甲萘威制备的非四氯化碳工艺研究.pdf

甲萘威制备的非四氯化碳工艺 * 官桂玉，孟洪，李春喜,王子镐 北京化工大学化学工程学院, 北京，100029 摘要：针对由甲基氨基甲酰氯(MCC)制备甲基异氰酸酯(MIC)后，再由MIC 制备甲萘威的非四氯化碳工艺进 行研究。选用甲苯、氯仿、四氯乙烯三种溶剂替代四氯化碳，同时在MCC 制备MIC 的工段引入有机碱除去 HCl；并对甲萘威的合成条件进行优化。条件优化后，对溶剂和缚酸剂进行选择。N-丁基咪唑为缚酸剂、氯 仿为溶剂时，甲萘威产率最高；而四氯乙烯为溶剂，N-丁基咪唑为缚酸剂时的BASIL 工艺，在操作方面既 省时省力、清洁简便，安全性又高。 关键词：甲基氨基甲酰氯；甲基异氰酸酯；甲萘威；BASIL 工艺 Process of preparing carbaryl without carbon tetrachloride Abstract ：The preparation of methyl isocyanate (MIC) by methyl carbamyl chloride (MCC) and the preparation of carbaryl by MIC was researched. During these two processes carbon tetrachloride was not used as solvent. Fistly, three solvents including toluene, chloroform and tetrachloroethylene were selected to substitute carbon tetrachloride. Meanwhile three kinds of organic alkalies including triethylamine, N-methyl imidazole(MIM), N- butyl imidazole(BIM) were selected to react with hydrochloric acid. Then influence factors of preparing carbaryl by MCC were investigated experimentally. Through the study on the influencing factors, the optimum condition had been determined. Under the optimum condition, the yield of carbaryl was the highest when the organic alkali was BIM. For a specified alkali, the yield of carbaryl in chloroform solvent was obviously higher than that in toluene solvent. When the organic alkali was BIM, the BASIL process could be applied in the reaction of decomposing MCC to prepare MIC. The used BIM can be reclaimed using sodium hydroxide, however, the water content in the recycled BIM was relatively high, which may reduce the yield of carbaryl. Pyrolytic process could be used to recover BIM from its hydrochloric salt via decomposing at high temperature. KEY WORDS: methy