CN109629045B - Milk protein fiber recovery and separation method - Google Patents
Milk protein fiber recovery and separation method Download PDFInfo
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- CN109629045B CN109629045B CN201811582040.6A CN201811582040A CN109629045B CN 109629045 B CN109629045 B CN 109629045B CN 201811582040 A CN201811582040 A CN 201811582040A CN 109629045 B CN109629045 B CN 109629045B
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- milk protein
- fibers
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- separating
- textile
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01G—PRELIMINARY TREATMENT OF FIBRES, e.g. FOR SPINNING
- D01G11/00—Disintegrating fibre-containing articles to obtain fibres for re-use
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- 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
- Y02W30/66—Disintegrating fibre-containing textile articles to obtain fibres for re-use
Abstract
The invention relates to a milk protein fiber recovery and separation method, which comprises the following steps: (1) recovering the textile containing milk protein fibers; (2) crushing the recovered textiles; (3) and (3) separating the crushed raw materials, and recovering to obtain the milk protein fiber. Compared with the prior art, the invention realizes the first breakthrough that two technologies of 'regeneration raw material' + 'cyclic regeneration' are superposed on one fiber, meets the general requirements of the international society on the chemical fiber on the low-carbon environmental protection and cyclic economy trends, and has important significance for promoting the lasting green development of the traditional chemical fiber.
Description
Technical Field
The invention relates to a fiber recycling technology, in particular to a milk protein fiber recycling and separating method.
Background
In order to meet the increasing requirements of people on living level and environmental awareness, the industry has continuously created various novel healthy, comfortable, environment-friendly and high-technology-content textile materials in recent years, and has actively introduced environmental and ecological standards such as Oeko-Tex100, ISO14000 and the like for standardization. At present, the international most famous clothing brands H & M, ZARA and the like pay attention to environmental protection consciousness and disclose promise: the fiber used in the brand of clothes must be recycled at 10% per year to avoid excessive consumption of petroleum resources and more white pollution. The major recyclable fibers on the market are recyclable PET fibers, corn fibers, DuPont biological SORONA fibers and the like, but the moisture absorption, air permeability and skin-friendly performance of the fibers are always poor.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for recovering and separating milk protein fibers.
The purpose of the invention can be realized by the following technical scheme:
a milk protein fiber recovery and separation method comprises the following steps:
(1) recovering the textile containing milk protein fibers;
(2) crushing the recovered textiles;
(3) and (3) separating the crushed raw materials, and recovering to obtain the milk protein fiber.
The textile in the step (1) comprises but is not limited to clothing, bedding or inner core.
And (2) crushing the textile into pieces with the length of 1-5 mm.
And (3) separating the milk protein fiber from other components by a specific gravity method or a dissolving method to obtain the milk protein fiber or milk protein fiber stock solution.
The specific gravity method is particularly suitable for blending or blending milk protein fibers and cotton, ramie, flax, viscose and other two fibers, and comprises the following steps: placing the ground textile into glycerol, controlling the temperature to be 20 +/-2 ℃ for violent oscillation, then standing for layering, taking the upper layer solution for suction filtration, and obtaining the milk protein fiber.
In the above step, 60-100mL of glycerin is added per gram of textile.
The dissolving method is particularly suitable for blending or blending milk protein fibers with cotton, viscose, tencel, modal, polyester fibers and the like, and comprises the following steps: placing the ground textile in water, carrying out violent shaking at the temperature of 20 +/-2 ℃ to further disperse the chopped fibers, then filtering, adding a sodium thiocyanate solution, shaking in a water bath at the temperature of 65-75 ℃ to fully dissolve the milk protein fibers, and filtering to obtain the milk protein fiber spinning stock solution.
Adding 80-120ml of water per gram of textile in the steps.
Because the sodium thiocyanate solution can directly dissolve the milk protein fibers into stock solution and does not react with other fibers, the reagent mainly used in the method is 36-55% (mass fraction) of the sodium thiocyanate solution, and the concentration of the adopted sodium thiocyanate solution is 36-55 wt%.
Compared with the prior art, the invention has the following advantages:
(1) recycling resources and recovering science and technology: the raw materials come from waste or eliminated textile raw materials or textiles containing milk fibers, so that the waste of a large amount of waste milk residues is avoided, the production and processing cost is low, and the fiber products meet the standard requirements of ecological textiles;
(2) can be recycled and reproduced: the innovative, environment-friendly and multidisciplinary cross technology (physics and chemistry) fiber recycling and recycling production technology is applied, the pollution of waste to the environment is reduced, the use of petroleum can be replaced or reduced to a certain extent, and the waste resources are reasonably utilized for reproduction;
(3) new technology, sustainability: the recycled textile with the milk fiber can be applied to waste textiles containing silk, wool and other protein biomasses in the future, and has the characteristic of sustainable development.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
A milk protein fiber recovery and separation method comprises the following steps:
(1) clothes, bedding, inner cores and the like containing milk protein fibers, and the clothes containing 100 percent of milk protein fibers are provided in the embodiment. The content of the milk protein fiber is selected based on the consideration of the recovery cost, the content is higher, and the recovery cost performance is higher;
(2) crushing the recovered clothes, bedding, inner cores and the like containing the milk protein fibers (the length is 1-5 mm);
(3) separating the crushed raw materials by a hydrometer method, and recovering to obtain the milk protein fiber.
