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Method for continuously synthesizing 1, 1-diethoxypropane

A technology of diethoxypropane and propionaldehyde, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as high operating intensity, non-continuous production, low efficiency, and slow reaction

Pending Publication Date: 2021-11-19
ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is carried out at low temperature, the reaction is slow, the reaction time is long, and the continuous production efficiency is low; and a large amount of calcium chloride and other absorbents are used to remove water, the operation intensity is high, the post-processing is troublesome, and the environmental protection pressure is high.

Method used

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  • Method for continuously synthesizing 1, 1-diethoxypropane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Turn on the preheater, mix propionaldehyde and ethanol with a molar ratio of 1:2 in the mixer (that is, the feed tank), then pass through the metering pump, pump into the preheater to preheat the raw material to 70°C, and pass through the solid load The trickle bed reaction of sulfonic acid resin was carried out, and the content of 1,1-diethoxypropane in the reaction solution was 29.7%. The reaction solution is continuously pumped into the rectification tower through the feed pump for separation, and a mixed component of unreacted raw materials propionaldehyde, ethanol and water produced by the reaction is obtained at the top of the tower, and the mixed component is dewatered through a membrane to obtain anhydrous propionaldehyde. Aldehyde and ethanol are applied mechanically to the condensation reaction, and 1,1-diethoxypropane with a content >98% is obtained in the tower reactor.

Embodiment 2

[0019] Turn on the preheater, mix propionaldehyde and ethanol with a molar ratio of 1:3, and then pump it into the preheater through a metering pump to preheat the raw material to 60°C, and then pass through the trickle bed reaction with sulfonic acid resin , the content of 1,1-diethoxypropane in the reaction solution was 38.7%. The reaction solution is continuously pumped into the rectification tower through the feed pump for separation, and a mixed component of unreacted raw materials propionaldehyde, ethanol and water produced by the reaction is obtained at the top of the tower, and the mixed component is dewatered through a membrane to obtain anhydrous propionaldehyde. Aldehyde and ethanol are applied mechanically to the condensation reaction, and 1,1-diethoxypropane with a content >98% is obtained in the tower reactor.

Embodiment 3

[0021] Turn on the preheater, mix propionaldehyde and ethanol with a molar ratio of 1:4, and then pump it into the preheater through the metering pump to preheat the raw material to 50°C, and then pass through the trickle bed reaction of the sulfonic acid resin , the content of 1,1-diethoxypropane in the reaction solution was 41.3%. The reaction solution is continuously pumped into the rectification tower through the feed pump for separation, and a mixed component of unreacted raw materials propionaldehyde, ethanol and water produced by the reaction is obtained at the top of the tower, and the mixed component is dewatered through a membrane to obtain anhydrous propionaldehyde. Aldehyde and ethanol are applied mechanically to the condensation reaction, and 1,1-diethoxypropane with a content >98% is obtained in the tower reactor.

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Abstract

The invention discloses a method for continuously synthesizing 1, 1-diethoxypropane. The method comprises the following steps: mixing absolute ethyl alcohol and propionaldehyde in a mixer, pumping into a preheater, preheating, continuously reacting in a trickle bed of an immobilized catalyst, neutralizing the reaction liquid, and rectifying to obtain 1, 1-diethoxypropane with the purity of 98% or above. According to the invention, continuous industrial production can be realized, waste salts such as calcium chloride are not generated, and green synthesis is realized.

Description

technical field [0001] The invention relates to the field of organic compound synthesis, in particular to a method for continuously synthesizing 1,1-diethoxypropane. Background technique [0002] 1,1-diethoxypropane is an important organic compound, which can be cracked to produce 1-ethoxypropene, and 1-ethoxypropene can be used as a raw material to synthesize β-carotene. 1,1-diethoxypropane can also be used as an intermediate to prepare a thiacloprid drug. Thiacloprid is a high-efficiency, low-toxicity, broad-spectrum neonicotinoid insecticide, which has the following advantages: ①It is very safe for humans and animals, and the agent has no odor and irritation; ②The vapor of the active ingredient Low pressure, will not pollute the air, and the half-life is short, and the residue can be quickly decomposed after entering the soil and rivers, causing little impact on the environment; ③The toxicity to aquatic organisms is also very low, and generally has basically no effect on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/56C07C43/303C07C41/58
CPCC07C41/56C07C41/58C07C43/303
Inventor 翟德伟陈新志霍鸿飞刘冬石霄鹏项学兵
Owner ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY