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D-calcium pantothenate total synthesis environment-friendly process

A calcium pantothenate, total synthesis technology, applied in the preparation of carboxylic acid amide, preparation of organic compounds, separation/purification of carboxylic acid amide, etc., can solve the problems of increased loss, poor working environment, and only 80-85%

Inactive Publication Date: 2020-07-14
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 recycles raw materials such as methanol, calcium, D-pantotolactone, β-alanine and other raw materials and returns them for use. The unrecoverable or deteriorated materials are sent to the environmental protection system as waste liquid Sulfuric acid and a large amount of organic solvents are used in the process of treatment and recovery, which increases the loss and the working environment is poor. The comprehensive utilization rate of the main raw materials in this process can only reach 80-85% in industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Preparation of calcium β-alanine: Put 89 kg (1000 moles) of β-alanine into a 1000-liter reactor, add 300 kg of water, start stirring, and after 10 minutes, drop 50% (volume ratio ) of sulfuric acid solution in 200 ml, then gradually add 30 kg (510 moles) of calcium oxide at no higher than 45 °C, and stir for half an hour after the addition is complete. Raise the temperature to 50-56°C and react for 3 hours, add 6 kg of diatomaceous earth, raise the temperature to boiling, filter the clear liquid into a 1500 liter evaporated kettle, wash the filter equipment and pipeline twice with 100 kg of water, and merge all the washing water into Evaporate to dryness inside the kettle. Turn on the steam valve, turn on the vacuum unit, turn on the evaporation kettle to stir, and dehydrate until the water content of calcium β-alanine is 0.98%. Add 240 kilograms of methanol into the evaporation kettle;

[0028] (2) Preparation of D-calcium pantothenate methanol solution: dissolve...

Embodiment 2

[0031] (1) Preparation of calcium β-alanine: Put 89 kg (1000 moles) of β-alanine into a 1000-liter reactor, add 600 kg of water, start stirring, and after 10 minutes, add 20% (volume ratio) of sulfuric acid solution 200 ml, then gradually add 40 kg (700 moles) of calcium oxide at no higher than 45 ° C, and stir for half an hour after the addition is complete. Raise the temperature to 72-75°C and react for 2 hours, add 8 kg of diatomaceous earth, raise the temperature to boiling, filter the clear liquid into a 1,500-liter evaporated kettle, wash the filter equipment and pipelines with 200 kg of water three times, and merge all the washing water into the steamer. In the dry kettle. Turn on the steam valve, turn on the vacuum unit, turn on the evaporation kettle to stir, and dehydrate until the water content of calcium β-alanine is 4.2%. Add 400 kilograms of methanol into the evaporation kettle;

[0032] (2), preparation of D-calcium pantothenate methanol solution: dissolve 136...

Embodiment 3

[0035](1) Preparation of calcium β-alanine: Put 89 kg (1000 moles) of β-alanine into a 1000-liter reactor, add 400 kg of water, start stirring, and after 10 minutes, add 40% (volume ratio) of sulfuric acid solution 100 ml, then gradually add 33 kg (580 moles) of calcium oxide at 10-20 ° C, and stir for half an hour after the addition is complete. Raise the temperature to 25°C and react for 8 hours, add 3 kg of diatomaceous earth, raise the temperature to boiling, filter the clear liquid into a 1500 liter evaporated kettle, wash the filter equipment and pipeline twice with 120 kg of water, and merge all the washing water into evaporated to dryness Inside the cauldron. Turn on the steam valve, turn on the vacuum unit, turn on the evaporation kettle to stir, and dehydrate until the water content of β-alanine calcium is 0.46%. Add 700 kilograms of methanol into the evaporation kettle;

[0036] (2) Preparation of D-calcium pantothenate methanol solution: Stir and heat up to reflu...

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Abstract

The invention relates to a complete set of new process for synthesizing D-calcium pantothenate. According to the invention, the method comprises the following steps: synthesizing beta-calcium aminopropionate from beta-aminopropionic acid and calcium oxide in water and / or methanol; after filtering, evaporating water and / or methanol in the beta-calcium aminopropionate solution to dryness under negative pressure; or after filtering, stirring and crystallizing for 8-40 hours at the temperature of 20-65 DEG C, filtering again, replacing mother liquor in a re-filtered filter cake with methanol for more than three times, enabling the moisture content in the filter cake to be less than 1%, removing 70% or more of solvent from filtrate, and applying the filtrate to a re-filtering step; soaking beta-calcium aminopropionate with methanol, adding a methanol solution of D-pantolactone, carrying out a reaction at a low temperature, carrying out a reflux reaction to synthesize D-calcium pantothenate,completely or partially evaporating methanol, adding water, dissolving, filtering, transferring into a spray dryer, and carrying out spray drying to obtain the product D-calcium pantothenate. The product quality meets the industrial standard, and the product yield is increased by 15%-20% compared with the existing process level.

Description

technical field [0001] The present invention relates to a kind of D-calcium pantothenate full-synthetic environment-friendly process, in particular to a complete set of new process for synthesizing D-calcium pantothenate with a product yield of 100%. 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 recycles raw materials such as methano...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C231/24C07C235/12C07C227/18C07C229/08
CPCC07C231/02C07C231/24C07C227/18
Inventor 吴江
Owner 安徽泰格生物科技有限公司
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