CN115045107B - Preparation method of antistatic carbon nanotube modified wool fiber - Google Patents
Preparation method of antistatic carbon nanotube modified wool fiber Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 207
- 210000002268 wool Anatomy 0.000 title claims abstract description 175
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 105
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 105
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 26
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 22
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 18
- 150000003839 salts Chemical class 0.000 claims description 16
- 229940074391 gallic acid Drugs 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 235000004515 gallic acid Nutrition 0.000 claims description 13
- 229910021529 ammonia Inorganic materials 0.000 claims description 11
- 229920001690 polydopamine Polymers 0.000 claims description 11
- 239000007983 Tris buffer Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000005470 impregnation Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000010981 drying operation Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 abstract description 42
- 239000011159 matrix material Substances 0.000 abstract description 22
- 229960003638 dopamine Drugs 0.000 abstract description 21
- 239000011231 conductive filler Substances 0.000 abstract description 7
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 22
- 229910052799 carbon Inorganic materials 0.000 description 19
- 230000004048 modification Effects 0.000 description 17
- 238000012986 modification Methods 0.000 description 17
- 239000000126 substance Substances 0.000 description 9
- 230000007246 mechanism Effects 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 238000009830 intercalation Methods 0.000 description 6
- 230000002687 intercalation Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 5
- -1 amino, imino Chemical group 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 239000004744 fabric Substances 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 239000004753 textile Substances 0.000 description 5
- 210000000085 cashmere Anatomy 0.000 description 4
- 238000010276 construction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000002216 antistatic agent Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
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- 238000010586 diagram Methods 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 229960001149 dopamine hydrochloride Drugs 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 125000001841 imino group Chemical group [H]N=* 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 229920002972 Acrylic fiber Polymers 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 206010020112 Hirsutism Diseases 0.000 description 1
- 241001145025 Saussurea involucrata Species 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009435 amidation Effects 0.000 description 1
- 238000007112 amidation reaction Methods 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 239000004020 conductor Substances 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 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
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000011885 synergistic combination Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
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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
- 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
- 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
- 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
- D06M15/61—Polyamines polyimines
-
- 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)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to a preparation method of antistatic carbon nanotube modified wool fibers, and belongs to the technical field of conductive fiber preparation. The preparation method provided by the invention comprises the following steps: (1) pretreating wool fibers; (2) Modifying the pretreated wool fiber by adopting (quasi) dopamine or a derivative thereof; (3) Immersing the wool fiber modified by the dopamine or the derivative thereof in a dispersion liquid of the carbon nano tube or the derivative thereof, drying, washing and drying to obtain the carbon nano tube modified wool fiber. The addition of the (quasi) dopamine or the derivative thereof improves the problems of poor dispersibility and easy agglomeration of the carbon nano tube, solves the problem of bonding firmness between the conductive filler and the matrix in the wool fiber, forms a continuous conductive path in the matrix of the wool fiber, and greatly improves the antistatic property and the washing resistance of the wool fiber.
Description
Technical Field
The invention belongs to the technical field of conductive fiber preparation, and particularly relates to a preparation method of antistatic carbon nanotube modified wool fibers.
Background
The textile material is an electric insulator material, has high electric resistance, particularly has wool, low terylene, acrylic fiber, chloron and other fibers with good elasticity, strong hygroscopicity and good warmth retention, is widely applied to textile raw materials, plays an increasingly important role in textile processing, and the textile made of the electric insulator material has the characteristics of plump texture, smooth and glutinous hand feeling, good drapability, noble and light and comfortable wearing and the like, and is popular with consumers for a long time. However, during the textile process, the fibers are in intimate contact and friction with each other or with the machine parts. Resulting in the transfer of charge on the surface of the object, resulting in static electricity. The fibers with the same charge repel each other, and the fibers with different charges attract the machine parts, so that the slivers are generated, the fiber hairiness is increased, the package is formed poorly, the fiber is stuck on the machine parts, the yarn breakage is increased, and the dispersible streak shadow is formed on the cloth cover. After the fiber is electrified, a large amount of dust is adsorbed, the fiber is easy to pollute, and the fiber and a human body and the fiber can be entangled or generate electric sparks. Therefore, electrostatic interference affects smooth fiber processing, and thus the wearability. When the electrostatic phenomenon is serious, the electrostatic voltage is up to several kilovolts, and spark can be generated due to discharge, so that fire disaster is caused, and serious consequences are caused. Therefore, effective reduction or removal of static electricity in fibrous materials is a technical problem that needs to be solved at present.
