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Preparation method of vitamin A acetate

A vitamin and acetate technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve the problems of difficult waste alkali treatment, large amount of alkali catalyst, and many by-products , to achieve the effect of easy separation, saving process and simple operation

Active Publication Date: 2021-06-01
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using this method to prepare vitamin A acetate can avoid the problems of many by-products and serious equipment corrosion caused by traditional acid catalysts in the reaction; it also solves the defects of large amount of alkali catalyst and difficulty in the treatment of spent alkali.

Method used

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  • Preparation method of vitamin A acetate
  • Preparation method of vitamin A acetate
  • Preparation method of vitamin A acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Catalyst preparation:

[0045] (1) Dissolve 0.05mol of copper hexacyanocobaltate(III) in 31mL of water / ethanol (the volume ratio of water to ethanol is 0.2:1), stir and dissolve, then feed nitrogen and heat up to 50°C with an oil bath After ℃, 69.0 g of 10 wt % potassium carbonate aqueous solution was added dropwise, and the dropping time was controlled to be 30 min. After the dropwise addition, the system was refluxed at 100° C. for 2 h. The obtained solid was filtered and dried, and then sealed with nitrogen for use, and recorded as solid one.

[0046] (2) Put 10g of activated carbon in 50mL, 10wt% sodium methoxide aqueous solution, stir and stand at 150°C for 3h, add 10g of PVP to the solution, stir vigorously and let stand for 2h, take out the solid and dry it. Recorded as solid two.

[0047] (3) Add 5 g of toluenesulfonic acid into 10 mL of methanol at 0° C., stir evenly, measure the pH of the system to be 3, and let it stand for use. Take 10g of the solid 2 pre...

Embodiment 2

[0050] Catalyst preparation:

[0051] (1) Dissolve 0.1 mol of copper hexacyanocobaltate (III) in 62 mL of water / ethanol (the volume ratio of water to ethanol is 0.3:1), stir and dissolve, then feed nitrogen and heat up to 100 °C with an oil bath After ℃, 138g, 10wt% potassium carbonate aqueous solution was added dropwise, and the dropping time was controlled to be 40min. After the dropwise addition, the system was refluxed at 120℃ for 4h. The obtained solid was filtered and dried, and then sealed with nitrogen for use, and recorded as solid one.

[0052] (2) Put 10g of activated carbon in 100mL, 15wt% sodium methoxide aqueous solution, stir and let it stand at 200°C for 4h, add 20g of PVP to the solution, stir vigorously and let it stand for 4h, take out the solid and dry it. Recorded as solid two.

[0053] (3) Add 5 g of toluenesulfonic acid into 10 mL of methanol at 1° C., stir evenly, measure the pH of the system to be 3.5, and let it stand still for use. Take 10g of the...

Embodiment 3

[0056] Catalyst preparation:

[0057] (1) Dissolve 0.1 mol of copper hexacyanocobaltate (III) in 62 mL of water / ethanol (the volume ratio of water to ethanol is 0.4:1), stir and dissolve, then feed nitrogen and heat up to 150 with an oil bath After ℃, 61g, 20wt% potassium carbonate aqueous solution was added dropwise, and the dropping time was controlled to be 50min. After the dropwise addition, the system was refluxed at 150℃ for 5h. The obtained solid was filtered and dried, and then sealed with nitrogen for use, and recorded as solid one.

[0058] (2) Put 10g of activated carbon in 70mL, 15wt% sodium methoxide aqueous solution, stir and let stand at 250°C for 5h, add 30g of PVP to the solution, stir vigorously and let stand for 6h, take out the solid and dry it, and the obtained solid Recorded as solid two.

[0059] (3) 10 g of toluenesulfonic acid was added into 33.3 ml of methanol at 2° C., and the pH of the system was measured to be 3.9 after stirring evenly. Take 10g...

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Abstract

The invention discloses a preparation method of vitamin A acetate. Thepreparation method is characterized in that raw materials including vinyl ionol, an organic phosphine compound and pentacarbonaldehyde react under the action of a catalyst to generate vitamin A acetate, and the vitamin A acetate is synthesized by adopting a one-step method. According to the invention, the problems of considerable byproducts, serious equipment corrosion and the like caused by a liquid acid catalyst in a reaction are avoided; and meanwhile, the defects of large dosage of a base catalyst, difficulty in waste alkali treatment and the like are overcome.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of vitamin A acetate. Background technique [0002] Vitamin A acetate is an important substance used in the fields of medicine and cosmetics, food and food supplements, animal nutrition feed additives, etc. It can maintain visual function, maintain the health of epithelial tissue cells, promote immunoglobulin synthesis, and maintain normal bone growth It plays an important role in development, promotion of growth and reproduction, and inhibition of tumor growth. [0003] The industrial synthesis of vitamin A acetate is mainly prepared from C10-C15 phosphine compounds (and C5-C10 aldehydes) under certain conditions through wittig reaction. Patent EP0382067 invented a method of combining 3,7,11-tri Methyldodeca-1,4,6,10-tetraen-3-ol reacts with triarylphosphine in the presence of boron trifluoride ether compound to give 3,7,11-trimethyld...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C403/12B01J31/16
CPCC07C403/12B01J31/16C07C2601/16B01J2531/845
Inventor 罗朝辉林龙程晓波吕英东张涛
Owner WANHUA CHEM GRP CO LTD
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