摘要
在阐述二甲苯麝香物理性质、应用以及对生物与环境影响作用的基础上,采用三步法合成了二甲苯麝香,旨在对二甲苯麝香做更深入的环境毒理性探索和监控生产提供依据.第一步,盐酸与叔丁醇反应合成烷基化剂——叔氯丁烷,产品直接从反应器中蒸出,叔氯丁烷的产率为89.58%;第二步,叔氯丁烷在无水三氯化铝催化下与间二甲苯作用合成中间体——叔丁基间二甲苯;正交试验得出优化工艺条件为:间二甲苯∶叔氯丁烷∶无水三氯化铝(摩尔比)为8∶1∶0.04,反应温度0℃,反应时间4h,叔丁基间二甲苯的产率为86.97%;第三步,叔丁基间二甲苯在0℃、混酸作用下硝化制得二甲苯麝香,以间二甲苯计二甲苯麝香的总收率为65.00%.主要产品的化学结构由熔点和红外光谱得到表征.
After expounding Musk xylene＇s nature, application and influence on the life and environment, the synthesis of musk xylene was carried out by three - step method in order to monitor the production process of suppliers. At first, tert - butyl chloride-the alkylation＇s agent, was synthesized by hydrochloride acid reacting with tert - butyl alcohol. Relatively high yield 89. 58% was got by controlling the reaction temperature higher than tert - butyl chloride＇s boiling point, and then the product-tert - butane chlorinated was being distillated out of the reactor directly when the reaction happened. At the second step, tert - butyl - m - xylene was synthesized by reacting chlorinate tert - butane with m - xylene in the presence catalyst of anhydrous aluminum chloride. Based on orthogonal test, the suitable conditions were established. The optimum reaction conditions were as follows ： Molecule ratio of m - xylene/chlorinated tert - butane/anhydrous aluminum chloride molar 8：1：0. 04, reaction temperature 0℃ , reaction time 4h, and the yield of product was about 86. 97%. The total yield of musk xylene is about 65.00% based on the amount of m - xylene. The chemical structure of the main products are characterized by IR and melt point.
出处
《嘉兴学院学报》
2009年第6期13-17,共5页
Journal of Jiaxing University
关键词
二甲苯麝香
物性
应用
生物与环境效应
合成
红外
musk xylene
nature
application
environmental ＆ ecological effect
synthesis
IR
