CN109985614A - A kind of TiO2/ graphene composite photocatalyst and preparation method thereof - Google Patents
A kind of TiO2/ graphene composite photocatalyst and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 65
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 55
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 35
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011259 mixed solution Substances 0.000 claims abstract description 23
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 17
- 239000010439 graphite Substances 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 17
- NMGYKLMMQCTUGI-UHFFFAOYSA-J diazanium;titanium(4+);hexafluoride Chemical compound [NH4+].[NH4+].[F-].[F-].[F-].[F-].[F-].[F-].[Ti+4] NMGYKLMMQCTUGI-UHFFFAOYSA-J 0.000 claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 235000019441 ethanol Nutrition 0.000 claims abstract description 14
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004327 boric acid Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 12
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000376 reactant Substances 0.000 abstract description 2
- 239000002344 surface layer Substances 0.000 abstract description 2
- 229910052719 titanium Inorganic materials 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 17
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 5
- 229940043267 rhodamine b Drugs 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- -1 graphite Alkene Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
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- 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
- C02F2101/34—Organic compounds containing oxygen
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- 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
- C02F2101/36—Organic compounds containing halogen
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- 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
- C02F2101/38—Organic compounds containing nitrogen
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- 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
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Abstract
The present invention relates to a kind of TiO2/ graphene composite photocatalyst and preparation method thereof, this method include weighing graphite oxide to be dissolved in ethyl alcohol;Then obtained solution is placed in supersonic wave cleaning machine after handling, adds aqueous isopropanol;Ammonium titanium fluoride and boric acid mixed solution are added, and is stirred;Then the mixed solution of acquisition is moved into the polytetrafluoroethyllining lining of autoclave, carries out hydro-thermal reaction;Finally reacted product is washed, is drying to obtain TiO2/ graphene composite photocatalyst.The selection of titanium source is ammonium titanium fluoride in this method, and reactant loads to graphene surface layer in a manner of hydro-thermal method, and gradually forming core is grown up on the surface, can there is better dispersion;In addition this method makes TiO2It is close compound between graphene, photocatalytic activity is improved, forbidden bandwidth is shortened, effectively improves photocatalytic degradation efficiency.
Description
Technical field
The present invention relates to photocatalysis technology, in particular to a kind of TiO2/ graphene composite photocatalyst and its preparation side.
Background technique
In recent years, with the continuous improvement of China's national life level, process of industrialization deepens continuously, in organic wastewater
Toxic persistent organic pollutants be processed into for problem very important in China's environmental improvement.Domestic enterprise is most at present
Organic wastewater is handled using biological denitrification process, but the indices being discharged, especially organic pollutants are difficult to reach one
Grade discharge standard, therefore, the advanced treating for implementing organic wastewater becomes development trend.
Photocatalysis technology is as a kind of novel green high-level oxidation technology, because its reaction condition is mild, contaminant degradation
Thoroughly, the advantages that without secondary pollution, shows great application prospect in Organic Waste Water Treatment field.Titanium dioxide
(TiO2) because of the advantages that its is cheap and easy to get, chemical property is stable, photocatalysis efficiency is high, become most widely used photocatalysis
Agent.But pure TiO2Forbidden bandwidth it is larger, it is poor to the response of visible light, in Photocatalytic Degradation Process, light induced electron-sky
The recombination rate in cave is fast, and the quantum efficiency of light-catalyzed reaction is lower.It is stranded in addition, titania powder recycles in solid-liquid system
The disadvantage of difficulty, reusable property difference significantly limits TiO2The application of photochemical catalyst.It can be seen that photochemical catalyst is in reality
There are still many problems in, and many researchers have done a lot of research work to this and developed plan in photocatalysis field at present
Slightly solve the above problems.
Summary of the invention
In view of the above-mentioned problems existing in the prior art, the object of the present invention is to provide a kind of TiO2/ graphene complex light is urged
Agent and its preparation side, the catalyst have the performances such as high catalytic efficiency, high stability.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of TiO2The preparation method of/graphene composite photocatalyst, includes the following steps:
S1: it weighs graphite oxide and is dissolved in ethyl alcohol;
S2: the solution that S1 is obtained is placed in supersonic wave cleaning machine after processing, adds aqueous isopropanol;
S3: into the mixed solution that S2 is obtained, ammonium titanium fluoride and boric acid mixed solution are added, and stir;
S4: the mixed solution that S3 is obtained moves into the polytetrafluoroethyllining lining of autoclave, carries out hydro-thermal reaction;
S5: reacted product is washed, is drying to obtain TiO2/ graphene composite photocatalyst.
