CN105944708A - TiO2-C@TiO2-rGO transparent self-supporting film, and production method and application thereof - Google Patents
TiO2-C@TiO2-rGO transparent self-supporting film, and production method and application thereof Download PDFInfo
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- CN105944708A CN105944708A CN201610287541.6A CN201610287541A CN105944708A CN 105944708 A CN105944708 A CN 105944708A CN 201610287541 A CN201610287541 A CN 201610287541A CN 105944708 A CN105944708 A CN 105944708A
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- 238000004519 manufacturing process Methods 0.000 title abstract 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 157
- 239000000463 material Substances 0.000 claims abstract description 149
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229920002678 cellulose Polymers 0.000 claims abstract description 40
- 239000001913 cellulose Substances 0.000 claims abstract description 40
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 29
- 238000005406 washing Methods 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000011941 photocatalyst Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 102
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 81
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 39
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- HHDOORYZQSEMGM-UHFFFAOYSA-L potassium;oxalate;titanium(4+) Chemical compound [K+].[Ti+4].[O-]C(=O)C([O-])=O HHDOORYZQSEMGM-UHFFFAOYSA-L 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 27
- 229910000077 silane Inorganic materials 0.000 claims description 27
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 26
- 238000002360 preparation method Methods 0.000 claims description 24
- 239000007864 aqueous solution Substances 0.000 claims description 21
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 16
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 14
- 238000003763 carbonization Methods 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 13
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 11
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 7
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 claims description 2
- 238000006731 degradation reaction Methods 0.000 claims description 2
- 244000025254 Cannabis sativa Species 0.000 claims 1
- KYNKUCOQLYEJPH-UHFFFAOYSA-N [K][Ti] Chemical compound [K][Ti] KYNKUCOQLYEJPH-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 238000010000 carbonizing Methods 0.000 abstract description 2
- 239000006087 Silane Coupling Agent Substances 0.000 abstract 2
- UHWHMHPXHWHWPX-UHFFFAOYSA-J dipotassium;oxalate;oxotitanium(2+) Chemical compound [K+].[K+].[Ti+2]=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O UHWHMHPXHWHWPX-UHFFFAOYSA-J 0.000 abstract 2
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 56
- 239000000835 fiber Substances 0.000 description 17
- 230000001699 photocatalysis Effects 0.000 description 12
- 238000010992 reflux Methods 0.000 description 12
- 239000010410 layer Substances 0.000 description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 10
- 238000007146 photocatalysis Methods 0.000 description 9
- 229920003043 Cellulose fiber Polymers 0.000 description 7
- 239000010409 thin film Substances 0.000 description 7
- 229920000049 Carbon (fiber) Polymers 0.000 description 6
- 239000004917 carbon fiber Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- YICOVXASQKWWDU-UHFFFAOYSA-N ethanol;3-triethoxysilylpropan-1-amine Chemical compound CCO.CCO[Si](OCC)(OCC)CCCN YICOVXASQKWWDU-UHFFFAOYSA-N 0.000 description 4
- KXHFTXJPJMEXKR-UHFFFAOYSA-N methanol 3-trimethoxysilylpropan-1-amine Chemical compound OC.CO[Si](OC)(OC)CCCN KXHFTXJPJMEXKR-UHFFFAOYSA-N 0.000 description 4
- DUZHCFGUSIJGMU-UHFFFAOYSA-N toluene;3-triethoxysilylpropan-1-amine Chemical compound CC1=CC=CC=C1.CCO[Si](OCC)(OCC)CCCN DUZHCFGUSIJGMU-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- JWDCJCRGZTUWDY-UHFFFAOYSA-N ethanol;3-trimethoxysilylpropan-1-amine Chemical compound CCO.CO[Si](OC)(OC)CCCN JWDCJCRGZTUWDY-UHFFFAOYSA-N 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- WACUFSIGNPLHOR-UHFFFAOYSA-N toluene;3-trimethoxysilylpropan-1-amine Chemical compound CC1=CC=CC=C1.CO[Si](OC)(OC)CCCN WACUFSIGNPLHOR-UHFFFAOYSA-N 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 silicon Alkane Chemical class 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/10—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation
- A62D3/17—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation to electromagnetic radiation, e.g. emitted by a laser
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B01J35/59—
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/28—Organic substances containing oxygen, sulfur, selenium or tellurium, i.e. chalcogen
Abstract
The invention discloses a TiO2-C@TiO2-rGO transparent self-supporting film. Raw materials of the TiO2-C@TiO2-rGO transparent self-supporting film comprise potassium titanium oxalate, diglycol, cellulose paper, graphene oxide and a silane coupling agent. The invention also discloses a production method of the TiO2-C@TiO2-rGO transparent self-supporting film. The method comprises the following steps: 1, preparing a reaction solution: dissolving potassium titanium oxalate in a diglycol-water solution to obtain a solution A; 2, carrying out a hydrothermal reaction: dipping the cellulose paper in the solution A obtained in step 1, carrying out the hydrothermal reaction, taking out the material obtained after the reaction, washing the material, and drying the washed material to obtain a material B; 3, modifying the material B with the silane coupling agent; 4, carrying out graphene oxide electrostatic self-assembling; and 5, carbonizing a material obtained in step 4. The invention also discloses an application of the TiO2-C@TiO2-rGO transparent self-supporting film as a visible light photocatalyst.