In recent years, with the increasing concern of electrostatic hazard at home and abroad. A great deal of research and tests are carried out on the aspect of antistatic fiber, remarkable results are obtained, and a great deal of attempts are carried out particularly in the technical field of antistatic wool fiber preparation. The current methods for preparing antistatic wool fibers mainly comprise three methods: firstly, an antistatic agent (such as nano MgO) is sprayed or impregnated on the surface of wool fibers, a layer of antistatic agent can be formed on the surface of the wool fibers, but the antistatic performance is temporary, and the antistatic agent drops off from the surface of the fibers after washing, so that the durability of the antistatic effect is affected; secondly, the conductive fiber with good conductivity is added in the wool fiber product processing process in a blending or weaving mode, so that the volume specific resistance of the fiber can be greatly reduced, and further, the generation of static electricity can be effectively prevented. Patent CN112239905A refers to a process for preparing blended wool conductive fibers, which is used for successfully preparing the blended wool conductive fibers from Belltron organic conductive fibers and wool fibers in a blending mode, and the process not only can improve the processing running condition of the fibers, but also can produce the blended wool fibers with excellent antistatic performance. However, the embedding of Belltron organic conductive fibers in the above patent greatly reduces the original excellent characteristics of cashmere fibers due to the influence of fineness and flexibility, so that the application of the cashmere fibers is limited in a certain range; thirdly, by means of the conductivity of the nano filler (such as carbon nano tube), the nano filler is bonded to wool fiber macromolecules by adopting a physical or chemical modification method, so that the aim of lasting antistatic function is fulfilled. Liu Rang adopts dopamine in-situ polymerization equally, so that the surface of wool fiber is covered with a discontinuous dopamine hydrophilic film, the hydrophobicity of the surface layer of the fiber is reduced, meanwhile, the carbon nano tube is loaded by utilizing the super-strong adhesion of the dopamine, and the antistatic effect is achieved by utilizing the conductivity of the carbon nano tube. However, there is no mention of the problem of adhesion effects between the conductive material and the wool fiber matrix (dopamine-carbon nanotubes to wool fabric composite antistatic finish [ J ]. Knitting industry 2020 (04): 41-44.).
The bonding force between the conductive filler (such as carbon nano tube) and the matrix in the antistatic wool fiber prepared by the current method is poor, and the bonding degree between the conductive layer and the wool fiber matrix is low, so that the conductive layer is fallen off due to the change of external environment (such as high temperature and humidity, the action of air and concentrated alkali, and the like), thereby affecting the antistatic durability and the washability of the antistatic wool fiber.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of antistatic carbon nanotube modified wool fibers, which solves the problem of bonding firmness of wool fiber conductive fillers and a matrix, and simultaneously forms a continuous conductive path in the wool fiber matrix, thereby greatly improving the antistatic performance and the washability of the wool fibers.
In order to solve the technical problems, the invention adopts a technical scheme that: the preparation method of the antistatic carbon nano tube modified wool fiber comprises the following steps:
(1) Carrying out ammonia/salt pretreatment on wool fibers to obtain wool fibers subjected to ammonia/salt pretreatment;
(2) Modifying the wool fiber pretreated by the ammonia/salt in the step (1) by using (quasi) dopamine or a derivative thereof to obtain the wool fiber modified by the (quasi) dopamine or the derivative thereof;
(3) Immersing the (quasi) dopamine or the derivative modified wool fiber obtained in the step (2) in a dispersion liquid of the carbon nano tube or the derivative thereof, drying, washing and drying to obtain the carbon nano tube modified wool fiber.
Further, the ammonia/salt pretreatment in the step (1) is to dip wool fibers into a solution containing 0.5-5.5g/L of ammonia water and 5-60 g/L of salt, take out the wool fibers after constant temperature dipping for 40-90min at 50 ℃, wash the wool fibers with water, dry the wool fibers, and weigh the wool fibers for standby, wherein the bath ratio is 1:50.
Further, the salt in the step (1) is one of sodium chloride, calcium chloride, sodium sulfate and the like.
Further, the (dopamine-like) or derivative thereof in the step (2) comprises one or more of gallic acid, dopamine hydrochloride, polydopamine-like (DATA), N-3, 4-dihydroxyphenethyl acrylamide (DAA) and MOA.
