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.
引文
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