A kind of preparation method of ethyl ether group-α, ω-double long-chain alkyl dimethyl ammonium chloride surfactant

A long-chain alkyl dimethyl ammonium chloride and surfactant technology, which is applied in the preparation of amino hydroxyl compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of low final yield, long reaction time, and limitations Problems such as the popularization and application of gemini surfactants to achieve the effect of increasing productivity and improving antistatic performance

Active Publication Date: 2021-07-16
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above-mentioned documents have synthesized ether-alpha, omega-two long-chain alkyl dimethyl ammonium chloride surfactants, the reaction time is too long and the final yield is low, which limits the development of this class of gemini surfactants. Promote application

Method used

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  • A kind of preparation method of ethyl ether group-α, ω-double long-chain alkyl dimethyl ammonium chloride surfactant
  • A kind of preparation method of ethyl ether group-α, ω-double long-chain alkyl dimethyl ammonium chloride surfactant
  • A kind of preparation method of ethyl ether group-α, ω-double long-chain alkyl dimethyl ammonium chloride surfactant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Weigh 31.4g (0.2mol) of octyldimethyl tertiary amine, 38.5g of isopropanol, and 0.4g of solid sodium hydroxide into a four-neck flask, start stirring and heating. Weigh 11.4 g (0.08 mol) of dichloroethyl ether and add it to the dropping funnel, and start dropping when the temperature reaches 50° C., and control the dropping time for 10 minutes. After the dichloroethyl ether is added dropwise, the reaction temperature is controlled at 80° C., and the reaction time is 6 hours, and the product etheryl-α,ω-bisoctyldimethylammonium chloride can be obtained. After chemical analysis (water / chloroform two-phase titration, bromophenol blue as indicator, titration with sodium tetraphenylborate standard solution) and calculation, the reaction yield is 50.47wt%.

[0038] Rotate the liquid product obtained in the above steps to remove the solvent, wash 3 times with diethyl ether to remove the excess reactant dichloroethyl ether, then wash 3 times with acetone to remove the excess re...

Embodiment 2

[0040] Weigh 37g (0.2mol) of decyldimethyl tertiary amine, 50g of isopropanol, and 0.6g of solid sodium carbonate into a four-necked bottle, start stirring and heating. Weigh 12.9 g (0.09 mol) of dichloroethyl ether and add it to the dropping funnel, start dropping when the temperature reaches 55°C, and control the dropping time for 15 minutes. After the dichloroethyl ether is added dropwise, the reaction temperature is controlled at 83° C., and the reaction time is 8 hours, and the product etheryl-α,ω-didecyldimethylammonium chloride can be obtained. After chemical analysis (water / chloroform two-phase titration, bromophenol blue as indicator, titrated with sodium tetraphenylborate standard solution) and calculated, the reaction yield was 53.21wt%.

[0041] Rotate the liquid product obtained in the above steps to remove the solvent, wash 4 times with diethyl ether to remove the excess reactant dichloroethyl ether, then wash 4 times with acetone to remove the excess reactant te...

Embodiment 3

[0043] Weigh 42.6g (0.2mol) of dodecyldimethyl tertiary amine, 58g of deionized water, and 0.8g of solid sodium carbonate into a four-neck flask, start stirring and heating. Weigh 15.1 g (0.105 mol) of dichloroethyl ether and add it to the dropping funnel, start dropping when the temperature reaches 60°C, and control the dropping time for 20 minutes. After the dichloroethyl ether is added dropwise, the reaction temperature is controlled at 95° C., and the reaction time is 8 hours, and the product etheryl-α,ω-didodecyldimethylammonium chloride can be obtained. After chemical analysis (water / chloroform two-phase titration, bromophenol blue as indicator, titrated with sodium tetraphenylborate standard solution) and calculated, the reaction yield was 80.02wt%.

[0044] Rotate the liquid product obtained in the above steps to remove the solvent, wash 5 times with diethyl ether to remove the excess reactant dichloroethyl ether, then wash 5 times with acetone to remove the excess rea...

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Abstract

A preparation method of diethyl ether-α,ω-double long-chain alkyl dimethyl ammonium chloride surfactant is to add long-chain alkyl dimethyl amine tertiary amine, a solvent and an alkaline catalyst into a reactor, Chloroethyl ether is added to the dropping funnel, when the temperature of addition is reached, the dichloroethyl ether is added dropwise to the reactor, and the product is obtained by reacting under stirring conditions diethyl ether-α,ω-double long-chain alkyl dimethyl chloride ammonium chloride, the resulting liquid product was rotary evaporated to remove the solvent, washed with ether and then washed with acetone and dried in vacuo to obtain the product. The present invention has the advantages of short reaction time and high yield.

Description

technical field [0001] The present invention relates to the preparation of a quaternary ammonium salt-type gemini surfactant, in particular to an ether-alpha, omega-double long-chain alkyl dimethyl ammonium chloride surface active agent with an ether group as a linking group The preparation method of the agent. Background technique [0002] In recent years, a kind of surfactant with a new molecular structure——gemini surfactant is attracting people's attention. Gemini surfactants are a class of surfactants that are formed by connecting two hydrophilic head groups and two long hydrophobic chains at or near the hydrophilic head group through a linking group. Classified by the structure of the hydrophilic group, gemini surfactants can be divided into ionic and nonionic, and ionic surfactants are further divided into cationic, anionic and zwitterionic gemini surfactants. Among cationic gemini surfactants, the research on quaternary ammonium salt type gemini surfactants is the m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/08C07C213/04C07C213/10B01F17/18B01F17/46C09K23/18C09K23/46
CPCC07C213/04C07C213/10C09K23/00
Inventor 王志飞李运玲宋永波李俊
Owner CHINA RES INST OF DAILY CHEM IND
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