CN102816224B - Hair keratin solution for spinning, preparation method and application thereof - Google Patents
Hair keratin solution for spinning, preparation method and application thereof Download PDFInfo
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- CN102816224B CN102816224B CN201210273538.0A CN201210273538A CN102816224B CN 102816224 B CN102816224 B CN 102816224B CN 201210273538 A CN201210273538 A CN 201210273538A CN 102816224 B CN102816224 B CN 102816224B
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Abstract
The invention relates to a hair keratin solution for spinning, a preparation method and application of the hair keratin solution. The preparation method comprises the steps of washing hair and removing impurities; adding into alkaline solution for dissolving; slowly adding 15-20% hydrochloric acid into the dissolved hair protein solution, to neutralize the solution to pH of 7.5-8.5; performing centrifugal separation; clarifying and filtering; and performing ultrafiltration to remove salt and small molecular compounds, to obtain hair keratin solution for spinning hair keratin composite fiber. The preparation method adopts low-grade hair as material to prepare keratin solution for spinning hair keratin composite fiber through dissolving and purification. The prepared keratin solution can be directly used for spinning protein fiber, and has broad development and application prospect.
Description
Technical field
The present invention relates to hair protein matter solution for a kind of spinning, also relate to a kind of preparation method and application of this protein soln simultaneously, belong to the comprehensive utilization field of hair raw material.
Technical background
Keratin sulfate (Keratin) claim again insoluble fibrin, be form that horn matter comprises hair, sends out, plumage, first, angle, hoof, squama etc.In hair, the molecular structure of keratin protein is very tight, laterally crosslinked by chemical bonds such as disulfide linkage between protein molecule segment, makes it have cyberspace structure, therefore can not be dissolved in usual vehicle, shows feature not soluble, not melting.Hair-keratin matter is dissolved, will first destroy disulfide linkage between keratin molecule, hydrogen bond etc., generally can adopt highly basic dissolution method, oxidation style dissolving, reduction method dissolving etc.
Summary of the invention
The object of the present invention is to provide hair protein matter solution for a kind of spinning, to reduce costs, improve solvability.
Meanwhile, the present invention also aims to provide the preparation method of a kind of spinning with hair protein matter solution.
Further, the present invention also aims to provide a kind of spinning application as spinning protein fibre aspect with hair protein matter solution.
To achieve these goals, technical scheme of the present invention has adopted hair protein matter solution for a kind of spinning, by following methods, is prepared: (1) hair cleans and removal of impurities; (2) hair after cleaning and removal of impurities is joined in alkali lye and dissolved; (3) with the dilute hydrochloric acid of concentration 15～20%, slowly join while stirring in the hair protein matter solution that step (2) dissolved, be neutralized to pH=7.5～8.5; (4) centrifugation: the protein liquid after neutralization is carried out to centrifugation, remove solid impurities more than 5 μ m, obtain purer hair protein matter solution; (5) clarification filtration: add flocculating aids in the hair protein matter solution making in step (4), carry out essence filter, obtain the protein soln of clear; (6) ultrafiltration desalination and filtering micromolecular compound: the ultra-filtration membrane of selecting molecular weight cut-off 3000～10000, remove more than 90% salinity and most micromolecular compound, make protein content in solution reach 6～10%, be met the hair-keratin matter solution for spinning of spinning hair-keratin matter conjugated fibre requirement.
The described hair of step (1) cleans and removal of impurities is: when adopted raw material is pig hair, after pig hair is dried, first remove the coffin in pig hair, the impurity that sandstone weight is larger, scurf in removing pig hair, impurity that sandy soil are tiny again, finally by length classifying machine, isolate longer dimension, bristles that economic worth is higher, remaining pig undercoat, then beat and wash through water unhairing machine, further remove impurity, can be used for extracting keratin protein.
In the water of described water unhairing machine, can add 0.1～0.5% sodium hydroxide, to remove the lipid impurity in hair, beat wash water and can be recycled after quartz sand filtration.
The described hair of step (1) cleans and removal of impurities is: when adopted raw material is human hair, first through removal of impurities, cleaning, minute chi, isolate longer dimension for purposes such as wig manufactures, the utility value of remaining size below 20～30mm is lower, can be directly used in extraction keratin protein.
The described hair of step (1) cleans and removal of impurities is: when adopted raw material is poultry feather: after first dryness in the sun, economy-combat is loose, selection by winnowing is gone out the larger sandstone impurity of weight, through water unhairing machine, beat and wash again, further remove impurity, can be used for extracting keratin protein.
The described hair of step (1) can, for the tankage of woollen mill and mao short flannel that lands, can be directly used in extraction keratin protein without removal of impurities.
