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Preparation method of biquaternary ammonium salt

A technology of biquaternary ammonium salt and diammonium salt is applied in chemical instruments and methods, preparation of amino-substituted functional groups, organic chemistry, etc., and can solve the problems of long production cycle, complicated process, low yield, etc., and achieves short production cycle, Simple process and high yield

Inactive Publication Date: 2015-06-10
YANCHENG TEACHERS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above three preparation methods all have the problems of complicated process, long production cycle, low yield and high cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 60g of ethylenediamine into the reactor, add concentrated hydrochloric acid dropwise, neutralize under magnetic stirring, then use a constant temperature water bath to evaporate about 70% of the water, and then vacuum dry to obtain ethylenediamine hydrochloric acid Salt; Weigh 67g of ethylenediamine hydrochloride and 270g of dimethyl carbonate, add them to a 1-liter autoclave, purge with nitrogen to drive off the air in the kettle, seal it, stir and raise the temperature, at a reaction temperature of 190℃ Continue the reaction for 10 hours; prepare about 88 g of N,N'-hexamethylethylenediammonium chloride diquaternary ammonium salt.

Embodiment 2

[0019] Weigh 60g of ethylenediamine into the reactor, add concentrated hydrochloric acid dropwise, neutralize under magnetic stirring, then use a constant temperature water bath to evaporate about 70% of the water, and then vacuum dry to obtain ethylenediamine hydrochloric acid Salt; Weigh 67g of ethylenediamine hydrochloride and 270g of dimethyl carbonate, add them to a 1-liter autoclave, purge with nitrogen to drive off the air in the kettle, seal, stir and raise the temperature, at a reaction temperature of 210℃ , The reaction continued for 10 hours; after the reaction, about 102 g of N,N'-hexamethylethylenediammonium chloride diquaternary ammonium salt was prepared.

Embodiment 3

[0021] Weigh 60g of ethylenediamine into the reactor, add concentrated hydrochloric acid dropwise, neutralize under magnetic stirring, then use a constant temperature water bath to evaporate about 70% of the water, and then vacuum dry to obtain ethylenediamine hydrochloric acid Salt; Weigh 67g of ethylenediamine hydrochloride and 270g of dimethyl carbonate, add them to a 1-liter autoclave, purge with nitrogen to drive off the air in the kettle, seal, stir, and raise the temperature, at a reaction temperature of 280℃ , Continue the reaction for 1.5 hours to obtain about 76g of N,N'-hexamethylethylenediammonium diquaternary ammonium chloride.

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Abstract

The invention provides a preparation method of a diquaternary ammonium salt. Dimethyl carbonate and a diammonium salt are placed in a reaction kettle, and the diquaternary ammonium salt is prepared under airtight conditions at the reaction temperature of 60-280 DEG C for the reaction time of 0.5-24 h. A substituent of nitrogen in cation [CH3NR1R2(CH2)nN(CH3)R3R4]<2+> of the diquaternary ammonium salt is one or more than one of alkyl, alkenyl, alkynyl and aryl selected from R1, R2, R3 and R4, or is an organic group containing hydrocarbon and one or more than one element of oxygen, nitrogen, phosphorus, sulfur, fluorine, chlorine and bromine; and an anion of the diquaternary ammonium salt is one of sulfate ion, hydrosulfate ion, nitrate ion, phosphate ion, hydrophosphate ion, dihydrophosphate ion, fluorine, chlorine, bromine, iodine, sulfur, carbonate ion, oxalate ion, acetate ion and carboxylate ion. The invention has the advantages of simple process, short production period, high yield and low cost; the diquaternary ammonium salt containing designated anions can be further synthesized; and the product has wide application.

Description

Technical field [0001] The invention relates to a method for preparing a surfactant, in particular to a method for preparing a double quaternary ammonium salt. Background technique [0002] Double quaternary ammonium salt is a new type of surfactant, belonging to the category of Gemini (twin or dimer) surfactants. In 1971, Bunton et al. synthesized a type of cationic Gemini surfactant for the first time: alkyl-α,ω-bis-dialkyl bis-methyl alkyl ammonium bromide (C n H 2n+1 N + (CH 3 ) 2 Br)(CH 2 ) 5 (C n H 2n+1 N + (CH 3 ) 2 Br), this is the original double quaternary ammonium salt. It is different from traditional surfactants in that it generally has two hydrophobic alkyl chains, two ionic head groups and one linking group. Due to the special structure of double quaternary ammonium salt surfactant, it has higher surface activity and a series of unique physical and chemical properties. It is widely used in daily chemical, textile, printing and dyeing, mining, asphalt, construction...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/20C07C211/63B01F17/18C09K23/18
Inventor 戴春华茆福林
Owner YANCHENG TEACHERS UNIV
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