The specific gravity is the ratio of the mass of a substance to the mass of pure water at the same volume and temperature, and is generally the specific gravity at 20 ℃ and is represented by r420, or the specific gravity is the ratio of the mass of a substance to the mass of water at the same volume and 4 ℃ and is represented by r 2020. The following table shows the specific gravities of the general fibers and the milk protein fibers.
As can be seen from the table, the milk protein fiber has a significant difference in specific gravity with other fibers (such as cotton, ramie, flax, viscose, etc.) blended therewithIf necessary, the solution may be delaminated by adjusting its specific gravity. Glycerol is a viscous liquid with a sweet orange taste and a colorless smell, and has a density (specific gravity) of 1.263-1.303g/cm3And does not react with the fibers and can be used as a solvent for separating different fibers.
The embodiment is particularly suitable for blending or blending the milk protein fiber and two fibers such as cotton, ramie, flax, viscose and the like, 80ml of glycerol is added into each gram of the mixture after being crushed, the mixture is violently shaken for 40 minutes at the temperature of 20 ℃, and after standing for 30 minutes, the layering condition of the solution is stable, at the moment, the milk protein fiber is on the upper layer of the solution, and other fibers are on the lower layer of the solution. The milk protein fiber and other fibers are respectively obtained by sucking and filtering the solid fibers on the upper layer and the lower layer.
Example 2
A milk protein fiber recovery and separation method comprises the following steps:
(1) garments, bedding, innercores, etc., containing milk protein fibers, in this example garments containing 60% milk protein fibers and 40% viscose;
(2) crushing the recovered clothes, bedding, inner cores and the like containing the milk protein fibers (the length is 1-5 mm);
(3) separating the crushed raw materials by a specific gravity method, adding 60ml of glycerol into each gram of the crushed mixture, violently shaking for 40 minutes at the temperature of 18 ℃, standing for 30 minutes until the solution is layered stably, wherein the milk protein fiber is on the upper layer of the solution, and the other fibers are on the lower layer of the solution. The milk protein fiber and other fibers are respectively obtained by sucking and filtering the solid fibers on the upper layer and the lower layer.
Example 3
A milk protein fiber recovery and separation method comprises the following steps:
(1) clothes, bedding, inner cores and the like containing milk protein fibers, clothes, bedding, inner cores and the like containing milk protein fibers), and the embodiment is bedding fabric containing 70% of milk protein fibers and 30% of cotton;
(2) crushing the recovered clothes, bedding, inner cores and the like containing the milk protein fibers (the length is 1-5 mm);
(3) separating the crushed raw materials by a specific gravity method, adding 100ml of glycerol into each gram of the crushed mixture, violently shaking for 40 minutes at the temperature of 22 ℃, standing for 30 minutes until the solution is layered stably, wherein the milk protein fiber is on the upper layer of the solution, and the other fibers are on the lower layer of the solution. The milk protein fiber and other fibers are respectively obtained by sucking and filtering the solid fibers on the upper layer and the lower layer.
Example 4
(1) Garments, bedding, inner cores, etc. containing milk protein fibers, garments, bedding, inner cores, etc. containing milk protein fibers), in this example, an inner core containing 50% milk protein fibers and 50% dacron;
(2) crushing the recovered clothes, bedding, inner cores and the like containing the milk protein fibers (the length is 1-5 mm);
(3) separating the crushed raw materials by using a dissolving method, placing the crushed textile into water, carrying out violent oscillation at the temperature of 20 ℃ to further disperse the chopped fibers, then filtering, adding a 45 wt% sodium thiocyanate solution, oscillating in a 70 ℃ water bath to fully dissolve the milk protein fibers, and filtering to obtain the milk protein fiber spinning solution.
