CN116590918A - Preparation method of antistatic wool fiber - Google Patents
Preparation method of antistatic wool fiber Download PDFInfo
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- CN116590918A CN116590918A CN202310876350.3A CN202310876350A CN116590918A CN 116590918 A CN116590918 A CN 116590918A CN 202310876350 A CN202310876350 A CN 202310876350A CN 116590918 A CN116590918 A CN 116590918A
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- antistatic
- wool fiber
- dopamine
- derivative
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- 239000000835 fiber Substances 0.000 title claims abstract description 80
- 210000002268 wool Anatomy 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 53
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229960003638 dopamine Drugs 0.000 claims abstract description 24
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 claims abstract description 23
- 229940005642 polystyrene sulfonic acid Drugs 0.000 claims abstract description 21
- 239000006185 dispersion Substances 0.000 claims abstract description 18
- 238000002791 soaking Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 8
- 239000012266 salt solution Substances 0.000 claims abstract description 6
- 239000002041 carbon nanotube Substances 0.000 claims description 28
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 24
- 239000010936 titanium Substances 0.000 claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 21
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 17
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 12
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 230000004048 modification Effects 0.000 claims description 9
- 238000012986 modification Methods 0.000 claims description 9
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 4
- 238000007654 immersion Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 claims description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 2
- 229940074391 gallic acid Drugs 0.000 claims description 2
- 235000004515 gallic acid Nutrition 0.000 claims description 2
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 claims description 2
- 239000010955 niobium Substances 0.000 claims description 2
- 229920001690 polydopamine Polymers 0.000 claims description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 11
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- 230000000536 complexating effect Effects 0.000 abstract 2
- 230000002708 enhancing effect Effects 0.000 abstract 1
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 15
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 8
- 150000003839 salts Chemical class 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 6
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- 238000005303 weighing Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 239000007983 Tris buffer Substances 0.000 description 5
- 125000003277 amino group Chemical group 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 5
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 5
- 239000004433 Thermoplastic polyurethane Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 4
- 239000002216 antistatic agent Substances 0.000 description 3
- 239000008280 blood Substances 0.000 description 3
- 210000004369 blood Anatomy 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 description 2
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 2
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 2
- 238000010668 complexation reaction Methods 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
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- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
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- 238000004108 freeze drying Methods 0.000 description 2
- -1 hydrogen ions Chemical class 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000004970 Chain extender Substances 0.000 description 1
- 206010013954 Dysphoria Diseases 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 241001145025 Saussurea involucrata Species 0.000 description 1
- 208000013738 Sleep Initiation and Maintenance disease Diseases 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical group 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000021523 carboxylation Effects 0.000 description 1
- 238000006473 carboxylation reaction Methods 0.000 description 1
- 210000000085 cashmere Anatomy 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
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- 239000012895 dilution Substances 0.000 description 1
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- 239000000428 dust Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000007350 electrophilic reaction Methods 0.000 description 1
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- 239000012530 fluid Substances 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 206010022437 insomnia Diseases 0.000 description 1
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- 239000012528 membrane Substances 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229940006186 sodium polystyrene sulfonate Drugs 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- 238000005507 spraying Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
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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
- 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
- D06M11/73—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 with carbon or compounds thereof
- D06M11/74—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 with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- 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
- D06M11/58—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 with nitrogen or compounds thereof, e.g. with nitrides
-
- 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
- D06M11/58—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 with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/59—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 with nitrogen or compounds thereof, e.g. with nitrides with ammonia; with complexes of organic amines with inorganic substances
- D06M11/60—Ammonia as a gas or in solution
-
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/368—Hydroxyalkylamines; Derivatives thereof, e.g. Kritchevsky bases
-
- 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
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
- D06M15/233—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated aromatic, e.g. styrene
-
- 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
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to a preparation method of antistatic wool fibers, and belongs to the technical field of conductive fiber preparation. The preparation method comprises the steps of firstly pretreating wool fibers by sequentially adopting ammonia water and salt solution, then modifying the wool fibers by adopting dopamine or a derivative thereof and polystyrene sulfonic acid solution, and finally soaking by adopting conductive mixed dispersion solution to obtain the antistatic wool fibers. The invention adopts the method of crosslinking and depositing dopamine or the derivative thereof with stable complexing structure and polystyrene sulfonic acid, thereby effectively relieving the problems of poor dispersibility and easy aggregation of conductive substances, forming an effective and stable conductive network structure, enhancing the complexing between a conductive substance layer and wool fibers, and avoiding a large amount of chemical adhesion reagents.
