CN108442099A - A kind of anti-ultraviolet nano zinc oxide composite textile and preparation method thereof - Google Patents
A kind of anti-ultraviolet nano zinc oxide composite textile and preparation method thereof Download PDFInfo
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- CN108442099A CN108442099A CN201810262666.2A CN201810262666A CN108442099A CN 108442099 A CN108442099 A CN 108442099A CN 201810262666 A CN201810262666 A CN 201810262666A CN 108442099 A CN108442099 A CN 108442099A
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- textile fabric
- zinc oxide
- oxide composite
- textile
- nano zinc
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- 239000004753 textile Substances 0.000 title claims abstract description 121
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000004744 fabric Substances 0.000 claims abstract description 96
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000012530 fluid Substances 0.000 claims abstract description 33
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 26
- 150000003751 zinc Chemical class 0.000 claims abstract description 24
- 235000019441 ethanol Nutrition 0.000 claims abstract description 16
- 230000009467 reduction Effects 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 32
- 239000000835 fiber Substances 0.000 claims description 28
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000006184 cosolvent Substances 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- -1 polypropylene Polymers 0.000 claims description 9
- 238000009987 spinning Methods 0.000 claims description 9
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 238000009832 plasma treatment Methods 0.000 claims description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 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
- 229920004933 Terylene® Polymers 0.000 claims description 4
- 229920002972 Acrylic fiber Polymers 0.000 claims description 3
- 229920000742 Cotton Polymers 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- 239000006260 foam Substances 0.000 claims description 3
- 239000008236 heating water Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920002994 synthetic fiber Polymers 0.000 claims description 3
- 239000012209 synthetic fiber Substances 0.000 claims description 3
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- 239000011667 zinc carbonate Substances 0.000 claims description 3
- 229910000010 zinc carbonate Inorganic materials 0.000 claims description 3
- 235000004416 zinc carbonate Nutrition 0.000 claims description 3
- 238000009941 weaving Methods 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 230000006750 UV protection Effects 0.000 abstract description 9
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 239000002243 precursor Substances 0.000 abstract description 4
- 230000003115 biocidal effect Effects 0.000 abstract description 3
- 230000002209 hydrophobic effect Effects 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract description 3
- 230000001954 sterilising effect Effects 0.000 abstract description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 23
- 238000000034 method Methods 0.000 description 20
- 229920000728 polyester Polymers 0.000 description 14
- 230000000694 effects Effects 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 6
- 229910052725 zinc Inorganic materials 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- 239000001569 carbon dioxide Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229920004934 Dacron® Polymers 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000003851 corona treatment Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000001802 infusion Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 230000004224 protection Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 239000004999 plastisol Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
Landscapes
- 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
A kind of anti-ultraviolet nano zinc oxide composite textile of present invention offer and preparation method thereof, the raw material for preparing of the anti-ultraviolet nano zinc oxide composite textile includes using zinc salt as metal precursor, ethyl alcohol, acetone, CO2And textile fabric, the preparation method that osmosis and thermal reduction are combined is assisted using supercritical fluid, anti-ultraviolet nano zinc oxide composite textile obtained is with environmentally protective, uniformity is good, binding strength is high, the features such as reproducible, and obtained anti-ultraviolet nano zinc oxide composite textile has the function of UV resistance, antibiotic and sterilizing, hydrophobic, antistatic etc..
Description
Technical field
The invention belongs to multifunctional textile lining field, and in particular to a kind of anti-ultraviolet nano zinc oxide composite spinning
Fabric and preparation method thereof.
Background technology
Nano zine oxide composite textile refers to by nano zine oxide plating or being wrapped in by means such as physics, chemistry
Fibrous inside, since nano zinc oxide particles have, the exclusive skin effect of nano material, catalytic efficiency be strong, macroscopic quantum tunnel
Channel effect and small-size effect, therefore have the property not available for common zinc oxide in magnetic, electrical, optical, heat etc., together
When nano zine oxide excellent physics, chemical property are all presented in terms of ultraviolet shielded, magnetic material, antibiotic and sterilizing, have
Vast potential for future development.
