Method for synthesizing epoxy chloropropane through phase-transfer catalysis

A technology of epichlorohydrin and phase transfer catalysis, which is applied in the direction of organic chemistry, can solve the problems of high energy consumption and high product cost, and achieve the effect of high purity

Active Publication Date: 2017-05-10
CHANGZHOU UNIV
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  • Abstract
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However, the problem of the multi-effect evaporation method is th

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  • Method for synthesizing epoxy chloropropane through phase-transfer catalysis

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[0026] Example 1

[0027] Reference attached figure 1 In the process of reactant premixing tank (1), dichloropropanol (weight composition: dichloropropanol 98%, hydrogen chloride 1%, water 1%) and phase transfer catalyst nonylphenol polyoxyethylene ether ( (Molecular weight 650) is mixed with 58kg / h powdered potassium hydroxide (150 mesh) input through the powdered alkali feed pump (2), and the feed flow rate is controlled to make the reactants premix the dichloropropanol in the kettle (1) The molar ratio of potassium hydroxide is 1.5:1, the weight ratio of nonylphenol polyoxyethylene ether and dichloropropanol is 0.005:1, and the average residence time of the materials in the premixing kettle is controlled to be 20 seconds and the mixing temperature is 35°C.

[0028] The above materials are mixed and transported to the preheater (4) by the preheater feed pump (3) (indirect steam heating is adopted, that is, the material goes through the pipe path and the steam goes through the sh...

Example Embodiment

[0032] Example 2

[0033] Reference attached figure 1 In the process of reactant premixing tank (1), dichloropropanol (weight composition: dichloropropanol 98%, hydrogen chloride 1%, water 1%) and phase transfer catalyst stearyl alcohol polyoxyethylene ether ( (Molecular weight 1180) is mixed with 41.5kg / h powdered sodium hydroxide (250 mesh) input through the powdered alkali feed pump (2), and the feed flow rate is controlled to make the reactants premix the dichloropropanol in the kettle (1) The molar ratio to sodium hydroxide is 2:1, the weight ratio of stearyl alcohol polyoxyethylene ether to dichloropropanol is 0.006:1, and the average residence time of the materials in the pre-mixing kettle is controlled to be 30 seconds, and the mixing temperature is 35°C ,

[0034] After the above materials are mixed, they are transported to the preheater (4) by the preheater feed pump (3) (indirect steam heating is adopted, that is, the material passes through the pipe pass, and the stea...

Example Embodiment

[0038] Example 3

[0039] Reference attached figure 1 In the process of reactant premixing kettle (1), dichloropropanol (weight composition: dichloropropanol 98%, hydrogen chloride 1%, water 1%) and phase transfer catalyst polyethylene glycol (molecular weight 2000) Mix with 24.8kg / h powdered lithium hydroxide (350 mesh) input through the powdered alkali feed pump (2), control the feed flow rate, and make the reactants premix the dichloropropanol and the hydroxide in the kettle (1) The lithium molar ratio is 3:1, the weight ratio of polyethylene glycol to dichloropropanol is 0.01:1, and the average residence time of the materials in the premixing kettle is controlled to be 40 seconds, and the mixing temperature is 40°C.

[0040] The above-mentioned materials are mixed and transported to the preheater (4) by the preheater feed pump (3) (indirect steam heating is adopted, that is, the material passes through the pipe and the water vapor passes through the shell), and the material is...

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Abstract

The invention belongs to the field of synthesis of epoxy compounds, and in particular relates to a method for synthesizing epoxy chloropropane through phase-transfer catalysis. The method disclosed by the invention comprises the following steps: carrying out a dehydrochlorination saponification reaction by using powdered alkali and excessive dichloropropanol, wherein the excessive dichloropropanol serves as a reactant and a reaction medium, and the traditional ionized catalyst is replaced by a liquid ether catalyst, so that the produced salt exists in the reaction system in a solid form and is easily separated. Therefore, the recovery of by-product salts is realized under low energy consumption, and the production of salt-containing saponification wastewater is avoided, so that the aims of energy conservation and emission reduction are achieved.

Description

technical field [0001] The invention belongs to the field of epoxy compound synthesis, and in particular relates to a method for synthesizing epichlorohydrin by phase transfer catalysis. Background technique [0002] Epichlorohydrin is an important basic chemical raw material and organic synthesis intermediate, mainly used in the production of epoxy resin, surfactant, medicine, pesticide, ion exchange resin, etc. [0003] Epichlorohydrin is mainly prepared by saponification reaction of corresponding dichloropropanol and alkali. Saponification reaction is a fast reaction, and the obtained product epichlorohydrin is unstable. In order to improve the product yield, the production method widely used in industry is to use relatively dilute caustic soda aqueous solution or lime emulsion to carry out saponification reaction in a tower reactor (so-called saponification tower), and directly heat it with water vapor in the tower reactor. The epichlorohydrin generated is stripped, an...

Claims

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Application Information

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IPC IPC(8): C07D303/08C07D301/26
CPCC07D301/26C07D303/08
Inventor 单玉华郑一天储海霞毛翠霞王超冯洋洋
Owner CHANGZHOU UNIV
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