CN106732504A - The preparation method and application of Graphene optically catalytic TiO 2 composite - Google Patents
The preparation method and application of Graphene optically catalytic TiO 2 composite Download PDFInfo
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- CN106732504A CN106732504A CN201611218366.1A CN201611218366A CN106732504A CN 106732504 A CN106732504 A CN 106732504A CN 201611218366 A CN201611218366 A CN 201611218366A CN 106732504 A CN106732504 A CN 106732504A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 258
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 237
- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 50
- 229910010413 TiO 2 Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 305
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 204
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 129
- 239000000725 suspension Substances 0.000 claims abstract description 74
- 238000000034 method Methods 0.000 claims abstract description 56
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 239000011261 inert gas Substances 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 238000002604 ultrasonography Methods 0.000 claims abstract description 14
- 238000005119 centrifugation Methods 0.000 claims abstract description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 22
- 229910052708 sodium Inorganic materials 0.000 claims description 22
- 239000011734 sodium Substances 0.000 claims description 22
- 229910002804 graphite Inorganic materials 0.000 claims description 20
- 239000010439 graphite Substances 0.000 claims description 20
- 239000000126 substance Substances 0.000 claims description 20
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 16
- 239000010453 quartz Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 238000003786 synthesis reaction Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 150000001336 alkenes Chemical class 0.000 claims description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 5
- 239000000975 dye Substances 0.000 claims description 3
- 239000010842 industrial wastewater Substances 0.000 claims description 2
- 238000004065 wastewater treatment Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 6
- 229910003471 inorganic composite material Inorganic materials 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 description 77
- 239000000243 solution Substances 0.000 description 54
- 239000000463 material Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 9
- 238000001027 hydrothermal synthesis Methods 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 7
- 241000790917 Dioxys <bee> Species 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 230000001603 reducing effect Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- -1 deposition Substances 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- GMMZXKSNKIUKOW-UHFFFAOYSA-N [O-2].[O-2].[Ti+4].C(C)O Chemical compound [O-2].[O-2].[Ti+4].C(C)O GMMZXKSNKIUKOW-UHFFFAOYSA-N 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002109 crystal growth method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 238000007571 dilatometry Methods 0.000 description 2
- 210000004700 fetal blood Anatomy 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910001487 potassium perchlorate Inorganic materials 0.000 description 2
- 239000012286 potassium permanganate Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- VYXSBFYARXAAKO-WTKGSRSZSA-N chembl402140 Chemical compound Cl.C1=2C=C(C)C(NCC)=CC=2OC2=C\C(=N/CC)C(C)=CC2=C1C1=CC=CC=C1C(=O)OCC VYXSBFYARXAAKO-WTKGSRSZSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229960002380 dibutyl phthalate Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000008202 granule composition Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000036284 oxygen consumption Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
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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
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a kind of preparation method and application of Graphene optically catalytic TiO 2 composite, belong to inorganic composite materials technical field, comprise the following steps：Graphene oxide is dissolved in ethanol and obtains graphene oxide ethanol solution through high frequency ultrasound repeatedly, centrifugation；Graphene oxide ethanol solution is added in titanium dioxide alcohol suspending liquid, stir and help dispersed with ultrasound, graphene oxide/titanium dioxide suspension is placed in light protected environment, and continuously 20 120 minutes inert gases are passed through in graphene oxide/titanium dioxide suspension；It is placed in again under ultraviolet light environments and reacts 0.5 2 hours, obtains Graphene/titanium dioxide suspension；Graphene/titanium dioxide suspension is placed in air dry oven and is dried, it is polished to obtain Graphene/optically catalytic TiO 2 composite.The present invention has that preparation time is short, efficiency high, process is simple, it is safe and reliable the characteristics of.
Description
Technical field
It is compound the present invention relates to inorganic composite materials technical field, more particularly to a kind of Graphene optically catalytic TiO 2
The preparation method and application of material.
Background technology
Graphene is a kind of two-dimension plane structure functional material of stabilization, with very excellent electric conductivity, translucency with
And larger specific surface area, thus its outstanding light, electrical property and catalytic performance can be shown.At present, Graphene has been obtained
Extensive concern is arrived.It is combined with semiconductor nano material by by Graphene, the composite of excellent performance can be prepared.When
When obtained material is irradiated by excitation source, light induced electron can be transferred in Graphene from semiconductor grain, effectively suppression
Light induced electron processed and hole it is compound, improve the life-span in light induced electron and hole, so as to improve photocatalysis efficiency, significantly improve light
The performance of catalysis material.This composite has potentially in fields such as solar energy, electrode material of lithium battery and sewage disposals
Using.
Titanium dioxide is a kind of nontoxic semi-conducting material, because it has fabulous photoelectric conversion capacity, excellent steady
The excellent specific property such as qualitative and cheap and easy to get, makes it in photovoltaic solar cell, light-catalyzed reaction, photocatalytic degradation, sewage disposal
Had a wide range of applications Deng field, but due to its forbidden band it is wider the characteristics of, have the shortcomings that degrading activity is slower.So people
Extensive study on the modification is carried out to titanium dioxide optical catalyst, deposition, semiconductor including catalyst surface noble metal
The compound of photochemical catalyst, the ion doping of photochemical catalyst, photosensitizer and form central hole structure etc..
