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Method for preparing vitamin A acetate

A technology of acetate and vitamin, which is applied in the field of preparing vitamin A acetate, can solve the problems of many side reactions, difficult product separation, high energy consumption, etc., and achieve the effects of reducing separation and purification operations, simple process operation, and shortened process flow

Active Publication Date: 2019-04-19
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, the synthesis process of vitamin A acetate prepared by chemical synthesis is complicated, the reaction conditions are harsh, and there are many side reactions and by-products, which bring great difficulties to the separation of subsequent products; and the energy consumption is high, and the impact on the environment is large. Therefore, it is necessary to seek a A green manufacturing process has become an urgent problem to be solved

Method used

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  • Method for preparing vitamin A acetate
  • Method for preparing vitamin A acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] (1) After the autoclave leak detection, add (264.5g, 1.01mol) triphenylphosphine and (96.8g, 38wt%, 1.01mol) hydrochloric acid wherein; 2 After 3 replacements, fill the autoclave with CO 2 Gas and start stirring, heat up so that the temperature in the autoclave is 45°C, and the pressure in the autoclave is maintained at 14MPa through a pressure regulating valve, and (220g, 1mol) vinyl-β ionol is pumped into the autoclave by an advection pump Carry out salt-forming reaction to prepare C15 phosphine salt.

[0062] (2) After 1 hour of salt-forming reaction, add (156.1g, 1.1mol) C5 aldehyde, (15.9g) [Bmim]OH ionic liquid and (1058g) solvent water into the high pressure reactor through a parallel flow pump, and then release the pressure to release Out of CO 2 , and mix the materials evenly.

[0063](3) Add (350mL) petroleum ether into the kettle, start stirring under nitrogen protection and heat to 35°C, then start to add lye (116.4g, 1.1mol of sodium carbonate and 550g o...

Embodiment 2

[0065] (1) After the autoclave leak detection, add (111g, 0.42mol) triphenylphosphine and (40.6g, 38wt%, 0.42mol) hydrochloric acid wherein; Use CO 2 After 3 replacements, fill the autoclave with CO 2 Gas and start stirring, heat up so that the temperature in the autoclave is 60°C, and the pressure in the autoclave is maintained at 25MPa through a pressure regulating valve, and (88g, 0.4mol) vinyl-β ionol is pumped into the high-pressure reaction by an advection pump A salt-forming reaction is carried out in the kettle to prepare C15 phosphine salt.

[0066] (2) After 2 hours of salt-forming reaction, add (65.3g, 0.46mol) C5 aldehyde, (53.3g) [Bmim] CH 3 COO ionic liquid and (890g) solvent water, then release pressure to release CO 2 , and mix the materials evenly.

[0067] (3) Add (890mL) n-heptane into the kettle, start stirring under nitrogen protection and heat to 50°C, then start to add lye (35.9g, 0.64mol of potassium hydroxide and 35g of water) into the kettle for Wi...

Embodiment 3

[0069] (1) After the autoclave leak detection, add (134.9g, 0.51mol) triphenylphosphine and (49.3g, 38wt%, 0.51mol) hydrochloric acid wherein; 2 After 3 replacements, fill the autoclave with CO 2 Gas and start stirring, heat up so that the temperature in the autoclave is 53°C, and the pressure in the autoclave is maintained at 20MPa through a pressure regulating valve, and (110g, 0.5mol) vinyl-β ionol is pumped into the high-pressure reaction by an advection pump A salt-forming reaction is carried out in the kettle to prepare C15 phosphine salt.

[0070] (2) After 1.5h of salt-forming reaction, add (80.2g, 0.56mol) C5 aldehyde, (32.4g) [Bmim]Im ionic liquid and (810g) solvent water in autoclave by advection pump, then release pressure Release CO 2 , and mix the materials evenly.

[0071] (3) Add (405mL) n-hexane into the kettle, start stirring under nitrogen protection and heat to 43°C, then start to add lye (26g, 0.65mol of sodium hydroxide and 100g of water) into the kett...

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Abstract

The invention belongs to the technical field of production of vitamin A and its derivatives, in particular to a method for preparing vitamin A acetate. The method comprises the following steps: (1) mixing triphenylphosphine and acid in supercritical CO2, and then contacting the obtained mixture with vinyl-beta-ionol for salt formation to obtain C15 phosphine salt; (2) after adding solvent water, ionic liquid and C5 aldehyde to the finished system of step (1) , CO2 is released for solvent replacement, and the materials are uniformly mixed; (3) adding an extractant to the system after the solvent replacement of step (2), stirring and adding an alkali solution for Wittig reaction to obtain the vitamin A acetate. The method of the invention has mild reaction conditions, safe production and easy control, and the purity and reaction yield of the final product are high.

Description

technical field [0001] The invention belongs to the technical field of production of vitamin A and derivatives thereof, and in particular relates to a method for preparing vitamin A acetate. Background technique [0002] The chemical name of vitamin A is retinol, which is the first discovered vitamin, a natural fat-soluble vitamin, and one of the essential nutrients for the human body. In 1913, four scientists including Davis in the United States discovered that cod liver oil could cure dry eye disease, and purified a yellow viscous liquid from cod liver oil. In 1920, British scientist Manot officially named it vitamin A. Internationally, vitamin A is officially regarded as an essential factor in nutrition. It participates in various physiological processes of the body; it can maintain normal visual response, maintain the normal shape and function of epithelial tissue, maintain normal bone development, and maintain skin cell function. However, vitamin A is very unstable and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/343C07C69/145C07F9/54
CPCC07C67/343C07F9/5442C07C2601/16C07C69/145Y02P20/54
Inventor 林龙梁海涛张涛吕英东黎源张旭程晓波王延斌朱龙龙
Owner WANHUA CHEM GRP CO LTD
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