Description
Technical field
The present invention relates to photocatalysis technology field, particularly relate to TiO2-C@TiO2The transparent self-supporting film of-rGO and
Its preparation method and application.
Background technology
Along with the development of global industry, environmental pollution has changed into serious social problem.The lasting evil of environment
Change and promote the new technology of research worker development to carry out pollution remission crisis.Photocatalysis is the most promising as one
Depollution of environment technology has obtained paying close attention to widely.
Various in the semi-conducting material of photocatalytic applications, TiO2Because it is nontoxic, catalysis activity is high, oxidation
The advantages such as ability is strong, good stability are considered as the green light catalyst and pollution control material attracted most attention.
But, TiO2There is high band gap and relatively low quantum efficiency, by a definite limitation in application, the most logical
Cross TiO2Carry out compound or doping vario-property, strengthen it to the response range of light and answering of suppression hole-electron
Close.
Some carbonaceous Nano-Materials, if CNT (CNT) and Graphene (GR) are due to its efficient electronics
Receiving ability, is widely used in promoting TiO2The separation of upper photo-generated carrier and transfer.At present, TiO2-C material
The preparation method of material is based on Hydrothermal Synthesis and self-assembly method, and the material of synthesis mostly is mealy structure, due to
The problem of Powder Recovery is easily caused secondary pollution.The most generally select and form TiO at carrier surface2Thin film solves
Certainly this problem.
Compared with the carrier of planar structure, carbon fiber has high pliability and corrosion resistance and big surface area.
Additionally, TiO2The cooperative effect formed with carbon fiber can extend the light induced electron life-span to a great extent and strengthen it
Photocatalysis performance.But, current most work is to use carbon fiber to carry out TiO as raw material2Negative
Carry, be extremely difficult to good interracial contact between the two.Although it addition, water-heat process can optimize TiO2With
Interface between carbon fiber, but the TiO obtained2Major part is Rutile Type TiO2, the photocatalysis energy of this component
Power relatively Anatase TiO2Low, therefore limit TiO2The extensive application of-C composite photocatalyst material.
Summary of the invention
The technical problem existed based on background technology, the present invention proposes a kind of TiO2-C@TiO2-rGO is transparent certainly
Support thin film and its preparation method and application, the TiO in the present invention2For Anatase, prepared thin film tool
Having the preferable transparency, add the space light utilization rate of thin film of the present invention, film-based fibre of the present invention has
Sandwich layer and shell double-layer structure, its center core layer is by carbon and TiO2Formed porous fibre constituted, shell by
TiO2-rGO granular layer forms, because of the loose structure of sandwich layer, with shell while increasing material specific surface area
In TiO2Also forming good contact, contribute to the photocatalysis of material, the present invention is simple to operate, adjusts
Prosecutor just, has good market prospect in photocatalysis field.
A kind of TiO that the present invention proposes2-C@TiO2The transparent self-supporting film of-rGO, its raw material includes: titanium oxalate
Potassium, diethylene glycol, cellulose paper, graphene oxide and silane coupler.
Preferably, during silane coupler is 3-aminopropyl triethoxysilane or 3-aminopropyl trimethoxysilane
One.
The invention allows for above-mentioned TiO2-C@TiO2The preparation method of the transparent self-supporting film of-rGO, including such as
Lower step:
Prepared by S1, reaction solution: be dissolved in by titanium potassium oxalate in diethylene glycol aqueous solution and obtain solution A；
S2, hydro-thermal reaction: cellulose paper be impregnated in the solution A obtained in S1, carry out hydro-thermal reaction,
Take out reacted material, washing, it is dried to obtain material B；
S3, silane coupler modified: the material B obtained in S2 is joined in silane coupler solution, return
Stream 2-6h, takes out reacted material, and washing is dried to obtain material C；
S4, graphene oxide electrostatic self-assembled: the material C obtained in S3 be impregnated in graphene oxide water-soluble
In liquid, stand 2-6h, take out reacted material, washing, it is dried to obtain material D；
S5, carbonization: the material D that will obtain in S4, in a nitrogen atmosphere, be warming up to 400-600 DEG C, protects
Temperature 2-4h obtains TiO2-C@TiO2The transparent self-supporting film of-rGO.
