CN110924160A - Preparation method of anti-ultraviolet cotton fabric - Google Patents
Preparation method of anti-ultraviolet cotton fabric Download PDFInfo
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- CN110924160A CN110924160A CN201911312119.1A CN201911312119A CN110924160A CN 110924160 A CN110924160 A CN 110924160A CN 201911312119 A CN201911312119 A CN 201911312119A CN 110924160 A CN110924160 A CN 110924160A
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- 239000004744 fabric Substances 0.000 title claims abstract description 146
- 229920000742 Cotton Polymers 0.000 title claims abstract description 118
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 161
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 96
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 89
- 239000004005 microsphere Substances 0.000 claims abstract description 56
- 238000010438 heat treatment Methods 0.000 claims abstract description 47
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 37
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 37
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 37
- 239000000661 sodium alginate Substances 0.000 claims abstract description 37
- 239000008367 deionised water Substances 0.000 claims abstract description 33
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 33
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 32
- 239000000725 suspension Substances 0.000 claims abstract description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004321 preservation Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 10
- 238000002791 soaking Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 34
- 238000001035 drying Methods 0.000 claims description 32
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 24
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 17
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 claims description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 12
- 239000004202 carbamide Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- 238000007654 immersion Methods 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 238000009830 intercalation Methods 0.000 claims description 2
- 230000002687 intercalation Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 230000006750 UV protection Effects 0.000 abstract description 22
- 238000007598 dipping method Methods 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 description 25
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 20
- 239000000243 solution Substances 0.000 description 20
- 239000003795 chemical substances by application Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 18
- 239000007864 aqueous solution Substances 0.000 description 17
- 238000002834 transmittance Methods 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000001914 filtration Methods 0.000 description 9
- 239000004408 titanium dioxide Substances 0.000 description 9
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- 229910002804 graphite Inorganic materials 0.000 description 7
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 7
- 230000009471 action Effects 0.000 description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 6
- 239000012298 atmosphere Substances 0.000 description 5
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
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- 230000008569 process Effects 0.000 description 5
- 238000012216 screening Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 150000001767 cationic compounds Chemical class 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 230000004224 protection Effects 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001449 anionic compounds Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000009881 electrostatic interaction Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
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- 239000010410 layer Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
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- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241001474374 Blennius Species 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
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- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000011787 zinc oxide Substances 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
- 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
- D06M15/13—Alginic acid or derivatives thereof
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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
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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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
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- 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
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- 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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Abstract
The invention relates to the technical field of fabrics, and discloses a preparation method of an ultraviolet-proof cotton fabric. The method comprises the following steps: 1) placing the cotton fabric in a sodium hydroxide solution for heating treatment; 2) placing the cotton fabric in a sodium alginate solution, adding dicyclohexylcarbodiimide, carrying out heat preservation reaction, taking out the cotton fabric after the reaction is finished, placing the cotton fabric in a polyethyleneimine water solution for dipping treatment, taking out the cotton fabric, and placing the cotton fabric in deionized water for rinsing; 3) adding the modified graphene oxide into deionized water for ultrasonic dispersion to obtain a modified graphene oxide suspension, and soaking the cotton fabric dried in the step 1) in the modified graphene oxide suspension. According to the invention, the ultraviolet-resistant folded graphene oxide microspheres are attached to the surface of the cotton fabric in an assembling manner, and the graphene oxide microspheres are not easy to agglomerate and fall off from the surface of the cotton fabric, so that the ultraviolet protection performance and the durability of the fabric are improved.
Description
Technical Field
The invention relates to the technical field of fabrics, in particular to a preparation method of an ultraviolet-proof cotton fabric.
Background
The strong long-wave ultraviolet rays in the sunlight can easily penetrate through the surface layer of the skin to destroy the fine structures in the skin, such as collagen, elastic fibrous tissues and the like, so that the skin becomes aged and relaxed. Many measures have been taken for this purpose, such as the application of uv-protected cosmetics, the use of sun visors and parasols, etc., but these measures have limited protection, effective time and scope. Therefore, more and more people tend to protect the body from excessive damage of ultraviolet rays by using more comprehensive and effective ultraviolet-proof clothes. It is generally accepted that UV protection products having a UV protection factor (UPF value) of greater than 50 and a UVA (320-420nmUV) transmittance of less than 5% pass. The cotton fabric is soft in hand feeling, has good hygroscopicity and air permeability, is harmless to human bodies and is environment-friendly, so that the cotton fabric is a textile fabric favored by people.
