Synthesis method of epoxypropyltrimethylammonium chloride

A technology of glycidyltrimethylammonium chloride and synthesis method, which is applied in the direction of organic chemistry, etc., can solve the problems of high impurity content in products, affecting the quality of glycidyltrimethylammonium chloride, affecting product quality, etc. , to achieve the effect of high product quality, cost saving and large economic benefits

Inactive Publication Date: 2012-05-02
莫智龙
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The advantage of this method is that the requirements for personnel and equipment are not high, but the impurity content of the product is high. The main impurities are epichlorohydrin, 1,3-dichloro-2-propanol, and diquaternary ammonium salt (change the melting and boiling point of the product) etc. seriously affect the quality of 3-chloro-2-hydroxypropyltrimethylammonium chloride products, thereby also affecting the quality of epoxypropyltrimethylammonium chloride

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1), first add 2mol of dichloroethane in the four-necked flask, then add 1mol of epichlorohydrin, the temperature is controlled at 20-25 degrees Celsius, and 0.99mol of trimethylamine gas is uniformly passed into the four-necked flask, and the tail gas Absorb with water.

[0025] (2), after filling the trimethylamine gas, react for another 8 hours. After the reaction is over, cool down to 5 degrees Celsius, stop stirring during the cooling process, and filter to obtain white crystals.

[0026] (3) Put the white crystals in an extraction bottle, add 1 mol of distilled water, shake, let stand for five minutes, and separate dichloroethane. Water bath heating, water bath temperature is 65 degrees centigrade, vacuum distillation, sampling detection, wherein sampling detection comprises the following steps:

[0027] ①Magnesium chloride saturated solution: Weigh 500g of magnesium chloride solid in a beaker, add 150ml of pure water to dissolve, let stand for 24 hours, transfer...

Embodiment 2

[0038] (1) First add 2mol of dichloroethane into the three-necked flask, then add 1mol of epichlorohydrin, control the temperature at 20-25 degrees Celsius, pass 0.99mol of trimethylamine gas into the three-necked flask at a uniform speed, and absorb the tail gas with water .

[0039] (2), after filling the trimethylamine gas, react for another 10 hours. After the reaction, cool down to 10 degrees Celsius, stop stirring during the cooling process, and filter to obtain white crystals.

[0040] (3) Put the white crystals in an extraction bottle, add 1 mol of deionized water, shake, let stand for five minutes, and separate dichloroethane. Water-bath heating again, water-bath temperature is 68 degrees centigrade, vacuum distillation, sampling detection, wherein detection method is identical with embodiment column 1, after the concentration of glycidyltrimethylammonium chloride solution reaches 69%, stop distillation, cooling, get the desired product.

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Abstract

The invention relates to a synthesis method of epoxypropyltrimethylammonium chloride. The method comprises the following steps: adding dichloroethane and epichlorohydrin in a reaction bottle in turn at 20-30 DEG C, injecting trimethylamine gas in the reaction bottle in a constant speed, reacting for 8-10h after injecting, reducing temperature to 5-15 DEG C while stopping stirring, filtrating to obtain white crystals; adding water to separate dichloroethane, heating with water bath to 60-70 DEG C, performing reduced pressure distillation, taking samples to test, stopping distillation when the concentration of epoxypropyltrimethylammonium chloride solution reaches 69%, and reducing temperature to obtain the desired product. The method overcomes the defect that the existing synthesized epoxypropyltrimethylammonium chloride contains impurities; intermediate 3-chloro-2-hydroxypropyltrimethyl ammonium chloride is not needed to prepare and the product is directly prepared so as to avoid the preparation of impurity 1,3-dichloro-2-propanol and bisquaternary ammonium salt, has high product quality and save the cost.

Description

technical field [0001] The present invention relates to a kind of synthetic method of glycidyl trimethyl ammonium chloride. Background technique [0002] At present, most epoxypropyltrimethylammonium chloride (commonly known as: cationic etherification agent, English abbreviation GTA) on the market is made of 3-chloro-2-hydroxypropyltrimethylammonium chloride plus sodium hydroxide converted to obtain. [0003] The synthetic method of 3-chloro-2-hydroxypropyltrimethylammonium chloride (English abbreviation CTA) is: first add hydrochloric acid reaction to trimethylamine solution to generate trimethylamine hydrochloride, then add equimolar epoxy chloride propane reaction. The advantage of this method is that the requirements for personnel and equipment are not high, but the impurity content of the product is high. The main impurities are epichlorohydrin, 1,3-dichloro-2-propanol, and diquaternary ammonium salt (change the melting and boiling point of the product) Etc. have ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/36
Inventor 莫智龙
Owner 莫智龙
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