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Novel method for synthesizing quaternary ammonium salts

A quaternary ammonium salt and a new method technology, which is applied in the field of preparation of quaternary ammonium salt, can solve the problems that the industrialization process of quaternary ammonium salt has not yet been found, high production cost, and large consumption

Active Publication Date: 2010-01-13
包珣
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] People have carried out a large amount of research and development to the production technology of high-purity quaternary ammonium salt, as the patent No. is that 200410012215.1 discloses to prepare ester amine class quaternary ammonium salt with dimethyl carbonate and ester amine reaction; Dimethyl ester, diethyl sulfate, dimethyl carbonate and diethyl carbonate, etc. are used as alkylating reagents to synthesize quaternary ammonium quaternized aminoacetonitrile; the patent application number is 200510061094.4. (Ammonia) salt is the method for synthesizing quaternary ammonium salt in the next step of catalyst action, but the used catalyzer of this preparation method is ionic liquid 1-ethyl-3-methylimidazole hydrobromide consumption big, causes production cost height
[0004] The existing published patents related to the production process of quaternary ammonium salts are generally the results of laboratory experiments or pilot tests for the preparation of kilograms of quaternary ammonium salts, and the industrialization process of hundreds of kilograms or tons of quaternary ammonium salts has not yet been found.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Weigh 400 kg of dodecyl dimethyl tertiary amine and place it in a 1000 liter enamel reaction kettle, pump 204 kg of concentrated hydrochloric acid, 125 kg of methanol and 0.4 kg of ionic liquid 1-ethyl-3 at a flow rate of 150 kg / hour - Methylimidazole hydrochloride, stirred at 55° C. and reacted under a nitrogen atmosphere under normal pressure, and the reaction time was 3 hours. After the reaction product was vacuum-dried (the drying temperature was controlled at 80°C), it was added to a 1000L high-pressure reactor, and after the reactor was purged three times with nitrogen, 188 kg of dimethyl carbonate and 80 kg of The methanol mixture was closed and reacted at a reaction temperature of 175° C. and a reaction pressure of 1.7 MPa, and reacted for 12 hours under stirring. The reaction product was vacuum-dried (the drying temperature was controlled at 80° C.) to obtain 492 kg of dodecyltrimethylammonium chloride, with a yield of 99.4% and a purity of 99.2% through quanti...

Embodiment 2

[0014] Weigh 400 kg of dodecyl dimethyl tertiary amine and place it in a 1000 liter enamel reactor, pump 298 kg of hydrobromic acid, 125 kg of ethanol and 0.4 kg of ionic liquid 1-ethyl- The mixture of 3-methylimidazolium hydrobromide was stirred and reacted at 50° C. for 3 hours, and reacted under normal pressure under a nitrogen atmosphere. After the reaction product was vacuum-dried (the drying temperature was controlled at 80°C), it was added to a 1000L high-pressure reactor, and after the reactor was purged three times with nitrogen, 188 kg of dimethyl carbonate and 80 kg of The methanol mixture was closed and reacted at a reaction temperature of 175° C. and a reaction pressure of 1.7 MPa, and reacted for 12 hours under stirring. The reaction product was vacuum dried (the drying temperature was controlled at 80° C.) to obtain about 573 kg of dodecyltrimethylammonium bromide with a yield of 99.1% and a purity of 99.2%.

Embodiment 3

[0016] Weigh 400 kg of tetradecyl dimethyl tertiary amine and place it in a 1000 liter enamel reaction kettle, pump 180 kg of concentrated hydrochloric acid, 125 kg of acetonitrile and 0.4 kg of ionic liquid 1-butyl-3 at a flow rate of 125 kg / hour - The mixture of methylimidazole hydrochloride was stirred and reacted at 60° C. for 3 hours, and reacted under normal pressure under a nitrogen atmosphere. After the reaction product was vacuum-dried (the drying temperature was controlled at 80°C), it was added to a 1000L high-pressure reactor, and after the reactor was purged three times with nitrogen, 168 kg of dimethyl carbonate and 80 kg of The methanol mixture was closed and reacted at a reaction temperature of 175° C. and a reaction pressure of 1.7 MPa, and reacted for 12 hours under stirring. The reaction product was vacuum-dried (the drying temperature was controlled at 80° C.) to obtain about 482 kg of tetradecyltrimethylammonium chloride with a yield of 99.6% and a purity ...

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Abstract

The invention discloses a novel method for synthesizing quaternary ammonium salt, which is characterized in that methyl-containing quaternary ammonium salts are prepared through the reaction of dimethyl carbonate, tertiary amine and inorganic acid or organic acid. The method specifically comprises the steps: putting tertiary amine in proportion in a reactor; pumping a corresponding amount of mixture of inorganic acid or organic acid, polar solvent and ionic liquid catalyst in appropriate controlled flow into the reactor; stirring for reaction at an appropriate temperature in nitrogen atmosphere; putting vacuum-dried products after reaction is completed in the reactor; blowing and washing the reactor with nitrogen; pumping the mixture of dimethyl carbonate and polar solvent in appropriate controlled flow into the reactor for hermetic reaction; performing reaction under the pressure between 0.5 and 3 MPa at reaction temperature between 100 and 200 DEG C; stirring till reaction is completed; and obtaining reaction products which are the methyl-containing quaternary ammonium salts. The method greatly improves the utilization rate of catalysts and is small in the amount of catalysts, and the reaction yield and purity of the method are over 99 percent.

Description

Technical field: [0001] The invention relates to a new synthesis process of quaternary ammonium salts, in particular to a process for preparing quaternary ammonium salts by reacting dimethyl carbonate, tertiary amine and no (organic) organic acid under the condition of catalyst and polar solvent. Background technique: [0002] Quaternary ammonium salts are a class of cationic surfactants, among which high-purity quaternary ammonium salts are excellent phase transfer catalysts and play a key role in organic synthesis. [0003] People have carried out a large amount of research and development to the production technology of high-purity quaternary ammonium salt, as the patent No. is that 200410012215.1 discloses to prepare ester amine class quaternary ammonium salt with dimethyl carbonate and ester amine reaction; Dimethyl ester, diethyl sulfate, dimethyl carbonate and diethyl carbonate, etc. are used as alkylating reagents to synthesize quaternary ammonium quaternized aminoac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/12C07C211/62C07C211/63
CPCY02P20/54
Inventor 翟和生
Owner 包珣
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