CN108442099B - Anti-ultraviolet nano zinc oxide composite textile fabric and preparation method thereof - Google Patents
Anti-ultraviolet nano zinc oxide composite textile fabric and preparation method thereof Download PDFInfo
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- 239000004744 fabric Substances 0.000 title claims abstract description 162
- 239000004753 textile Substances 0.000 title claims abstract description 127
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 67
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title description 2
- 239000012530 fluid Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 22
- 230000009467 reduction Effects 0.000 claims abstract description 9
- 230000008595 infiltration Effects 0.000 claims abstract description 4
- 238000001764 infiltration Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000000835 fiber Substances 0.000 claims description 27
- 239000007789 gas Substances 0.000 claims description 23
- 150000003751 zinc Chemical class 0.000 claims description 21
- 229920000728 polyester Polymers 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000009832 plasma treatment Methods 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000006184 cosolvent Substances 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 7
- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical group [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 claims description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- -1 polypropylene Polymers 0.000 claims description 4
- 229920002994 synthetic fiber Polymers 0.000 claims description 4
- 239000012209 synthetic fiber Substances 0.000 claims description 4
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004677 Nylon Substances 0.000 claims 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims 1
- 229920001778 nylon Polymers 0.000 claims 1
- 230000006750 UV protection Effects 0.000 abstract description 10
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 3
- 230000003115 biocidal effect Effects 0.000 abstract description 2
- 230000003068 static effect Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 230000004224 protection Effects 0.000 abstract 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 20
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 4
- 229920004933 Terylene® Polymers 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 229920002972 Acrylic fiber Polymers 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 2
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 2
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 2
- 229920006052 Chinlon® Polymers 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 2
- 235000009120 camo Nutrition 0.000 description 2
- 235000005607 chanvre indien Nutrition 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011487 hemp Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 210000002268 wool Anatomy 0.000 description 2
- 239000004246 zinc acetate Substances 0.000 description 2
- 239000011667 zinc carbonate Substances 0.000 description 2
- 229910000010 zinc carbonate Inorganic materials 0.000 description 2
- 235000004416 zinc carbonate Nutrition 0.000 description 2
- 229920001944 Plastisol Polymers 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000004999 plastisol Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000004808 supercritical fluid chromatography Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
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
- D06M11/32—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
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
- D06M10/025—Corona discharge or low temperature plasma
-
- 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
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
-
- 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
- D06M11/76—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 oxides or carbonates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
-
- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides an anti-ultraviolet nano zinc oxide composite textile fabric and a preparation method thereof2And the textile fabric is prepared by adopting a preparation method combining a supercritical fluid assisted infiltration method and a thermal reduction method, the prepared anti-ultraviolet nano zinc oxide composite textile fabric has the characteristics of environmental protection, good uniformity, high bonding fastness, good repeatability and the like, and the obtained anti-ultraviolet nano zinc oxide composite textile fabric has the functions of ultraviolet resistance, antibiosis, disinfection, hydrophobicity, static resistance and the like.
Description
Technical Field
The invention belongs to the field of multifunctional textile fabrics, and particularly relates to an anti-ultraviolet nano zinc oxide composite textile fabric and a preparation method thereof.
Background
The nano zinc oxide composite textile fabric is characterized in that nano zinc oxide is plated or wrapped inside fibers through physical and chemical means, and nano zinc oxide particles have surface effect, high catalytic efficiency, macroscopic quantum tunneling effect and small size effect which are unique to nano materials, so that the nano zinc oxide composite textile fabric has special performance which is not possessed by common zinc oxide in the aspects of magnetism, electricity, light, heat and the like, and simultaneously, the nano zinc oxide shows excellent physical and chemical properties in the aspects of ultraviolet shielding, magnetic materials and antibacterial disinfection, and has wide development prospect.
The traditional preparation method of the nano-zinc oxide composite textile fabric comprises an impregnation method, a coating method, a magnetron sputtering method, a spinning solution adding method and the like, wherein the impregnation method and the coating method have the problems of poor and uneven bonding fastness of the composite fabric, and the service life of the composite fabric is greatly reduced. The magnetron sputtering method has relatively high cost and is not easy to popularize and industrially produce in a large range. The spinning solution adding method has the problems that the adding of the nano zinc oxide material increases the difficulty of spinning and the forming of fibers. However, the supercritical fluid method can solve these problems.
At present, most of research focuses on supercritical fluid dyeing and conventional chemical preparation of nano zinc oxide composite textile fabric, and no report of preparing nano zinc oxide composite textile fabric by adopting a supercritical fluid technology is available.
Disclosure of Invention
The invention aims to solve the technical problem of providing an anti-ultraviolet nano zinc oxide composite textile fabric and a preparation method thereof.
In order to solve the technical problems, the embodiment of the invention provides an anti-ultraviolet nano zinc oxide composite textile fabric, which comprises the following preparation raw materials: zinc salt, ethanol, CO2The zinc salt, the cosolvent and the textile fabric comprise the following components in percentage by weight:
0.5-40 parts of zinc salt;
0.5-80 parts of a cosolvent;
and 20-99 parts of a textile fabric.
Wherein the textile fabric is one or a mixture of natural fibers and synthetic fibers.
Preferably, the textile fabric is one or a mixture of cotton, wool, silk, hemp, terylene, chinlon, acrylic fiber and polypropylene fiber.
Wherein the zinc salt is one of zinc acetylacetonate, zinc carbonate and zinc acetate.
Wherein the cosolvent is one of methanol, ethanol, n-butanol, isobutanol, acetone, ethylene glycol and triethylene glycol.
The invention also provides a preparation method of the uvioresistant nano-zinc oxide composite textile fabric, which adopts a preparation method combining a supercritical fluid assisted infiltration method and a thermal reduction method and comprises the following steps:
(1) ultrasonically cleaning 20-99 parts of textile fabric in 0.5-80 parts of ethanol and acetone solution for 10-20 min;
(2) cleaning the textile fabric cleaned by the ultrasonic wave in the step (1) by using deionized water, and drying the textile fabric in an oven at 50-70 ℃ for later use;
(3) dissolving 0.5-40 parts of zinc salt in 0.5-80 parts of cosolvent, adding into supercritical fluid equipment, putting the textile fabric dried in the step (2) into the supercritical fluid equipment, and introducing CO into the supercritical fluid equipment2Gas, zinc salt with supercritical CO2Entering the fiber of the textile fabric, finishing the supercritical state after the supercritical permeation reaction for 1-12 h under the conditions of the supercritical treatment pressure of 8-40 MPa and the temperature of 32-100 ℃, and discharging CO2Taking out the textile fabric by gas, and solidifying the zinc salt in the fiber of the textile fabric;
(4) putting the textile fabric permeated by the supercritical fluid in the step (3) into a hydrothermal reaction kettle, and carrying out thermal reduction for 1-12 h at the temperature of 100-200 ℃;
(5) and taking out the textile fabric from the hydrothermal reaction kettle, washing with water, and drying to obtain the anti-ultraviolet nano zinc oxide composite textile fabric. The invention adopts the theoretical basis of preparing the uvioresistant nano zinc oxide composite textile fabric by the supercritical carbon dioxide method as follows: the supercritical fluid has the characteristics of good diffusivity, strong permeability, low surface tension and the like, and is widely applied to modification and treatment of textiles in recent years. The supercritical carbon dioxide has plasticizing expansion and extremely strong diffusion performance, assists the nanoparticles to enter the inside and the surface of the fiber for carrying, so that the nanoparticles are uniformly carried in the inside and the surface of the fiber, and CO2 is rapidly gasified after the reaction is finished, thereby being environment-friendly, pollution-free and rapid in reaction. And the carbon dioxide has the characteristics of no toxicity, no odor, no combustion, safe treatment process, lower cost, wide applicable auxiliary agent range and the like.
The preparation method of the uvioresistant nano zinc oxide composite textile fabric further comprises the step of alkali decrement treatment of the textile fabric before the step (1), and the preparation method specifically comprises the following steps: preparing a sodium hydroxide solution with the mass concentration of 3-20%, soaking the textile fabric in the sodium hydroxide solution, heating in a water bath at the solid-liquid ratio of 1:30 at the temperature of 60-80 ℃ for 5-20 minutes, washing with deionized water, and drying in an oven at the temperature of 60 ℃.
The preparation method of the uvioresistant nano zinc oxide composite textile fabric can also comprise a textile fabric plasma treatment step before the step (1), and the preparation method specifically comprises the following steps: starting a plasma instrument, connecting argon, firstly washing gas for two minutes to remove air, putting the textile fabric into the plasma instrument, adjusting the gas flow to be 1L/min, adjusting the output power of the plasma instrument to be 800-1200W, carrying out plasma treatment for 2-6 minutes at normal pressure, taking out the textile fabric, and closing the plasma instrument.