Further, the modification in the step (2) is to dip the wool fiber after ammonia/salt pretreatment into a mixed solution containing dopamine or derivatives thereof and tris buffer solution, wherein the pH value of the solution is 8-10, wash the solution with water and dry the solution to obtain the wool fiber; wherein the concentration of the dopamine (like) or the derivative thereof in the mixed solution is 0.5-6.5mg/m L; the concentration of tris buffer was 0.5-4.5M.
Further, the dipping in the modification process in the step (2) is dipping for 24-48 hours at room temperature of 20-30 ℃ under magnetic stirring at 60-100 rpm.
Further, the concentration of the carbon nanotubes and the derivatives thereof in the step (3) is 5-45mM.
Further, the temperature of the soaking in the step (3) is 65-85 ℃ and the time is 30-90min.
Further, the pH of the dispersion of the carbon nanotubes or derivatives thereof in the step (3) is 3.5-6.5.
Further, the carbon nanotubes and their derivatives 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).
The invention has the following advantages:
(1) The antistatic carbon nanotube modified wool fiber takes dopamine or a derivative thereof as a matrix, and the antistatic carbon nanotube modified wool fiber is prepared on the surface of the matrix by using an alternate intercalation assembly composite technology; the modification of the dopamine (or the derivative thereof) means that amino, imino and phenolic hydroxyl in the dopamine (or the derivative thereof) can be mutually bonded with carboxyl, amino and hydroxyl in wool fibers through coordination, hydrogen bond association, electrostatic interaction, hydrophobic interaction and even covalent reaction, so that the dopamine (or the derivative thereof) is firmly adhered to the surface of the wool fibers; the alternate intercalation composite technology is a process of obtaining a highly oriented continuous conductive path through alternate intercalation of bonding driving forces between two different substances, and the alternate intercalation effect not only increases the contact area of the carbon nano tube or the derivative thereof and the matrix, but also enhances the adhesion effect of the carbon nano tube or the derivative thereof and the matrix.
(2) The antistatic carbon nanotube modified wool fiber has an interface dynamic cooperative bonding action mode: amine groups, imino groups, phenolic hydroxyl groups and the like in the polydopamine on the surface of the matrix form covalent bonds and non-covalent bonds in a cooperative manner with oxygen-containing groups in the conductive filler deposited on the matrix.
(3) The invention adopts the rapid deposition method of dopamine, which not only solves the problems of dispersibility and reagglomeration of the conductive nano filler, but also enhances the adhesion between the conductive filler layer and wool fibers, and does not need a large amount of chemical adhesion reagent.
(4) The antistatic carbon nanotube modified wool fiber prepared by adopting the alternate intercalation composite technology not only enhances the adhesiveness between the conductive layer and the matrix, but also improves the problems of poor dispersibility and easy agglomeration of carbon nanotubes or derivatives thereof, so that the conductive filler can be uniformly dispersed, and a new thought is provided for the development of the antistatic fiber. The preparation method has the advantages of wide applicability, strong flexibility, high efficiency and the like, is an excellent way for efficiently and controllably preparing the high-performance antistatic wool fiber, and is convenient for industrial production.
(5) The volume specific resistance of the antistatic carbon nanotube modified wool fiber prepared by the method is below 21.4 kiloohm cm, and after 500 times of friction, the volume specific resistance is below 68.5 kiloohm cm; after 150 times of water washing, the volume specific resistance is 56.7 [ omega ] cm; the modified wool fiber has good washing fastness and antistatic property, and is suitable for preparing antistatic fabrics.
Drawings
Fig. 1 is a schematic diagram of a process for preparing an acidified carbon nanotube-modified wool fiber according to example 1 of the present invention.
FIG. 2 is a scanning electron microscope image of the acidified carbon nanotube-modified wool fiber of example 1; wherein a-b, c-d and e-f are respectively the electron microscope pictures of wool fiber, dopamine modified wool fiber and acidified carbon nano tube modified wool fiber at 100 mu m and 50 mu m.
Fig. 3 is an infrared spectrogram of the wool fiber before and after modification, wherein a, b and c are the wool fiber, the dopamine-modified wool fiber and the acidified carbon nanotube-modified wool fiber respectively.
Fig. 4 shows XRD patterns of wool fibers before and after modification, wherein a, b, and c are wool fibers, dopamine-modified wool fibers, and acidified carbon nanotube-modified wool fibers, respectively.
