CN113957714B - Modified animal fluff fiber and preparation method thereof - Google Patents
Modified animal fluff fiber and preparation method thereof Download PDFInfo
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- CN113957714B CN113957714B CN202111320173.8A CN202111320173A CN113957714B CN 113957714 B CN113957714 B CN 113957714B CN 202111320173 A CN202111320173 A CN 202111320173A CN 113957714 B CN113957714 B CN 113957714B
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- 239000000835 fiber Substances 0.000 title claims abstract description 164
- 241001465754 Metazoa Species 0.000 title claims abstract description 161
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 241001122767 Theaceae Species 0.000 claims abstract description 90
- 239000002028 Biomass Substances 0.000 claims abstract description 85
- 150000008442 polyphenolic compounds Chemical class 0.000 claims abstract description 48
- 235000013824 polyphenols Nutrition 0.000 claims abstract description 48
- 238000011282 treatment Methods 0.000 claims abstract description 36
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 32
- 238000001179 sorption measurement Methods 0.000 claims abstract description 27
- 238000004132 cross linking Methods 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 230000009920 chelation Effects 0.000 claims abstract description 18
- 230000001590 oxidative effect Effects 0.000 claims abstract description 12
- 238000009832 plasma treatment Methods 0.000 claims abstract description 12
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims abstract description 10
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910001431 copper ion Inorganic materials 0.000 claims abstract description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 91
- 239000000243 solution Substances 0.000 claims description 59
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 57
- 239000003431 cross linking reagent Substances 0.000 claims description 47
- 229960000583 acetic acid Drugs 0.000 claims description 41
- 239000011259 mixed solution Substances 0.000 claims description 39
- 239000003999 initiator Substances 0.000 claims description 35
- 239000012362 glacial acetic acid Substances 0.000 claims description 32
- 239000007864 aqueous solution Substances 0.000 claims description 28
- 229920001661 Chitosan Polymers 0.000 claims description 18
- 108090000790 Enzymes Proteins 0.000 claims description 15
- 102000004190 Enzymes Human genes 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 13
- 238000005238 degreasing Methods 0.000 claims description 12
- 229920002101 Chitin Polymers 0.000 claims description 10
- 241000283973 Oryctolagus cuniculus Species 0.000 claims description 9
- 238000010382 chemical cross-linking Methods 0.000 claims description 9
- 108010029541 Laccase Proteins 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims 2
- 238000002791 soaking Methods 0.000 claims 2
- 102000004400 Aminopeptidases Human genes 0.000 claims 1
- 108090000915 Aminopeptidases Proteins 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 21
- 230000000840 anti-viral effect Effects 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 9
- 239000004753 textile Substances 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000004381 surface treatment Methods 0.000 abstract description 3
- 238000005530 etching Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 66
- 238000005406 washing Methods 0.000 description 37
- 229940088598 enzyme Drugs 0.000 description 27
- 239000008367 deionised water Substances 0.000 description 23
- 229910021641 deionized water Inorganic materials 0.000 description 23
- 238000003756 stirring Methods 0.000 description 19
- 230000002779 inactivation Effects 0.000 description 18
- 230000005764 inhibitory process Effects 0.000 description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- 239000000047 product Substances 0.000 description 14
- 238000002156 mixing Methods 0.000 description 13
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 12
- 230000018044 dehydration Effects 0.000 description 10
- 238000006297 dehydration reaction Methods 0.000 description 10
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 8
- 210000004209 hair Anatomy 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- XYHKNCXZYYTLRG-UHFFFAOYSA-N 1h-imidazole-2-carbaldehyde Chemical compound O=CC1=NC=CN1 XYHKNCXZYYTLRG-UHFFFAOYSA-N 0.000 description 6
- GWYFCOCPABKNJV-UHFFFAOYSA-M 3-Methylbutanoic acid Natural products CC(C)CC([O-])=O GWYFCOCPABKNJV-UHFFFAOYSA-M 0.000 description 6
- 241000222122 Candida albicans Species 0.000 description 6
- 241000588724 Escherichia coli Species 0.000 description 6
- 241000712431 Influenza A virus Species 0.000 description 6
- 241000713196 Influenza B virus Species 0.000 description 6
- 102000005348 Neuraminidase Human genes 0.000 description 6
- 108010006232 Neuraminidase Proteins 0.000 description 6
- 241000191967 Staphylococcus aureus Species 0.000 description 6
- GWYFCOCPABKNJV-UHFFFAOYSA-N beta-methyl-butyric acid Natural products CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 6
- 229940095731 candida albicans Drugs 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 241001529453 unidentified herpesvirus Species 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 5
- 210000002268 wool Anatomy 0.000 description 5
- 210000000085 cashmere Anatomy 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 241000700605 Viruses Species 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- CITFYDYEWQIEPX-UHFFFAOYSA-N Flavanol Natural products O1C2=CC(OCC=C(C)C)=CC(O)=C2C(=O)C(O)C1C1=CC=C(O)C=C1 CITFYDYEWQIEPX-UHFFFAOYSA-N 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 235000010208 anthocyanin Nutrition 0.000 description 2
- 229930002877 anthocyanin Natural products 0.000 description 2
- 239000004410 anthocyanin Substances 0.000 description 2
- 150000004636 anthocyanins Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000001580 bacterial effect Effects 0.000 description 2
- 244000052616 bacterial pathogen Species 0.000 description 2
- 230000003385 bacteriostatic effect Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- 230000001877 deodorizing effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 150000002206 flavan-3-ols Chemical class 0.000 description 2
- 235000011987 flavanols Nutrition 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- 235000017173 flavonoids Nutrition 0.000 description 2
- 150000002215 flavonoids Chemical class 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 230000002147 killing effect Effects 0.000 description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 2
- 239000011976 maleic acid Substances 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 239000005445 natural material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- 235000005074 zinc chloride Nutrition 0.000 description 2
- 239000011592 zinc chloride Substances 0.000 description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 description 2
- 229960001763 zinc sulfate Drugs 0.000 description 2
- 102000016943 Muramidase Human genes 0.000 description 1
- 108010014251 Muramidase Proteins 0.000 description 1
- 108010062010 N-Acetylmuramoyl-L-alanine Amidase Proteins 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000002421 finishing Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229960000274 lysozyme Drugs 0.000 description 1
- 239000004325 lysozyme Substances 0.000 description 1
- 235000010335 lysozyme Nutrition 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000005541 medical transmission Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 239000011492 sheep wool Substances 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/06—Inorganic compounds or elements
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/08—Organic compounds
- D06M10/10—Macromolecular compounds
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
- D06M2101/12—Keratin fibres or silk
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Inorganic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to the technical field of textile fibers, and particularly relates to a modified animal fluff fiber and a preparation method thereof. According to the invention, animal fluff fiber, biomass, tea polyphenol and metal ion copper ion and/or zinc ion are used as raw materials, and plasma treatment and subsequent sequential crosslinking treatment, oxidative polymerization-adsorption treatment and chelation reaction are combined, so that the etching degree of the surface treatment of the animal fluff fiber is increased, the crosslinking, adsorption and metal ion chelation strength of modified substances are increased, the antibacterial, mildew-proof and antiviral functions of the animal fluff fiber are endowed, the structural stability of the modified animal fluff fiber is obviously increased, and the antibacterial, mildew-proof and antiviral durability of the modified animal fluff fiber is improved.
