Process for synthesizing diacetylmonoxime ethyl ether by continuous reactions in microtube

Abstract

The invention discloses a process for synthesizing butanone oxime ethyl ether through continuous microtube reaction. The process adopts continuous microtube reaction technology, under the conditions of temperature 30-45℃, pressure 0.1MPa and strong base, butanone oxime and diethyl sulfate are reacted to directly synthesize butanone oxime ethyl ether; the strong base is hydrogen Sodium oxide, potassium hydroxide or alcohol amine compounds. In this process, diethyl sulfate, lye and butanone oxime are respectively fed by precision micropumps, butanone oxime is mixed with lye and diethyl sulfate in turn, and then reacted in a microtube reactor. After the heater, it is condensed and collected at low temperature, the chromatographic separator is left to stand for stratification, the water phase is extracted and separated by a micro-extraction tower, and the oil phase product containing butanone oxime ether is purified by rectification in a rectification tower to obtain the final product butanone oxime ether. The process has high selectivity of butanone oxime ethyl ether, can significantly enhance mass transfer and heat transfer, effectively avoid the hydrolysis of diethyl sulfate, has simple process, long stable operation time, low cost, is easy to scale up, and meets the requirements of industrial production.

Description

technical field [0001] The invention relates to a process for synthesizing butanone oxime ethyl ether through continuous microtube reaction, belonging to the technical field of fine chemicals. Background technique [0002] Oxime ethers are organic synthesis intermediates with high added value, which can be used to synthesize a series of new pharmaceutical and pesticide products. Oxime O-alkylation batch reaction directly synthesizes oxime ether, using oxime and alkylating reagent in the presence of a strong base, the reaction is difficult to control the temperature of the system, the utilization rate of the alkylating reagent is not high, and the product quality is unstable question. For example, in the reaction of using diethyl sulfate as an ethylating reagent to synthesize butanone oxime ethyl ether ["Zhejiang Chemical Industry", 2012], the reaction condition is that the ratio of the amount of butanone oxime, diethyl sulfate and sodium hydroxide is 1:1.3:1, diethyl sulfa...

AI Technical Summary

Problems solved by technology

Although the yield of butanone oxime ethyl ether reaches 92.65%, because diethyl sulfate is active in nature, it is especially easy to decompose in water. In the intermittent reaction, it is necessary to adopt the method feeding of diethyl sulfate continuously and slowly, which is complicated to operate and difficult to control. Long operating time, high cost and low equipment utilization

The temperature of the reaction system is easy to rise rapidly, the reaction may be excessive, and the product quality is unstable

Due to the long reaction time, the unreacted excess diethyl sulfate is almost completely decomposed, resulting in waste of raw materials and equipment corrosion

Does not meet the requirements of industrial production

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