Preparation method and production device of high-purity ethyl cyanoformate

Abstract

The invention relates to a preparation method and a production device of high-purity ethyl cyanoformate. The preparation method comprises the following specific steps of: cleaning a reaction kettle, and adding 100KG of an S-1500 aromatic hydrocarbon solvent into the reaction kettle; adding 695KG of ethyl chloroformate and 175KG of hydrocyanic acid dropwise into the kettle; adding 30KG of a triethylamine catalyst and 20KG of purified water into the reaction kettle, starting the reaction kettle, performing stirring and mixing, and then closing the reaction kettle; lowering the temperature in thereaction kettle to 2DEG C, then starting the reaction kettle, and adding ethyl chloroformate and hydrocyanic acid dropwise under low-speed stirring; further performing stirring for 30min at the end of dropwise adding to obtain an ethyl cyanoformate crude product, then transferring the ethyl cyanoformate crude product into a distillation tower, carrying out atmospheric distillation on the ethyl cyanoformate crude product, and removing fractions before 90DEG C to obtain colorless fuming fractions at 115-116DEG C; carrying out cyanation reaction on the raw materials and distillation separation of ethyl cyanoformate, and then performing split-phase washing to recover the catalyst. Compared with the prior art, the method improves the quality of the ethyl cyanoformate finished product, and is easy for industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for preparing high-purity ethyl cyanoformate and a production device thereof. Background technique [0002] Ethyl cyanoformate, molecular formula C 4 h 5 NO 2 , a colorless transparent liquid, is a very important chemical intermediate, as a raw material for organic synthesis, it is widely used in the fields of medicine, pesticide, chemical industry and textile, and can be used to produce esters, amides and heterocyclic compounds and synthesize Pharmaceuticals, herbicides, fungicides, insecticides, and many other chemicals can also be used as intermediates in the synthesis of the anti-infective drug cefazolin and in the synthesis of tetrazoleacetic acid, ethyl cyanoformate often passes through green The cyanidation method of ethyl formate is synthesized, such as using ethyl chloroformate and metal cyanide as raw materials for synthesis, using ethyl chloroform...

AI Technical Summary

Problems solved by technology

[0002] Ethyl cyanoformate, molecular formula C 4 h 5 NO 2 , a colorless transparent liquid, is a very important chemical intermediate, as a raw material for organic synthesis, it is widely used in the fields of medicine, pesticide, chemical industry and textile, and can be used to produce esters, amides and heterocyclic compounds and synthesize Pharmaceuticals, herbicides, fungicides, insecticides, and many other chemicals can also be used as intermediates in the synthesis of the anti-infective drug cefazolin and in the synthesis of tetrazoleacetic acid, ethyl cyanoformate often passes through green The cyanidation method of ethyl formate is synthesized, such as using ethyl chloroformate and metal cyanide as raw materials for synthesis, using ethyl chloroformate and trimethylcyanosilane as raw materials for synthesis, but due to extremely harsh reaction conditions and A large amount of or high-cost raw material consumption leads to difficulty in industrialized production and the purity of the finished product of ethyl cyanoformate is low, so it is necessary to make improvements

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