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Process for synthesizing diacetylmonoxime ethyl ether by continuous reactions in microtube

A technology of butanone oxime and internal reaction is applied in the field of continuous microtube internal reaction synthesis of butanone oxime ethyl ether, which can solve the problems of low equipment utilization rate, long operation time, waste of raw materials, etc., and achieves reduction of operation time and cost, mass transfer And the effect of strengthening the heat transfer process and improving product quality

Active Publication Date: 2013-09-18
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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

Method used

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  • Process for synthesizing diacetylmonoxime ethyl ether by continuous reactions in microtube
  • Process for synthesizing diacetylmonoxime ethyl ether by continuous reactions in microtube

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Experimental program
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Effect test

Embodiment 1

[0028] The microtube reactor has an inner diameter of 2.1mm and a length of 5m.

[0029] The ratio of the amount of butanone oxime, diethyl sulfate, and 18% sodium hydroxide aqueous solution is 1:1.25:1.15. Feed continuously, the reaction temperature is 30°C, and the residence time is 20 min. The reaction product is collected by low-temperature condensation, and the product is separated into an oil phase after standing, and the residual organic matter in the water phase is extracted and recovered with an extractant. The product was analyzed by gas chromatography with GC1690 gas chromatograph. The chromatographic column is a GsBP-INOWAX (specification: 30m×0.32mm×0.25μm) capillary column, FID detector, and n-butanol as the internal standard for quantitative calculation. The analysis method is the same below. The conversion rate of butanone oxime is 83.41%, the yield of butanone oxime ether is 16.80%, and the selectivity is 16.80%.

Embodiment 2

[0031] The microtube reactor has an inner diameter of 2.1mm and a length of 5m.

[0032] The ratio of the amount of butanone oxime, diethyl sulfate, and 18% sodium hydroxide aqueous solution is 1:1:1. Feed continuously, the reaction temperature is 30°C, and the residence time is 3 min. The reaction product is collected by low-temperature condensation, the product is separated into the oil phase after standing, the residual organic matter in the water phase is extracted and recovered with an extractant, and the product is analyzed by gas chromatography. The conversion rate of butanone oxime was 87.64%, the yield of butanone oxime ether was 15.81%, and the selectivity was 18.04%.

Embodiment 3

[0034] The microtube reactor has an inner diameter of 1mm and a length of 20m.

[0035] The ratio of the amount of butanone oxime, diethyl sulfate, and 18% sodium hydroxide aqueous solution is 1:1:1. The feed is continuous, the reaction temperature is 40°C, and the residence time is 60 min. The reaction product is collected by low-temperature condensation, and the product is separated into an oil phase after standing. The residual organic matter in the water phase is extracted and recovered with an extractant, and the product is analyzed by gas chromatography. The conversion rate of butanone oxime is 77.87%, the yield of butanone oxime ether is 53.10%, and the selectivity is 68.19%.

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Abstract

The invention discloses a process for synthesizing diacetylmonoxime ethyl ether by continuous reactions in a microtube. In the process, diacetylmonoxime and diethyl sulfate are directly reacted to synthesize diacetylmonoxime ethyl ether in a condition that the temperature is 30-45 DEG C and the pressure is 0.1MPa in the presence of strong base with the adoption of a continuous reaction technology in the microtube, wherein the strong base is sodium hydroxide, potassium hydroxide or an alcamine compound. In the process, diethyl sulfate, the alkali liquor and diacetylmonoxime are respectively fed by a precise micro pump, wherein diacetylmonoxime sequentially mixed with the alkali liquor and diethyl sulfate reacts in a microtube reactor. The product through a heat exchanger is condensed and collected at low temperature, and is stewed and layered by a chromatographic separator. A water phase is extracted and separated by a micro extraction tower, and an oil phase containing diacetylmonoxime ethyl ether is rectified and purified by a rectifying tower, so that the final product diacetylmonoxime ethyl ether is obtained. The process is high in selectivity of diacetylmonoxime ethyl ether, mass transfer and heat transfer can be remarkably enhanced, and hydrolysis of diethyl sulfate is effectively avoided. The process is simple in process, long in stable transfer time, low in cost, easy to amplify and suitable for the industrialized production requirement.

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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/38C07C249/12
Inventor 朱明乔王萌卢建刚刘建青陈幼坚
Owner ZHEJIANG UNIV
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