CN107190349B - Method for preparing nanofiber by using yak hair - Google Patents
Method for preparing nanofiber by using yak hair Download PDFInfo
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- CN107190349B CN107190349B CN201710324144.6A CN201710324144A CN107190349B CN 107190349 B CN107190349 B CN 107190349B CN 201710324144 A CN201710324144 A CN 201710324144A CN 107190349 B CN107190349 B CN 107190349B
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- 210000004209 hair Anatomy 0.000 title claims abstract description 142
- 239000002121 nanofiber Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 34
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- 108010076876 Keratins Proteins 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000003756 stirring Methods 0.000 claims abstract description 42
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- 230000009467 reduction Effects 0.000 claims abstract description 27
- 238000009987 spinning Methods 0.000 claims abstract description 19
- BYEAHWXPCBROCE-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-ol Chemical compound FC(F)(F)C(O)C(F)(F)F BYEAHWXPCBROCE-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229920002635 polyurethane Polymers 0.000 claims abstract description 17
- 239000004814 polyurethane Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 230000020477 pH reduction Effects 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims description 31
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 24
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 18
- 239000012530 fluid Substances 0.000 claims description 18
- 238000000502 dialysis Methods 0.000 claims description 16
- 239000000706 filtrate Substances 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 14
- 239000012425 OXONE® Substances 0.000 claims description 12
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 12
- 239000004202 carbamide Substances 0.000 claims description 12
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 12
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims description 11
- GCHCGDFZHOEXMP-UHFFFAOYSA-L potassium adipate Chemical compound [K+].[K+].[O-]C(=O)CCCCC([O-])=O GCHCGDFZHOEXMP-UHFFFAOYSA-L 0.000 claims description 9
- 239000001608 potassium adipate Substances 0.000 claims description 9
- 235000011051 potassium adipate Nutrition 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 239000011888 foil Substances 0.000 claims description 8
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 8
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- 235000010233 benzoic acid Nutrition 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 7
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- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims description 7
- 235000011082 potassium citrates Nutrition 0.000 claims description 7
- OKBMCNHOEMXPTM-UHFFFAOYSA-M potassium peroxymonosulfate Chemical compound [K+].OOS([O-])(=O)=O OKBMCNHOEMXPTM-UHFFFAOYSA-M 0.000 claims description 7
- 238000007710 freezing Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 239000000835 fiber Substances 0.000 abstract description 14
- 238000000605 extraction Methods 0.000 abstract description 7
- 239000000243 solution Substances 0.000 description 53
- 210000002268 wool Anatomy 0.000 description 28
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- 238000004108 freeze drying Methods 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- HJKYXKSLRZKNSI-UHFFFAOYSA-I pentapotassium;hydrogen sulfate;oxido sulfate;sulfuric acid Chemical compound [K+].[K+].[K+].[K+].[K+].OS([O-])(=O)=O.[O-]S([O-])(=O)=O.OS(=O)(=O)O[O-].OS(=O)(=O)O[O-] HJKYXKSLRZKNSI-UHFFFAOYSA-I 0.000 description 5
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- 241000282849 Ruminantia Species 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- -1 bisulfite ions Chemical class 0.000 description 1
- 210000000085 cashmere Anatomy 0.000 description 1
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- 239000003638 chemical reducing agent Substances 0.000 description 1
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- 230000003628 erosive effect Effects 0.000 description 1
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- 235000019441 ethanol Nutrition 0.000 description 1
- 238000009950 felting Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- 210000004919 hair shaft Anatomy 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
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- 244000144972 livestock Species 0.000 description 1
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- 230000028327 secretion Effects 0.000 description 1
- 239000011492 sheep wool Substances 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/46—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from vertebrates
- C07K14/47—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from vertebrates from mammals
-
- 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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/46—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from vertebrates
- C07K14/47—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from vertebrates from mammals
- C07K14/4701—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from vertebrates from mammals not used
- C07K14/4741—Keratin; Cytokeratin
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Genetics & Genomics (AREA)
- Medicinal Chemistry (AREA)
- Molecular Biology (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- General Health & Medical Sciences (AREA)
- Biophysics (AREA)
- General Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- Mechanical Engineering (AREA)
- Toxicology (AREA)
- Zoology (AREA)
- Gastroenterology & Hepatology (AREA)
- Cosmetics (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides a method for preparing nano-fibers by using yak hair, which comprises the following steps: cleaning yak hair with water for several times, removing impurities, spin-drying with a centrifuge, and drying for later use; crushing the dried yak hair by a hair crusher; putting the crushed yak hair into an acidification treatment solution and a pretreatment solution in sequence for treatment; putting yak hair into reduction treatment liquid for treatment to obtain keratin powder; dissolving keratin powder in hexafluoroisopropanol, adding a certain amount of polyurethane, stirring at the temperature of 20-25 ℃ for 10-15 minutes, adding a certain amount of epoxy acrylate, uniformly mixing, heating to 60-80 ℃, and then continuously stirring for 1 hour to obtain a spinning solution; and (4) carrying out electrostatic spinning by using the obtained spinning solution. The invention effectively solves the problems of low keratin extraction rate and poor fiber forming quality of the existing yak hair nano fiber.
