CN102942992A - Technique for simultaneously extracting lipid and gossypol from cotton seed - Google Patents
Technique for simultaneously extracting lipid and gossypol from cotton seed Download PDFInfo
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- CN102942992A CN102942992A CN2012105206444A CN201210520644A CN102942992A CN 102942992 A CN102942992 A CN 102942992A CN 2012105206444 A CN2012105206444 A CN 2012105206444A CN 201210520644 A CN201210520644 A CN 201210520644A CN 102942992 A CN102942992 A CN 102942992A
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Abstract
The invention belongs to the technical field of processing of oil-bearing crops, and particularly relates to a technique for simultaneously extracting lipid and gossypol from cotton seed. The invention provides a clean production technique for processing cotton seed, which has the advantages of great convenience, high efficiency, low cost and is easy to operate and control; and the existing cotton seed leaching plant can be slightly reconstructed to implement industrialized large-scale production of simultaneously extracting cotton oil and gossypol from cotton seed as well as coproduction of detoxified cotton seed protein. Compared with the prior art, by utilizing mixed solvent technology and ethanol secondary leaching technology, the technique can reduce the consumption of the No.6 solvent by 30-60%, and greatly reduce the requirement and dependence of the grease processing industry for the petroleum product; the technique can obtain high-quality gossypol and phospholipid on the premise of not generating wastewater, thereby eliminating a large pollution source of cotton seed processing industry; and meanwhile, the technique can enhance the yield of cotton oil, gossypol and detoxified cotton seed protein by 3-5%, and greatly lower the production cost, thereby having wide application prospects in the field of cotton seed processing.
Description
Technical field
The invention belongs to the processing technique field of oil crops, is to belong to a kind of technique of extracting simultaneously lipid and gossypol from cottonseed specifically.
Background technology
Cottonseed is the by product of Cotton Production, one of large vegetable oil material resource of China.The cottonseed grease and the cottonseed protein that wherein contain high-quality, and valuable medicinal raw material gossypol.Take cottonseed as raw material, can the processing Oleum Gossypii semen, the multiple product such as cottonseed protein, gossypol.But because gossypol has the toxicity that can cause male sterility, thereby Oleum Gossypii semen and cottonseed protein must thoroughly remove gossypol, otherwise can cause poisoning before edible or feed as Nonruminantia animals such as pig, chickens.
Existing cottonseed processing technique is with No. 6 solvents cottonseed to be leached extracting, obtains Oleum Gossypii semen and cotton dregs, and then with thermal treatment, add the methods such as molysite cotton dregs carried out detoxification treatment, cotton dregs are changed into can be for use as the cottonseed protein of feed.
No. 6 used in this technique solvent through-stone olein heat up in a steamer product, from crude oil, be necessary to use from renewable resources, and security is unquestionable, the low-carbon (LC) alcohols partly or entirely substitute, to reduce the dependence to oil.
Summary of the invention
This patent has been invented a kind of technique of extracting simultaneously lipid and gossypol from cottonseed.Comparatively unique is, it by No. 6 solvent/low-carbon alcohol type mixed solvents utilization and to the regulation and control of the concentration of used low-carbon alcohol, the separation-extraction technology of Cottonseed phenol organically has been integrated in the extraction process of separation and Extraction Oleum Gossypii semen from cottonseed, has realized obtaining simultaneously from cottonseed the purpose of Oleum Gossypii semen, detoxicated cottonseed protein and gossypol.Operate according to this patent, compare with traditional method before this, can not reduce wherein arbitrary product, Oleum Gossypii semen, detoxicated cottonseed protein or gossypol, the prerequisite of productive rate under, the other two kinds of products of the acquisition of high-quality high yield.This is vital for the comprehensive utilization of the large oil crops resource with a very important position in the national economy for cottonseed in this improvement, the efficient utilization of resource rate is greatly increased, greatly improve the degree of utilizing of oil resource, increase utility value.
One of most important purpose of the present invention, to solve exactly detoxication of cotton seeds serialization, clean and environmental friendliness, making cottonseed protein can be the available feed protein resource of crossing without any other processing.As a result along band, another object of the present invention is to realize that cottonseed leaches the part renewable resources problem with solvent, alleviating the dependence to oil, and reduces production costs, and guarantees quality product.
