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Method for preparing dichloropropanol by glycerin chlorination

A technology of dichloropropanol and glycerin, applied in the direction of introducing halogen preparation, chemical recovery, organic chemistry, etc., can solve the problems of catalyst loss, long reaction time, low activity, etc., and achieve improved utilization rate, fast reaction speed, and improved yield rate effect

Active Publication Date: 2009-11-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This technology is currently the mainstream technology for the production of epichlorohydrin, and the technology is mature. The main problem is that the discharge of three wastes is particularly large, it is not easy to treat, and the environmental pollution is particularly serious.
Some of these catalysts have low boiling points. In order to improve the conversion rate of glycerol in the reaction process, the water generated in the reaction process needs to be continuously evaporated, which easily leads to catalyst loss; some have high boiling points, which overcome the problem of catalyst loss, but have low activity. long reaction time

Method used

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  • Method for preparing dichloropropanol by glycerin chlorination
  • Method for preparing dichloropropanol by glycerin chlorination
  • Method for preparing dichloropropanol by glycerin chlorination

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a three-neck flask with a stirring and reflux device, add 92.05g (1.00mol) of glycerin and 11.43g (0.10mol) of cyclopentyl carboxylic acid (also known as cyclopentyl formic acid, English name: cyclopentanecarboxylic acid, provided by Bailingwei Chemical Reagent Company) , heated to 110°C, and hydrogen chloride gas was introduced, and the flow rate of hydrogen chloride gas was 200ml / min. After reacting for 8 hours, 112.18 g of chlorinated liquid was obtained, and 73.87 g of acidic distillate was obtained by reflux during the reaction, and the conversion rate of glycerol was 99.68% through chromatographic analysis. The chlorinated liquid was distilled under reduced pressure to obtain 69.20 g of reduced-pressure fractions and 42.98 g of bottom liquid. The acidic distillate and the reduced-pressure fractions were combined. Obtain the total yield of dichloropropanol by chromatographic analysis: 73.76%, the total yield of monochloropropanediol: 19.13%, and the reaction pro...

Embodiment 2

[0029] In a there-necked flask with a stirring and reflux device, add 92.25g (1.002mol) glycerin and the 42.98g still bottom residue obtained in Example 1, heat to 110°C, feed hydrogen chloride gas, and the flow rate of hydrogen chloride gas is 200ml / min. After reacting for 8 hours, 146.32 g of chlorinated liquid was obtained. During the reaction, reflux was condensed to obtain 68.90 g of acidic distillate, and the conversion rate of glycerin was 99.58% through chromatographic analysis. The chlorinated liquid was distilled under reduced pressure to obtain 94.35 g of reduced-pressure fractions and 51.97 g of bottom liquid. The acidic distillate and the reduced-pressure fractions were combined. Obtain the total yield of dichloropropanol by chromatographic analysis: 82.61%, the total yield of monochloropropanediol: 15.28%, and the reaction product composition sees the following table 2:

[0030] Table 2

[0031]

[0032]

Embodiment 3

[0034] In a there-necked flask with a stirring and reflux device, add 92.21g (1.002mol) of glycerin and the 51.97g residue at the bottom of the still obtained in Example 2, heat to 110°C, feed hydrogen chloride gas, and the flow rate of hydrogen chloride gas is 200ml / min. After reacting for 8 hours, 161.02 g of chlorinated liquid was obtained. During the reaction, reflux was condensed to obtain 68.60 g of acidic distillate, and the conversion rate of glycerin was 99.49% through chromatographic analysis. The chlorinated liquid was distilled under reduced pressure to obtain 101.85 g of reduced-pressure fractions and 59.17 g of bottom liquid. The acidic distillate and the reduced-pressure fractions were combined. Obtain the total yield of dichloropropanol by chromatographic analysis: 87.91%, the total yield of monochloropropanediol: 11.88%, and the composition of the reaction product is shown in the following table 3:

[0035] table 3

[0036]

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Abstract

The invention relates to a method for preparing dichloropropanol by glycerin chlorination, comprising the following steps: guiding chlorine hydride to the glycerin for reaction under the catalysis of naphthenic acid functioning as catalyst, and collecting the dichloropropanol as the product of the reaction after the reaction is finished. Compared with the prior method for preparing dichloropropanol, the method for preparing the dichloropropanol by glycerin chlorination has the advantages that the catalyst can be reutilized, has high activity and good selectivity and less byproducts of reaction are generated.

Description

technical field [0001] The present invention relates to a method for producing fine chemicals. Specifically, the invention provides a method for synthesizing dichloropropanol from glycerol. Background technique [0002] Dichloropropanol includes two isomers of dichloropropanol, namely 1,3-dichloro-2-propanol and 2,3-dichloro-1-propanol, and their main use is to synthesize epoxy chloride propane. Epichlorohydrin is one of the main monomers for the production of epoxy resins. The global annual output is more than 1.5 million tons, all of which are produced through dichloropropanol. The main industrial production methods are propylene high temperature chlorination method and allyl acetate method. Propylene high-temperature chlorination method uses propylene as raw material, reacts with chlorine gas at high temperature to generate 3-chloropropene, then reacts with hypochlorous acid to produce dichloropropanol, and finally saponifies to obtain epichlorohydrin. This technology...

Claims

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Application Information

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IPC IPC(8): C07C31/42C07C31/36C07C29/62
CPCY02P20/584
Inventor 戴祖贵杜泽学张永强刘易陈艳凤
Owner CHINA PETROLEUM & CHEM CORP
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