The preparation method of traditional nano zine oxide composite textile include infusion process, cladding process, magnetron sputtering method and
Spinning solution additive process etc., wherein infusion process and cladding process there are the binding strength of compound fabric is poor, it is uneven the problems such as, it is compound
Fabric service life substantially reduces.The cost is relatively high for magnetron sputtering method, is not easy to popularization and a wide range of industrial production.And it spins
Silk stock solution additive process has problems in that the addition of nano zinc oxide material increases the difficulty of spinning and the forming of fiber.But
It is supercritical fluid rule to solve these problems.
Currently, most of research concentrates on the conventional chemical of supercritical fluid dyeing, nano zine oxide composite textile
In preparation, the report that nano zine oxide composite textile is prepared using supercritical fluid technique there is no.
Invention content
The technical problem to be solved in the present invention is to provide a kind of anti-ultraviolet nano zinc oxide composite textile and its preparations
Method prepares anti-ultraviolet nano zinc oxide composite textile using supercritical carbon dioxide process, and there is UV resistance, antibacterial to disappear
The functions such as malicious, hydrophobic, antistatic, binding strength is good, water-fastness, uniformity is good, environmentally protective, energy saving anhydrous.
In order to solve the above technical problems, the embodiment of the present invention provides a kind of anti-ultraviolet nano zinc oxide Compound spinning surface of second order
Material, preparing raw material includes：Zinc salt, ethyl alcohol, CO2, cosolvent, acetone and textile fabric, wherein zinc salt, cosolvent and weaving
Fabric is by weight percentage：
0.5 ~ 40 part of zinc salt；
0.5 ~ 80 part of cosolvent；
20 ~ 99 parts of textile fabric.
Wherein, the textile fabric mixes for one or both of natural fiber and synthetic fibers.
Preferably, the textile fabric is one or more mixed in cotton, hair, silk, fiber crops, terylene, polyamide fibre, acrylic fibers and polypropylene fibre
It closes.
Wherein, the zinc salt is one kind in zinc acetylacetonate, zinc carbonate, zinc acetate.
Wherein, the cosolvent is one in methanol, ethyl alcohol, n-butanol, isobutanol, acetone, ethylene glycol, triethylene glycol
Kind.
The present invention also provides a kind of preparation methods of anti-ultraviolet nano zinc oxide composite textile, using supercritical fluid
The preparation method for assisting osmosis and thermal reduction to be combined, includes the following steps：
（1）By 20 ~ 99 parts of textile fabric, 10 ~ 20min of ultrasonic cleaning in 0.5 ~ 80 part of ethyl alcohol and acetone soln；
（2）By step（1）Textile fabric after middle ultrasonic cleaning is cleaned up with deionized water, and 50 ~ 70 DEG C of drying of baking oven are standby
With；
（3）0.5 ~ 40 part of zinc salt is dissolved in 0.5 ~ 80 part of cosolvent, is then added in Supercritical fluid device, it will
Step（2）The textile fabric of middle drying is put into Supercritical fluid device, and CO is passed through into Supercritical fluid device2Gas, zinc
Salt is with supercritical CO2Into the fibrous inside of textile fabric, in 32 ~ 100 DEG C of 8 ~ 40MPa of first supercritical processing pressure, temperature conditions
Under terminate supercriticality after overcritical 1 ~ 12h of permeable reactive, CO is discharged2Gas, takes out textile fabric, and zinc salt is cured in spinning
The fibrous inside of knitted fabric；
（4）By step（3）It is middle permeated using supercritical fluid after textile fabric be put into hydrothermal reaction kettle, 100 ~ 200 DEG C of items
1 ~ 12h is heat-treated under part；
（5）Textile fabric is taken out from hydrothermal reaction kettle, through washing, being drying to obtain anti-ultraviolet nano zinc oxide Compound spinning surface of second order
Material.The present invention use supercritical carbon dioxide process prepare the theoretical foundation of anti-ultraviolet nano zinc oxide composite textile for：It is super
Critical fluids have the characteristics that good diffusivity, strong permeance property, surface tension is low is widely used in changing for textile in recent years
Property and processing in.Supercritical carbon dioxide has plasticising expansion and extremely strong diffusion, and nano particle is assisted to enter in fiber
Portion and surface appendix make the uniform appendix of nano particle on fibrous inside and surface, and CO2 gasifies rapidly after reaction, environmental protection
It is pollution-free, it is swift in response.And carbon dioxide itself have it is nontoxic, tasteless, non-ignitable, processing procedure safety, cost is relatively low, can answer
The features such as used additives range is wide.