FIG. 5 is a process for preparing the acidified carbon nanotube-modified wool fiber 1 of example 1; wherein a and b are respectively the preparation process of the acidified carbon nanotube modified wool fiber and the synthesis mechanism of the acidified carbon nanotube and the dopamine 2 modified wool fiber 3.
FIG. 6 shows the synthesis mechanism of acidified carbon nanotubes and polydopamine modified wool fibers in example 1; wherein 2 is polydopamine; 4 is hydrogen bond; 3 is wool fiber; 1 is an acidified carbon nanotube; 5.7 is pi-pi conjugation and 8 is a chemical bond (esterification reaction).
Fig. 7 is a schematic diagram of the preparation process of the acidified carbon nanotube-modified wool fiber of example 2 of this invention.
FIG. 8 is a scanning electron microscope image of the acidified carbon nanotube-modified wool fiber of example 2; wherein a-b, c-d and e-f are respectively the electroscopic pictures of wool fiber, wool fiber modified by gallic acid and hexamethylenediamine and acidified carbon nano tube modified wool fiber at 100 mu m and 50 mu m.
Fig. 9 is an infrared spectrogram of wool fiber before and after modification, wherein a, b and c are wool fiber, wool fiber modified by gallic acid and hexamethylenediamine, and acidified carbon nanotube modified wool fiber respectively.
Fig. 10 shows XRD patterns of wool fibers before and after modification, wherein a, b, and c are wool fibers, wool fibers modified by gallic acid and hexamethylenediamine, and acidified carbon nanotube modified wool fibers, respectively.
FIG. 11 is a process for preparing the acidified carbon nanotube-modified wool fiber 1 of example 2; wherein a and b are respectively the preparation process of the acidified carbon nanotube modified wool fiber and the synthesis mechanism of the acidified carbon nanotube and gallic acid 2 cooperated with hexamethylenediamine 3 modified wool fiber 4.
FIG. 12 is a synthetic mechanism of acidified carbon nanotubes and polydopamine modified wool fiber in example 2; wherein 2 is hexamethylenediamine; 5 is hydrogen bond; 4 is wool fiber; 1 is an acidified carbon nanotube; 9 is amidation, 8 is hydroxylamino, 3 is hexamethylenediamine, and 6 is esterification.
FIG. 13 is a scanning electron microscope image of the acidified carbon nanotube-modified wool fiber of comparative example 3; wherein a-b and c-d are respectively the electron microscope pictures of the wool fiber and the acidified carbon nano tube modified wool fiber at 100 mu m and 50 mu m.
Fig. 14 is an infrared spectrogram of the wool fiber before and after modification, wherein a and b are the wool fiber and the acidified carbon nanotube modified wool fiber, respectively.
Fig. 15 is an XRD pattern of wool fibers before and after modification, wherein a and b are wool fibers and acidified carbon nanotube-modified wool fibers, respectively.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be embodied in other ways than those described herein, and persons skilled in the art will be able to make similar generalizations without departing from the spirit of the invention and therefore the invention is not limited to the specific embodiments disclosed below.
The wool fiber adopted in the embodiment is purchased from a saussurea involucrata cashmere stock company, the carbon nanotube dispersion liquid takes sodium dodecyl benzene sulfonate as a solvent, and the carbon nanotube is purchased from a Nanjing Xianfeng nanomaterial technology Co., ltd; other solutions not specifically described are water as a solvent.
The preparation method of the acidified carbon nano tube comprises the following steps: mixing carbon nano tubes and 75% concentrated nitric acid according to the mass-volume ratio of 1g:90mL of the mixture is stirred and mixed uniformly, the mixture is reacted for 12 hours at 135 ℃, and the obtained product is filtered, washed to be neutral and dried in vacuum, thus obtaining the acidified carbon nano tube.
The testing method comprises the following steps:
abrasion resistance test: the test was performed with reference to national standard GB/T21196.
Specific resistance test: and measuring the specific resistance value of the modified fiber by adopting a fiber specific resistance meter, weighing 15g of fiber, uniformly filling the fiber into a fiber test box, placing a fiber sample to be tested in an environment with the temperature of room temperature and the relative humidity of 65% +/-10% for balancing 4h, and then testing.
Measurement of water washing durability: reference (Cheng Wenqing. Preparation of conductive cashmere fibers and performance [ D ]. Beijing clothing college 2014) carried out a wash durability test.