Preferably, in S1, in diethylene glycol aqueous solution, the volume ratio of diethylene glycol and water is 2-3:2-3.
Preferably, in S1, the mol ratio of titanium potassium oxalate and diethylene glycol is 1:80-130.
Preferably, in S2, cellulose paper be impregnated in the solution A obtained in S1, is warming up to 130-170 DEG C,
Carry out hydro-thermal reaction 5-9h, take out reacted material, washing, it is dried to obtain material B.
Preferably, in S2, the thickness of cellulose paper is 40-50 μm.
Preferably, in S2, the weight ratio of cellulose paper and solution A is 1:300-400.
Preferably, in S3, in silane coupler solution, the volume ratio of silane coupler and solvent is 1-3:
97-99。
Preferably, in S3, the solvent in silane coupler solution is the one in toluene, ethanol or methanol.
Preferably, in S3, bulking value (g/ml) ratio of material B and silane coupler solution is 1:400-600.
Preferably, in S3, joining in silane coupler solution by the material B obtained in S2, reflux 2-6h,
Take out reacted material, wash with a kind of solvent in toluene, ethanol or methanol, be dried to obtain material C.
Preferably, in S4, in graphene oxide water solution, the concentration of graphene oxide is 0.5-1mg/ml.
Preferably, in S4, the material C obtained in S3 be impregnated in graphene oxide water solution, stand
2-6h, takes out reacted material, washes with water, is dried to obtain material D.
Preferably, in S4, bulking value (g/ml) ratio of material C and graphene oxide water solution is 1:
40-60。
The invention allows for above-mentioned TiO2-C@TiO2The transparent self-supporting film of-rGO is as visible light catalyst
Application.
Preferably, TiO2-C@TiO2The transparent self-supporting film of-rGO is as visible light catalyst degradation of methylene blue
Application.
Above-mentioned TiO2-C@TiO2In the preparation method of-rGO film, in S1, hydro-thermal reaction is technology commonly used in the art
Means.
Above-mentioned TiO2-C@TiO2In the preparation method of-rGO film, in S3, backflow is technological means commonly used in the art,
Do not specify its reflux temperature, determine its reflux temperature according to concrete operations.
Above-mentioned TiO2-C@TiO2In the preparation method of-rGO film, water is deionized water.
Graphene oxide, is called for short GO, is the oxide of Graphene.After oxidized, oxygen-containing functional group on it
Increase and make character relatively Graphene more active, can the improvement itself via the various reactions with oxygen-containing functional group
Character.
Above-mentioned TiO2-C@TiO2-rGO transparent self-supporting film fiber has sandwich layer and a shell double-layer structure, wherein,
Shell is TiO2-rGO granular layer, the TiO in shell2For spherical particle, GO covers at TiO2Spherical particle table
Face, rGO is to obtain after GO carbonizing reduction；Sandwich layer is by TiO2Uniformly penetrate into inside cellulose fibre, carbon
TiO is formed after change2-C porous fibre, C represent carbon be by after cellulose fibre carbonization obtain, cellulose paper by
Cellulose fibre is constituted；@represents TiO2-C is at TiO2Inside-rGO.
TiO in the present invention2For Anatase, prepared thin film has the preferable transparency, adds this
The space light utilization rate of invention thin film；The present invention selects titanium potassium oxalate, diethylene glycol, water and cellulose paper to enter
Row hydro-thermal reaction, the TiO that reaction generates2A part uniformly penetrates into inside cellulose fibre, forms TiO2-fine
Cellulose fiber, a part of TiO2Uniform load is at this fiber surface in the form of balls；TiO2-cellulose fibre warp
TiO is formed after carbonization2-C porous fibre, carries out TiO using carbon fiber as carrier with common2Load is formed
Film is different, and the present invention is not to carry out TiO with carbon fiber for carrier2Load, but carbon and TiO2Formation is many
Hole fiber is as the sandwich layer of self-supporting film fiber；TiO2The spherical TiO of-cellulose fiber surface2Granule is through silicon
Alkane is coupling agent modified, constitute TiO after graphene oxide electrostatic self-assembled and carbonization2-rGO granule shell；TiO2-C
Porous fibre sandwich layer, because of its loose structure, with the TiO in shell while increasing material specific surface area2Also
Form good contact；Shell is closely coated on core fibers outer surface and forms TiO2-C@TiO2-rGO is transparent certainly
Support thin film, the visible light catalytic ability of the present invention can be greatly increased so that the present invention is especially suitable for dirt
The photocatalysis treatment of dye thing；The present invention is simple to operate, and regulation and control are convenient, have good city in photocatalysis field
Field prospect.
Accompanying drawing explanation
Fig. 1 is TiO2-C@TiO2The optical photograph of the transparent self-supporting film of-rGO.
Fig. 2 is TiO2-C@TiO2The XRD figure spectrum of the transparent self-supporting film of-rGO.
