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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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the problem of the multi-effect evaporation method is that the energy consumption is high, resulting in high product cost.

Method used

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  • Method for synthesizing epoxy chloropropane through phase-transfer catalysis

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Experimental program
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Effect test

Embodiment 1

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

[0028] 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 goes through the tube side, and the water vapor goes through the shell side), and the material after preheating to 50°C Aft...

Embodiment 2

[0033] Refer to attached figure 1 The flow process, in the reactant premix tank (1), dichloropropanol (weight composition: dichloropropanol 98%, hydrogen chloride 1%, water 1%) and phase transfer catalyst stearyl polyoxyethylene ether ( Molecular weight 1180) is mixed with the 41.5kg / h powdery sodium hydroxide (250 order) that is imported by powdery alkali feed pump (2), controls feed flow rate, makes dichloropropanol in the reactant premix still (1) The molar ratio to sodium hydroxide is 2:1, the weight ratio of stearyl polyoxyethylene ether to dichloropropanol is 0.006:1, and the average residence time of the materials in the premixing tank 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 goes through the tube side, and the water vapor goes through the shell side), and the materia...

Embodiment 3

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

[0040] 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 goes through the tube side, and the water vapor goes through the shell side), and the material after preheating to 70°C...

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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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