Alkali lye in step (2) is prepared by following methods: in water, add sodium hydroxide to be mixed with 2.5～5% alkali lye, then add the sulphite of hair dry weight 2～10% or/and sulfhydryl compound is heated to 80～98 ℃.
Described sulphite is any in S-WAT, sodium bisulfite, potassium sulfite, Potassium hydrogen sulfite.
Described sulfhydryl compound can be selected any in Thiovanic acid, Thioglycolic acid sodium salt, mercaptoethanol, halfcystine.
In step (2), the dissolving of hair is: the add-on of alkali lye is 5～10 times of hair dry weight, after solution adds, should make temperature remain on 80-85 ℃, and after 5-10 minute, hair starts to dissolve, stirring and dissolving 30～120 minutes.
Flocculating aids in described (5) is diatomite or perlite, and diatomite or the perlite addition in protein soln is 20～150 grams per liters.
Technical scheme of the present invention has also adopted the preparation method of hair protein matter solution for a kind of spinning, comprises the following steps: (1) hair cleans and removal of impurities; (2) hair after cleaning and removal of impurities is joined in alkali lye and dissolved; (3) with the dilute hydrochloric acid of concentration 15～20%, slowly join while stirring in the hair protein matter solution that step (2) dissolved, be neutralized to pH=7.5～8.5; (4) centrifugation: the protein liquid after neutralization is carried out to centrifugation, remove solid impurities more than 5 μ m, obtain purer hair protein matter solution; (5) clarification filtration: add flocculating aids in the hair protein matter solution making in step (4), carry out essence filter, obtain the protein soln of clear; (6) ultrafiltration desalination and filtering micromolecular compound: the ultra-filtration membrane of selecting molecular weight cut-off 3000～10000, remove more than 90% salinity and most micromolecular compound, make protein content in solution reach 6～10%, be met the hair-keratin matter solution for spinning of spinning hair-keratin matter conjugated fibre requirement.
Technical scheme of the present invention has also adopted a kind of spinning application as spinning protein fibre aspect with hair protein matter solution.
The present invention is that employing waste-low-grade hair is raw material, through dissolving, purifying, makes its keratin protein solution, for spinning hair-keratin matter conjugated fibre.Hair raw material comprises: extract pig undercoat after bristles, human hair hair wastes, woollen mill's tankage (land hair), poultry feather etc., these raw material use propertieies are poor, economic worth is low, the keratin protein solution of making, directly applies to spinning protein fibre, has good exploitation prospect.
Adopt method of the present invention, protein soln after ultrafiltration can be directly used in spinning hair-keratin matter conjugated fibre, reduced the technological process of protein dissolving, filtration, reduced production cost, and because purification precision is high, can improve stoste stability when spinning hair-keratin matter conjugated fibre, reduce filter and spinning jet and change number of times and improve stoste utilization ratio, the final yield rate that improves product, can obtain better economic benefit.
Method simple practical of the present invention, adopts that alkali with low cost is molten, the method for preparing keratin solution of UF membrane sepn, and the protein soln of making can be directly used in spinning keratin protein conjugated fibre.Adopting low-grade hair is raw material, is dissolved and further deep processing and utilization.Hair raw material comprises: extract pig undercoat after bristles, human hair hair wastes, woollen mill's tankage (land hair), poultry feather etc., these raw material use propertieies are poor, economic worth is low, greatly reduce cost.
Embodiment
Embodiment 1
Hair protein matter solution for the spinning of the present embodiment, by following methods, prepare and obtain:
The wet pig hair of 1000kg of take after removal of impurities, cleaning, dehydration is example, its average moisture content approximately 33～34%, and pure pig hair content approximately 65% is 650kg.Its keratin protein extracting method is as follows:
1) Alkali liquid compounding: to adding 4000 premium on currency (6.15 times that pig hair shaft is heavy) in the alkali liquor preparing tank of 10000 liters, then add 120kg sodium hydroxide, 30kg S-WAT to be mixed with sodium hydrate content to be 2.9% solution, to be heated to 95 ℃;
2) hair dissolves: the wet pig hair 1000kg that adds removal of impurities, cleaning in hair dissolving vessel, add again above-mentioned whole mixing solutions, solution adds rear temperature to remain on 80 ℃, after 10 minutes, hair starts to dissolve, opening whipping appts stirs, dissolve after 30 minutes, sampling is observed, to all dissolvings (approximately more than 90% dissolving) substantially of pig hair;
3) neutralization: the dilute hydrochloric acid by concentration 15%, slowly join while stirring in the hair protein matter solution that above-mentioned dissolving is good, be neutralized to pH=7.5;
4) centrifugation: more than 3000 horizontal screw centrifuges carries out centrifugation to the protein liquid after neutralization by separating factor, removes solid impurities more than 5 μ m, obtains approximately 4600 liters of purer hair protein matter solution; Filtrate can room temperature be placed 1 day.