Description
Technical Field
The invention relates to the technical field of nanofiber preparation, in particular to a method for preparing nanofibers by using yak hair.
Background
Animal fibers are also known as protein fibers because their major constituent is protein. Animal fibers are divided into three categories: the main sources of the hair and down of animals, the down and feather of poultry and silk are artificially raised animals.
Animal hair is of many kinds, and the most important is sheep wool, wool for short. Wool is widely used in the manufacture of various textiles, as well as in the manufacture of felts. Besides wool, there are cashmere, rabbit hair, camel hair, yak hair, etc. Animal hair other than wool, sometimes collectively referred to as specialty animal hair, is also used to make textiles, either as pure or blended with other fibers. In blending, the warmth retention property and the hand feeling of the fabric can be improved by utilizing the special luster, fineness and softness of the fabric. The down feather and feather of poultry can be blended with other fibers in textile, and can also be used as filling materials, such as duck down, goose down and the like. The silk is gland secretion of silkworm, and includes mulberry silk, tussah silk, castor-oil plant silk, rhizoma dioscoreae silk, etc.
Taking wool as an example, wool is a natural fiber with relatively high utilization value. Wool is one of the most imported products in domestic animal products, the current import accounts for 2/3 of the domestic wool yield, and the wool becomes one of the largest world-wide wool-importing countries, and compared with the imported wool, the domestic wool is inferior in quality, short and thick in wool, and has no competitiveness in the international market. This causes a lot of inferior wool to be produced in domestic wool processing and use, and if these waste wools are discarded, it is a waste of resources undoubtedly, and it will also cause pollution to the environment. If these waste resources can be recycled, not only can the current situation of wool resource shortage be relieved, but also reference can be provided for the recycling of other animal hair.
For a long time, the related research is mostly spread around wool, and the research on wool recycling can be divided into two aspects in general: on one hand, the value of the wool is improved by fully utilizing the technical means; on the other hand, the regeneration theory is researched, the fibrous regeneration of the wool keratin is realized, and the expected wool keratin modified viscose fiber is obtained. The regeneration technology of wool keratin has been widely studied at present, most of the technologies are used for dissolving waste wool by a chemical method to prepare wool keratin solution, and the selection of proper solvent and dissolving conditions is the key for preparing the wool keratin solution. At present, the mode of preparing keratin stock solution by animal hair mostly adopts a urea/sodium sulfide/SDS process, namely, a mixed system of sodium sulfide, urea and sodium dodecyl sulfate is taken as a solvent, the animal hair to be treated is put into the mixed solution, and the keratin solution with a certain concentration is prepared after dissolution and filtration.
