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Method of extracting gossypol acetate from cotton seed oil niger

A technology of cotton oil soapstock and gossypol acetate, which is applied in the separation/purification of carbonyl compounds, organic chemistry and other directions to achieve the effects of reducing pollution, small demand and reducing the pressure of purification

Inactive Publication Date: 2007-08-15
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a method for extracting gossypol acetate from cotton oil soapstock of cottonseed processing waste, which can prepare high-purity medicinal gossypol acetate quickly and with low pollution, and reduce the extraction solvent needs, simplify the production process, and reduce product costs

Method used

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  • Method of extracting gossypol acetate from cotton seed oil niger
  • Method of extracting gossypol acetate from cotton seed oil niger

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Weigh 100 grams of oil factory cotton oil soapstock with a balance and add it to 100 grams, adjust its acidity to 0.1mol.L with sulfuric acid -1 in methanol solution, stirred evenly, placed in ultrasonic extraction equipment with a power of 50W, ultrasonically extracted for 5 minutes, heated and refluxed in a water bath for 30 minutes, cooled to room temperature, centrifuged at 3000 rpm for 20 minutes, and washed with 2 times Wash the aqueous phase three times with methanol in the volume of the cooling liquid, collect the organic phase, and concentrate to the original 1 / 3 volume in a rotary evaporator at a vacuum of 0.08Mpa, then add 1 / 6 volume of glacial acetic acid to the concentrated solution, Simultaneously in the ultrasonic equipment of 100W, induced crystallization 3 minutes, after decompression suction filtration, normal hexane washing and drying, obtain 0.87 gram product, its infrared spectrogram and ultraviolet scan collection of illustrative plates are consiste...

Embodiment 2

[0024] Weigh 100 grams of protein factory cotton oil soap stock with a balance and add it to 500 grams, adjust its acidity to 0.5mol.L with phosphoric acid -1 In the ethanol solution, stir evenly, place in an ultrasonic extraction equipment with a power of 100W, after ultrasonic extraction for 10 minutes, heat and reflux in a water bath for 80 minutes, cool to room temperature, centrifuge at 3000 rpm for 20 minutes, and use 2 times Wash the aqueous phase three times with the ethanol volume of the cooling liquid, collect the organic phase, and concentrate it to the original 1 / 3 in the rotary evaporator under the vacuum degree of 0.08Mpa, then add 1 / 4 volume of glacial acetic acid to the concentrated solution, Simultaneously in the ultrasonic equipment of 100W, induced crystallization 5 minutes, after decompression suction filtration, normal hexane washing and drying, obtain 1.07 gram product, its infrared spectrogram and ultraviolet scanning collection of illustrative plates are...

Embodiment 3

[0026] Weigh 100 grams of oil factory cotton oil soap stock with a balance and add it to 1000 grams, adjust its acidity to 1.0mol.L with nitric acid -1Diethyl ether solution, stirred evenly, placed in ultrasonic extraction equipment with a power of 200W, ultrasonically extracted for 20 minutes, heated and refluxed in a water bath for 100 minutes, cooled to room temperature, centrifuged at 3000 rpm for 20 minutes, and washed with 2 times Wash the aqueous phase three times with diethyl ether in the volume of the cooling liquid, collect the organic phase, and concentrate it in a rotary evaporator under 0.08Mpa until the volume is 1 / 3 of the original volume, then add 1 / 3 of the volume of glacial acetic acid to the concentrated solution, Simultaneously, crystallization was induced in a 200W ultrasonic device for 8 minutes, and after vacuum filtration, n-hexane washing and drying, 0.94 g of product was obtained, and its infrared spectrum and ultraviolet scanning spectrum were consist...

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Abstract

The invention discloses an extracting method of gossypol acetate from cotton seed oil soap stock, which comprises the following steps: dissolving cotton seed oil soap stock into organic acid solvent; transmitting into ultrasonic equipment to do ultrasonic extraction; heating to reflux; centrifuging; separating; decompressing; condensing; acidifying through acetic acid; inducing to crystallize through ultrasound; sucking to obtain the product as yellow crystal with melting point (mp) at 171-178 deg.c; displaying the consistent ultraviolet adsorption spectrum and infrared spectrum with standard mass completely; testing the most ultraviolet adsorption of gossypol acetate at 365nm through VIA method with content at 80-95% and receiving rate at 1-3%.

Description

technical field [0001] The invention relates to a method for extracting gossypol acetate, in particular to a method for extracting gossypol acetate from cotton oil soapstock. Background technique [0002] Gossypol, also known as gossypol or gossypol, is a yellow polyphenol pigment formed in cotton plants, with a high content in cottonseed. When processing cottonseed protein or refining cottonseed oil, in order to reduce the content of free fatty acids, phospholipids, pigments and gossypol in the product and improve the quality of the product, dilute lye is often added during the production process for refining. During alkali refining, all the gossypol in cottonseed oil enters the soapstock, and is easily converted into various dark-colored compounds under alkaline conditions, thus turning the soapstock into dark brown. Cotton oil soapstock is usually discarded as waste, causing a certain degree of environmental pollution. However, the content of gossypol in cotton oil soap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/57C07C45/78
Inventor 吴道澄贾光锋徐梁
Owner XI AN JIAOTONG UNIV
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