5) clarification filtration: add the super-cell of 200kg in protein soln, carry out essence filter with diatomite filter, Ex-all impurity, obtains the protein soln of clear;
6) ultrafiltration desalination and filtering micromolecular compound: use W-UF cross-flow ultrafiltration system, select the ultra-filtration membrane of molecular weight cut-off 5000, remove more than 90% salinity and most micromolecular compound, make protein content in solution reach 8%, be met the hair-keratin matter solution of spinning hair-keratin matter conjugated fibre requirement.
Embodiment 2
Hair protein matter solution for the spinning of the present embodiment, by following methods, prepare and obtain:
The wet human hair of 1000kg of take after removal of impurities, cleaning, dehydration is example, its average moisture content approximately 31～32%, and pure human hair content approximately 67% is 670kg.Its keratin protein extracting method is as follows:
1) Alkali liquid compounding: to adding 4000 premium on currency (human hair dry weight 5.97 times) in the alkali liquor preparing tank of 10000 liters, then add 120kg sodium hydroxide, 30kg Thioglycolic acid sodium salt to be mixed with sodium hydrate content to be 2.9% solution, to be heated to 90 ℃;
2) hair dissolves: the wet human hair 1000kg that adds removal of impurities, cleaning in hair dissolving vessel, add again above-mentioned whole mixing solutions, solution adds rear temperature to remain on 78 ℃, after 10 minutes, hair starts to dissolve, opening whipping appts stirs, dissolve after 30 minutes, sampling is observed, to human hair all dissolvings (approximately more than 90% dissolving) substantially;
Other step is with embodiment 1.
Embodiment 3
Hair protein matter solution for the spinning of the present embodiment, by following methods, prepare and obtain:
The wet poultry feather of 1250kg of take after removal of impurities, cleaning, dehydration is example, its average moisture content approximately 42～45%, and pure feather content approximately 52% is 650kg.Its keratin protein extracting method is as follows:
1) Alkali liquid compounding: to adding 3600 premium on currency (feather dry weight 6.15 times) in the alkali liquor preparing tank of 10000 liters, then add 120kg sodium hydroxide, 30kg sodium bisulfite to be mixed with sodium hydrate content to be 3.3% solution, to be heated to 98 ℃;
2) hair dissolves: the wet feather 1250kg that adds removal of impurities, cleaning in hair dissolving vessel, add again above-mentioned whole mixing solutions, solution adds rear temperature to remain on 78 ℃, after 10 minutes, hair starts to dissolve, opening whipping appts stirs, dissolve after 30 minutes, sampling is observed, to feather all dissolvings (dissolve approximately 90% left and right) substantially;
Other step is with embodiment 1.
Claims (9)
1. a hair protein matter solution for spinning, is characterized in that: by following methods, prepared: (1) hair cleans and removal of impurities; (2) hair after cleaning and removal of impurities is joined in alkali lye and dissolved; (3) with the dilute hydrochloric acid of concentration 15～20%, slowly join while stirring in the hair protein matter solution that step (2) dissolved, be neutralized to pH=7.5～8.5; (4) centrifugation: the protein liquid after neutralization is carried out to centrifugation, remove solid impurities more than 5 μ m, obtain purer hair protein matter solution; (5) clarification filtration: add flocculating aids in the hair protein matter solution making in step (4), carry out essence filter, obtain the protein soln of clear; (6) ultrafiltration desalination and filtering micromolecular compound: the ultra-filtration membrane of selecting molecular weight cut-off 3000～10000, remove more than 90% salinity and most micromolecular compound, make protein content in solution reach 6～10%, be met the hair-keratin matter solution for spinning of spinning hair-keratin matter conjugated fibre requirement;
Described alkali lye is prepared by following methods: in water, add sodium hydroxide to be mixed with 2.5～5% alkali lye, then add the sulphite of hair dry weight 2～10% or/and sulfhydryl compound is heated to 80～98 ℃.
2. a preparation method for hair protein matter solution for spinning, is characterized in that: comprise the following steps:
(1) hair cleans and removal of impurities;
(2) hair after cleaning and removal of impurities is joined in alkali lye and dissolved;
(3) with the dilute hydrochloric acid of concentration 15～20%, slowly join while stirring in the hair protein matter solution that step (2) dissolved, be neutralized to pH=7.5～8.5;
(4) centrifugation: the protein liquid after neutralization is carried out to centrifugation, remove solid impurities more than 5 μ m, obtain purer hair protein matter solution;
(5) clarification filtration: add flocculating aids in the hair protein matter solution making in step (4), carry out essence filter, obtain the protein soln of clear;
(6) ultrafiltration desalination and filtering micromolecular compound: the ultra-filtration membrane of selecting molecular weight cut-off 3000～10000, remove more than 90% salinity and most micromolecular compound, make protein content in solution reach 6～10%, be met the hair-keratin matter solution for spinning of spinning hair-keratin matter conjugated fibre requirement;
Alkali lye in step (2) is prepared by following methods: in water, add sodium hydroxide to be mixed with 2.5～5% alkali lye, then add the sulphite of hair dry weight 2～10% or/and sulfhydryl compound is heated to 80～98 ℃.
