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Method for separating alpha-ketoglutaric acid from conversion solution

A technology of ketoglutaric acid and ketoglutarate, which is applied in the field of preparation of α-ketoglutaric acid, can solve the problems that materials cannot be recycled multiple times, separation and purification are difficult, and there are many by-products of fermentation, etc., to achieve Good crystal form, avoid a large amount of distilled water, and high economic benefits

Active Publication Date: 2015-04-22
JING JING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the disadvantage of the fermentation method is that there are many fermentation by-products, the subsequent separation and purification work is difficult, the yield is low, and the purification cost is too high
Although the enzymatic conversion method has fewer by-products than the fermentation method, it also has the problems of difficulty in subsequent separation and purification, low yield and high purification cost
[0004] At present, the separation and purification methods of α-ketoglutaric acid in the conversion liquid are mainly as follows: firstly, the conversion liquid is pretreated, and the conversion liquid is added with aluminum sulfate, polyacrylamide, chitosan or other inorganic aluminum salts, iron Salt, polymer flocculant, etc., and then filtered; the filtered conversion solution is then absorbed and eluted by cationic resin and anionic resin, and the eluent is mostly sulfuric acid or ammonia water, which introduces other impurities. It affects subsequent purification, resulting in poor product quality and low yield, and the crystallized product is yellow-white or yellow powder; and the traditional process often crystallizes the unqualified crude product first, and then performs secondary crystallization to make the product meet the qualified standard, and the cost of secondary crystallization is high. The process is complicated, and because the solvent is water, the evaporation temperature is high, the energy waste is serious, and the material cannot be recycled multiple times

Method used

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  • Method for separating alpha-ketoglutaric acid from conversion solution
  • Method for separating alpha-ketoglutaric acid from conversion solution
  • Method for separating alpha-ketoglutaric acid from conversion solution

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) Take 5L of conversion solution containing 8% ketoglutaric acid and 5kg, filter it through a ceramic filter membrane with a membrane pore size of 0.05μm, control the pressure at 6.5-7.5Mpa, and the temperature at 20-30°C, collect Permeate;

[0027] (2) Filtrate the Tao filter permeate through a polyvinylidene fluoride ultrafiltration membrane with a molecular weight cut-off greater than 3000. The operating pressure is 7.5-8.5Mpa and the operating temperature is 20-30°C, and the ultrafiltration permeate is collected;

[0028] (3) Pass the ultrafiltration permeate through the composite membrane of cellulose acetate and polyamide, concentrate and filter by reverse osmosis, the operating pressure is 10-12Mpa, the operating temperature is 20-30°C, collect and extract 1.7L of concentrated solution, and detect its Light transmission is 96.3%;

[0029] (4) Heat the extracted concentrated solution to 33°C to 37°C, slowly add 132g of calcium chloride to the concentrated solut...

Embodiment 2

[0037] (1) Take 8kg of 8L conversion solution containing 11% ketoglutaric acid, filter through a ceramic filter membrane with a membrane pore size of 0.01 μm, control the pressure at 8.5-9.3Mpa, and the temperature at 30-35°C, collect Permeate;

[0038](2) Filter the Tao filter permeate through a polycarbonate ultrafiltration membrane with a molecular weight cut-off greater than 3000. The operating pressure is 8.5-9.3Mpa and the operating temperature is 30-35°C, and the ultrafiltration permeate is collected;

[0039] (3) Pass the ultrafiltration permeate through the polyamide reverse osmosis membrane, reverse osmosis concentration and filtration, the operating pressure is 14-15Mpa, the operating temperature is 30-35°C, collect and extract the concentrated solution of 2.8L, and the light transmission is 97 %;

[0040] (4) Raise the temperature of the extracted concentrated solution to 35°C-40°C, add 300g of calcium chloride to the concentrated solution with stirring, the addit...

Embodiment 3

[0048] (1) Take 3kg of 3L conversion solution containing 9% ketoglutaric acid, filter through a ceramic filter membrane with a membrane pore size of 0.10μm, control the pressure at 5.5-6.5Mpa, and the temperature at 10-20°C, collect Permeate;

[0049] (2) Filter the Tao filter permeate through a polysulfoneamide ultrafiltration membrane with a molecular weight cut-off greater than 3000, operate at a pressure of 5.5-6.5Mpa, and operate at a temperature of 10-20°C to collect the ultrafiltration permeate;

[0050] (3) Pass the ultrafiltration permeate through the cellulose acetate reverse osmosis membrane, reverse osmosis concentration and filtration, the operating pressure is 12-14Mpa, the operating temperature is 10-20°C, collect and extract the concentrated solution of 0.95L, and detect its light transmission as 97.5%;

[0051] (4) Heat the extracted concentrated solution to 30°C to 35°C, slowly add 85g of calcium chloride to the concentrated solution under stirring, the addi...

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Abstract

The invention discloses a method for separating alpha-ketoglutaric acid from a conversion solution, which comprises the following steps: sequentially carrying out ceramic filtration, ultrafiltration and reverse osmosis on the conversion solution to obtain an alpha-ketoglutaric acid concentrated solution; reacting the obtained concentrated solution with calcium superchloride, and filtering to obtain alpha-ketoglutarate; adding the alpha-ketoglutarate and ethanol into a reaction kettle, slowly and dropwisely adding sulfuric acid, stopping adding the acid when the pH value of the ethanol solution is 1.3-1.5, stirring to react to generate a calcium sulfate precipitate, filtering, and collecting the filtrate which is a ketoglutaric acid ethanol solution; eluting the residual alpha-ketoglutaric acid from the calcium sulfate with ethanol, and collecting the eluting solution; and mixing the filtrate and eluting solution, and heating and concentrating under reduced pressure to precipitate the alpha-ketoglutaric acid crystal. The membrane filtration technique is adopted to avoid abundant water evaporation; and thus, the method has the advantages of energy saving, high production yield, favorable crystal form, light color of the crystal grain, and stable product quality, and can easily implement industrialized large-scale production.

Description

technical field [0001] The invention relates to the technical field of preparation of alpha-ketoglutaric acid. Background technique [0002] α-ketoglutaric acid is an important organic acid, which plays an important role in the metabolism of microbial cells. It is one of the important intermediate metabolites of the trihydroxy acid cycle and participates in the metabolism of amino acids, sugars, proteins and fats, etc. It is an important physiological process and is an important precursor substance for the synthesis of various amino acids and proteins. Therefore, it is widely used in the food, medicine, chemical and cosmetic industries, and the market demand is huge. At present, the production and preparation methods of α-ketoglutaric acid mainly include chemical synthesis, microbial fermentation synthesis and enzyme-catalyzed conversion. Among them, the chemical synthesis method has long chemical synthesis routes, low yields, and the use of toxic chemical reagents and othe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/347C07C51/42
CPCC07C51/42C07C51/43C07C51/487C07C59/347Y02P20/10
Inventor 李斌水王殿涛
Owner JING JING PHARMA
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