The preparation method of above-mentioned anti-ultraviolet nano zinc oxide composite textile further includes step（1）Woven face before
Expect that alkali decrement treatment step, concrete operations are：The sodium hydroxide solution for preparing 3%-20% mass concentrations, soaks foam by textile fabric
In sodium hydroxide solution, solid-to-liquid ratio 1:30,60-80 DEG C of heating water baths dry after being rinsed well with deionized water after 5-20 minutes
60 DEG C of drying of case.
The preparation method of above-mentioned anti-ultraviolet nano zinc oxide composite textile can also include step（1）Before
Textile fabric plasma treatment step, concrete operations are：Plasma instrument is opened, argon gas is connected, first gas washing removes for two minutes
Textile fabric is put into plasma instrument by air, and adjusting gas flow 1L/min adjusts plasma instrument output power
For 800-1200W, atmospheric pressure plasma jet treatment 2-6 minutes takes out textile fabric, closes plasma instrument.
It is mainly to the reason of textile fabric progress alkali decrement treatment or plasma treatment before treatment with supercritical fluid：
Keep fiber surface uneven the corrasion on textile fabric surface by plasma and alkali decrement treatment, increases fiber
Specific surface area improve the permeability of supercritical fluid to improve the adsorptivity of fiber.Through processing fiber surface these
A large amount of unevenness and crackle make incident light that multiple reflections and suction occur on nano zine oxide anti-ultraviolet fabric obtained surface
It receives, improves the effect of UV resistance.
The preparation method of above-mentioned anti-ultraviolet nano zinc oxide composite textile further includes step（3）Woven face later
Expect that plasma treatment step, concrete operations are：Plasma instrument is opened, connects argon gas, two minutes removal air of first gas washing will
Textile fabric is put into plasma instrument, and adjusting gas flow 1L/min, adjusting plasma instrument output power is
1000W, atmospheric pressure plasma jet treatment 1-2 minutes take out textile fabric, close instrument.
The treatment effect of corona treatment is carried out to textile fabric between treatment with supercritical fluid and thermal reduction processing
It is：Discharge excitation gas forms high-energy particle flow in normal-temperature plasma processing procedure.Due to the effect of these high energy particles,
Fiber surface is hit by ion stream, neutral particle, energy is transferred to fiber, with energy dissipation, causes fiber, high score
Sub- material surface a series of physical, chemical modification, such as etching, dehydrogenation, addition, oxidation reaction.Plasma is for fiber
Bombardment activates fiber surface so that the beta-diketon structure and fabric macromolecular chain of zinc acetylacetonate are opened, and post-processing heat is reduced
Required temperature is restored, thermal reduction is more abundant, and the zinc oxide crystal form of generation is more uniform, and the combination of zinc oxide and fiber surface is more
Add secure rigid.
The above-mentioned technical proposal of the present invention has the beneficial effect that：The present invention is prepared anti-using supercritical carbon dioxide process
Ultraviolet nanometer zinc oxide composite textile, has the function of UV resistance, antibiotic and sterilizing, hydrophobic, antistatic etc., binding strength is good,
It is water-fastness, uniformity is good, environmentally protective, energy saving anhydrous.
