CN109594325B - Zinc oxide nanorod array modified moisture-conductive cotton fiber or fabric thereof and preparation method thereof - Google Patents
Zinc oxide nanorod array modified moisture-conductive cotton fiber or fabric thereof and preparation method thereof Download PDFInfo
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- CN109594325B CN109594325B CN201811508172.4A CN201811508172A CN109594325B CN 109594325 B CN109594325 B CN 109594325B CN 201811508172 A CN201811508172 A CN 201811508172A CN 109594325 B CN109594325 B CN 109594325B
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 286
- 229920000742 Cotton Polymers 0.000 title claims abstract description 194
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 143
- 239000004744 fabric Substances 0.000 title claims abstract description 114
- 239000002073 nanorod Substances 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 51
- 239000000243 solution Substances 0.000 claims abstract description 45
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002159 nanocrystal Substances 0.000 claims abstract description 34
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 19
- 239000011248 coating agent Substances 0.000 claims abstract description 18
- 238000000576 coating method Methods 0.000 claims abstract description 18
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004246 zinc acetate Substances 0.000 claims abstract description 17
- 229920002678 cellulose Polymers 0.000 claims abstract description 15
- 239000001913 cellulose Substances 0.000 claims abstract description 15
- 108010022355 Fibroins Proteins 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 13
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 238000002791 soaking Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000002386 leaching Methods 0.000 claims description 8
- 230000002040 relaxant effect Effects 0.000 claims description 7
- 239000012460 protein solution Substances 0.000 claims 1
- 229920001046 Nanocellulose Polymers 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 description 15
- 229920004933 Terylene® Polymers 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000005020 polyethylene terephthalate Substances 0.000 description 6
- 230000035699 permeability Effects 0.000 description 5
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229920000297 Rayon Polymers 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000010041 electrostatic spinning Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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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
- D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/06—Inorganic compounds or elements
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/05—Cellulose or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/15—Proteins or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention provides a zinc oxide nanorod array modified moisture-conductive cotton fiber or fabric thereof and a preparation method thereof, wherein the preparation method comprises the following steps: after the cotton fiber is treated by low-temperature liquid nitrogen, micro-stretching to obtain the pretreated cotton fiber; dripping the ethanol solution of zinc acetate into the ethanol solution of sodium hydroxide, and heating for reaction to obtain a zinc oxide nanocrystal solution; repeatedly coating a zinc oxide nanocrystalline solution on one surface of the pretreated cotton fiber, drying at room temperature, completely soaking in a mixed solution of zinc nitrate and hexamethylenetetramine, and vibrating at constant temperature to obtain zinc oxide modified moisture-conducting cotton fiber or fabric thereof; and coating a fibroin solution containing nano-cellulose on the other surface of the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof, and drying at room temperature to obtain the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof. One surface of the prepared zinc oxide nanorod array modified moisture-conductive cotton fiber or fabric thereof comprises a zinc oxide nanorod array, and the other surface of the prepared zinc oxide nanorod array modified moisture-conductive cotton fiber or fabric thereof comprises nano cellulose whiskers and fibroin, so that the moisture conductivity of the cotton fiber is remarkably improved.
Description
Technical Field
The invention belongs to the technical field of textile materials, and particularly relates to a zinc oxide nanorod array modified moisture-permeable cotton fiber or fabric thereof and a preparation method thereof.
Background
The cotton fiber is an important raw material in the textile industry, the main component of the cotton fiber is cellulose, the cellulose contains a plurality of hydrophilic groups such as hydroxyl, and the cotton fiber has natural curling and a hollow cavity structure, and the cross section is in a waist circle shape, so the cotton fiber has excellent hygroscopicity, heat retention, softness, dyeing property and antistatic property, and good serviceability, is the most widely used natural clothing fiber, but the cotton fiber has the defects of poor moisture conductivity, easy wrinkling, poor elasticity, easy shrinkage, non-corrosion resistance and the like.