In recent years, the composite of Graphene titanium dioxide is occurred in that.At present, the preparation method of Graphene mainly has microcomputer
Tool stripping method, chemical vapour deposition technique, electronation graphene oxide method and solvent-thermal method etc., and Graphene titanium dioxide is multiple
The preparation method of condensation material is mainly hydro-thermal method, solvent-thermal method and thermal reduction etc., such as：
Publication No. CN 105964236A, publication date is that the Chinese patent literature of on 09 28th, 2016 discloses one kind
The preparation method of graphene/titanium dioxide photocatalyst, the Graphene/titanic oxide nano compound material is received by single-layer graphene
Rice titanium dioxide granule composition, the titanium dioxide nanoparticle is dispersed in graphenic surface, and the titanium dioxide granule is sharp
Perovskite type crystal.The patent document, is to be scattered in a certain proportion of ethanol/glacial acetic acid solution by by presoma Butyl Phthalate
In, then to its a certain amount of graphene oxide solution of addition, calcined by hydro-thermal method and Muffle furnace and Graphene/titanium dioxide is obtained
Photochemical catalyst.
Publication No. CN 103337611A, publication date is that the Chinese patent literature on October 02 in 2013 discloses one kind
The preparation method of Graphene and composite titania material, it is characterised in that comprise the following steps：1) by before containing titanium ion
Drive body to be dissolved in absolute ethyl alcohol, be configured to solution, add graphene oxide solution, titanium ion is by the surface of oxidized Graphene
Adsorb and hydrolyze, generate amorphous titanium hydroxide nanometer microparticle；The graphene oxide and titanium hydroxide that will be obtained are answered
Condensation material is deposited, dried, and obtains final product graphene oxide and amorphous titanium peroxide composite；2) in closed high-pressure hydrothermal reaction kettle
Middle addition aqueous solution, by step 1) graphene oxide that obtains and amorphous titanium peroxide composite be placed on aqueous solution
Side, carries out the reduction of graphene oxide and the crystallization of amorphous titanium peroxide, obtains final product Graphene composite titania material.The patent
Document, is that the presoma containing titanium ion is dissolved in absolute ethyl alcohol, is configured to solution, adds graphene oxide solution, is sunk
It is long-pending, dry, then be that can obtain Graphene composite titania material by hydro-thermal method.
Publication No. CN 105561963A, publication date is that the Chinese patent literature of on 05 11st, 2016 discloses one kind
The preparation method of nano titanium oxide/graphene oxide composite material, it is characterised in that comprise the following steps：By graphite oxide
Alkene solid dissolving in deionized water and absolute ethyl alcohol, ultrasonically treated 30-90min；Nano titanium oxide is subsequently adding, 1- is stirred
3h, is well mixed it and obtains suspension；Then suspension is reacted into 1-3h in 100-120 DEG C；Finally by filtering and air-dry
Regeneration obtains nano titanium oxide/graphene oxide composite material.The patent document, is that graphene oxide is dissolved in into water and second
In the mixed solution of alcohol, then nano titanium oxide is added thereto to, by stirring and thermal response, Graphene/titanium dioxide is obtained
Optic catalytic composite material.
Publication No. CN 104084186A, publication date is that the Chinese patent literature on October 08 in 2014 discloses one kind
Graphene/optically catalytic TiO 2 composite, it is characterised in that Graphene/optically catalytic TiO 2 composite is by three-dimensional
Graphene skeleton and titanium dioxide nanoparticle are constituted, and the Graphene has macroporous structure, and the titanium dioxide is mesoporous two
Titanium oxide, macropore and it is mesoporous be interconnected, the titanium dioxide nanoparticle is scattered on graphene nanometer sheet, the nanometer two
Titan oxide particles are filled in the macropore of the Graphene, and the titanium dioxide is pure anatase crystal.The patent document, will
Mix with graphene oxide ethanol solution through titania nanoparticles obtained in sol-gel process, ammonia is added after ultrasonic disperse
Water, is combined by hydro-thermal method and thermal reduction and prepares Graphene/optically catalytic TiO 2 composite.
In prior art with above-mentioned patent document as representative, when Graphene/optically catalytic TiO 2 composite is prepared,
It is mostly to be carried out by hydro-thermal method or thermal reduction, it has many defects, is mainly reflected in：
1st, the reaction condition of hydro-thermal method is usually HTHP, and technical difficulty is larger, relatively costly；
2nd, hydro-thermal method is typically to be reacted in closed container, and whole course of reaction cannot be observed, not intuitively, during synthesis
Between more long, low production efficiency；
3rd, thermal reduction typically need to the high-temperature calcination under vacuum or atmosphere of inert gases, high energy consumption, complex process, security
It is poor.
The content of the invention
A kind of defect in order to overcome above-mentioned prior art of the invention, there is provided Graphene optically catalytic TiO 2 composite
Preparation method and application, the present invention prepare Graphene/optically catalytic TiO 2 composite have to organic dyestuff it is excellent
Photocatalytic Degradation Property, sewage disposal field of Environment Protection is can be widely applied for, with preparation time is short, the letter of efficiency high, technique
Single, safe and reliable the characteristics of.