Example 5
(1) Garments, bedding, innercores and the like comprising milk protein fibers, in this example garments comprising 90% milk protein fibers and 10% modal;
(2) crushing the recovered clothes, bedding, inner cores and the like containing the milk protein fibers (the length is 1-5 mm);
(3) separating the pulverized raw materials by using a dissolving method, placing the pulverized textile in water, controlling the temperature at 18 ℃ to perform violent shaking to further disperse the chopped fibers, then filtering, adding 36 wt% sodium thiocyanate solution, shaking in a water bath at 65 ℃ to fully dissolve the milk protein fibers, and filtering to obtain a milk protein fiber spinning stock solution
Example 6
(1) Garments, bedding, innercores and the like comprising milk protein fibers, in this example garments comprising 80% milk protein fibers and 20% tencel;
(2) crushing the recovered clothes, bedding, inner cores and the like containing the milk protein fibers (the length is 1-5 mm);
(3) separating the crushed raw materials by using a dissolving method, placing the crushed textile into water, carrying out violent oscillation at the temperature of 22 ℃ to further disperse the chopped fibers, then filtering, adding a sodium thiocyanate solution with the concentration of 55wt%, oscillating in a water bath at 75 ℃ to fully dissolve the milk protein fibers, and filtering to obtain the milk protein fiber spinning solution.
Example 7
Cutting 5 g of recycled textile fabric (80% of milk protein fiber and 20% of cotton) into fibers with the length of 3mm, adding 300ml of glycerol, violently shaking at 19 ℃ for 40 minutes, standing for 30 minutes, after the solution is layered, sucking and filtering the milk protein fiber on the upper layer, and using the cotton fiber on the lower layer as a paper pulp raw material of high-grade paper.
Example 8
Cutting 5 g of recycled textile fabric (component: 100% milk protein fiber) into 5mm long fibers, adding into 500ml of water solution, and vigorously shaking in water bath at 20 deg.C for 40 min to further disperse and filter the chopped fibers; the filtered mixture was added to 500ml of 36% sodium thiocyanate solution and shaken in a water bath at 70 ℃ for 30 minutes to dissolve the milk protein fibers sufficiently for filtration. The filtered liquid is the milk protein fiber spinning solution.
Example 9
Cutting 5 g of recycled textile fabric (component: 50% of milk protein fiber and 50% of modal) into fibers with the length of 4mm, adding the fibers into 600ml of glycerol aqueous solution, and violently shaking the fibers on a water bath at 21 ℃ for 40 minutes to further disperse and filter the cut fibers; the lower layer cellulose fiber can be reused as a paper pulp raw material of high-grade paper.
Example 10
Cutting 5 g of recycled textile fabric (70% of milk protein fiber and 30% of terylene) into fibers with the length of 3mm, adding the fibers into 400ml of aqueous solution, and violently shaking the fibers for 40 minutes on a water bath at the temperature of 22 ℃ to further disperse and filter the cut fibers; the filtered mixture was added to 500ml of 55% sodium thiocyanate solution and shaken in a water bath at 75 ℃ for 30 minutes to dissolve the milk protein fibers sufficiently for filtration. The filtered liquid is the milk protein fiber spinning solution.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (8)
1. A method for recovering and separating milk protein fibers is characterized by comprising the following steps:
(1) recovering the textile containing milk protein fibers;
(2) crushing the recovered textiles;
(3) separating the crushed raw materials, and recovering to obtain milk protein fibers;
separating milk protein fiber from other components by a specific gravity method or a dissolving method to obtain milk protein fiber or milk protein fiber stock solution;
specifically, milk protein fibers are separated from cotton, ramie, flax and viscose by a hydrometer method, and the following steps are adopted: placing the ground textile in glycerol, violently shaking, standing for layering, taking the upper layer solution, sucking and filtering to obtain milk protein fibers; wherein the glycerol does not react with the fibers;
or separating the milk protein fiber from cotton, viscose, tencel, modal and polyester fiber by a dissolving method, and adopting the following steps: placing the crushed textile in water, carrying out violent oscillation to further disperse the chopped fibers, then filtering, adding a sodium thiocyanate solution, oscillating in a water bath to fully dissolve the milk protein fibers, and filtering to obtain a milk protein fiber spinning stock solution; wherein, the sodium thiocyanate solution directly dissolves the milk protein fiber into stock solution without reacting with other fibers.
2. The method for recovering and separating milk protein fibers according to claim 1, wherein the textile in step (1) includes but is not limited to clothes, bedding or inner core.
3. The method for recovering and separating milk protein fibers according to claim 1, wherein the textile in the step (2) is crushed into a length of 1-5 mm.
4. The method for recovering and separating the milk protein fibers according to claim 1, wherein the specific gravity method comprises the following steps: placing the ground textile into glycerol, controlling the temperature to be 20 +/-2 ℃ for violent oscillation, then standing for layering, taking the upper layer solution for suction filtration, and obtaining the milk protein fiber.
5. The method for recovering and separating milk protein fibers according to claim 4, wherein 60-100mL of glycerin is added per gram of textile in the above step.