At present, in order to improve the moisture conductivity of cotton fiber fabrics, cotton fibers and moisture-conductive quick-drying functional fibers are blended into yarns or are directly manufactured into the cotton fiber fabrics with moisture conductivity functions, for example, the yarns disclosed in Chinese patent CN1563533 with moisture conductivity and steam permeability comfort functions and contact comfort functions are formed by blending fine denier circular cross-section terylene, cotton fibers or viscose fibers and H-shaped cross-section terylene fibers, the H-shaped cross-section terylene fibers are used as main fibers to ensure that the yarns have high moisture conductivity and comfort functions, the fine denier terylene is used to reduce the elastic touch amount of the yarns, and the fine denier terylene and the H-shaped cross-section terylene fibers are combined to form more and finer capillaries so as to improve the moisture conductivity; the method has the advantages that the cotton fiber or the viscose fiber is adopted to improve the ventilation comfort function and the contact comfort of the yarn, the influence on the moisture-conducting comfort function of the yarn is small, the method uses a large amount of raw materials, and the cotton blended yarn is endowed with certain moisture-conducting property, but the influence on the wearability of the cotton fiber is large. At present, aiming at the finishing of the modified aspect of the cotton fiber with moisture-conducting function, the Chinese patent CN 108385231A discloses a device for moisture-conducting function of the cotton and submicron fiber composite yarn and a using method thereof, the original cotton is carded and peeled to obtain a cotton net, the cotton net is introduced between an upper roller for holding the cotton net and a lower roller for holding the cotton net, a reciprocating motion macro-electrostatic spinning nozzle is utilized to fly polymer spinning solution to the cotton net under the action of a high-voltage electrostatic field, a solvent is volatilized, jet flow is stretched and solidified into submicron fiber, part of the submicron fiber is attached to the cotton net and penetrates into the cotton net to be arranged in a certain direction to obtain the cotton net compounded with the submicron fiber, and finally the cotton net compounded with the submicron fiber is subjected to horn mouth slivering, drawing, roving and spun yarn to prepare the moisture-conducting function submicron fiber composite yarn, the method adds the electrostatic spinning technology into the preparation process of the cotton yarn, the cotton yarn contains a concave-convex structure formed by superfine fibers, the concave-convex structure is similar to a plurality of microcapillaries, so that a differential capillary effect common to porous hollow fibers is formed, and the cotton yarn has good moisture-conducting performance. According to the prior art, the micro-nano material is used for carrying out surface modification on the cotton fiber, so that the possibility is provided for improving the moisture conductivity of the cotton fiber.
Disclosure of Invention
The invention provides a zinc oxide nanorod array modified moisture-conductive cotton fiber or fabric and a preparation method thereof, and the zinc oxide nanorod array modified moisture-conductive cotton fiber or fabric is prepared by subjecting a cotton fiber or a cotton fiber fabric to low-temperature and micro-stretching treatment, attaching zinc oxide nanocrystals to one surface of the cotton fiber or the cotton fiber fabric, growing the zinc oxide nanocrystals into a zinc oxide nanorod array, and attaching nanocellulose whiskers and fibroin to the other surface of the cotton fiber or the cotton fiber fabric, so that the moisture-conductive performance of the cotton fiber or the cotton fiber fabric is remarkably improved, and the heat-insulating property and the wearability of the cotton fiber or the cotton fiber fabric are less influenced.
In order to solve the technical problems, the technical scheme of the invention is as follows:
the utility model provides a modified wet cotton fiber of leading of zinc oxide nanorod array or its fabric, the modified wet cotton fiber of leading of zinc oxide nanorod array or its fabric's one side includes zinc oxide nanorod array, the bottom of zinc oxide nanorod array distributes in cotton fiber surface or cotton fibrous cavity, the cotton fiber surface is surpassed at the top of zinc oxide nanorod array, the modified wet cotton fiber of leading of zinc oxide nanorod array or its fabric's another side includes nanometer cellulose whisker and fibroin.
The invention also provides a preparation method of the zinc oxide nanorod array modified moisture-conductive cotton fiber or fabric thereof, which comprises the following steps:
(1) after the cotton fiber or the cotton fiber fabric is treated by low-temperature liquid nitrogen, micro-stretching to obtain the pretreated cotton fiber;
(2) dripping the ethanol solution of zinc acetate into the ethanol solution of sodium hydroxide, and heating for reaction to obtain a zinc oxide nanocrystal solution;
(3) repeatedly coating the zinc oxide nanocrystalline solution prepared in the step (2) on one surface of the pretreated cotton fiber prepared in the step (1), and drying at room temperature to obtain a zinc oxide nanocrystalline modified cotton fiber or fabric thereof;
(4) completely soaking the zinc oxide nanocrystal modified cotton fiber or fabric thereof prepared in the step (3) in a mixed solution of zinc nitrate and hexamethylenetetramine, vibrating at a constant temperature, taking out, and leaching to obtain zinc oxide modified moisture-conducting cotton fiber or fabric thereof;
(5) and (3) coating the other side of the zinc oxide nanorod array modified moisture-conductive cotton fiber or fabric thereof prepared in the step (4) with a fibroin solution containing nano-cellulose, and drying at room temperature to obtain the zinc oxide nanorod array modified moisture-conductive cotton fiber or fabric thereof.
