CN102226132A - Method for extracting lanolin from wool scouring wastewater - Google Patents

Method for extracting lanolin from wool scouring wastewater Download PDF

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Publication number
CN102226132A
CN102226132A CN2011101197441A CN201110119744A CN102226132A CN 102226132 A CN102226132 A CN 102226132A CN 2011101197441 A CN2011101197441 A CN 2011101197441A CN 201110119744 A CN201110119744 A CN 201110119744A CN 102226132 A CN102226132 A CN 102226132A
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China
Prior art keywords
lanolin
solution
mud
alkane
washing
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CN2011101197441A
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Chinese (zh)
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CN102226132B (en
Inventor
肖俊伟
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ZHANGJIAGANG YUXIN WOOL INDUSTRY CO LTD
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ZHANGJIAGANG YUXIN WOOL INDUSTRY CO LTD
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Publication of CN102226132A publication Critical patent/CN102226132A/en
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/74Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

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  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention relates to a method for extracting lanolin from wool scouring wastewater/sludge, which comprises the following steps: drying the wool scouring wastewater/sludge with hot air until the moisture content of sludge is lower than 15%; extracting lanolin in the sludge by using petroleum ether, alkane or halogenated alkane, and filtering to obtain an extracting solution, wherein the amount of the extractant is 4-5 times of sludge by weight; adding 5 wt% sulfuric acid which accounts for 2-3% of the extracting solution by volume, stirring for 30 minutes while keeping the temperature of 60-70 DEG C, standing for 1 hour, taking the supernatant solution, adding a solution containing 15 wt% of ethanol and 3 wt% of sodium hydroxide (the volume of the solution is twice as that of the sulfuric acid), stirring for 30 minutes while keeping the temperature of 60-70 DEG C, standing for 1 hour, and taking the supernatant solution; washing with equivalent volume of 50 wt% ethanol solution; and evaporating under reduced pressure to remove the extractant in the solution. All the solvents can be recycled, and the lanolin is extracted from sludge, thereby reducing the treatment load of three wastes and increasing the utilization ratio of the lanolin resource.

