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Preparation method of biquaternary ammonium salt

A technology of double quaternary ammonium salt and diammonium salt, which is applied in chemical instruments and methods, preparation of functional groups substituted with amino groups, organic chemistry, etc., can solve the problems of long production cycle, complex process and high cost, and achieve short production cycle and simple process , low cost effect

Inactive Publication Date: 2011-02-16
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 and place it in a reactor, add concentrated hydrochloric acid drop by drop, carry out neutralization reaction under magnetic stirring, then use a constant temperature water bath to evaporate and remove about 70% of water, and then carry out vacuum drying to obtain ethylenediamine hydrochloric acid Salt; Weigh 67g ethylenediamine hydrochloride and 270g dimethyl carbonate, add them to a 1-liter high-pressure reaction kettle, use nitrogen to blow away the air in the kettle, seal it, stir and heat up, and the reaction temperature is 190°C The reaction was continued for 10 hours; about 88 g of N, N'-hexamethylethylenediammonium diquaternary ammonium chloride were obtained.

Embodiment 2

[0019] Weigh 60g of ethylenediamine and place it in a reactor, add concentrated hydrochloric acid drop by drop, carry out neutralization reaction under magnetic stirring, then use a constant temperature water bath to evaporate and remove about 70% of water, and then carry out vacuum drying to obtain ethylenediamine hydrochloric acid Salt; Weigh 67g of ethylenediamine hydrochloride and 270g of dimethyl carbonate, add them to a 1-liter high-pressure reaction kettle, blow away the air in the kettle with nitrogen, seal it, stir, and heat up, at a reaction temperature of 210°C , and continued to react for 10 hours; after the reaction, about 102 g of N, N'-hexamethylethylenediammonium diquaternary ammonium chloride were obtained.

Embodiment 3

[0021] Weigh 60g of ethylenediamine and place it in a reactor, add concentrated hydrochloric acid drop by drop, carry out neutralization reaction under magnetic stirring, then use a constant temperature water bath to evaporate and remove about 70% of water, and then carry out vacuum drying to obtain ethylenediamine hydrochloric acid Salt; Weigh 67g of ethylenediamine hydrochloride and 270g of dimethyl carbonate, add them to a 1-liter high-pressure reaction kettle, blow away the air in the kettle with nitrogen, seal it, stir, and heat up, at a reaction temperature of 280°C , continued the reaction for 1.5 hours, and obtained about 76 g 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 preparation method of a surfactant, in particular to a preparation method of a diquaternary ammonium salt. Background technique [0002] Diquaternary ammonium salts are a new class of surfactants that belong to the category of Gemini (twinned or dimerized) surfactants. In 1971, Bunton et al synthesized a class of cationic Gemini surfactants for the first time: alkyl-α, ω-bis-dialkyl dimethyl 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), which is the original double quaternary ammonium salt. Unlike traditional surfactants, it generally has two hydrophobic alkyl chains, two ionic head groups and a linking group. Due to the special structure of diquaternary ammonium salt surfactant, it has higher surface activity and a series of other unique physical and chemical properties. It is widely used in daily chemical industry, textile, printing and dyeing, mining, asphalt, con...

Claims

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Application Information

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IPC IPC(8): C07C211/63B01F17/18C07C209/20C09K23/18
Inventor 戴春华茆福林
Owner YANCHENG TEACHERS UNIV
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