Preferably, in the step (1), the temperature of the low-temperature liquid nitrogen treatment is-5-0 ℃ and the time is 5-15 min.
Preferably, in the step (1), the micro-stretching strength is 10 to 30cN/cm, the stretching time is 3 to 5s, the relaxation time and the stretching time in the intermittent stretching are 1 to 3 min.
Preferably, in the step (2), the mass ratio of the zinc acetate to the sodium hydroxide is 2: 0.8-1.2.
Preferably, in the step (2), the dropping rate is 0.5-1ml/min, the heating reaction temperature is 60-65 ℃, and the heating reaction is continued for 15-30min after the dropping is finished.
Preferably, in the step (3), the thickness of the zinc oxide nanocrystals in the cotton fiber or fabric modified with zinc oxide nanocrystals is 0.1 to 0.2 μm.
Preferably, in the step (4), the molar ratio of zinc nitrate to hexamethylenetetramine in the mixed solution of zinc nitrate and hexamethylenetetramine is 1:1, and the content of zinc nitrate is 0.03 to 0.05 mol/L.
Preferably, in the step (4), the constant temperature shaking is performed at 70-90 ℃ for 1-2 h.
Preferably, in the step (4), the diameter of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or fabric thereof is 200-400nm, the length is 1-3 μm, and the density is 320-480/cm 2.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention reduces the crystallinity and the grain size of the cotton fiber by processing the cotton fiber with low-temperature liquid nitrogen, then loosens cellulose macromolecules in the cotton fiber further by a micro-stretching process, even forms micro gaps, exposes partial cavity structure, enables the zinc oxide nanocrystals to be attached to the surface of the cotton fiber, or enables the zinc oxide nanocrystals to enter the cavity of the cotton fiber, and can be embedded into the crystallization area of the cotton fiber due to the small grain size of the zinc oxide nanocrystals, and can form good bonding force with active group hydroxyl on the surface of the cotton fiber due to the hydrophilic and oleophobic properties of the zinc oxide surface, thereby improving the bonding force between the zinc oxide nanorods and the cotton fiber.
(2) The invention is characterized in that after the cotton fiber or the cotton fiber fabric is subjected to low-temperature and micro-stretching treatment, zinc oxide nano-crystals are attached to one surface of the cotton fiber or the cotton fiber fabric, then the zinc oxide nano-crystals grow into a zinc oxide nano-rod array, the hydrophilic moisture-conducting performance of the cotton fiber or the cotton fiber fabric on the one surface is adjusted by controlling the size and the density of the zinc oxide nano-rods by utilizing the structure and the surface performance of the zinc oxide nano-rods, then nano-cellulose whiskers and fibroin are attached to the other surface of the cotton fiber or the cotton fiber fabric, and micro holes remained after the low-temperature and micro-stretching treatment are filled to form a film, so that the mechanical property and the service performance of the cotton fiber or the cotton fiber fabric are improved.
(3) The zinc oxide nanorod array modified moisture-permeable cotton fiber or fabric thereof prepared by the invention combines physical treatment and nanotechnology and is used in the modification and finishing of the cotton fiber, the moisture permeability of the cotton fiber and the fabric thereof is obviously improved by changing the microscopic form of the surface of the cotton fiber, and the influence on the heat preservation property and the wearability of the cotton fiber and the fabric thereof is small.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1:
(1) treating cotton fiber or cotton fiber fabric with low temperature liquid nitrogen at-5 deg.C for 5min, micro-stretching at 10cN/cm for 3s, relaxing, and stretching for 1min to obtain pretreated cotton fiber.
(2) According to the mass ratio of the zinc acetate to the sodium hydroxide of 2:0.8, dripping the ethanol solution of the zinc acetate into the ethanol solution of the sodium hydroxide at the speed of 0.5ml/min, heating to react at 60 ℃, and continuing to heat to react for 15min after dripping is finished to obtain the zinc oxide nano-crystalline solution.