The reason for performing alkali deweighting treatment or plasma treatment on the textile fabric before the supercritical fluid treatment is mainly as follows: the surface of the fiber is uneven through the etching effect of the plasma and alkali decrement treatment on the surface of the textile fabric, and the specific surface area of the fiber is increased, so that the adsorbability of the fiber is improved, and the permeability of the supercritical fluid is improved. The large number of tiny pits and cracks on the surface of the treated fiber enable incident light to be reflected and absorbed for multiple times on the surface of the prepared nano zinc oxide ultraviolet-proof fabric, and the ultraviolet-proof effect is improved.
The preparation method of the uvioresistant nano zinc oxide composite textile fabric further comprises the step of plasma treatment of the textile fabric after the step (3), and the preparation method specifically comprises the following operations: starting a plasma instrument, connecting argon, firstly washing gas for two minutes to remove air, putting the textile fabric into the plasma instrument, adjusting the gas flow to be 1L/min, adjusting the output power of the plasma instrument to be 1000W, carrying out plasma treatment for 1-2 minutes at normal pressure, taking out the textile fabric, and closing the instrument.
the plasma bombardment of the plasma on the fiber activates the surface of the fiber, so that β -diketone structure of zinc acetylacetonate and a fabric macromolecular chain are opened, the temperature required by post-treatment thermal reduction is reduced, the thermal reduction is more sufficient, the crystal form of the generated zinc oxide is more uniform, and the combination of the zinc oxide and the surface of the fiber is firmer and more compact.
The technical scheme of the invention has the following beneficial effects: the ultraviolet-resistant nano zinc oxide composite textile fabric prepared by the supercritical carbon dioxide method has the functions of ultraviolet resistance, antibiosis, disinfection, hydrophobicity, static resistance and the like, and is good in binding fastness, washable, good in uniformity, green, environment-friendly, energy-saving and anhydrous.
Drawings
Fig. 1 is an electron microscope photograph of the ultraviolet-resistant nano zinc oxide composite textile fabric prepared in the first embodiment of the invention;
FIG. 2 is an electron microscope photograph of the uvioresistant nano-zinc oxide composite textile fabric prepared in the second embodiment of the invention;
FIG. 3 is an electron microscope scanning photograph of a polyester fabric according to a second embodiment of the present invention;
fig. 4 is an electron microscope scanning photograph of the anti-ultraviolet nano zinc oxide composite textile fabric prepared in the second embodiment of the invention;
FIG. 5 is a photograph showing the contact angle of the polyester fabric according to the second embodiment of the present invention;
fig. 6 is a contact angle photograph of the ultraviolet resistant nano zinc oxide composite textile fabric prepared in the second embodiment of the present invention;
fig. 7 is a graph comparing ultraviolet resistance of the textile fabric in the invention, and the nano zinc oxide composite fabrics prepared in examples 1 and 3.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
The invention provides an anti-ultraviolet nano zinc oxide composite textile fabric which is prepared from the following raw materials in parts by weight: zinc salt, ethanol, CO2The zinc salt, the cosolvent and the textile fabric comprise the following components in percentage by weight:
0.5-40% of zinc salt;
0.5-80% of a cosolvent;
and 20-99% of a textile fabric.
Wherein the textile fabric is one or a mixture of natural fibers and synthetic fibers.
Preferably, the textile fabric is one or a mixture of cotton, wool, silk, hemp, terylene, chinlon, acrylic fiber and polypropylene fiber.
Wherein the zinc salt is one of zinc acetylacetonate, zinc carbonate and zinc acetate.
Wherein the cosolvent is one of methanol, ethanol, n-butanol, isobutanol, acetone, ethylene glycol and triethylene glycol.