Description

Extract the method for lanolin in the waste water from washing wool mud
Technical field
The present invention relates to the Treatment of Wastewater from Wool Washing field, relate in particular to the method for extracting lanolin in a kind of waste water from washing wool mud.
Background technology
Lanolin is the smegma thing of sheep, and it is deposited on the wool fiber, can soft wool and the influence of resisting outside poor environment.From physical properties, it is wax rather than fat; From chemical property, it does not contain glycerine, and is different with common animal-plant oil.Lanolin is the multicomponent mixture of Ester, can reclaim from wash wool liquid and gets.Degras is a kind of brown, dope frowzy, and refining back is yellow butyrous thickness body of paste.Lanolin mainly is the lipid acid (C by higher molecular weight 7-C 14) with the Fatty Alcohol(C12-C14 and C12-C18) (C of equivalent roughly 12-C 36), sterol, formed esters such as trimethylammonium sterol contain a spot of free acid, free alcohol and alkane and undetermined thing in addition.According to the sheep kind, weather and raising condition difference, the composition of lanolin is also different.
Separablely from lanolin go out more than 180 kind of lipid acid, three classes of kind more than 70 (Fatty Alcohol(C12-C14 and C12-C18), sterol, trimethylammonium sterol) Fatty Alcohol(C12-C14 and C12-C18).Lanolin is separated or modification, can obtain many valuable expensive goods, as emulsifying agent, wetting Agent for Printing Inks, lubricant, the spread-coating agent, permeate agent, solubilizing agent, skin-care agents etc. are widely used in makeup, medicine, leather, metal rust preventing, aspects such as gardens.Especially makeup and medical aspect, have other products to be difficult to the alternate special performance.Single with regard to makeup, account for about 40% of whole makeup with the prescription of its matrix, and also had very big growth momentum.Therefore, lanolin has the title of " soft gold " in the world.
The fusing point 38-42 of lanolin ℃. it is water-soluble hardly, but can absorb the moisture that is equivalent to 2 times of own wts, is soluble in ether, benzene, chloroform, acetone and sherwood oil are insoluble in cold alcohol, but dissolve in hot ethanol.How to come from waste water from washing wool, to extract lanolin at present according to physics, the chemical property of lanolin, method has mechanical centrifuging, acid to split method, coagulant sedimentation etc., but according to statistics, the rate of recovery of lanolin only is raw wool butyraceous 40-50%, and people have ignored the yolk that remains 40-50% after waste water from washing wool carries out pre-treatment dosing flocculation usually in the mud that obtains.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, and the method for extracting lanolin is provided in a kind of waste water from washing wool mud, and this method technology is simple and improved the lanolin efficiency of resource.
For achieving the above object, the technical solution used in the present invention is:
Extract the method for lanolin in a kind of waste water from washing wool mud, mud refers to wool waste water from washing wool isolated wet mud after traditional dosing flocculation treatment, the present invention includes following steps:
1) waste water from washing wool mud, with warm air drying to the moisture content of mud less than 15%;
2) be extraction agent with sherwood oil, alkane or halogenated alkane, extract the lanolin in the mud of above-mentioned drying, the extraction agent consumption be mud weight 4-5 doubly, filter extracting solution;
3) adding volume in said extracted liquid is that extracting solution 2-3%, concentration are the sulfuric acid of 5wt%, being incubated 60-70 ℃ stirred 30 minutes, leave standstill and get upper solution after 1 hour and add the solution that contains 15wt% ethanol and 3wt% sodium hydroxide, add solution volume be aforementioned 2 times of adding the sulfuric acid volume, be incubated 60-70 ℃ and stirred 30 minutes, leave standstill after 1 hour and get upper solution;
4) solution that makes with isopyknic 50 wt % ethanolic soln washing steps 3 is got upper solution after the washing;
5) extraction agent sherwood oil, alkane or the halogenated alkane in the step 4 gained solution removed in underpressure distillation, makes lanolin of the present invention after the residuum cooling.
Be liquid under the used extraction agent room temperature of step 2, as: alkane is C5 ~ C16 alkane; Halogenated alkane is not included as methyl chloride, monochloroethane and the monobromethane etc. of gas.
Further, described alkane is hexane, octane, heptane or solvent oil.
Further, described halogenated alkane is methylene dichloride, trichloromethane or ethylene dichloride.
Further, described sherwood oil boiling range is 60 ~ 90 ℃.
Beneficial effect of the present invention is:
The present invention will extract lanolin through the wet mud utilization of waste material of dosing flocculation from mud, alleviated the three wastes and handled load, improve the utilization ratio of lanolin resource; Technology of the present invention, equipment used are all very simple, and all recyclable utilization of solvent for use, and the filter residue after step 2 is filtered is handled also recyclable extraction agent, economic environmental protection through single vaporization.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment:
Get the wet mud of 500kg after dosing flocculation and centrifuge dehydration, put into baking oven, 70 ℃ of constant temperature carried out drying 7 hours, to moisture content less than 15%, take out and to be cooled to room temperature; Get the container that the dried mud of 100kg places 500L, divide 3 batches to add sherwood oil 450kg altogether, every batch was all fully stirred 30 minutes, and described sherwood oil boiling range is 60 ~ 90 ℃; Leach supernatant liquor after leaving standstill, merge the 400L extracting solution, evaporate sherwood oil residual in the mud filter residue to recycle; The adding mass concentration is 5% sulfuric acid 10L, and insulation was stirred 30 minutes, after static 1 hour to 60 ℃, divide and fall down a layer acid solution, get upper solution and add the solution 20L that contains 15wt% ethanol and 3wt% sodium hydroxide, be incubated 60 ℃ and stirred 30 minutes, after static 1 hour, divide to fall subnatant, get upper solution; Add the 200L lanolin solution that 50 wt % ethanol 200L washing upper strata makes again, be incubated 60 ℃ and stirred 30 minutes, after static 1 hour, divide the alcohol layer of the face that falls down, get upper solution, repeat twice of above-mentioned washing with alcohol with isopyknic 50 wt % ethanol again; Underpressure distillation lanolin solution, the evaporation remove sherwood oil, cool off tawny lanolin.
After testing, the lanolin purity height that the present invention makes, weight is 20kg, accounts for 20% of dried mud weight, is equivalent to the rate of recovery of lanolin in the raw wool has been improved 30-40% again.
The used extraction agent of the present invention also is not limited to sherwood oil, also available alkane such as hexane, octane, heptane or solvent oil, and also available halogenated alkane such as methylene dichloride, trichloromethane or ethylene dichloride, final gained lanolin all can reach the same high purity and the rate of recovery; Extracting liquid filtering gained filter residue is handled recyclable again extraction agent, economic environmental protection through single vaporization.
Technology of the present invention, equipment used are all very simple, and all recyclable utilization of solvent for use; To from mud, extract lanolin through the wet mud utilization of waste material of dosing flocculation, and alleviate the three wastes and handled load, improve the utilization ratio of lanolin resource.

