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Crystallization method of thiamine mononitrate

A technology of thiamine nitrate and thiamine sulfate, applied in the direction of organic chemistry, can solve the problems of poor crystal fluidity, small bulk density, and low market competitiveness

Inactive Publication Date: 2017-04-26
HUAZHONG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Regarding the crystallization of vitamin B1 nitrate or hydrochloride, there have been studies abroad as early as the 1960s and 1970s. In China, the "Research on the Morphological Construction and Precipitation Process of Thiamin Nitrate Crystal" published by Tianjin University at the beginning of this century has already It shows that our country attaches great importance to the appearance quality of crystals, but there are differences in the crystallization of finished products produced by different processes, all of which are conventional needle-shaped crystals, with poor crystal fluidity, low bulk density, and low market competitiveness.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0024] The first step of mixing: take 380kg (pure amount) of thiothiamine, a synthetic intermediate of vitamin B1, and obtain about 3500kg of thiamine sulfate solution through oxidation in a temporary storage tank, put 90kg of ammonium nitrate into a heating tank containing 80kg of purified water In the pot, heat the temperature above 50°C to completely dissolve the ammonium nitrate, then lower the temperature properly, add the ammonium nitrate solution to the thiamine sulfate solution in the temporary storage tank and mix well, and the mixing temperature is controlled at 20-25°C. After the mixing is completed, keep the temperature of the above mixed solution at 20-25°C and store it in a turnover container for future use.

[0025] The second part of mixing: Add 100kg of purified water with a temperature of 20-25°C into the refining reactor to ensure that the stirring of the refining tank can touch and stir the purified water, turn on the stirring, and control the speed at 20r / m...

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Abstract

The invention relates to an improvement in a crystallization method of thiamine mononitrate. A traditional method comprises the following steps: mixing a crude nitric acid B1, namely, thiamine sulfate solution with an ammonium nitrate aqueous solution in a matched amount, then adding 20%-25% ammonia dropwise until the PH of the mixture reaches 7.2 to 7.5, performing cooling, and separating the solid-liquid mixture to obtain crystals of nitric acid B1. The invention relates to the improvement in the crystallization method of thiamine mononitrate, the mixing sequence and the proportion of three solutions (the thiamine sulfate solution, the ammonium nitrate solution and ammonia) are adjusted, the three solutions are mixed simultaneously, and accordingly, the crystal form of thiamine mononitrate is changed with adoption of the crystallization method. The crystallization method of thiamine mononitrate is improved to replace a traditional crystallization process, the crystal form of a product is changed from the original needle shape into a rod or ball shape, the product particles become larger, the bulk density increases, the packaging volume decreases, and great benefit is provided for reducing the transportation cost and the operating cost and improving the market competitiveness of the product.

Description

technical field [0001] The invention relates to a crystallization method of a pharmaceutical compound, in particular to a crystallization method of vitamin B1 thiamine nitrate. Background technique [0002] Vitamin B1 is a kind of vitamin auxiliary drug, which can maintain normal glucose metabolism and nervous and digestive system functions. For the prevention and treatment of vitamin B deficiency 1 It is also used as an adjuvant treatment for neuritis and indigestion caused by beriberi. [0003] Vitamin B1 can be divided into two forms of hydrochloride and nitrate, both of which can be transformed into each other, and can be used as feed additives, food additives and pharmaceutical preparations. [0004] Vitamin B1, also known as thiamine, is a white crystal or crystalline powder. Its hydrochloride is easily soluble in water, slightly soluble in methanol and ethanol, insoluble in ether, and has good stability in acidic environment; its nitrate is slightly soluble In wate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D415/00
CPCC07D415/00
Inventor 王定军刘玉亭付林李桂莲魏旭力
Owner HUAZHONG PHARMA
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