Fig. 3 is TiO2-C@TiO2The displaing micro picture of the transparent self-supporting film of-rGO.
Fig. 4 is TiO2-C@TiO2The microstructure of-rGO transparent self-supporting film fiber surface.
Fig. 5 is TiO2-C@TiO2The cross-section photographs of-rGO transparent self-supporting film fiber.
Fig. 6 is TiO2-C@TiO2-rGO transparent self-supporting film Visible Light Induced Photocatalytic methylene blue curve.
Detailed description of the invention
Below, by specific embodiment, technical scheme is described in detail.
Embodiment 1
A kind of TiO2-C@TiO2The transparent self-supporting film of-rGO, its raw material includes: titanium potassium oxalate, diethylene glycol,
Cellulose paper, graphene oxide and 3-aminopropyl triethoxysilane.
Above-mentioned TiO2-C@TiO2The preparation method of the transparent self-supporting film of-rGO, comprises the steps:
Prepared by S1, reaction solution: be dissolved in by titanium potassium oxalate in diethylene glycol aqueous solution and obtain solution A；
S2, hydro-thermal reaction: cellulose paper be impregnated in the solution A obtained in S1, carry out hydro-thermal reaction,
Take out reacted material, washing, it is dried to obtain material B；
S3, silane coupler modified: the material B obtained in S2 is joined 3-aminopropyl triethoxysilane
In solution, reflux 4h, takes out reacted material, and washing is dried to obtain material C；
S4, graphene oxide electrostatic self-assembled: the material C obtained in S3 be impregnated in graphene oxide water-soluble
In liquid, stand 4h, take out reacted material, washing, it is dried to obtain material D；
S5, carbonization: the material D that will obtain in S4, under nitrogen atmosphere, be warming up to 500 DEG C, is incubated 2h
Obtain TiO2-C@TiO2The transparent self-supporting film of-rGO.
Embodiment 2
A kind of TiO2-C@TiO2The transparent self-supporting film of-rGO, its raw material includes: titanium potassium oxalate, diethylene glycol,
Cellulose paper, graphene oxide and 3-aminopropyl trimethoxysilane.
Above-mentioned TiO2-C@TiO2The preparation method of the transparent self-supporting film of-rGO, comprises the steps:
Prepared by S1, reaction solution: be dissolved in by titanium potassium oxalate in diethylene glycol aqueous solution and obtain solution A, wherein, and two
In glycol aqueous solution, the volume ratio of diethylene glycol and water be the mol ratio of 1:3, titanium potassium oxalate and diethylene glycol be 1:
80；
S2, hydro-thermal reaction: be that 50 μm cellulose papers impregnated in the solution A obtained in S1 by thickness, rise
Temperature, to 130 DEG C, carries out hydro-thermal reaction 9h, takes out reacted material, washing, is dried to obtain material B, its
In, the weight ratio of cellulose paper and solution A is 1:300；
S3, silane coupler modified: the material B obtained in S2 is joined 3-aminopropyl trimethoxysilane
In toluene solution, reflux 6h, takes out reacted material, washs with toluene, is dried to obtain material C, its
In, in 3-aminopropyl trimethoxysilane toluene solution, 3-aminopropyl trimethoxysilane and the volume of toluene
Than bulking value (g/ml) ratio for 1:99, material B and 3-aminopropyl trimethoxysilane toluene solution
For 1:400；
S4, graphene oxide electrostatic self-assembled: it is 1mg/ml that the material C obtained in S3 impregnated in concentration
In graphene oxide water solution, stand 2h, take out reacted material, wash with water, be dried to obtain material
D, wherein, bulking value (g/ml) ratio of material C and graphene oxide water solution is 1:60；
S5, carbonization: the material D that will obtain in S4, in a nitrogen atmosphere, be warming up to 400 DEG C, is incubated 4h
Obtain TiO2-C@TiO2The transparent self-supporting film of-rGO.
Embodiment 3
A kind of TiO2-C@TiO2The transparent self-supporting film of-rGO, its raw material includes: titanium potassium oxalate, diethylene glycol,
Cellulose paper, graphene oxide and 3-aminopropyl triethoxysilane.
