Preparation process for thiamine hydrochloride

A technology for the preparation of thiamine hydrochloride, which is applied in the direction of organic chemistry, can solve the problems of low bulk density, poor fluidity, and large fluctuations in total chlorine content of thiamine hydrochloride, so as to reduce the risk of environmental pollution and solve the fluctuation of total chlorine Larger and more stable total chlorine content

Inactive Publication Date: 2013-11-13
江苏兄弟维生素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional preparation process of thiamine hydrochloride is: add chlorosulfonic acid dropwise into a hydrogen chloride generating tank filled with hydrochloric acid, pass the generated hydrogen chloride into a mixture of thiamine nitrate and methanol, and convert thiamine nitrate into thiamine hydrochloride , the main defects of this process are: the chlorosulfonic acid used in the production of hydrogen chloride is a highly toxic and dangerous chemical. When sulfonic acid produces hydrogen chloride, mixed waste acid containing sulfuric acid and hydrochloric acid is produced, which is difficult to handle, and the waste acid contains a large amount of residual hydrogen chloride, and the utilization rate of hydrogen chloride is low
At the same time, the thiamine hydrochloride produced by this process has low bulk density, poor fluidity, and large fluctuations in total chlorine content.

Method used

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  • Preparation process for thiamine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Preparation of hydrogen chloride gas:

[0018] Weigh 700.5g of 31% hydrochloric acid and heat it to 110°C. The volatilized hydrogen chloride gas is condensed by a condenser tube and then scrubbed with concentrated sulfuric acid to dry and dehydrate.

[0019] (2) Preparation of acid methanol solution:

[0020] Pass the dried hydrogen chloride gas into 88g of methanol for absorption. After three hours, detect the mass concentration of hydrogen chloride in the prepared acid methanol, and stop the ventilation when it reaches 33%. The entire preparation process takes about 3.5 hours.

[0021] (3) Preparation of thiamine hydrochloride:

[0022] Add 100.1 g of thiamine nitrate and 500.0 g of methanol into a four-neck flask to prepare a methanol solution of thiamine nitrate; control the temperature at 0-70°C, and add the prepared methanol hydrochloric acid solution dropwise to the methanol of thiamine nitrate In the solution, it took 2 hours and 10 minutes. After the drop...

Embodiment 2

[0024] (1) Preparation of hydrogen chloride gas:

[0025] Weigh 700.2g of 31% hydrochloric acid and heat it to 110°C. The volatilized hydrogen chloride gas is condensed by a condenser tube and then scrubbed with concentrated sulfuric acid to dry and dehydrate.

[0026] (2) Preparation of acid methanol solution:

[0027] Pass the dried hydrogen chloride gas into 88g of methanol for absorption. After three hours, detect the mass concentration of hydrogen chloride in the prepared acid methanol, and stop the ventilation when it reaches 33%. The entire preparation process takes about 3 hours and 20 minutes.

[0028] (3) Preparation of thiamine hydrochloride:

[0029] Add 100.0 g of measured thiamine nitrate and 500.5 g of methanol into a four-neck flask to prepare a methanol solution of thiamine nitrate; control the temperature at 0-70°C, and add dropwise the prepared methanol hydrochloric acid solution to the methanol of thiamine nitrate In the solution, it took 2 hours and 05 m...

Embodiment 3

[0031] (1) Preparation of hydrogen chloride gas:

[0032] Weigh 700.3g of 31% hydrochloric acid and heat it to 110°C. The volatilized hydrogen chloride gas is condensed by a condenser tube and then scrubbed with concentrated sulfuric acid to dry and dehydrate.

[0033] (2) Preparation of acid methanol solution:

[0034] Pass the dried hydrogen chloride gas into 88g of methanol for absorption. After three hours, detect the mass concentration of hydrogen chloride in the prepared acid methanol, and stop the ventilation when it reaches 33%. The entire preparation process takes about 3 hours and 30 minutes.

[0035] (3) Preparation of thiamine hydrochloride:

[0036] Add 100.1 g of measured thiamine nitrate and 500.4 g of methanol into a four-neck flask to prepare a methanol solution of thiamine nitrate; control the temperature at 0-70°C, and add the prepared methanol solution of hydrochloric acid dropwise to the methanol of thiamine nitrate In the solution, it took 2 hours and 1...

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Abstract

The invention relates to the field of preparation technology of chemical products, and particularly relates to a preparation process for thiamine hydrochloride. The preparation process comprises the steps of heating concentrated hydrochloric acid, subjecting a desorbed hydrogen chloride gas to cooling, drying and dehydration to obtain a hydrogen chloride gas; introducing the dry hydrogen chloride gas to a methanol solution to obtain a hydrogen chloride-containing acid methanol solution; dropwise adding the acid methanol solution to a methanol solution of thiamine nitrate for reaction; and obtaining thiamine hydrochloride after filtering, washing and drying. The preparation process for thiamine hydrochloride can prevent use of highly toxic and dangerous chemical chlorosulfonic acid, so that environment risks can be reduced; the utilization rate of hydrochloric acid and bulk density of thiamine hydrochloride can be increased; and a total chlorine content of thiamine hydrochloride is stable.

Description

technical field [0001] The invention relates to the technical field of preparation of chemical products, in particular to a preparation process of thiamine hydrochloride. Background technique [0002] Thiamine hydrochloride is the hydrochloride salt of thiamine, a form of vitamin B1. The traditional preparation process of thiamine hydrochloride is: add chlorosulfonic acid dropwise into a hydrogen chloride generating tank filled with hydrochloric acid, pass the generated hydrogen chloride into a mixture of thiamine nitrate and methanol, and convert thiamine nitrate into thiamine hydrochloride , the main defects of this process are: the chlorosulfonic acid used in the production of hydrogen chloride is a highly toxic and dangerous chemical. When sulfonic acid produces hydrogen chloride, mixed waste acid containing sulfuric acid and hydrochloric acid is produced, which is difficult to handle, and the waste acid contains a large amount of residual hydrogen chloride, and the uti...

Claims

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Application Information

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IPC IPC(8): C07D417/06
Inventor 李健平李来成陈英明
Owner 江苏兄弟维生素有限公司
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