Description of the drawings
Fig. 1 is the electromicroscopic photograph of anti-ultraviolet nano zinc oxide composite textile prepared by the embodiment of the present invention one；
Fig. 2 is the electromicroscopic photograph of anti-ultraviolet nano zinc oxide composite textile prepared by the embodiment of the present invention two；
Fig. 3 is the electron microscope scanning photo of dacron in the embodiment of the present invention two；
Fig. 4 is that the electron microscope scanning of the anti-ultraviolet nano zinc oxide composite textile prepared in the embodiment of the present invention two shines
Piece；
Fig. 5 is the contact angle photo of dacron in the embodiment of the present invention two；
Fig. 6 is the contact angle photo of the anti-ultraviolet nano zinc oxide composite textile prepared in the embodiment of the present invention two；
Fig. 7 is the anti-purple for the nano zine oxide composite material that in the present invention prepared by textile fabric original sample, embodiment 1 and embodiment 3
Outer performance comparison figure.
Specific implementation mode
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool
Body embodiment is described in detail.
The present invention provides a kind of anti-ultraviolet nano zinc oxide composite textile, preparing raw material includes：Zinc salt, second
Alcohol, CO2, cosolvent, acetone and textile fabric, wherein zinc salt, cosolvent and textile fabric are by weight percentage：
Zinc salt 0.5 ~ 40%；
Cosolvent 0.5 ~ 80%；
Textile fabric 20 ~ 99%.
Wherein, the textile fabric mixes for one or both of natural fiber and synthetic fibers.
Preferably, the textile fabric is one or more mixed in cotton, hair, silk, fiber crops, terylene, polyamide fibre, acrylic fibers and polypropylene fibre
It closes.
Wherein, the zinc salt is one kind in zinc acetylacetonate, zinc carbonate, zinc acetate.
Wherein, the cosolvent is one in methanol, ethyl alcohol, n-butanol, isobutanol, acetone, ethylene glycol, triethylene glycol
Kind.
The present invention also provides a kind of preparation methods of anti-ultraviolet nano zinc oxide composite textile, using supercritical fluid
The preparation method for assisting osmosis and thermal reduction to be combined, includes the following steps：
（1）By 20 ~ 99 parts of textile fabric, 10 ~ 20min of ultrasonic cleaning in 0.5 ~ 80 part of ethyl alcohol and acetone soln；
（2）By step（1）Textile fabric after middle ultrasonic cleaning is cleaned up with deionized water, and 50 ~ 70 DEG C of drying of baking oven are standby
With；
（3）0.5 ~ 40 part of zinc salt is dissolved in 0.5 ~ 80 part of cosolvent, is then added in Supercritical fluid device, it will
Step（2）The textile fabric of middle drying is put into Supercritical fluid device, and CO is passed through into Supercritical fluid device2Gas surpasses
Critical CO2There is plasticising expansion to textile fabric and permeate by force, zinc salt is with supercritical CO2Into in the fiber of textile fabric
Portion terminates under the conditions of 8 ~ 40MPa of first supercritical processing pressure, 32 ~ 100 DEG C of temperature after overcritical 1 ~ 12h of permeable reactive overcritical
CO is discharged in state2Gas, takes out textile fabric, and zinc salt is cured in the fibrous inside of textile fabric；
（4）By step（3）It is middle permeated using supercritical fluid after textile fabric be put into hydrothermal reaction kettle, 100 ~ 200 DEG C of items
1 ~ 12h is heat-treated under part；
（5）Textile fabric is taken out from hydrothermal reaction kettle, through washing, being drying to obtain anti-ultraviolet nano zinc oxide Compound spinning surface of second order
Material.