Yak is a special cattle species in alpine regions, and is a herbivorous ruminant livestock. Mainly produced in the area with the altitude of more than 3000 meters in Qinghai-Tibet plateau of China, the diameter of yak hair is more than 25 micrometers, the length can exceed 20 centimeters, the appearance is flat and straight, the surface is smooth, some have continuous hair pith, the toughness is hard and glossy, and the felting property is low. Yak hair fiber is mostly composed of a scale layer and a cortical layer, only contain few medullary layer, because yak's special living environment, compare in the loose arrangement of wool scale layer, yak hair's scale layer is more inseparable than the wool, the hair shaft is hugged closely to the scale, and its scale layer has the effect of relatively strong anti enzyme and chemical agent etching, the process of utilizing processing wool handles the yak hair and can only dissolve minute quantity keratin, the extraction rate of keratin is very low promptly, and then the cost of obtaining yak hair nanofiber is higher, the yak hair raw materials waste is more serious, a specific nanofiber preparation process to yak hair is needed urgently to be researched and developed.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for preparing nanofibers by using yak hair, and solves the problem that no special preparation process for the yak hair nanofibers exists in the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for preparing nano-fibers by using yak hair comprises the following steps:
step [1 ]: cleaning yak hair with water for several times, removing impurities, spin-drying with a centrifuge, and drying for later use;
step [2 ]: crushing the dried yak hair by a hair crusher;
step [3 ]: putting the crushed yak hair into an acidizing fluid, soaking for 20-30 minutes at 30-35 ℃, and dehydrating and drying;
step [4 ]: putting the yak hair subjected to acidification treatment and drying into a pretreatment solution, stirring for 8-10 minutes at 30-35 ℃, filtering, and washing with water until the pH value of the yak hair is neutral;
step [5 ]: putting the yak hair treated in the step (4) into reduction treatment liquid, stirring for 40-50 minutes at 35 ℃, heating to 100 ℃, soaking and dissolving for 1.2-2 hours, filtering, fully washing the yak hair which is not dissolved by distilled water, collecting filtrate and washing liquid, putting the filtrate and the washing liquid into a dialysis bag for dialysis, and then freezing and drying to obtain keratin powder;
step [6 ]: dissolving keratin powder in hexafluoroisopropanol, adding a certain amount of polyurethane, stirring at the temperature of 20-25 ℃ for 10-15 minutes, adding a certain amount of epoxy acrylate, uniformly mixing, heating to 60-80 ℃, and then continuously stirring for 1 hour to obtain a spinning solution;
step [7 ]: carrying out electrostatic spinning by using the obtained spinning solution, and receiving the nano-filaments by using an aluminum foil to obtain the blended nano-fiber;
further, the acidizing fluid consists of the following components in concentration: 5-8 g/L of sulfuric acid, 12-16 g/L of potassium citrate, 23-29 g/L of benzoic acid, 140-150 g of ethanol and the balance of water.
Further, the weight ratio of the acidizing fluid to the yak hair is 5-6: 1.
Further, the pretreatment liquid consists of the following components in concentration: 60-90 g/L potassium peroxymonosulfate, 10-15 g/L potassium hydroxide, 34-45 g/L polyethylene glycol, 5-7 g/L sodium lignosulfonate and the balance of water.
Further, the weight ratio of the pretreatment liquid to the yak hair is 5-8: 1-3.
Further, the reduction treatment liquid consists of the following components in concentration: 30-38/38 g g/L of sodium sulfide, 280-320 g/L of urea, 12-15 g/L of sodium dodecyl sulfate, 12-18 g/L of potassium adipate, 18-23 g/L of butanol and the balance of water.
Further, the weight ratio of the reduction treatment solution to the yak hair is 20-30: 1.
Further, in the step [5], the mass ratio of the keratin powder, the hexafluoroisopropanol, the polyurethane and the epoxy acrylate is 1: 2-3: 1-1.5: 0.17-0.19.
Furthermore, the length of the yak hair crushed by the hair crusher is 1-3 mm.
The invention has the following positive effects:
1. according to the method, the yak hair is firstly subjected to acidification treatment, a mixed system of sulfuric acid, potassium citrate, benzoic acid, ethanol and water is adopted, the scale layer on the surface of yak hair fibers can be moderately eroded, the compactness of the scale layer is effectively reduced, the scale layer is loose and easy to strip, excessive erosion is not carried out on the scale layer, and the structure below the scale layer is prevented from being damaged.
2. The invention adds a pretreatment step before the reduction treatment process, adopts a combined system of potassium monopersulfate/potassium hydroxide/polyethylene glycol/sodium lignosulfonate, and crushes yak hair before the pretreatment so as to carry out better oxidation treatment on the yak hair, wherein compared with the traditional condition of singly adopting potassium monopersulfate, the treatment liquid is added with polyhydroxy structural compound polyethylene glycol and simultaneously added with sodium lignosulfonate. We find in the initial stage of research that when single potassium monopersulfate is used, oxidation treatment is firstly carried out on yak hair contacted with yak hair at the initial stage when the yak hair is added, transition stripping damage is easily generated on a scale layer on the surface of yak hair fiber at the moment, and then keratin is oxidized, and the extraction rate and the extraction quality of keratin are finally affected, so that the invention adds the polyethylene glycol with high viscosity which belongs to polymer class on the basis of the potassium monopersulfate, because the polyethylene glycol generates stronger complexing effect in the oxidation treatment process and has high viscosity, a sticky film layer is easily formed on the surface of the yak hair fiber, transition damage to the surface of the yak hair is better prevented, the oxidation process of the potassium monopersulfate on the yak hair is milder, oxidation of the keratin is powerfully reduced while the scale layer on the surface of the yak hair fiber is effectively stripped, provides a powerful basis for improving the extraction rate and the extraction quality of the keratin.