Specifically, at first, we find that cottonseed leaches resulting wet cotton dregs through No. 6 solvent/low-carbon alcohol type mixed solvents, from different through No. 6 resulting wet cotton dregs of solvent extraction, have good low-carbon alcohol solution wettable/perviousness, can directly carry out extracting gossypol with low-carbon alcohol is that the purpose secondary leaches, and needn't be in advance with solvent removal.Under the secondary extract technology condition that we take, low-carbon alcohol can cement out mixed solvent replacing whole residual in the cotton dregs that wet, and can be under suitable condition and the mixed solvent AUTOMATIC ZONING, thereby can not cause disadvantageous effect to the technological process that mixed solvent leaches cottonseed.Established thus with No. 6 solvent/low-carbon alcohol type mixed solvents and low-carbon alcohol solution and leached continuously with continuation method, from cottonseed, extracted simultaneously the basis of lipid and gossypol.
Secondly, we find that the low carbon alcohol solution with suitable concentration leaches resulting wet cotton dregs as solvent to No. 6 solvent/low-carbon alcohol type mixed solvents and carries out cold soaking, can under the prerequisite that keeps the basic unchangeability of cottonseed protein, effectively wherein contained gossypol and pure dissolubility pigment isopolarity component be extracted, the indexs such as color and luster, smell, protein content, function quality and security of gained cottonseed protein concentrate are significantly improved.
We find that in extracting the Extraction techniques such as solvent, extraction time, extraction temperature and solid-liquid ratio, extracting times, it is of paramount importance extracting the composition of solvent and extracting temperature for extraction effect.Wherein, mixed solvent leaches used mixed solvent and should be comprised of normal hexane (or No. 6 solvents) and the low carbon alcohol solution ratio according to 1: 0.01～100 (v/v), used low-carbon alcohol can be methyl alcohol, also can be ethanol, the concentration of low-carbon alcohol should be 70%～100% (w/w) in its aqueous solution.Immersion extracting should be at 30～78 ℃, preferably 45～68 ℃, 0.01～1.0MPa, condition under carry out; The amount of each required mixed solvent of immersion extracting should be the 10%-500% (w/v) of the cottonseed material quantity of throwing in, and the time of soaking extraction should be 0.15～12hr time
-1, extracting times should be 6-25 time; The concentration of the used low-carbon alcohol of low-carbon alcohol secondary immersion extracting should be 30%～100% (w/w); The secondary immersion extracting is at 0～78 ℃, preferably 4～38 ℃, 0.01～1.0MPa, condition under carry out; The amount of each required low-carbon alcohol of immersion extracting should be the 10%-500% (w/v) of the cottonseed material quantity of throwing in, and the time of soaking extraction should be 0.15～12hr time
-1, extracting times should be 1-10 time; Used cottonseed can be through the cotton benevolence sheet of the shelling of temperature adjustment modifier treatment, also can be through the cotton benevolence of the shelling of puffing.Solid-liquid separation can be that filtering separation, centrifugation or screw press separate; Solvent recuperation is processed should be at 30～180 ℃, preferably 50～125 ℃, 0.01～1.0MPa, condition under carry out, can do thermal source with indirect steam, open steam or hot nitrogen.
Embodiment
Following example will specify working method of the present invention, but can not be as limitation of the invention.
Example one
1000g is added in the leacher through the cotton benevolence sheet of the shelling of temperature adjustment modifier treatment, the mixed solvent that the aqueous ethanolic solution that adds 2500ml and by normal hexane and concentration be 89% (v/v) forms according to 4: 1 ratio, at 60 ℃ of lower 120min that soak, then leach leach liquor, obtain mixing oil.Adding 2500ml concentration in the wet degreasing face dregs of rice after the filtering leach liquor is the aqueous ethanolic solution of 65% (v/v), soaks 120min under 60 ℃ again, then leaches leach liquor, obtains ethanol extract and wet degreasing detoxification cotton dregs.
Mixing oil is put on the Rotary Evaporators, and 60 ℃, reclaim mixed solvent under the 1kPa to solvent-free distillating, obtain the 38g crude cotton seed oil.The ethanol extract is put on the Rotary Evaporators, and 60 ℃, Recycled ethanol obtains 10g brown syrup to solvent-free distillating under the 1kPa.After testing, gossypol content has wherein reached more than 70%, can be used as gossypol and sells.Wet degreasing detoxification cotton dregs are put in the vacuum drying oven 60 ℃, and dry 14h under the 1kPa obtains color and luster and is white, and content is 73% detoxicated cottonseed protein.
Example two
1000g is added in the leacher through the cotton benevolence of the shelling of puffing, the mixed solvent that the methanol aqueous solution that adds 2000ml and by normal hexane and concentration be 90% (v/v) forms according to 1: 1 ratio, at 60 ℃ of lower 120min that soak, then leach leach liquor, obtain mixing oil.Adding 2500ml concentration in the wet defatted cotton dregs after the filtering leach liquor is the methanol aqueous solution of 70% (v/v), soaks 120min under 60 ℃ again, then leaches leach liquor, obtains methyl alcohol extract and wet degreasing detoxification cotton dregs.
