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Synthesis method and application of 2-chloride, 3-poly hydroxypropyl dodecylamine quaternary ammonium salt surfactant

A technology of surfactant and polyhydroxypropyl, which is applied in the field of 2-chlorination, can solve the problems of high price and difficulty in mass production of Gemini surfactant, and achieve the effects of easy industrialization, high conversion rate and good performance

Inactive Publication Date: 2017-02-22
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although in recent decades, the development and research of Gemini surfactants has been a hot spot, but at present, Gemini surfactants are relatively expensive and difficult to produce in large quantities, and there is still a distance from industrialization

Method used

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  • Synthesis method and application of 2-chloride, 3-poly hydroxypropyl dodecylamine quaternary ammonium salt surfactant
  • Synthesis method and application of 2-chloride, 3-poly hydroxypropyl dodecylamine quaternary ammonium salt surfactant
  • Synthesis method and application of 2-chloride, 3-poly hydroxypropyl dodecylamine quaternary ammonium salt surfactant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] The Gemini surfactant 2-chlorinated, 3-polyhydroxypropyl dodecylamine quaternary ammonium salt surfactant is synthesized by a two-step method, that is, dodecylamine is first reacted with epichlorohydrin to synthesize with dichloro substitution The intermediate of the base; the dichloro intermediate is then reacted with N,N-dimethyldodecylamine to synthesize the Gemini surfactant 2-chlorinated, 3-polyhydroxypropyldodecylamine quaternary ammonium salt Surfactant. The specific operations are as follows:

[0063] 1) Synthesis of intermediate N,N-bis(2-hydroxy-3-chloropropyl)dodecylamine:

[0064] In a four-necked flask equipped with mechanical stirring, reflux condenser, thermometer and dropping funnel, accurately weigh 9.2680g (0.05mol) of dodecylamine and add, then add 50mL of absolute ethanol as solvent, stir to dissolve dodecylamine, Then take 9.3455 g (approximately 7.92 ml, 0.10 mol) of epichlorohydrin with a purity of 99% into the dropping funnel, and slowly add dropwis...

Embodiment 2

[0085] According to the results of the single factor experiment in Example 1, the fixed solvent dosage in the experiment was 50mL. The orthogonal experiment was used to investigate the influence of the four factors of raw material molar ratio, reaction temperature, reaction time, and reaction solvent on the yield of the target product. The L9(34) orthogonal table has investigated the four factors and three levels of the reaction. The orthogonal experimental conditions are designed in Table 1, and the target product yield is used as an indicator. The results obtained from the orthogonal experimental conditions in Table 1 are listed in Table 2. .

[0086] Table 1 Orthogonal experimental factors-level table

[0087] factor Raw material molar ratio (A) Reaction temperature (B) Response time (C) Reaction solvent (D) 1 1.8:190℃12h Absolute ethanol 2 2.0:1100℃14h N-propanol 3 2.2:1110℃16h Isopropanol

[0088] Table 2 Orthogonal experiment optimization data table

[0089]

[0090] It ca...

Embodiment 3

[0092] The actual optimal scheme of Examples 1 and 2 was used to produce 2-chlorinated, 3-polyhydroxypropyl dodecylamine quaternary ammonium salt surfactant, and the specific steps are:

[0093] 1) Synthesis of intermediate N,N-bis(2-hydroxy-3-chloropropyl)dodecylamine:

[0094] In a four-necked flask equipped with mechanical stirring, reflux condenser, thermometer and dropping funnel, accurately weigh dodecylamine (its infrared spectrum such as Figure 7 As shown) 9.2680g (0.05mol) was added, and then 50mL of absolute ethanol was added as a solvent, stirred to dissolve dodecylamine, and then 99% pure epichlorohydrin ((The infrared spectrum is as Figure 8 Shown)) 9.3455g (approximately 7.92ml, 0.10mol) into the dropping funnel, slowly dripped, after the dripping is completed, continue to stir and react at room temperature for 12h. After the reaction is stopped, set the temperature of the water bath of the rotary evaporator to 40°C, and distill under reduced pressure for 2 hours to ...

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Abstract

The invention discloses a synthesis method and an application of a 2-chloride, 3-poly hydroxypropyl dodecylamine quaternary ammonium salt surfactant. According to the synthesis method of the surfactant, firstly, dodecylamine and epichlorohydrin react to synthesize an intermediate with a di-chlorine substituent group, and the intermediate and N,N-dimethyl dodecylamine react to synthesize the 2-chloride, 3-poly hydroxypropyl dodecylamine quaternary ammonium salt surfactant. The method realizes synthesis of a target product with a two-step method and has the advantages that the cost is low and the surface activity of the product is high. The synthesized 2-chloride, 3-poly hydroxypropyl dodecylamine quaternary ammonium salt surfactant is applied to a combinational surfactant, and the performance of an obtained surfactant with a combined system is superior to that of a corresponding single system.

Description

Technical field [0001] The invention belongs to the technical field of fine chemicals, and specifically relates to a synthesis method and application of a 2-chlorinated, 3-polyhydroxypropyl dodecylamine quaternary ammonium salt surfactant. Background technique [0002] Gemini surfactants are two traditional surfactant molecules that are connected by a special linking group to form a new type of surfactant. Gemini surfactant quaternary ammonium salt has excellent properties such as reducing the surface tension of the solution, solubilizing, wetting, anti-corrosion, antistatic, emulsification and demulsification, dispersion and agglomeration, foaming and defoaming, etc., and thus is an important class Fine chemicals are widely used in various fields of production and life such as synthetic detergents, food industry, textile industry, agriculture, mining industry, petroleum exploration and mining, paper industry, transportation, civil construction industry, environmental protection,...

Claims

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Application Information

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IPC IPC(8): B01F17/18C09K23/18
CPCC09K23/16
Inventor 胡震于海莲王青松
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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