Description
Technical Field
The invention belongs to the technical field of textile fiber preparation, and particularly relates to an antistatic wool fiber and a preparation method thereof.
Background
The wool fabric has the characteristics of softness, comfort, ventilation and warmth retention, is popular with consumers, is generally woven by adopting blended yarns with certain wool fiber content, is easy to generate electrostatic phenomenon due to friction and induction in the processing and using processes, and accumulated electrostatic charges are easy to adsorb dust and cause the fabric product to be attached and entangled on limbs when being worn, so that discomfort is generated, the pH of human blood is raised, calcium in blood is lowered, blood sugar is raised and the like. Especially in autumn and winter, static electricity is more likely to be generated, the static electricity can influence the health of people, can stimulate the skin, the brain and the like of people, and can cause people to feel tired, dysphoria, insomnia and headache, thereby influencing the wearability of the people. In addition, the electrostatic interference not only affects the smooth proceeding of fiber processing, but also has serious consequences because the electrostatic pressure reaches several kilovolts, and spark is generated due to discharge, causing fire. Therefore, wool fibers and products thereof need to be treated to reduce the resistivity and improve the static electricity problem.
In recent years, with the increasing concern of electrostatic hazard at home and abroad. A great deal of research and test are carried out on the aspect of antistatic fiber, remarkable results are obtained, and a plurality of attempts are made in the technical field of antistatic wool fiber preparation. The existing antistatic wool fiber has the following problems: firstly, the static electricity eliminating method for the wool fiber disclosed in the prior art adopts antistatic spraying or dipping antistatic agent on the surface of the wool fiber, and a layer of antistatic agent can be formed on the surface of the wool fiber, but the effect of the treatment method is not durable, when air is dried, the antistatic agent falls off from the surface of the fiber, and the durability of the antistatic effect is affected; secondly, organic conductive fibers with good conductivity are mixed or woven into the wool product. Although these methods can improve the antistatic ability of wool, there is also a problem that the antistatic durability is drastically reduced during the process of rubbing.
Disclosure of Invention
The invention provides a preparation method of antistatic wool fibers, which aims to solve the problem that when the existing method is used for preparing or using antistatic wool fibers, the content of conductive substances is reduced due to the change of external environments such as high temperature, humidity, air or concentrated alkali, and the like, and the antistatic durability is affected by static discharge caused by current flow resistance.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the antistatic wool fiber comprises the following steps:
(1) Pretreatment of wool fibers: firstly, immersing wool fibers in an ammonia water solution, and then immersing in a salt solution;
(2) Modification of wool fibers: preparing a modified solution from dopamine or derivatives thereof and polystyrene sulfonic acid, wherein the mass ratio of the dopamine or derivatives thereof to the polystyrene sulfonic acid is 1:2-2:1, immersing the pretreated wool fibers in the modified solution of the dopamine or derivatives thereof for modification treatment, wherein the immersion temperature is 20-30 ℃, magnetically stirring for 8-36h at 40-200rpm, and washing and drying to obtain modified wool fibers;
(3) Preparing a conductive mixed dispersion solution: adding an Mxene two-dimensional material or a derivative thereof and a carbon nano tube or a derivative thereof into a dimethylformamide solution, and continuously stirring to obtain a conductive mixed dispersion solution;
(4) And (3) immersing the wool fiber obtained by modification in the step (2) in the conductive mixed dispersion solution in the step (3), and drying, washing and drying to obtain the antistatic wool fiber.
