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Process method for crystallization purification of proline

A process method, proline technology, applied in the direction of organic chemistry, can solve the problems of unfavorable safety production, poor fluidity, high cost, etc., and achieve the effect of beautiful finished products, high safety, and high environmental protection

Active Publication Date: 2015-05-13
STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the crystals obtained by this process are needle-like fine crystals or white powder, which have poor fluidity and are easy to absorb moisture. Moreover, a large amount of ethanol is needed in the crystallization process, which is costly and is not conducive to safe production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Dissolve 260g of crude proline in 100ml of deionized water, heat with stirring at 80°C, and keep the temperature in a water bath for 30 minutes. After the proline is fully dissolved, add 8g of activated carbon for decolorization, filter, and cool the decolorization solution to 65°C under vacuum. Concentrate, stop concentrating when crystals precipitate out. Pour the concentrated solution into a crystallization tank, stir the solution at a speed of 250rpm, and keep it at a constant temperature for 30 minutes to obtain a crystallization solution; adjust the rotation speed to 350rpm, and when the temperature of the crystallization solution drops to 60°C, cool down at a rate of 5°C / h. After the temperature drops to 40°C, cool down to 10°C at a rate of 10°C / h; keep at this temperature for 30 minutes, vacuum filter the crystallization solution, and dry the wet product in a vacuum oven at 45°C for 3 hours to obtain dry proline Crystal 121.3g, the yield of the obtained proline ...

Embodiment 2

[0014] Dissolve 700g of crude proline in 250ml of deionized water, heat with stirring at 78°C, and keep the temperature in a water bath for 30 minutes. After the proline is fully dissolved, add 25g of activated carbon for decolorization, filter, and cool the decolorization liquid to 65°C after fine filtration. Concentrate, stop concentrating when crystals precipitate out. The concentrated solution was poured into a crystallization tank, the solution was stirred at a speed of 300 rpm, and kept at a constant temperature for 30 minutes to obtain a crystallization solution. Adjust the rotation speed to 400rpm. When the temperature of the crystallization solution drops to 60°C, cool down at a rate of 4°C / h. When the temperature drops to 45°C, cool down to 10°C at a rate of 8°C / h; keep at this temperature for 30 minutes , the crystallization solution was vacuum filtered, and the wet product was baked in a vacuum oven at 45°C for 3 hours to obtain 336.9 g of dry proline crystals, and...

Embodiment 3

[0016] Dissolve 350g of crude proline in 140ml of deionized water, heat with stirring at 75°C, and keep the temperature in a water bath for 30 minutes. After the proline is fully dissolved, add 10g of activated carbon for decolorization, filter, and cool the decolorization liquid to 63°C after fine filtration. Concentrate, and stop concentrating when crystals are precipitated; pour the concentrated solution into a crystallization tank, stir the solution at a speed of 280 rpm, and keep at constant temperature for 30 minutes to obtain a crystallization solution. Adjust the rotation speed to 380rpm. When the temperature of the crystallization solution drops to 60°C, cool down at a rate of 3°C / h; when the temperature drops to 45°C, cool down to 10°C at a rate of 10°C / h; keep at this temperature for 30 minutes , the crystallization solution was vacuum filtered, and the wet product was baked in a vacuum oven at 45°C for 3 hours to obtain 164.8 g of dry proline crystals, and the yield...

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PUM

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Abstract

The invention belongs to the fields of medical industry and food and particularly discloses a process method for crystallization purification of proline. The method sequentially comprises the following steps of dissolving a proline crude product to obtain a proline solution, carrying out decolorizing filtration on the proline solution to obtain a secondary refined filtrate, concentrating the secondary refined filtrate to obtain a concentrated solution of the proline, carrying out primary crystallization on the concentrated solution of the proline to obtain a crystallization solution, carrying out cooling crystallization on the crystalline liquid of the proline to obtain a cooling crystallization solution, finally filtering and drying the cooling crystallization solution to obtain a proline finished product. By adopting the way of water crystallization, no organic solvent is added in the method, so that the method is high in safety and good in environment protection; and compared with existing crystallization technologies, the method disclosed by the invention has the advantages of simplicity in operation, good repeatability, attractive finished products and high crystallization yield.

Description

technical field [0001] The invention belongs to the fields of pharmaceutical industry and food, and in particular relates to a process for proline crystallization and purification. Background technique [0002] L-proline is a component of various proteins such as gelatin, gluten (gliadin), zein, herring protein, salmon protein, casein, etc. It is a non-essential amino acid and passes through the grain Amino acids are metabolized. L-proline is one of the important amino acids for the synthesis of human protein, an important raw material for amino acid infusion, and the main intermediate for the synthesis of first-line antihypertensive drugs such as captopril and enalapril. It has been widely used in food and pharmaceutical industry. [0003] At present, there are three ways to prepare L-proline: one is the hydrolysis extraction method, and the raw materials used include horse-faced fish, gelatin, chicken feathers, etc.; the other is the fermentation method. Japan has achiev...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D207/16
Inventor 朱义福刘玉光李红徐珍珍吴平刚江燕斌
Owner STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG
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