CN100447225C - Raw wool treating supercritical CO2 process - Google Patents
Raw wool treating supercritical CO2 process Download PDFInfo
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- CN100447225C CN100447225C CNB2007100109396A CN200710010939A CN100447225C CN 100447225 C CN100447225 C CN 100447225C CN B2007100109396 A CNB2007100109396 A CN B2007100109396A CN 200710010939 A CN200710010939 A CN 200710010939A CN 100447225 C CN100447225 C CN 100447225C
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- extraction
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- raw wool
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
Abstract
The raw wool treating supercritical CO2 process includes the following steps: 1. depurating raw wool; 2. extracting depurated raw wool with supercritical CO2 to obtain lanolin and degreased wool. The supercritical CO2 process has the conditions, including extraction pressure 30-40 MPa, extraction temperature 60-75 deg.c, the first stage separation pressure 9-10 MPa, the first stage separation temperature 45-50 deg.c, the second stage separation pressure 5-6MPa, and the second stage separation temperature 36-42 deg.c. The present invention has simple technological process, high product yield, environment friendship, low cost and high product quality.
Description
Technical field
The present invention relates to the method that a kind of direct processing raw wool extracts refined wool fat and scoured wool, particularly a kind of supercritical CO of using
2Handle the method for raw wool extracting and refining lanolin and scoured wool.
Background technology
Wool is a kind of textile materials of top grade.From the raw wool that chimera shears off, contain 9%～12% lanolin, as the wool of wool textile raw material should be that raw wool is deviate from fat content behind the lanolin and is equal to or less than 1% scoured wool, so should deal with to the raw wool of cutting from chimera, the purpose of handling one is to be equal to or less than 1% scoured wool in order to obtain fat content, can obtain lanolin besides.Lanolin is the comparatively complicated crude substance of a kind of composition, lanolin after refining has good water-absorbent, wettability, film-forming properties, lipophilicity, emulsifying property and dispersiveness, it is non-crystallizable when temperature is low, has germicidal action, nontoxic nonirritant, stronger emulsifying stability is arranged near body temperature and to the perviousness of skin, refined wool fat can be made into multiple derivative through deep processing.Lanolin extensively is used in pharmaceutical industries and cosmetic industry, in addition, lanolin and derivative can also be as rust-preventive agent, and lubricant is used for mechanical industry, be used for papermaking, leather industry as softening agent, machining agent, lanolin is the higher chemical of a kind of economic worth.In the prior art, the method of handling raw wool obtains that fat content is equal to or less than 1% scoured wool and the method for lanolin mainly includes three steps, it at first is 40～50 ℃ water-detergent solution washing raw wool with temperature, raw wool is done skimming treatment, obtain fat content and be equal to or less than 1% scoured wool and a large amount of lanolated wool washing waste water; Isolate degras with isolating method from wool washing waste water then, separation method has methods such as centrifugal separation, foamet, acid cleavage one extraction process, chemical flocculation one extraction process or ultra-filtration membrane partition method; At last degras is made with extra care, obtained refined wool fat, the purified method generally is to take out lanolin with organic solvent extracting earlier, removes free fatty acids, aldehyde, alcohol, residual soap and other impurity again from the lanolin that solvent extraction goes out.The treatment process of this raw wool has following deficiency:
1. the step of handling raw wool is many, and technology is numerous and diverse;
2. make the fat content of washing the back scoured wool be equal to or less than 1% with water-detergent solution washing raw wool and need to consume a large amount of water and washing composition, otherwise the raw wool degreasing is unclean, has the problem that scoured wool after washing is of low quality, waste Freshwater resources and consume a large amount of washing composition with water-detergent solution washing raw wool;
3. a large amount of wool washing waste waters is a high concentrated organic wastewater, wherein mainly contain lanolin and washing composition, also contain wool perspiration simultaneously, the sheep excrement, impurity such as grass bits and silt, lanolin mixes with impurity because of emulsification and saponification are the emulsification suspended state, highly muddy, be difficult to separate, the method yield that extracts degras with above-mentioned separation method from wool washing waste water is low, yield has only 10%～45%, the method complex process that has, the cost height is because yield is low, produce a large amount of waste water that are difficult to reuse after extracting degras, BOD in the waste water, the COD value is higher, difficult treatment, contaminate environment greatly after the discharging;
4. it is low degras to be carried out purified method complex process, cost height, yield, and the refined wool fat that obtains contains the solvent of equal amount, poor product quality.