Further, in the step (1), the bath ratio is 1:70 after soaking for 30-60min at the constant temperature of 50 ℃.
Further, the dopamine or the derivative thereof comprises one of polystyrene sulfonic acid including gallic acid, dopamine hydrochloride, polydopamine (DATA) and N-3, 4-dihydroxyphenethyl acrylamide (DAA).
Further, the concentration of the modifying solution in the step (2) is 0.5-4.5mg/mL, and the pH is 8-10.
Further, the concentration of dimethylformamide in the conductive mixed dispersion solution in the step (3) is 15-45 mg/mL, the concentration of the Mxene two-dimensional material or the derivative thereof is 5-35mg/mL, and the concentration of the carbon nano tube or the derivative thereof is 15-25mg/mL.
Further, the constant temperature of the constant temperature magnetic stirrer in the step (3) is 25-45 ℃, the stirring speed is 100-400rpm, and the stirring time is 2.5-8.5h.
Further, the carbon nanotubes or the derivatives thereof in the step (3) include one or more of aminated carbon nanotubes, acidified carbon nanotubes, acrylamido carbon nanotubes (AM-CNTs), 2-dimethylolpropionylated carbon nanotubes (DMPA-CNTs).
Further, the MXene two-dimensional material or the derivative thereof comprises titanium carbide (Ti 3 C 2 Tx), dititanium carbide (Ti) 2 C) Niobium carbide (Nb) 2 C) Vanadium carbide (V) 2 C) Dititanium carbide (Ti) 2 CN), titanium nitride (Ti) 2 N) is provided.
The antistatic function means: the wool fiber molecular chain contains a large amount of amino groups, N in the amino groups can generate electrophilic reaction to cause charge aggregation, and dopamine or derivatives thereof, mxene two-dimensional materials or derivatives thereof are combined with hydroxyl groups in the carbon nano tubes or derivatives thereof and the amino groups, so that the oxygen electronegativity in the hydroxyl groups is weakened, the binding capacity to hydrogen ions is reduced, and further, lone pair electrons in the amino groups are combined with the hydrogen ions, and the charges are not easy to aggregate, thereby achieving the antistatic aim.
The invention has the following advantages:
(1) When the antistatic wool fiber is prepared, dopamine or derivatives thereof and polystyrene sulfonic acid are used as dynamic crosslinking points, mxene or derivatives thereof and wool fiber, carbon nano tubes or derivatives thereof are bonded and crosslinked to construct a stable conductive network structure, and the complexation crosslinking means that amino, phenolic hydroxyl and the like in the polystyrene sulfonic acid are subjected to intercalation and locking with hydrophilic groups of the Mxene or derivatives thereof through hydrogen bonds and pi-pi stacking; on the other hand, mxene or its derivative builds a stable conductive network structure with TPU, carbon nanotube or its derivative by metal chelation, covalent reaction, etc., and the stable conductive network structure refers to a three-dimensional conductive network structure between Mxene or its derivative, carbon nanotube or its derivative.
(2) The method for crosslinking and depositing the dopamine or the derivative thereof and the polystyrene sulfonic acid not only improves the problems of poor dispersibility and easy aggregation of conductive substances, but also can effectively stabilize a conductive network structure, simultaneously enhances the complexation between a conductive substance layer and wool fibers, and does not need a large amount of chemical adhesion reagents.
(3) The volume specific resistance of the antistatic wool fiber prepared by the method is less than 20Ω & cm, has better antistatic performance, and is suitable for preparing antistatic wool yarns.
Drawings
FIG. 1 shows an Mxene two-dimensional material (Ti 3 C 2 Tx) mixing the conductive material with dopamine bonding the cross-linked wool fibers: the synthetic mechanism and chemical structure between polystyrene sulfonic acids.
FIG. 2 is a nuclear magnetic resonance spectrum of dopamine hydrochloride, dopamine hydrochloride and polystyrene sulfonic acid.
