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作 者:张怀敏 张文生 闫建波 Zhang Huai-min;Zhang Wen-sheng;Yan Jian-bo(Lian Zhong Xing Ye chemical Co.,LTD,Henan Puyang 457000)
机构地区:[1]濮阳市联众兴业化工有限公司,河南濮阳457000
出 处:《江西化工》2020年第2期24-27,共4页Jiangxi Chemical Industry
摘 要:本实验依据次磺酰胺的N-酰化反应机理,采用N-叔丁基-2-苯并噻唑次磺酰胺、乙酸酐为起始原料,经反应合成目标产物N-叔丁基-双(2-苯并噻唑)次磺酰胺(TBSI).首先,根据实验方案探索性合成目标产物TBSI,将保温过后的产物进行溶解,然后洗涤,再进行重结晶,最后干燥,将最后处理过的产物进行检测等步骤.目标产物TB-SI分别采用FTIR,HPLC,XRD,TG-DTA,1 HNMR进行检测分析,FTIR检测得出TBSI的化学键型,HPLC检测得出TBSI的纯度为95.615%.TG-DTA检测得出TBSI的分解温度为368.5℃,TBSI分解温度十分高,拥有长时间的耐焦烧.对TBSI进行了分析检测,得到了目标产物TBSI作为橡胶硫化促进剂的各项指标,所得数据具有很高的实用价值,对TBSI的工业化生产有一定的指导意义.In this dissertation vulcanization accelerator TBSI had been synthesized according to N-amidization mechanism of sulfenamide.The main reaction materials were N-tert-Butyl-2-benzothi azolesulfenimide(NS)and acetic anhydride.After certain reaction processes,objective product was synthesized.The heat-treated product is dissolved,then washed,recrystallized,finally dried,and the final treated product is subjected to detection and the like.TBSI was detected by FTIR,HPLC,XRD,TG-DTA,1HNMR.The purity of TBSI was 95.615%by HPLC.The TG-DTA test shew that the decomposition temperature of TBSI was 368.5℃.TBSI had a very high decomposition temperature in the industry and had a long-term scorch resistance.As a new vulcanization accelerator,TBSI also had been determined.The target product TBSI was analyzed and tested,and the obtained data has high practical value,which would have certain guiding significance for the industrial production of TBSI.
关 键 词:N-叔丁基-双(2-苯并噻唑) 次磺酰胺(TBSI) FTIR HPLC XRD TG-DTA 1HNMR
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