Chinese patent publication No. CN106480581 discloses a waterproof and anti-ultraviolet high-strength light and thin fabric and a preparation method thereof, which comprises blending ceramic fibers and triangular anisotropic polyester fibers to form warps, adding nano silica sol and nano titania sol into a solvent, fully stirring, adding a graphite oxide solution, adding a polystyrene high polymer dropwise, uniformly stirring to obtain a coating finishing liquid, coating the coating finishing liquid on the surface of a base fabric, and drying to obtain an anti-ultraviolet fabric. Chinese patent publication No. CN103409843 discloses a method for preparing cotton nylon fibers with an anti-ultraviolet function, which comprises mixing titanium dioxide, silicon dioxide and zinc oxide, carrying out surface modification by using a coupling agent to obtain an ultraviolet screening agent, and then carrying out melt blending spinning on the ultraviolet screening agent and polyamide chips to obtain the cotton nylon fibers with anti-ultraviolet function, wherein most of the ultraviolet screening agent is dispersed in the nylon fibers, the ultraviolet screening agent on the surfaces of the nylon fibers is less, and the prepared nylon fibers have limited ultraviolet protection performance. Chinese patent publication No. CN108978184 discloses a preparation method of comfortable skin garment fabric, which comprises the steps of soaking polyester fibers in a dispersion liquid containing nano titanium dioxide, and then blending the polyester fibers with modal fibers and titanium dioxide fibers to obtain the fabric with an ultraviolet-proof effect, wherein titanium dioxide has strong photocatalytic property, and the titanium dioxide can cause damage to fabric fibers under the irradiation of light after contacting the fabric.
Disclosure of Invention
The invention provides a preparation method of an ultraviolet-proof cotton fabric in order to overcome the technical problems. According to the invention, the ultraviolet-resistant folded graphene oxide microspheres are attached to the surface of the cotton fabric in an assembling manner, and the graphene oxide microspheres are not easy to agglomerate and fall off from the surface of the cotton fabric, so that the ultraviolet protection performance and the durability of the fabric are improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an ultraviolet-proof cotton fabric comprises the following steps:
1) placing the cotton fabric in a sodium hydroxide solution, heating to 70-80 ℃ in a water bath, carrying out heat preservation treatment for 30-40min, taking out the cotton fabric, and airing at room temperature;
2) placing the cotton fabric dried in the step 1) into a sodium alginate solution, adding dicyclohexylcarbodiimide, heating to 60-75 ℃ in a water bath, carrying out heat preservation reaction for 5-10h, taking out the cotton fabric after the reaction is finished, placing the cotton fabric into a polyethyleneimine water solution, heating to 60-70 ℃ in the water bath, carrying out immersion treatment for 20-50min, rinsing in deionized water after being taken out, and placing in an oven for drying for later use;
3) adding the modified graphene oxide into deionized water for ultrasonic dispersion for 10-20min to obtain a modified graphene oxide suspension, placing the cotton fabric dried in the step 1) into the modified graphene oxide suspension for soaking for 1-3h, taking out the cotton fabric, and placing the cotton fabric into an oven for drying to obtain the modified graphene oxide suspension.
Preferably, the mass concentration of the sodium hydroxide solution in the step 1) is 0.5-1%.
Preferably, the concentration of the sodium alginate solution in said step 2) is 1-10 wt%.
Preferably, the concentration of the polyethyleneimine solution in the step 2) is 1 to 5 wt%.
Preferably, the preparation method of the modified graphene oxide comprises the following steps: adding graphite powder into sulfuric acid, uniformly stirring, sequentially adding potassium ferrate and hydrogen peroxide solution for intercalation oxidation, separating, washing and drying to obtain graphene oxide, quickly heating the graphene oxide in a nitrogen atmosphere, roasting at high temperature to obtain folded graphene oxide microspheres, adding the folded graphene oxide microspheres into deionized water, stirring to form a suspension, adding titanium sulfate and urea into the suspension, adjusting the pH to 2-3, heating in a water bath to 75-85 ℃, stirring for reaction for 3-5h, washing with water after separation, drying, placing in a muffle furnace, roasting in a nitrogen atmosphere, and cooling at room temperature to obtain the modified graphene oxide.
Preferably, the mass ratio of the folded graphene microspheres to the titanium sulfate is 1: 0.3-0.6.
Preferably, the mass ratio of the titanium sulfate to the urea is 1: 3-5.
Preferably, the high-temperature roasting temperature is 150-200 ℃.