The present invention is achieved through the following technical solutions：
The preparation method of Graphene optically catalytic TiO 2 composite, it is characterised in that comprise the following steps：
A, synthesize graphene oxide using chemical method, graphene oxide is dissolved in ethanol through high frequency ultrasound repeatedly, centrifugation
Obtain graphene oxide ethanol solution；
B, titanium dioxide sample is weighed, be placed in quartz test tube, add ethanol solution, and ultrasonic disperse, obtain titanium dioxide
Titanium alcohol suspending liquid；
C, graphene oxide ethanol solution is added in titanium dioxide alcohol suspending liquid, stirs and help with ultrasonic uniform point
Dissipate, obtain graphene oxide/titanium dioxide suspension；
D, graphene oxide/titanium dioxide suspension is placed in light protected environment, and it is outstanding to graphene oxide/titanium dioxide
Continuously 20-120 minutes inert gas is passed through in turbid liquid；
E, the graphene oxide/titanium dioxide suspension that will be passed through after 20-120 minutes inert gas are placed in ultraviolet light environments
Under, reacted 0.5-2 hours in stirring and inert gas environment, obtain Graphene/titanium dioxide suspension；
F, by Graphene/titanium dioxide suspension be placed in air dry oven dry, it is polished to obtain Graphene/dioxy
Change titanium optic catalytic composite material.
In the step a, chemical method synthesis graphene oxide refers to prepare graphene oxide by Hummers methods, is obtained
Graphene oxide ethanol solution concentration be 8.2-8.8mg/ml.
In the step b, titanium dioxide sample is titania powder, and the amount of weighing is 0.7g, and ultrasonic time is 10-30 points
Clock, the concentration for obtaining titanium dioxide alcohol suspending liquid is 5-12g/L.
In the step c, the addition of graphene oxide ethanol solution is 400 μ L-8ml, and ultrasonic time is 10-30 points
Clock.
In the step d, the inert gas time is passed through for 30 points to continuous in graphene oxide/titanium dioxide suspension
Clock.
In the step e, the ultraviolet light for using is 300W high-pressure sodium lamps, and is filtered out more than 400 by ultraviolet filter
The light source of nano waveband, the light source that high-pressure sodium lamp is produced is 10cm with the distance of graphene oxide/titanium dioxide suspension.
In the step f, the temperature in air dry oven is 60-90 DEG C.
Graphene/optically catalytic TiO 2 composite, it is adaptable to the photocatalytic degradation of organic dyestuff.
Graphene/optically catalytic TiO 2 composite, it is adaptable to life and Industrial Waste Water Treatments.
Beneficial effects of the present invention are mainly manifested in following aspect：
First, the present invention, graphene oxide is synthesized first by chemical method, and graphene oxide is dissolved in ethanol through repeatedly high
Frequency ultrasound, centrifugation obtain graphene oxide ethanol solution；Then titanium dioxide sample is weighed, is placed in quartz test tube, add second
Alcoholic solution, and ultrasonic disperse, obtain titanium dioxide alcohol suspending liquid；Graphene oxide ethanol solution is added to titanium dioxide again
In alcohol suspending liquid, stir and help dispersed with ultrasound, obtain graphene oxide/titanium dioxide suspension；Stone will be aoxidized again
Black alkene/titanium dioxide suspension is placed in light protected environment, and to being continuously passed through 20- in graphene oxide/titanium dioxide suspension
120 minutes inert gases；Graphene oxide/titanium dioxide the suspension after 20-120 minutes inert gas will be passed through again is placed in purple
Under outer reticle circle border, reacted 0.5-2 hours in stirring and inert gas environment, obtain Graphene/titanium dioxide suspension；Finally
Graphene/titanium dioxide suspension is placed in air dry oven and is dried, it is polished to obtain Graphene/optically catalytic TiO 2
Composite.Wherein, by the irradiation using ultraviolet source, two in graphene oxide/titanium dioxide suspension can be activated
Titan oxide particles, it is rapid to produce the light induced electron with extremely strong reproducibility, the reduction of graphene oxide can be completed in several minutes,
Complete compound between Graphene and titanium dioxide granule simultaneously.Using specific ethanol as solvent because titanium dioxide is in purple
Outer light excites the hole (h+) with strong oxidizing property of lower generation easily compound with target product light induced electron, in the form of heat
It is useless to scatter and disappear, and hole (h+) can be by ethanol solution to capture, so as to greatly reduce its compound with light induced electron, extension
The survival duration of light induced electron.Whole preparation method, for prior art, whole preparation process is gentle, it is not necessary to which high temperature is high
The reaction environment of pressure, improves safe operation reliability；Required equipment is simple and easy to get, simple to operate, it is not necessary to any cosolvent,
Additive, catalyst, low cost, whole course of reaction are nontoxic, harmless, pollution-free, and reaction speed is fast, and generated time is short, reaction
Carried out in quartz test tube, be easy to intuitively observe；Can be prepared by ambient temperature, eliminate the environment of high temperature, it is to avoid
The agglomeration of composite, obtained Graphene/optically catalytic TiO 2 composite has splendid photocatalysis performance.