3. The reduction treatment solution adopts a combined system of sodium sulfide/urea/sodium dodecyl sulfate/potassium adipate/butanol, namely, potassium adipate and butanol are added on the basis of the traditional sodium sulfide/urea/SDS, and a higher-content reducing agent sodium bisulfite is adopted, wherein the potassium adipate is used as a complex corrosion inhibitor of a low-hydroxyl structure (compared with polyethylene glycol in a pretreatment solution), the butanol is used as a corrosion inhibition regulator, and the two are combined to jointly restrict bisulfite ions in the solution, so that the total extraction rate of keratin is improved while the keratin is dissolved.
4. According to the invention, a keratin powder/polyurethane/epoxy acrylate combined system is used as a spinning solution, especially the addition of epoxy acrylate, so that lateral cross-linking points among macromolecules are effectively reduced, a keratin molecular structure and a keratin molecular conformation are converted, and the acting force among molecular mechanisms is effectively increased together with polyurethane, the thermal stability of the molecular structure is improved, the filament forming uniformity is effectively improved, and the fiber forming quality of keratin is effectively improved.
Detailed Description
The following is a detailed description of preferred embodiments of the invention.
Example 1
The preferred embodiment 1 of the invention provides a method for preparing nano fibers by using yak hair, which comprises the following steps:
step [1 ]: cleaning yak hair with water for several times, removing impurities, spin-drying with a centrifuge, and drying for later use;
step [2 ]: crushing the dried yak hair to 2mm by a hair crusher;
step [3 ]: putting the crushed yak hair into an acidizing fluid, soaking for 20-30 minutes at 30-35 ℃, and dehydrating and drying;
wherein the acidizing fluid consists of the following components in concentration: 7g/L sulfuric acid, 14g/L potassium citrate, 25g/L benzoic acid, 145g ethanol and the balance of water; the weight ratio of the acidizing fluid to the yak hair is 6: 1.
Step [4 ]: putting the yak hair subjected to acidification treatment and drying into the pretreatment liquid, stirring for 10 minutes at 35 ℃, filtering, and washing with water until the pH value of the yak hair is neutral;
the pretreatment liquid comprises the following components in concentration: 750g/L potassium peroxymonosulfate, 12g/L potassium hydroxide, 37g/L polyethylene glycol, 6g/L sodium lignosulfonate and the balance of water;
the weight ratio of the pretreatment liquid to the yak hair is 8: 1.
Step [5 ]: putting the yak hair treated in the step [4] into a reduction treatment solution (wherein the reduction treatment solution comprises the following components in concentration of 33/33 g g per liter of sodium sulfide, 289g/L of urea, 13.5g/L of sodium dodecyl sulfate, 13.4g/L of potassium adipate and 20g/L of butanol, the weight ratio of the reduction treatment solution to the yak hair is 30:1), stirring at 35 ℃ for 45 minutes, heating to 100 ℃, soaking and dissolving for 1.5 hours, filtering, sufficiently washing the undissolved yak hair with distilled water, collecting filtrate and water washing solution, mixing and weighing, putting into a dialysis bag for dialysis, freeze-drying to obtain keratin powder, weighing, and calculating to obtain the mass fraction of the keratin in the mixed solution (the filtrate and the water washing solution) to be 3.67%.
Step [6 ]: dissolving keratin powder in hexafluoroisopropanol, then adding a certain amount of polyurethane and stirring, stirring at the temperature of 20 ℃, stirring for 15 minutes, then adding a certain amount of epoxy acrylate, uniformly mixing, heating to 80 ℃, and then continuously stirring for 1 hour to obtain a spinning solution; wherein the mass ratio of the keratin powder to the hexafluoroisopropanol to the polyurethane to the epoxy acrylate is 1:3:1: 0.18.
Step [7 ]: and (3) carrying out electrostatic spinning by using the obtained spinning solution, and receiving the nano-filaments by using an aluminum foil to obtain the blended nano-fiber. And randomly selecting 100 obtained nanofibers, observing the nanofibers by using a scanning electron microscope, and calculating to obtain the nanofibers with the minimum diameter of 158nm, the maximum diameter of 438nm and the average diameter of 231 nm.
