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Crystalline powder of L-lysine L-glutamate

A technology of crystalline powder and glutamate, applied in the field of L-lysine L-glutamate crystalline powder and its preparation, can solve the problems of high product viscosity, solvent residue, serious product agglomeration, etc. Less water content, less methanol residue and better tapped density

Inactive Publication Date: 2017-11-07
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the report on the dissolution and crystallization of L-lysine L-glutamate, there is either oil precipitation, or the product has high viscosity during the crystallization process, severe agglomeration, or easy to have solvent residues, which will seriously affect the product. the quality of
[0007] For example, in the patent CN102557974A, ethanol is used as anti-solvent for crystallization. By repeating the process, we found that the product agglomerates seriously during this process, and oil separation is easy to occur, resulting in subsequent separation difficulties and low product purity, which seriously affects the product. the quality of
[0008] For another example, in the patent US4415590, methanol is used as an antisolvent to carry out crystallization of L-lysine L-glutamate. Although the product particle size and stability are better, under the technique of using methanol as an antisolvent, the resulting L- In lysine L-glutamate crystalline powder, there will inevitably be the problem of methanol residue, and the residue is still high. In some products, the mass fraction of methanol residue is even greater than 3.2%, or even greater than 5%. Even more likely to 9%

Method used

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  • Crystalline powder of L-lysine L-glutamate
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  • Crystalline powder of L-lysine L-glutamate

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Add 10g of L-lysine L-glutamate into 80g of pure water, fully stir and dissolve to form an aqueous solution of L-lysine L-glutamate, then transfer it to a 500mL crystallization tank, and control the temperature at 10°C , and then add 420mL of anhydrous methanol to it as an anti-solvent for crystallization. After the white crystal substance appears, put it in the tank and carry out solid-liquid separation by suction filtration. Wash the crystal with 40mL of 90vol.% ethanol, and then in 4 ° C , put the separated crystals into 90vol.% ethanol for stirring conversion, the mass ratio of crystals and ethanol is 0.1:10, after stirring for 10h, the crystals are separated from solid and liquid by suction filtration, and then drummed at 30°C Air-dried for 10 hours, L-lysine L-glutamate crystalline powder was obtained, wherein the product purity was 99.1%, and the yield was 78.8%.

Embodiment 2

[0045] Add 30g of L-lysine L-glutamate into 100g of pure water, fully stir and dissolve to form an aqueous solution of L-lysine L-glutamate, then transfer it to a 500mL crystallization tank, and control the temperature at 15°C , and then add 400mL of 90vol.% methanol as an anti-solvent to crystallize. After the white crystal material appears, put it in the tank and carry out solid-liquid separation by suction filtration. Wash the crystal with 60mL of 95vol.% ethanol, and then in 25 ℃ , the separated crystals were put into 95vol.% ethanol and stirred for transformation. The mass ratio of crystals and ethanol was 1:10. After stirring for 30 hours, the crystals were subjected to solid-liquid separation by means of suction filtration, and then the crystals were separated at 70°C Blow drying for 12 hours to obtain L-lysine L-glutamate crystalline powder, wherein the product purity is 99.2%, and the yield is 81.6%.

Embodiment 3

[0047] Add 50g of L-lysine L-glutamate into 100g of pure water, fully stir and dissolve to form an aqueous solution of L-lysine L-glutamate, then transfer it to a 500mL crystallization tank, and control the temperature at 20°C , then add 300mL of 80vol.% anhydrous methanol to it as anti-solvent to carry out crystallization, after the white crystal substance appears, go down the tank, carry out solid-liquid separation with the mode of suction filtration, wash crystal with 80mL of 98vol.% ethanol, then in At 35°C, put the separated crystals into 98vol.% ethanol for stirring transformation, the mass ratio of the crystals to ethanol is 1.5:10, after stirring for 60 hours, the crystals are separated from the solid and liquid by suction filtration, and then separated at 45 Blow drying at ℃ for 15 hours to obtain L-lysine L-glutamate crystalline powder, wherein the product purity is 99.5%, and the yield is 88.9%.

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Abstract

The invention discloses crystalline powder of L-lysine L-glutamate and a preparation method of the crystalline powder of the L-lysine L-glutamate. The methanol content of the crystalline powder is less than 0.5wt%, the bulk density of the crystalline powder is more than 0.4g / ml, and the tapped density of the crystalline powder is more than 0.5g / ml. According to the preparation method, crystal obtained by crystallizing L-lysine L-glutamate methanol water is put into ethanol for converting, so that the problem that methanol is left over in a dilution crystallization process is effectively solved; compared with the existing products on the market, the prepared crystalline powder not only has good graininess, flowability and stability, but is also very low in amount of residual methanol.

Description

technical field [0001] The invention belongs to the technical field of crystallization, and in particular relates to a crystal powder of L-lysine L-glutamate and a preparation method thereof. Background technique [0002] L-lysine L-glutamate, English name L-Lysine L-glutamate, molecular formula C 11 h 23 N 3 o 6 , relative molecular mass 293.32. It is formed by complex crystallization of L-lysine and L-glutamic acid according to the mass ratio of 1:1. Its structure is as follows: [0003] [0004] L-Lysine L-Glutamate is white or white crystalline powder, odorless and has a unique taste. The melting point is 197°C. It is easily soluble in water, but hardly soluble in ethanol. Its aqueous solution is clear and colorless, with a pH value of 6.0-7.5. [0005] As an amino acid compound salt, L-lysine L-glutamate is different from amino acid derivatives. It has the biological effects of two amino acids at the same time, and even enhances the biological effects of each...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/42C07C229/26C07C229/24A61K31/198A61P3/14A61P7/00A61P3/00
CPCC07C227/42C07C229/24C07C229/26
Inventor 应汉杰黎青青杨朋朋王森吴菁岚朱晨杰柳东陈勇欧阳平凯
Owner NANJING UNIV OF TECH
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