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摘要
以邻苯二胺、二硫化碳为原料,在4-二甲氨基吡啶(DMAP)催化下合成了2-巯基苯并咪唑,然后加入氧化锌得到2-巯基苯并咪唑锌盐。考察了不同催化剂及其质量分数、反应介质、反应原料的摩尔比、成盐条件等对2-巯基苯并咪唑锌盐合成工艺的影响。结果表明,反应的最优工艺条件是:以水为反应介质,加入理论产量的1.0‰ DMAP催化剂,反应原料n(邻苯二胺)∶n(二硫化碳)∶n(氧化锌)=1∶1.5∶0.52,成盐反应温度为125~130℃。相对于传统工艺,该工艺反应时间短、操作简单、三废少,适合工业化规模生产。
Abstract
2-Mercaptobenzimidazole is synthesized from 1,2-diaminobenzene and carbon disulfide under the catalysis of DMAP (4-dimethylaminopyridine),and reacts with zinc oxide to obtain 2-mercaptobenzimidazol zinc salt.The effects of the types and dosages of catalyst,the reaction medium,the molar ratio of raw materials and salt-forming conditions on the synthesis of 2-mercaptobenzimidazol zinc salt are investigated.The optimum conditions are obtained as follows:water as the reaction medium,the dosage of DMAP catalyst is 0.1% of theoretical yield,n(1,2-diaminobenzene)∶n(carbon disulfide)∶n(zinc oxide)=1∶1.5∶0.52,and salt-forming reaction temperature is in the range of 125-130℃.Compared with traditional process,this process needs short reaction time,operates easily,generates less wastes,and is suitable for industrial scale production.
关键词
邻苯二胺
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DMAP
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2-巯基苯并咪唑锌盐
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2-巯基苯并咪唑
Key words
1,2-diaminobenzene
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4-dimethylaminopyridine
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2-mercaptobenzimidazole zinc salt
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2-mercaptobenzimidazole
Author summay
李合平(1979-),男,博士,副教授,研究方向为精细化学品研究,peaceli1984@126.com。
2-巯基苯并咪唑锌盐合成新工艺的研究[J].
现代化工, 2023, 43(8): 209-212 DOI:10.16606/j.cnki.issn0253-4320.2023.08.039