The surface of the graphene oxide is provided with rich oxygen-containing functional groups (carboxyl, hydroxyl, epoxy and the like), polyethyleneimine molecules are provided with more amino groups, and the functional groups can absorb ultraviolet energy and convert the absorbed ultraviolet energy into heat energy for dissipation. The method comprises the following steps of immersing the cotton fabric into a sodium hydroxide solution for heating treatment, so that fibers in the cotton fabric are loose, more active groups such as carboxyl groups are exposed on the surface of the fibers, and the loose cotton fabric facilitates the modified substances to enter the interior of the cotton fabric, thereby being beneficial to fully modifying the cotton fabric fibers by the modified substances; then placing the cotton fabric in a sodium alginate solution for soaking treatment, under the action of a condensing agent dicyclohexylcarbodiimide condensing agent, carrying out condensation reaction on carboxyl on the surface of the cotton fabric and hydroxyl on the sodium alginate, thereby grafting the sodium alginate on the surface of the cotton fabric, because the sodium alginate is an anionic compound, polyethyleneimine is protonated into a cationic compound after being dissolved in water, the polyethyleneimine is assembled on the surface of the sodium alginate through intermolecular electrostatic action of layer-by-layer self-assembly, and the hydroxyl in the sodium alginate molecule and amino on the polyethyleneimine molecule form hydrogen bond action, thereby firmly combining the polyethyleneimine on the sodium alginate, the surface of graphene oxide is loaded with carboxyl and other groups which are ionized and show negative electricity, and graphite oxide is assembled on the surface of the polyethyleneimine through electrostatic action between the graphene oxide and the cationic compound of the polyethyleneimine, the electrostatic acting force and the physical adhesion acting force between the graphene oxide and the fabric enable the graphene oxide to be stably combined with the fabric fiber, and the graphene oxide is not easy to fall off from the surface of the fabric fiber. In addition, the graphene oxide is dispersed on the surface of the fabric fiber rather than in the fiber, so that the fabric has relatively better ultraviolet protection performance and cannot cause adverse effect on the mechanical strength of the fiber.
Because the graphene oxide is of a lamellar structure, the flaky graphene oxide is easy to agglomerate, so that the graphene oxide is extremely difficult to uniformly disperse on the surface of fabric fibers, and the overall ultraviolet protection performance of the cotton fabric is reduced. The invention aims to solve the problem that flake graphite oxide is easy to agglomerate, flake graphene oxide is subjected to modification treatment, potassium ferrate and hydrogen peroxide are sequentially used for carrying out oxidation treatment on graphene in the preparation process of the modified graphene oxide, and then the flake graphite oxide is subjected to folding shrinkage deformation under the condition of high-temperature roasting to obtain folded graphene oxide microspheres, wherein the folded graphene oxide microspheres are different from the flake graphene oxide microspheres in that: the contact mode between the folded graphene microspheres is point-point contact, the contact mode between the flaky graphene oxide is surface-to-surface contact, and the point-point contact mode can greatly reduce the agglomeration between the graphene oxide relative to the surface-to-surface contact mode. Therefore, compared with the flaky graphene oxide, the folded graphene oxide microspheres have better dispersion performance and are more uniformly dispersed on the fiber surface of the fabric, so that the integral ultraviolet protection performance of the cotton fabric is improved. However, the problem encountered in the practical experimental process is that the prepared folded graphene oxide microspheres are shrunk into a three-dimensional spherical structure, and the folded graphene oxide microspheres are easily broken in the process of carrying out an ultrasonic dispersion step on the folded graphene oxide microspheres, so that the structure of the graphene oxide microspheres is modified, and further the dispersion performance is reduced. On the other hand, titanium dioxide is an inorganic titanium dioxide ultraviolet screening agent, the action principle of ultraviolet rays is mainly reflection of ultraviolet rays, and the ultraviolet protection effect of the cotton fabric is remarkably improved due to the sea-island structural relationship between the corrugated graphite oxide and the titanium dioxide. In addition, because titanium dioxide has strong photocatalytic performance, the direct contact with fabric fibers can cause the photocatalytic degradation of fiber fabrics and the damage of the fabric fibers, and the nano titanium dioxide is deposited and filled in the fold grooves of the folded graphene microspheres, which is equivalent to the coating effect of the folded graphene microspheres on the nano titanium dioxide, so that the damage of cotton fabric fibers caused by the strong photocatalytic performance of the titanium dioxide is avoided.
In the preparation process of the modified graphene oxide, the mass ratio of the folded graphene microspheres to the titanium sulfate must be controlled within a certain proportion range. When the addition amount of titanium sulfate relative to the folded graphene microspheres is too large, a large amount of nano titanium dioxide is deposited on the surfaces of the folded graphene microspheres, the folded graphene microspheres are completely coated, oxygen-containing functional groups on the surfaces of the graphene oxide are shielded by nano silicon dioxide, and the absorption of the graphene oxide on ultraviolet rays is influenced. When the addition amount of titanium sulfate relative to the folded graphene microspheres is too small, the amount of nano titanium dioxide generated by hydrolysis of titanium sulfate is too small, so that the folded grooves of the folded graphene microspheres are not sufficiently filled, the strength of the folded graphene microspheres cannot be effectively improved, and the folded graphene microspheres are easy to break in the ultrasonic dispersion process, so that the microsphere-shaped structure is changed, and the dispersion of the folded graphene microspheres is not facilitated. The mass ratio of the folded graphene microspheres to the titanium sulfate is controlled within the proportion range of the invention, and the graphene oxide can have better ultraviolet absorption capacity and keep the dispersion effect of the folded graphene microspheres.