2nd, the present invention, in step a, chemical method synthesis graphene oxide refers to prepare graphite oxide by Hummers methods
Alkene, the graphene oxide ethanol solution concentration for obtaining is 8.2-8.8mg/ml, and the preparation method of current Graphene mainly has machinery
Stripping, epitaxial crystal growth method, chemical meteorology deposition method, the dilatometry of graphite oxide and reducing process.And by graphite oxidation into
Graphite oxide, obtains the graphite oxide solution of individual layer under ultrasound condition, then by electronation, it has also become prepare Graphene
Effective way.The method for oxidation of graphite mainly has Brodie methods, Staudemaier methods, Hummers methods, is with inorganic strong matter
Sub- acid (concentrated sulfuric acid and fuming nitric aicd or their mixture) treatment original graphite, graphite layers are inserted by strong acid small molecule, then
With strong oxidizer (KMnO4,KClO4Deng) it is aoxidized, the wherein Brodie methods reaction time is long, Straudemaier methods
It is more serious to graphite linings structural damage using the concentrated sulfuric acid and the mixing acid treatment graphite of fuming nitric aicd, compared to these sides
For method, graphene oxide is prepared using specific Hummers methods, it is not only simple to operate, time-consuming short and safe, lead to
Cross and the graphene oxide that Hummers methods are prepared is scattered in ethanol, the graphene oxide ethanol solution concentration for obtaining is
8.2-8.8mg/ml, with excellent stability, can Cord blood more than two months.
3rd, the present invention, in step b, titanium dioxide sample is titania powder, and the amount of weighing is 0.7g, and ultrasonic time is
10-30 minutes, the concentration of titanium dioxide alcohol suspending liquid is obtained for 5-12g/L, if configured titanium dioxide alcohol suspending liquid is dense
Degree is less than 5g/L, then or cause the titanium oxide under ultraviolet lighting be stimulated produced by light induced electron amount it is very few, it is impossible to will be follow-up
The graphene oxide of addition is reduced to Graphene in high quality, so as to cause obtained compound ratio resistance excessive, it is impossible to make
Light induced electron is separated with hole, and then improves the purpose of composite photocatalysis performance；If configured titanium dioxide ethanol
Turbid liquid concentration is higher than 12g/L, then titanium oxide can be caused superfluous, causes unnecessary waste.Hanged by by titanium dioxide ethanol
The concentration of turbid liquid is controlled to this particular range of 5-12g/L, can well balance the two, i.e.,：Both titanium oxide will not be caused
Surplus is caused to waste, and composite photocatalysis performance can be improved again.
4th, the present invention, in step c, the addition of graphene oxide ethanol solution is 400 μ L-8ml, and ultrasonic time is 10-
30 minutes, by controlling the addition of graphene oxide ethanol solution, it is capable of the quality of Effective Regulation Graphene/titanium dioxide
Than；Ultrasonic time is 10-30 minutes, and titanium dioxide can be made to be fully contacted with graphene oxide, the two is fully combined.
5th, the present invention, in step d, be to the inert gas time is continuously passed through in graphene oxide/titanium dioxide suspension
30 minutes, the light induced electron with strong reducing property that titanium oxide is produced under follow-up ultraviolet excitation was by by the dissolving in solution
Oxygen consumption, continuously inert gas is passed through 30 minutes by suspension, can effectively discharge the dissolved oxygen in suspension, so that
Lifting reduces the unwanted losses of light induced electron, makes it that graphene oxide orientation in solution is reduced into Graphene.
6th, the present invention, in step e, the ultraviolet light for using is 300W high-pressure sodium lamps, and is filtered out greatly by ultraviolet filter
In the light source of 400 nano wavebands, the light source that high-pressure sodium lamp is produced is with the distance of graphene oxide/titanium dioxide suspension
10cm, using specific 300W high-pressure sodium lamps as light source, with sufficiently large intensity of illumination, the ultraviolet luminous energy launched is very
Good is perforated through opaque Graphene titanium dioxide suspension, so as to fully activate titanium oxide therein, produces it
Substantial amounts of reactant-light induced electron；Because the energy of light source of 300W high-pressure sodium lamps is larger, the temperature liter of suspension is easily caused
Height, and etoh solvent is volatile substances, thus the light source that high-pressure sodium lamp is produced is suspended with graphene oxide/titanium dioxide
The distance controlling of liquid is 10cm, can greatly reduce heat transfer, better controls over the concentration of suspension, makes reaction more stable homogeneous
Generation.
7th, the present invention, in step f, the temperature in air dry oven is 60-90 DEG C, and Graphene/optically catalytic TiO 2 is multiple
Condensation material is nano material, and surface can be huge, and agglomeration easily occurs, and exists by by the temperature control in air dry oven
It is dried under 60-90 DEG C of lower temperature, can effectively reduces the generation of agglomeration, the further obtained Graphene of control/
The premium properties of optically catalytic TiO 2 composite.
Brief description of the drawings
Fig. 1 is Graphene/optically catalytic TiO 2 composite projection electron-microscope scanning figure prepared by the present invention；
Fig. 2 is Graphene/optically catalytic TiO 2 composite X-ray diffraction scanning figure prepared by the present invention；
Fig. 3 is Graphene/optically catalytic TiO 2 composite prepared by the present invention and pure titinium dioxide in light application time
Under to the photocatalytic degradation curve comparison figure of rhodamine 6G；
Fig. 4 is the degradation rate of Graphene/optically catalytic TiO 2 composite prepared by the present invention and pure titinium dioxide
Contrast block diagram.