Summary of the invention
The objective of the invention is in order to overcome above-mentioned deficiency, propose that a kind of technology is simple, water is few, three-waste free discharge, cost are low, refined wool fat yield height, good product quality, wash the low a kind of supercritical CO of back woolen fat content
2Handle the method for raw wool.
The present invention is achieved using the following method.
Supercritical CO
2Handling the woolen method has the following steps:
(1) gets the raw wool of cutting from chimera, remove tangible impurity in the raw wool, obtain the removal of impurities raw wool;
(2) removal of impurities raw wool supercritical CO
2The method of extraction extraction treatment obtains refined wool fat and scoured wool, supercritical CO
2Extraction conditions is: extracting pressure 30～40MPa, 60～75 ℃ of extraction temperature, flash trapping stage pressure 9～10MPa, 45～50 ℃ of flash trapping stage temperature, secondary separating pressure 5～6MPa, 36～42 ℃ of secondary separation temperatures.
Extraction time and extracting pressure, extraction temperature and CO
2Flow relevant, after extracting pressure, extraction temperature were certain, the extraction time was only and CO
2Flow relevant, CO
2Flow big, the time of extraction is few, CO
2Flow little, the time of extraction is many.The extraction time with begin to be extracted into do not have isolate to flow out till, specifically the time of extracting can be selected because of concrete extraction process.
The present invention's supercritical CO
2Method of extraction is handled raw wool, basically only just can obtain scoured wool and refined wool fat with a step, simple, the refined wool fat yield height of technology, water consumption is few, three-waste free discharge, cost are low, the fat content of refined wool fat good product quality, scoured wool is low.Lanolin is the comparatively complicated crude substance of a kind of composition, is a kind of multi-component composition, and the less component of molecular weight is arranged in the lanolin, and the bigger component of molecular weight is also arranged, and uses supercritical CO
2Handle raw wool when separating, can take out different components in the different time.
Below in conjunction with embodiment, the present invention is further described.
Embodiment
Embodiment 1
Supercritical CO
2The method of extraction lanolin has the following steps:
(1) gets the raw wool of cutting from chimera, remove tangible impurity in the raw wool, consider group, sheep excrement agglomerate etc. to be worth doing, obtain the removal of impurities raw wool as earth agglomerate, long careless bar, grass;
(2) be the removal of impurities raw wool supercritical CO of 913Kg to weight
2The method of extraction extraction treatment obtains refined wool fat and fat content 0.5%～0.6% scoured wool, supercritical CO
2Extraction conditions is: extracting pressure 35MPa, and 70 ℃ of extraction temperature, flash trapping stage pressure 9.5MPa, 47.5 ℃ of flash trapping stage temperature, secondary separating pressure 5.5MPa, 39 ℃ of secondary separation temperatures obtain refined wool fat 110Kg.
Embodiment 2
Supercritical CO
2The method of extraction lanolin has the following steps:
(1) with step (1) among the embodiment 1
(2) supercritical CO
2Extraction conditions is: extracting pressure 32.5MPa, and 65 ℃ of extraction temperature, flash trapping stage pressure 9.25MPa, 46.5 ℃ of flash trapping stage temperature, secondary separating pressure 5.25MPa, 37.5 ℃ of secondary separation temperatures, other is with step (2) among the embodiment 1.
Embodiment 3
Supercritical CO
2The method of extraction lanolin has the following steps:
(1) with step (1) among the embodiment 1
(2) supercritical CO
2Extraction conditions is: extracting pressure 37.5MPa, and 67.5 ℃ of extraction temperature, flash trapping stage pressure 9.75MPa, 48.5 ℃ of flash trapping stage temperature, secondary separating pressure 5.75MPa, 40.5 ℃ of secondary separation temperatures, other is with step (2) among the embodiment 1.