Description
Technical Field
The invention belongs to the technical field of textile fibers, and particularly relates to a modified animal fluff fiber and a preparation method thereof.
Background
The animal fluff fiber has the characteristics of softness, fineness, light weight, good warmth retention property and good comfort, is a high-grade textile raw material in textile fibers, and is deeply favored by consumers. However, animal fluff fiber itself is a natural protein fiber, which has the problem of being easy to be damaged by worms, and is easy to be eroded by bacteria and mold, and can cause disease transmission and fiber performance deterioration.
At present, a plurality of antibacterial finishing methods are carried out on animal fluff fibers, such as the use of antibacterial auxiliary agents such as heavy metals, chitin, lysozyme, quaternary ammonium salt organic antibacterial agents or plant extracts, and finishing methods of surface impregnation, surface nano crystallization, surface wrapping or graft copolymerization. For example, chinese patent applications CN107675484A, CN106012512A, CN103266467A, CN101413208A and CN101565894a both provide a method for finishing animal fluff fibers, but the above technical solutions are only simple physical surface treatments, and the obtained animal fluff fiber product is not resistant to washing and rubbing, so that the durability of the antibacterial, mildew-proof and antiviral functions is poor.
Disclosure of Invention
In view of the above, the invention aims to provide a modified animal fluff fiber and a preparation method thereof, and the modified animal fluff fiber provided by the invention has the characteristics of washing resistance, friction resistance, antibacterial and mildew resistance, excellent antiviral performance and long durability.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of modified animal fluff fiber, which comprises the following steps:
degreasing and plasma treating animal fluff fibers to obtain pretreated animal fluff fibers;
immersing the pretreated animal fluff fiber into a glacial acetic acid aqueous solution of biomass under the condition of a cross-linking agent, and performing cross-linking treatment to obtain a biomass modified animal fluff fiber; the biomass is chitin and/or chitosan;
under the condition of an enzyme initiator, immersing the biomass modified animal fluff fiber into a tea polyphenol solution for oxidative polymerization-adsorption treatment to obtain a tea polyphenol-biomass modified animal fluff fiber;
immersing the tea polyphenol-biomass modified animal fluff fiber into a metal ion solution for chelation reaction to obtain the modified animal fluff fiber; the metal ions in the metal ion solution are copper ions and/or zinc ions.
Preferably, the animal fluff fiber is cashmere, wool or rabbit wool.
Preferably, the conditions of the plasma treatment include: the plasma gas is air, the pressure is 30-60 Pa, the output power is 60-200W, and the time is 60-180 s.
Preferably, the crosslinking agent includes a physical crosslinking agent and a chemical crosslinking agent;
the physical cross-linking agent comprises sodium polyphosphate;
the chemical crosslinking agent comprises citric acid, tetrabutyl carboxylic acid or maleic acid.
Preferably, the temperature of the crosslinking treatment is 40-55 ℃ and the time is 120-240 min.
Preferably, the enzyme initiator is laccase or a complex aminoacase;
the pH value of the tea polyphenol solution is 4-5.
Preferably, the temperature of the oxidative polymerization-adsorption treatment is 35-50 ℃ and the time is 60-180 min.
Preferably, the pH value of the metal ion solution is 5.5-6.5.
Preferably, the temperature of the chelation reaction is 10-15 ℃ and the time is 40-120 min.
The invention also provides the modified animal fluff fiber obtained by the preparation method.
The invention provides a preparation method of modified animal fluff fiber, which comprises the following steps: degreasing and plasma treating animal fluff fibers to obtain pretreated animal fluff fibers; immersing the pretreated animal fluff fiber into a glacial acetic acid aqueous solution of biomass under the condition of a cross-linking agent, and performing cross-linking treatment to obtain a biomass modified animal fluff fiber; the biomass is chitin and/or chitosan; under the condition of an enzyme initiator, immersing the biomass modified animal fluff fiber into a tea polyphenol solution for oxidative polymerization-adsorption treatment to obtain a tea polyphenol-biomass modified animal fluff fiber; immersing the tea polyphenol-biomass modified animal fluff fiber into a metal ion solution for chelation reaction to obtain the modified animal fluff fiber; the metal ions in the metal ion solution are copper ions and/or zinc ions.
