CN103102695B - Preparation of regenerative keratin solution and method of wet spinning - Google Patents
Preparation of regenerative keratin solution and method of wet spinning Download PDFInfo
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- CN103102695B CN103102695B CN201310072813.7A CN201310072813A CN103102695B CN 103102695 B CN103102695 B CN 103102695B CN 201310072813 A CN201310072813 A CN 201310072813A CN 103102695 B CN103102695 B CN 103102695B
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Abstract
The invention belongs to the field of natural high polymer materials, and relates to a method for preparation and wet spinning of a regenerative keratin solution. The method comprises the following steps of: degreasing raw materials of coarse animal hairs, wools and waste wool textiles by using a non-ionic surface active agent, wherein the coarse animal hairs include pig hairs, sheep wools, rabbit hairs, camel hairs, yak hairs and the like, and the wools and waste wool textiles do not have spinning and weaving utility values; grinding the raw materials into nano-scale superfine powder by using a superfine grinding technology; fully swelling the keratin superfine powder by using a mixed solution of ZnCl2 and urea, wherein the mixed solution has a swelling function; and dissolving the fully-swelled keratin superfine powder by using an ionic liquid of 1-butyl-3-methylimidazole chloride or 1-ethyl-3-methylimidazole diethyl phosphate to obtain a regenerative keratin spinning solution which has the characteristics of high keratin concentration, complete dissolution and high molecular weight, and regenerative keratin fibers can be obtained by adopting wet spinning. By adopting the method, waste resources are recycled, so that the method has broad prospects and application values, and accords with the current research concept and direction of environmental protection.
Description
Technical field
The invention belongs to natural macromolecular material Application Areas, relate to a kind of technology of animal hair regeneration, be specifically related to a kind of regeneration keratin solution of the applicable wet-spinning of animal hair preparation and method of wet-spinning thereof utilized.
Background technology
In environmental problem day by day serious today, the resource utilization recycling of waste receive widespread attention.China has a large amount of hairs inferior, waste and old hair, spinning leftovers and other many animal hairs every year, has all arbitrarily processed with the form of waste, and this not only causes environmental pollution, more causes the waste of keratin resource.Discarded animal hair is dissolved and makes keratin solution, by precipitation bath (precipitation bath is a kind of body lotion that makes keratin solution solidificating fiber), keratin solution is prepared into regenerated keratin again, realize waste resource recycling, there is bright prospects and using value, and meet research theory and the direction of current environmental protection.But, in animal hair, protein molecule is laterally connected to form space reticulated structure by a large amount of cystine linkages, makes keratic compact structure, causes the natural animal hair can not melting, and is difficult to be dissolved in conventional solvent.In order to dissolve natural animal hair, just must adopt the solvent of difference in functionality
,to destroy cystine linkage, salt type bond and the hydrogen bond etc. between protein molecule, according to the difference of adopted solvent, the method of its dissolving can be divided into acid process, basic process, oxidation style, reduction method etc., but the keratolysis thing molecular weight obtaining by these methods is generally lower, be not suitable for the preparation of the regenerated keratin of high protein content, and environment is had to larger pollution, do not meet the requirement of green industry development.
Have now a kind of method with ion liquid dissolving natural animal hair, ionic liquid refers in room temperature or approaches under room temperature and presents liquid, the complete salt being made up of zwitterion, also referred to as low temperature molten salt.Ionic liquid is green solvent, nontoxic, tasteless, Heat stability is good, can be recycled, and has applied in recent years the dissolving of the natural polymer including silk fibroin, Keratin sulfate and Mierocrystalline cellulose etc.Application number is 200510077289.8, name is called the Chinese patent of " using ion liquid dissolving animal hair to prepare the method for regenerated protein ", a kind of method of utilizing the direct dissolving animal hair of ionic liquid to send out is disclosed, the method technical process is: solidify-regenerated protein of raw material-cleaning-ion liquid dissolving-precipitation bath, it is still lower that the method obtains keratolysis thing molecular weight, can only obtain the cotton-shaped regenerated keratin of sheet, keratin solution can not meet the actual requirement of wet-spinning.
Summary of the invention
The object of the invention is to cause in order to overcome existing animal hair dissolution method the defect that keratolysis thing molecular weight is on the low side, keratin solution can not meet wet-spinning requirement, invent and a kind ofly adopt mode that physics and chemistry combines to come that dissolving animal hair is sent out and the preparation of regeneration keratin solution and the method for wet-spinning of spinning.