Above-mentioned TiO2-C@TiO2The preparation method of the transparent self-supporting film of-rGO, comprises the steps:
Prepared by S1, reaction solution: be dissolved in by titanium potassium oxalate in diethylene glycol aqueous solution and obtain solution A, wherein, and two
In glycol aqueous solution, the volume ratio of diethylene glycol and water be the mol ratio of 3:2, titanium potassium oxalate and diethylene glycol be 1:
90；
S2, hydro-thermal reaction: be that 40 μm cellulose papers impregnated in the solution A obtained in S1 by thickness, rise
Temperature, to 170 DEG C, carries out hydro-thermal reaction 5h, takes out reacted material, washing, is dried to obtain material B, its
In, the weight ratio of cellulose paper and solution A is 1:400；
S3, silane coupler modified: the material B obtained in S2 is joined 3-aminopropyl triethoxysilane
In ethanol solution, reflux 2h, takes out reacted material, by washing with alcohol, is dried to obtain material C, its
In, in 3-aminopropyl triethoxysilane ethanol solution, 3-aminopropyl triethoxysilane and the volume of ethanol
Than bulking value (g/ml) ratio for 3:97, material B and 3-aminopropyl triethoxysilane ethanol solution
For 1:600；
S4, graphene oxide electrostatic self-assembled: it is 0.5mg/ml that the material C obtained in S3 impregnated in concentration
In graphene oxide water solution, stand 6h, take out reacted material, wash with water, be dried to obtain material
D, wherein, bulking value (g/ml) ratio of material C and graphene oxide water solution is 1:40；
S5, carbonization: the material D that will obtain in S4, in a nitrogen atmosphere, be warming up to 600 DEG C, is incubated 4h
Obtain TiO2-C@TiO2The transparent self-supporting film of-rGO.
Embodiment 4
A kind of TiO2-C@TiO2The transparent self-supporting film of-rGO, its raw material includes: titanium potassium oxalate, diethylene glycol,
Cellulose paper, graphene oxide and 3-aminopropyl trimethoxysilane.
Above-mentioned TiO2-C@TiO2The preparation method of the transparent self-supporting film of-rGO, comprises the steps:
Prepared by S1, reaction solution: be dissolved in by titanium potassium oxalate in diethylene glycol aqueous solution and obtain solution A, wherein, and two
In glycol aqueous solution, the volume ratio of diethylene glycol and water is that the mol ratio of 11:14, titanium potassium oxalate and diethylene glycol is
1:105；
S2, hydro-thermal reaction: be that 48 μm cellulose papers impregnated in the solution A obtained in S1 by thickness, rise
Temperature, to 140 DEG C, carries out hydro-thermal reaction 8h, takes out reacted material, washing, is dried to obtain material B, its
In, the weight ratio of cellulose paper and solution A is 1:330；
S3, silane coupler modified: the material B obtained in S2 is joined 3-aminopropyl trimethoxysilane
In methanol solution, reflux 5h, takes out reacted material, washs with methanol, is dried to obtain material C, its
In, in 3-aminopropyl trimethoxysilane methanol solution, 3-aminopropyl trimethoxysilane and the volume of methanol
Than bulking value (g/ml) ratio for 3:197, material B and 3-aminopropyl trimethoxysilane methanol solution
For 1:450；
S4, graphene oxide electrostatic self-assembled: it is 0.9mg/ml that the material C obtained in S3 impregnated in concentration
In graphene oxide water solution, stand 3h, take out reacted material, wash with water, be dried to obtain material
D, wherein, bulking value (g/ml) ratio of material C and graphene oxide water solution is 1:55；
S5, carbonization: the material D that will obtain in S4, in a nitrogen atmosphere, be warming up to 450 DEG C, is incubated 4h
Obtain TiO2-C@TiO2The transparent self-supporting film of-rGO.
Embodiment 5
A kind of TiO2-C@TiO2The transparent self-supporting film of-rGO, its raw material includes: titanium potassium oxalate, diethylene glycol,
Cellulose paper, graphene oxide and 3-aminopropyl triethoxysilane.
Above-mentioned TiO2-C@TiO2The preparation method of the transparent self-supporting film of-rGO, comprises the steps:
Prepared by S1, reaction solution: be dissolved in by titanium potassium oxalate in diethylene glycol aqueous solution and obtain solution A, wherein, and two
In glycol aqueous solution, the volume ratio of diethylene glycol and water is that the mol ratio of 14:11, titanium potassium oxalate and diethylene glycol is
1:130；
S2, hydro-thermal reaction: be that 42 μm cellulose papers impregnated in the solution A obtained in S1 by thickness, rise
Temperature, to 160 DEG C, carries out hydro-thermal reaction 6h, takes out reacted material, washing, is dried to obtain material B, its
In, the weight ratio of cellulose paper and solution A is 1:370；
S3, silane coupler modified: the material B obtained in S2 is joined 3-aminopropyl triethoxysilane
In toluene solution, reflux 3h, takes out reacted material, washs with toluene, is dried to obtain material C, its
In, in 3-aminopropyl triethoxysilane toluene solution, 3-aminopropyl triethoxysilane and the volume of toluene
Than bulking value (g/ml) ratio for 1:39, material B and 3-aminopropyl triethoxysilane toluene solution
For 1:550；
S4, graphene oxide electrostatic self-assembled: it is 0.7mg/ml that the material C obtained in S3 impregnated in concentration
In graphene oxide water solution, stand 5h, take out reacted material, wash with water, be dried to obtain material
D, wherein, bulking value (g/ml) ratio of material C and graphene oxide water solution is 1:45；
S5, carbonization: the material D that will obtain in S4, in a nitrogen atmosphere, be warming up to 550 DEG C, is incubated 2.5
H obtains TiO2-C@TiO2The transparent self-supporting film of-rGO.
