Method for preparing hydroxypropyl diquaternary ammonium salt

A technology of diquaternary ammonium salt and hydroxypropyl, which is applied in the field of preparation of surfactant——hydroxypropyl diquaternary ammonium salt, which can solve problems such as inability to produce, high production cost, cumbersome operation, etc., and achieve easy operation and waste-free Few, Versatile Effects

Inactive Publication Date: 2008-04-30
JIANGSU FEIXIANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the two-step method is mostly used, that is, the halo-substituted hydroxypropyl monoquaternary ammonium salt is first prepared and purified, and then quaternized with another tertiary amine, which is cumbersome to operate and high in production cost. Alkyl groups impose stability requirements that prevent many species from being produced

Method used

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  • Method for preparing hydroxypropyl diquaternary ammonium salt
  • Method for preparing hydroxypropyl diquaternary ammonium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 203g of dodecyl dimethyl tertiary amine and 80g of ethanol into a 500ml reactor, start stirring and reflux, replace with nitrogen three times, add 84.4g of 20% hydrochloric acid dropwise, control the dropping temperature not greater than 60°C, and finish the dropping Then heat up to 50°C, start adding 46.26g of epichlorohydrin dropwise, cool with a water bath, control the temperature of the material to not exceed 60°C, keep the temperature at 50-85°C for 1 hour after dropping, and slowly raise the temperature to reflux (80-90°C) , constant temperature for 8 hours, lower the temperature to below 60°C and add 30g of ethanol, cool to below 40°C and discharge the material for analysis. Obtained 433.7g light yellow transparent liquid, measured quaternary ammonium compound active matter content 59.5%, free amine 0.7%, calculated yield 98.5%.

[0016] Take 500 g of the above light yellow liquid, add 150 g of acetone while stirring, filter to remove the solvent, and dry to ...

Embodiment 2

[0018] Add 101.5g of dodecyl dimethyl tertiary amine and 80g of ethanol into a 500ml reactor, start stirring and reflux, replace with nitrogen three times, drop in 84.4g of 20% hydrochloric acid, control the dropping temperature not more than 60°C, drop After the completion, the temperature was raised to 50°C, and 46.26g of epichlorohydrin was added dropwise, cooled in a water bath, and the temperature of the material was controlled not to exceed 60°C. Dialkyl dimethyl tertiary amine, slowly heat up to reflux (80-90°C), keep the temperature constant for 8 hours, cool down to below 60°C, add 30g of ethanol, cool down to below 40°C, and discharge for analysis. 455.0 g of light yellow transparent liquid was obtained, the content of quaternary ammonium compound active matter was 56.02%, the free amine was 0.83%, and the calculated yield was 98.1%.

Embodiment 3

[0020] Add 229.39g of tetradecyl dimethyl tertiary amine and 80g of isopropanol into a 500ml reactor, start stirring and reflux, replace with nitrogen three times, add 88g of 20% hydrochloric acid dropwise, and control the dropping temperature not to exceed 60°C. After dropping, the temperature was raised to 50°C, and 46.26g of epichlorohydrin was added dropwise, cooled in a water bath, and the temperature of the material was controlled not to exceed 60°C. ℃), keep the temperature for 12 hours, cool down to below 60°C and add 20g of ethanol, cool down to below 40°C and discharge for analysis. A light yellow transparent liquid was obtained, the content of the active substance of the quaternary ammonium compound was measured to be 56.7%, the free amine was 0.88%, and the calculated yield was 96.9%.

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Abstract

The invention discloses a preparation method of hydroxy propyl bisquaternary ammonium salt, and the preparation method has the advantages that the process is simple, and the process is green and environment-protective. The invention comprises the following steps: under the required air atmosphere, the HX water solution in the formula (1) is poured into a reaction vessel, the control temperature is 15 DEG C to 60 DEG C, chloroepoxy propane is dropped into the reaction vessel, after the reaction, the substance in the formula (2) is added at one time or in several times, or dropped continuously, the temperature rises to 40 DEG C to 120 DEG C, after the sufficient reaction, the target product of hydroxy propyl bisquaternary ammonium salt can be obtained, and the structure of the target product is expressed with the formula (3). The product can be extensively applied in the preparation of sterilization and algae extermination, metal anticorrosion, fabric dyeing and finishing, asphalt emulsification, waste paper deinking, fiber dispersion and electropositive ion monomer containing repellency water base.

Description

technical field [0001] The invention relates to a preparation method of surfactant-hydroxypropyl diquaternary ammonium salt. Background technique [0002] At present, the excellent properties of diquaternary ammonium surfactants are gradually being recognized and tend to be widely used, but their synthesis research lags far behind the application research. This may be related to the fact that this type of product has not yet been industrialized on a large scale, and the preparation of a small number of test products basically stays in the experimental stage, with insufficient consideration of cost and operation. At present, the two-step method is mostly used, that is, the halo-substituted hydroxypropyl monoquaternary ammonium salt is first prepared and purified, and then quaternized with another tertiary amine, which is cumbersome to operate and high in production cost. Alkyl groups impose stability requirements that prevent many species from being produced. Contents of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/40C07C213/04B01F17/18C09K23/18
Inventor 李胜兵陈军张鹏陈飞杜涛
Owner JIANGSU FEIXIANG CHEM
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