Specific embodiment
Embodiment 1
The preparation method of Graphene optically catalytic TiO 2 composite, comprises the following steps：
A, synthesize graphene oxide using chemical method, graphene oxide is dissolved in ethanol through high frequency ultrasound repeatedly, centrifugation
Obtain graphene oxide ethanol solution；
B, titanium dioxide sample is weighed, be placed in quartz test tube, add ethanol solution, and ultrasonic disperse, obtain titanium dioxide
Titanium alcohol suspending liquid；
C, graphene oxide ethanol solution is added in titanium dioxide alcohol suspending liquid, stirs and help with ultrasonic uniform point
Dissipate, obtain graphene oxide/titanium dioxide suspension；
D, graphene oxide/titanium dioxide suspension is placed in light protected environment, and it is outstanding to graphene oxide/titanium dioxide
Continuously 20 minutes inert gases are passed through in turbid liquid；
E, the graphene oxide/titanium dioxide suspension that will be passed through after 20 minutes inert gases are placed under ultraviolet light environments,
Reacted 0.5 hour in stirring and inert gas environment, obtain Graphene/titanium dioxide suspension；
F, by Graphene/titanium dioxide suspension be placed in air dry oven dry, it is polished to obtain Graphene/dioxy
Change titanium optic catalytic composite material.
The present embodiment is most basic implementation method, and for prior art, whole preparation process is gentle, it is not necessary to high temperature
The reaction environment of high pressure, improves safe operation reliability；Required equipment is simple and easy to get, simple to operate, it is not necessary to any hydrotropy
Agent, additive, catalyst, low cost, whole course of reaction are nontoxic, harmless, pollution-free, and reaction speed is fast, and generated time is short, instead
Should be carried out in quartz test tube, be easy to intuitively observe；Can be prepared by ambient temperature, eliminate the environment of high temperature, it is to avoid
The agglomeration of composite, obtained Graphene/optically catalytic TiO 2 composite has splendid photocatalysis performance.
Embodiment 2
The preparation method of Graphene optically catalytic TiO 2 composite, comprises the following steps：
A, synthesize graphene oxide using chemical method, graphene oxide is dissolved in ethanol through high frequency ultrasound repeatedly, centrifugation
Obtain graphene oxide ethanol solution；
B, titanium dioxide sample is weighed, be placed in quartz test tube, add ethanol solution, and ultrasonic disperse, obtain titanium dioxide
Titanium alcohol suspending liquid；
C, graphene oxide ethanol solution is added in titanium dioxide alcohol suspending liquid, stirs and help with ultrasonic uniform point
Dissipate, obtain graphene oxide/titanium dioxide suspension；
D, graphene oxide/titanium dioxide suspension is placed in light protected environment, and it is outstanding to graphene oxide/titanium dioxide
Continuously 30 minutes inert gases are passed through in turbid liquid；
E, the graphene oxide/titanium dioxide suspension that will be passed through after 30 minutes inert gases are placed under ultraviolet light environments,
Reacted 0.8 hour in stirring and inert gas environment, obtain Graphene/titanium dioxide suspension；
F, by Graphene/titanium dioxide suspension be placed in air dry oven dry, it is polished to obtain Graphene/dioxy
Change titanium optic catalytic composite material.
In the step a, chemical method synthesis graphene oxide refers to prepare graphene oxide by Hummers methods, is obtained
Graphene oxide ethanol solution concentration be 8.2mg/ml.
In the step b, titanium dioxide sample is titania powder, and the amount of weighing is 0.7g, and ultrasonic time is 10 minutes,
The concentration for obtaining titanium dioxide alcohol suspending liquid is 5g/L.
In the step c, the addition of graphene oxide ethanol solution is 400 μ Lml, and ultrasonic time is 10 minutes.
In the step e, the ultraviolet light for using is 300W high-pressure sodium lamps, and is filtered out more than 400 by ultraviolet filter
The light source of nano waveband, the light source that high-pressure sodium lamp is produced is 10cm with the distance of graphene oxide/titanium dioxide suspension.
In the step f, the temperature in air dry oven is 60 DEG C.
The present embodiment is a better embodiment.
Embodiment 3
The preparation method of Graphene optically catalytic TiO 2 composite, comprises the following steps：
A, synthesize graphene oxide using chemical method, graphene oxide is dissolved in ethanol through high frequency ultrasound repeatedly, centrifugation
Obtain graphene oxide ethanol solution；
B, titanium dioxide sample is weighed, be placed in quartz test tube, add ethanol solution, and ultrasonic disperse, obtain titanium dioxide
Titanium alcohol suspending liquid；
C, graphene oxide ethanol solution is added in titanium dioxide alcohol suspending liquid, stirs and help with ultrasonic uniform point
Dissipate, obtain graphene oxide/titanium dioxide suspension；
D, graphene oxide/titanium dioxide suspension is placed in light protected environment, and it is outstanding to graphene oxide/titanium dioxide
Continuously 60 minutes inert gases are passed through in turbid liquid；
E, the graphene oxide/titanium dioxide suspension that will be passed through after 60 minutes inert gases are placed under ultraviolet light environments,
Reacted 1 hour in stirring and inert gas environment, obtain Graphene/titanium dioxide suspension；
F, by Graphene/titanium dioxide suspension be placed in air dry oven dry, it is polished to obtain Graphene/dioxy
Change titanium optic catalytic composite material.
In the step a, chemical method synthesis graphene oxide refers to prepare graphene oxide by Hummers methods, is obtained
Graphene oxide ethanol solution concentration be 8.4mg/ml.
In the step b, titanium dioxide sample is titania powder, and the amount of weighing is 0.7g, and ultrasonic time is 15 minutes,
The concentration for obtaining titanium dioxide alcohol suspending liquid is 7g/L.
In the step c, the addition of graphene oxide ethanol solution is 1ml, and ultrasonic time is 15 minutes.