The animal fluff is degreased and plasma treated, so that the surface structure of the animal fluff fiber is etched, oxygen-containing groups are increased, the surface area of the animal fluff fiber is increased, and proteins on the surface of the animal fluff fiber are partially degraded to generate amino acids, thereby facilitating the adsorption and reaction of subsequent substances. Biomass on-ice vinegarFree amino groups (NH) are released from the aqueous acid environment 4 + ) Amino can inhibit or destroy bacterial reproduction by combining with negative electrons, so that the antibacterial activity of the modified animal villus fiber is improved; under the condition of a cross-linking agent, the biomass and the pretreated animal fluff fiber are cross-linked, so that the cross-linking stability of the biomass on the pretreated animal fluff fiber is improved, and the structural stability, the antibacterial performance and the bacteriostatic performance of the modified animal fluff fiber are improved. The tea polyphenol contained in the tea polyphenol solution comprises various natural substances including anthocyanins, flavonoids and flavanols, has a strong astringing effect, has obvious inhibiting and killing effects on pathogenic bacteria, bacteria and virus microorganisms, and improves the antibacterial and antiviral properties of the modified animal villus fiber; under the condition of an enzyme initiator, the tea polyphenol is oxidized into active quinone substances, and after polymerization, the active quinone substances are combined with animal villus fibers and biomass through hydrogen bonds and Van der Waals force, so that the structural stability and antibacterial and antiviral properties of the modified animal villus fibers are improved. Zinc ions and copper ions have antibacterial and mildew-proof functions; the invention chelates biomass, tea polyphenol and metal ions, and improves the structural stability and antibacterial and mildew-proof properties of the metal ions in the modified animal villus fiber. According to the invention, animal fluff fiber, biomass, tea polyphenol and metal ion copper ion and/or zinc ion are used as raw materials, and plasma treatment and subsequent sequential crosslinking treatment, oxidative polymerization-adsorption treatment and chelation reaction are combined, so that the etching degree of the surface treatment of the animal fluff fiber is increased, the crosslinking, adsorption and metal ion chelation strength of modified substances are increased, the antibacterial, mildew-proof and antiviral functions of the animal fluff fiber are endowed, the structural stability of the modified animal fluff fiber is obviously increased, and the antibacterial, mildew-proof and antiviral durability of the modified animal fluff fiber is improved.
Experimental results show that the inhibition rate of the modified animal villus fiber obtained by the preparation method of the invention to staphylococcus aureus is 89.3-92.8%, the inhibition rate to escherichia coli is 89.5-92.3%, and the inhibition rate to candida albicans is 88.6-91.6%; the mildew-proof grade can reach more than 1 grade; the inactivation rate of influenza A virus is 83.388.2 percent, the inactivation rate of the virus to the influenza B virus is 82.5 to 86.1 percent, and the inactivation rate to the herpesvirus is 80.9 to 85.0 percent; the reduction rate of ammonia is 88.5-92.7%, the reduction rate of trimethylamine is 86.3-91.0%, and the reduction rate of isovaleric acid is 88.2-93.1%; volume resistivity of 1X 10 4 ～1×10 6 Ω·cm。
Detailed Description
The invention provides a preparation method of modified animal fluff fiber, which comprises the following steps:
degreasing and plasma treating animal fluff fibers to obtain pretreated animal fluff fibers;
immersing the pretreated animal fluff fiber into a glacial acetic acid aqueous solution of biomass under the condition of a cross-linking agent, and performing cross-linking treatment to obtain a biomass modified animal fluff fiber; the biomass is chitin and/or chitosan;
under the condition of an enzyme initiator, immersing the biomass modified animal fluff fiber into a tea polyphenol solution for oxidative polymerization-adsorption treatment to obtain a tea polyphenol-biomass modified animal fluff fiber;
immersing the tea polyphenol-biomass modified animal fluff fiber into a metal ion solution for chelation reaction to obtain the modified animal fluff fiber; the multi-metal ions in the metal ions are copper ions and/or zinc ions.
In the present invention, the components of the preparation method are commercially available products well known to those skilled in the art unless otherwise specified.
The animal fluff fiber is degreased and plasma treated to obtain the pretreated animal fluff fiber.
In the present invention, the animal fluff fiber is preferably cashmere, wool or rabbit wool.
In the present invention, the degreasing preferably includes the steps of: washing animal fluff fiber with ethanol; the mass fraction of the ethanol in the ethanol aqueous solution used for ethanol washing is preferably 15-35%, more preferably 20-30%; the temperature of the aqueous ethanol solution is 30 to 40 ℃, more preferably 32 to 38 ℃. In the present invention, the time for the ethanol washing is preferably 15 to 25 minutes, more preferably 18 to 23 minutes. The invention removes the ester substances on the surface of animal fluff fiber through degreasing.
In the present invention, the conditions of the plasma treatment include: the plasma gas is preferably air; the pressure is preferably 30 to 60Pa, more preferably 35 to 55Pa, still more preferably 40 to 50Pa; the output power is preferably 60 to 200W, more preferably 80 to 180W, still more preferably 100 to 160W; the time is preferably 60 to 180 seconds, more preferably 70 to 170 seconds, still more preferably 80 to 160 seconds.
The defatted animal fiber obtained by degreasing is preferably subjected to water washing and dehydration prior to the plasma treatment. In the present invention, the water for washing is preferably deionized water; the water washing is not particularly limited, and water washing known to those skilled in the art may be used. The present invention is not particularly limited, and dehydration known to those skilled in the art may be employed. In the present invention, the dehydrated animal fluff fiber obtained by the dehydration preferably has a water content of 55 to 70%.