6. The method for recovering and separating milk protein fibers according to claim 1, wherein the dissolving method comprises the following steps: placing the ground textile in water, carrying out violent shaking at the temperature of 20 +/-2 ℃ to further disperse the chopped fibers, then filtering, adding a sodium thiocyanate solution, shaking in a water bath at the temperature of 65-75 ℃ to fully dissolve the milk protein fibers, and filtering to obtain the milk protein fiber spinning stock solution.
7. The method for recovering and separating milk protein fibers according to claim 6, wherein 80-120ml of water is added per gram of textile in the above step.
8. The method for recovering and separating milk protein fibers according to claim 1, wherein the concentration of the sodium thiocyanate solution is 36-55 wt%.
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Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1590609A (en) * | 2003-09-03 | 2005-03-09 | 中国皮革和制鞋工业研究院 | Collagen protein-polyacrylonitrile composite fiber and its preparation method |
CN101514497A (en) * | 2009-03-09 | 2009-08-26 | 东华大学 | Method for separating and extracting fibrillar structural body in natural keratin fiber |
CN101608364A (en) * | 2009-07-21 | 2009-12-23 | 上海水星家用纺织品有限公司 | A kind of milk protein fiber modification preparation and the application in home textile product thereof |
CN101748629A (en) * | 2008-12-01 | 2010-06-23 | 财团法人工业技术研究院 | Fiber decomposition device |
CN102817101A (en) * | 2012-07-31 | 2012-12-12 | 上海全宇生物科技遂平有限公司 | Hair keratin composite fiber and spinning method thereof |
CN103102695A (en) * | 2013-03-07 | 2013-05-15 | 河南鼎大生物科技有限公司 | Method for preparation and wet spinning of regenerative keratin solution |
CN103382599A (en) * | 2013-08-06 | 2013-11-06 | 上海婉静纺织科技有限公司 | Blended fabric of milk protein fiber, Viloft fiber and polyester fiber |
CN104862818A (en) * | 2015-06-09 | 2015-08-26 | 江南大学 | Preparation method of keratin complex fiber |
WO2016050357A1 (en) * | 2014-10-02 | 2016-04-07 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e. V. | Methods for preparing and orientating biopolymer nanofibres and a composite material comprising the same |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20050255779A1 (en) * | 2004-04-22 | 2005-11-17 | Ngk Spark Plug Co., Ltd. | Organic-inorganic composite porous material, method for producing fibrous organic material, and method for producing organic-inorganic composite porous material |
CN103467382A (en) * | 2013-09-16 | 2013-12-25 | 浙江丽晶化学有限公司 | Method for preparing thiocyanate-containing ionic liquid and application of ionic liquid in polyacrylonitrile spinning processing |
CN107227556A (en) * | 2017-05-22 | 2017-10-03 | 海宁杰盛新材料有限公司 | A kind of preparation method of collagen fabric skin |
CN107724081A (en) * | 2017-10-25 | 2018-02-23 | 深圳市恒锋环境资源控股有限公司 | A kind of gloves regeneration cotton yarn textile material and preparation method thereof and system |
-
2018
- 2018-12-24 CN CN201811582040.6A patent/CN109629045B/en active Active
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1590609A (en) * | 2003-09-03 | 2005-03-09 | 中国皮革和制鞋工业研究院 | Collagen protein-polyacrylonitrile composite fiber and its preparation method |
CN101748629A (en) * | 2008-12-01 | 2010-06-23 | 财团法人工业技术研究院 | Fiber decomposition device |
CN101514497A (en) * | 2009-03-09 | 2009-08-26 | 东华大学 | Method for separating and extracting fibrillar structural body in natural keratin fiber |
CN101608364A (en) * | 2009-07-21 | 2009-12-23 | 上海水星家用纺织品有限公司 | A kind of milk protein fiber modification preparation and the application in home textile product thereof |
CN102817101A (en) * | 2012-07-31 | 2012-12-12 | 上海全宇生物科技遂平有限公司 | Hair keratin composite fiber and spinning method thereof |
CN103102695A (en) * | 2013-03-07 | 2013-05-15 | 河南鼎大生物科技有限公司 | Method for preparation and wet spinning of regenerative keratin solution |
CN103382599A (en) * | 2013-08-06 | 2013-11-06 | 上海婉静纺织科技有限公司 | Blended fabric of milk protein fiber, Viloft fiber and polyester fiber |
WO2016050357A1 (en) * | 2014-10-02 | 2016-04-07 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e. V. | Methods for preparing and orientating biopolymer nanofibres and a composite material comprising the same |
CN104862818A (en) * | 2015-06-09 | 2015-08-26 | 江南大学 | Preparation method of keratin complex fiber |
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