Drawings
FIG. 1 is a graph of the number of times of washing and the average UVB transmittance of cotton fabric of example 1 and comparative example 1.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples. In the present invention, unless otherwise specified, all the raw materials and equipment used are commercially available or commonly used in the art, and the methods in the specific examples are conventional in the art unless otherwise specified.
The cotton fabric used in the specific embodiment is cotton plain white gray fabric, 70mm multiplied by 70mm, 115g/m2(ii) a The used sodium alginate is produced by Qingdao double-forming seaweed Limited company, the granularity is 30 meshes, the water content is less than or equal to 15 percent, and the water-insoluble content is less than or equal to 0.6; the polyethyleneimine used was a polyethylene produced by Lenbeck corporation, viscosity 8300-. The graphite powder is crystalline flake graphite produced by Qingdao Tianyuan Daigao graphite Limited, the size of the crystalline flake is 10 mu m, the fixed carbon content is 99 percent, the hardness is 1.2, and the density is 1.98; the sulfuric acid used was concentrated sulfuric acid having a mass concentration of 97%.
Example 1
The preparation method of the modified graphene oxide comprises the following steps:
adding graphite powder into sulfuric acid according to the mass-to-volume ratio of 1g/30mL, uniformly stirring, cooling to below zero DEG C in an ice bath, adding potassium ferrate according to the mass ratio of 1:5 of the graphite powder to the potassium ferrate, uniformly stirring, replacing with a water bath, heating to 40 ℃, keeping at a constant temperature for 20min, continuously heating to 75 ℃, keeping at a constant temperature for 30min, then adding a 20% hydrogen peroxide aqueous solution, keeping at a constant temperature for oxidizing for 10min, adding deionized water for diluting, filtering, separating, washing, drying in a drying oven at 50 ℃ to obtain graphene oxide, placing the graphene oxide in a muffle furnace, rapidly heating to 450 ℃ in the atmosphere of nitrogen, roasting at a high temperature for 2h to obtain folded graphene oxide microspheres, adding the folded graphene oxide microspheres into deionized water according to the mass-to-volume ratio of 1g/50mL, stirring to form a suspension, adding titanium sulfate and urea into the suspension, wherein the mass ratio of the folded graphene microspheres to the titanium sulfate is 1:0.5, the mass ratio of the titanium sulfate to the urea is 1:3, adjusting the pH to 2.5, heating in a water bath to 85 ℃, stirring for reaction for 3h, filtering, separating, washing with water, drying in a drying oven at 50 ℃, then roasting in a muffle furnace in a nitrogen atmosphere at 180 ℃ for 3h, and cooling at room temperature to obtain the modified graphene oxide.
The preparation method of the ultraviolet-proof cotton fabric comprises the following steps:
1) placing the cotton fabric in a sodium hydroxide aqueous solution with the mass concentration of 1%, heating the cotton fabric to 75 ℃ in a water bath, carrying out heat preservation treatment for 35min, taking out the cotton fabric, and airing the cotton fabric at room temperature;
2) adding sodium alginate into deionized water, stirring and dissolving to prepare a sodium alginate aqueous solution with the concentration of 8 wt%, placing the cotton fabric dried in the step 1) into the sodium alginate aqueous solution, then adding a dicyclohexylcarbodiimide condensing agent, heating in a water bath to 70 ℃, carrying out heat preservation reaction for 8 hours, and taking out the cotton fabric a after the reaction is finished, wherein the addition amount of the dicyclohexylcarbodiimide condensing agent is 2% of the mass of the sodium alginate; adding polyethyleneimine into deionized water, heating, stirring and dissolving to obtain a polyethyleneimine water solution with the solubility of 3 wt%, immersing the cotton fabric a into the polyethyleneimine water solution, heating in a water bath to 60 ℃, performing immersion treatment for 50min, taking out, rinsing in the deionized water, and drying in an oven at 60 ℃ for later use;
3) adding the modified graphene oxide into deionized water according to the mass-volume ratio of 1g/40mL, performing ultrasonic dispersion for 15min under the power of 150W to obtain a modified graphene oxide suspension, placing the cotton fabric dried in the step 1) into the modified graphene oxide suspension for soaking for 2h, taking out, and placing the cotton fabric into an oven to dry for 3h at the temperature of 50 ℃ to obtain the modified graphene oxide suspension.