Example 1: a method for preparing antistatic carbon nanotube-modified wool fibers, comprising the steps of:
(1) Immersing wool fibers in a solution containing ammonia water (2 g/L) and salt (10 g/L), immersing at a constant temperature of 50 ℃ for 60 min, taking out, washing with water, drying, and weighing for later use, wherein the bath ratio is 1:50, so as to obtain ammonia/salt pretreated wool fibers;
(2) Immersing the wool fibers pretreated by ammonia/salt obtained in the step (1) into a mixed solution containing dopamine hydrochloride (2 mg/mL) and tris buffer solution (1M), wherein the pH value of the solution is 8.5; then magnetically stirring at 80rpm for 24 hours at room temperature 25 ℃;
(3) Immersing the polydopamine modified wool fiber obtained in the step (2) in 35mM of an acidified carbon nanotube dispersion liquid, wherein the pH of the solution is 4, the immersion temperature is 80 ℃, the immersion time is 60min, then drying is carried out at 60 ℃ for 30min, and then the immersion-drying operation is repeated for 3 times; the acidified carbon nanotube modified wool fiber is obtained, and a scanning electron microscope image is shown in figure 2.
Performing performance test and structural characterization on the obtained acidified carbon nanotube modified wool fiber, wherein the test results are as follows:
Fig. 3 is an infrared spectrum of wool fibers before and after modification. By comparison, the characteristic absorption peak positions of the three wool fibers, namely, 3273.5cm -1 in N-H-based stretching vibration (νN-H), 1514.30 in N-H-based bending vibration (δN-H) and 1630.5cm -1 in C=O-based stretching vibration (νC=O), are not changed. It is shown that the modification treatment of the acidified carbon nanotubes does not damage the structure of the wool fiber, and meanwhile, the C=O group stretching vibration characteristic peak of the acidified carbon nanotubes appears at 1712cm -1 of the acidified carbon nanotube modified fiber, which shows that the acidified carbon nanotubes are successfully attached to the wool fiber. In addition, from the XRD test results of fig. 4, it was found that the modification of dopamine and acidified carbon nanotubes on the surface of wool fibers did not affect the structural properties.
FIG. 5 shows the synthesis mechanism and chemical structure of dopamine and acidified carbon nanotubes with wool fibers, respectively; wherein fig. 5 (a) and fig. 5 (b) are the preparation process of the acidified carbon nanotube-modified wool fiber 1 and the synthesis mechanism of the acidified carbon nanotube and the dopamine 2-modified wool fiber 3, respectively. As can be seen from fig. 5: the prepared acidified carbon nanotube modified wool fiber has a covalent bond and non-covalent bond cooperative bonding mode and a net-shaped conductive network structure construction.
As can be seen from fig. 6, the acidified carbon nanotube 1 can be intercalated to act as a nano space barrier in the substrate coated with the polydopamine 2 modified wool fiber 3, so that stacking of the acidified carbon nanotube is further inhibited, and the oxygen-containing group of the acidified carbon nanotube and the amino group, the imino group, the phenolic hydroxyl group and the like in the polydopamine 2 are inlaid on the substrate in a mode that the chemical bond 8 and the hydrogen bond 4 are cooperatively combined.
The method promotes the uniform and compact adhesion of the acidified carbon nanotubes on the dopamine-modified wool fiber matrix, enhances the interfacial adhesion, and improves the stability and durability of the acidified carbon nanotubes. In addition, regarding the construction of the mesh-type conductive network structure: on one hand, amino, imino, phenolic hydroxyl and the like in the polydopamine 1 on the surface of the matrix form chemical bonds 8 with hydroxyl, amino, carboxyl and other groups on wool fibers to form dynamic and collaborative bonding with the interface of the hydrogen bond 4; on the other hand, the bonding driving force between the acidified carbon nano tube and the polydopamine is alternately intercalated on the wool fiber, so that the net-shaped conductive network structure which is highly oriented and continuously conductive is obtained.
Tables 1 and 2 show the results of the friction and water wash resistance tests of the acidified carbon nanotube-modified wool fibers, as can be seen from tables 1 and 2: after 600 times of friction, the volume specific resistance of the acidified carbon nano tube modified wool fiber is only 84.50 [ mu ] cm; after 150 times of water washing, the volume specific resistance is only 56.7 [ mu ] cm, which indicates that the modified wool fiber has good washing fastness and antistatic property and is suitable for preparing antistatic fabrics.
