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Method for recovering D-calcium pantothenate mother liquor

A technology of mother liquor recovery and calcium pantothenate, applied in chemical instruments and methods, calcium/strontium/barium compounds, calcium/strontium/barium sulfate, etc., can solve problems such as environmental pollution, waste of resources, loss of crystallization, etc. The effect of environmental pollution, avoidance of resource waste, and short response time

Active Publication Date: 2020-02-28
安徽泰格生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] According to relevant literature reports, the existing process of calcium pantothenate includes first splitting to obtain D-pantothenate lactone to directly obtain D-calcium pantothenate, and also obtaining DL-calcium pantothenate first and then inducing resolution to obtain D-calcium pantothenate, but due to the In the process of calcium production, calcium pantothenate is crystallized, and the crystallization will be lost. The mother liquor also contains a lot of calcium pantothenate, and there are a small amount of unreacted raw and auxiliary materials. If the mother liquor is thrown away, it will not only waste resources, but also cause environmental pollution. Pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Present embodiment provides a kind of D-calcium pantothenate mother liquor recovery method, concrete steps are:

[0025] (1) Get D-calcium pantothenate mother liquor 400g, reclaim methanol under vacuum, 50 ℃ condition to condenser without reflux;

[0026] (2) Add 400g of water to the product obtained after removing methanol in step (1), distill at atmospheric pressure to 100°C, add sulfuric acid dropwise to adjust the pH to 1, then keep stirring at 80°C for 1 hour, cool down to 30°C, add Sodium hydroxide adjusts pH to 5, filters, reclaims precipitated calcium sulfate and filtrate respectively;

[0027] (3) add ethyl acetate in step (2) gained filtrate, extract 3 times, share 400ml ethyl acetate, collect ethyl acetate phase and aqueous phase respectively, merge and concentrate ethyl acetate phase and obtain 71g specific optical rotation-43 ° D-pantolactone;

[0028] (4) Concentrate the aqueous phase obtained in step (3) to a water content of 31%, cool to 0° C. to cryst...

Embodiment 2

[0031] Present embodiment provides a kind of D-calcium pantothenate mother liquor recovery method, concrete steps are:

[0032] (1) Get D-calcium pantothenate mother liquor 400g, reclaim methanol under vacuum, 50 ℃ condition to condenser without reflux;

[0033] (2) Add 400g of water to the product obtained after removing methanol in step (1), distill at atmospheric pressure to 100°C, add sulfuric acid dropwise to adjust the pH to 1, then keep stirring at 80°C for 3 hours, then cool to 30°C, add Sodium hydroxide adjusts pH to 5, filters, reclaims precipitated calcium sulfate and filtrate respectively;

[0034] (3) add ethyl acetate in step (2) gained filtrate, extract 3 times, share 400ml ethyl acetate, collect ethyl acetate phase and aqueous phase respectively, merge and concentrate ethyl acetate phase and obtain 70g specific optical rotation-43.5 ° D-pantolactone;

[0035] (4) Concentrate the aqueous phase obtained in step (3) to a water content of 30%, cool to 0° C. to cr...

Embodiment 3

[0038] Present embodiment provides a kind of D-calcium pantothenate mother liquor recovery method, concrete steps are:

[0039] (1) Get D-calcium pantothenate mother liquor 400g, reclaim methanol under vacuum, 50 ℃ condition to condenser without reflux;

[0040] (2) Add 400g of water to the product obtained after removing methanol in step (1), distill at atmospheric pressure to 100°C, add sulfuric acid dropwise to adjust the pH to 1, then keep stirring at 80°C for 1 hour, cool down to 30°C, add Sodium hydroxide adjusts pH to 5, filters, reclaims precipitated calcium sulfate and filtrate respectively;

[0041] (3) add ethyl acetate in step (2) gained filtrate, extract 3 times, share 400ml ethyl acetate, collect ethyl acetate phase and aqueous phase respectively, merge and concentrate ethyl acetate phase and obtain 69g specific rotation-42 ° D-pantolactone;

[0042] (4) Concentrate the aqueous phase obtained in step (3) to a water content of 35%, cool to 10° C. to crystallize,...

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PUM

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Abstract

The invention relates to a recovery method for D-calcium pantothenate mother liquor. The recovery method comprises the following steps: subjecting D-calcium pantothenate mother liquor to recovery of methanol; heating a product obtained after recovery of methanol, adjusting a pH value to 1-3, carrying out sufficient stirring, then performing cooling to room temperature, adjusting a pH value to 4-6,carrying out filtering, and respectively recovering precipitated calcium sulfate and a filtrate; adding ethyl acetate into the obtained filtrate, carrying out sufficient extracting, respectively collecting an ethyl acetate phase and a water phase, and recovering D-pantoic acid lactone in the ethyl acetate phase; and concentrating, cooling and crystallizing the obtained water phase, carrying out filtering and respectively recovering crystallized beta-aminopropionic acid and a filtrate containing D-calcium pantothenate. According to the method provided by the invention, the residual target products and a small amount of unreacted raw materials and auxiliary materials in the D-calcium pantothenate mother liquor are efficiently and fully recovered according to a specific sequence, so resourcewaste and environmental pollution are avoided; and the method has the advantages of easy availability of raw materials, environment-friendly and safe conditions, short reaction time, recyclable solvents, simple steps, high purity of recovered products and the like.

Description

technical field [0001] The invention relates to the field of chemical production, in particular to a method for recovering D-calcium pantothenate mother liquor. Background technique [0002] Calcium pantothenate is mainly used in medicine, food and feed additives. It is a component of coenzyme A. It participates in the metabolism of carbohydrates, fats and proteins. It is an indispensable trace substance for humans and animals to maintain normal physiological functions. More than 70% is used as feed additive. In recent years, my country's feed industry has developed rapidly, and the demand for calcium D-pantothenate has increased accordingly. The feed industry alone has a demand of no less than 30,000 tons per year. Therefore, the development prospects are very broad, with good domestic and foreign market prospects and extremely high economic returns. [0003] According to relevant literature reports, the existing process of calcium pantothenate includes first splitting to...

Claims

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Application Information

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IPC IPC(8): C07C29/80C07C31/04C01F11/46C07D307/20C07C227/40C07C229/08C07C231/24C07C235/12
CPCC01F11/468C07C29/80C07C227/40C07C231/24C07D307/20C07C31/04C07C229/08C07C235/12
Inventor 周多祥汪洪湖李涛孟军陶勇
Owner 安徽泰格生物科技有限公司
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