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Method for concentrating, crystallizing and recovering vitamin C mother liquor

A recovery method, concentrated crystallization technology, applied in solution crystallization, chemical instruments and methods, sugar derivatives, etc., to achieve the effect of increasing production costs

Active Publication Date: 2014-07-16
NORTHEAST PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Method for concentrating, crystallizing and recovering vitamin C mother liquor
  • Method for concentrating, crystallizing and recovering vitamin C mother liquor

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Experimental program
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Embodiment 1

[0016] According to the different contents of 2-keto-L-gulonic acid and vitamin C in the vitamin C mother liquor, the present invention selects the type and particle size of the added crystal seed, and the sum of the quality of 2-keto-L-gulonic acid and vitamin C and the crystal seed The mass ratio of the seed amount was compared and analyzed in experiments, and the specific experimental conditions and experimental results are shown in Table 1 and Table 2.

[0017] Table 1 Comparative analysis experiments of various experimental conditions

[0018]

[0019] Table 2 Comparative analysis of each experimental condition Experiment 2

[0020]

[0021] The results show:

[0022] 1. When the content ratio of 2-keto-L-gulonic acid to vitamin C in the vitamin C mother liquor is less than or equal to 1.13, vitamin C crystals are added as seed crystals. The crystal size is 125 μm-180 μm, and the recovery rate is high.

[0023] 2. When the content ratio of 2-keto-L-gulonic acid t...

Embodiment 2

[0026] 250ml vitamin C mother liquor (the ratio of 2-keto-L-gulonic acid content to vitamin C content in the mother liquor is 1.13, vitamin C content is 123.1mg / ml, 2-keto-L-gulonic acid content is 139.0mg / ml) The flow is put into the rotary evaporator, the relative vacuum degree is 0.098MPa, the concentration temperature is 37.5°C, and when 195ml of condensed water is evaporated, add 3.7g of vitamin C crystals (+80 mesh to -100 mesh international standard sieve, the particle size of the seed crystal is between 150-180μm) as a seed crystal, continue to feed 250ml of vitamin C mother liquor, concentrate to the end, cool down to 0°C, filter with suction, and dry to obtain a dry product of vitamin C. Recover 55.6g of the obtained vitamin C once dry product, wherein the content of vitamin C is 47.23%, the content of 2-keto-L-gulonic acid is 48.82%, and the recovery rate of vitamin C and 2-keto-L-gulonic acid is 37.9%.

Embodiment 3

[0028] 250ml vitamin C mother liquor (the ratio of 2-keto-L-gulonic acid content to vitamin C content in the mother liquor is 1.13, vitamin C content is 123.1mg / ml, 2-keto-L-gulonic acid content is 139.0mg / ml) The flow was added to a rotary evaporator, the relative vacuum degree was 0.098MPa, the concentration temperature was 37.2°C, and when 180ml of condensed water was evaporated, 3.7g of 2-keto-L-gulonic acid crystals (+70 mesh to -100 mesh international standard sieve 150-212μm) as the seed crystal, continue to add 250ml vitamin C mother liquor, concentrate to the end, cool down to 0°C, filter and dry to obtain a dry product of vitamin C. Recover 54.4g of the obtained vitamin C once dry product, wherein the content of vitamin C is 46.07%, the content of 2-keto-L-gulonic acid is 52.83%, and the recovery rate of vitamin C and 2-keto-L-gulonic acid is 38.3%.

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Abstract

The invention relates to a method for concentrating, crystallizing and recovering vitamin C mother liquor in a concentration and crystallization technology of the vitamin C mother liquor. The method comprises the following steps: performing decompression, evaporation and concentration on the vitamin C mother liquor in an evaporator, wherein the concentration condition is characterized in that the relative vacuum degree is greater than or equal to 0.092MPa, when the content ratio of 2-keto-L-gulonic acid to vitamin C in the vitamin C mother liquor is less than or equal to 1.13, concentrating the vitamin C mother liquor to vitamin C under a quasi stabilization zone under the concentration condition, concentrating the vitamin C mother liquor to 2-keto-L-gulonic acid under a quasi stabilization zone under the concentration condition; when the content ratio of 2-keto-L-gulonic acid to vitamin C in the vitamin C mother liquor is less than or equal to 1.13, adding the vitamin C mother liquor in continuous flow, concentrating to a terminal point, filtering, and recovering to obtain the vitamin C crystals. The method solves the problems that the esterification conversion reaction of the 2-keto-L-gulonic acid on industrial production of vitamin C is stable, when the content of 2-keto-L-gulonic acid in the vitamin C mother liquor is high, recovery rate through concentration and crystallization of the vitamin C mother liquor is low, and the crystallization recovery rate of the vitamin C mother liquor is influenced, and the production cost is increased.

Description

technical field [0001] The invention relates to a method for recovering vitamin C mother liquor concentration and crystallization in the field of vitamin C mother liquor concentration and crystallization technology. Background technique [0002] L-Ascorbic acid, also known as vitamin C, has the function of maintaining the normal metabolism of the human body, has the ability to resist infection, and is an essential nutrient for humans. It has a wide range of uses and is used in food, feed and cosmetics. There are a wide range of applications. [0003] At present, in the industrial production of vitamin C, the important intermediate of vitamin C, 2-keto-L-gulonic acid crystals, is mainly obtained through two-step fermentation and crystallization purification, and the 2-keto-L-gulonic acid crystals and methanol undergo esterification conversion reaction To obtain vitamin C, the esterification conversion reaction is a reversible organic reaction, and the reaction is very unstab...

Claims

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Application Information

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IPC IPC(8): C07D307/62C07H7/027C07H1/06B01D9/02
CPCC07D307/62C07H1/06C07H7/027
Inventor 于霞李春杰牛宏伟宋宗宝王彦春刘中敢李秀媛
Owner NORTHEAST PHARMA GRP
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