The degreasing and plasma treatment are carried out on animal fluff, so that the surface structure of animal fluff fiber is etched, oxygen-containing groups are increased, the surface area of the animal fluff fiber is increased, and the protein on the surface of the animal fluff fiber is partially degraded to generate amino acid, thereby facilitating the adsorption and reaction of subsequent substances.
After the pretreated animal fluff fiber is obtained, the pretreated animal fluff fiber is immersed into a glacial acetic acid aqueous solution of biomass under the condition of a cross-linking agent, and cross-linking treatment is carried out, so that the biomass modified animal fluff fiber is obtained.
In the present invention, the biomass is chitin and/or chitosan.
In the present invention, the mass fraction of the biomass in the aqueous glacial acetic acid solution of the biomass is preferably 2 to 5%, more preferably 2.5 to 4.5%, still more preferably 3 to 4%.
In the invention, the preparation method of the glacial acetic acid aqueous solution of biomass preferably comprises the following steps: mixing biomass and glacial acetic acid aqueous solution, and completely dissolving the biomass in the glacial acetic acid aqueous solution to obtain the glacial acetic acid aqueous solution of the biomass.
In the present invention, the mass fraction of glacial acetic acid in the aqueous glacial acetic acid solution is preferably 0.5 to 1.5%, more preferably 0.7 to 1.3%. In the present invention, the mixing of the biomass and the aqueous glacial acetic acid solution is preferably stirring. In the present invention, the temperature of the stirring is preferably 40 to 55 ℃, more preferably 42 to 53 ℃; the rotation speed is preferably 300 to 500rpm, more preferably 350 to 450rpm.
After the aqueous glacial acetic acid solution of biomass is obtained, the aqueous glacial acetic acid solution of biomass and the cross-linking agent are preferably mixed, and the pretreated animal fluff fiber is immersed into the obtained biomass-cross-linking agent mixed solution containing the aqueous glacial acetic acid solution of biomass and the cross-linking agent for cross-linking treatment.
In the present invention, the crosslinking agent preferably includes a physical crosslinking agent and a chemical crosslinking agent. In the present invention, the physical crosslinking agent preferably includes sodium polyphosphate. In the present invention, the mass fraction of the physical crosslinking agent in the biomass-crosslinking agent mixed solution is preferably 0.5 to 1.5%, more preferably 0.7 to 1.3%. In the present invention, the chemical crosslinking agent preferably includes citric acid, tetrabutyl carboxylic acid or maleic acid, more preferably citric acid. In the present invention, the mass fraction of the chemical crosslinking agent in the biomass-crosslinking agent mixed solution is preferably 0.05 to 0.15%, more preferably 0.08 to 0.13%.
In the present invention, the bath ratio of the pretreated animal fluff fiber and biomass-crosslinking agent mixed solution is preferably 1: (20 to 40), more preferably 1: (25-35). In the present invention, the temperature of the crosslinking treatment is preferably 40 to 55 ℃, more preferably 43 to 52 ℃, still more preferably 45 to 50 ℃; the time is preferably 120 to 240 minutes, more preferably 140 to 220 minutes, still more preferably 160 to 200 minutes. In the present invention, the crosslinking treatment is preferably performed under stirring.
After the crosslinking treatment, the present invention preferably sequentially subjects the resulting crosslinked product to water washing and dehydration. In the present invention, the water for washing is preferably deionized water; the water washing is not particularly limited, and water washing known to those skilled in the art may be used. The present invention is not particularly limited, and dehydration known to those skilled in the art may be employed. In the present invention, the water content of the dehydrated biomass-modified animal fluff fiber obtained by the dehydration is preferably 55 to 70%.
In the invention, the biomass releases free amino (NH) in the glacial acetic acid aqueous solution environment 3 + ) Amino can inhibit or destroy bacterial reproduction by combining with negative electrons, and improve antibacterial activity of modified animal villus fiber. In the invention, the chemical crosslinking agent has a bridging crosslinking effect, so that crosslinking reaction occurs between amino groups on biomass and carboxyl groups on citric acid, and between carboxyl groups on citric acid and amino groups on animal fluff fibers; the chemical crosslinking agent promotes precipitation between the biomass and forms hydrogen bonds, thereby forming physical crosslinks between the biomass and the animal fluff fibers, inside the biomass. Under the condition of a cross-linking agent, the biomass and the pretreated animal fluff fiber are cross-linked, so that the cross-linking stability of the biomass on the pretreated animal fluff fiber is improved, and the structural stability, the antibacterial performance and the bacteriostatic performance of the modified animal fluff fiber are improved.
After obtaining biomass modified animal fluff fiber, under the condition of an enzyme initiator, the biomass modified animal fluff fiber is immersed into a tea polyphenol solution for oxidation polymerization-adsorption treatment, so that the tea polyphenol-biomass modified animal fluff fiber is obtained.
In the present invention, the pH of the tea polyphenol solution is preferably 4 to 5, more preferably 4.2 to 4.8. In the present invention, the agent for adjusting the pH value of the tea polyphenol solution is preferably acetic acid or citric acid. In the invention, the preparation method of the tea polyphenol solution preferably comprises the following steps: mixing water and tea polyphenols to obtain the tea polyphenols solution, more preferably adding tea polyphenols to water to obtain the tea polyphenols solution. In the present invention, the temperature of the water is preferably 35 to 50 ℃, more preferably 40 to 45 ℃; the pH is preferably 4 to 5, more preferably 4.2 to 4.8. In the present invention, the concentration of tea polyphenol in the tea polyphenol solution is preferably 2.5 to 5.0% by mass, more preferably 3 to 4.5% by mass.