Wherein figure 2a is an H-profile of dopamine hydrochloride; FIG. 2b is a graph of dopamine hydrochloride C; FIG. 2c is an H-spectrum of dopamine hydrochloride and polystyrene sulfonic acid; FIG. 2d is a graph C of dopamine hydrochloride and polystyrene sulfonic acid.
Reference numerals illustrate: dopamine 1, polystyrene sulfonic acid 2, hydrogen bond 3, mxene two-dimensional material 4, covalent reaction 5, hydrogen bond 6, wool fiber 7 and CNTs-DMPA 8.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof.
The wool fibers used in this example were purchased from saussurea involucrata cashmere stock company;
2, 2-Dimethylol propionic acid (DMPA) was purchased from Nanjing Runbang chemical Co., ltd;
thionyl chloride (SOCl) 2 ) Purchased from Tianjin chemical reagent Co., ltd;
carboxylated carbon nanotubes (CNTs-COOH) were purchased from Nanjing Xianfeng nanomaterial technologies Co., ltd;
dopamine hydrochloride is purchased from the national pharmaceutical company, the company of the state pharmaceutical industry, the state rui;
triethylamine (TEA) was purchased from national pharmaceutical chemicals limited.
Example 1: preparation of modification solution (DA: PSS):
(1) Preparing a Tris buffer solution, and adjusting the pH to 8.5 by using dilute hydrochloric acid;
(2) Weighing 4g of sodium polystyrene sulfonate with the molecular weight of 70 kDa, adding into a Tris buffer solution, and stirring for 5min;
(3) Adding 2g of dopamine hydrochloride, continuously stirring, and reacting for 12 hours at normal temperature and normal pressure;
the dopamine hydrochloride monomer is easy to oxidize in the air, the color of the reaction system is gradually changed from colorless to pale yellow, and finally the reaction system is changed into dark brown;
(4) Dialyzing the reacted product by using a dialysis membrane with the molecular weight of 1000 Da, thoroughly removing inorganic salt, unreacted monomers or oligomers of dopamine and buffer substances, and further freeze-drying a dopamine dispersion system with impurities removed to obtain a solid product DA (dynamic random access system) PSS, and preparing a modified solution with the concentration of 0.5-4.5mg/mL and the pH of 8-10 for modification treatment of wool fibers;
as is clear from FIGS. 2a to 2d, the broad peak of DA: PSS at 0 to 2.3ppm is alkane proton on polystyrene sulfonic acid, the signal peak around 9.0ppm is proton signal peak of phenolic hydroxyl group, unlike the two very sharp phenolic hydroxyl proton peaks of raw material dopamine hydrochloride, the phenolic hydroxyl group in DA: PSS complex is two humps, thus no self polymerization occurs between dopamine monomers.
Example 2: the preparation method of the MXene two-dimensional material nano lamellar powder comprises the following steps: from MAX phase (Ti 3 AlC 2 ) Preparation of MXene (Ti) by selectively etching away Al layer 3 C 2 Tx) two-dimensional material.
(1) Firstly, dispersing 2.5g LiF into 12 mol/L of 50 mL hydrochloric acid solution under stirring;
(2) To the solution was slowly added 2.5g MAX (Ti 3 AlC 2 ）；
(3) Then, the solution is reacted for 48 hours at 40 ℃ under magnetic stirring, so that after the Al layer is completely etched for 48 hours, the obtained product is diluted by deionized water and centrifuged, and the process is repeated for a plurality of times until the pH value of the supernatant fluid is more than 6.0;
(4) And freeze-drying the precipitate obtained by centrifugation for 12 hours to obtain the MXene two-dimensional material nano lamellar powder.