Example 2
The preparation method of the modified graphene oxide comprises the following steps:
adding graphite powder into sulfuric acid according to the mass-to-volume ratio of 1g/30mL, uniformly stirring, cooling to below zero DEG C in an ice bath, adding potassium ferrate according to the mass ratio of 1:5 of the graphite powder to the potassium ferrate, uniformly stirring, replacing with a water bath, heating to 40 ℃, keeping at a constant temperature for 20min, continuously heating to 75 ℃, keeping at a constant temperature for 30min, then adding a 20% hydrogen peroxide aqueous solution, keeping at a constant temperature for oxidizing for 10min, adding deionized water for diluting, filtering, separating, washing, drying in a drying oven at 50 ℃ to obtain graphene oxide, placing the graphene oxide in a muffle furnace, rapidly heating to 450 ℃ in the atmosphere of nitrogen, roasting at a high temperature for 2h to obtain folded graphene oxide microspheres, adding the folded graphene oxide microspheres into deionized water according to the mass-to-volume ratio of 1g/50mL, stirring to form a suspension, adding titanium sulfate and urea into the suspension, wherein the mass ratio of the folded graphene microspheres to the titanium sulfate is 1:0.4, the mass ratio of the titanium sulfate to the urea is 1:5, adjusting the pH to 2.5, heating in a water bath to 75 ℃, stirring for reaction for 5h, filtering, separating, washing with water, drying in a drying oven at 50 ℃, then roasting in a muffle furnace in a nitrogen atmosphere at 160 ℃ for 3h, and cooling at room temperature to obtain the modified graphene oxide.
The preparation method of the ultraviolet-proof cotton fabric comprises the following steps:
1) placing the cotton fabric in a sodium hydroxide aqueous solution with the mass concentration of 0.5%, heating the cotton fabric to 75 ℃ in a water bath, carrying out heat preservation treatment for 35min, taking out the cotton fabric, and airing the cotton fabric at room temperature;
2) adding sodium alginate into deionized water, stirring and dissolving to prepare a sodium alginate aqueous solution with the concentration of 5wt%, placing the cotton fabric dried in the step 1) into the sodium alginate aqueous solution, then adding a dicyclohexylcarbodiimide condensing agent, heating in a water bath to 65 ℃, carrying out heat preservation reaction for 6 hours, and taking out the cotton fabric a after the reaction is finished, wherein the addition amount of the dicyclohexylcarbodiimide condensing agent is 2% of the mass of the sodium alginate; adding polyethyleneimine into deionized water, heating, stirring and dissolving to obtain a polyethyleneimine water solution with the solubility of 2 wt%, immersing the cotton fabric a into the polyethyleneimine water solution, heating in a water bath to 70 ℃, performing immersion treatment for 20min, taking out, rinsing in the deionized water, and drying in an oven at 60 ℃ for later use;
3) adding the modified graphene oxide into deionized water according to the mass-volume ratio of 1g/40mL, performing ultrasonic dispersion for 15min under the power of 150W to obtain a modified graphene oxide suspension, placing the cotton fabric dried in the step 1) into the modified graphene oxide suspension for soaking for 2h, taking out, and placing the cotton fabric into an oven to dry for 3h at the temperature of 50 ℃ to obtain the modified graphene oxide suspension.
Example 3
The preparation method of the modified graphene oxide comprises the following steps:
adding graphite powder into sulfuric acid according to the mass-to-volume ratio of 1g/30mL, uniformly stirring, cooling to below zero DEG C in an ice bath, adding potassium ferrate according to the mass ratio of 1:5 of the graphite powder to the potassium ferrate, uniformly stirring, replacing with a water bath, heating to 40 ℃, keeping at a constant temperature for 20min, continuously heating to 75 ℃, keeping at a constant temperature for 30min, then adding a 20% hydrogen peroxide aqueous solution, keeping at a constant temperature for oxidizing for 10min, adding deionized water for diluting, filtering, separating, washing, drying in a drying oven at 50 ℃ to obtain graphene oxide, placing the graphene oxide in a muffle furnace, rapidly heating to 450 ℃ in the atmosphere of nitrogen, roasting at a high temperature for 2h to obtain folded graphene oxide microspheres, adding the folded graphene oxide microspheres into deionized water according to the mass-to-volume ratio of 1g/50mL, stirring to form a suspension, adding titanium sulfate and urea into the suspension, wherein the mass ratio of the folded graphene microspheres to the titanium sulfate is 1:0.6, the mass ratio of the titanium sulfate to the urea is 1:4, adjusting the pH to 3, heating in a water bath to 80 ℃, stirring for reaction for 4h, filtering, separating, washing with water, drying in a drying oven at 50 ℃, then roasting in a muffle furnace in a nitrogen atmosphere at 200 ℃ for 3h, and cooling at room temperature to obtain the modified graphene oxide.