After the tea polyphenol solution is obtained, the invention preferably mixes the tea polyphenol solution and the enzyme initiator, and the biomass modified animal fluff fiber is immersed into the obtained tea polyphenol-enzyme initiator mixed solution to carry out oxidative polymerization-adsorption treatment.
In the present invention, the enzyme-type initiator is preferably laccase or a complex aminoacase. In the present invention, the concentration of the enzyme-based initiator in the tea polyphenol-enzyme-based initiator mixed solution is preferably 60 to 85U/mL, more preferably 65 to 80U/mL.
In the invention, the bath ratio of the mixed solution of the biomass modified animal fluff fiber and the tea polyphenol enzyme initiator is preferably 1: (20 to 40), more preferably 1: (25-35). In the present invention, the temperature of the oxidative polymerization-adsorption treatment is preferably 35 to 50 ℃, more preferably 38 to 48 ℃, still more preferably 40 to 45 ℃; the time is preferably 60 to 180 minutes, more preferably 80 to 160 minutes, still more preferably 100 to 140 minutes. In the present invention, the oxidative polymerization-adsorption treatment is preferably performed under air-circulation conditions; in the present invention, the ventilation is preferably obtained by stirring.
After the oxidative polymerization-adsorption treatment, the present invention preferably sequentially subjects the resulting physisorbed product to water washing and dehydration. In the present invention, the water for washing is preferably deionized water; the water washing is not particularly limited, and water washing known to those skilled in the art may be used. The present invention is not particularly limited, and dehydration known to those skilled in the art may be employed. In the present invention, the water content of the dehydrated tea polyphenol-biomass modified animal fluff fiber obtained by dehydration is preferably 55 to 65%.
In the invention, tea polyphenol contained in the tea polyphenol solution is a generic term for phenolic compounds in tea, and comprises various natural substances of anthocyanins, flavonoids and flavanols, so that the tea polyphenol solution has a strong astringing effect, has obvious inhibiting and killing effects on pathogenic bacteria, bacteria and virus microorganisms, and improves the antibacterial and antiviral properties of modified animal villus fibers; under the condition of an enzyme initiator, the tea polyphenol is oxidized into active quinone substances, and after polymerization, the active quinone substances are combined with animal villus fibers and biomass through hydrogen bonds and Van der Waals force, so that the structural stability and antibacterial and antiviral properties of the modified animal villus fibers are improved.
After obtaining tea polyphenol-biomass modified animal villus fiber, the invention immerses the tea polyphenol-biomass modified animal villus fiber into a metal ion solution for chelation reaction to obtain the modified animal villus fiber.
In the invention, the metal ions in the metal ion solution are copper ions and/or zinc ions. In the present invention, the solute in the metal ion solution preferably includes one or more of copper sulfate, copper chloride, zinc sulfate and zinc chloride. In the present invention, the concentration of the metal ions in the metal ion solution is preferably 4 to 6wt.%, more preferably 4.2 to 5.8wt.%, still more preferably 4.5 to 5.5wt.%. In the present invention, the pH of the metal ion solution is preferably 5.5 to 6.5, more preferably 5.7 to 6.3. In the present invention, the agent for adjusting the pH of the metal ion solution is preferably acetic acid, citric acid or sodium bicarbonate.
The temperature of the chelation reaction is preferably 10 to 15 ℃, more preferably 11 to 14 ℃; the time is preferably 40 to 120 minutes, more preferably 60 to 100 minutes.
After the chelation reaction, the present invention preferably dehydrates and steam dries the resulting chelation reaction product. In the present invention, the water content of the dehydrated modified animal nap fiber obtained by the dehydration is preferably 60 to 70%, more preferably 62 to 68%. In the present invention, the temperature of the steam drying is preferably 85 to 105 ℃, more preferably 90 to 100 ℃. In the present invention, the moisture content of the modified animal fluff fiber obtained after the steam drying is preferably 12 to 16%, more preferably 13 to 15%. After the steam is dried, the obtained modified animal fluff fiber is preferably opened; the present invention is not particularly limited, and the opening known to those skilled in the art may be employed.
In the invention, zinc ions and copper ions have antibacterial and mildew-proof functions; the invention carries out chelation reaction to chelate biomass, tea polyphenol and metal ions, thereby improving the structural stability and antibacterial and mildew-proof properties of the metal ions in the modified animal villus fiber.
The invention also provides the modified animal fluff fiber obtained by the preparation method.
In the invention, the modified animal hair fiber macroscopically still has the appearance of an animal hair fiber; microcosmic including animal fluff fiber, biomass attached to the surface of the animal fluff fiber, tea polyphenol and metal ions; the biomass is chitin and/or chitosan; the metal ions are copper ions and/or zinc ions.
In order to further illustrate the present invention, the modified animal fluff fiber provided by the present invention and the method of preparing the same are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The reagents used in the examples are all commercially available.