Example 3: the preparation method of the CNTs-DMPA powder comprises the following steps:
3.0g of carboxylated CNTs are placed in a 500mL four-necked flask, 30mL of N, N-Dimethylformamide (DMF) is added, the mixture is dispersed for 30min by ultrasound, stirring is started, and then 100 mL of SOCl is slowly added 2 Heating to 70 ℃ and stirring for reaction for 16h, cooling, filtering, washing with DMF for 3 times, and removing unreacted SOCl on the surface 2 The filter cake was transferred to a 500mL Erlenmeyer flask, 80g of DMPA (DMF as solvent) and 20mL of TEA were added separately, heated to 50deg.C and reacted with magnetic stirring for 24h. After cooling, suction filtration is carried out, the filter cake is washed by deionized water for 5 times, and then is dried to constant weight in an oven at 60 ℃ to obtain chemically modified CNTs, which are marked as CNTs-DMPA.
TPU is a short name of Thermoplastic Urethane, the Chinese name is thermoplastic polyurethane elastomer, and the TPU is a high polymer material formed by the joint reaction polymerization of diphenylmethane diisocyanate (MDI), toluene Diisocyanate (TDI), macromolecular polyol and a chain extender.
Tris buffer solution refers to Tris-HCl (Tris hydrochloride buffer solution), and is specifically obtained by mixing Tris (Tris) solution with hydrochloric acid uniformly and then adding water for dilution.
CNTs-DMPA, wherein carboxylated CNTs are prepared by the reaction of thionyl chloride (SOCl) 2 ) And after surface modification of Triethylamine (TEA), crosslinking 2, 2-dimethylolpropionic acid (DMPA) to obtain CNTs-DMPA.
Carboxylation CNTs are obtained by placing carbon nanotubes into a mixed acid solution of concentrated sulfuric acid and concentrated nitric acid for etching ultrasonic treatment, and then placing the carbon nanotubes at 70-80 ℃ for stirring.
Embodiment four: a method of making an antistatic wool fiber comprising the steps of:
(1) Sequentially soaking wool fibers in a solution containing ammonia water (1.5 g/L) and salt (12 g/L), respectively soaking at constant temperature of 50 ℃ for 40 min, taking out, washing with water, drying, and weighing for later use, wherein the bath ratio is 1:70, so as to obtain ammonia and salt pretreated wool fibers;
(2) Immersing the wool fiber pretreated by ammonia/salt obtained in the step (1) in a solution containing dopamine: in a solution of polystyrene sulfonic acid (DA: PSS), the pH of the solution is 8.5, the solution is magnetically stirred at 100rpm for 12h at room temperature of 25 ℃, and the DA is obtained by washing and drying: PSS modified wool fibres, wherein the modifying solution: the concentration of dopamine and polystyrene sulfonic acid (DA: PSS) is 2.5mg/mL;
(3) Respectively weighing MXene (Ti) 3 C 2 Tx) and CNTs-DMPA, then sequentially added into DMF solution with mass-volume concentration of 20mg/mL, stirred for several hours by using a constant temperature magnetic stirrer, and finally MXene two-dimensional material (Ti 3 C 2 Tx) a mixed dispersion solution having a pH of 4.5, wherein the MXene two-dimensional material (Ti 3 C 2 Tx) is 10 mg/mL, CNTs-DMPA is 20mg/mL, the constant temperature of the constant temperature magnetic stirrer is 40 ℃, the stirring speed is 300rpm, and the stirring time is 6h;
(4) The modified wool fiber obtained in the step (2) is treated in MXene two-dimensional material (Ti 3 C 2 Tx), soaking in the mixed dispersion liquid at 70 ℃ for 60min, drying at 60 ℃ for 60min, and repeating soaking-drying for 5 times to obtain the antistatic wool fiber.
As shown in FIG. 1, mxene (Ti 3 C 2 Tx) mixing the conductive material with dopamine bonding the cross-linked wool fibers: the synthetic mechanism and chemical structure between polystyrene sulfonic acids. As can be seen from fig. 1: dopamine 1 on the one hand: amine groups, phenolic hydroxyl groups and the like in polystyrene sulfonic acid 2 are reacted with Mxene (Ti 3 C 2 Tx) 4 is bonded and crosslinked with hydrophilic groups;
on the other hand Mxene (Ti 3 C 2 Tx) through covalent reaction 5, hydrogen bond interaction 6, and wool fiber 7, CNTs-DMPA 8, a stable conductive network structure is constructed.