The invention also provides a preparation method of the uvioresistant nano-zinc oxide composite textile fabric, which adopts a preparation method combining a supercritical fluid assisted infiltration method and a thermal reduction method and comprises the following steps:
(1) ultrasonically cleaning 20-99 parts of textile fabric in 0.5-80 parts of ethanol and acetone solution for 10-20 min;
(2) cleaning the textile fabric cleaned by the ultrasonic wave in the step (1) by using deionized water, and drying the textile fabric in an oven at 50-70 ℃ for later use;
(3) dissolving 0.5-40 parts of zinc salt in 0.5-80 parts of cosolvent, adding into supercritical fluid equipment, putting the textile fabric dried in the step (2) into the supercritical fluid equipment, and introducing into the supercritical fluid equipmentCO2Gas, supercritical CO2Has the functions of plasticizing, expanding and strong permeating on textile fabrics, and the zinc salt is along with supercritical CO2Entering the fiber of the textile fabric, finishing the supercritical state after the supercritical permeation reaction for 1-12 h under the conditions of the supercritical treatment pressure of 8-40 MPa and the temperature of 32-100 ℃, and discharging CO2Taking out the textile fabric by gas, and solidifying the zinc salt in the fiber of the textile fabric;
(4) putting the textile fabric permeated by the supercritical fluid in the step (3) into a hydrothermal reaction kettle, and carrying out thermal reduction for 1-12 h at the temperature of 100-200 ℃;
(5) and taking out the textile fabric from the hydrothermal reaction kettle, washing with water, and drying to obtain the anti-ultraviolet nano zinc oxide composite textile fabric.
The preparation method of the uvioresistant nano zinc oxide composite textile fabric further comprises the step of alkali decrement treatment of the textile fabric before the step (1), and the preparation method specifically comprises the following steps: preparing a sodium hydroxide solution with the mass concentration of 3-20%, soaking the textile fabric in the sodium hydroxide solution, heating in a water bath at the solid-liquid ratio of 1:30 at the temperature of 60-80 ℃ for 5-20 minutes, washing with deionized water, and drying in an oven at the temperature of 60 ℃.
The preparation method of the uvioresistant nano zinc oxide composite textile fabric can also comprise a textile fabric plasma treatment step before the step (1), and the preparation method specifically comprises the following steps: starting a plasma instrument, connecting argon, firstly washing gas for two minutes to remove air, putting the textile fabric into the plasma instrument, adjusting the gas flow to be 1L/min, adjusting the output power of the plasma instrument to be 800-1200W, carrying out plasma treatment for 2-6 minutes at normal pressure, taking out the textile fabric, and closing the plasma instrument.
The preparation method of the uvioresistant nano zinc oxide composite textile fabric further comprises the step of plasma treatment of the textile fabric after the step (3), and the preparation method specifically comprises the following operations: starting a plasma instrument, connecting argon, firstly washing gas for two minutes to remove air, putting the textile fabric into the plasma instrument, adjusting the gas flow to be 1L/min, adjusting the output power of the plasma instrument to be 1000W, carrying out plasma treatment for 1-2 minutes at normal pressure, taking out the textile fabric, and closing the instrument.
The present invention is described in detail below with reference to examples, which are intended to be illustrative only and are not to be construed as limiting the scope of the invention, and many insubstantial modifications and adaptations of the invention may be made by those skilled in the art.
Example 1
Respectively ultrasonically cleaning a 10cm × 10cm polyester fabric for 15min by using acetone and ethanol solution, then cleaning the fabric by using deionized water, and drying the fabric in an oven for later use; then 1.5g of zinc acetylacetonate is dissolved in 25ml of ethanol and added into supercritical fluid equipment; placing the polyester fabric subjected to ultrasonic cleaning into supercritical fluid equipment, and introducing CO into the supercritical fluid equipment2Performing supercritical reaction on the gas for 6 hours under the conditions of 15Mpa of pressure and 80 ℃, and taking out the polyester fabric; and then placing the polyester fabric subjected to supercritical reaction into a hydrothermal reaction kettle, heating for 4 hours at 180 ℃, taking out the polyester fabric, washing with water, and drying to obtain the uvioresistant nano zinc oxide composite textile fabric.
The scanning electron microscope shows that the obtained electron microscope photo of the uvioresistant nano-zinc oxide composite textile fabric is shown in figure 1, and nano-zinc oxide substances are loaded on the fiber surface.
Example 2
Respectively ultrasonically cleaning a 10cm × 10cm polyester fabric for 15min by using acetone and ethanol solution, then cleaning the fabric by using deionized water, and drying the fabric in an oven for later use; then 1g of zinc acetylacetonate is dissolved in 25ml of ethanol and added into supercritical fluid equipment; placing the polyester fabric subjected to ultrasonic cleaning into supercritical fluid equipment, and introducing CO into the supercritical fluid equipment2Performing supercritical reaction on the gas for 4 hours under the conditions of 10Mpa of pressure and 60 ℃, and taking out the polyester fabric; and then placing the polyester fabric subjected to the supercritical reaction into a hydrothermal reaction kettle, heating for 3 hours at 120 ℃, finally taking out the polyester fabric, washing with water, and drying to obtain the uvioresistant nano zinc oxide composite textile fabric.
