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Method for preparing gossypol acetate from cottonseed cake, cottonseed meal, or cotton root bark

A technology of gossypol acetate and cottonseed meal, which is applied in the separation/purification of carbonyl compounds, organic chemistry, etc., can solve the problems of toxicity, flammability and explosion, and low extraction rate, and achieve mild operating conditions, less environmental pollution, and high product quality. The effect of high purity

Inactive Publication Date: 2010-07-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Gossypol acetic acid is the medicinal form of gossypol. At present, gossypol acetate is generally prepared by solvent extraction ~ aniline precipitation conversion method. Commonly used extraction solvents include acetone, isopropanol, ethanol, etc., not only the extraction rate is low, The process equipment is complex and costly, and most organic solvents are toxic, pollute the environment, and are flammable and explosive, posing production safety hazards

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1) Weigh 50 grams of cottonseed cake, dry and pulverize it, and weigh another 5 grams of sodium carbonate, and add them to a PM100 planetary ball mill. The ball milling medium is agate balls, and the ratio of medium to material is 1:1 (w / w). The rotating speed is 650 rpm, grinding for 30 minutes;

[0017] 2) Take the ground powder prepared in step 1), use 275 grams of distilled water, extract 3 times under stirring at room temperature, each time for 5 minutes, filter, and combine the filtrates;

[0018] 3) Add glacial acetic acid to the filtrate obtained in step 2), and stir to completely precipitate the crystals to obtain 0.8 g of gossypol acetate crude product.

[0019] 4) Take the gossypol acetate crude product obtained in step 3), and recrystallize it three times with 16 grams of ether to obtain the gossypol acetate fine product.

Embodiment 2

[0021] 1) Weigh 100 grams of cottonseed meal, dry and pulverize it, and then weigh 1 gram of sodium bicarbonate and add it to a 8000D-230 high-energy vibratory mill. The ball milling medium is agate balls, and the medium-to-material ratio is 1:1 (w / w), the rotating speed is 600 rpm, grinding for 3 hours;

[0022] 2) Take the ground powder prepared in step 1), use 5050 grams of distilled water, extract 5 times under stirring at room temperature, each time for 5 minutes, filter, and combine the filtrates;

[0023] 3) Add glacial acetic acid to the filtrate obtained in step 2), and stir to completely precipitate the crystals to obtain 0.6 g of gossypol acetate crude product.

[0024] 4) Take the gossypol acetate crude product obtained in step 3), and recrystallize twice with 15 grams of ether to obtain the gossypol acetate fine product.

Embodiment 3

[0026] 1) Weigh 100 grams of cotton root bark, dry and pulverize it, and weigh another 8 grams of sodium hydroxide, and add it to a GSY-2 stirring ball mill. The ball milling medium is agate balls, and the medium to material ratio is 1:1 (w / w ), the rotating speed is 500 rpm, grinding for 2 hours;

[0027] 2) Take the ground powder prepared in step 1), use 1080 grams of distilled water, extract 3 times under stirring at room temperature, each time for 5 minutes, filter, and combine the filtrates;

[0028] 3) Add glacial acetic acid to the filtrate obtained in step 2), and stir to completely precipitate the crystals to obtain 1.4 grams of gossypol acetate crude product.

[0029] 4) Take the gossypol acetate crude product obtained in step 3), and recrystallize it three times with 32 grams of ether to obtain the gossypol acetate fine product.

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PUM

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Abstract

The invention discloses a method for preparing gossypol acetate from cottonseed cake, cottonseed meal, or cotton root bark. The method comprises the following steps: (1) parching and grinding the cottonseed cake, cottonseed meal, or cotton root bark into the high-energy mill, put grinding auxiliary agent, 1 to 10 wt % of the cottonseed cake, cottonseed meal, or cotton root bark in to the high-energy mill for solid-state grinding. (2) mixing the ground power obtained from step 1 with water, and extracting and filtrating while churning and finally combining the filtrates. (3) putting the filtrate obtained from step 2 into acetic acid, churning for crystallization of the gossypol acetate crude product. (4) recrystalizing the crude product of gossypol acetate obtained through step 3, using aether 20 to 25 times of the weight of gossypol acetate, and finally the refined gossypol acetate is obtained. The invention overcomes the defects of low extraction yield, complicated technological equipments, high cost, non-recyclable menstruum in the existing organic solvent extraction method. The method of the invention is high in extraction yield, simple in process, cheap in equipment investment, moderate in operating condition, friendly to environment and high in purity.

Description

technical field [0001] The invention relates to the field of deep processing and utilization of cotton industry, in particular to a method for preparing gossypol acetate from cottonseed cake, cottonseed meal or cotton root bark. Background technique [0002] Gossypol is a polyphenolic substance widely present in the genus Gossypium. It was used as an anti-fertility drug for men in the early days. Viruses, anti-parasites, etc.; in addition, gossypol and its derivatives also have the effect of killing certain tumor cells, such as cervical cancer, uterine fibroids, ovarian cancer, adrenal cortical cancer, prostate cancer, digestive tract cancer, especially Gastric cancer, etc.; gossypol and its derivatives also show good application prospects in the fields of chemical industry, genetic engineering, rocket fuel, oil drilling, rubber and plastics industry, etc., and their good antioxidant properties and stabilizer effects indicate that gossypol and its derivatives Things have hu...

Claims

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Application Information

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IPC IPC(8): C07C47/57C07C45/78
Inventor 叶瑛夏枚生张路李海晏姚志通戴凌青
Owner ZHEJIANG UNIV
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