The preparation method of above-mentioned anti-ultraviolet nano zinc oxide composite textile further includes step（1）Woven face before
Expect that alkali decrement treatment step, concrete operations are：The sodium hydroxide solution for preparing 3%-20% mass concentrations, soaks foam by textile fabric
In sodium hydroxide solution, solid-to-liquid ratio 1:30,60-80 DEG C of heating water baths dry after being rinsed well with deionized water after 5-20 minutes
60 DEG C of drying of case.
The preparation method of above-mentioned anti-ultraviolet nano zinc oxide composite textile can also include step（1）Before
Textile fabric plasma treatment step, concrete operations are：Plasma instrument is opened, argon gas is connected, first gas washing removes for two minutes
Textile fabric is put into plasma instrument by air, and adjusting gas flow 1L/min adjusts plasma instrument output power
For 800-1200W, atmospheric pressure plasma jet treatment 2-6 minutes takes out textile fabric, closes plasma instrument.
The preparation method of above-mentioned anti-ultraviolet nano zinc oxide composite textile further includes step（3）Woven face later
Expect that plasma treatment step, concrete operations are：Plasma instrument is opened, connects argon gas, two minutes removal air of first gas washing will
Textile fabric is put into plasma instrument, and adjusting gas flow 1L/min, adjusting plasma instrument output power is
1000W, atmospheric pressure plasma jet treatment 1-2 minutes take out textile fabric, close instrument.
With reference to embodiment, the present invention will be described in detail, it is necessary to be pointed out that embodiment is served only for the present invention
Further explanation, be not understood to limiting the scope of the invention, which can be according to this hair
It is bright to make some nonessential improvement and adjustment.
Embodiment 1
The polyester fabric that size is 10cm × 10cm is used into acetone and ethanol solution ultrasonic cleaning 15min respectively, is then spent
Ionized water cleans up, and baking oven is dried for standby；Then 1.5g zinc acetylacetonates are dissolved in the ethyl alcohol of 25ml, are added overcritical
In fluid device；Polyester fabric after ultrasonic cleaning is put into Supercritical fluid device, and into Supercritical fluid device
It is passed through CO2Gas, supercritical reaction 6h under the conditions of pressure 15Mpa, 80 DEG C of temperature, takes out polyester fabric；It again will be overcritical anti-
Polyester fabric after answering is put into hydrothermal reaction kettle, and 4h is heated under the conditions of 180 DEG C, finally takes out polyester fabric through washing, drying
Up to anti-ultraviolet nano zinc oxide composite textile.
It observes under a scanning electron microscope, the electromicroscopic photograph of obtained anti-ultraviolet nano zinc oxide composite textile is such as
Shown in Fig. 1, the nano oxidized zinc material of fiber surface appendix.
Embodiment 2
The polyester fabric that size is 10cm × 10cm is used into acetone and ethanol solution ultrasonic cleaning 15min respectively, is then spent
Ionized water cleans up, and baking oven is dried for standby；Then 1g zinc acetylacetonates are dissolved in the ethyl alcohol of 25ml, shooting flow is added
In body equipment；Polyester fabric after ultrasonic cleaning is put into Supercritical fluid device, and is led into Supercritical fluid device
Enter CO2Gas, supercritical reaction 4h under the conditions of pressure 10Mpa, temperature 60 C take out polyester fabric；Again by supercritical reaction
Polyester fabric afterwards is put into 120 DEG C of heating 3h in hydrothermal reaction kettle, finally takes out polyester fabric through washing, being drying to obtain uvioresistant
Nano zine oxide composite textile.
It observes under a scanning electron microscope, the electromicroscopic photograph of obtained anti-ultraviolet nano zinc oxide composite textile is such as
Shown in Fig. 2, the nano oxidized zinc material of fiber surface appendix.
The microstructure of gained anti-ultraviolet nano zinc oxide composite textile and macro property are as follows in the present embodiment：
1, the pattern of anti-ultraviolet nano zinc oxide composite textile
Fig. 3 is the electron microscope of textile fabric original sample in the present embodiment（SEM）Scanned photograph, Fig. 4 are made from the present embodiment
The electron microscope of anti-ultraviolet nano zinc oxide composite textile（SEM）Scanned photograph is can be found that by comparison：It is overcritical
CO2There is plasticising expansion to textile fabric and by force permeate, originally smooth textile fabric surface and inside appendix nanometer
Zinc oxide particles have the effect of antiultraviolet..
