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Method for extracting gossypol acetic acid from cottonseed meal in presence of solid acid catalyst

A technology of gossypol acetate and solid acid, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carbonyl compounds, etc., to achieve simple preparation process, reduce pollution, and facilitate industrial production

Inactive Publication Date: 2012-01-04
朱明远
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to improve the extraction rate of gossypol acetate, the above-mentioned traditional method mostly adopts aniline as a drug intermediate, and a small amount of aniline remains in the resulting gossypol acetate product, which will cause hypokalemia when used as a medicinal reagent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Embodiment 1 gets 1mol, and dissolves 1L B and 9L water, add 10mol Acetate ethyl ester and 1mol 80C 10 After removing the upper solution by centrifugation, dry to obtain ZrSO / HMS-1 solid acid chemical agent; after crushing 1 kg of coarse cotton meal, add 3L of acetone aqueous solution with a mass fraction of 80%, and add 100mL of 3mol / L H 3 PO 4 The pH value of the solution was adjusted, and after soaking at room temperature for 8 hours, it was filtered to collect the obtained acetone solution. Mix the prepared 3L gossypol acetone solution with 1L 5% glacial acetic acid acetone solution, add 7 grams of ZrSO 4 / HMS-1 catalyst, reacted under stirring conditions for 150 minutes, filtered, stood at a temperature of 10°C for 4 hours, filtered under reduced pressure, and washed the obtained crystals with petroleum ether until the filtrate was colorless to obtain gossypol acetate. The weight of gossypol acetate is 0.891 g, and the purity reaches 100% by high perfo...

Embodiment 2

[0011] Example 2 Dissolve 1 mol of dodecylamine in 1 L of ethanol and 5 L of water, add 10 mol of tetraethyl orthosilicate and 1 mol of isobutanol, age at 20°C for 50 hours, centrifuge to remove the supernatant, and dry to obtain ZrSO 4 / HMS-2 solid acid catalyst; after pulverizing 1 kg of coarse cotton meal, add 3L mass fraction of 80% acetone aqueous solution, add 100mL of 3mol / L H 3 PO 4 The pH value of the solution was adjusted, and after soaking at room temperature for 8 hours, it was filtered to collect the obtained acetone solution. Mix the prepared 3L gossypol acetone solution with 1L 5% glacial acetic acid acetone solution, add 3 grams of ZrSO 4 / HMS-1 catalyst, react under stirring conditions for 100 minutes, filter, stand at a temperature of 10°C for 4 hours, filter under reduced pressure, wash the obtained crystals with petroleum ether until the filtrate is colorless, and obtain gossypol acetate. Gossypol acetate has a weight of 0.829 grams, and is detected by hi...

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Abstract

The invention relates to a method for extracting gossypol acetic acid from cottonseed meal in the presence of a solid acid catalyst which is ZrSO4 / HMS solid acid. The ZrSO4 / HMS solid acid catalyst with a loading capacity of 10 to 70 mass percent is prepared by first preparing a hexagonal mesoporous silica (HMS) by using laurylamine as a template agent and then loading ZrSO4 on the HMS molecular sieve. The method comprises: immersing a coarse cottonseed meal sample in acetone aqueous solution serving as a solvent for extraction; and adding 5-percent glacial acetic acid in a volume which is 1 to 3 times that of the obtained solution and ZrSO4 / HMS solid catalyst in an amount which is 1 to 10 percent based on the mass of the solution into the obtained solution, reacting, filtering, crystallizing and purifying to obtain gossypol acetate. The method provided by the invention achieves high gossypol acetate extraction rate and purity and makes technical process simple, and therefore is convenient for industrial production.

Description

technical field [0001] The invention relates to a method for extracting gossypol acetate from cotton dregs, in particular to a method of extracting gossypol acetate with ZrSO 4 / HMS solid acid is a method of extracting gossypol acetate from cotton meal with catalyst. Background technique [0002] Gossypol acetate is a complex salt of gossypol and acetic acid, which is more stable than gossypol, and its molecular formula is C 32 h 34 o 10 . Gossypol acetate is a compound with a wide range of pharmacological effects. It can be used as a male birth control drug with an effective rate of 98%, and as a drug for treating gastric cancer with an effective rate of 63%. It has a good curative effect; gossypol acetate is used as an antioxidant, flame retardant, stabilizer, rodenticide, etc. in industry, and is a very valuable industrial raw material. [0003] Extracting gossypol acetate from cottonseed meal includes: ether-acid method, acetone-acid method, ether-water release meth...

Claims

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Application Information

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IPC IPC(8): C07C53/10C07C51/41C07C47/57C07C45/61C07C45/78
Inventor 朱明远东世宏代斌
Owner 朱明远
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