The preparation method of the ultraviolet-proof cotton fabric comprises the following steps:
1) placing the cotton fabric in a sodium hydroxide aqueous solution with the mass concentration of 0.8%, heating the cotton fabric to 80 ℃ in a water bath, carrying out heat preservation treatment for 40min, taking out the cotton fabric, and airing the cotton fabric at room temperature;
2) adding sodium alginate into deionized water, stirring and dissolving to prepare a 10wt% sodium alginate aqueous solution, placing the cotton fabric dried in the step 1) into the sodium alginate aqueous solution, then adding a dicyclohexylcarbodiimide condensing agent, heating in a water bath to 75 ℃, carrying out heat preservation reaction for 10 hours, and taking out the cotton fabric a after the reaction is finished, wherein the addition amount of the dicyclohexylcarbodiimide condensing agent is 2% of the mass of the sodium alginate; adding polyethyleneimine into deionized water, heating, stirring and dissolving to obtain a polyethyleneimine water solution with the solubility of 5wt%, immersing the cotton fabric a into the polyethyleneimine water solution, heating in a water bath to 65 ℃, performing immersion treatment for 30min, taking out, rinsing in deionized water, and drying in an oven at 60 ℃ for later use;
3) adding the modified graphene oxide into deionized water according to the mass-volume ratio of 1g/40mL, performing ultrasonic dispersion for 20min under the power of 150W to obtain a modified graphene oxide suspension, placing the cotton fabric dried in the step 1) into the modified graphene oxide suspension for dipping for 3h, taking out, and placing the cotton fabric into an oven to dry for 3h at the temperature of 50 ℃ to obtain the modified graphene oxide suspension.
Example 4
The preparation method of the modified graphene oxide comprises the following steps:
adding graphite powder into sulfuric acid according to the mass-to-volume ratio of 1g/30mL, uniformly stirring, cooling to below zero DEG C in an ice bath, adding potassium ferrate according to the mass ratio of 1:5 of the graphite powder to the potassium ferrate, uniformly stirring, replacing with a water bath, heating to 40 ℃, keeping at a constant temperature for 20min, continuously heating to 75 ℃, keeping at a constant temperature for 30min, then adding a 20% hydrogen peroxide aqueous solution, keeping at a constant temperature for oxidizing for 10min, adding deionized water for diluting, filtering, separating, washing, drying in a drying oven at 50 ℃ to obtain graphene oxide, placing the graphene oxide in a muffle furnace, rapidly heating to 450 ℃ in the atmosphere of nitrogen, roasting at a high temperature for 2h to obtain folded graphene oxide microspheres, adding the folded graphene oxide microspheres into deionized water according to the mass-to-volume ratio of 1g/50mL, stirring to form a suspension, adding titanium sulfate and urea into the suspension, wherein the mass ratio of the folded graphene microspheres to the titanium sulfate is 1:0.3, the mass ratio of the titanium sulfate to the urea is 1:4, adjusting the pH to 2, heating in a water bath to 80 ℃, stirring for reaction for 4h, filtering, separating, washing with water, drying in a drying oven at 50 ℃, then roasting in a muffle furnace in a nitrogen atmosphere at 150 ℃ for 3h, and cooling at room temperature to obtain the modified graphene oxide.
The preparation method of the ultraviolet-proof cotton fabric comprises the following steps:
1) placing the cotton fabric in a sodium hydroxide aqueous solution with the mass concentration of 0.8%, heating the cotton fabric to 70 ℃ in a water bath, carrying out heat preservation treatment for 30min, taking out the cotton fabric, and airing the cotton fabric at room temperature;
2) adding sodium alginate into deionized water, stirring and dissolving to prepare a sodium alginate aqueous solution with the concentration of 1 wt%, placing the cotton fabric dried in the step 1) into the sodium alginate aqueous solution, then adding a dicyclohexylcarbodiimide condensing agent, heating in a water bath to 60 ℃, carrying out heat preservation reaction for 5 hours, and taking out the cotton fabric a after the reaction is finished, wherein the addition amount of the dicyclohexylcarbodiimide condensing agent is 2% of the mass of the sodium alginate; adding polyethyleneimine into deionized water, heating, stirring and dissolving to obtain a polyethyleneimine water solution with the solubility of 1 wt%, immersing the cotton fabric a into the polyethyleneimine water solution, heating in a water bath to 65 ℃, performing immersion treatment for 30min, taking out, rinsing in the deionized water, and drying in an oven at 60 ℃ for later use;
3) adding the modified graphene oxide into deionized water according to the mass-volume ratio of 1g/40mL, performing ultrasonic dispersion for 10min under the power of 150W to obtain a modified graphene oxide suspension, placing the cotton fabric dried in the step 1) into the modified graphene oxide suspension for soaking for 1h, taking out, and placing the cotton fabric into an oven to dry for 3h at the temperature of 50 ℃ to obtain the modified graphene oxide suspension.
Comparative example 1: the comparative example 1 and the example 1 are different in that the reaction step of the cotton fabric and the sodium alginate in the step 2) is removed in the preparation method of the ultraviolet-proof cotton fabric.
Comparative example 2: comparative example 2 is different from example 1 in that the modified graphene oxide was replaced with a commercially available ordinary graphene oxide (manufactured by Nanjing Xiapong nanomaterial Co., Ltd., sheet diameter > 5 μm).
