Method of separating 1,2-dichloropropane with DD mixture

A technology of dichloropropane and mixture, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as imperfect treatment methods, difficult distillation and separation, etc.

Inactive Publication Date: 2006-10-18
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Abstract
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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 of separating 1,2-dichloropropane with DD mixture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1 (two-step method)

[0043] 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.

[0044] After installing a stirring device, a water separator, and a condenser on the three-necked flask, add 0.5 mol of acrylic acid and 0.04 g of a polymerization inhibitor DPPH, stir and cool, and add 0.5 mol of sodium hydroxide for neutralization. Then use benzene azeotropic dehydration, vacuum drying to obtain about 47g of sodium acrylate.

[0045] 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, and reac...

Embodiment 2

[0046] Embodiment 2 (two-step method)

[0047] 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. The purity of 1,2-dichloropropane was 95.5%, and the calculated yield was 82.5%.

Embodiment 3

[0048] Embodiment 3 (two-step method)

[0049] 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, then the purity of 1,2-dichloropropane was 95.0%, and the calculated yield was 83.0%.

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Abstract

The process of separating 1, 2-dichloropropane from DD mixture has the 1, 3-trichloropropane in DD mixture reacted with acrylic acid or methacrylic acid, alkali, catalyst and polymerization inhibitor to convert into 3-chloro-2-propenyl acrylate or 3-chloro-2-propenyl-2-methacrylate with boiling point different obviously to that of 1, 2-trichloropropane and distilled for separation from 1, 2-dichloropropane. The technological process includes the steps of: pre-treatment of the material, catalytic esterification reaction, and product separation. The present invention provides one comprehensive utilizing way of DD mixture, and the separated 1, 2-dichloropropane is one important organic intermediate and solvent.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and relates to a comprehensive utilization method of a chemical by-product, a DD mixture, in particular to a method for separating 1,2-dichloropropane by using a DD mixture. 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 proble...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/395C07C19/01C07C67/10C07C69/587
Inventor 封禄田石爽孙剑飞赫秀娟
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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