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Method for synthesizing dichloropropanol by glycerine

A technology of dichloropropanol and glycerin, which is applied in the direction of organic chemistry, the introduction of halogen preparation, etc., can solve the problems of large discharge of three wastes, serious environmental pollution, and long reaction time, and achieve reduced environmental pollution, high chlorination activity, and high reaction time. fast 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
At present, there is no report on the synthesis of dichloropropanol by first esterifying glycerol and then chlorinating

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In a three-necked flask with a stirring and reflux device, add 92.2g (1.00mol) of glycerin, 60.2g (1.00mol) of glacial acetic acid and 34.2g (0.35mol) of toluene, after heating to 90°C, add 3.0g of strong acidic cation Exchange resin (Amberlyst35 American Rohm and Haas company production), react after 2 hours, filter out solid acid catalyst, heat up and remove the mixture of toluene and water, obtain the mixture of glyceryl acetate, glycerol, glacial acetic acid etc. It was transferred into a three-neck flask, heated to a reaction temperature of 100° C., and then hydrogen chloride gas was introduced. The flow rate of hydrogen chloride gas was 200 ml / min. After reacting for 8 hours, 110.7 g of chlorinated liquid at the bottom of the kettle was obtained. During the reaction, reflux was condensed to obtain 92.0 g of acidic distillate, and a total of 202.7 g of synthetic liquid was obtained. It can be known by chromatographic analysis that the conversion rate of glycerin is...

Embodiment 2

[0023] Add 88.9g (1.01mol) of n-butyric acid, the temperature of glyceride chlorination reaction is 110°C, and other conditions are the same as in Example 1. Obtain 167.9g of chlorinated liquid at the bottom of the still, condense and reflux in the reaction process to obtain acidic distillate 101.6g, obtain synthetic liquid 269.5g in total, as can be known by chromatographic analysis, the conversion rate of glycerol is 100%, and the total yield of dichloropropanol is: 67.8%, total yield of monochloropropanediol: 5.1%.

Embodiment 3

[0025] In a three-neck flask with a stirring and reflux device, add 140.4g (1.53mol) of glycerin, 90.7g (1.51mol) of glacial acetic acid and 46.2g (0.47mol) of toluene, after heating to 90°C, add 11.2g of activated carbon to load P-toluenesulfonic acid (made by conventional methods, the method is as follows: take 20.0 grams of activated carbon, wash with water, dry at 115 ° C until the quality is constant, soak in 120 mL of p-toluenesulfonic acid aqueous solution with a mass fraction of 25% for 30 hours, and suction filter. Dry at 110°C for 5 hours, put it into a desiccator and cool it down to obtain an activated carbon-supported catalyst containing 30.2wt% p-toluenesulfonic acid), after reacting for 2 hours, filter out the solid acid catalyst, heat up to remove the mixture of toluene and water, and obtain glycerol acetate Mixture of esters, glycerol, glacial acetic acid, etc. The mixture was added into a pressure reactor, hydrogen chloride gas was fed to maintain a reaction p...

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Abstract

The invention provides a method for synthesizing dichloropropanol by glycerine, which comprises the following steps: the glycerine and organic acid are processed through esterification reaction under the catalysis of solid acid functioning as catalyst to generate organic acid glycerine ester, chlorine hydride is guided to the organic acid glycerine ester for chlorination reaction, and the dichloropropanol as the product of reaction is collected after the chlorination reaction finishes. The method for synthesizing dichloropropanol by glycerine is characterized in that firstly, during the esterification reaction of the glycerine and the organic acid under the catalysis of the solid acid, generated water is removed, thus the dissolution of the chlorine hydride during the esterification reaction is lessened, and the corrosion to equipment is reduced; secondly, high chlorination activity and rapid reaction speed are guaranteed through the esterification reaction, and particularly, the reaction time is markedly shortened under pressure; and thirdly, the dosage of the chlorine hydride is reduced and the environmental pollution is alleviated.

Description

technical field [0001] The present invention relates to a method for producing fine chemicals. Specifically, the present invention provides a new method for synthesizing dichloropropanol from glycerol. Background technique [0002] Dichloropropanol includes two isomers, namely 1,3-dichloro-2-propanol and 2,3-dichloro-1-propanol, and their main use is to synthesize epichlorohydrin. 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 synthesized 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 is currently...

Claims

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Application Information

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