2, the uv resistance of anti-ultraviolet nano zinc oxide composite textile prepared by supercritical fluid can be as shown in table 1
1 textile fabric of table original sample, padding method and supercritical CO2Anti-ultraviolet nano zinc oxide composite textile prepared by method
Uv resistance energy comparison sheet
Conclusion：By padding processing and supercritical CO2The uv resistance of treated textile fabric can have different degrees of raising,
But supercritical CO2The uv resistance of the textile fabric of processing can be better than traditional treatment method, and treatment effect significantly improves,
Reason is：Supercritical CO2Metal precursor in processing procedure（I.e.：Zinc salt）With CO2Fibrous inside is penetrated into, is significantly carried
High UV resistance effect, durability and washing fastness.
The zinc salt that heretofore described metal precursor refers to just sometimes can because to restore later in profession
It is referred to as metal precursor, it is also possible to be write as zinc salt.
3, the contact angle of the anti-ultraviolet nano zinc oxide composite textile of differential responses time
Fig. 5 is the contact angle photo of dacron in the present embodiment, and Fig. 6 is the anti-ultraviolet nano zinc oxide prepared in the present embodiment
The contact angle photo of composite textile.The contact angle that dacron original sample is obtained by test is 91.5o, and is passed through overcritical
CO2The contact angle of anti-ultraviolet nano zinc oxide composite textile prepared by technology has reached 145.5 °, in comparison, has bright
Aobvious raising, this is because with CO during treatment with supercritical fluid2Pressure increases, supercritical CO2Plastisol effect and
Diffusion effect significantly improves, and is conducive to nano zine oxide and is diffused into fibrous inside gap, blocks fiber gap, reduces water
The infiltration of molecule, to improve contact angle, it can be seen that, supercritical CO2For the compound tool of nano zine oxide and textile fabric
There is positive effect.
Embodiment 3
The polyester fabric that size is 10cm × 10cm is used into acetone and ethanol solution ultrasonic cleaning 15min respectively, is then spent
Ionized water cleans up, and baking oven is dried for standby；Then 1.5g zinc acetylacetonates are dissolved in the ethyl alcohol of 25ml, are added overcritical
In fluid device；Polyester fabric after ultrasonic cleaning is put into Supercritical fluid device, and into Supercritical fluid device
It is passed through CO2Gas, supercritical reaction 6h under the conditions of pressure 15Mpa, 80 DEG C of temperature, takes out polyester fabric；Fabric is put into
Gas ions process instrumentation opens plasma instrument, connects argon gas, and first gas washing 2min removes air, adjusting gas flow 1L/
Min adjusts plasma instrument output power 1000W, and atmospheric pressure plasma jet treatment 2 minutes takes out fabric, closes instrument.So
The polyester fabric after supercritical reaction is put into hydrothermal reaction kettle again afterwards, 4h is heated under the conditions of 180 DEG C, finally takes out terylene face
Material is through washing, being drying to obtain nano zine oxide composite textile.
The uvioresistant performance of nano zine oxide composite material prepared by textile fabric original sample, embodiment 1 and embodiment 3
Comparison diagram is as shown in fig. 7, as shown in Figure 7：Pass through supercritical CO in embodiment 12Assist nano zine oxide prepared by infiltration compound
The uvioresistant performance of fabric is significantly improved as former state compared with textile fabric, and road corona treatment system in the increase of embodiment 3
The anti-ultraviolet property of standby nano zine oxide composite material improves compared to embodiment 1.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of anti-ultraviolet nano zinc oxide composite textile, which is characterized in that it prepares raw material and includes：Zinc salt, ethyl alcohol,
CO2, cosolvent, acetone and textile fabric, wherein zinc salt, cosolvent and textile fabric are by weight percentage：
Zinc salt 0.5 ~ 40%；
Cosolvent 0.5 ~ 80%；
Textile fabric 20 ~ 99%.
2. anti-ultraviolet nano zinc oxide composite textile according to claim 1, which is characterized in that the textile fabric
It is mixed for one or both of natural fiber and synthetic fibers.
