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原釜羰基合成丙二酸二乙酯

Synthesis of Diethyl Malonate in Situ

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【作者】 谢荣锦刘泺王丽华

【Author】 XIE Rong-jin, LIU Luo, WANG Li-hua (Department of Chemical and Biochemical Engineering, Zhejiang University, Hangzhou 310027, China)

【机构】 浙江大学化学工程与生物工程学系浙江大学化学工程与生物工程学系 浙江杭州310027浙江杭州310027浙江杭州310027

【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。

【Abstract】 A powder of Fe-Mn alloy with cobalt chloride was fed in a reactor, and sodium thiosulfate and alcohol were added after carbon monoxid 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 1.5MPa, the optimal temperature is about 333K and the optimal reaction time is about 3hr . The synthesis of DEM is conducted according to the table of three factors and three level crisscross test . On the optimal condition of 363K , 1.6MPa , the molar ratio of ClCHCOOC2H5 : CH3CH2OH 1:3.7 and reaction time 5hr , the yield of DEM is about 95% .This process really simplifies the production of diethyl malonate.

  • 【文献出处】 高校化学工程学报 ,Journal of Chemical Engineering of Chinese Universities , 编辑部邮箱 ,2002年02期
  • 【分类号】TQ225.242
  • 【被引频次】10
  • 【下载频次】190
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