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A kind of preparation method of thiamine nitrate massive crystal product

A technology for thiamine nitrate and crystals, which is applied in the field of preparation of thiamine nitrate bulk crystals, can solve problems such as affecting the market competitiveness of products, restricting product processing procedures, uneven particle size distribution, etc., achieving easy control, good fluidity, good stability

Active Publication Date: 2018-12-28
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many manufacturers of thiamine nitrate in China, and the crystal habit of the thiamine nitrate produced is rod-shaped (aspect ratio ≥ 5:1), and the particle size distribution is uneven, resulting in poor product fluidity and low bulk density (compactness ≤0.65g / mL) and other issues, which will seriously restrict the subsequent processing of the product and affect the market competitiveness of the product

Method used

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  • A kind of preparation method of thiamine nitrate massive crystal product
  • A kind of preparation method of thiamine nitrate massive crystal product
  • A kind of preparation method of thiamine nitrate massive crystal product

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Use dilute nitric acid solution to adjust 75mL of distilled water to pH = 3.5, add 100g of thiothiamine solids to the distilled water in portions, and stir at a speed of 200r / min. , drop 30% hydrogen peroxide, the total mass of hydrogen peroxide added is 115g, after the reaction is complete, the reaction solution is decolorized with 10g of activated carbon for 1 hour, filtered and set aside.

[0036](2) At 30°C, add 76.5g of ammonium nitrate solution with a mass fraction of 55% to the solution obtained from the above oxidation reaction, and add 0.1g of sodium octadecyl sulfate, stir and mix, and use a mass fraction of 10% ammonia water Adjust the pH. When the pH is adjusted to 3.9, add 1.5 g of thiamine nitrate seed crystals, grow the crystals for 0.5 h, then continue to adjust the pH to pH = 6.8, control the dripping time of ammonia water to 80 min, and then lower the temperature to 5°C.

[0037] (3) Filtrate, wash with 40 mL of absolute ethanol, and dry at 40° C. ...

Embodiment 2

[0040] (1) Use dilute sulfuric acid solution to adjust 75mL of distilled water to pH = 3, add 100g of thiothiamine solids to the distilled water in portions, and stir at a speed of 800r / min. , 20% hydrogen peroxide was added dropwise, and the total mass of the added hydrogen peroxide was 180 g. After the reaction was complete, the reaction solution was decolorized with 10 g of activated carbon for 1 hour, filtered and set aside.

[0041] (2) at 30 DEG C, in the solution that above-mentioned oxidation reaction obtains, add 120g massfraction to be the ammonium nitrate solution of 40%, and add 1.0g decyl sodium sulfate, stir and mix, adjust pH with the ammoniacal liquor of massfraction 25%, When the pH value is 4.0, add 2 g of thiamine nitrate seed crystals, grow the crystals for 1 h, then continue to adjust the pH to pH=7, control the dripping time of ammonia water to 100 min, and then lower the temperature to 5°C.

[0042] (3) Filtrate, wash with 40 mL of absolute ethanol, and ...

Embodiment 3

[0045] (1) Use dilute nitric acid solution to adjust 75mL of distilled water to pH = 4, add 100g of thiothiamine solids to the distilled water in portions, and stir at a speed of 400r / min. , drop 30% hydrogen peroxide, the total mass of hydrogen peroxide added is 115g, after the reaction is complete, the reaction solution is decolorized with 10g of activated carbon for 1 hour, filtered and set aside.

[0046] (2) At 20°C, add 68.5g of ammonium nitrate solution with a mass fraction of 60% to the solution obtained from the above oxidation reaction, and add 0.2g of sodium lauryl sulfate, stir and mix, and use 10% of the mass fraction of ammonia water Adjust the pH. When the pH is adjusted to 3.9, add 1.5 g of thiamine nitrate seed crystals, grow the crystals for 2 hours, then continue to adjust the pH to pH=6.8, control the dripping time of ammonia water to 90 minutes, and then lower the temperature to 5°C.

[0047] (3) Filtrate, wash with 40 mL of absolute ethanol, and dry at 40...

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Abstract

The present invention discloses a preparation method for a bulk crystal product of thiamine nitrate. The method comprises: adding solid thiothiamine into acidic distilled water with pH=2-6, adding hydrogen peroxide dropwise thereto based on mass fraction with stirring, carrying out reaction, oxidation and decolorization to obtain a thiamine sulfate solution; adding a solution of 40-60 wt% ammonium nitrate to the obtained solution from the above oxidation reaction, and an additive is added with stirring and mixing; When ammonia liquor is used to adjust pH to 3.9-4.3, adding a thiamine nitrate seed and growning for 0.5-2 h, continuing to adjust pH to 6.80-7.05, followed by lowering a temperature to 5 DEG C at a rate of 0.5 DEG C / min; and filtering, washing, and driying to obtain a thiamine nitrate crystal. The product is a bulk crystal with an aspect ratio of 1:1 to 4:1, a bulk density of 0.80-0.93 g / mL, and an angle of repose of 25 DEC to 38 DEC, and has better fluidity, and crystal properties are significantly improved. The preparation process is simple, and is easy for industrialization.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical crystallization, and in particular relates to a preparation method of thiamine nitrate block crystals. Background technique [0002] Thiamine nitrate, also known as thiamine nitrate, English name thiamine nitrate, molecular formula C 12 h 17 N 5 o 4 S, molecular weight 327.36, CAS number 532-43-4, chemical name 3-[(4-amino-2-methyl-5-pyrimidinyl)methyl]-5-(2-hydroxyethyl)-4- Methylthiazolium nitrate, its molecular structure is shown below. [0003] [0004] Thiamin Nitrate as Vitamin B 1 of nitrates, vitamin B 1 It is a compound composed of a pyrimidine ring and a thiazole ring. Because the molecule contains sulfur and amine, it is also named thiamine. Vitamin B 1 It naturally exists in rice bran, bran, lean meat, peanuts and other foods. The pure product is usually prepared by chemical synthesis. It is an essential nutrient for humans and animals. It lacks vitamin B 1 prone to ...

Claims

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Application Information

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IPC IPC(8): C07D417/06
CPCC07B2200/13C07D417/06
Inventor 龚俊波王海生韩丹丹李新发李涛王静康尹秋响侯宝红李晓娜于博
Owner TIANJIN UNIV
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