Example 1
Washing cashmere with an ethanol aqueous solution with the mass fraction of 15% and the temperature of 40 ℃ for 25min to degrease, washing with deionized water, and then dehydrating to obtain degreased cashmere with the water content of 70%; taking air as plasma gas, and performing plasma treatment for 180s at 60W and 30Pa to obtain pretreated animal fluff fibers;
mixing chitin and glacial acetic acid aqueous solution with mass fraction of 0.5% under stirring condition at 40deg.C and 500rpm to obtain glacial acetic acid aqueous solution of chitin with mass fraction of 2%; adding citric acid and sodium polyphosphate into the obtained glacial acetic acid aqueous solution of chitin to obtain a biomass-crosslinking agent mixed solution, wherein the mass fraction of the citric acid in the biomass-crosslinking agent mixed solution is 0.05%, and the mass fraction of the sodium polyphosphate is 0.5%; according to the bath ratio of 1:40, immersing the pretreated animal fluff fiber into a biomass-cross-linking agent mixed solution, carrying out cross-linking treatment for 240min at 40 ℃ under stirring, washing the obtained cross-linked product with deionized water, and then dehydrating to obtain the biomass modified animal fluff fiber with the water content of 70%;
adjusting the pH of deionized water to 4 by acetic acid, adding tea polyphenol at 50 ℃ to obtain a tea polyphenol solution with the mass percent concentration of 2.5%, and mixing the tea polyphenol solution with laccase to obtain a tea polyphenol-enzyme initiator mixed solution, wherein the concentration of laccase in the tea polyphenol-enzyme initiator mixed solution is 60U/mL; according to the bath ratio of 1:40, immersing the biomass modified animal fluff fiber into a tea polyphenol-enzyme initiator mixed solution, stirring for 60min at 50 ℃ for oxidation polymerization-adsorption treatment, washing the obtained physical adsorption product with deionized water, and dehydrating to obtain the tea polyphenol-biomass modified animal fluff fiber with the water content of 65%;
immersing the obtained tea polyphenol-biomass modified animal fluff fiber into a zinc sulfate solution with the concentration of 4wt.%, adjusting the pH value to 5.5 by acetic acid, carrying out chelation reaction at the temperature of 10 ℃ for 120min, dehydrating the reaction product until the water content is 70%, then drying by steam at the temperature of 85 ℃ until the water content is 16%, and opening to obtain the modified animal fluff fiber.
According to GB T209444.3-2008, evaluation of antibacterial Properties of textiles, section 3: the oscillation method shows that the inhibition rate of the modified animal villus fiber obtained in the example 1 to staphylococcus aureus is 89.3%, the inhibition rate to escherichia coli is 89.5%, and the inhibition rate to candida albicans is 88.6%; the mildew resistance grade can reach grade 1 according to the detection of a petri dish method in GB/T24346-2009 evaluation of mildew resistance of textiles; according to ISO 198184-2014, the inactivation rate of influenza A virus is 83.3%, the inactivation rate of influenza B virus is 82.5% and the inactivation rate of herpes virus is 80.9%; determination of deodorizing properties of textiles according to GB/T33610.2-2017 part 2: detecting a pipe method, wherein the reduction rate of ammonia gas is 88.5%; determination of deodorizing Properties of textiles according to GB/T33610.3-2019 part 3: gas chromatography gave a reduction of 86.3% for trimethylamine and 88.2% for isovaleric acid; volume resistivity of 1X 10 6 Ω·cm。
Example 2
Washing sheep wool with an ethanol aqueous solution with the mass fraction of 23% and the temperature of 36 ℃ for 22min for degreasing, and dehydrating after washing with deionized water to obtain degreased wool with the water content of 65%; taking air as plasma gas, and performing plasma treatment for 130s at 110W and 40Pa to obtain pretreated animal fluff fibers;
mixing chitosan and glacial acetic acid aqueous solution with the mass fraction of 0.85% under the stirring condition of 45 ℃ and 420rpm to obtain the glacial acetic acid aqueous solution of chitosan with the mass fraction of 3%; adding citric acid and sodium polyphosphate into the obtained glacial acetic acid aqueous solution of chitosan to obtain a biomass-crosslinking agent mixed solution, wherein the mass fraction of the citric acid in the biomass-crosslinking agent mixed solution is 0.1%, and the mass fraction of the sodium polyphosphate is 0.9%; according to the bath ratio of 1:35, immersing the pretreated animal fluff fiber into a biomass-cross-linking agent mixed solution, carrying out cross-linking treatment for 200min at 45 ℃ under stirring, washing the obtained cross-linked product with deionized water, and then dehydrating to obtain a biomass modified animal fluff fiber with the water content of 65%;
adjusting the pH of deionized water to 4.3 by acetic acid, adding tea polyphenol at 45 ℃ to obtain a tea polyphenol solution with the mass percent concentration of 3.5%, and mixing the tea polyphenol solution with laccase to obtain a tea polyphenol-enzyme initiator mixed solution, wherein the concentration of laccase in the tea polyphenol-enzyme initiator mixed solution is 70U/mL; according to the bath ratio of 1:35, immersing the biomass modified animal fluff fiber into a tea polyphenol-enzyme initiator mixed solution, stirring for 100min at 45 ℃ for oxidation polymerization-adsorption treatment, washing the obtained physical adsorption product with deionized water, and dehydrating to obtain the tea polyphenol-biomass modified animal fluff fiber with the water content of 60%;
immersing the obtained tea polyphenol-biomass modified animal fluff fiber into a zinc chloride solution with the concentration of 4.9wt.%, adjusting the pH value to 6.0 by acetic acid, carrying out chelation reaction at 12 ℃ for 100min, dehydrating the reaction product until the water content is 66%, then drying by steam at 95 ℃ until the water content is 15.2%, and opening to obtain the modified animal fluff fiber.