Comparative example 3: the comparative example 3 is different from the example 1 in the preparation method of the modified graphene oxide:
adding graphite powder into sulfuric acid according to the mass-volume ratio of 1g/30mL, uniformly stirring, cooling to below zero DEG C in an ice bath, adding potassium ferrate according to the mass ratio of 1:5 of the graphite powder to the potassium ferrate, uniformly stirring, replacing with a water bath, heating to 40 ℃, keeping at a constant temperature for 20min, continuously heating to 75 ℃, keeping at a constant temperature for 30min, then adding a 20% hydrogen peroxide aqueous solution, keeping at a constant temperature for oxidizing for 10min, adding deionized water for diluting, filtering, separating, washing, drying in a drying oven at 50 ℃ to obtain graphene oxide, placing the graphene oxide in a muffle furnace, rapidly heating to 450 ℃ in the atmosphere of nitrogen, and roasting at a high temperature for 2h to obtain the modified graphene oxide.
Firstly, ultraviolet resistance testing:
the average transmittance and the ultraviolet protection index UPF value of UVA (315 + 400nm) in a long-wave ultraviolet region and UVB (280 + 315nm) in a medium-wave ultraviolet region are respectively calculated by measuring the cotton fabric fabrics prepared in the examples 1 to 4 and the comparative examples 2 to 3 according to AS/NZS4399 'evaluation and grading standard of solar protection clothes'. Generally, when the transmittance of UVA and UVB of the fabric is lower than 5% and the UPF (ultraviolet protection index) value is higher than 40, the fabric is proved to have ultraviolet protection capability. The average transmittances of UVA and UVB and the UPF value of the ultraviolet protection index of the cotton fabric prepared in the examples 1 to 4 and the comparative examples 2 to 3 are shown in the following table:
according to the test results, the ultraviolet protection performance of the cotton fabric prepared in the embodiments 1 to 4 meets the standard (the ultraviolet protection index UPF value is more than 40, and the transmittances of UVA and UVB are lower than 5%), and the cotton fabric prepared in the comparative examples 2 to 3 does not meet the standards of UVB transmittance composite regulation, but the UVA transmittance and the UPF protection coefficient do not meet the standards. In addition, as can be seen from comparison of the test results of examples 1-4 and comparative examples 2-3, the ultraviolet protection index UPF value, UVA and UVB transmittance of the fabric of examples 1-4 are obviously superior to those of comparative examples 2-3, and the invention is proved to have better ultraviolet protection performance. The ultraviolet protection performance of the cotton fabric is superior to that of the comparative example 2 in the examples 1 to 4, because the folded graphene oxide microspheres have better dispersion performance and are more uniformly dispersed on the fiber surface of the fabric compared with the flaky graphene oxide microspheres in the comparative example 2, so that the overall ultraviolet protection performance of the cotton fabric is improved. The ultraviolet protection performance of the cotton fabric in the embodiments 1 to 4 is superior to that of the comparative example 3, because the folded graphene oxide microspheres prepared in the comparative example 3 are shrunk into a three-dimensional spherical structure, the folded graphene oxide microspheres are easily broken in the process of carrying out an ultrasonic dispersion step on the folded graphene oxide microspheres, so that the structure of the graphene oxide microspheres is modified, and the dispersion performance is reduced; according to the preparation method, titanium sulfate is hydrolyzed to generate nano titanium dioxide, the nano titanium dioxide is deposited and filled in the 'fold grooves' of the folded graphene microspheres, and the nano sodium dioxide is combined with each other at a high temperature, so that the graphene microspheres with empty interiors are changed into solid graphene microspheres, the graphene microspheres have better strength, and the breakage rate of the folded graphene microspheres is greatly reduced in the ultra-dispersion process of the folded graphene oxide microspheres.
Secondly, washing fastness test:
in order to detect the firmness of the combination of the ultraviolet shielding agent (graphene oxide and polyethyleneimine) and the cotton fabric, a washing test was performed on the cotton fabric of example 1 and comparative example 1. The test was carried out using JIS washing method, the washing procedure being: soaking the cotton fabric in 2g/L soap powder solution, washing with shaking water at 40 ℃ for 10min, washing with clear water for 2min to finish primary washing, and drying at 80 ℃. The average ultraviolet UVB transmittance of each ultraviolet ray was measured after washing 15 times in this manner. The test results are shown in fig. 1.