Claims (4)

1. extract the method for lanolin in the waste water from washing wool mud, it is characterized in that may further comprise the steps:
1) waste water from washing wool mud, with warm air drying to the moisture content of mud less than 15%;
2) be extraction agent with sherwood oil, alkane or halogenated alkane, extract the lanolin in the mud of above-mentioned drying, the extraction agent consumption be mud weight 4-5 doubly, filter extracting solution;
3) adding volume in said extracted liquid is that extracting solution 2-3%, concentration are the sulfuric acid of 5wt%, being incubated 60-70 ℃ stirred 30 minutes, leave standstill and get upper solution after 1 hour and add the solution that contains 15wt% ethanol and 3wt% sodium hydroxide, add solution volume be aforementioned 2 times of adding the sulfuric acid volume, be incubated 60-70 ℃ and stirred 30 minutes, leave standstill after 1 hour and get upper solution;
4) solution that makes with isopyknic 50 wt % ethanolic soln washing steps 3 is got upper solution after the washing;
5) extraction agent sherwood oil, alkane or the halogenated alkane in the step 4 gained solution removed in underpressure distillation, makes lanolin of the present invention after the residuum cooling.
2. extract the method for lanolin in the waste water from washing wool mud according to claim 1, the alkane that it is characterized in that described step 2 is hexane, octane, heptane or solvent oil.
3. extract the method for lanolin in the waste water from washing wool mud according to claim 1, the halogenated alkane that it is characterized in that described step 2 is methylene dichloride, trichloromethane or ethylene dichloride.
4. extract the method for lanolin in the waste water from washing wool mud according to claim 1, the sherwood oil boiling range that it is characterized in that described step 2 is 60 ~ 90 ℃.
CN2011101197441A 2011-05-10 2011-05-10 Method for extracting lanolin from wool scouring wastewater Expired - Fee Related CN102226132B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102642958A (en) * 2012-04-23 2012-08-22 西安交通大学 Ultrasonic demulsification device for rendering of scouring wastewater
CN103555428A (en) * 2013-10-30 2014-02-05 南京求是化工工程有限公司 Method for extracting wool fat in wool-scouring wastewater sludge by extractive distillation
CN113073011A (en) * 2021-04-30 2021-07-06 海宁恒力羊绒股份有限公司 Method for extracting lanolin from wool washing wastewater

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4288377A (en) * 1980-06-27 1981-09-08 Arutjunian Norair S Process for purification of wool grease
CN1364864A (en) * 2001-06-07 2002-08-21 甘肃长城热泵有限公司 Method for recovering hanoline from wool washing waste water by ceramic film treatment
CN1907879A (en) * 2006-08-08 2007-02-07 国家海洋局杭州水处理技术研究开发中心 Method for treatment of wool washing waste water

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4288377A (en) * 1980-06-27 1981-09-08 Arutjunian Norair S Process for purification of wool grease
CN1364864A (en) * 2001-06-07 2002-08-21 甘肃长城热泵有限公司 Method for recovering hanoline from wool washing waste water by ceramic film treatment
CN1907879A (en) * 2006-08-08 2007-02-07 国家海洋局杭州水处理技术研究开发中心 Method for treatment of wool washing waste water

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《中国油脂》 19960425 华聘聘等 粗羊毛脂的初步脱色--盐酸酸炼法 第21-23页 1-4 第21卷, 第2期 *
华聘聘等: "粗羊毛脂的初步脱色——盐酸酸炼法", 《中国油脂》, vol. 21, no. 2, 25 April 1996 (1996-04-25), pages 21 - 23 *
郑顺姬等: "羊毛脂的回收与精制", 《皮革化工》, vol. 21, no. 1, 25 February 2004 (2004-02-25), pages 5 - 9 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102642958A (en) * 2012-04-23 2012-08-22 西安交通大学 Ultrasonic demulsification device for rendering of scouring wastewater
CN102642958B (en) * 2012-04-23 2014-04-23 西安交通大学 Ultrasonic demulsification device for rendering of scouring wastewater
CN103555428A (en) * 2013-10-30 2014-02-05 南京求是化工工程有限公司 Method for extracting wool fat in wool-scouring wastewater sludge by extractive distillation
CN103555428B (en) * 2013-10-30 2015-09-23 南京求是化工工程有限公司 A kind of extracting rectifying extracts the method for lanolin in waste water from washing wool mud
CN113073011A (en) * 2021-04-30 2021-07-06 海宁恒力羊绒股份有限公司 Method for extracting lanolin from wool washing wastewater

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