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 met

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0023] Example 1

[0024] In the reactor, 71 kg of β-alanine, 26.80 kg of calcium oxide, and 426 kg of anhydrous methanol were added. Slowly increase the temperature to 33°C. The temperature was controlled at 33°C, and the reaction was stirred for 1 hour. Add diatomaceous earth to aid filtration, continue to stir and react for 0.5h, and filter. Collect the filtrate, cool the filtrate to 2°C, and add 100 kg of D-pantolactone. The temperature was controlled at 2°C, the reaction was stirred for 4 hours, 1.0 kg of seed crystals were added, and then the reaction was continued to stir for 16 hours, 1.0 kg of purified water was added, and then the temperature was reduced to -15°C. After stirring and crystallizing for 4 hours, it was filtered with suction, and the reaction flask and filter cake were washed with anhydrous methanol solution. The filter cake was collected, dissolved in 50 kg of water, and then spray-dried to obtain 164.77 kg of white powdery solid.

[0025] After evapora...

Example Embodiment

[0026] Example 2

[0027] In the reactor, 71 kg of β-alanine, 26.80 kg of calcium oxide, and 426 kg of anhydrous methanol were added. Slowly increase the temperature to 37°C. The temperature was controlled at 37°C, and the reaction was stirred for 1 hour. Add diatomaceous earth, continue to stir and react for 0.5h, and filter. Collect the filtrate, cool the filtrate to -2°C, and add 100 kg of D-pantolactone. The temperature was controlled at -2°C, the reaction was stirred for 4 hours, 1.0 kg of seed crystals were added, and then the reaction was continued to stir for 16 hours, 1.0 kg of purified water was added, and then the temperature was lowered to -20°C. After stirring and crystallizing for 4 hours, it was filtered with suction, and the reaction flask and filter cake were washed with anhydrous methanol solution. The filter cake was collected, dissolved in 50 kg of water, and then spray-dried to obtain 164.77 kg of white powdery solid.

[0028] After evaporating the above m...

Example Embodiment

[0029] Example 3

[0030] In the reactor, 71 kg of β-alanine, 26.80 kg of calcium oxide, and 426 kg of anhydrous methanol were added. Slowly increase the temperature to 45°C. The temperature was controlled at 45°C, and the reaction was stirred for 1 hour. Add diatomaceous earth, continue to stir and react for 0.5h, and filter. Collect the filtrate, cool the filtrate to 10°C, and add 100 kg of D-pantolactone. The temperature was controlled at 10°C, the reaction was stirred for 4 hours, 1.0 kg of seed crystals were added, and then the reaction was continued to stir for 12 hours, and 1.0 kg of purified water was added, and then the temperature was reduced to -15°C. Stir and crystallize for 4h. Suction filtration, wash the reaction flask and filter cake with anhydrous methanol solution. The filter cake was collected, dissolved in 50 kg of water, and then spray-dried to obtain 164.77 kg of white powdery solid.

[0031] After evaporating the above methanol mother liquor to dryness,...

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PUM

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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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