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Method for preparing epoxy chloropropane by cyclizing chloropropene

A technology of epichlorohydrin and chloropropene, applied in the chemical industry, organic chemistry, sustainable manufacturing/processing, etc., can solve the problems of difficult control of reaction temperature, low conversion rate of epichlorohydrin, etc. The effect of not heating in time, inhibiting side reactions, improving conversion rate and selectivity

Active Publication Date: 2013-01-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is that the reaction temperature is not easy to control in the production of epichlorohydrin by the direct epoxidation of allyl chloride in the prior art, and the conversion rate and the yield of epichlorohydrin are not high. A new allyl chloride is provided A method for preparing epichlorohydrin by cyclization, which has the characteristics of stable reaction temperature, high conversion rate of hydrogen peroxide and high yield of epichlorohydrin

Method used

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  • Method for preparing epoxy chloropropane by cyclizing chloropropene
  • Method for preparing epoxy chloropropane by cyclizing chloropropene

Examples

Experimental program
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Embodiment 1

[0023] according to figure 1 As shown, the theoretical plate number of the stripping section of the catalytic distillation column is 15, the separation efficiency of the catalytic reaction section is equivalent to the theoretical plate number of 18, and the catalyst is SiO 2 / TiO 2 The titanium-silicon molecular sieve with a molar ratio of 80, 30% by weight of hydrogen peroxide and methanol mixture (methanol content of 70% by weight) entered the first theoretical plate (counting from top to bottom, the same below) at a flow rate of 1.00 g / min. The flow rate of 2.00 g / min enters from the bottom of the catalytic reaction section, the operating temperature of the reaction section is 43 to 48 °C, the weight ratio of the first part of the tower to the second part of the material is 3:1, and the bottom of the tower is extracted with a flow of 3.00 g / min, The bottom of the tower is drawn into the top of the extraction tower with a theoretical plate number of 15, the extractant water...

Embodiment 2

[0025] according to figure 1 As shown, the theoretical plate number of the stripping section of the catalytic distillation column is 30, the separation efficiency of the catalytic reaction section is equivalent to the theoretical plate number of 50, and the catalyst is SiO 2 / TiO 2 Molar ratio of 180 titanium-silicon molecular sieve, 50% by weight of hydrogen peroxide and methanol mixture (methanol content of 30% by weight) at a flow rate of 1.00 g / min, and propene chloride at a flow rate of 12.00 g / min from the top of the catalytic distillation column to enter, the reaction section The operating temperature is 38-43°C, the weight ratio of the first part of the column to the second part of the material is 1:1, the bottom of the column is extracted at a flow rate of 13.00 g / min, and the bottom of the column is extracted into an extraction column with a theoretical plate number of 40 At the top, the extraction agent ethylene glycol enters the bottom of the extraction tower at 2...

Embodiment 3

[0027] according to figure 1 As shown, the number of theoretical plates in the stripping section of the catalytic distillation column is 5, the separation efficiency of the catalytic reaction section is equivalent to 5 theoretical plates, and the catalyst is SiO 2 / TiO 2 Molar ratio of 20 titanium-silicon molecular sieves, 2 wt% hydrogen peroxide and methanol mixture (methanol content of 50 wt%) entered the first theoretical plate at a flow rate of 1.00 g / min, and propene chloride flowed from the middle of the catalytic reaction section at a flow rate of 5 g / min Entering, the operating temperature of the reaction section is 42-46 °C, the weight ratio of the first part of the tower to the second part of the material is 15:1, the bottom of the tower is extracted at a flow rate of 6.00 g / min, and the number of theoretical plates extracted from the bottom of the tower is 5 At the top of the extraction tower, the extraction agent 1,3-propanediol enters the bottom of the extraction...

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Abstract

The invention relates to a method for preparing epoxy chloropropane by cyclizing chloropropene, which mainly solves the problems of difficulty in controlling reaction temperature, and low conversion rate and yield of epoxy chloropropane in the process of producing epoxy chloropropane by directly epoxidating chloropropene. The method comprises steps as follows: chloropropene, hydrogen peroxide andmethanol are subjected to epoxidation reaction in a catalytic distillation tower, the components are separated during the reaction, a tower top steam is condensed and refluxed, the first part of the tower bottom material is vaporized by a reboiler and returns to the catalytic distillation tower, the second part of the tower bottom material is used as a produced liquid stream I, and the weight ratio of the first part to the second part is (1-15):1, wherein the mixture of hydrogen peroxide and solvent can enter via the tower top, and the chloropropene can enter in any position from the upper part of the stripping section to the tower top; the stream I and an extractant respectively enter the bottom and top of a extraction tower, an epoxy-chloropropane-rich mixture stream II is produced fromthe tower top, and a methanol-rich mixture stream III is obtained from the tower bottom; the stream II enters a finished product tower, the chloropropene is produced from the tower top, the epoxy chloropropane is produced from the side stream, and small amounts of heavy components are produced from the tower bottom; and the stream III enters an extractant recovery tower, the methanol is produced from the tower top, and the recycled extractant is obtained at the tower bottom. The technical scheme provided by the invention solves the problems, and can be used for industrial production of epoxy chloropropane.

Description

technical field [0001] The invention relates to a method for preparing epichlorohydrin by cyclization of chloropropene. Background technique [0002] Epichlorohydrin is an important basic organic chemical raw material and intermediate because it contains active epoxy groups and chlorine atoms in its molecule, so it is widely used in the synthesis of epoxy resin, glycerin and chlorohydrin rubber. , medicine, pesticides, surfactants, glass fiber reinforced plastics, ion exchange resins, coatings and plasticizers, etc. At present, epichlorohydrin is produced from propylene as raw material, and the production methods mainly include chloropropene method and allyl alcohol method. The chloropropene method, also known as the high temperature chlorination method, is the main method for the production of epichlorohydrin with mature technology and flexible production process. However, the chloropropene method also has some serious defects, such as many by-products, high energy consum...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/08C07D301/12
CPCY02P20/10
Inventor 钟禄平肖剑高焕新
Owner CHINA PETROLEUM & CHEM CORP
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