Fifth embodiment: a method of making an antistatic wool fiber comprising the steps of:
(1) Sequentially soaking wool fibers in ammonia water (1.5 g/L) solution and salt solution (12 g/L), respectively soaking at a constant temperature of 55 ℃ for 60min, taking out, washing with water, drying, and weighing for later use, wherein the bath ratio is 1:70, so as to obtain ammonia and salt pretreated wool fibers;
(2) Immersing the wool fiber pretreated by ammonia/salt obtained in the step (1) in a solution containing dopamine: in a solution of polystyrene sulfonic acid (DA: PSS), the pH of the solution is 10, magnetic stirring is carried out at 40rpm at 30 ℃ for 8 h, and DA is obtained by washing and drying: PSS modified wool fibres, wherein the modifying solution: the concentration of dopamine and polystyrene sulfonic acid (DA: PSS) is 2.5mg/mL;
(3) Respectively weighing MXene (Ti) 3 C 2 Tx) and CNTs-DMPA, then sequentially added into DMF solution with mass-volume concentration of 45mg/mL, stirred for several hours by using a constant temperature magnetic stirrer, and finally MXene two-dimensional material (Ti 3 C 2 Tx) a mixed dispersion solution having a pH of 4.5, wherein the MXene two-dimensional material (Ti 3 C 2 Tx) is at a concentration of35 The concentration of the CNTs-DMPA is 25mg/mL, the constant temperature of the constant temperature magnetic stirrer is 25 ℃, the stirring speed is 400rpm, and the stirring time is 6h;
(4) The modified wool fiber obtained in the step (2) is treated in MXene two-dimensional material (Ti 3 C 2 Tx), soaking in the mixed dispersion liquid at 70 ℃ for 60min, drying at 60 ℃ for 60min, and repeating soaking-drying for 5 times to obtain the antistatic wool fiber.
Comparative example:
(1) Sequentially soaking wool fibers in a solution containing ammonia water (1.5 g/L) and salt (12 g/L), respectively soaking at constant temperature of 50 ℃ for 40 min, taking out, washing with water, drying, and weighing for later use, wherein the bath ratio is 1:70, so as to obtain ammonia and salt pretreated wool fibers;
(2) CNTs with certain concentration are respectively weighed and then added into DMF solution with mass volume concentration of 25mg/mL, after stirring for a plurality of hours by using a constant-temperature magnetic stirrer, CNTs dispersion solution is obtained, the pH value of the mixed dispersion solution is 4.5, wherein the concentration of CNTs is 30 mg/mL, the constant-temperature of the constant-temperature magnetic stirrer is 40 ℃, the stirring speed is 350rpm, and the stirring time is 6 hours;
(3) Soaking the wool fibers obtained in the step (1) in the dispersion liquid of CNTs at 70 ℃ for 60min, drying at 60 ℃ for 60min, and repeating the soaking and drying for 5 times to obtain the antistatic wool fibers.
The antistatic wool fibers prepared in example 4, example 5 and comparative example were subjected to abrasion and water washing resistance tests, and the results are shown in tables 1 and 2.
TABLE 1 conductivity results of rub resistance and wash resistance tests
TABLE 2 specific resistance results of Friction and Water washing resistance test
As can be seen from tables 1 and 2, the PEDOT-PSS conductive composite fiber obtained by the preparation method provided by the invention has conductivity within 864-935S/cm after 700 times of friction; after 240 times of water washing, the conductivity is within 861-935S/cm, and after 700 times of friction, the volume specific resistance of the wool fiber is only 52 Ω & cm; after 240 times of water washing, the volume specific resistance is only 53 Ω & cm, which indicates that the wool fiber obtained by the preparation method of the invention has good washing resistance and antistatic property, and is suitable for preparing antistatic fabrics. In the comparative example, the wool fiber is not modified, and the conductive mixed dispersion solution obtained by adding the Mxene two-dimensional material or the derivative thereof and the carbon nanotube or the derivative thereof into the dimethylformamide solution is not treated, after friction resistance and ultrasonic washing, the conductivity is far lower than the numerical values of the embodiment 4 and the embodiment 5 of the invention, the specific resistance value is far higher than the specific resistance value of the embodiment 4 and the embodiment 5, the higher the conductivity is proved to be better, the lower the specific resistance value is, the conductivity is better, the antistatic property is better, the durability of the conductivity can be proved through friction resistance and ultrasonic washing, and the water resistance and the antistatic effect of the wool fiber prepared in the comparative example are not good.
