摘要
采用精馏-结晶法分离以环己酮为原料合成十二烷二酸二甲酯的粗品,探讨了各种工艺条件对结晶分离的影响。结果表明:结晶分离最佳工艺条件为:m(精馏双酯):m(甲醇)=1:0.8～1.5,结晶溶液始温30℃左右,终温5～8℃,降温速率2～3℃/min,搅拌速度5～25r/min;结晶母液中甲醇可通过蒸馏回收循环使用,残留双酯返回精馏系统。所得十二烷二酸二甲酯的纯度可达99.5%以上,符合医药中间体、香料等行业的使用要求。
Raw dodecanedioic acid dimethyl ester is synthesized from cyclohexanone through separation by rectification and crystallization. Effect of various process conditions on crystallization separation are studied. Results show that the best conditions for crystallization separation is:m(rectification diester):m(methanol)=1:0.8-1.5, starting temperature of the crystallization solution at about 30 ℃, ending temperature at 5-8℃, temperature drop rate 2-3 ℃/min, stirring rate at 5-25 r/min; methanol in the crystallization mother liquid can be recycled and reused, the remaining diester is recycled to the rectification system. Resultant dodecanedioic acid dimethyl ester is over 99.5% in purity, which meets the requirements of medicine intermediates and flavorand has a value to be promoted.
出处
《化工生产与技术》
CAS
2007年第3期26-28,共3页
Chemical Production and Technology
关键词
十二烷二酸二甲酯
环己酮
精馏
结晶
分离
dodecanedioic acid dimethyl ester
cyclohexanone, rectification
crystallization
separation
