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Method for synthesizing epichlorohydrin

A technology of epichlorohydrin and a synthesis method, applied in directions such as organic chemistry, can solve the problems of high requirements for equipment, inconvenient operation, and high purification costs, and achieve the effects of low production cost, convenient operation and low cost

Inactive Publication Date: 2008-04-09
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Regarding the synthesis of epichlorohydrin and 1,3-dichloropropanol, the literature (Ullmaan`s Encyclopedia of Industrial Chemistry, 5 edVol.A9, P.539-540) describes the preparation of glycerol and hydrochloric acid under the catalysis of acetic acid , the solution concentration of 1,3-dichloropropanol prepared by this method is 5-15%, and 2,3-dichloropropanol exists in the product, and the purification cost is high
In order to overcome the above shortcomings, Krafft, Philippe (W02005 / 054167 A1) and (PCT / CZ2004 / 000049) proposed to use a countercurrent gas-liquid reaction tower to carry out chlorination of glycerol. These methods are inconvenient to operate and require high equipment

Method used

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  • Method for synthesizing epichlorohydrin
  • Method for synthesizing epichlorohydrin
  • Method for synthesizing epichlorohydrin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The synthetic method of epichlorohydrin is realized through the following steps:

[0050] 1) Preparation of 1,3-dichloropropanol:

[0051] Add 110 g (1 mole) of R-3-chloro-1,2-propanediol and 13.6 g (0.1 mole) of zinc chloride into a 250 ml three-necked flask, raise the temperature to 90° C., and feed 3 moles of hydrogen chloride gas. ℃ for 5 hours, follow the reaction, when R-3-chloro-1,2-propanediol is completely converted to 1,3-dichloropropanol, cool, neutralize to neutral with calcium carbonate, filter, and use the mother liquor directly for Next reaction.

[0052] 2) Preparation of epichlorohydrin:

[0053] Add the 1,3-dichloropropanol prepared in the previous step to a 2500ml four-neck flask, add 1000ml of water, slowly add 130ml of 30% sodium hydroxide solution in portions, and pass water vapor under reduced pressure. Steam distillation, add lye, continue to react for 1 hour, steam distillation to no oil drops, and then separate the organic layer from the obt...

Embodiment 2

[0055] The synthetic method of epichlorohydrin is realized through the following steps:

[0056] 1) Preparation of 1,3-dichloropropanol:

[0057] Add 110 grams (1mol) of R-3-chloro-1,2-propanediol and 238 grams (2 moles) of thionyl chloride into a 250ml three-necked flask, react at room temperature for 2 hours, and neutralize with sodium carbonate until the pH is neutral. properties, filtered, and the mother liquor was directly used in the next step without purification.

[0058] 2) Preparation of epichlorohydrin:

[0059] Add 1,3-dichloropropanol in a 2500ml four-necked flask, add 1000ml of water, slowly add 130ml of 30% sodium hydroxide solution in portions, and feed water vapor under reduced pressure to carry out steam distillation. Finish the lye, continue to react for 2 hours, steam distill until there is no oil drop, and separate the organic layer from the obtained distillate, add an appropriate amount of sodium chloride to the water layer, separate the organic layer a...

Embodiment 3

[0061] The synthetic method of epichlorohydrin is realized through the following steps:

[0062] 1) Preparation of 1,3-dichloropropanol:

[0063] Add 110 grams (1mol) of R-3-chloro-1,2-propanediol and 59 grams (0.4 moles) of phosphorus oxychloride into a 250ml three-necked flask, react at room temperature for 2 hours, neutralize to neutral with sodium carbonate, After filtration, the mother liquor was directly used in the next reaction without purification.

[0064] 2) Preparation of epichlorohydrin:

[0065] In a 2500ml four-necked flask, add 1,3-dichloropropanol, add 1000ml of water, slowly add 130ml of 30% sodium hydroxide solution in portions, and under reduced pressure, let people steam to carry out steam distillation, After adding the lye, continue to react for 2 hours, steam distill until there is no oil drop, separate the organic layer until the obtained distillate is static, add an appropriate amount of sodium chloride to the water layer, separate the organic layer ...

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Abstract

The invention relates to a synthesis method of epichlorohydrin, which is a reclaim utilization method of R-3-chloro-1, 2-propanediol during the separation and the preparation of S-epichlorohydrin by utilizing the dynamics of epichlorohydrin and a utilization method of utilizing glycerin which is the byproduct in the production of biodiesel. The R-3-chloro-1, 2-propanediol is reacted with chlorinating agent with the catalysis of the acid catalyst to generate the 1, 3-dichloro propanol, the obtained 1,3-dichloro propanol is reacted with alkali to generate the epichlorohydrin; the glycerin is reacted with the chlorinating agent with the catalysis of the acid catalyst to generate the 1,3-dichloro propanol, and the obtained 1,3-dichloro propanol is reacted with alkali to generate the epichlorohydrin. The synthesis method of the invention is simple, which can effectively convert the highly toxic waste R-3-chloro-1, 2-propanediol and the crude glycerin into the epichlorohydrin, the yield is high, the production cost is low, the environment pollution is reduced, so the synthesis method is an ideal method for industrialization reclaiming and utilization of R-3-chloro-1, 2-propanediol and the crude glycerin.

Description

technical field [0001] The invention relates to the fields of organic chemistry and medicinal chemistry, in particular to a synthesis method of epichlorohydrin. Background technique [0002] Epichlorohydrin is widely used in plastics, medicine and other fields, such as preparing epoxy resin with epichlorohydrin, using epichlorohydrin to perform kinetic resolution to prepare S-epichlorohydrin, and then to synthesize L-carnitine. Regarding the synthesis of epichlorohydrin and 1,3-dichloropropanol, the literature (Ullmaan`s Encyclopedia of Industrial Chemistry, 5 edVol.A9, P.539-540) describes the preparation of glycerol and hydrochloric acid under the catalysis of acetic acid , the solution concentration of 1,3-dichloropropanol prepared by this method is 5-15%, and 2,3-dichloropropanol exists in the product, and the purification cost is high. In order to overcome the above shortcomings, Krafft, Philippe (W02005 / 054167 A1) and (PCT / CZ2004 / 000049) proposed to use a countercurre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/26C07D303/08
Inventor 申永存滕汉兵马超张毅刘盟
Owner WUHAN UNIV OF TECH
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