Claims (8)
1. A preparation method of antistatic wool fiber is characterized in that: the method comprises the following steps:
(1) Pretreatment of wool fibers: firstly, immersing wool fibers in an ammonia water solution, and then immersing in a salt solution to finish pretreatment;
(2) Modification of wool fibers: preparing a modified solution from dopamine or derivatives thereof and polystyrene sulfonic acid, wherein the mass ratio of the dopamine or derivatives thereof to the polystyrene sulfonic acid is 1:2-2:1, immersing the pretreated wool fibers in the modified solution of the dopamine or derivatives thereof and the polystyrene sulfonic acid for modification treatment, wherein the immersion temperature is 20-30 ℃, stirring the modified solution for 8-36h at 40-200rpm in the immersion process, and washing and drying after the immersion is finished to obtain modified wool fibers;
(3) Preparing a conductive mixed dispersion solution: adding an Mxene two-dimensional material or a derivative thereof, a carbon nano tube or a derivative thereof into a dimethylformamide solution, and continuously stirring to obtain a conductive mixed dispersion solution;
(4) And (3) immersing the wool fiber obtained by modification in the step (2) in the conductive mixed dispersion solution in the step (3), and drying, washing and drying to obtain the antistatic wool fiber.
2. The method for producing an antistatic wool fiber according to claim 1, characterized in that: and (3) soaking the wool fibers in ammonia water and a salt solution at a constant temperature of 50 ℃ for 30-60min during pretreatment in the step (1), wherein the bath ratio of the ammonia water solution to the salt solution is 1:70.
3. The method for producing an antistatic wool fiber according to claim 1, characterized in that: the dopamine or the derivative thereof comprises one of gallic acid, dopamine hydrochloride, polydopamine (DATA) or N-3, 4-dihydroxyphenethyl acrylamide (DAA).
4. The method for producing an antistatic wool fiber according to claim 1, characterized in that: the concentration of the modifying solution in the step (2) is 0.5-4.5mg/mL, and the pH value is 8-10.
5. The method for producing an antistatic wool fiber according to claim 1, characterized in that: the concentration of dimethylformamide in the conductive mixed dispersion solution in the step (3) is 15-45 mg/mL, the concentration of Mxene two-dimensional material or derivative thereof is 5-35mg/mL, and the concentration of carbon nano tube or derivative thereof is 15-25mg/mL.
6. The method for producing an antistatic wool fiber according to claim 1, characterized in that: the constant temperature of the constant temperature magnetic stirrer in the step (3) is 25-45 ℃, the stirring speed is 100-400rpm, and the stirring time is 2.5-8.5h.
7. The method for producing an antistatic wool fiber according to claim 1, characterized in that: the carbon nanotubes or derivatives thereof in the step (3) include one or more of aminated carbon nanotubes, acidified carbon nanotubes, acrylamido carbon nanotubes (AM-CNTs), 2-dimethylolpropionic acid and acidified carbon nanotubes (DMPA-CNTs).
8. The method for producing an antistatic wool fiber according to claim 1, characterized in that: the MXene two-dimensional material or the derivative thereof comprises titanium carbide (Ti 3 C 2 Tx), dititanium carbide (Ti) 2 C) Niobium carbide (Nb) 2 C) Vanadium carbide (V) 2 C) Dititanium carbide (Ti) 2 CN) or titanium nitride (Ti) 2 N) is provided.
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