In the step e, the ultraviolet light for using is 300W high-pressure sodium lamps, and is filtered out more than 400 by ultraviolet filter
The light source of nano waveband, the light source that high-pressure sodium lamp is produced is 10cm with the distance of graphene oxide/titanium dioxide suspension.
In the step f, the temperature in air dry oven is 70 DEG C.
The present embodiment is another better embodiment.
Embodiment 4
The preparation method of Graphene optically catalytic TiO 2 composite, comprises the following steps：
A, synthesize graphene oxide using chemical method, graphene oxide is dissolved in ethanol through high frequency ultrasound repeatedly, centrifugation
Obtain graphene oxide ethanol solution；
B, titanium dioxide sample is weighed, be placed in quartz test tube, add ethanol solution, and ultrasonic disperse, obtain titanium dioxide
Titanium alcohol suspending liquid；
C, graphene oxide ethanol solution is added in titanium dioxide alcohol suspending liquid, stirs and help with ultrasonic uniform point
Dissipate, obtain graphene oxide/titanium dioxide suspension；
D, graphene oxide/titanium dioxide suspension is placed in light protected environment, and it is outstanding to graphene oxide/titanium dioxide
Continuously 80 minutes inert gases are passed through in turbid liquid；
E, the graphene oxide/titanium dioxide suspension that will be passed through after 80 minutes inert gases are placed under ultraviolet light environments,
Reacted 1.5 hours in stirring and inert gas environment, obtain Graphene/titanium dioxide suspension；
F, by Graphene/titanium dioxide suspension be placed in air dry oven dry, it is polished to obtain Graphene/dioxy
Change titanium optic catalytic composite material.
In the step a, chemical method synthesis graphene oxide refers to prepare graphene oxide by Hummers methods, is obtained
Graphene oxide ethanol solution concentration be 8.6mg/ml.
In the step b, titanium dioxide sample is titania powder, and the amount of weighing is 0.7g, and ultrasonic time is 25 minutes,
The concentration for obtaining titanium dioxide alcohol suspending liquid is 9g/L.
In the step c, the addition of graphene oxide ethanol solution is 400 μ L-8ml, and ultrasonic time is 25 minutes.
In the step e, the ultraviolet light for using is 300W high-pressure sodium lamps, and is filtered out more than 400 by ultraviolet filter
The light source of nano waveband, the light source that high-pressure sodium lamp is produced is 10cm with the distance of graphene oxide/titanium dioxide suspension.
In the step f, the temperature in air dry oven is 80 DEG C.
The present embodiment is another better embodiment.
Embodiment 5
The preparation method of Graphene optically catalytic TiO 2 composite, comprises the following steps：
A, synthesize graphene oxide using chemical method, graphene oxide is dissolved in ethanol through high frequency ultrasound repeatedly, centrifugation
Obtain graphene oxide ethanol solution；
B, titanium dioxide sample is weighed, be placed in quartz test tube, add ethanol solution, and ultrasonic disperse, obtain titanium dioxide
Titanium alcohol suspending liquid；
C, graphene oxide ethanol solution is added in titanium dioxide alcohol suspending liquid, stirs and help with ultrasonic uniform point
Dissipate, obtain graphene oxide/titanium dioxide suspension；
D, graphene oxide/titanium dioxide suspension is placed in light protected environment, and it is outstanding to graphene oxide/titanium dioxide
Continuously 120 minutes inert gases are passed through in turbid liquid；
E, the graphene oxide/titanium dioxide suspension that will be passed through after 120 minutes inert gases are placed under ultraviolet light environments,
Reacted 2 hours in stirring and inert gas environment, obtain Graphene/titanium dioxide suspension；
F, by Graphene/titanium dioxide suspension be placed in air dry oven dry, it is polished to obtain Graphene/dioxy
Change titanium optic catalytic composite material.
In the step a, chemical method synthesis graphene oxide refers to prepare graphene oxide by Hummers methods, is obtained
Graphene oxide ethanol solution concentration be 8.8mg/ml.
In the step b, titanium dioxide sample is titania powder, and the amount of weighing is 0.7g, and ultrasonic time is 30 minutes,
The concentration for obtaining titanium dioxide alcohol suspending liquid is 12g/L.
In the step c, the addition of graphene oxide ethanol solution is 8ml, and ultrasonic time is 30 minutes.
In the step d, the inert gas time is passed through for 30 points to continuous in graphene oxide/titanium dioxide suspension
Clock.
In the step e, the ultraviolet light for using is 300W high-pressure sodium lamps, and is filtered out more than 400 by ultraviolet filter
The light source of nano waveband, the light source that high-pressure sodium lamp is produced is 10cm with the distance of graphene oxide/titanium dioxide suspension.
In the step f, the temperature in air dry oven is 90 DEG C.