The scanning electron microscope shows that the obtained electron microscope photo of the uvioresistant nano-zinc oxide composite textile fabric is shown in fig. 2, and nano-zinc oxide substances are loaded on the fiber surface.
The microstructure and the macroscopic properties of the ultraviolet-resistant nano zinc oxide composite textile fabric obtained in the embodiment are as follows:
1. appearance of uvioresistant nano zinc oxide composite textile fabric
Fig. 3 is an electron microscope (SEM) scanning photograph of the textile fabric in the present embodiment as it is, and fig. 4 is an electron microscope (SEM) scanning photograph of the uv-resistant nano zinc oxide composite textile fabric prepared in the present embodiment, which can be found by comparing: supercritical CO2The nano zinc oxide particle-loaded anti-ultraviolet fabric has the effects of plasticizing, expanding and strong permeability on textile fabrics, and has the anti-ultraviolet effect because the nano zinc oxide particles are loaded on the surface and the inside of the original smooth textile fabrics.
2. The ultraviolet resistance of the ultraviolet resistant nano zinc oxide composite textile fabric prepared by the supercritical fluid is shown in table 1
TABLE 1 original textile fabric, padding method and supercritical CO2Ultraviolet resistance comparison table of ultraviolet resistance nano zinc oxide composite textile fabric prepared by method
And (4) conclusion: by padding treatment and supercritical CO2The ultraviolet resistance of the treated textile fabric is improved to different degrees, but the supercritical CO2The ultraviolet resistance of the treated textile fabric is superior to that of the traditional treatment method, and the treatment effect is obviously improved because of the following reasons: supercritical CO2The metal precursor (i.e., zinc salt) is accompanied by CO during the treatment2The ultraviolet-proof fiber can penetrate into the fiber, and the ultraviolet-proof effect, the durability and the washing fastness are obviously improved.
The metal precursor is referred to as a zinc salt in the present invention, and since the zinc salt is reduced later, it is sometimes referred to as a metal precursor in the art and may be written as a zinc salt.
3. Contact angle of uvioresistant nano zinc oxide composite textile fabric with different reaction times
FIG. 5 shows the terylene in this exampleContact angle photo of the fabric, and fig. 6 is a contact angle photo of the anti-ultraviolet nano zinc oxide composite textile fabric prepared in this example. The contact angle of the original shape of the polyester fabric is 91.5 degrees after the test, and the contact angle is subjected to supercritical CO2The contact angle of the uvioresistant nano zinc oxide composite textile fabric prepared by the technology reaches 145.5 degrees, and compared with the contact angle, the contact angle is obviously improved because of the CO in the supercritical fluid treatment process2Pressure increase, supercritical CO2The plastisol effect and the diffusion effect are obviously improved, and the nano zinc oxide is favorably diffused into the internal gaps of the fibers to block the fiber gaps and reduce the permeation of water molecules, so that the contact angle is improved, and therefore, the supercritical CO is obtained2Has positive effect on the compounding of the nano zinc oxide and the textile fabric.
Example 3
Respectively ultrasonically cleaning a 10cm × 10cm polyester fabric for 15min by using acetone and ethanol solution, then cleaning the fabric by using deionized water, and drying the fabric in an oven for later use; then 1.5g of zinc acetylacetonate is dissolved in 25ml of ethanol and added into supercritical fluid equipment; placing the polyester fabric subjected to ultrasonic cleaning into supercritical fluid equipment, and introducing CO into the supercritical fluid equipment2Performing supercritical reaction on the gas for 6 hours under the conditions of 15Mpa of pressure and 80 ℃, and taking out the polyester fabric; putting the fabric into a plasma treatment instrument, starting the plasma instrument, connecting argon, firstly washing gas for 2min to remove air, adjusting the gas flow to be 1L/min, adjusting the output power of the plasma instrument to be 1000W, carrying out plasma treatment for 2min at normal pressure, taking out the fabric, and closing the instrument. And then placing the polyester fabric subjected to supercritical reaction into a hydrothermal reaction kettle, heating for 4 hours at 180 ℃, taking out the polyester fabric, washing with water, and drying to obtain the nano-zinc oxide composite textile fabric.
