粗促进剂M钠盐合成促进剂TBBS新工艺的研究
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摘要
研究粗促进剂M钠盐(M-Na盐)合成促进剂TBBS新工艺。粗促进剂M经碱溶和甲苯萃取提纯后,在氧化剂次氯酸钠氧化下与叔丁胺反应生成促进剂TBBS的最佳反应条件:叔丁胺与M-Na盐的物质的量比为1. 03∶1,反应温度为40℃,此条件下反应收率在99%以上(按粗促进剂M折算);萃取剂甲苯直接套用最大次数为2,多次套用会影响促进剂TBBS的质量;经蒸馏回收后的甲苯可以套用,但需掺入50%的新甲苯才不影响产品质量。新工艺工序少,生产效率提高。
The new synthetic process of accelerator TBBS from the sodium salt of crude accelerator M was studied. Firstly,the crude accelerator M was purified by alkali solution and toluene extraction. Then accelerator TBBS was obtained by reaction between the sodium salt of accelerator M and tert-butylamine using sodium hypochlorite as oxidant. The optimal reaction conditions were as follows:the molar ratio of tertbutylamine to M sodium salt was 1. 03∶1,and the reaction temperature was 40 ℃. Under these conditions,the reaction yield was over 99%(based on crude accelerator M). Extractant toluene could be directly applied for 2 times at most,and more repeated application would affect the quality of accelerator TBBS. Toluene recovered by distillation could be applied,but it needed 50% of new toluene so that the product quality was not affected. The new process had fewer working procedures and higher production efficiency.
The new synthetic process of accelerator TBBS from the sodium salt of crude accelerator M was studied. Firstly,the crude accelerator M was purified by alkali solution and toluene extraction. Then accelerator TBBS was obtained by reaction between the sodium salt of accelerator M and tert-butylamine using sodium hypochlorite as oxidant. The optimal reaction conditions were as follows:the molar ratio of tertbutylamine to M sodium salt was 1. 03∶1,and the reaction temperature was 40 ℃. Under these conditions,the reaction yield was over 99%(based on crude accelerator M). Extractant toluene could be directly applied for 2 times at most,and more repeated application would affect the quality of accelerator TBBS. Toluene recovered by distillation could be applied,but it needed 50% of new toluene so that the product quality was not affected. The new process had fewer working procedures and higher production efficiency.
引文
[1]佚名.硫化促进剂M无废水工艺获突破[J].橡胶工业,2018,65(3):298.
[2]丁军委,孙国庆.粗2-巯基苯并噻唑合成促进剂N-环己基-2-苯并噻唑次磺酰胺的研究[J].精细石油化工,2008,25(5):47-50.
[2]丁军委,孙国庆.粗2-巯基苯并噻唑合成促进剂N-环己基-2-苯并噻唑次磺酰胺的研究[J].精细石油化工,2008,25(5):47-50.