Example 2
The preferred embodiment 2 of the invention provides a method for preparing nano fibers by using yak hair, which comprises the following steps:
step [1 ]: cleaning yak hair with water for several times, removing impurities, spin-drying with a centrifuge, and drying for later use;
step [2 ]: crushing the dried yak hair to 2mm by a hair crusher;
step [3 ]: putting the crushed yak hair into the pretreatment liquid, stirring for 10 minutes at 35 ℃, filtering, and washing with water until the pH value of the yak hair is neutral;
the pretreatment liquid comprises the following components in concentration: 750g/L potassium peroxymonosulfate, 12g/L potassium hydroxide, 37g/L polyethylene glycol, 6g/L sodium lignosulfonate and the balance of water;
the weight ratio of the pretreatment liquid to the yak hair is 8: 1.
Step [4 ]: putting the yak hair treated in the step [3] into a reduction treatment solution (wherein the reduction treatment solution comprises the following components in concentration of 33/33 g g per liter of sodium sulfide, 289g/L of urea, 13.5g/L of sodium dodecyl sulfate, 13.4g/L of potassium adipate and 20g/L of butanol, the weight ratio of the reduction treatment solution to the yak hair is 30:1), stirring at 35 ℃ for 45 minutes, heating to 100 ℃, soaking and dissolving for 1.5 hours, filtering, sufficiently washing the undissolved yak hair with distilled water, collecting filtrate and water washing solution, mixing and weighing, putting into a dialysis bag for dialysis, freeze-drying to obtain keratin powder, weighing, and calculating to obtain the mass fraction of the keratin in the mixed solution (the filtrate and the water washing solution) to be 2.17%.
Step [5 ]: dissolving keratin powder in hexafluoroisopropanol, then adding a certain amount of polyurethane and stirring, stirring at the temperature of 20 ℃, stirring for 15 minutes, then adding a certain amount of epoxy acrylate, uniformly mixing, heating to 80 ℃, and then continuously stirring for 1 hour to obtain a spinning solution; wherein the mass ratio of the keratin powder to the hexafluoroisopropanol to the polyurethane to the epoxy acrylate is 1:3:1: 0.18.
Step [6 ]: and (3) carrying out electrostatic spinning by using the obtained spinning solution, and receiving the nano-filaments by using an aluminum foil to obtain the blended nano-fiber. And randomly selecting 100 obtained nanofibers, observing the nanofibers by using a scanning electron microscope, and calculating to obtain the nanofibers with the minimum diameter of 168nm, the maximum diameter of 480nm and the average diameter of 259 nm.
Example 3
The preferred embodiment 3 of the invention provides a method for preparing nano fibers by using yak hair, which comprises the following steps:
step [1 ]: cleaning yak hair with water for several times, removing impurities, spin-drying with a centrifuge, and drying for later use;
step [2 ]: crushing the dried yak hair to 2mm by a hair crusher;
step [3 ]: putting the crushed yak hair into an acidizing fluid, soaking for 20-30 minutes at 30-35 ℃, and dehydrating and drying;
wherein the acidizing fluid consists of the following components in concentration: 7g/L sulfuric acid, 14g/L potassium citrate, 25g/L benzoic acid, 145g ethanol and the balance of water; the weight ratio of the acidizing fluid to the yak hair is 6: 1.
Step [4 ]: putting the yak hair subjected to acidification treatment and drying into the pretreatment liquid, stirring for 10 minutes at 35 ℃, filtering, and washing with water until the pH value of the yak hair is neutral;
the pretreatment liquid comprises the following components in concentration: 750g/L potassium peroxymonosulfate, 12g/L potassium hydroxide and the balance of water;
the weight ratio of the pretreatment liquid to the yak hair is 8: 1.
Step [5 ]: putting the yak hair treated in the step [4] into a reduction treatment solution (wherein the reduction treatment solution comprises the following components in concentration of 33/33 g g per liter of sodium sulfide, 289g/L of urea, 13.5g/L of sodium dodecyl sulfate, 13.4g/L of potassium adipate and 20g/L of butanol, the weight ratio of the reduction treatment solution to the yak hair is 30:1), stirring at 35 ℃ for 45 minutes, heating to 100 ℃, soaking and dissolving for 1.5 hours, filtering, sufficiently washing the undissolved yak hair with distilled water, collecting filtrate and water washing solution, mixing and weighing, putting into a dialysis bag for dialysis, freeze-drying to obtain keratin powder, weighing, and calculating to obtain the mass fraction of the keratin in the mixed solution (the filtrate and the water washing solution) to be 2.26%.
