摘要
在反应釜中,加入铁锰合金粉、氯化钴、硫代硫酸钠、乙醇及通入CO气体,制备四羰基钴钠。接着在同一反应釜中,加入氯乙酸乙酯及溶剂,合成了丙二酸二乙酯。该法极大地简化了生产工艺。
A powder of Fe-Mn alloy with cobalt chloride was fed in a reactor, and sodium thiosulfate and alcohol were added after carbon monoxide was introduced to synthesis sodium tetracarbonylcobaltate which was the catalyst of the following diethyl malonate syntheses in situ. Then methylbenzene was added and carbonylation of ethyl chloroacetate was followed to produce diethyl malonate (DEM) in the same reactor. For preparing catalyst, on pressure 1.5 MPa, the optimal temperature is about 333 K and the optimal reaction time is about 3 hr. The synthesis of DEM is conducted according to the table of three factors and three level crisscross test. On the optimal condition of 363 K, 1.6 MPa, the molar ratio of ClCHCOOC2H5:CH3CH2OH 1:3.7 and reaction time 5 hr, the yield of DEM is about 95%. This process really simplifies the production of diethyl malonate.
出处
《高校化学工程学报》
EI
CAS
CSCD
北大核心
2002年第2期194-197,共4页
Journal of Chemical Engineering of Chinese Universities
关键词
氰化法
四羰基钴钠
羰化法
丙二酸二乙酯
Carbonylation
Cobalt compounds
Cyanides
In situ processing
Optimization
Sodium compounds