Mixing oil is put on the Rotary Evaporators, and 60 ℃, reclaim mixed solvent under the 1kPa to solvent-free distillating, obtain the 39.8g crude cotton seed oil.The methyl alcohol extract is put on the Rotary Evaporators, and 60 ℃, reclaim methyl alcohol under the 1kPa to solvent-free distillating, obtain 10.6g brown syrup.After testing, gossypol content has wherein reached more than 70%, can be used as gossypol and sells.Wet degreasing detoxification cotton dregs are put in the vacuum drying oven 60 ℃, and dry 14h under the 1kPa obtains color and luster and is white, and content is 75% detoxicated cottonseed protein.
Example three
1000g is added in the leacher through the cotton benevolence of the shelling of puffing, the mixed solvent that the aqueous ethanolic solution that adds 3000ml and by normal hexane and concentration be 86% (v/v) forms according to 3: 1 ratio, at 60 ℃ of lower 120min that soak, then leach leach liquor, obtain mixing oil.Adding 2000ml concentration in the wet defatted soybean meal after the filtering leach liquor is the aqueous ethanolic solution of 70% (v/v), soaks 120min under 60 ℃ again, then leaches leach liquor, obtains ethanol extract and wet degreasing detoxification cotton dregs.
Mixing oil is put on the Rotary Evaporators, and 60 ℃, reclaim mixed solvent under the 1kPa to solvent-free distillating, obtain the 37.8g crude cotton seed oil.The ethanol extract is put on the Rotary Evaporators, and 60 ℃, Recycled ethanol obtains 11.2g brown syrup to solvent-free distillating under the 1kPa.After testing, gossypol content has wherein reached more than 70%, can be used as gossypol and sells.Wet degreasing detoxification cotton dregs are put in the vacuum drying oven 60 ℃, and dry 14h under the 1kPa obtains color and luster and is white, and content is 70% detoxicated cottonseed protein.
Claims (9)
1. technique of from cottonseed, extracting simultaneously lipid and gossypol.This technique is comprised of the following step:
1) with mixed solvent cottonseed is carried out immersion extracting, extraction of lipid contained in the cottonseed in solvent, is then carried out solid-liquid separation, obtain mixing oil and wet defatted cotton dregs;
2) mixing oil is processed through solvent recuperation, obtains Oleum Gossypii semen.The solvent cycle that recovery obtains is used;
3) with low-carbon alcohol wet defatted cotton dregs is carried out the secondary immersion extracting, gossypol extracting contained in the cottonseed in low-carbon alcohol, is then carried out solid-liquid separation, obtain low-carbon alcohol extract and wet degreasing detoxification cotton dregs;
4) wet degreasing detoxification cotton dregs are processed through solvent recuperation, obtain detoxicated cottonseed protein.The solvent cycle that recovery obtains is used;
5) the low-carbon alcohol extract is processed through solvent recuperation, obtains gossypol.The solvent cycle that recovery obtains is used.
2. the technique of extracting simultaneously lipid and gossypol from cottonseed as claimed in claim 1 is characterized in that the mixture that described mixed solvent is comprised of according to the ratio of 1: 0.01～100 (v/v) a kind of non-polar solvent and low carbon alcohol solution.Non-polar solvent wherein can be normal hexane or No. 6 solvents, and low-carbon alcohol can be methyl alcohol, also can be ethanol, and the concentration of low-carbon alcohol is 70%～100% (w/w) in its aqueous solution.
3. the technique of extracting simultaneously lipid and gossypol from cottonseed as claimed in claim 1 is characterized in that described cottonseed can be through the cotton benevolence sheet of the shelling of temperature adjustment modifier treatment, also can be through the cotton benevolence of the shelling of puffing.
4. the technique of from cottonseed, extracting simultaneously lipid and gossypol as claimed in claim 1, it is characterized in that described immersion extracting is at 30～78 ℃, preferably 45～68 ℃, 0.01～1.0MPa, condition under carry out 6-25 time, the amount of each required mixed solvent of immersion extracting is the 10%-500% (w/v) of institute's input cottonseed material quantity, and the time of immersion extraction is 0.15～12 hr time
-1
5. the technique of extracting simultaneously lipid and gossypol from cottonseed as claimed in claim 1 is characterized in that described low-carbon alcohol is that concentration is the methyl alcohol of 30%～100% (w/w), or ethanol, the aqueous solution.