Step [6 ]: dissolving keratin powder in hexafluoroisopropanol, then adding a certain amount of polyurethane and stirring, stirring at the temperature of 20 ℃, stirring for 15 minutes, then adding a certain amount of epoxy acrylate, uniformly mixing, heating to 80 ℃, and then continuously stirring for 1 hour to obtain a spinning solution; wherein the mass ratio of the keratin powder to the hexafluoroisopropanol to the polyurethane to the epoxy acrylate is 1:3:1: 0.18.
Step [7 ]: and (3) carrying out electrostatic spinning by using the obtained spinning solution, and receiving the nano-filaments by using an aluminum foil to obtain the blended nano-fiber. And randomly selecting 100 obtained nanofibers, observing the nanofibers by using a scanning electron microscope, and calculating to obtain the nanofibers with the minimum diameter of 118nm, the maximum diameter of 409nm and the average diameter of 252 nm.
Example 4
The preferred embodiment 4 of the invention provides a method for preparing nano fibers by using yak hair, which comprises the following steps:
step [1 ]: cleaning yak hair with water for several times, removing impurities, spin-drying with a centrifuge, and drying for later use;
step [2 ]: crushing the dried yak hair to 2mm by a hair crusher;
step [3 ]: putting the crushed yak hair into an acidizing fluid, soaking for 20-30 minutes at 30-35 ℃, and dehydrating and drying;
wherein the acidizing fluid consists of the following components in concentration: 7g/L sulfuric acid, 14g/L potassium citrate, 25g/L benzoic acid, 145g ethanol and the balance of water; the weight ratio of the acidizing fluid to the yak hair is 6: 1.
Step [4 ]: putting the yak hair subjected to acidification treatment and drying into the pretreatment liquid, stirring for 10 minutes at 35 ℃, filtering, and washing with water until the pH value of the yak hair is neutral;
the pretreatment liquid comprises the following components in concentration: 750g/L potassium peroxymonosulfate, 12g/L potassium hydroxide, 37g/L polyethylene glycol, 6g/L sodium lignosulfonate and the balance of water;
the weight ratio of the pretreatment liquid to the yak hair is 8: 1.
Step [5 ]: putting the yak hair treated in the step [4] into a reduction treatment solution (wherein the reduction treatment solution comprises the following components in concentration of 33/33 g g/L sodium sulfide, 289g/L urea and 13.5g/L sodium dodecyl sulfate, the weight ratio of the reduction treatment solution to the yak hair is 30:1), stirring for 45 minutes at 35 ℃, heating to 100 ℃, soaking and dissolving for 1.5 hours, filtering, fully washing the undissolved yak hair with distilled water, collecting filtrate and water washing solution, mixing and weighing, putting into a dialysis bag for dialysis, freezing and drying to obtain keratin powder, weighing, and calculating to obtain the keratin mass fraction in the mixed solution (filtrate and water washing solution) of 2.41%.
Step [6 ]: dissolving keratin powder in hexafluoroisopropanol, then adding a certain amount of polyurethane and stirring, stirring at the temperature of 20 ℃, stirring for 15 minutes, then adding a certain amount of epoxy acrylate, uniformly mixing, heating to 80 ℃, and then continuously stirring for 1 hour to obtain a spinning solution; wherein the mass ratio of the keratin powder, the hexafluoroisopropanol, the polyurethane and the epoxy acrylate is 1:3:1:0.18
Step [7 ]: and (3) carrying out electrostatic spinning by using the obtained spinning solution, and receiving the nano-filaments by using an aluminum foil to obtain the blended nano-fiber. And randomly selecting 100 obtained nanofibers, observing the nanofibers by using a scanning electron microscope, and calculating to obtain the nanofibers with the minimum diameter of 143nm, the maximum diameter of 534nm and the average diameter of 229 nm.
Example 5
The preferred embodiment 5 of the invention provides a method for preparing nano fibers by using yak hair, which comprises the following steps:
step [1 ]: cleaning yak hair with water for several times, removing impurities, spin-drying with a centrifuge, and drying for later use;
step [2 ]: crushing the dried yak hair to 2mm by a hair crusher;
step [3 ]: putting the crushed yak hair into an acidizing fluid, soaking for 20-30 minutes at 30-35 ℃, and dehydrating and drying;
wherein the acidizing fluid consists of the following components in concentration: 7g/L sulfuric acid, 14g/L potassium citrate, 25g/L benzoic acid, 145g ethanol and the balance of water; the weight ratio of the acidizing fluid to the yak hair is 6: 1.
