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A kind of aqueous solution crystallization method of d-pantolactone

A technology of pantolactone and aqueous solution, which is applied in organic chemistry methods, organic chemistry, etc., can solve the problems of refining D-sodium pantoate lactone, cumbersome steps, pollution, etc., and achieve reduced equipment investment and simple steps , Reduce the effect of the process

Active Publication Date: 2021-09-17
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

[0005] However, no matter what resolution method will encounter the refining problem of D-sodium pantoate lactone
In the prior art, in the step of extracting D-pantoolactone, the traditional method is to use organic solvents to extract and then refine to obtain qualified D-pantoolactone. Solvents such as ethyl acetate, dichloromethane, and toluene are used. There are problems of toxicity and pollution, and the steps are cumbersome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The present embodiment provides a kind of aqueous solution crystallization method of D-pantolactone, and concrete steps are:

[0022] Take 2L of the lactonized D-pantoate solution (containing 20.1% D-pantoate lactone and 15% inorganic salt) and concentrate under reduced pressure at 60°C to adjust the concentration of D-pantoate lactone At 30.0%, the cooling rate is 8°C / h to 1°C, the stirring speed is 30r / min, the temperature is kept at 1°C for 2h, and 300g of material is obtained by suction filtration.

[0023] The yield of D-pantolactone obtained in this example is 75%, the specific rotation is -50.0°, the crystals are regular, uniform and the particles are large.

Embodiment 2

[0025] The present embodiment provides a kind of aqueous solution crystallization method of D-pantolactone, and concrete steps are:

[0026] Take 2L of the lactonized D-pantoate solution (containing 18.1% D-pantoate lactone and 14% inorganic salt) and concentrate under reduced pressure at 60°C to adjust the concentration of D-pantoate lactone At 28.0%, the cooling rate is 8°C / h to 3°C, the stirring speed is 30r / min, the temperature is kept at 3°C ​​for 2h, and 260g of material is obtained by suction filtration.

[0027] The yield of D-pantolactone obtained in this example was 72%, the specific rotation was -49.9°, and the crystals were regular, uniform and large in size.

Embodiment 3

[0029] The present embodiment provides a kind of aqueous solution crystallization method of D-pantolactone, and concrete steps are:

[0030] Take 2L of the lactonized D-pantoate solution (containing 19.1% D-pantoate lactone and 14.5% inorganic salt) and concentrate under reduced pressure at 60°C to adjust the concentration of D-pantoate lactone At 30.0%, the cooling rate is 8°C / h to 4°C, the stirring speed is 30r / min, the temperature is kept at 4°C for 2h, and 260g of material is obtained by suction filtration.

[0031] The yield of D-pantolactone obtained in this example was 68%, the specific rotation was -50.2°, and the purity was 98.1%. The crystals are regular, uniform and large in size.

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Abstract

The present invention relates to an aqueous solution crystallization method of D-pantolactone, which comprises the following steps: using an aqueous inorganic salt solution containing 15-23% D-pantolactone as a raw material, concentrating and making D-pantolactone in it When the concentration of the ester reaches 28-35%, the temperature is lowered to 0-5°C at a rate of 2-8°C / h, and the temperature is maintained for crystallization. The method provided by the invention realizes crystallization by adjusting the concentration of D-pantoic acid lactone in an aqueous solution of inorganic salt and controlling the cooling rate, and is preferably suitable for using D-pantoic acid as a raw material and adopting a lactonization process to prepare D ‑A mixed solution obtained from pantotolactone. The method has the characteristics of simple steps, easy operation and high quality, and is an effective method for the crystallization and purification of D-pantolactone.

Description

technical field [0001] The invention relates to the field of chemical production, in particular to an aqueous solution crystallization method of D-pantolactone. Background technique [0002] D-pantolactone is a white crystalline powder, easily soluble in methanol, ethanol, and water. Boiling point 120~122℃, density 1.165g / cm 3 , the specific rotation (20°C) is -45~-50.8 (C=2.5, water). [0003] D-pantothenolactone can be used to produce D-calcium pantothenate, D-panthenol and D-panthenol ethyl ether, and the market is huge. For example, the lack of calcium D-pantothenate in the human body can cause the following symptoms: growth arrest, weight loss, sudden death, skin and hair disorders, nervous system disorders, digestive organ disorders, liver dysfunction, affecting antibody formation, etc. Calcium D-pantothenate can also be used as a food additive and feed additive. It plays an important role in the formation of epidermal tissue. It is used as an active ingredient in p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/33
CPCC07B2200/13C07D307/33
Inventor 段小瑞汪洪湖杜斌李涛陶勇
Owner 安徽泰格生物科技有限公司
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