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Novel process for preparing D-pantothenic acid calcium salt

A new technology for calcium pantothenate, applied in the field of new technology for the preparation of D-calcium pantothenate, can solve the problems of only 80-85%, poor working environment, increased loss, etc., to ensure process stability, shorten production process, Make sure to generate safe results

Active Publication Date: 2020-08-11
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] The synthetic route of calcium D-pantothenate is currently used in the industry to react β-alanine and calcium oxide in methanol to synthesize calcium β-alanine, and then add D-pantothenate lactone to synthesize calcium D-pantothenate after filtration. D-calcium pantothenate is precipitated through low-temperature crystallization, and the mother liquor is recycled from raw materials such as methanol, calcium, D-pantolactone, β-alanine and other raw materials to be used; the unrecoverable or deteriorated materials are used as waste liquid and handed over to the environmental protection system Sulfuric acid and a large amount of organic solvents are used in the treatment and recovery process, which increases the loss and the working environment is poor. The comprehensive utilization rate of the main raw materials of this process can only reach 80-85% in industrial production, and D-pantolactone It is also necessary to use biological enzymes and other resolution reagents to resolve from DL-pantoate lactone and then undergo a complicated extraction process to obtain

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Preparation and splitting system: add 10,000 kg of tap water to a 15m³ reactor, add 2,600 kg (20 kilomoles) of pantoanolactone, and prepare an aqueous solution of pantoanolactone with a content of 20.63%, and then add 1,000 Kg of biological enzymes, stirred at 23-30°C for 0.5 hours, set aside;

[0031] (2) Add β-alanine calcium aqueous solution dropwise: Slowly add 26% β-alanine calcium aqueous solution 4154 kg (5 kilomoles) under stirring at 23-30°C, keep the reaction during the dropping process The pH value of the system is between 6.8-7.3. After 23 hours of reaction, the clear liquid is filtered out, and the specific optical rotation of the clear liquid (converted by L-pantolactone) is 57.1° at 23°C;

[0032] (3) Dehydration and solvent addition: After the reaction is completed, the supernatant is concentrated in a vacuum higher than -0.085MPa to 115°C, cooled to 65°C and added with 1280 kg of methanol, stirred and cooled to 20°C;

[0033] (4) Separation and pur...

Embodiment 2

[0036] (1) Preparation and splitting system: add 8000 kg of tap water to a 15m³ reactor, add 2300 kg (17.692 kilomoles) of pantothenolactone to prepare a pantotolactone aqueous solution with a content of 22.33%, and then add 900 Kg of biological enzyme, stirred for 1.5 hours at 23-30°C, set aside;

[0037] (2) Add β-alanine calcium aqueous solution dropwise: 4777 kg (4.423 kilomoles) of β-alanine calcium aqueous solution with a content of 20% is slowly added dropwise under stirring at 23-30°C, and the reaction is maintained during the dropping process The pH value of the system is between 6.1-6.5. After 29 hours of reaction, the clear liquid is filtered out, and the specific optical rotation of the clear liquid (converted by L-pantolactone) is 57.3° when detected at 28°C;

[0038] (3) Dehydration and solvent addition: After the reaction is completed, the supernatant is concentrated in a vacuum higher than -0.085MPa to 120°C, cooled to 60°C and added with 1810 kg of methanol, s...

Embodiment 3

[0042] (1) Preparation and splitting system: add 9000 kg of tap water to a 15m³ reactor, add 2600 kg (20 kilomoles) of pantothenolactone to prepare a pantotolactone aqueous solution with a content of 22.41%, and then add 1000 Kg of biological enzyme, stirred for 1 hour at 23-30°C, set aside;

[0043] (2) Add β-alanine calcium aqueous solution dropwise: Slowly add 3600 kg (5 thousand moles) of β-alanine calcium aqueous solution with a content of 30% under stirring at 23-30°C, and keep the reaction during the dropping process The pH value of the system is between 6.8 and 7.1. After 26 hours of reaction, the clear liquid is filtered out, and the specific optical rotation of the clear liquid (converted by L-pantolactone) is 57.5° when detected at 26°C;

[0044] (3) Dehydration and solvent addition: After the reaction is completed, the supernatant is concentrated in a vacuum higher than -0.085MPa to 118°C, cooled to 50°C and added with 1550 kg of methanol, stirred and cooled to 30°...

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PUM

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Abstract

The invention provides a novel process for preparing a D-pantothenic acid calcium salt and relates to a novel process for preparing a D-pantothenic acid calcium salt. According to the basic scheme ofthe invention, the novel process comprises the following steps of: preparing a water solution with the content of 16-26% from DL-pantolactone, adding a biological enzyme which is 5-15% of mass of thewater solution, performing uniform mixing, and then slowly dropwise adding a calcium di-beta-alaninate water solution in which the content of calcium di-beta-alaninate is 20-30% in a molar amount of 0.49-0.51 fold that of D-pantolactone contained in the water solution at 23-30 DEG C; performing reaction all the time until complete hydrolysis of the D-pantolactone, filtering out a clear liquid andrecycling the biological enzyme in a filter cake; keeping a pH value of a reaction system between 6.0 and 7.3 during dropwise adding; concentrating the clear liquid in vacuum of -0.085MPa or above andat 115-120 DEG C after reaction is completed, performing cooling to 65 DEG C or below, adding methanol of which the weight is 0.5-0.8 fold that of D-pantothenic acid calcium di-beta-alaninate, performing mixing and cooling to 20-40 DEG C, performing filtering, and washing, pulping and rewashing the filter cake with the methanol to achieve purification; collecting filtrate of a few times, recovering the methanol and then forming the DL-pantolactone in a racemization manner to reuse; and drying the filter cake through two levels of temperature zones of 105-125 DEG C and 150-160 DEG C, and performing cooling and discharging to obtain the D-pantothenic acid calcium salt. According to the novel process, a precursor substance D-pantothenic acid calcium di-beta-alaninate of the D-pantothenic acid calcium salt is generated in one step during resolution reaction, so that the process of extracting and separating the D-pantolactone is avoided.

Description

technical field [0001] The invention relates to a new process for preparing calcium D-pantothenate. Background technique [0002] Calcium D-pantothenate is vitamin B5 with the chemical name (R)-(+)-N-(2,4-dihydroxy-3,3-dimethyl-1-oxobutyl)-beta-alanine Calcium salt, English name: D-(+)-Pantothenic acid calcium salt, as an important nutritional ingredient, is widely used in feed additives, food additives, medicine and other fields; [0003] The synthetic route of calcium D-pantothenate is currently used in the industry to react β-alanine and calcium oxide in methanol to synthesize calcium β-alanine, and then add D-pantothenate lactone to synthesize calcium D-pantothenate after filtration. D-calcium pantothenate is precipitated through low-temperature crystallization, and the mother liquor is recycled from raw materials such as methanol, calcium, D-pantolactone, β-alanine and other raw materials to be used; the unrecoverable or deteriorated materials are used as waste liquid ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P41/00C12P13/04C07C231/02
CPCC12P41/005C12P13/04C07C231/02C07B2200/07C07C235/12
Inventor 吴江
Owner 安徽泰格生物科技有限公司
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