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Green synthesis method of D-calcium pantothenate

A technology for green synthesis, calcium pantothenate, applied in the field of green synthesis of D-calcium pantothenate, can solve the problems of large D-pantothenate, low content of D-pantothenate, etc., achieves simple operation, less waste, and industrial adaptability strong effect

Inactive Publication Date: 2018-06-08
CHONGQING BEISHENG PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the content of D-calcium pantothenate prepared by this method is low, and the content of D-pantothenic acid is relatively large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In the reactor, add β-alanine 71kg, calcium oxide 26.80kg, anhydrous methanol 426kg. Slowly warm to 33°C. The temperature was controlled at 33° C., and the reaction was stirred for 1 h. Diatomaceous earth was added to aid in filtering, and the stirring reaction was continued for 0.5h, and filtered. The filtrate was collected, the temperature of the filtrate was lowered to 2° C., and 100 kg of D-pantolactone was added. Control the temperature at 2°C, stir and react for 4 hours, add 1.0 kg of seed crystals, continue to stir and react for 16 hours, add 1.0 kg of purified water, and then lower the temperature to -15°C. Stir and crystallize for 4 hours, then filter with suction, and wash the reaction flask and filter cake with anhydrous methanol solution. Collect the filter cake, dissolve the filter cake in 50kg of water, and then spray dry to obtain 164.77kg of white powdery solid.

[0025] After evaporating the above methanol mother liquor to dryness, add 100kg of 6 mo...

Embodiment 2

[0027] In the reactor, add β-alanine 71kg, calcium oxide 26.80kg, anhydrous methanol 426kg. Slowly warm to 37°C. The temperature was controlled at 37°C, and the reaction was stirred for 1 h. Add diatomaceous earth, continue to stir the reaction for 0.5h, and filter. Collect the filtrate, cool the filtrate to -2°C, and add 100 kg of D-pantolactone. Control the temperature at -2°C, stir and react for 4 hours, add 1.0 kg of seed crystals, continue to stir and react for 16 hours, add 1.0 kg of purified water, and then lower the temperature to -20°C. Stir and crystallize for 4 hours, then filter with suction, and wash the reaction flask and filter cake with anhydrous methanol solution. Collect the filter cake, dissolve the filter cake in 50kg of water, and then spray dry to obtain 164.77kg of white powdery solid.

[0028] After evaporating the above methanol mother liquor to dryness, add 100kg of 6 mole hydrochloric acid, then raise the temperature to 90°C, hydrolyze for 3h, th...

Embodiment 3

[0030] In the reactor, add β-alanine 71kg, calcium oxide 26.80kg, anhydrous methanol 426kg. Slowly raise the temperature to 45°C. The temperature was controlled at 45° C., and the reaction was stirred for 1 h. Add diatomaceous earth, continue to stir the reaction for 0.5h, and filter. Collect the filtrate, cool the filtrate to 10° C., and add 100 kg of D-pantolactone. Control the temperature at 10°C, stir and react for 4 hours, add 1.0 kg of seed crystals, continue to stir and react for 12 hours, add 1.0 kg of purified water, and then lower the temperature to -15°C. Stirring and crystallization for 4h. Suction filtration, washing reaction flask and filter cake with anhydrous methanol solution. Collect the filter cake, dissolve the filter cake in 50kg of water, and then spray dry to obtain 164.77kg of white powdery solid.

[0031] After evaporating the above methanol mother liquor to dryness, add 100kg of 6 mole hydrochloric acid, then raise the temperature to 90°C, hydrol...

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Abstract

The invention discloses a green synthesis method of D-calcium pantothenate. The green synthesis method of D-calcium pantothenate provided by the invention comprises the steps that beta-alanine is added into methyl alcohol; then, a calcium source is added; temperature rise and stirring are performed for reaction; filtering is performed; filter liquid is collected; filter liquid is subjected to temperature cooling; then, D-pantolactone is added; stirring reaction is performed; seed crystals are added; stirring reaction is continuously performed; after the reaction is finished, water is added; crystallization is continuously performed at -15 DEG C to -20 DEG C; then, filtering and washing are performed; filtering cake and filtering liquid are respectively collected; the filtering cake is dried; the filtering liquid is subjected to acid hydrolysis; DL-pantolactone is recovered. The green synthesis method has the advantages that the D-calcium pantothenate is prepared from calcium pantothenate; the process route operation is simple; the reaction conditions are mild; safety is realized; the environment is protected; the raw materials are cheap and can be easily obtained; the industrial adaptability is high; the wastes are few; the used raw materials can be recovered and utilized; the goal of clean production is reached.

Description

technical field [0001] The invention relates to the fields of medicine, food and feed additives, in particular to a green synthesis method of calcium D-pantothenate. Background technique [0002] Calcium D-pantothenate, also known as vitamin B5, is an essential vitamin for human life activities, and can be used as a feed additive and food additive, and its market capacity is huge. [0003] In the prior art, the main synthesis method of D-calcium pantothenate is to condense DL-pantothenate and calcium β-alanine, and then undergo multiple crystallizations to obtain qualified D-calcium pantothenate. This method prepares calcium pantothenate pollution Large, low yield. [0004] After research and development, D-calcium pantothenate is also obtained through microbial fermentation in the prior art. At present, this preparation method has not yet been scaled up for industrial production. [0005] The third synthesis method is to use D-pantothenate as a raw material, then condense...

Claims

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Application Information

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IPC IPC(8): C07C235/12C07C231/02C07C231/24C07C227/18C07C229/08
CPCC07C227/18C07C231/02C07C231/24C07C229/08C07C235/12
Inventor 潘敬坤丁宝
Owner CHONGQING BEISHENG PHARMA TECH CO LTD
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