Lanolin is the comparatively complicated crude substance of a kind of composition, it is a kind of multi-component composition, having in low temperature, low pressure in the lanolin is leachable component, also have in the just leachable component of high temperature, high pressure, low temperature, low pressure are that leachable component is a light constituent, in high temperature, the leachable component of high pressure ability is heavy constituent, uses supercritical CO
2When method of extraction was handled raw wool, light constituent can separate out when temperature and pressure is low, and heavy constituent need just to separate out when temperature and pressure is higher.Using supercritical CO
2When method of extraction was handled raw wool, for energy-conservation and reduce cost, extraction conditions can be with the method that heats up and/or boost piecemeal piecemeal.
The method of temperature programming and programmed pressure is a plurality of sections before and after the extraction time is divided into from start to end, and the following upper limit that is limited to from the invention scheme also correspondingly is divided into the front and back plurality of sections respectively extraction temperature and extracting pressure, is using supercritical CO
2When method of extraction is handled raw wool, make temperature and pressure heat up piecemeal from front to back, boost on a time period.The extraction time can be by the selected extraction time of the selected explanation of above-mentioned extraction time.
The extraction time period can be impartial plurality of sections, also can be unequal plurality of sections, in the ratio of light constituent in the lanolin and heavy constituent, can find out best segmentation at an easy rate.
Embodiment 4
Supercritical CO
2The method of extraction lanolin has the following steps:
(1) with step (1) among the embodiment 1
(2) supercritical CO
2Extraction conditions is: the extraction time average is divided into three sections, extracting pressure, flash trapping stage pressure, secondary separating pressure, extraction temperature, flash trapping stage temperature and the secondary separation temperature following upper limit that is limited to from the invention scheme also correspondingly is divided into three sections respectively, heat up piecemeal on a time period, boost, other is with step (2) among the embodiment 1.
Lanolin is the comparatively complicated crude substance of a kind of composition, is a kind of multi-component composition, in order to improve extraction efficiency, is using supercritical CO
2When method of extraction is handled raw wool, can be at supercritical CO
2Add a spot of entrainment agent in the extraction agent, entrainment agent can be ethanol, ether equal solvent, CO
2The ratio of weight rate and the weight rate of entrainment agent be 20～50: 1.
Embodiment 5
Supercritical CO
2The method of extraction lanolin has the following steps:
(1) with step (1) among the embodiment 1
(2) supercritical CO
2Extraction conditions is: at supercritical CO
2Add ethanol, ether equal solvent in the extraction agent, CO
2The ratio of weight rate and the weight rate of entrainment agent be 20～50: 1, other is with step (2) in embodiment 1,2,3 or 4.
Claims (6)
1. supercritical CO
2Handle the method for raw wool, comprise and get the raw wool of cutting from chimera, remove tangible impurity in the raw wool, obtain the removal of impurities raw wool; It is characterized in that: also have the following steps: removal of impurities raw wool supercritical CO
2The method of extraction extraction treatment obtains refined wool fat and scoured wool, supercritical CO
2Extraction conditions is: extracting pressure 30～40MPa, 60～75 ℃ of extraction temperature, flash trapping stage pressure 9～10MPa, 45～50 ℃ of flash trapping stage temperature, secondary separating pressure 5～6MPa, 36～42 ℃ of secondary separation temperatures.
2. by the described supercritical CO of claim 1
2Handle the method for raw wool, it is characterized in that: described supercritical CO
2Extraction conditions is: extracting pressure 35MPa, 70 ℃ of extraction temperature, flash trapping stage pressure 9.5MPa, 47.5 ℃ of flash trapping stage temperature, secondary separating pressure 5.5MPa, 39 ℃ of secondary separation temperatures.
3. by the described supercritical CO of claim 1
2Handle the method for raw wool, it is characterized in that: described supercritical CO
2Extraction conditions is: extracting pressure 32.5MPa, 65 ℃ of extraction temperature, flash trapping stage pressure 9.25MPa, 46.5 ℃ of flash trapping stage temperature, secondary separating pressure 5.25MPa, 37.5 ℃ of secondary separation temperatures.
4. by the described supercritical CO of claim 1
2Handle the method for raw wool, it is characterized in that: described supercritical CO
2Extraction conditions is: extracting pressure 37.5MPa, 67.5 ℃ of extraction temperature, flash trapping stage pressure 9.75MPa, 48.5 ℃ of flash trapping stage temperature, secondary separating pressure 5.75MPa, 40.5 ℃ of secondary separation temperatures.
