Preparation method of vitamin A palmitate

A technology of palmitate and vitamins, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of thermal deterioration of VA alcohol, affecting product quality, and reaction process Complicated problems, to achieve the effects of easy crystallization, stable storage of crystallization, and good selectivity

Active Publication Date: 2021-04-30
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction process is complex and filtered multiple times, and the steps are cumbersome
In addition, in the process of decompressing and distilling excess organic alcohol, it is easy to cause VA alcohol to deteriorate due to heat, which affects product quality.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]Put 20g of silicon dioxide in 200mL of 5wt% hydrochloric acid, soak it at 50°C for 2h, quickly add 20g of polystyrene powder under stirring, filter vigorously to obtain a white solid, dry at 50°C for 5h, grind until use. Add 1 mol of sodium sulfide dropwise into 500mL of butanol and water mixed solvent, wherein the volume ratio of water and butanol is 0.1:1, weigh 10g of the above solid powder and pour it into the sodium sulfide solution, stir at 50°C for 8h , bubbling 50 mL / min of nitrogen gas into the system, and raising the temperature of the system to 250° C. under reflux, and stopping the nitrogen gas feeding. The prepared 0.5mol / L, 1L methanol solution of potassium ferricyanide was added dropwise thereto, and the dropwise flow rate was controlled to ensure that the dropwise addition time was 1h. After the dropwise addition, the obtained solid was taken out by filtration, and roasted at 100°C for 5h in a nitrogen atmosphere to obtain the catalyst Na 2 S-K 3 [Fe(C...

Embodiment 2

[0044] Put 20g of silicon dioxide in 200mL of 10wt% hydrochloric acid, soak at 100°C for 6h, quickly add 60g of polystyrene powder under stirring, filter after vigorously stirring, dry at 80°C for 8h, and grind for later use. Add 1mol of sodium sulfide dropwise to 500mL of mixed solvent of butanol and water, wherein the volume ratio of water to butanol is 0.25:1, weigh 20g of the above solid powder and add it to the sodium sulfide solution, and stir at 100°C for 12h 100 mL / min of nitrogen gas was blown into the system, and the temperature of the system was raised to 300° C. under reflux, and the nitrogen gas flow was stopped. The prepared 1.0 mol / L, 1 L methanol solution of sodium hexacyanocobaltate (III) was added dropwise thereto, and the dropping flow rate was controlled to ensure that the dropping time was 1.5 h. After the dropwise addition, the obtained solid was taken out by filtration, and roasted at 200°C for 8h in a nitrogen atmosphere to obtain the catalyst Na 2 S-N...

Embodiment 3

[0047] Put 20g of silicon dioxide in 200mL of 15wt% hydrochloric acid, soak at 250°C for 12h, quickly add 100g of polystyrene powder under stirring, vigorously stir and filter, dry at 120°C for 12h, and grind for later use. Add 1mol of potassium sulfide dropwise into 500mL of mixed solvent of butanol and water, wherein the volume ratio of water and butanol is 0.5:1, weigh 50g, take the above white powder and pour it into potassium sulfide solution, stir at 150°C for 16h 250 mL / min of nitrogen gas was blown into the system, and the temperature of the system was raised to 450° C. under reflux, and the nitrogen gas flow was stopped. The prepared 2.0mol / L, 1L methanol solution of potassium cyanate was added dropwise thereto, and the dropwise flow rate was controlled to ensure that the dropwise addition time was 2.5h. After the dropwise addition, the obtained solid was taken out by filtration, and calcined at 300° C. for 10 h in a nitrogen atmosphere to obtain catalyst K 2 S-KCN@P...

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PUM

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Abstract

The invention provides a preparation method of vitamin A palmitate. According to the method, metal cyanide is adopted to modify alkali metal sulfide to obtain a solid base catalyst for vitamin A palmitate, VA acetate and palmitic acid are taken as raw materials, vitamin A palmitate is synthesized by a one-step method, and the method has the advantages of mild reaction conditions, high selectivity, and no by-products. A product obtained through the reaction can be more stably stored at a low temperature and is easy to crystallize and separate out, and the yield is high; the problem of equipment corrosion existing in a solid acid catalytic system in traditional vitamin A palmitate synthesis is solved, and the process is green and environmentally friendly.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a preparation method of vitamin A palmitate. Background technique [0002] Vitamin A, also known as retinol, is a natural fat-soluble vitamin and one of the essential nutrients for the human body. However, vitamin A is irritating to the skin, and its chemical properties are relatively active. It is easily damaged by acid, air, oxidizing agents, high temperature or ultraviolet rays. However, vitamin A ester derivatives are relatively stable and non-irritating. Available on the market in the form of esters. In the series of vitamin A ester products, vitamin A acetate and vitamin A palmitate have the largest market share. Due to the long carbon chain, low melting point and good oil solubility of VA palmitate, it has been widely used in food, Drugs and cosmetics have become the most commonly used additives in food or cosmetics. [0003] VA palmitate is mainly prepared b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C403/12B01J31/18
CPCC07C403/12B01J31/1805B01J2231/49Y02P20/584
Inventor 罗朝辉林龙翟文超张弈宇王嘉辉高洪坤
Owner WANHUA CHEM GRP CO LTD
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