The present embodiment is preferred forms, and in step a, chemical method synthesis graphene oxide refers to by Hummers methods
Graphene oxide is prepared, the graphene oxide ethanol solution concentration for obtaining is 8.8mg/ml, the preparation method master of current Graphene
There are mechanical stripping, epitaxial crystal growth method, chemical meteorology deposition method, the dilatometry of graphite oxide and reducing process.And by stone
Ink is oxidized to graphite oxide, and the graphite oxide solution of individual layer is obtained under ultrasound condition, then by electronation, it has also become prepare
The effective way of Graphene.The method for oxidation of graphite mainly has Brodie methods, Staudemaier methods, Hummers methods, is to use
Inorganic strong protonic acid (concentrated sulfuric acid and fuming nitric aicd or their mixture) processes original graphite, and strong acid small molecule is inserted into graphite
Interlayer, then with strong oxidizer (KMnO4,KClO4Deng) it is aoxidized, the wherein Brodie methods reaction time is long,
Straudemaier methods are more tight to graphite linings structural damage using the concentrated sulfuric acid and the mixing acid treatment graphite of fuming nitric aicd
Again, for compared to these methods, graphene oxide is prepared using specific Hummers methods, it is not only simple to operate, time-consuming short,
And it is safe, it is scattered in ethanol by by the graphene oxide that Hummers methods are prepared, the graphene oxide for obtaining
Ethanol solution concentration is 8.8mg/ml, with excellent stability, can Cord blood more than two months.In step b, titanium dioxide
Sample is titania powder, and the amount of weighing is 0.7g, and ultrasonic time is 30 minutes, obtains the concentration of titanium dioxide alcohol suspending liquid
It is 12g/L, if configured titanium dioxide alcohol suspending liquid concentration is less than 5g/L, or causes the titanium oxide under ultraviolet lighting to be excited
Light induced electron amount produced by hair is very few, it is impossible to which the follow-up graphene oxide for adding is reduced into Graphene in high quality, so that
Cause obtained compound ratio resistance excessive, it is impossible to light induced electron is separated with hole, and then improve composite light
The purpose of catalytic performance；If configured titanium dioxide alcohol suspending liquid concentration is higher than 12g/L, titanium oxide can be caused superfluous, led
Cause unnecessary waste.12g/L is controlled to by by the concentration of titanium dioxide alcohol suspending liquid, can be flat well by the two
Weighing apparatus, i.e.,：Both titanium oxide surplus will not have been caused to cause to waste, composite photocatalysis performance can have been improved again.In step c, oxidation
The addition of Graphene ethanol solution is 8ml, and ultrasonic time is 30 minutes, by the addition for controlling graphene oxide ethanol solution
Amount, the mass ratio of energy Effective Regulation Graphene/titanium dioxide；Ultrasonic time is 30 minutes, can make titanium dioxide with oxidation stone
Black alkene is fully contacted, and the two is fully combined.In step d, to being continuously passed through in graphene oxide/titanium dioxide suspension
The inert gas time is 30 minutes, and the light induced electron with strong reducing property that titanium oxide is produced under follow-up ultraviolet excitation will
By the dissolved oxygen depletion in solution, continuously inert gas is passed through 30 minutes by suspension, can effectively discharge suspension
In dissolved oxygen so that lifted reduce light induced electron unwanted losses, make its by solution graphene oxide orientation be reduced to
Graphene.In step e, the ultraviolet light for using is 300W high-pressure sodium lamps, and is filtered out more than 400 nanometer waves by ultraviolet filter
The light source of section, the light source that high-pressure sodium lamp is produced is 10cm with the distance of graphene oxide/titanium dioxide suspension, using specific
Used as light source, with sufficiently large intensity of illumination, the ultraviolet luminous energy launched is perforated through impermeable 300W high-pressure sodium lamps well
Bright Graphene titanium dioxide suspension, so as to fully activate titanium oxide therein, makes it produce substantial amounts of reactant-light
Raw electronics；Because the energy of light source of 300W high-pressure sodium lamps is larger, the temperature for being easily caused suspension is raised, and etoh solvent is
Volatile substances, thus be with the distance controlling of graphene oxide/titanium dioxide suspension by the light source that high-pressure sodium lamp is produced
10cm, can greatly reduce heat transfer, better control over the concentration of suspension, make the generation of reaction more stable homogeneous.Step f
In, the temperature in air dry oven is 90 DEG C, and Graphene/optically catalytic TiO 2 composite is nano material, and surface can be huge
Greatly, easily there is agglomeration, be dried under 90 DEG C of lower temperatures by by the temperature control in air dry oven, can
The generation of agglomeration is effectively reduced, further the Optimality of the obtained Graphene/optically catalytic TiO 2 composite of control
Energy.
The present invention prepares the contrast such as table 1 below of Graphene/optically catalytic TiO 2 composite compared with art methods：
Table 1
As it can be seen from table 1 the present invention is compared with publication number CN 105964236A, CN 103337611A, CN 105561963A
And for CN 104084186A, with preparation time is short, efficiency high, process is simple, it is safe and reliable the characteristics of.
Claims (9)
1. the preparation method of Graphene optically catalytic TiO 2 composite, it is characterised in that comprise the following steps：
A, synthesize graphene oxide using chemical method, graphene oxide is dissolved in ethanol and is obtained through high frequency ultrasound repeatedly, centrifugation
Graphene oxide ethanol solution；
B, titanium dioxide sample is weighed, be placed in quartz test tube, add ethanol solution, and ultrasonic disperse, obtain titanium dioxide second
Alcohol suspension；
C, graphene oxide ethanol solution is added in titanium dioxide alcohol suspending liquid, stirs and help dispersed with ultrasound,
Obtain graphene oxide/titanium dioxide suspension；
D, graphene oxide/titanium dioxide suspension is placed in light protected environment, and to graphene oxide/titanium dioxide suspension
In be continuously passed through 20-120 minutes inert gas；
E, the graphene oxide/titanium dioxide suspension that will be passed through after 20-120 minutes inert gas are placed under ultraviolet light environments,
Reacted 0.5-2 hours in stirring and inert gas environment, obtain Graphene/titanium dioxide suspension；
F, by Graphene/titanium dioxide suspension be placed in air dry oven dry, it is polished to obtain Graphene/titanium dioxide
Optic catalytic composite material.