Embodiment 6
A kind of TiO2-C@TiO2The transparent self-supporting film of-rGO, its raw material includes: titanium potassium oxalate, diethylene glycol,
Cellulose paper, graphene oxide and 3-aminopropyl trimethoxysilane.
Above-mentioned TiO2-C@TiO2The preparation method of the transparent self-supporting film of-rGO, comprises the steps:
Prepared by S1, reaction solution: be dissolved in by titanium potassium oxalate in diethylene glycol aqueous solution and obtain solution A, wherein, and two
In glycol aqueous solution, the volume ratio of diethylene glycol and water be the mol ratio of 1:1, titanium potassium oxalate and diethylene glycol be 1:
120；
S2, hydro-thermal reaction: be that 45 μm cellulose papers impregnated in the solution A obtained in S1 by thickness, rise
Temperature, to 150 DEG C, carries out hydro-thermal reaction 7h, takes out reacted material, washing, is dried to obtain material B, its
In, the weight ratio of cellulose paper and solution A is 1:350；
S3, silane coupler modified: the material B obtained in S2 is joined 3-aminopropyl trimethoxysilane
In ethanol solution, reflux 4h, takes out reacted material, by washing with alcohol, is dried to obtain material C, its
In, in 3-aminopropyl trimethoxysilane ethanol solution, 3-aminopropyl trimethoxysilane and the volume of ethanol
Than bulking value (g/ml) ratio for 1:49, material B and 3-aminopropyl trimethoxysilane ethanol solution
For 1:500；
S4, graphene oxide electrostatic self-assembled: it is 0.8mg/ml that the material C obtained in S3 impregnated in concentration
In graphene oxide water solution, stand 4h, take out reacted material, wash with water, be dried to obtain material
D, wherein, bulking value (g/ml) ratio of material C and graphene oxide water solution is 1:50；
S5, carbonization: the material D that will obtain in S4, in a nitrogen atmosphere, be warming up to 550 DEG C, is incubated 3h
Obtain TiO2-C@TiO2The transparent self-supporting film of-rGO.
Embodiment 7
A kind of TiO2-C@TiO2The transparent self-supporting film of-rGO, its raw material includes: titanium potassium oxalate, diethylene glycol,
Cellulose paper, graphene oxide and 3-aminopropyl triethoxysilane.
Above-mentioned TiO2-C@TiO2The preparation method of the transparent self-supporting film of-rGO, comprises the steps:
Prepared by S1, reaction solution: be dissolved in by 0.001mol titanium potassium oxalate in 20ml diethylene glycol aqueous solution and obtaining
Solution A, wherein, in diethylene glycol aqueous solution, the volume ratio of diethylene glycol and water is 1:1；
S2, hydro-thermal reaction: be that 49 μm cellulose papers impregnated in the solution A obtained in S1 by thickness, rise
Temperature, to 150 DEG C, carries out hydro-thermal reaction 6h, takes out reacted material, washing, is dried to obtain material B, its
In, the weight ratio of cellulose paper and solution A is 1:350；
S3, silane coupler modified: the material B obtained in S2 is joined 3-aminopropyl triethoxysilane
In toluene solution, reflux 4h, takes out reacted material, washs with toluene, is dried to obtain material C, its
In, in 3-aminopropyl triethoxysilane toluene solution, 3-aminopropyl triethoxysilane and the volume of toluene
Than bulking value (g/ml) ratio for 2:98, material B and 3-aminopropyl triethoxysilane toluene solution
For 1:500；
S4, graphene oxide electrostatic self-assembled: it is 0.5mg/ml that the material C obtained in S3 impregnated in concentration
In graphene oxide water solution, stand 4h, take out reacted material, wash with water, be dried to obtain material
D, wherein, bulking value (g/ml) ratio of material C and graphene oxide water solution is 1:50；
S5, carbonization: the material D that will obtain in S4, in a nitrogen atmosphere, be warming up to 500 DEG C, is incubated 2h
Obtain TiO2-C@TiO2The transparent self-supporting film of-rGO.
Detecting embodiment 7, the specific surface area obtaining embodiment 7 is 136.4m2/ g, fibre diameter is
11-12 μm, it is seen that after photoirradiation 3h, 84.1% methylene blue is degraded.
Fig. 1 is TiO2-C@TiO2The optical photograph of-rGO film, as seen from Figure 1 TiO2-C@TiO2-rGO
Film has the preferable transparency.
