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Method for preparing acrylic ester and separation 1, 2-dichloropropane by using DD mixing agent

A technology of dichloropropane and acrylate, which is applied in the field of comprehensive utilization of chemical by-products - DD mixture, which can solve problems such as imperfect treatment methods and difficult rectification separation

Inactive Publication Date: 2005-10-26
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some people in China tried to separate 1,3-dichloropropene and 1,2-dichloropropane in the DD mixture by rectification, and carried out small-scale production, but due to the similar boiling points of each component (1,2-dichloropropane Chloropropane 97°C, cis 1,3-dichloropropene 102°C, trans 1,3-dichloropropene 110°C), it is difficult to completely separate the components by rectification, and the DD mixture can decompose HCl after heating, so High requirements are placed on the tower efficiency and corrosion resistance of the rectification unit
In short, the current treatment methods for DD mixtures are not perfect

Method used

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  • Method for preparing acrylic ester and separation 1, 2-dichloropropane by using DD mixing agent
  • Method for preparing acrylic ester and separation 1, 2-dichloropropane by using DD mixing agent
  • Method for preparing acrylic ester and separation 1, 2-dichloropropane by using DD mixing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1 (two-step method)

[0042] The DD mixture was dehydrated and simply distilled to remove impurities, and its component content was analyzed by gas chromatography. The acrylic acid is refined by vacuum distillation to remove possible polymers and impurities, and an appropriate amount of polymerization inhibitor is added to prevent its polymerization.

[0043] After installing a stirring device, a water separator, and a condenser on the there-necked flask, add 36 g (0.5 mol) of acrylic acid and 0.04 g of a polymerization inhibitor DPPH, stir and cool, and add 20 g (0.5 mol) of sodium hydroxide to neutralize. Then use benzene azeotropic dehydration, vacuum drying to obtain about 47g of sodium acrylate.

[0044] After installing stirring device, condenser and thermometer on the 500ml there-necked flask, add DD mixture 241.3g (containing 1,3-dichloropropene 23%, 0.5mol), sodium acrylate 47g (0.5mol), DPPH0. 04g, triethylamine 3ml. Heat the oil bath to 85-90°C,...

Embodiment 2

[0045] Embodiment 2 (two-step method)

[0046] Implementation steps are the same as in Example 1. The conditions of the esterification reaction were changed as follows: the reaction temperature was 75-80° C., the reaction time was 4 hours, and the amount of triethylamine was 2.5 ml, so the yield of 3-chloro-2-propenyl acrylate was 6.8%.

Embodiment 3

[0047] Embodiment 3 (two-step method)

[0048] Implementation steps are the same as in Example 1. The conditions of the esterification reaction were changed to: the reaction temperature was 75-80°C, the reaction time was 5 hours, and the amount of triethylamine was 3.0ml, so the yield of 3-chloro-2-propenyl acrylate was 22.7%.

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Abstract

The present invention relates to a method capable of utilizing DD mixture to prepare acrylate and separating 1,2-dichloropropane from it. Said invention utilizes the action of 1,3-dichloropropene in the DD mixture and acrylic acid or methylacrylic acid, alkali, catalyst and and polymerization inhibitor to synthesize 3-chloro-2-propenyl acrylate or 3-chloro-2-propenyl 2-methacrylate, and utilizes the distillation to make it be separated from 1,2-dichloropropane. Said method includes the steps of raw material pretreatment, catalytic esterification reaction, product separation and product refinement.

Description

Technical field: [0001] The invention relates to a comprehensive utilization method of a chemical by-product-DD mixture, in particular to a method for separating and preparing 1,2-dichloropropane and acrylate by using the DD mixture as the main raw material. Background technique: [0002] DD mixture is a high-boiling by-product produced by the thermal chlorination of propylene to produce 3-chloropropene. The main components are 1,2-dichloropropane and 1,3-dichloropropene (including cis and trans isomers). 3-Chloropropene is mainly used in the production of epichlorohydrin. At present, the production capacity of epichlorohydrin in my country is 45,000 tons per year, and about 230 kg of DD mixture is produced for each ton of epichlorohydrin produced, so nearly 10,000 tons of DD mixture is produced every year. Moreover, the production equipment of epichlorohydrin is still increasing, and the generation of DD mixture is also increasing correspondingly, so the problem of DD mixt...

Claims

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Application Information

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IPC IPC(8): C07C69/653
Inventor 封禄田孙剑飞石爽
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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