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Method for preparing betaine hydrochloride

A technology of betaine hydrochloride and hydrochloric acid, which is applied in the preparation of organic compounds, chemical instruments and methods, and cyanide reaction preparation, can solve the problems of high energy consumption, large alcohol solvent consumption, cumbersome operation, etc., and achieve high yield, The effect of less raw material consumption and simple separation

Inactive Publication Date: 2012-08-01
CHINA ANIMAL HUSBANDRY IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current desalination technology generally adopts ion exchange and alcohol solution. The former is cumbersome to operate and consumes a lot of energy; the latter requires a large amount of alcohol solvent.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 394g of trimethylamine aqueous solution with a mass fraction of 33% into the reaction flask, cool down to about 0°C, add 94.5g of chloroacetic acid in batches under stirring, seal the reaction device, stir at 20-30°C for 1 hour, then heat up to 50°C React at ~60°C for 1.5h, then raise the temperature to 80-90°C for 0.5h. After the reaction is over, use 37% hydrochloric acid to adjust the pH to 1 to 3, raise the temperature, evaporate the water in the solution under reduced pressure, add an appropriate amount of chloroform, reflux for 15 minutes, heat filter, and filter the cake with a small amount of After washing with chloroform, dry and weigh to obtain betaine hydrochloride 147.34g, the yield in terms of chloroacetic acid is 96.2%, and the purity is 99.2%; the filtrate evaporates the solvent, and the gained solid is the hydrochloride of trimethylamine, weighing 108g , 99.5%.

Embodiment 2

[0017] Add 325g of trimethylamine aqueous solution with a mass fraction of 40% in the reaction flask, cool down to about 0°C, add 94.5g of chloroacetic acid in batches under stirring, seal the reaction device, stir at 20-30°C for 1 hour, then heat up to 50°C React at ~60°C for 1.5h, then raise the temperature to 80-90°C for 0.5h. After the reaction is over, use 20% hydrochloric acid to adjust the pH to 1 to 3, raise the temperature, evaporate the water in the solution under reduced pressure, add an appropriate amount of ethanol, reflux for 15 minutes, heat filter, and filter the cake with a small amount of ethanol After washing, dry and weigh to obtain betaine hydrochloride 146.5g, the yield in terms of chloroacetic acid is 95.7%, and the purity is 99.3%; 99.6%.

Embodiment 3

[0019] Add 325g of trimethylamine aqueous solution with a mass fraction of 40% in the reaction flask, cool down to about 0°C, add 94.5g of chloroacetic acid in batches under stirring, seal the reaction device, stir at 20-30°C for 1 hour, then heat up to 50°C React at ~60°C for 1.5h, then raise the temperature to 80-90°C for 0.5h. After the reaction is over, adjust the pH to 1.5 with 37% hydrochloric acid, increase the temperature, evaporate the water in the solution under reduced pressure, add an appropriate amount of ethanol, reflux for 15 minutes, heat filter, and filter the cake with a small amount of chloroform After washing with the mixed solution of ethanol (volume ratio is 1: 1), dry and weigh to obtain betaine hydrochloride 148.2g, in terms of chloroacetic acid, the yield is 96.8%, and the purity is 99.5%; the filtrate evaporates the solvent, and the gained solid is trimethylamine The hydrochloride, weighing 108.1g, purity is 99.7%.

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Abstract

The invention relates to a method for preparing betaine hydrochloride, comprising the following steps: reacting chloroacetic acid with an aqueous solution of trimethylamine, then acidizing the reaction solution, and then dehydrating to obtain a product, and carrying out aftertreatment on the product to obtain the betaine hydrochloride. The method has the advantages of short reaction steps, low raw material consumption, simple operation, and high yield.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of betaine hydrochloride. Background technique [0002] Betaine hydrochloride is an important fine chemical product, which is a feed additive. The product has three methyl groups and is an important methyl group donor, which can partially replace methionine and is widely used in poultry, livestock and fish feed. At present, there are two sources of betaine. One is the extraction method, that is, extraction from the waste residue and waste liquid of beet sugar production. This method has limited raw materials and high energy consumption. Another method is chemical synthesis. At present, in the synthesis, chloroacetic acid is firstly reacted with sodium hydroxide to obtain sodium chloroacetate, and then sodium chloroacetate is reacted with trimethylamine to obtain a mixture of betaine and sodium chloride. After desalination, the obtained be...

Claims

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Application Information

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IPC IPC(8): C07C229/12C07C227/08
Inventor 吴强三付光武潘春刚
Owner CHINA ANIMAL HUSBANDRY IND
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