3. anti-ultraviolet nano zinc oxide composite textile according to claim 1 or 2, which is characterized in that the weaving
Fabric is one or more mixing in cotton, hair, silk, fiber crops, terylene, polyamide fibre, acrylic fibers and polypropylene fibre.
4. anti-ultraviolet nano zinc oxide composite textile according to claim 1, which is characterized in that the zinc salt is second
One kind in acyl acetone zinc, zinc carbonate, zinc acetate.
5. anti-ultraviolet nano zinc oxide composite textile according to claim 1, which is characterized in that the cosolvent is
One kind in methanol, ethyl alcohol, n-butanol, isobutanol, acetone, ethylene glycol, triethylene glycol.
6. a kind of preparation method of anti-ultraviolet nano zinc oxide composite textile according to any one of claims 1 to 5,
It is characterized in that, assisting the preparation method that osmosis and thermal reduction are combined using supercritical fluid, include the following steps：
（1）By the textile fabric of 20 ~ 99g, 10 ~ 20min of ultrasonic cleaning in the ethyl alcohol and acetone soln of 0.5 ~ 80g；
（2）By step（1）Textile fabric after middle ultrasonic cleaning is cleaned up with deionized water, and 50 ~ 70 DEG C of drying of baking oven are standby
With；
（3）0.5 ~ 40 part of zinc salt is dissolved in the cosolvent of 0.5 ~ 80g, is then added in Supercritical fluid device, it will
Step（2）The textile fabric of middle drying is put into Supercritical fluid device, and CO is passed through into Supercritical fluid device2Gas, zinc
Salt is with supercritical CO2Into the fibrous inside of textile fabric, in 32 ~ 100 DEG C of 8 ~ 40MPa of first supercritical processing pressure, temperature conditions
Under terminate supercriticality after overcritical 1 ~ 12h of permeable reactive, CO is discharged2Gas, takes out textile fabric, and zinc salt is cured in spinning
The fibrous inside of knitted fabric；
（4）By step（3）It is middle permeated using supercritical fluid after textile fabric be put into hydrothermal reaction kettle, 100 ~ 200 DEG C of items
1 ~ 12h is heat-treated under part；
（5）Textile fabric is taken out from hydrothermal reaction kettle, through washing, being drying to obtain anti-ultraviolet nano zinc oxide Compound spinning surface of second order
Material.
7. the preparation method of anti-ultraviolet nano zinc oxide composite textile according to claim 6, which is characterized in that also
Including step（1）Textile fabric alkali decrement treatment step before, concrete operations are：Prepare the hydrogen-oxygen of 3%-20% mass concentrations
Change sodium solution, textile fabric is soaked into foam in sodium hydroxide solution, solid-to-liquid ratio 1:30,60-80 DEG C of heating water baths 5-20 minutes
Afterwards the 60 DEG C of drying of rear baking oven are rinsed well with deionized water.
8. the preparation method of anti-ultraviolet nano zinc oxide composite textile according to claim 6, which is characterized in that also
Including step（1）Textile fabric plasma treatment step before, concrete operations are：Plasma instrument is opened, argon gas is connected,
Textile fabric is put into plasma instrument by the removal air of first gas washing two minutes, adjusting gas flow 1L/min, adjust etc. from
Daughter instrument output power is 800-1200W, and atmospheric pressure plasma jet treatment 2-6 minutes takes out textile fabric, closes plasma
Instrument.
9. the preparation method of anti-ultraviolet nano zinc oxide composite textile according to claim 6, which is characterized in that also
Including step（3）Textile fabric plasma treatment step later, concrete operations are：Plasma instrument is opened, argon gas is connected,
Textile fabric is put into plasma instrument by the removal air of first gas washing two minutes, adjusting gas flow 1L/min, adjust etc. from
Daughter instrument output power is 1000W, and atmospheric pressure plasma jet treatment 1-2 minutes takes out textile fabric, closes instrument.
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