Fig. 2 is TiO2-C@TiO2The XRD figure spectrum of-rGO film, TiO as seen from Figure 22-C@TiO2-rGO
TiO in film2For Anatase structure.
Fig. 3 is TiO2-C@TiO2The displaing micro picture of-rGO film, as seen from Figure 3 TiO2-C@TiO2-rGO
Film intactly maintains the microstructure of cellulose paper.
Fig. 4 is TiO2-C@TiO2The microstructure on-rGO membrane fiber surface, rGO nanometer as seen from Figure 4
Sheet covers at TiO2Particle surface.
Fig. 5 is TiO2-C@TiO2The cross-section photographs of-rGO membrane fiber, as seen from Figure 5 TiO2-C@TiO2-rGO
The shell of film contacts well with sandwich layer.
Fig. 6 is TiO2-C@TiO2-rGO film Visible Light Induced Photocatalytic methylene blue curve, as seen from Figure 6
TiO2-C@TiO2-rGO film has good photocatalysis.
Embodiment 8
A kind of TiO2-C@TiO2The transparent self-supporting film of-rGO, its raw material includes: titanium potassium oxalate, diethylene glycol,
Cellulose paper, graphene oxide and 3-aminopropyl triethoxysilane.
Above-mentioned TiO2-C@TiO2The preparation method of the transparent self-supporting film of-rGO, comprises the steps:
Prepared by S1, reaction solution: be dissolved in by 0.001mol titanium potassium oxalate in 20ml diethylene glycol aqueous solution and obtaining
Solution A, wherein, in diethylene glycol aqueous solution, the volume ratio of diethylene glycol and water is 3:2；
S2, hydro-thermal reaction: be that 40 μm cellulose papers impregnated in the solution A obtained in S1 by thickness, rise
Temperature, to 150 DEG C, carries out hydro-thermal reaction 5h, takes out reacted material, washing, is dried to obtain material B, its
In, the weight ratio of cellulose paper and solution A is 1:350；
S3, silane coupler modified: the material B obtained in S2 is joined 3-aminopropyl triethoxysilane
In ethanol solution, reflux 3h, takes out reacted material, by washing with alcohol, is dried to obtain material C, its
In, in 3-aminopropyl triethoxysilane ethanol solution, 3-aminopropyl triethoxysilane and the volume of ethanol
Than bulking value (g/ml) ratio for 3:97, material B and 3-aminopropyl triethoxysilane ethanol solution
For 1:500；
S4, graphene oxide electrostatic self-assembled: it is 1mg/ml that the material C obtained in S3 impregnated in concentration
In graphene oxide water solution, stand 3h, take out reacted material, wash with water, be dried to obtain material
D, wherein, bulking value (g/ml) ratio of material C and graphene oxide water solution is 1:50；
S5, carbonization: the material D that will obtain in S4, in a nitrogen atmosphere, be warming up to 500 DEG C, is incubated 2h
Obtain TiO2-C@TiO2The transparent self-supporting film of-rGO.
Detecting embodiment 8, the specific surface area obtaining embodiment 8 is 126.8m2/ g, fibre diameter is
11-12 μm, it is seen that after photoirradiation 4h, 94.2% methylene blue is degraded.
Embodiment 9
A kind of TiO2-C@TiO2The transparent self-supporting film of-rGO, its raw material includes: titanium potassium oxalate, diethylene glycol,
Cellulose paper, graphene oxide and 3-aminopropyl trimethoxysilane.
Above-mentioned TiO2-C@TiO2The preparation method of the transparent self-supporting film of-rGO, comprises the steps:
Prepared by S1, reaction solution: be dissolved in by 0.001mol titanium potassium oxalate in 20ml diethylene glycol aqueous solution and obtaining
Solution A, wherein, in diethylene glycol aqueous solution, the volume ratio of diethylene glycol and water is 2:3；
S2, hydro-thermal reaction: be that 50 μm cellulose papers impregnated in the solution A obtained in S1 by thickness, rise
Temperature, to 150 DEG C, carries out hydro-thermal reaction 9h, takes out reacted material, washing, is dried to obtain material B, its
In, the weight ratio of cellulose paper and solution A is 1:350；
S3, silane coupler modified: the material B obtained in S2 is joined 3-aminopropyl trimethoxysilane
In methanol solution, reflux 6h, takes out reacted material, washs with methanol, is dried to obtain material C, its
In, in 3-aminopropyl trimethoxysilane methanol solution, 3-aminopropyl trimethoxysilane and the volume of methanol
Than bulking value (g/ml) ratio for 1:99, material B and 3-aminopropyl trimethoxysilane methanol solution
For 1:500；
S4, graphene oxide electrostatic self-assembled: it is 0.5mg/ml that the material C obtained in S3 impregnated in concentration
In graphene oxide water solution, stand 5h, take out reacted material, wash with water, be dried to obtain material
D, wherein, bulking value (g/ml) ratio of material C and graphene oxide water solution is 1:50；
S5, carbonization: the material D that will obtain in S4, in a nitrogen atmosphere, be warming up to 500 DEG C, is incubated 2h
Obtain TiO2-C@TiO2The transparent self-supporting film of-rGO.