The object of the invention is to realize as follows:
Described regeneration keratin solution, makes taking animal hair as raw material, and its preparation comprises washing, pulverizing, swelling, four steps of dissolving:
(1) washing
Animal hair is washed with nonionic washing soln, nonionic washing soln is nonionic table
The mixed aqueous solution of surface-active agent and auxiliary agent, wherein the quality of nonionogenic tenside accounts for the 0.3-2.5% of solution total mass, and the quality of auxiliary agent accounts for the 0.5-6.0% of solution total mass; According to the ratio of the quality 1:5-40 of animal hair and nonionic washing soln, animal hair is put into nonionic washing soln, the temperature of nonionic washing soln is 30-70 DEG C, pH value is 7-8, utilization is washed and is dried associating wool washing machine washing 10-60 min, washing post-drying, bake out temperature is 40-90 DEG C;
(2) pulverize
Utilize air-flow supper micron mill the animal hair of step (1) gained to be ground into the fine powder of diameter 100-1000 nanometer;
(3) swelling
The fine powder of step (2) gained is immersed in to zinc chloride (ZnCl
2) and urea (CO (NH
2)
2) mixed aqueous solution in carry out swelling treatment, wherein zinc chloride (ZnCl
2) the quality per-cent that accounts for whole mixing solutions quality be 10-40%, urea (CO (NH
2)
2) the quality per-cent that accounts for whole mixing solutions quality be 5-25%, soaking temperature is 30-65 DEG C, soak time is 10-125min; After filtration, use again deionized water (deionized water refers to and removed the pure water being after ionic species impurity, deionized water be prepared as prior art) washing to neutral, refilter, then drying at 50-75 DEG C of temperature, being balanced moisture regain is the raw material micro mist of 10-20%;
(4) dissolve
The raw material micro mist of step (3) gained is joined in ionic liquid, and the quality of ionic liquid is 3-10 times of raw material micro mist quality, and at the temperature of 80-120 DEG C, violent stirring 10-200min, obtains the keratin solution of regenerating.
Described animal hair is the animal coarse wool such as pig hair, goathair, sheep's wool, the rabbit hair, Pilus Cameli, yak hair, and the wool of adhesive-bonded utility value and discarded wool textile.
Described nonionogenic tenside is Polyethylene Octylphenol Ether, nonyl phenol polyethenoxy ether, ethoxylated dodecyl alcohol or Brij.
Described auxiliary agent is sodium sulfate or ammonium sulfate.
Described ionic liquid is 1-butyl-3-Methylimidazole villaumite or 1-ethyl-3-methylimidazole diethyl phosphoric acid.
The method of carrying out wet-spinning by described regeneration keratin solution, its technical process comprises: solidify, drawing-off, washing, dry, heat setting type, the processing condition of described wet-spinning are as follows:
(1) solidify
Coagulation bath composition: the ionic liquid aqueous solution that water or concentration are 5-40%;
Coagulation bath temperature: 10-40 DEG C;
Spinning speed: 5-35 m/min;
(2) drawing-off
Composition is bathed in drawing-off: water or concentration are 5-45% ionic liquid aqueous solution;
Drawing-off bath temperature: 60-95 DEG C;
Drafting multiple: 2.5-9.5 doubly;
(3) washing
Washing temperature: 40-65 DEG C;
(4) dry
Drying temperature: 50-80 DEG C;
(5) heat setting type
Heat setting temperature: 110-135 DEG C;
Heat-setting time: 1-10min.
Compared with prior art, advantage of the present invention is:
(1) animal hair that the present invention is worth taking adhesive-bonded, as raw material, has been developed regeneration keratin solution, and this solution has the advantages that Keratin sulfate concentration is high, dissolving is complete, molecular weight is large; This solution need not be dialysed, and has good spinning property, can be directly used in wet-spinning;
(2) dissolution process involved in the present invention is simple, dissolution rate 100%, and chemical reagent used is all recyclable, is applicable to suitability for industrialized production;
(3) directly wet-spinning of regeneration keratin solution of the present invention, prepare regenerated keratin (long filament or short fiber), also can be with other macromolecular material as polyacrylonitrile, polyvinyl alcohol, cellulose blending, or with the compound or functional protein fiber of inorganic functional nanoparticle blend preparation regeneration.
