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Preparation method for crude proline product

A technology for proline and crude products is applied in the field of preparation of crude proline products, and can solve the problems of low solvent boiling point, low efficiency, easy moisture absorption and the like, and achieve the effects of good crystal form and high purity

Inactive Publication Date: 2018-10-16
WUXI JINGHAI AMINO ACID
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Existing purification methods mainly include ion exchange resin method, anhydrous ethanol recrystallization method, ethanol-ether method, water-ethanol-acetone method, wherein, ion exchange resin method has low yield and low efficiency, and is not suitable for application and production; The water-ethanol recrystallization method cannot remove inorganic salts, and the operation process is easy to absorb moisture, and absolute ethanol is expensive and difficult to recycle; both the ethanol-ether method and the water-ethanol-acetone method have the disadvantages of low solvent boiling point, flammability and difficulty in recycling

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Specific steps are as follows:

[0038] (1) Take 10L of proline fermentation broth, pass through 2L of regenerated 732 resin, and perform adsorption. Determine whether the adsorption is over by measuring whether the adsorption discharge liquid leaks out amino acids. The adsorption rate is 20mL / min, and finally a volume of 5L is obtained. For the adsorption resin, wash away unadsorbed amino acids and some impurities with 6L of water, and elute the adsorption resin with 4% sodium hydroxide to obtain liquid A;

[0039] (2) Put the liquid A in (1) into a decolorization tank for decolorization, the decolorization temperature is 60°C, the decolorization time is 30min, the amount of activated carbon added is 5‰ of the quality of liquid A, the stirring speed is 200r / min, and the activated carbon is removed by filtration. Decolorization was repeated twice to obtain a decolorization solution;

[0040] (3) passing the decolorizing solution in (2) successively through 301 anion re...

Embodiment 2

[0047] Specific steps are as follows:

[0048] (1) Take 10L of proline fermentation broth, pass through 2L of regenerated 732 resin, and perform adsorption. Determine whether the adsorption is over by measuring whether the adsorption discharge liquid has amino acids leaking out. The adsorption rate is 15mL / min, and finally a volume of 5L is obtained. For the adsorption resin, wash away unadsorbed amino acids and some impurities with 6L of water, and elute the adsorption resin with 4% sodium hydroxide to obtain liquid A;

[0049] (2) Put the liquid A in (1) into a decolorization tank for decolorization, the decolorization temperature is 55°C, the decolorization time is 1h, the amount of activated carbon added is 5‰ of the quality of liquid A, the stirring speed is 180r / min, and the activated carbon is removed by filtration. Decolorization was repeated twice to obtain a decolorization solution;

[0050] (3) passing the decolorizing solution in (2) successively through 301 anion...

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Abstract

The invention discloses a preparation method for a crude proline product, and belongs to the technical field of separation and extraction. The method comprises the following steps that proline fermentation liquor is firstly adsorbed by strong acid cation resin and then is sequentially filtered through weak alkaline anion resin and weak acid cation resin so as to obtain the proline crude product. The crude proline product prepared by using the method is proline monohydrate and has the advantages of being good in crystal form, high in purity (the purity is greater than 99%, and the light transmittance is greater than 99%) and capable of controlling the specific rotation to be within -84.5 degrees to -86 degrees.

Description

technical field [0001] The invention relates to a method for preparing crude proline, belonging to the technical field of separation and extraction. Background technique [0002] L-proline (referred to as proline) is one of the eighteen kinds of amino acids that the human body synthesizes protein. It has certain physiological activities and is widely used in medicine, agriculture, chemical industry and food, especially in medicine. Intermediates for the synthesis of new drugs. [0003] At present, there are three main methods for the production of L-proline: protein hydrolysis, synthesis and microbial fermentation. However, these three methods will produce pigments, sugars, other amino acids, organic acids and inorganic salts, etc. Impurities. Therefore, in order to obtain high-purity proline, proline must be extracted, separated and purified. [0004] Existing purification methods mainly include ion exchange resin method, anhydrous ethanol recrystallization method, ethan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/16
CPCC07D207/16
Inventor 宁健飞蔡立明陈晓双
Owner WUXI JINGHAI AMINO ACID
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