研究为企业选定工作标准品,对TBSI工业化生产进行跟踪检测,评判TBSI的产品性能指标,填报立项TBSI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-t-butyl-2-benzothiazole sulfenimide （TBSI）was prepared by NS-acetic anhydride method with acetic anhydride as solvent.It was detected with FTIR,XRD,UV-Vis,TG-DTA.Micro-structure and essence disciplinarian of them were disclosed.Chemical bond types into TBSI molecule were revealed with FTIR.TBSI phase composition and structure were revealed with crystallographic data from XRD detecting such as cell parameters and crystal face index.The phase composition and qualitative identification of TBSI structure were completed.The absorption peaks were detected by UV-vis at 228.3,281.3 and 298.3 nm,respectively caused by n→σ,π→π,n→π electron transition.It could provide basic data with the enterprise of ZBPD product quality inspection.Two kinds of information were detected with TG-DTA as quality change and thermal effect. There were three absorption peaks of 46.5,188.9,368. 5 ℃ due to a few residual solvent volatilization in the sample,phase transition peak and decomposition peak.The decomposition temperature of TBSI was very high.It could provided reference with research on rubber vulcanizing properties with TBSI on rubber vulcanizing machine.This study could provide basis experimental data on the enterprises to designate the working standard tracing detection of TBSI industrialized production.Performance index of TBSI was j udged.The proj ect of TBSI industry standard could be declared by the enterprises,written a draft standard.