2. the preparation method of Graphene optically catalytic TiO 2 composite according to claim 1, it is characterised in that：Institute
State in step a, chemical method synthesis graphene oxide refers to prepare graphene oxide by Hummers methods, the graphite oxide for obtaining
Alkene ethanol solution concentration is 8.2-8.8mg/ml.
3. the preparation method of Graphene optically catalytic TiO 2 composite according to claim 1, it is characterised in that：Institute
State in step b, titanium dioxide sample is titania powder, the amount of weighing is 0.7g, and ultrasonic time is 10-30 minutes, obtains two
The concentration of titanium oxide alcohol suspending liquid is 5-12g/L.
4. the preparation method of Graphene optically catalytic TiO 2 composite according to claim 1, it is characterised in that：Institute
State in step c, the addition of graphene oxide ethanol solution is 400 μ L-8ml, and ultrasonic time is 10-30 minutes.
5. the preparation method of Graphene optically catalytic TiO 2 composite according to claim 1, it is characterised in that：Institute
State in step d, the inert gas time is passed through for 30 minutes to continuous in graphene oxide/titanium dioxide suspension.
6. the preparation method of Graphene optically catalytic TiO 2 composite according to claim 1, it is characterised in that：Institute
State in step e, the ultraviolet light for using is 300W high-pressure sodium lamps, and is filtered out more than 400 nano wavebands by ultraviolet filter
Light source, the light source that high-pressure sodium lamp is produced is 10cm with the distance of graphene oxide/titanium dioxide suspension.
7. the preparation method of Graphene optically catalytic TiO 2 composite according to claim 1, it is characterised in that：Institute
State in step f, the temperature in air dry oven is 60-90 DEG C.
8. the application of Graphene according to claim 1 and optically catalytic TiO 2 composite, it is characterised in that：It is applicable
In the photocatalytic degradation of organic dyestuff.
9. the application of Graphene according to claim 1 and optically catalytic TiO 2 composite, it is characterised in that：It is applicable
In life and Industrial Waste Water Treatments.
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| CN107469772A (en) * | 2017-10-13 | 2017-12-15 | 山东理工大学 | A kind of method of heavy metal classes incretion interferent in removal reverse osmosis concentrated water |
| CN108640214A (en) * | 2018-05-31 | 2018-10-12 | 江苏理工学院 | One kind having photocatalysis performance seperation film and preparation method thereof |
| CN109290064A (en) * | 2018-09-20 | 2019-02-01 | 东北大学秦皇岛分校 | A kind of preparation method of the compound self-degradation flocculant of graphene/titanium dioxide/polyacrylamide |
| CN109482239A (en) * | 2018-11-23 | 2019-03-19 | 宁波石墨烯创新中心有限公司 | Graphene catalysis material, preparation process and application |
| CN109651860A (en) * | 2018-12-24 | 2019-04-19 | 湖北航天化学技术研究所 | A kind of graphene/nanometer titanium dioxide composite material and preparation method and application |
| CN113756135A (en) * | 2021-08-25 | 2021-12-07 | 重庆纤维研究设计院股份有限公司 | TiO 22Preparation method of photocatalyst filter paper |
| CN115449278A (en) * | 2022-10-20 | 2022-12-09 | 沈阳大学 | Graphene-loaded titanium dioxide composite anticorrosive paint and preparation method thereof |
| CN116216703A (en) * | 2023-03-09 | 2023-06-06 | 上海集成电路装备材料产业创新中心有限公司 | Patterning device and method based on atomic force microscope |
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| CN107469772A (en) * | 2017-10-13 | 2017-12-15 | 山东理工大学 | A kind of method of heavy metal classes incretion interferent in removal reverse osmosis concentrated water |
| CN108640214A (en) * | 2018-05-31 | 2018-10-12 | 江苏理工学院 | One kind having photocatalysis performance seperation film and preparation method thereof |
| CN109290064A (en) * | 2018-09-20 | 2019-02-01 | 东北大学秦皇岛分校 | A kind of preparation method of the compound self-degradation flocculant of graphene/titanium dioxide/polyacrylamide |
| CN109290064B (en) * | 2018-09-20 | 2020-10-20 | 东北大学秦皇岛分校 | Preparation method of graphene/titanium dioxide/polyacrylamide composite self-degradation flocculant |
| CN109482239A (en) * | 2018-11-23 | 2019-03-19 | 宁波石墨烯创新中心有限公司 | Graphene catalysis material, preparation process and application |
| CN109651860A (en) * | 2018-12-24 | 2019-04-19 | 湖北航天化学技术研究所 | A kind of graphene/nanometer titanium dioxide composite material and preparation method and application |
| CN109651860B (en) * | 2018-12-24 | 2021-06-11 | 湖北航天化学技术研究所 | Graphene/nano titanium dioxide composite material and preparation method and application thereof |
| CN113756135A (en) * | 2021-08-25 | 2021-12-07 | 重庆纤维研究设计院股份有限公司 | TiO 22Preparation method of photocatalyst filter paper |
| CN115449278A (en) * | 2022-10-20 | 2022-12-09 | 沈阳大学 | Graphene-loaded titanium dioxide composite anticorrosive paint and preparation method thereof |
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Application publication date: 20170531 |