Step [4 ]: putting the yak hair subjected to acidification treatment and drying into the pretreatment liquid, stirring for 10 minutes at 35 ℃, filtering, and washing with water until the pH value of the yak hair is neutral;
the pretreatment liquid comprises the following components in concentration: 750g/L potassium peroxymonosulfate, 12g/L potassium hydroxide, 37g/L polyethylene glycol, 6g/L sodium lignosulfonate and the balance of water;
the weight ratio of the pretreatment liquid to the yak hair is 8: 1.
Step [5 ]: putting the yak hair treated in the step [4] into a reduction treatment solution (wherein the reduction treatment solution comprises the following components in concentration of 33/33 g g per liter of sodium sulfide, 289g/L of urea, 13.5g/L of sodium dodecyl sulfate, 13.4g/L of potassium adipate and 20g/L of butanol, the weight ratio of the reduction treatment solution to the yak hair is 30:1), stirring at 35 ℃ for 45 minutes, heating to 100 ℃, soaking and dissolving for 1.5 hours, filtering, sufficiently washing the undissolved yak hair with distilled water, collecting filtrate and water washing solution, mixing and weighing, putting into a dialysis bag for dialysis, freeze-drying to obtain keratin powder, weighing, and calculating to obtain the mass fraction of the keratin in the mixed solution (the filtrate and the water washing solution) to be 3.63%.
Step [6 ]: dissolving keratin powder in hexafluoroisopropanol, then adding a certain amount of polyurethane and stirring, wherein the stirring temperature is 20 ℃, and stirring for 1.5 hours to obtain a spinning solution; wherein the mass ratio of the keratin powder to the hexafluoroisopropanol to the polyurethane is 1:3: 1.
Step [7 ]: and (3) carrying out electrostatic spinning by using the obtained spinning solution, and receiving the nano-filaments by using an aluminum foil to obtain the blended nano-fiber. And randomly selecting 100 obtained nanofibers, observing the nanofibers by using a scanning electron microscope, and calculating to obtain the nanofibers with the minimum diameter of 222nm, the maximum diameter of 693nm and the average diameter of 408 nm.
Example 6
The preferred embodiment 6 of the invention provides a method for preparing nano fibers by using yak hair, which comprises the following steps:
step [1 ]: cleaning yak hair with water for several times, removing impurities, spin-drying with a centrifuge, and drying for later use;
step [2 ]: crushing the dried yak hair to 2mm by a hair crusher;
step [3 ]: putting the crushed yak hair into a reduction treatment solution (wherein the reduction treatment solution comprises the following components in percentage by weight of 33/33 g g/L sodium sulfide, 289g/L urea and 13.5g/L sodium dodecyl sulfate, and the weight ratio of the reduction treatment solution to the yak hair is 30:1), stirring for 45 minutes at 35 ℃, heating to 100 ℃, soaking and dissolving for 1.5 hours, filtering, fully washing the undissolved yak hair with distilled water, collecting filtrate and water washing solution, mixing and weighing, putting into a dialysis bag for dialysis, freeze-drying to obtain keratin powder, weighing, and calculating to obtain the keratin mass fraction of 1.01% in the mixed solution (filtrate and water washing solution).
Step [4 ]: dissolving keratin powder in hexafluoroisopropanol, stirring at 20 ℃, and stirring for 1.5 hours to obtain a spinning solution; wherein the mass ratio of the keratin powder to the hexafluoroisopropanol is 1: 3.
Step [5 ]: and (3) carrying out electrostatic spinning by using the obtained spinning solution, and receiving the nano-filaments by using an aluminum foil to obtain the blended nano-fiber. And randomly selecting 100 obtained nanofibers, observing the nanofibers by using a scanning electron microscope, and calculating to obtain the nanofibers with the minimum diameter of 356nm, the maximum diameter of 1025nm and the average diameter of 764 nm.
