医药级橡胶硫化促进剂DM的精制工艺研究  

Refining process of pharmaceutical grade rubber vulcanization accelerator DM

作　　者：许宝明 王欣辉 王娜 代振旭 张恒 XU Baoming;WANG Xinhui;WANG Na;DAI Zhenxu;ZHANG Heng(College of Marine Science and Biological Engineering,Qingdao University of Science&Technology,Qingdao Shandong 266042;Guangdong Provincial Key Lab of Green Chemical Product Technology,Guangzhou Guangdong 510641)

机构地区：[1]青岛科技大学海洋科学与生物工程学院,山东青岛266042 [2]广东省绿色化学产品技术重点实验室,广东广州510641

出　　处：《首都师范大学学报（自然科学版）》2023年第3期36-40,共5页Journal of Capital Normal University：Natural Science Edition

基　　金：山东省自然科学基金项目(ZR2022MB135);广东省绿色化学产品技术重点实验室开放基金资助项目(GC202112)。

摘　　要：医药级2,2’-二硫化二苯并噻唑(2,2’-dibenzothiazoledisulfde,DM)是一种重要的医药中间体,可由工业级的橡胶硫化促进剂DM精制而成。为了更高效地生产医药级DM,本文采用多种溶剂耦合吸附剂对DM粗品进行了精制提纯,研究了不同溶剂、吸附剂、溶剂的循环次数对精制后DM熔点的影响。实验结果表明,以四氯乙烯为溶剂、活性炭为吸附剂的实验效果最佳,制得的DM熔点为180.1~182.6℃、纯度为99.48%,完全达到医药级DM的产品标准,溶剂循环使用次数以1~2次为宜。本文的重结晶-吸附耦合工艺能有效精制DM,重结晶的溶剂可以重复使用,工艺过程对环境污染较小,所得产物纯度高,是一种绿色、高效、低成本的生产医药级DM的生产工艺。Pharmaceutical grade 2,2'-dibenzothiazoledisulfde(DM)is an important pharmaceutical intermediate that can be refined from industrial grade rubber vulcanization accelerator DM.In order to produce pharmaceutical grade DM more efficiently,the crude DM was refined and purified by using various solvent-coupled adsorbents in this paper.And the effects of different solvents,adsorbents,and the number of solvent cycles on the melting point of DM after refining were investigated.The experimental results showed that tetrachloroethylene was the best solvent and activated carbon was the adsorbent.The melting point of DM produced was 180.1 to 182.6℃,and the purity was 99.48%,which fully met the standard of pharmaceutical grade DM.The number of solvent cycles was one.This recrystallization-adsorption coupling process can effectively refine DM.The recrystallized solvent can be reused.The process is less polluting to the environment,and the purity of product is high,which is a green,efficient and low-cost production process for pharmaceutical grade DM.

关 键 词：医药级橡胶硫化促进剂DM 精制 吸附 重结晶 工艺研究 

分 类 号：O6-322[理学—化学] TQ460.4[化学工程—制药化工]