(3) And repeatedly coating the zinc oxide nanocrystal solution on one surface of the pretreated cotton fiber, and drying at room temperature to obtain the zinc oxide nanocrystal modified cotton fiber or fabric with the thickness of 0.1 mu m.
(4) Completely soaking the cotton fiber or fabric modified by the zinc oxide nanocrystals into a mixed solution of zinc nitrate and hexamethylenetetramine in a molar ratio of 1:1, wherein the content of the zinc nitrate is 0.03mol/L, shaking at a constant temperature of 70 ℃ for 1h, taking out, and leaching to obtain the zinc oxide modified moisture-conducting cotton fiber or fabric thereof.
(5) And coating a fibroin solution containing 5 wt% of nano-cellulose on the other side of the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof, and drying at room temperature to obtain the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof, wherein the diameter of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 200nm, the length of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 1 mu m, and the density of the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 320/cm 2.
Example 2:
(1) treating cotton fiber or cotton fiber fabric with low temperature liquid nitrogen at 0 deg.C for 15min, micro-stretching at 30cN/cm strength for 5s, relaxing, and stretching for 3min to obtain pretreated cotton fiber.
(2) According to the mass ratio of the zinc acetate to the sodium hydroxide of 2:1.2, dripping the ethanol solution of the zinc acetate into the ethanol solution of the sodium hydroxide at the speed of 1ml/min, heating to react at 65 ℃, and continuing to heat to react for 30min after the dripping is finished to obtain the zinc oxide nanocrystal solution.
(3) And repeatedly coating the zinc oxide nanocrystal solution on one surface of the pretreated cotton fiber, and drying at room temperature to obtain the zinc oxide nanocrystal modified cotton fiber or fabric thereof with the thickness of 0.2 mu m.
(4) Completely soaking the cotton fiber or fabric modified by the zinc oxide nanocrystals into a mixed solution of zinc nitrate and hexamethylenetetramine in a molar ratio of 1:1, wherein the content of the zinc nitrate is 0.05mol/L, shaking at a constant temperature of 90 ℃ for 2h, taking out, and leaching to obtain the zinc oxide modified moisture-conducting cotton fiber or fabric thereof.
(5) And coating a fibroin solution containing 10 wt% of nano-cellulose on the other side of the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof, and drying at room temperature to obtain the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof, wherein the diameter of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 400nm, the length of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 3 mu m, and the density of the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 480/cm 2.
Example 3:
(1) treating cotton fiber or cotton fiber fabric with low temperature liquid nitrogen at-2 deg.C for 12min, micro-stretching at 20cN/cm strength for 4s, relaxing, and stretching for 2min to obtain pretreated cotton fiber.
(2) According to the mass ratio of the zinc acetate to the sodium hydroxide of 2:0.9, dripping the ethanol solution of the zinc acetate into the ethanol solution of the sodium hydroxide at the speed of 0.6ml/min, heating to react at 63 ℃, and continuing to heat to react for 20min after dripping is finished to obtain the zinc oxide nano-crystalline solution.
(3) And repeatedly coating the zinc oxide nanocrystal solution on one surface of the pretreated cotton fiber, and drying at room temperature to obtain the zinc oxide nanocrystal modified cotton fiber or fabric with the thickness of 0.15 mu m.
(4) Completely soaking the cotton fiber or fabric modified by the zinc oxide nanocrystals into a mixed solution of zinc nitrate and hexamethylenetetramine in a molar ratio of 1:1, wherein the content of the zinc nitrate is 0.04mol/L, shaking at a constant temperature of 80 ℃ for 2 hours, taking out, and leaching to obtain the zinc oxide modified moisture-conducting cotton fiber or fabric thereof.
(5) And coating a fibroin solution containing 10 wt% of nano-cellulose on the other side of the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof, and drying at room temperature to obtain the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof, wherein the diameter of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 400nm, the length of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 3 mu m, and the density of the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 480/cm 2.
Example 4:
(1) and (3) carrying out micro-stretching on the cotton fiber or the cotton fiber fabric for 3.5s at the strength of 15cN/cm after the cotton fiber or the cotton fiber fabric is subjected to low-temperature liquid nitrogen at the temperature of-4 ℃ for 12min, and relaxing, wherein the stretching time in the intermittent stretching is 2.5min, so as to obtain the pretreated cotton fiber.