According to the test results, the change of the UVB transmittance of the cotton fabric in the embodiment 1 of the invention along with the increase of the washing times is very small, while the UVB transmittance of the cotton fabric in the comparative example 1 along with the increase of the washing times shows an obvious increasing trend, and the cotton fabric has relatively stable ultraviolet protection performance. The invention is characterized in that the cotton fabric is soaked in sodium alginate solution, under the action of a condensing agent dicyclohexylcarbodiimide condensing agent, carboxyl on the surface of the cotton fabric fiber and hydroxyl on the sodium alginate are subjected to condensation reaction, so that the sodium alginate is grafted on the surface of the cotton fabric, because the sodium alginate is an anionic compound, polyethyleneimine is protonated into a cationic compound after being dissolved in water, the polyethyleneimine is assembled on the surface of the sodium alginate through intermolecular electrostatic interaction of layer-by-layer self-assembly, and the hydroxyl in the sodium alginate molecule and amino on the polyethyleneimine molecule form hydrogen bond interaction, so that the polyethyleneimine is firmly combined on the sodium alginate, the surface of graphene oxide is loaded with groups which show negative electricity through ionization such as carboxyl, and the graphene oxide is assembled on the surface of the polyethyleneimine through electrostatic interaction between the graphene oxide and the cationic compound of the polyethyleneimine, the electrostatic acting force and the physical adhesion acting force between the graphene oxide and the fabric enable the graphene oxide to be stably combined with the fabric fiber, and the graphene oxide is not easy to fall off from the surface of the fabric fiber.
Claims (8)
1. The preparation method of the ultraviolet-proof cotton fabric is characterized by comprising the following steps of:
1) placing the cotton fabric in a sodium hydroxide solution, heating to 70-80 ℃ in a water bath, carrying out heat preservation treatment for 30-40min, taking out the cotton fabric, and airing at room temperature;
2) placing the cotton fabric dried in the step 1) into a sodium alginate solution, adding dicyclohexylcarbodiimide, heating to 60-75 ℃ in a water bath, carrying out heat preservation reaction for 5-10h, taking out the cotton fabric after the reaction is finished, placing the cotton fabric into a polyethyleneimine water solution, heating to 60-70 ℃ in the water bath, carrying out immersion treatment for 20-50min, rinsing in deionized water after being taken out, and placing in an oven for drying for later use;
3) adding the modified graphene oxide into deionized water for ultrasonic dispersion for 10-20min to obtain a modified graphene oxide suspension, placing the cotton fabric dried in the step 1) into the modified graphene oxide suspension for soaking for 1-3h, taking out the cotton fabric, and placing the cotton fabric into an oven for drying to obtain the modified graphene oxide suspension.
2. The preparation method of the ultraviolet-proof cotton fabric according to claim 1, wherein the mass concentration of the sodium hydroxide solution in the step 1) is 0.5-1%.
3. The method for preparing the ultraviolet-proof cotton fabric according to claim 2, wherein the concentration of the sodium alginate solution in the step 2) is 1-10 wt%.
4. The preparation method of the ultraviolet-proof cotton fabric according to claim 1, wherein the concentration of the polyethyleneimine solution in the step 2) is 1-5 wt%.
5. The preparation method of the ultraviolet-proof cotton fabric according to claim 1, wherein the preparation method of the modified graphene oxide comprises the following steps: adding graphite powder into sulfuric acid, uniformly stirring, sequentially adding potassium ferrate and hydrogen peroxide solution for intercalation oxidation, separating, washing and drying to obtain graphene oxide, quickly heating the graphene oxide in a nitrogen atmosphere, roasting at high temperature to obtain folded graphene oxide microspheres, adding the folded graphene oxide microspheres into deionized water, stirring to form a suspension, adding titanium sulfate and urea into the suspension, adjusting the pH to 2-3, heating in a water bath to 75-85 ℃, stirring for reaction for 3-5h, washing with water after separation, drying, placing in a muffle furnace, roasting in a nitrogen atmosphere, and cooling at room temperature to obtain the modified graphene oxide.
6. The preparation method of the ultraviolet-proof cotton fabric according to claim 5, wherein the mass ratio of the folded graphene microspheres to the titanium sulfate is 1: 0.3-0.6.
7. The preparation method of the ultraviolet-proof cotton fabric according to claim 5, wherein the mass ratio of the titanium sulfate to the urea is 1: 3-5.
8. The preparation method of the ultraviolet-proof cotton fabric as claimed in claim 5, wherein the high-temperature roasting temperature is 150-200 ℃.
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| CN111990409A (en) * | 2020-07-08 | 2020-11-27 | 厦门大学 | Broad-spectrum antiviral material and preparation method and application thereof |
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| CN111990409A (en) * | 2020-07-08 | 2020-11-27 | 厦门大学 | Broad-spectrum antiviral material and preparation method and application thereof |
| CN111990409B (en) * | 2020-07-08 | 2021-06-22 | 厦门大学 | Broad-spectrum antiviral material and preparation method and application thereof |
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| CN114411410A (en) * | 2022-01-10 | 2022-04-29 | 常熟理工学院 | Preparation method of hydrophobic anti-ultraviolet bifunctional cotton fabric |
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