TABLE 1 results of abrasion resistance test of acidified carbon nanotube modified wool fibers
Table 2 test results of washing resistance of acidified carbon nanotube-modified wool fibers
Example 2: a method for preparing antistatic carbon nanotube modified wool fiber, as shown in fig. 7, comprising the steps of:
(1) Immersing wool fibers in a solution containing 2g/L of ammonia water and 10g/L of salt, immersing at a constant temperature of 50 ℃ for 60 min hours, taking out, washing with water, drying, weighing for standby, wherein the bath ratio is 1:50, and obtaining ammonia/salt pretreated wool fibers;
(2) Immersing the wool fibers pretreated by ammonia/salt obtained in the step (1) into a mixed solution containing 2mg/mL of gallic acid, 1mg/mL of hexamethylenediamine and 1M of tris buffer solution, wherein the pH value of the solution is 8.5; then magnetically stirring at 80rpm for 24 hours at room temperature 25 ℃;
(3) Immersing the polydopamine modified wool fiber obtained in the step (2) in 35mM of an acidified carbon nanotube dispersion liquid, wherein the pH of the solution is 4, the immersion temperature is 80 ℃, the immersion time is 60min, then drying is carried out at 60 ℃ for 30min, and then the immersion-drying operation is repeated for 3 times; the acidified carbon nanotube modified wool fiber is obtained, and a scanning electron microscope image is shown in fig. 8.
Performing performance test and structural characterization on the obtained acidified carbon nanotube modified wool fiber, wherein the test results are as follows:
Fig. 9 is an infrared spectrum of wool fibers before and after modification. By comparison, the characteristic absorption peak positions of the three wool fibers, namely 3273.5 cm -1 for N-H-based stretching vibration (νN-H), 1514.30 for N-H-based bending vibration (δN-H) and 1630.5cm -1 for C=O-based stretching vibration (νC=O), are not changed. It is shown that the modification treatment of the acidified carbon nanotubes does not damage the structure of the wool fiber, and meanwhile, the c=o group tensile vibration characteristic peak of the acidified carbon nanotubes appears at 1712 cm -1 in the acidified carbon nanotube modified fiber, which shows that the acidified carbon nanotubes are successfully attached to the wool fiber. In addition, from the XRD test results of fig. 10, it was found that the modification of gallic acid and acidified carbon nanotubes on the surface of wool fiber did not affect the structural properties.
FIG. 11 shows the synthesis mechanism and chemical structure of gallic acid-co-hexamethylenediamine and acidified carbon nanotubes, respectively, with wool fibers; wherein fig. 11 (a) and fig. 11 (b) are a preparation process of the acidified carbon nanotube-modified wool fiber 1 and a synthesis mechanism of the acidified carbon nanotube-gallic acid 2 synergistic hexamethylenediamine 3-modified wool fiber 4, respectively. As can be seen from fig. 11: the prepared acidified carbon nanotube modified wool fiber has a covalent bond and non-covalent bond cooperative bonding mode and a net-shaped conductive network structure construction.
As can be seen from fig. 12, the acidified carbon nanotube 1 can be intercalated to act as a nano space barrier in the matrix coated with the gallic acid 3 synergistically modified wool fiber 4, so that stacking of the acidified carbon nanotube is further inhibited, and the oxygen-containing group of the acidified carbon nanotube and carboxyl and phenolic hydroxyl in the gallic acid 3 are inlaid on the matrix in a manner of synergistic combination of chemical bond and hydrogen bond 5. The method promotes the acidified carbon nano tube to be uniformly and tightly adhered to the gallic acid and hexamethylenediamine modified wool fiber matrix, enhances the interfacial adhesion effect, and improves the stability and the durability of the acidified carbon nano tube. In addition, regarding the construction of the mesh-type conductive network structure: on one hand, carboxyl and phenolic hydroxyl in gallic acid 3 on the surface of a matrix form chemical bonds 8, 6 and 9 with hydroxyl, amino, carboxyl and other groups on wool fibers to form dynamic and collaborative bonding with the interface of a hydrogen bond 5; on the other hand, the bonding driving force between the acidified carbon nano tube and the gallic acid is alternately intercalated on the wool fiber, so that the net-shaped conductive network structure which is highly oriented and continuously conductive is obtained.
