Preparation method of quaternary ammonium salt GTMAC

A technology of quaternary ammonium salt and mixed solvent, which is applied in the field of preparation of quaternary ammonium salt-glyceryl trimethyl ammonium chloride (GTMAC)

Inactive Publication Date: 2016-04-20
JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the reaction process, a catalyst needs to be added, which affects the properties of the product; in addition, the use of a single solvent has problems such as incomplete reaction of trimethylamine, which makes the reaction conversion rate low and the synthesis yield is not high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The preparation method of glyceryl trimethylammonium chloride in this example includes the following steps: 1000g of epichlorohydrin (10.81mol) is placed in a 5000mL reactor, and 915g (8.65mol) of mixed solvent (toluene: Chloroform = 1:1 molar ratio) after stirring evenly, then feed 160g trimethylamine (2.71mol); control trimethylamine aeration speed 80g / h, control the temperature in the reactor at 20°C; keep warm for 1h after passing trimethylamine After the reaction was completed, it was separated by suction filtration under dry conditions and washed with 100 g of the mixed solvent to obtain 405.5 g of a solid, with an epoxy value of 95.0% and a solid content of 99.15%.

Embodiment 2

[0018] The preparation method of glyceryl trimethylammonium chloride in this example includes the following steps: 500g of epichlorohydrin (5.40mol) is placed in a 5000mL reaction kettle, and 457g (4.14mol) of mixed solvent (toluene: Chloroform = 1:2 molar ratio) after stirring evenly, then pass 80g trimethylamine (1.35mol); control trimethylamine aeration speed 40g / h, control reactor temperature 30°C; after passing trimethylamine, keep warm for 1h and the reaction ends , and then separated by suction filtration under dry conditions, washed with 50 g of the mixed solvent to obtain 200 g of solid, and the epoxy value was 93.1%, and the solid content was 99.0%.

Embodiment 3

[0020] The preparation method of glyceryl trimethylammonium chloride in this example includes the following steps: 1000g of epichlorohydrin (10.81mol) is placed in a 5000mL reactor, and 915g (9.28mol) of mixed solvent (toluene: Chloroform:cyclohexane=1:1:1 molar ratio) after stirring evenly, then pass 160g trimethylamine (2.71mol); control trimethylamine aeration speed 80g / h, control reactor temperature 25°C; After the amine was incubated for 1 h, the reaction was completed, and then it was separated by suction filtration under dry conditions, and washed with 100 g of mixed solvent to obtain 409.1 g of solid, with an epoxy value of 93.5% and a solid content of 98.8%.

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Abstract

The invention belongs to the field of fine chemicals and in particular relates to a preparation method of a quaternary ammonium salt GTMAC. The preparation method comprises the following steps: (1) preparing a mixed solvent, and uniformly mixing the mixed solvent with epoxy chloropropane; (2) introducing trimethylamine gas into a mixed solvent system; controlling the temperature in a reactor to be 10 DEG C to 35 DEG C and the controlling a gas introduction speed to be 40g / h to 80g / h; meanwhile, stirring at a high speed and circularly cooling by chilled water; (3) after introducing the trimethylamine, keeping warm for 1 hour, and then separating, washing and purifying to obtain the product. The preparation method provided by the invention takes the mixed solvent as a reaction system and the synthesis yield is remarkably improved; an effective value of the product is further improved.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a preparation method of a quaternary ammonium salt—glyceryl trimethyl ammonium chloride (GTMAC). Background technique [0002] Glyceryltrimethylammonium chloride (GTMAC), also known as 2,3-epoxypropyltrimethylammonium chloride, as a quaternary ammonium cationic etherification agent, is widely used in sewage treatment, textile, Paper industry, daily chemical industry, oilfield additives and other fields. The reason why the traditional etherification agent 3-chloro-2 hydroxypropyltrimethylammonium chloride (CHPTMAC) can modify cellulose, lignin, chitosan, starch, etc. is that it can Under the catalysis, the active intermediate GTMAC is generated, and then the cationic quaternization of cellulose, lignin, chitosan and starch is carried out. Theoretically, alkali and CHPTMAC are 1:1 (molar ratio), but in actual production, excessive alkali is used, the reaction efficiency ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/27
CPCC07D301/27C07D303/08
Inventor 魏焱欧阳亮英瑜李中生周雍玉徐三善
Owner JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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