3. the preparation method of hair protein matter solution for spinning according to claim 2, it is characterized in that: the described hair of step (1) cleans and removal of impurities is: when adopted raw material is pig hair, after pig hair is dried, first remove the coffin in pig hair, the impurity that sandstone weight is larger, scurf in removing pig hair, impurity that sandy soil are tiny again, finally by length classifying machine, isolate longer dimension, bristles that economic worth is higher, remaining pig undercoat, through water unhairing machine, beat and wash again, further remove impurity, for extracting keratin protein.
4. the preparation method of hair protein matter solution for spinning according to claim 2, it is characterized in that: the described hair of step (1) cleans and removal of impurities is: when adopted raw material is human hair, first through removal of impurities, cleaning, minute chi, that isolates longer dimension manufactures purposes for wig, the utility value of remaining size below 20～30mm is lower, is directly used in extraction keratin protein.
5. the preparation method of hair protein matter solution for spinning according to claim 2, it is characterized in that: the described hair of step (1) cleans and removal of impurities is: when adopted raw material is poultry feather: after first dryness in the sun, economy-combat pine, selection by winnowing are removed the sandstone impurity that weight is larger, through water unhairing machine, beat and wash again, further remove impurity, for extracting keratin protein.
6. the preparation method of hair protein matter solution for spinning according to claim 2, is characterized in that: described sulphite is any in S-WAT, sodium bisulfite, potassium sulfite, Potassium hydrogen sulfite.
7. the preparation method of hair protein matter solution for spinning according to claim 2, is characterized in that: described sulfhydryl compound is selected any in Thiovanic acid, Thioglycolic acid sodium salt, mercaptoethanol, halfcystine.
8. the preparation method of hair protein matter solution for spinning according to claim 2, it is characterized in that: in step (2), the dissolving of hair is: the add-on of alkali lye is 5～10 times of hair dry weight, after adding, solution should make temperature remain on 80-85 ℃, after 5-10 minute, hair starts to dissolve, stirring and dissolving 30～120 minutes.
9. spinning as claimed in claim 1 application as spinning protein fibre aspect with hair protein matter solution.
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| JP5998195B2 (en) * | 2014-12-25 | 2016-09-28 | 神奈川県 | Hair extract composition, film, and molded article |
| CN107502982B (en) * | 2017-08-31 | 2021-03-30 | 四川大学 | Preparation method of feather keratin viscose fiber |
| CN108837703B (en) * | 2018-07-16 | 2021-02-09 | 五邑大学 | Preparation method of water-alcohol separation membrane |
| CN110106706A (en) * | 2019-05-23 | 2019-08-09 | 叶盛 | A kind of preparation method of modified protein UV resistance finishing agent |
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| CN1693371A (en) * | 2004-05-07 | 2005-11-09 | 香港理工大学 | Nano woolen emulsion and powder, its preparation process and application |
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| CN1693371A (en) * | 2004-05-07 | 2005-11-09 | 香港理工大学 | Nano woolen emulsion and powder, its preparation process and application |
Non-Patent Citations (4)
| Title |
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| 夏永林.羽毛蛋白的提取及其提取物特性分析.《国外丝绸》.2007,(第2期), |
| 羽毛蛋白的提取及其提取物特性分析;夏永林;《国外丝绸》;20071231(第2期);第16-17、20页 * |
| 角蛋白的分子构成、提取及应用;贾如琰等;《化学通报》;20081231(第4期);第265-271页 * |
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Denomination of invention: Hair keratin solution for spinning, preparation method and application thereof Effective date of registration: 20140514 Granted publication date: 20140402 Pledgee: Henan Baosight private science and Technology Investment Company Limited Pledgor: Shanghai Quanyu Biological Science and Technology Suiping Co., Ltd. Registration number: 2014990000353 |
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Date of cancellation: 20160719 Granted publication date: 20140402 Pledgee: Henan Baosight Silicon Valley Technology Investment Limited Pledgor: Shanghai Quanyu Biological Science and Technology Suiping Co., Ltd. Registration number: 2014990000353 |
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Change date: 20160719 Registration number: 2014990000353 Pledgee after: Henan Baosight Silicon Valley Technology Investment Limited Pledgee before: Henan Baosight private science and Technology Investment Company Limited |