According to the test method of example 1, the inhibition rate of the modified animal fluff fiber obtained in example 2 to staphylococcus aureus is measured to be 90.3%, the inhibition rate to escherichia coli is measured to be 91.5%, and the inhibition rate to candida albicans is measured to be 89.8%; the mildew-proof grade can reach grade 1; the inactivation rate of the influenza A virus is 85.3 percent, the inactivation rate of the influenza B virus is 83.6 percent, and the inactivation rate of the herpesvirus is 81.8 percent; the reduction rate of ammonia gas is 90.5%; the reduction rate of trimethylamine is 87.9 percent, and the reduction rate of isovaleric acid is 90.5 percent; volume resistivity of 8.2X10 5 Ω·cm。
Example 3
Washing rabbit hair with ethanol water solution with mass fraction of 28% and temperature of 33 ℃ for 18min for degreasing, washing with deionized water, and dehydrating to obtain defatted rabbit hair with water content of 60.5%; taking air as plasma gas, and performing plasma treatment for 100s at 160W and 50Pa to obtain pretreated animal fluff fibers;
mixing chitosan and glacial acetic acid aqueous solution with the mass fraction of 1.2% under the stirring condition of 50 ℃ and 360rpm to obtain the glacial acetic acid aqueous solution of chitosan with the mass fraction of 4%; adding citric acid and sodium polyphosphate into the obtained glacial acetic acid aqueous solution of chitosan to obtain a biomass-crosslinking agent mixed solution, wherein the mass fraction of the citric acid in the biomass-crosslinking agent mixed solution is 0.12%, and the mass fraction of the sodium polyphosphate is 1.2%; according to the bath ratio of 1:28, immersing the pretreated animal fluff fiber into a biomass-cross-linking agent mixed solution, carrying out cross-linking treatment for 160min at 50 ℃ under stirring, washing the obtained cross-linked product with deionized water, and then dehydrating to obtain biomass modified animal fluff fiber with the water content of 60%;
adjusting the pH of deionized water to 4.8 by acetic acid, adding tea polyphenol at 40 ℃ to obtain a tea polyphenol solution with the mass percent concentration of 4.3%, and mixing the tea polyphenol solution with the neuraminidase to obtain a tea polyphenol-enzyme initiator mixed solution, wherein the concentration of the neuraminidase in the tea polyphenol-enzyme initiator mixed solution is 78U/mL; according to the bath ratio of 1:28, immersing the biomass modified animal fluff fiber into a tea polyphenol-enzyme initiator mixed solution, stirring for 150min at 41 ℃ for oxidation polymerization-adsorption treatment, washing the obtained physical adsorption product with deionized water, and dehydrating to obtain the tea polyphenol-biomass modified animal fluff fiber with the water content of 57.5%;
immersing the obtained tea polyphenol-biomass modified animal fluff fiber into a copper sulfate solution with the concentration of 5.6wt.%, adjusting the pH value to 6.2 by citric acid, carrying out chelation reaction at the temperature of 14 ℃ for 70min, dehydrating the reaction product until the water content is 62.5%, then drying by steam at the temperature of 100 ℃ until the water content is 13.8%, and opening to obtain the modified animal fluff fiber.
According to the test method of example 1, the inhibition rate of the modified animal fluff fiber obtained in example 3 to staphylococcus aureus is 91.5%, the inhibition rate to escherichia coli is 92.3%, and the inhibition rate to candida albicans is 90.9%; the mildew-proof grade can reach 0 grade; the inactivation rate of the influenza A virus is 86.6%, the inactivation rate of the influenza B virus is 84.9%, and the inactivation rate of the herpesvirus is 83.0%; the reduction rate of ammonia gas is 91.1 percent, the reduction rate of trimethylamine is 89.2 percent, and the reduction rate of isovaleric acid is 91.3 percent; volume resistivity of 1.5X10 5 Ω·cm。
Example 4
Washing rabbit hair with ethanol water solution with mass fraction of 35% and temperature of 30 ℃ for 15min for degreasing, washing with deionized water, and dehydrating to obtain defatted rabbit hair with water content of 55%; taking air as plasma gas, and performing plasma treatment for 60s under 200W and 60Pa to obtain pretreated animal fluff fibers;
mixing chitosan and glacial acetic acid aqueous solution with the mass fraction of 1.5% under the stirring condition of 55 ℃ and 300rpm to obtain the glacial acetic acid aqueous solution of chitosan with the mass fraction of 5%; adding citric acid and sodium polyphosphate into the obtained glacial acetic acid aqueous solution of chitosan to obtain a biomass-crosslinking agent mixed solution, wherein the mass fraction of the citric acid in the biomass-crosslinking agent mixed solution is 0.15%, and the mass fraction of the sodium polyphosphate is 1.5%; according to the bath ratio of 1:20, immersing the pretreated animal fluff fiber into a biomass-cross-linking agent mixed solution, carrying out cross-linking treatment for 120min at 55 ℃ under stirring, washing the obtained cross-linked product with deionized water, and then dehydrating to obtain a biomass modified animal fluff fiber with the water content of 55%;
adjusting the pH of deionized water to 5 by acetic acid, adding tea polyphenol at 35 ℃ to obtain a tea polyphenol solution with the mass percent concentration of 5%, and mixing the tea polyphenol solution with the neuraminidase to obtain a tea polyphenol-enzyme initiator mixed solution, wherein the concentration of the neuraminidase in the tea polyphenol-enzyme initiator mixed solution is 85U/mL; according to the bath ratio of 1:20, immersing the biomass modified animal fluff fiber into a tea polyphenol-enzyme initiator mixed solution, stirring for 180min at 35 ℃ for oxidation polymerization-adsorption treatment, washing the obtained physical adsorption product with deionized water, and dehydrating to obtain the tea polyphenol-biomass modified animal fluff fiber with the water content of 55%;
immersing the obtained tea polyphenol-biomass modified animal fluff fiber into a copper chloride solution with the concentration of 6wt.%, adjusting the pH value to be 6.5 by sodium bicarbonate, carrying out chelation reaction at 15 ℃ for 40min, dehydrating the reaction product to the water content of 60%, then drying by steam at 105 ℃ to the water content of 12%, and opening to obtain the modified animal fluff fiber.