Embodiment
Case study on implementation 1
(1) with nonionic washing soln, animal hair is washed, in nonionic washing soln, the quality of nonionogenic tenside accounts for 1.2% of solution total mass, and the quality of auxiliary agent accounts for 4.5% of solution total mass; According to the ratio of the quality 1:22 of animal hair and nonionic washing soln, animal hair is put into nonionic washing soln, the temperature of nonionic washing soln is 50 DEG C, pH value is 7.0, utilization is washed and is dried associating wool washing machine washing 30min, washing post-drying, and bake out temperature is 90 DEG C;
(2) utilize air-flow supper micron mill the animal hair of step (1) gained to be ground into the fine powder of diameter 800 nanometers;
(3) fine powder of step (2) gained is immersed in to zinc chloride (ZnCl
2) and urea (CO (NH
2)
2) mixed aqueous solution in carry out swelling treatment, wherein zinc chloride (ZnCl
2) the quality per-cent that accounts for whole mixing solutions quality be 35%, urea (CO (NH
2)
2) the quality per-cent that accounts for whole mixing solutions quality be 20%, soaking temperature is 65 DEG C, soak time is 100min, after filtration, more extremely neutral with deionized water wash, refilter, then drying at 75 DEG C of temperature, is balanced moisture regain and is 18% raw material micro mist;
(4) the raw material micro mist of step (3) gained is joined to ionic liquid 1-butyl-3-methyl imidazolium
In villaumite, the consumption of ionic liquid is 8 times of raw material micro mist quality, at the temperature of 110 DEG C, stirs 35min, obtains the keratin solution of regenerating;
(5) by the regeneration keratin solution of step (4) gained, utilize wet-spinning to obtain regenerated keratin, technical process comprise solidify, drawing-off, washing, dry, heat setting type, the processing condition of described wet-spinning are as follows:
Coagulation bath composition: water
Coagulation bath temperature: 10 DEG C
Spinning speed: 5 ms/min
Composition is bathed in drawing-off: water
Drawing-off bath temperature: 95 DEG C
Drafting multiple: 2.5 times
Washing temperature: 65 DEG C
Drying temperature: 80 DEG C
Heat setting temperature: 135 DEG C
Heat-setting time: 10min.
case study on implementation 2
(1) with nonionic washing soln, animal hair is washed, in nonionic washing soln, the quality of nonionogenic tenside accounts for 2.4% of solution total mass, and the quality of auxiliary agent accounts for 0.8% of solution total mass; According to the ratio of the quality 1:30 of animal hair and nonionic washing soln, animal hair is put into nonionic washing soln, the temperature of nonionic washing soln is 45 DEG C, pH value is 7.5, utilization is washed and is dried associating wool washing machine washing 50min, washing post-drying, and bake out temperature is 70 DEG C;
(2) utilize air-flow supper micron mill the animal hair of step (1) gained to be ground into the fine powder of diameter 600 nanometers;
(3) fine powder of step (2) gained is immersed in to zinc chloride (ZnCl
2) and urea (CO (NH
2)
2) mixed aqueous solution in carry out swelling treatment, wherein zinc chloride (ZnCl
2) the quality per-cent that accounts for whole mixing solutions quality be 25%, urea (CO (NH
2)
2) the quality per-cent that accounts for whole mixing solutions quality be 15%, soaking temperature is 50 DEG C, soak time is 60min, after filtration, more extremely neutral with deionized water wash, refilter, then drying at 65 DEG C of temperature, is balanced moisture regain and is 15% raw material micro mist;
(4) the raw material micro mist of step (3) gained is joined to ionic liquid 1-ethyl-3-methylimidazole
In diethyl phosphoric acid, the consumption of ionic liquid is 5 times of raw material micro mist quality, at the temperature of 100 DEG C, stirs 68min, obtains the keratin solution of regenerating;
(5) the regeneration keratin solution of step (4) gained, utilizes wet-spinning to obtain regenerated keratin, technical process comprise solidify, drawing-off, washing, dry, heat setting type.The processing condition of described wet-spinning are as follows:
Coagulation bath composition: 10% ionic liquid 1-ethyl-3-methylimidazole p diethylaminobenzoic acid aqueous solution of ester
Coagulation bath temperature: 30 DEG C
Spinning speed: 25 ms/min
Composition is bathed in drawing-off: 10% ionic liquid aqueous solution
Drawing-off bath temperature: 65 DEG C
Drafting multiple: 7.5 times
Washing temperature: 55 DEG C
Drying temperature: 50 DEG C
Heat setting temperature: 130 DEG C
Heat-setting time: 8min.