(2) According to the mass ratio of the zinc acetate to the sodium hydroxide of 2:1.1, dripping the ethanol solution of the zinc acetate into the ethanol solution of the sodium hydroxide at the speed of 0.8ml/min, heating to react at 64 ℃, and continuing to heat to react for 25min after dripping is finished to obtain the zinc oxide nano-crystalline solution.
(3) And repeatedly coating the zinc oxide nanocrystal solution on one surface of the pretreated cotton fiber, and drying at room temperature to obtain the zinc oxide nanocrystal modified cotton fiber or fabric with the thickness of 0.13 mu m.
(4) Completely soaking the cotton fiber or fabric modified by the zinc oxide nanocrystalline into a mixed solution of zinc nitrate and hexamethylenetetramine in a molar ratio of 1:1, wherein the content of the zinc nitrate is 0.042mol/L, shaking at a constant temperature of 75 ℃ for 1.5h, taking out, and leaching to obtain the zinc oxide modified moisture-conducting cotton fiber or fabric thereof.
(5) And coating a fibroin solution containing 6 wt% of nano-cellulose on the other side of the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof, and drying at room temperature to obtain the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof, wherein the diameter of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 320nm, the length of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 2.3 mu m, and the density of the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 400/cm 2.
Example 5:
(1) treating cotton fiber or cotton fiber fabric with low temperature liquid nitrogen at-5 deg.C for 15min, micro-stretching at 10cN/cm for 5s, relaxing, and stretching for 1min to obtain pretreated cotton fiber.
(2) According to the mass ratio of the zinc acetate to the sodium hydroxide of 2:1.2, dripping the ethanol solution of the zinc acetate into the ethanol solution of the sodium hydroxide at the speed of 0.5ml/min, heating to react at 65 ℃, and continuing to heat to react for 15min after dripping is finished to obtain the zinc oxide nano-crystalline solution.
(3) And repeatedly coating the zinc oxide nanocrystal solution on one surface of the pretreated cotton fiber, and drying at room temperature to obtain the zinc oxide nanocrystal modified cotton fiber or fabric thereof with the thickness of 0.2 mu m.
(4) Completely soaking the cotton fiber or fabric modified by the zinc oxide nanocrystals into a mixed solution of zinc nitrate and hexamethylenetetramine in a molar ratio of 1:1, wherein the content of the zinc nitrate is 0.03mol/L, shaking at a constant temperature of 90 ℃ for 1h, taking out, and leaching to obtain the zinc oxide modified moisture-conducting cotton fiber or fabric thereof.
(5) And coating a fibroin solution containing 10 wt% of nano-cellulose on the other side of the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof, and drying at room temperature to obtain the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof, wherein the diameter of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 270nm, the length of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 1.8 mu m, and the density of the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 370 pieces/cm 2.
Example 6:
(1) treating cotton fiber or cotton fiber fabric with low temperature liquid nitrogen at 0 deg.C for 5min, micro-stretching at 30cN/cm strength for 3s, relaxing, and stretching for 3min to obtain pretreated cotton fiber.
(2) According to the mass ratio of the zinc acetate to the sodium hydroxide of 2:0.8, dripping the ethanol solution of the zinc acetate into the ethanol solution of the sodium hydroxide at the speed of 1ml/min, heating to react at the temperature of 60 ℃, and continuing to heat to react for 30min after the dripping is finished to obtain the zinc oxide nanocrystal solution.
(3) And repeatedly coating the zinc oxide nanocrystal solution on one surface of the pretreated cotton fiber, and drying at room temperature to obtain the zinc oxide nanocrystal modified cotton fiber or fabric with the thickness of 0.1 mu m.
(4) Completely soaking the cotton fiber or fabric modified by the zinc oxide nanocrystals into a mixed solution of zinc nitrate and hexamethylenetetramine in a molar ratio of 1:1, wherein the content of the zinc nitrate is 0.05mol/L, shaking at a constant temperature of 70 ℃ for 2 hours, taking out, and leaching to obtain the zinc oxide modified moisture-conducting cotton fiber or fabric thereof.
