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Preparation method of thiamine mononitrate

A technology of thiamine nitrate and thiamine sulfate, which is applied in the field of chemical engineering, can solve the problems of time and manpower consumption, potential safety hazards, cumbersome steps, etc., and achieve the effects of reducing energy consumption and production costs, avoiding danger, and simple operating conditions

Inactive Publication Date: 2019-06-28
CHIFENG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Using ammonium nitrate as the salt-transfer reagent in the preparation process of thiamine nitrate has many problems in production: on the one hand, ammonium nitrate solid belongs to a class of dangerous goods, and there are certain safety hazards in the large-scale use of ammonium nitrate solid in industrial production; On the other hand, the preparation of ammonium nitrate solution in advance consumes time and manpower, and a set of ammonium nitrate preparation reaction kettle is added
Although the method avoids the use of ammonium nitrate in large quantities, calcium ions are introduced in the preparation method, and there is still a large amount of ammonium sulfate in the mother liquor, and the steps are more cumbersome

Method used

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  • Preparation method of thiamine mononitrate
  • Preparation method of thiamine mononitrate
  • Preparation method of thiamine mononitrate

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Embodiment 1: a kind of preparation method of thiamine nitrate comprises following processing steps:

[0041] S1. Thoroughly mix 25 g of thiothiamine with 26 g of 35% hydrogen peroxide; adjust the pH of the solution to 4 with 0.5 g of 1% sulfuric acid, and control the oxidation temperature at 10-16°C. Add 1.75g ​​of activated carbon for decolorization, the decolorization temperature is 23°C, stir for 1h, and filter with suction to obtain thiamine sulfate;

[0042] S2. Fully mix 75.65 g of thiamine sulfate and 3.45 g of nitric acid with a mass fraction of 65% according to a mass ratio of 22:1; add the nitric acid at one time, and control the temperature below 10°C. The stirring speed is 112r / min;

[0043] S3. Use a peristaltic pump to slowly add ammonia water. The rotation speed of the peristaltic pump is 0.1-0.7 rpm. Add ammonia water with a mass fraction of 16.57% to the mixed solution of thiamine sulfate and nitric acid, and adjust the pH value of the mixed solution ...

Embodiment 2

[0046] Embodiment 2: a kind of preparation method of thiamine nitrate comprises following processing steps:

[0047] S1. Thoroughly mix 25g of thiothiamine with 26g of 35% hydrogen peroxide; use 0.5g of 1% sulfuric acid to adjust the pH of the solution to 4, and control the oxidation temperature at 10-16°C. Add 1.75g ​​of activated carbon for decolorization, the decolorization temperature is 23°C, stir for 1h, and filter with suction to obtain thiamine sulfate;

[0048] S2. Fully mix 75.65 g of thiamine sulfate and 3.45 g of nitric acid with a mass fraction of 65% according to a mass ratio of 22:1; add the nitric acid at one time, and control the temperature below 10°C. The stirring speed is 112r / min;

[0049] S3. Use a peristaltic pump to slowly add ammonia water. The speed of the peristaltic pump is 0.1-0.7 rpm. Add ammonia water with a mass fraction of 21.04% to the mixed solution of thiamine sulfate and nitric acid, and adjust the pH value of the mixed solution to about 7...

Embodiment 3

[0052] Embodiment 3: a kind of preparation method of thiamine nitrate comprises following processing steps:

[0053]S1. Thoroughly mix 25 g of thiothiamine with 26 g of 35% hydrogen peroxide; adjust the pH of the solution to 4 with 0.5 g of 1% sulfuric acid, and control the oxidation temperature at 10-16°C. Add 1.75g ​​of activated carbon for decolorization, the decolorization temperature is 23°C, stir for 1h, and filter with suction to obtain thiamine sulfate;

[0054] S2. Fully mix 75.66 g of thiamine sulfate and 8.22 g of nitric acid with a mass fraction of 65% according to a mass ratio of 9:1; add the nitric acid at one time, and control the temperature below 10°C. The stirring speed is 112r / min;

[0055] S3. Use a peristaltic pump to slowly add ammonia water. The speed of the peristaltic pump is 0.1-0.7 rpm. Add ammonia water with a mass fraction of 21.04% to the mixed solution of thiamine sulfate and nitric acid, and adjust the pH value of the mixed solution to about 7....

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Abstract

The invention discloses a preparation method of thiamine mononitrate. The preparation method comprises the steps that thiothiamine is oxidized by hydrogen peroxide to obtain thiamine mononitrate, thenthe thiamine mononitrate is converted into salt by using dilute nitric acid and neutralized by using ammonium hydroxide, and finally, cooling, crystallization, filtration and separation are carried out to obtain a thiamine mononitrate solid. The preparation method of the thiamine mononitrate has the advantages that the viewpoint of salt conversion by the ammonium nitrate is improved, the potential safety hazards caused by the use of a large number of the thiamine mononitrate solid during production are avoided, and the step of the preparation of the ammonium nitrate is reduced; on the premiseof not affecting the product quality and yield, the natural stacking density of thiamine mononitrate crystals is improved; the process steps are simple, the production cost is low, control is easy, the stability is good, the particle size is moderate, the degree of purification is high, and industrial large-scale production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, in particular to a preparation method of thiamine nitrate. Background technique [0002] Thiamine nitrate is a vitamin drug, which is often used in the preparation of food additives and multivitamin preparations, and is also used to treat beriberi caused by vitamin B1 deficiency. It also has an auxiliary therapeutic effect on neuritis and indigestion. At present, the quality of domestically produced thiamine nitrate has a certain gap in terms of purity and particle size compared with similar foreign products, and it is at a disadvantage in market competition. Therefore, narrowing the gap between domestic and foreign products, reducing costs and creating benefits is the top priority. [0003] In the past, thiamine nitrate was prepared by adding a barium salt, such as barium nitrate, to change barium nitrate into barium sulfate. However, this method of precipitation is time-consuming...

Claims

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Application Information

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IPC IPC(8): C07D415/00
Inventor 张国银林道兵王文王淑霞王志军王丽敏郑玲艳
Owner CHIFENG PHARMA CO LTD
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