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Synthetic method for glycine betaine hydrochloride

A synthesis method, hydrochloride technology, applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve the problems of solid waste, poor purity, and low yield of inorganic salts, and reduce side reactions Effect

Pending Publication Date: 2019-06-28
山东瑞弘生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a method for synthesizing betaine hydrochloride to solve the problems of poor purity, low yield and a large amount of solid waste of inorganic salts existing in the existing production process of betaine hydrochloride

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0015] A method for synthesizing betaine hydrochloride, adding 94.5g of monochloroacetic acid, 12g of catalyst, and 59 g of ethanol successively in a reaction bottle, then heating up to reflux at 105°C, dehydrating the molecular sieve at the reflux place, and completing the reaction in 3 hours, distilling the reaction solution with water After washing twice, the separated ethyl chloroacetate was distilled under reduced pressure at 72°C / 0.09kPa. The purity of the ethyl chloroacetate fraction was 99.7%, and the yield was 97.4%.

[0016] Add the ethyl monochloroacetate obtained in the previous step into the reaction flask, add a certain amount of water, and start feeding trimethylamine gas. The system temperature is kept at 43-45°C, and the reaction is completed in 6 hours. Add hydrochloric acid to raise the temperature for hydrolysis, and reflux at 95°C to collect the distilled water and ethanol. After collection, cool down at 10°C to crystallize and centrifuge to obtain betaine...

example 2

[0018] A method for synthesizing betaine hydrochloride, adding 94.5g of monochloroacetic acid, 15g of catalyst, and 92g of ethanol successively into a reaction bottle, then heating up to reflux at 110°C, dehydrating molecular sieves at the reflux place, and completing the reaction in 5 hours, distilling the reaction solution with water After washing twice, the separated ethyl chloroacetate was distilled under reduced pressure at 74°C / 0.09kPa. The purity of the ethyl chloroacetate fraction was 99.61%, and the yield was 96.3%.

[0019] Add the ethyl monochloroacetate obtained in the previous step into the reaction flask, add a certain amount of water, and start to feed trimethylamine gas, keep the system temperature at 33-40°C, and complete the reaction in 5 hours. Add hydrochloric acid to raise the temperature for hydrolysis, and reflux at 90°C to collect the distilled water and ethanol. After collection, cool down at 10°C to crystallize and centrifuge to obtain betaine hydroch...

example 3

[0021] A method for synthesizing betaine hydrochloride, adding 94.5g of monochloroacetic acid, 10g of catalyst, and 72 g of ethanol in turn to the reaction bottle, then heating up to reflux at 100°C, dehydrating the molecular sieve at the reflux place, and completing the reaction in 8 hours, distilling the reaction solution with water After washing twice, the separated ethyl chloroacetate was distilled under reduced pressure. The ethyl chloroacetate fraction was 72-73°C / 0.09kPa with a purity of 99.9% and a yield of 96.4%.

[0022] Add the ethyl monochloroacetate obtained in the previous step into the reaction flask, add a certain amount of water, and start feeding trimethylamine gas, keep the system temperature at 35-40°C, and complete the reaction in 5 hours. Add hydrochloric acid to raise the temperature for hydrolysis, and reflux at 100°C to collect the distilled water and ethanol. After collection, cool down at 15-20°C to crystallize and centrifuge to obtain betaine hydroc...

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Abstract

The invention relates to a synthetic method for glycine betaine hydrochloride. The synthetic method comprises the following steps: successively adding monochloro acetic acid, a catalyst and ethanol into a reaction bottle; then raising the temperature to 100-115 DEG C; dehydrating a molecular sieve in a reflux position; carrying out a reaction for 2-8 hours; washing a reaction liquid twice; distilling separated ethyl chloroacetate at a reduced pressure; adding ethyl monochloroacetate into the reaction bottle; adding a certain amount of water; introducing trimethylamine gas; keeping the temperature at 20-45 DEG C; carrying out a reaction for 2-6 hours; then adding hydrochloric acid to raise the temperature and hydrolyze to distill water and ethanol therein; and reducing the temperature by 10-15 DEG C and carrying out crystallization and centrifugalization to obtain the glycine betaine hydrochloride. By synthesizing ethyl monochloroacetate from monochloro acetic acid and ethanol, synthesizing ethyl glycine betaine hydrochloride from the obtained pure ethyl monochloroacetate and trimethylamine, raising the temperature to hydrolyze in the presence of hydrochloric acid to obtain ethanol,and cooling the concentrated liquor to separate out glycine betaine hydrochloride, the purity of the prepared glycine betaine hydrochlorid is over 99% and the yield reaches over 97%. Inorganic salt solid waste is avoided.

Description

technical field [0001] The invention relates to the technical field of furfural bioprocessing and utilization, in particular to a method for synthesizing betaine hydrochloride. Background technique [0002] Betaine hydrochloride is a general term for a class of organic compounds, also known as betaine hydrochloride, which is white to slightly yellow crystalline powder with sour taste and hygroscopicity, easily soluble in water and ethanol, insoluble in ether, Chloroform, reacts with alkali. Betaine hydrochloride is a high-efficiency, high-quality, economical nutritional additive widely used in livestock, poultry and aquaculture to induce food and promote growth. [0003] The current betaine hydrochloride production process uses chloroacetic acid and sodium hydroxide solution 1:1.2 (molar ratio) for neutralization reaction at 20-40°C, and then controls the temperature at 15-40°C to introduce trimethylamine for quaternization to generate betaine , and then acidified with hyd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/08C07C227/00C07C229/12C07C67/08C07C69/63
Inventor 李风光禹建科
Owner 山东瑞弘生物科技股份有限公司
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