A comparison graph of the ultraviolet resistance of the textile fabric as it is and the nano zinc oxide composite fabrics prepared in examples 1 and 3 is shown in fig. 7, and it can be known from fig. 7 that: example 1 by supercritical CO2The ultraviolet resistance of the nano zinc oxide composite fabric prepared by the permeation assistance is obviously improved compared with the original textile fabric, and the middle lane is added in the example 3Compared with the example 1, the ultraviolet resistance of the nano zinc oxide composite fabric prepared by the plasma treatment is improved to a certain extent.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (5)
1. A preparation method of an uvioresistant nano-zinc oxide composite textile fabric is characterized in that a preparation method combining a supercritical fluid assisted infiltration method and a thermal reduction method is adopted, and comprises the following steps:
(1) the alkali deweighting treatment step of the textile fabric comprises the following specific operations: the textile fabric is one or two of synthetic fibers, a sodium hydroxide solution with the mass concentration of 3-20% is prepared, the textile fabric is immersed in the sodium hydroxide solution, the solid-liquid ratio is 1:30, the textile fabric is heated in a water bath at 60-80 ℃ for 5-20 minutes, then is washed clean by deionized water, and is dried in an oven at 60 ℃;
(1) ultrasonically cleaning 20-99 g of textile fabric in 0.5-80 g of ethanol and acetone solution for 10-20 min;
(2) cleaning the textile fabric cleaned by the ultrasonic wave in the step (1) by using deionized water, and drying the textile fabric in an oven at 50-70 ℃ for later use;
(3) dissolving 0.5-40 g of zinc salt in 0.5-80 g of cosolvent, adding the obtained solution into supercritical fluid equipment, putting the textile fabric dried in the step (2) into the supercritical fluid equipment, and introducing CO into the supercritical fluid equipment2Gas, zinc salt with supercritical CO2Entering the fiber of the textile fabric, finishing the supercritical state after the supercritical permeation reaction for 1-12 h under the conditions of the supercritical treatment pressure of 8-40 MPa and the temperature of 32-100 ℃, and discharging CO2Taking out the textile fabric by gas, and solidifying the zinc salt in the fiber of the textile fabric;
(3) the plasma treatment step of the textile fabric comprises the following specific operations: starting a plasma instrument, connecting argon, firstly washing gas for two minutes to remove air, putting the textile fabric into the plasma instrument, adjusting the gas flow to be 1L/min, adjusting the output power of the plasma instrument to be 1000W, carrying out normal-pressure plasma treatment for 1-2 minutes, taking out the textile fabric, and closing the instrument;
(4) putting the textile fabric treated in the step (3)' into a hydrothermal reaction kettle, and carrying out thermal reduction for 1-12 h at the temperature of 100-200 ℃;
(5) and taking out the textile fabric from the hydrothermal reaction kettle, washing with water, and drying to obtain the anti-ultraviolet nano zinc oxide composite textile fabric.
2. The preparation method of the ultraviolet-resistant nano zinc oxide composite textile fabric according to claim 1, further comprising a textile fabric plasma treatment step before the step (1), and the preparation method specifically comprises the following steps: starting a plasma instrument, connecting argon, firstly washing gas for two minutes to remove air, putting the textile fabric into the plasma instrument, adjusting the gas flow to be 1L/min, adjusting the output power of the plasma instrument to be 800-1200W, carrying out plasma treatment for 2-6 minutes at normal pressure, taking out the textile fabric, and closing the plasma instrument.
3. The method for preparing the uvioresistant nano-zinc oxide composite textile fabric according to claim 1, wherein the textile synthetic fiber fabric is one or a mixture of polyester, nylon, acrylic and polypropylene.
4. The preparation method of the ultraviolet-resistant nano zinc oxide composite textile fabric according to claim 1, wherein the zinc salt is zinc acetylacetonate.
5. The preparation method of the uvioresistant nano-zinc oxide composite textile fabric according to claim 1, wherein the cosolvent is one of methanol, ethanol, n-butanol, isobutanol, acetone, ethylene glycol and triethylene glycol.
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| CN111172747A (en) * | 2019-12-30 | 2020-05-19 | 比音勒芬服饰股份有限公司 | Anti-ultraviolet fabric and preparation method and application thereof |
| CN111349974A (en) * | 2020-03-12 | 2020-06-30 | 重庆大学 | Preparation method of nanofiber hydrogen sensing material subjected to plasma treatment |
| CN112575474A (en) * | 2020-12-02 | 2021-03-30 | 安徽农业大学 | Method for manufacturing polyester fiber textile garment fabric and processing equipment thereof |
| CN113463224A (en) * | 2021-07-02 | 2021-10-01 | 和也健康科技有限公司 | Preparation method of nano antibacterial stone needle fiber material for cosmetic cotton |
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