Crystallization method integrating anti-solvent crystallization, vacuum evaporation and cooling or anti-solvent crystallization

A vacuum evaporation and anti-solvent technology, which is applied in the anti-solvent water-soluble amino acid crystallization system, integrated anti-solvent-vacuum evaporation-cooling or anti-solvent crystallization field, can solve the problem of small particles with many crystals, crystallized products with large particle size, and particle size Uneven distribution and other problems, to improve product purity and crystallization process yield, increase particle size, and achieve the effect of particle size

Active Publication Date: 2015-11-11
肇东星湖生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at the problem that the existing anti-solvent crystallization technology has many small particle crystals and uneven particle size distribution, and provides an integrated anti-solvent-vacuum evaporation-cooling or anti-solvent system with simple operation, high purity and high yield. Crystallization method, the obtained crystallized product has large particle size and narrow distribution

Method used

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  • Crystallization method integrating anti-solvent crystallization, vacuum evaporation and cooling or anti-solvent crystallization
  • Crystallization method integrating anti-solvent crystallization, vacuum evaporation and cooling or anti-solvent crystallization
  • Crystallization method integrating anti-solvent crystallization, vacuum evaporation and cooling or anti-solvent crystallization

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Embodiment 1

[0034] Weigh 20 g of glycine and measure 100 mL of water in a graduated cylinder. After the two are fully mixed, they are added to the crystallization kettle. The water bath is heated to 60° C. and stirred at a stirring speed of 300 r / min to fully dissolve the glycine. Add 300 mL of anti-solvent absolute ethanol at an addition rate of 3 mL / min, and crystals will precipitate out in the solution. Stir fully for 10 minutes to allow the crystals to grow fully. Reduce the pressure of the system to 45-55kPa, the volume of the volatile liquid is 30mL, and fully stir for 5min to dissolve the small crystal particles. Then, cooling crystallization (ie, cooling to 50°C) or anti-solvent crystallization (ie, continuing to add 170 mL of anti-solvent absolute ethanol at a rate of 3 mL / min) was used to promote crystal growth. Then reduce the pressure of the system to 35-45kPa, the volume of the volatile liquid is 10mL, and fully stir for 5min to fully dissolve the small crystal particles. Gly...

Embodiment 2

[0037] Weigh 20g of 5'sodium inosinate (IMP), measure 200mL of water in a graduated cylinder, mix the two thoroughly and add to the crystallization kettle, heat the water bath to 60°C, and stir at a stirring speed of 300r / min to fully dissolve IMP. Add 300 mL of anti-solvent absolute ethanol at an addition rate of 3 mL / min, and crystals will precipitate out in the solution. Stir fully for 10 minutes to allow the crystals to grow fully. Reduce the pressure of the system to 40-50kPa, the volume of the volatile liquid is 30mL, and fully stir for 5min to fully dissolve the small crystal particles. Cool down to 50°C, reduce the system pressure to 30-40kPa, and the volume of the volatile liquid is 10mL. Stir fully for 5 minutes to dissolve the small crystal particles. The IMP crystals were obtained by suction filtration under reduced pressure in a Buchner funnel, washed with 30 mL of absolute ethanol, and dried at an absolute pressure of 40 kPa and a temperature of 60° C. for 24 hour...

Embodiment 3

[0040] Weigh 20g of 5'-taste nucleotide disodium (I+G), measure 200mL of water, mix the two thoroughly, add them to the crystallization kettle, heat the water bath to 60°C, and stir at a stirring speed of 300r / min to make I +G is fully dissolved. Add 300 mL of anti-solvent absolute ethanol at an addition rate of 3 mL / min, and crystals will precipitate out in the solution. Stir fully for 10 minutes to allow the crystals to grow fully. Reduce the pressure of the system to 40-50kPa, the volume of the volatile liquid is 30mL, and fully stir for 5min to fully dissolve the small crystal particles. Cool down to 50°C, reduce the system pressure to 30-40kPa, and the volume of the volatile liquid is 10mL. Stir fully for 5 minutes to dissolve the small crystal particles. I+G crystals were obtained by vacuum filtration in a Buchner funnel, washed with 30 mL of absolute ethanol, and dried at an absolute pressure of 40 kPa and a temperature of 60° C. for 24 hours to obtain I+G crystal produ...

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Abstract

The invention provides a crystallization method integrating anti-solvent crystallization, vacuum evaporation and cooling or anti-solvent crystallization. The method comprises the following steps: (1) preliminary anti-solvent crystallization: placing a to-be-crystallized amino acid material into a crystallizer, adding solvent water and allowing the material to be fully dissolved, carrying out heating to 30 to 80 DEG C, adding an anti-solvent into the crystallizer, carrying out full stirring, and allowing a part of the solute in the solution to be crystallized and separated out so as to obtain a to-be-crystallized material; (2) vacuum evaporation and cooling or anti-solvent crystallization: continuing stirring, subjecting an obtained solid-liquid system to evaporation under an absolute pressure of 20 to 60 kPa, cooling the obtained solid-liquid system or adding the same anti-solvent as in the step 1 so as to promote crystals to continue to grow, and repeating the step 2 for 1 to 3 times; and (3), filtering and drying: carrying out filtering, washing and drying so as to prepare a crystallization product. The method provided by the invention has the advantages of convenient and fast operation, high yield and easy realization of industrial scale production, and can obtain the crystallization product with narrow particle-size distribution and a large particle size.

Description

Technical field [0001] The invention relates to an anti-solvent crystallization method, in particular to an integrated anti-solvent-vacuum evaporation-cooling or anti-solvent crystallization method. By regulating the crystal grain size in the anti-solvent crystallization, the preparation has a narrow particle size distribution and a large particle size. The crystal products are especially suitable for water-soluble amino acid crystallization systems with anti-solvents whose normal boiling point is lower than water. Background technique [0002] High-purity amino acids are important synthetic raw materials for a variety of active biological and pharmaceutical components. Crystallization is an effective method to obtain high-purity amino acid solid products, and the crystal size, distribution and crystal form have an extremely important influence on the quality of crystal products. For this reason, the preparation of amino acid crystals with large particle size and narrow distribu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D9/00C07H19/20C07H1/06C07C229/08C07C227/42
Inventor 江燕斌魏卓关国强
Owner 肇东星湖生物科技有限公司
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