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Method for separating L-phenylalanine from aspartame synthesis mother liquid

A technology for synthesizing phenylalanine and mother liquor, which is applied in the direction of organic chemical methods, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of large amount of extractant, high cost of liquid film, and high regeneration cost, and achieve process control. Convenience, simple operation, high porosity effect

Active Publication Date: 2017-05-17
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The organic solvent extraction method requires a large amount of extractant and high cost; activated carbon or resin adsorption can effectively separate L-phenylalanine, but there are limitations such as difficult elution or low yield; liquid membrane separation method can generate particles Larger, higher-purity L-phenylalanine, but the cost of liquid membrane is higher, which is limited to laboratory separation and purification; for D, L-phenylalanine mixture, use aminoacylase, etc. Amino acid is converted, and L-phenylalanine is separated by enzymatic resolution method. The use and regeneration cost of this method is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 500 mL of aspartame synthesis mother liquor aqueous solution with a total solute concentration of 10 mg / mL, carry out conventional antisolvent crystallization, filter and dry to obtain crude crystals of D,L-phenylalanine.

[0023] Dissolve D,L-phenylalanine crude crystals in water to prepare an aqueous solution with a concentration of 10 mg / mL; take an anion-exchange gel column with a column length of 15 cm and a diameter of 16 mm, at room temperature at a flow rate of 0.5–2 cm / mL Adsorption chromatography was carried out for 1 min to obtain a solution containing crude L-phenylalanine; at 45°C and a vacuum of 0.09 MPa, vacuum evaporation was carried out to remove the solvent to obtain a crude product containing L-phenylalanine;

[0024] The resulting crude product containing L-phenylalanine was configured as 40 mL of 30 mg / mL aqueous solution, subjected to freeze crystallization for 30 h, and conventionally dried to obtain 0.91 g of refined L-phenylalanine. The obta...

Embodiment 2

[0026] Take 800 mL of the aspartame synthesis mother liquor aqueous solution with a total solute concentration of 100 mg / mL for anti-solvent crystallization, filter and dry to obtain crude crystals of D,L-phenylalanine.

[0027] Dissolve D,L-phenylalanine crude crystals in water to prepare an aqueous solution with a concentration of 30 mg / mL; take an anion-exchange gel column with a column length of 15 cm and a diameter of 16 mm, at room temperature with a flow rate of 0.5-2 cm / mL min for adsorption chromatography to obtain a solution containing crude L-phenylalanine; evaporate under reduced pressure at 65°C and a vacuum of 0.09 MPa to remove the solvent to obtain crude L-phenylalanine.

[0028] The obtained L-phenylalanine crude product was configured as 180 mL of 50 mg / mL aqueous solution for cooling crystallization, frozen and crystallized at -5°C for 30 h, and conventionally dried to obtain 7.1 g of refined L-phenylalanine. The obtained L-phenylalanine was taken and prepar...

Embodiment 3

[0030] Take 800 mL of aspartame synthetic mother liquor aqueous solution with a total solute concentration of 100 mg / mL for antisolvent crystallization, filter and dry to obtain crude crystals.

[0031] The crude crystals were dissolved in water to prepare an aqueous solution with a concentration of 20 mg / mL; an anion-exchange gel column with a column length of 15 cm and a diameter of 16 mm was used for adsorption chromatography at room temperature at a flow rate of 0.5-2 cm / min to obtain The solution of the crude L-phenylalanine was evaporated under reduced pressure at 50° C. and a vacuum of 0.09 MPa to remove the solvent to obtain the crude L-phenylalanine.

[0032] The obtained L-phenylalanine crude product was configured as 180 mL of 40 mg / mL aqueous solution, subjected to freeze crystallization for 30 h, and conventionally dried to obtain 5.6 g of refined L-phenylalanine. The obtained L-phenylalanine was taken and prepared as an aqueous solution with a concentration of 5 ...

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Abstract

The invention discloses a method for separating L-phenylalanine from aspartame synthesis mother liquid. The method is characterized in that by combining crystallizing and cryogel adsorption chromatography techniques, the L-phenylalanine is extracted from the aspartame synthesis mother liquid containing aspartic acid and D,L-phenylalanine. The method comprises the following steps of performing anti-solvent crystallizing on a water solution of the aspartame synthesis mother liquid; performing chromatographic separation by a cryogel medium to remove impurities; then, freezing, crystallizing, refining, and drying, so as to obtain the L-phenylalanine. The separation method has the advantages that the technology process is simple, the process control is easy, the operation is convenient, the industrial amplification is easy, the purity of the obtained L-phenylalanine is high, the specific rotation is -32, and the industrial application prospect is good.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering and biological separation, and in particular relates to a method for separating L-phenylalanine from aspartame synthesis mother liquor by using crystallization and crystal gel adsorption chromatography technology. Background technique [0002] Phenylalanine has L-type and D-type, and the biologically active optical isomer L-phenylalanine is an essential amino acid for humans and animals. It is an aromatic amino acid. It is white crystal or crystalline powder solid at room temperature. It is commonly used As food additives, nutritional supplements and intermediates of some anticancer drugs, it is also an important precursor for the synthesis of many proteins and neurotransmitters. [0003] L-phenylalanine is also an important raw material for the production of the sweetener aspartame. In the process of producing aspartame with aspartic acid and phenylalanine as the main raw materials,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/36C07C227/40C07C227/42
CPCC07B2200/07C07C227/40C07C227/42C07C229/36
Inventor 祝铃钰韩建福章渊昶张颂红贠军贤
Owner ZHEJIANG UNIV OF TECH
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