Tables 3 and 4 show the results of the friction and water wash resistance tests of the acidified carbon nanotube-modified wool fibers, as can be seen from tables 3 and 4: after 600 times of friction, the volume specific resistance of the acidified carbon nano tube modified wool fiber is only 55.4-ohm cm; after 150 times of water washing, the volume specific resistance is only 42.3 [ delta ] cm, which indicates that the modified wool fiber has good washing fastness and antistatic property and is suitable for preparing antistatic fabrics.
TABLE 3 results of abrasion resistance test of acidified carbon nanotube modified wool fibers
Table 4 test results of water-wash resistance of acidified carbon nanotube modified wool fibers
Comparative example 3:
step (2) was omitted and the other materials were consistent with examples 1 and 2 to obtain acidified carbon nanotube-modified wool fibers, as shown in FIG. 13.
Performing performance test and structural characterization on the obtained acidified carbon nanotube modified wool fiber, wherein the test results are as follows:
Fig. 14 and 15 are infrared spectra of wool fibers before and after modification. By comparison, the characteristic absorption peak positions of N-H group stretching vibration (v N-H) and N-H group bending vibration (delta N-H) in the two wool fibers are 3273.5 cm -1, 1514.30 and C=O group stretching vibration (v C=O is 1630.5cm -1, so that the modification treatment of the acidified carbon nano tube does not damage the structure of the wool fibers, and the C=O group stretching vibration characteristic peak of the acidified carbon nano tube appears at 1712 cm -1 of the acidified carbon nano tube modified fiber, so that the acidified carbon nano tube is successfully attached to the wool fibers.
Tables 5 and 6 show the results of the friction and water wash resistance tests for the acidified carbon nanotube-modified wool fibers, as can be seen from tables 5 and 6: after 600 times of friction, the volume specific resistance of the acidified carbon nano tube modified wool fiber is 1545.8-ohm cm; after 150 times of washing, the volume specific resistance was 1348.6. Delta. Cm, which indicates that the wool fiber had poor washing resistance and abrasion resistance.
TABLE 5 results of abrasion resistance test of acidified carbon nanotube modified wool fibers
Table 6 test results of washing resistance of acidified carbon nanotube modified wool fiber
The invention provides a low-temperature green impregnation process based on interface dynamic synergistic bonding effect, and provides a method for preparing antistatic carbon nanotube modified wool fibers by using an alternate intercalation assembly composite technology, which solves the problem of bonding firmness of conductive fillers and a matrix in the wool fibers, and simultaneously forms a continuous conductive path in the wool fiber matrix, thereby greatly improving the antistatic performance and the water washing resistance of the wool fibers.
The above describes in detail the preparation method of the antistatic carbon nanotube modified wool fiber provided by the application, and specific examples are applied to illustrate the principle and the implementation of the application, and the above examples are only used for helping to understand the method and the core idea of the application; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in accordance with the ideas of the present application, the present description should not be construed as limiting the present application in view of the above.
Claims (1)
1. A method for preparing antistatic carbon nanotube modified wool fibers, which is characterized by comprising the following steps:
(1) Immersing wool fibers in a solution containing 2g/L ammonia water and 10g/L salt for 60min at a constant temperature of 50 ℃, taking out, washing with water, drying, weighing for later use, wherein the bath ratio is 1:50, obtaining ammonia/salt pretreated wool fibers;
(2) Immersing the wool fibers pretreated by ammonia/salt obtained in the step (1) into a mixed solution containing 2mg/mL of gallic acid, 1mg/mL of hexamethylenediamine and 1M of tris buffer solution, wherein the pH value of the solution is 8.5; then magnetically stirring at 80rpm for 24 hours at room temperature 25 ℃;
(3) Impregnating the polydopamine modified wool fiber obtained in the step (2) in 35mM of an acidified carbon nanotube dispersion liquid, wherein the pH value of the solution is 4, the impregnation temperature is 80 ℃, the impregnation time is 60min, then drying is carried out at 60 ℃ for 30min, and then the impregnation and drying operation is repeated for 3 times, so that the acidified carbon nanotube modified wool fiber, namely the antistatic carbon nanotube modified wool fiber, is obtained;
the preparation method of the acidified carbon nano tube comprises the following steps: mixing carbon nano tubes and 75% concentrated nitric acid according to the mass-volume ratio of 1g:90mL of the mixture is stirred and mixed uniformly, the mixture is reacted for 12 hours at 135 ℃, and the obtained product is filtered, washed to be neutral and dried in vacuum, thus obtaining the acidified carbon nano tube.
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