Detecting embodiment 9, the specific surface area obtaining embodiment 9 is 136.8m2/ g, fibre diameter is
11-12 μm, it is seen that after photoirradiation 3h, the methylene blue of 83.2% is degraded.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention not office
Being limited to this, any those familiar with the art is in the technical scope that the invention discloses, according to this
The technical scheme of invention and inventive concept thereof in addition equivalent or change, all should contain the protection in the present invention
Within the scope of.
Claims (10)
1. a TiO2-C@TiO2The transparent self-supporting film of-rGO, it is characterised in that its raw material includes: grass
Acid titanium potassium, diethylene glycol, cellulose paper, graphene oxide and silane coupler.
TiO the most according to claim 12-C@TiO2The transparent self-supporting film of-rGO, it is characterised in that
Silane coupler is the one in 3-aminopropyl triethoxysilane or 3-aminopropyl trimethoxysilane.
3. a TiO as claimed in claim 1 or 22-C@TiO2The preparation side of the transparent self-supporting film of-rGO
Method, it is characterised in that comprise the steps:
Prepared by S1, reaction solution: be dissolved in by titanium potassium oxalate in diethylene glycol aqueous solution and obtain solution A；
S2, hydro-thermal reaction: cellulose paper be impregnated in the solution A obtained in S1, carry out hydro-thermal reaction,
Take out reacted material, washing, it is dried to obtain material B；
S3, silane coupler modified: the material B obtained in S2 is joined in silane coupler solution, return
Stream 2-6h, takes out reacted material, and washing is dried to obtain material C；
S4, graphene oxide electrostatic self-assembled: the material C obtained in S3 be impregnated in graphene oxide water-soluble
In liquid, stand 2-6h, take out reacted material, washing, it is dried to obtain material D；
S5, carbonization: the material D that will obtain in S4, in a nitrogen atmosphere, be warming up to 400-600 DEG C, protects
Temperature 2-4h obtains TiO2-C@TiO2The transparent self-supporting film of-rGO.
TiO the most according to claim 32-C@TiO2The preparation method of the transparent self-supporting film of-rGO, its
Being characterised by, in S1, in diethylene glycol aqueous solution, the volume ratio of diethylene glycol and water is 2-3:2-3.
5. according to TiO described in claim 3 or 42-C@TiO2The preparation method of the transparent self-supporting film of-rGO,
It is characterized in that, in S1, the mol ratio of titanium potassium oxalate and diethylene glycol is 1:80-130.
6. according to TiO described in any one of claim 3-52-C@TiO2The preparation of the transparent self-supporting film of-rGO
Method, it is characterised in that in S2, impregnated in cellulose paper in the solution A obtained in S1, is warming up to
130-170 DEG C, carry out hydro-thermal reaction 5-9h, take out reacted material, washing, it is dried to obtain material B.
7. according to TiO described in any one of claim 3-62-C@TiO2The preparation of the transparent self-supporting film of-rGO
Method, it is characterised in that in S2, the thickness of cellulose paper is 40-50 μm；Preferably, in S2, fine
The weight ratio of dimension element paper and solution A is 1:300-400.
8. according to TiO described in any one of claim 3-72-C@TiO2The preparation of the transparent self-supporting film of-rGO
Method, it is characterised in that in S3, in silane coupler solution, the volume ratio of silane coupler and solvent is
1-3:97-99；Preferably, in S3, the solvent in silane coupler solution is in toluene, ethanol or methanol
One；Preferably, in S3, bulking value (g/ml) ratio of material B and silane coupler solution is 1:
400-600；Preferably, in S3, the material B obtained in S2 is joined in silane coupler solution, return
Stream 2-6h, takes out reacted material, washs with a kind of solvent in toluene, ethanol or methanol, is dried
To material C.
9. according to TiO described in any one of claim 3-82-C@TiO2The preparation of the transparent self-supporting film of-rGO
Method, it is characterised in that in S4, in graphene oxide water solution, the concentration of graphene oxide is
0.5-1mg/ml；Preferably, in S4, the material C obtained in S3 be impregnated in graphene oxide water solution
In, stand 2-6h, take out reacted material, wash with water, be dried to obtain material D；Preferably, S4
In, bulking value (g/ml) ratio of material C and graphene oxide water solution is 1:40-60.
10. a TiO as claimed in claim 1 or 22-C@TiO2The transparent self-supporting film of-rGO is as visible
The application of photocatalyst；Application preferably as visible light catalyst degradation of methylene blue.
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