(5) And coating a fibroin solution containing 5 wt% of nano-cellulose on the other side of the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof, and drying at room temperature to obtain the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof, wherein the diameter of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 240nm, the length of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 2.7 mu m, and the density of the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 415/cm 2.
The results of moisture permeability, moisture absorption and mechanical properties of the zinc oxide nanorod array modified moisture-permeable cotton fiber fabrics prepared in examples 1-6 and the untreated cotton fiber fabric were determined as follows:
as can be seen from the above table, the moisture permeability of the zinc oxide nanorod array modified moisture-permeable cotton fiber fabric prepared by the method is remarkably improved, which means that the moisture permeability is remarkably improved, and the mechanical property is not greatly reduced.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (7)
1. A zinc oxide nanorod array modified moisture-conductive cotton fiber fabric is characterized in that: one side of the moisture-conductive cotton fiber fabric modified by the zinc oxide nanorod array comprises the zinc oxide nanorod array, the bottom of the zinc oxide nanorod array is distributed on the surface of the cotton fiber or in a cavity of the cotton fiber, the top of the zinc oxide nanorod array exceeds the surface of the cotton fiber, and the other side of the moisture-conductive cotton fiber fabric modified by the zinc oxide nanorod array comprises nano-cellulose whiskers and fibroin;
the preparation method comprises the following steps:
(1) after the cotton fiber fabric is subjected to low-temperature liquid nitrogen treatment, micro-stretching to obtain a pretreated cotton fiber fabric; the temperature of the low-temperature liquid nitrogen treatment is-5-0 ℃, and the time is 5-15 min; the micro-stretching strength is 10-30cN/cm, stretching for 3-5s, relaxing, and stretching time in intermittent stretching is 1-3 min;
(2) dripping the ethanol solution of zinc acetate into the ethanol solution of sodium hydroxide, and heating for reaction to obtain a zinc oxide nanocrystal solution;
(3) repeatedly coating the zinc oxide nanocrystalline solution prepared in the step (2) on one surface of the pretreated cotton fiber prepared in the step (1), and drying at room temperature to obtain a zinc oxide nanocrystalline modified cotton fiber fabric;
(4) completely soaking the zinc oxide nanocrystalline modified cotton fiber fabric prepared in the step (3) in a mixed solution of zinc nitrate and hexamethylenetetramine, vibrating at a constant temperature, taking out, and leaching to obtain a zinc oxide nanorod array modified moisture-conductive cotton fiber fabric;
(5) and (4) coating the silk protein solution containing nano-cellulose on the other surface of the zinc oxide nanorod array modified moisture-conductive cotton fiber fabric prepared in the step (4), and drying at room temperature to obtain the zinc oxide nanorod array modified moisture-conductive cotton fiber fabric.
2. The zinc oxide nanorod array modified moisture-wicking cotton fabric as claimed in claim 1, wherein: in the step (2), the mass ratio of the zinc acetate to the sodium hydroxide is 2: 0.8-1.2.
3. The zinc oxide nanorod array modified moisture-wicking cotton fabric as claimed in claim 1, wherein: in the step (2), the dropping rate is 0.5-1mL/min, the heating reaction temperature is 60-65 ℃, and the heating reaction is continued for 15-30min after the dropping is finished.
4. The zinc oxide nanorod array modified moisture-wicking cotton fabric as claimed in claim 1, wherein: in the step (3), the thickness of the zinc oxide nanocrystals in the cotton fiber or fabric modified by the zinc oxide nanocrystals is 0.1-0.2 μm.
5. The zinc oxide nanorod array modified moisture-wicking cotton fabric as claimed in claim 1, wherein: in the step (4), the molar ratio of zinc nitrate to hexamethylenetetramine in the mixed solution of zinc nitrate and hexamethylenetetramine is 1:1, and the content of zinc nitrate is 0.03-0.05 mol/L.
6. The zinc oxide nanorod array modified moisture-wicking cotton fabric as claimed in claim 1, wherein: in the step (4), the constant-temperature shaking temperature is 70-90 ℃ and the time is 1-2 h.
7. The zinc oxide nanorod array modified moisture-wicking cotton fabric as claimed in claim 1, wherein: in the step (4), the diameter of the zinc oxide nanorod array in the zinc oxide nanorod array modified moisture-conductive cotton fiber or the fabric thereof is 200-400nm, the length is 1-3 μm, and the density is 320-480 pieces/cm2。
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