5. by the described supercritical CO of claim 1
2Handle the method for raw wool, it is characterized in that: described supercritical CO
2Extraction conditions is: the extraction time is divided into plurality of sections from start to end, extracting pressure and extraction temperature under be limited to the upper limit and also correspondingly be divided into plurality of sections respectively, heat up piecemeal on a time period, boost.
6. by claim 1,2,3,4 or 5 described supercritical COs
2Handle the method for raw wool, it is characterized in that: described supercritical CO
2Extraction conditions is: at supercritical CO
2Add ethanol or ether, CO in the extraction agent
2The ratio of weight rate and the weight rate of ethanol or ether be 20～50: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100109396A CN100447225C (en) | 2007-04-13 | 2007-04-13 | Raw wool treating supercritical CO2 process |
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| CNB2007100109396A CN100447225C (en) | 2007-04-13 | 2007-04-13 | Raw wool treating supercritical CO2 process |
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| CN100447225C true CN100447225C (en) | 2008-12-31 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329694A (en) * | 2011-08-31 | 2012-01-25 | 朱新亮 | Wool grease low-temperature extraction process |
| CN102674503B (en) * | 2012-04-23 | 2014-01-29 | 西安交通大学 | Wool-washing wastewater treatment method by coupling ultrasonic demulsification and supercritical water oxidation |
| CN105386133A (en) * | 2014-06-30 | 2016-03-09 | 耿云花 | Preparation method of cotton stalk bark fiber |
| CN110511829A (en) * | 2019-09-12 | 2019-11-29 | 大连工业大学 | One kind being suitable for super (Asia) critical CO2Hair detergent and using one bath segmentation scouring of wool method |
| CN110528089B (en) * | 2019-09-12 | 2022-02-18 | 大连工业大学 | Super (sub) critical CO2 wool scouring method |
| CN110541202B (en) * | 2019-09-12 | 2021-12-03 | 大连工业大学 | Tunnel type supercritical (subcritical) CO2Waterless wool washing method |
| CN112251938A (en) * | 2020-10-12 | 2021-01-22 | 贵州航天乌江机电设备有限责任公司 | Method for supercritical cleaning and drying duck feather |
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| CN1390150A (en) * | 1999-10-21 | 2003-01-08 | 拉维药物实验室有限公司 | Method for fractionating raw material comprising several constituents using supercritical pressure solvent |
| EP1201736B1 (en) * | 1999-07-09 | 2005-04-27 | Consejo Superior De Investigaciones Cientificas | Compositions of internal lipid extract of wool and use thereof in the preparation of products for skin care and treatment |
| CN1772856A (en) * | 2004-11-08 | 2006-05-17 | 浙江霸力（鞋业）集团有限公司 | Technological process of extracting and recovering lanoline from un-degreased wool |
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2007
- 2007-04-13 CN CNB2007100109396A patent/CN100447225C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1201736B1 (en) * | 1999-07-09 | 2005-04-27 | Consejo Superior De Investigaciones Cientificas | Compositions of internal lipid extract of wool and use thereof in the preparation of products for skin care and treatment |
| CN1390150A (en) * | 1999-10-21 | 2003-01-08 | 拉维药物实验室有限公司 | Method for fractionating raw material comprising several constituents using supercritical pressure solvent |
| CN1772856A (en) * | 2004-11-08 | 2006-05-17 | 浙江霸力（鞋业）集团有限公司 | Technological process of extracting and recovering lanoline from un-degreased wool |
Non-Patent Citations (4)
| Title |
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| 用超临界CO2处理羊毛回收羊毛脂的研究. 修国华，金革，斋藤功夫.沈阳化工学院学报，第9卷第4期. 1995 |
| 用超临界CO2处理羊毛回收羊毛脂的研究. 修国华，金革，斋藤功夫.沈阳化工学院学报，第9卷第4期. 1995 * |
| 超临界萃取技术及其在日用化工中的应用. 陈立军，沈慧芳，黄洪，黎永津，陈焕钦.日用化学化工，第34卷第5期. 2004 |
| 超临界萃取技术及其在日用化工中的应用. 陈立军，沈慧芳，黄洪，黎永津，陈焕钦.日用化学化工，第34卷第5期. 2004 * |
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