case study on implementation 3
(1) with nonionic washing soln, animal hair is washed, in nonionic washing soln, the quality of nonionogenic tenside accounts for 0.8% of solution total mass, and the quality of auxiliary agent accounts for 4.0% of solution total mass; According to the ratio of the quality 1:18 of animal hair and nonionic washing soln, animal hair is put into nonionic washing soln, the temperature of nonionic washing soln is 60 DEG C, pH value is 8.0, utilization is washed and is dried associating wool washing machine washing 15min, washing post-drying, and bake out temperature is 50 DEG C;
(2) utilize air-flow supper micron mill the animal hair of step (1) gained to be ground into the fine powder of diameter 500 nanometers;
(3) fine powder of step (2) gained is immersed in to zinc chloride (ZnCl
2) and urea (CO (NH
2)
2) mixed aqueous solution in carry out swelling treatment, wherein zinc chloride (ZnCl
2) the quality per-cent that accounts for whole mixing solutions quality be 18%, urea (CO (NH
2)
2) the quality per-cent that accounts for whole mixing solutions quality be 15%, soaking temperature is 40 DEG C, soak time is 30min, after filtration, more extremely neutral with deionized water wash, refilter, then drying at 65 DEG C of temperature, is balanced moisture regain and is 10% raw material micro mist;
(4) the raw material micro mist of step (3) gained is joined in ionic liquid 1-butyl-3-methyl imidazolium chlorine, the consumption of ionic liquid is 4 times of raw material micro mist quality, at 90 DEG C of temperature, stirs 25min, obtains the keratin solution of regenerating;
(5) the regeneration keratin solution of step (4) gained utilizes wet-spinning to obtain regenerated keratin, technical process comprise solidify, drawing-off, washing, dry, heat setting type.The processing condition of described wet-spinning are as follows:
Coagulation bath composition: the ionic liquid 1-butyl-3-methyl imidazolium chlorine water solution that concentration is 15%
Coagulation bath temperature: 15 DEG C
Spinning speed: 25 ms/min
Composition is bathed in drawing-off: the aqueous solution
Drawing-off bath temperature: 95 DEG C
Drafting multiple: 5.5 times
Washing temperature: 55 DEG C
Drying temperature: 60 DEG C
Heat setting temperature: 130 DEG C
Heat-setting time: 5min.
case study on implementation 4
(1) with nonionic washing soln, animal hair is washed, in nonionic washing soln, the quality of nonionogenic tenside accounts for 1.0% of solution total mass, and the quality of auxiliary agent accounts for 3.2% of solution total mass; According to the ratio of the quality 1:16 of animal hair and nonionic washing soln, animal hair is put into nonionic washing soln, the temperature of nonionic washing soln is 50 DEG C, pH value is 7.8, utilization is washed and is dried associating wool washing machine washing 50min, washing post-drying, and bake out temperature is 60 DEG C;
(2) utilize air-flow supper micron mill the animal hair of step (1) gained to be ground into the fine powder of diameter 300 nanometers;
(3) fine powder of step (2) gained is immersed in to zinc chloride (ZnCl
2) and urea (CO (NH
2)
2) mixed aqueous solution in carry out swelling treatment, wherein zinc chloride (ZnCl
2) the quality per-cent that accounts for whole mixing solutions quality be 10%, urea (CO (NH
2)
2) the quality per-cent that accounts for whole mixing solutions quality be 6%, soaking temperature is 30 DEG C, soak time is 25min, after filtration, then with deionized water wash to neutral, refilter, then drying at 55 DEG C of temperature, is balanced moisture regain and is 15% raw material micro mist;
(4) the raw material micro mist of step (3) gained is joined in ionic liquid 1-ethyl-3-methylimidazole diethyl phosphoric acid, the consumption of ionic liquid is 7 times of raw material micro mist quality, at 105 DEG C of temperature, stirs 18min, obtains the keratin solution of regenerating;
(5) the regeneration keratin solution of step (4) gained utilizes wet-spinning to obtain regenerated keratin, technical process comprise solidify, drawing-off, washing, dry, heat setting type, the processing condition of described wet-spinning are as follows:
Coagulation bath composition: the ionic liquid 1-ethyl-3-methylimidazole p diethylaminobenzoic acid aqueous solution of ester that concentration is 20%
Coagulation bath temperature: 35 DEG C
Spinning speed: 30 ms/min
Composition is bathed in drawing-off: the ionic liquid 1-ethyl-3-methylimidazole p diethylaminobenzoic acid aqueous solution of ester that concentration is 8%
Drawing-off bath temperature: 80 DEG C
Drafting multiple: 9 times
Washing temperature: 45 DEG C
Drying temperature: 60 DEG C
Heat setting temperature: 120 DEG C
The dryness finalization time: 10min.