6. the technique of from cottonseed, extracting simultaneously lipid and gossypol as claimed in claim 1, it is characterized in that described secondary immersion extracting is at 0～78 ℃, preferably 4～38 ℃, 0.01～1.0MPa, condition under carry out 1-10 time, the amount of each required low-carbon alcohol of immersion extracting is the 10%-500% (w/v) of institute's input cottonseed material quantity, and the time of immersion extraction is 0.15～12 hr time
-1
7. the technique of extracting simultaneously lipid and gossypol from cottonseed as claimed in claim 1 is characterized in that described solid-liquid separation can be that filtering separation, centrifugation or screw press separate.
8. the technique of from cottonseed, extracting simultaneously lipid and gossypol as claimed in claim 8, it is characterized in that described solvent recuperation processing means that heating makes solvent evaporation, then the process that reclaims of condensation, used thermal barrier can be indirect steam, open steam or hot nitrogen.
9. the technique of extracting simultaneously lipid and gossypol from cottonseed as claimed in claim 1 is characterized in that described solvent recuperation processes at 30～180 ℃, preferably 50～125 ℃, 0.01～1.0MPa, condition under carry out.
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Cited By (8)
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| CN103265611A (en) * | 2013-04-27 | 2013-08-28 | 武汉工业学院 | Method for dephenolization and saccharide removal of cottonseed and synchronous enrichment of protein |
| CN103725421A (en) * | 2013-09-25 | 2014-04-16 | 山东渤海实业股份有限公司 | Method for increasing utilization rate of cottonseed oil mixture refining by-products |
| CN104673484A (en) * | 2015-01-28 | 2015-06-03 | 安徽嘉旗粮油工程技术有限公司 | Production method for synchronously extracting cottonseed oil and degossypolized cottonseed protein from cottonseed germ flakes |
| CN105693488A (en) * | 2016-03-18 | 2016-06-22 | 江南大学 | Clean production process for high purity gossypol |
| CN105861160A (en) * | 2016-04-21 | 2016-08-17 | 武汉轻工大学 | Continuous producing method for recovering grease from vegetable oil spent bleaching clay |
| CN107011411A (en) * | 2017-04-28 | 2017-08-04 | 济南中棉生物科技有限公司 | A kind of cottonseed protein production method that can extract a variety of byproducts |
| CN112552371A (en) * | 2020-12-24 | 2021-03-26 | 常州市芙丽佳生物科技有限公司 | Method for preparing olive kernel extract based on extraction and purification technology |
| CN115651750A (en) * | 2022-09-21 | 2023-01-31 | 新疆冠农果茸股份有限公司 | Preparation method of cottonseed mixed oil |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265611A (en) * | 2013-04-27 | 2013-08-28 | 武汉工业学院 | Method for dephenolization and saccharide removal of cottonseed and synchronous enrichment of protein |
| CN103265611B (en) * | 2013-04-27 | 2014-12-24 | 武汉工业学院 | Method for dephenolization and saccharide removal of cottonseed and synchronous enrichment of protein |
| CN103725421A (en) * | 2013-09-25 | 2014-04-16 | 山东渤海实业股份有限公司 | Method for increasing utilization rate of cottonseed oil mixture refining by-products |
| CN103725421B (en) * | 2013-09-25 | 2015-07-15 | 山东渤海实业股份有限公司 | Method for increasing utilization rate of cottonseed oil mixture refining by-products |
| CN104673484A (en) * | 2015-01-28 | 2015-06-03 | 安徽嘉旗粮油工程技术有限公司 | Production method for synchronously extracting cottonseed oil and degossypolized cottonseed protein from cottonseed germ flakes |
| CN105693488A (en) * | 2016-03-18 | 2016-06-22 | 江南大学 | Clean production process for high purity gossypol |
| CN105861160A (en) * | 2016-04-21 | 2016-08-17 | 武汉轻工大学 | Continuous producing method for recovering grease from vegetable oil spent bleaching clay |
| CN107011411A (en) * | 2017-04-28 | 2017-08-04 | 济南中棉生物科技有限公司 | A kind of cottonseed protein production method that can extract a variety of byproducts |
| CN107011411B (en) * | 2017-04-28 | 2020-12-18 | 济南中棉生物科技有限公司 | Cottonseed protein production method capable of extracting multiple byproducts |
| CN112552371A (en) * | 2020-12-24 | 2021-03-26 | 常州市芙丽佳生物科技有限公司 | Method for preparing olive kernel extract based on extraction and purification technology |
| CN115651750A (en) * | 2022-09-21 | 2023-01-31 | 新疆冠农果茸股份有限公司 | Preparation method of cottonseed mixed oil |
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Application publication date: 20130227 |