The above embodiments are only preferred embodiments of the present invention, and it should be understood that the above embodiments are only for assisting understanding of the method and the core idea of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalents and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A method for preparing nano-fibers by using yak hair is characterized by comprising the following steps:
step [1 ]: cleaning yak hair with water for several times, removing impurities, spin-drying with a centrifuge, and drying for later use;
step [2 ]: crushing the dried yak hair by a hair crusher;
step [3 ]: putting the crushed yak hair into an acidizing fluid, soaking for 20-30 minutes at 30-35 ℃, and dehydrating and drying;
step [4 ]: putting the yak hair subjected to acidification treatment and drying into a pretreatment solution, stirring for 8-10 minutes at 30-35 ℃, filtering, and washing with water until the pH value of the yak hair is neutral; the pretreatment liquid comprises the following components in concentration: 60-90 g/L potassium peroxymonosulfate, 10-15 g/L potassium hydroxide, 34-45 g/L polyethylene glycol, 5-7 g/L sodium lignosulfonate and the balance of water;
step [5 ]: putting the yak hair treated in the step (4) into reduction treatment liquid, stirring for 40-50 minutes at 35 ℃, heating to 100 ℃, soaking and dissolving for 1.2-2 hours, filtering, fully washing the yak hair which is not dissolved by distilled water, collecting filtrate and washing liquid, putting the filtrate and the washing liquid into a dialysis bag for dialysis, and then freezing and drying to obtain keratin powder;
step [6 ]: dissolving keratin powder in hexafluoroisopropanol, adding a certain amount of polyurethane, stirring at the temperature of 20-25 ℃ for 10-15 minutes, adding a certain amount of epoxy acrylate, uniformly mixing, heating to 60-80 ℃, and then continuously stirring for 1 hour to obtain a spinning solution;
step [7 ]: and (3) carrying out electrostatic spinning by using the obtained spinning solution, and receiving the nano-filaments by using an aluminum foil to obtain the blended nano-fiber.
2. The method for preparing the nanofiber by using the yak hair as the claim 1, wherein the method comprises the following steps: the acidizing fluid consists of the following components in concentration: 5-8 g/L of sulfuric acid, 12-16 g/L of potassium citrate, 23-29 g/L of benzoic acid, 140-150 g of ethanol and the balance of water.
3. The method for preparing the nanofiber by using the yak hair as the claim 2, is characterized in that: the weight ratio of the acidizing fluid to the yak hair is 5-6: 1.
4. The method for preparing the nanofiber by using the yak hair as the claim 1, wherein the method comprises the following steps: the weight ratio of the pretreatment liquid to the yak hair is 5-8: 1-3.
5. The method for preparing the nanofiber by using the yak hair as the claim 1, wherein the method comprises the following steps: the reduction treatment liquid consists of the following components in concentration: 30-38/38 g g/L of sodium sulfide, 280-320 g/L of urea, 12-15 g/L of sodium dodecyl sulfate, 12-18 g/L of potassium adipate and 18-23 g/L of butanol.
6. The method for preparing the nanofiber by using the yak hair as the claim 5, wherein the method comprises the following steps: the weight ratio of the reduction treatment solution to the yak hair is 20-30: 1.
7. The method for preparing the nanofiber by using the yak hair as the claim 1, wherein the method comprises the following steps: in the step [5], the mass ratio of the keratin powder to the hexafluoroisopropanol to the polyurethane to the epoxy acrylate is 1: 2-3: 1-1.5: 0.17-0.19.
8. The method for preparing the nanofiber by using the yak hair as the claim 1, wherein the method comprises the following steps: the length of the yak hair crushed by the hair crusher is 1-3 mm.
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| WO2010074029A1 (en) * | 2008-12-24 | 2010-07-01 | 旭化成せんい株式会社 | Polyketone fiber having phenol-treated surface, and fiber-reinforced composite material comprising the fiber |
| CN103993424A (en) * | 2014-06-13 | 2014-08-20 | 东华大学 | Preparing method of polyurethane-keratin composite nano fiber film |
| CN104018247A (en) * | 2014-06-13 | 2014-09-03 | 东华大学 | Preparation method of tubular polyurethane/keratin composite nanofiber material |
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| WO2010074029A1 (en) * | 2008-12-24 | 2010-07-01 | 旭化成せんい株式会社 | Polyketone fiber having phenol-treated surface, and fiber-reinforced composite material comprising the fiber |
| CN103993424A (en) * | 2014-06-13 | 2014-08-20 | 东华大学 | Preparing method of polyurethane-keratin composite nano fiber film |
| CN104018247A (en) * | 2014-06-13 | 2014-09-03 | 东华大学 | Preparation method of tubular polyurethane/keratin composite nanofiber material |
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