Claims (2)
1. a preparation for the keratin solution of regenerating, is characterized in that: described regeneration keratin solution, to make taking animal hair as raw material, and its preparation comprises washing, pulverizing, swelling, four steps of dissolving:
(1) washing
Animal hair is washed with nonionic washing soln, nonionic washing soln right and wrong from
The mixed aqueous solution of sub-surface promoting agent and auxiliary agent, wherein the quality of nonionogenic tenside accounts for the 0.3-2.5% of solution total mass, and the quality of auxiliary agent accounts for the 0.5-6.0% of solution total mass; According to the ratio of the quality 1:5-40 of animal hair and nonionic washing soln, animal hair is put into nonionic washing soln, the temperature of nonionic washing soln is 30-70 DEG C, pH value is 7-8, utilization is washed and is dried associating wool washing machine washing 10-60 min, washing post-drying, bake out temperature is 40-90 DEG C;
(2) pulverize
Utilize air-flow supper micron mill the animal hair of step (1) gained to be ground into the fine powder of diameter 100-1000 nanometer;
(3) swelling
The fine powder of step (2) gained is immersed in the mixed aqueous solution of zinc chloride and urea and carries out swelling treatment, wherein to account for the per-cent of whole mixing solutions quality be 10-40% to the quality of zinc chloride, the per-cent that the quality of urea accounts for whole mixing solutions quality is 5-25%, soaking temperature is 30-65 DEG C, and soak time is 10-125min; After filtration, more extremely neutral with deionized water wash, refilter, then drying at 50-75 DEG C of temperature, being balanced moisture regain is the raw material micro mist of 10-20%;
(4) dissolve
The raw material micro mist of step (3) gained is joined in ionic liquid, and the quality of ionic liquid is 3-10 times of raw material micro mist quality, and at the temperature of 80-120 DEG C, violent stirring 10-200min, obtains the keratin solution of regenerating.
2. the preparation of regeneration keratin solution according to claim 1, it is characterized in that: described animal hair comprises the animal coarse wool such as pig hair, goathair, sheep's wool, the rabbit hair, Pilus Cameli, yak hair, and the wool of adhesive-bonded utility value and discarded wool textile.
3. the preparation of regeneration keratin solution according to claim 1, is characterized in that: described nonionogenic tenside is Polyethylene Octylphenol Ether, nonyl phenol polyethenoxy ether, ethoxylated dodecyl alcohol or Brij.
4. the preparation of regeneration keratin solution according to claim 1, is characterized in that: described auxiliary agent is sodium sulfate or ammonium sulfate.
5. the preparation of regeneration keratin solution according to claim 1, is characterized in that: described ionic liquid is 1-butyl-3-Methylimidazole villaumite or 1-ethyl-3-methylimidazole diethyl phosphoric acid.
6. the regeneration keratin solution obtaining according to the preparation of regeneration keratin solution claimed in claim 1 is carried out the method for wet-spinning, it is characterized in that: its technical process comprises: solidify, drawing-off, washing, dry, heat setting type, the processing condition of described wet-spinning are as follows:
(1) solidify
Coagulation bath composition: the ionic liquid aqueous solution that water or concentration are 5-40%;
Coagulation bath temperature: 10-40 DEG C;
Spinning speed: 5-35 m/min;
(2) drawing-off
Composition is bathed in drawing-off: water or concentration are 5-45% ionic liquid aqueous solution;
Drawing-off bath temperature: 60-95 DEG C;
Drafting multiple: 2.5-9.5 doubly;
(3) washing
Washing temperature: 40-65 DEG C;
(4) dry
Drying temperature: 50-80 DEG C;