According to the test method of example 1, the inhibition rate of the modified animal fluff fiber obtained in example 4 to staphylococcus aureus is 92.8%, the inhibition rate to escherichia coli is 91.1%, and the inhibition rate to candida albicans is 91.6%; the mildew-proof grade can reach 0 grade; the inactivation rate of the influenza A virus is 88.2%, the inactivation rate of the influenza B virus is 86.1%, and the inactivation rate of the herpesvirus is 85.0%; the reduction rate of ammonia gas is 92.7%, trimethylamine is 91.0% and isovaleric acid is 93.1%; volume resistivity of 1X 10 4 Ω·cm。
Comparative example 1
Washing rabbit hair with ethanol water solution with mass fraction of 35% and temperature of 30 ℃ for 15min for degreasing, washing with deionized water, and dehydrating to obtain defatted rabbit hair with water content of 55%; taking air as plasma gas, and performing plasma treatment for 60s under 200W and 60Pa to obtain pretreated animal fluff fibers;
mixing chitosan and glacial acetic acid aqueous solution with the mass fraction of 1.5% under the stirring condition of 55 ℃ and 300rpm to obtain the glacial acetic acid aqueous solution of chitosan with the mass fraction of 5%; adding citric acid and sodium polyphosphate into the obtained glacial acetic acid aqueous solution of chitosan to obtain a biomass-crosslinking agent mixed solution, wherein the mass fraction of the citric acid in the biomass-crosslinking agent mixed solution is 0.15%, and the mass fraction of the sodium polyphosphate is 1.5%; according to the bath ratio of 1:20, immersing the pretreated animal fluff fiber into a biomass-cross-linking agent mixed solution, carrying out cross-linking treatment for 120min at 55 ℃ under stirring, washing the obtained cross-linked product with deionized water, and then dehydrating to obtain a biomass modified animal fluff fiber with the water content of 55%;
adjusting the pH of deionized water to 5 by acetic acid, adding tea polyphenol at 35 ℃ to obtain a tea polyphenol solution with the mass percent concentration of 5%, and mixing the tea polyphenol solution with the neuraminidase to obtain a tea polyphenol-enzyme initiator mixed solution, wherein the concentration of the neuraminidase in the tea polyphenol-enzyme initiator mixed solution is 85U/mL; according to the bath ratio of 1:20, immersing the biomass modified animal fluff fiber into a tea polyphenol-enzyme initiator mixed solution, stirring for 180min at 35 ℃ for oxidation polymerization-adsorption treatment, washing the obtained physical adsorption product with deionized water, and dehydrating to obtain the tea polyphenol-biomass modified animal fluff fiber with the water content of 55%;
and (3) drying the obtained tea polyphenol-biomass modified animal villus fiber by steam at 105 ℃ until the water content is 12%, and opening to obtain the modified animal villus fiber.
According to the test method of example 1, the inhibition rate of the modified animal fluff fiber obtained in comparative example 1 to staphylococcus aureus is 89.5%, the inhibition rate to escherichia coli is 88.9%, and the inhibition rate to candida albicans is 89.1%; the mildew-proof grade can reach grade 1; the inactivation rate of the influenza A virus is 88.2%, the inactivation rate of the influenza B virus is 86.1%, and the inactivation rate of the herpesvirus is 85.0%; the reduction rate of ammonia gas is 90.9%, the reduction rate of trimethylamine is 89.3%, and the reduction rate of isovaleric acid is 91.5%; volume resistivity of 1.8X10 4 Ω·cm。
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (7)
1. A method for preparing modified animal fluff fiber, comprising the following steps:
degreasing and plasma treating animal fluff fibers to obtain pretreated animal fluff fibers;
the animal fluff fiber is rabbit fluff;
the conditions of the plasma treatment include: the plasma gas is air, the pressure is 60Pa, the output power is 200W, and the time is 60s;
immersing the pretreated animal fluff fiber into a glacial acetic acid aqueous solution of biomass under the condition of a cross-linking agent, and performing cross-linking treatment to obtain a biomass modified animal fluff fiber; the biomass is chitin and/or chitosan;
the crosslinking agent is a physical crosslinking agent and a chemical crosslinking agent;
the physical cross-linking agent is sodium polyphosphate;
the chemical cross-linking agent is citric acid;
under the condition of an enzyme initiator, immersing the biomass modified animal fluff fiber into tea polyphenol liquid, and performing oxidative polymerization-adsorption treatment to obtain tea polyphenol-biomass modified animal fluff fiber;
under the condition of enzyme initiator, soaking the biomass modified animal fluff fiber into tea polyphenol liquid to mix the tea polyphenol solution with the enzyme initiator, and soaking the biomass modified animal fluff fiber into the obtained tea polyphenol-enzyme initiator mixed solution, wherein the concentration of the enzyme initiator in the tea polyphenol-enzyme initiator mixed solution is 60-85U/mL;
the enzyme initiator is laccase or aminopeptidase;
immersing the tea polyphenol-biomass modified animal fluff fiber into a metal ion solution for chelation reaction to obtain the modified animal fluff fiber; the metal ions in the metal ion solution are copper ions and/or zinc ions.
2. The method according to claim 1, wherein the crosslinking treatment is carried out at a temperature of 40 to 55 ℃ for 120 to 240 minutes.
3. The process according to claim 1, wherein the pH of the tea polyphenol solution is 4 to 5.
4. A method according to claim 1 or 3, wherein the temperature of the oxidative polymerization-adsorption treatment is 35 to 50 ℃ for 60 to 180min.
5. The method according to claim 1, wherein the pH of the metal ion solution is 5.5 to 6.5.
6. The method according to claim 1 or 5, wherein the chelating reaction is carried out at a temperature of 10 to 15 ℃ for 40 to 120 minutes.
7. A modified animal fluff fiber obtained by the production process according to any one of claims 1 to 6.
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