(5) heat setting type
Heat setting temperature: 110-135 DEG C;
Heat-setting time: 1-10min.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103710775B (en) * | 2013-12-18 | 2016-02-24 | 中国科学院过程工程研究所 | A kind of preparation method of ionic liquid keratin spinning solution |
| CN104101524A (en) * | 2014-07-07 | 2014-10-15 | 西北农林科技大学 | Method for quickly extracting, purifying and detecting protein in hair |
| CN109881279B (en) * | 2018-03-26 | 2021-08-03 | 新乡化纤股份有限公司 | Ion liquid method for regenerating animal keratin fiber and preparation method thereof |
| CN109629045B (en) * | 2018-12-24 | 2021-12-31 | 上海正家牛奶丝科技有限公司 | Milk protein fiber recovery and separation method |
| CN114622304B (en) * | 2022-02-07 | 2023-03-28 | 江南大学 | Preparation method of functional keratin composite fiber based on ionic liquid |
| CN117946242A (en) * | 2024-03-27 | 2024-04-30 | 张家港扬子染整有限公司 | Method for extracting high-concentration keratin |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1660901A (en) * | 2004-12-24 | 2005-08-31 | 中国科学院长春应用化学研究所 | Method for preparing solution of keratin |
| CN1884641A (en) * | 2005-06-21 | 2006-12-27 | 中国科学院过程工程研究所 | Method for preparing regenerated protein fiber using ion liquid dissolving animal hair |
| CN1884642A (en) * | 2005-06-21 | 2006-12-27 | 中国科学院过程工程研究所 | Biological protein hair fiber preparation method by dissolving animal hair and cellulose material mixture |
| US20090051068A1 (en) * | 2006-01-12 | 2009-02-26 | Thüringisches Institute Für Textil-Und Kunststoff-Forschung E.V. | Method for Producing Molded Bodies from Proteins |
| CN101660215A (en) * | 2009-09-23 | 2010-03-03 | 陈福库 | Protein and cellulose composite fiber and manufacturing method thereof |
| US7682539B1 (en) * | 2006-01-11 | 2010-03-23 | The United States Of America As Represented By The Secretary Of The Air Force | Regeneration of silk and silk-like fibers from ionic liquid spin dopes |
| CN102493020A (en) * | 2011-12-06 | 2012-06-13 | 山东海龙股份有限公司 | Regenerated animal micro powder protein cellulose fiber and preparation method thereof |
-
2013
- 2013-03-07 CN CN201310072813.7A patent/CN103102695B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1660901A (en) * | 2004-12-24 | 2005-08-31 | 中国科学院长春应用化学研究所 | Method for preparing solution of keratin |
| CN1884641A (en) * | 2005-06-21 | 2006-12-27 | 中国科学院过程工程研究所 | Method for preparing regenerated protein fiber using ion liquid dissolving animal hair |
| CN1884642A (en) * | 2005-06-21 | 2006-12-27 | 中国科学院过程工程研究所 | Biological protein hair fiber preparation method by dissolving animal hair and cellulose material mixture |
| US7682539B1 (en) * | 2006-01-11 | 2010-03-23 | The United States Of America As Represented By The Secretary Of The Air Force | Regeneration of silk and silk-like fibers from ionic liquid spin dopes |
| US20090051068A1 (en) * | 2006-01-12 | 2009-02-26 | Thüringisches Institute Für Textil-Und Kunststoff-Forschung E.V. | Method for Producing Molded Bodies from Proteins |
| CN101660215A (en) * | 2009-09-23 | 2010-03-03 | 陈福库 | Protein and cellulose composite fiber and manufacturing method thereof |
| CN102493020A (en) * | 2011-12-06 | 2012-06-13 | 山东海龙股份有限公司 | Regenerated animal micro powder protein cellulose fiber and preparation method thereof |
Non-Patent Citations (12)
| Title |
|---|
| .天然蛋白质材料在离子液体中的溶解与再生.《丝绸》.2008,(第2008年 05期),全文. * |
| 再生蛋白纤维的研制及性能分析;奚柏君;《中国优秀硕士学位论文全文数据库》;20031001;第10-12页，2.4.4节至2.4.5节 * |
| 咪唑类离子液体用于羊毛纤维的溶解及角蛋白溶液的应用研究;王明;《中国优秀硕士学位论文全文数据库》;20101001;摘要 * |
| 奚柏君.再生蛋白纤维的研制及性能分析.《中国优秀硕士学位论文全文数据库》.2003,第10-12页，2.4.4节至2.4.5节. |
| 张玉梅 * |
| 王华平 * |
| 王强 * |
| 王明.咪唑类离子液体用于羊毛纤维的溶解及角蛋白溶液的应用研究.《中国优秀硕士学位论文全文数据库》.2010,摘要. |
| 程凌燕 * |
| 范雪荣.离子液体在纺织中的应用.《印染》.2008,(第2008年第7期),44-47. * |
| 袁久刚 * |
| 谢桂军 * |
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