Preferably, TiO2The preparation method of/graphene composite photocatalyst, includes the following steps:
S1: it weighs graphite oxide and is dissolved in ethyl alcohol;
S2: the solution that S1 is obtained is placed in supersonic wave cleaning machine, and after being ultrasonically treated 30 ~ 120 min, aqueous isopropanol is added,
Wherein, the ratio between the quality of graphite oxide, the volume of ethyl alcohol and volume of isopropanol are as follows: 10 ~ 50mg: 10 ~ 25mL: 5 ~ 15mL;
S3: again into the mixed solution that S2 is obtained, 25 mL of ammonium titanium fluoride and boric acid mixed solution that molar ratio is 1:3, institute is added
The concentration for stating ammonium titanium fluoride is 0.05 mol/L, and stirs 1h;
S4: the mixed solution that S3 is obtained moves into the polytetrafluoroethyllining lining of autoclave, carries out hydro-thermal reaction;
In the reaction process, temperature condition is 100 ~ 150oC, hydro-thermal reaction 16 ~ for 24 hours;
S5: reacted product is washed, is drying to obtain TiO2/ graphene composite photocatalyst.
As a further preference, preferably, TiO2The preparation method of/graphene composite photocatalyst, including it is as follows
Step:
S1: it weighs graphite oxide and is dissolved in ethyl alcohol;
S2: the solution that S1 is obtained is placed in supersonic wave cleaning machine, and after being ultrasonically treated 30 min, aqueous isopropanol is added;
Wherein, the ratio between the quality of graphite oxide, the volume of ethyl alcohol and volume of isopropanol are as follows: 50mg: 10mL: 10mL;
S3: again into the mixed solution that S2 is obtained, 25 mL of ammonium titanium fluoride and boric acid mixed solution that molar ratio is 1:3, institute is added
The concentration for stating ammonium titanium fluoride is 0.05 mol/L, and stirs 1h;
S4: the mixed solution that S3 is obtained moves into the polytetrafluoroethyllining lining of autoclave, carries out hydro-thermal reaction;
In the reaction process, temperature condition is 140oC, hydro-thermal reaction 16h;
S5: reacted product is washed, is drying to obtain TiO2/ graphene composite photocatalyst.
A kind of TiO2/ graphene composite photocatalyst prepares gained, the TiO using the above method2/ graphene complex light
Graphene content 9% ~ 33% in catalyst.
Compared with the existing technology, the present invention at least has the advantages that
1, the selection of titanium source is ammonium titanium fluoride when the method for the present invention prepares catalyst, and reactant loads to stone in a manner of hydro-thermal method
Black alkene surface layer, gradually forming core is grown up on the surface, can there is better dispersion.
2, the method for the present invention makes TiO2It is close compound between graphene, improve photocatalytic activity, shorten forbidden bandwidth,
Effectively improve photocatalytic degradation efficiency.
3, the catalyst environmental protection that the present invention obtains is simple, does not introduce other additives, will not generate too much not to environment
Benefit influences, and does not generate by-product.
4, the catalyst that the present invention obtains has preferable photocatalytic degradation effect, and the catalyst being prepared is in 5min
Just there is 82% degradation rate, may be up to 98% in the degradation rate of 25 min.
Detailed description of the invention
Fig. 1 is TiO of the invention2/ graphene photo-catalyst rhodamine B degradation solution curve.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Titanium dichloride load is a kind of effective solution means on the basis material of high-specific surface area by the method for the present invention.
Graphene is as a kind of specific surface area with superelevation (up to 2600 m2/ g) two-dimensional surface material, be one good multiple
The substrate of condensation material.Meanwhile graphene also has excellent electrical properties, a good electron acceptor can be by photoproduction electricity
Son cracking is transmitted to surface, it is suppressed that electron-hole it is compound.
The TiO of claimed preparation2The method of/graphene composite photocatalyst, it is also necessary to which protection passes through the party
The product of method preparation, i.e. TiO2/ graphene composite photocatalyst.
A kind of embodiment 1: TiO2The preparation method of/graphene composite photocatalyst, TiO2For main active component, graphite
Alkene is as catalyst carrier, and graphene content is 10 mg.
Its preparation process the following steps are included:
Ultrasound 30min in 10 mL ethyl alcohol is added in the graphite oxide of 10 mg;Then 10 mL aqueous isopropanols are added, and stir
1 h;
The ammonium titanium fluoride (0.05 mol/L) and 25 mL of boric acid mixed solution that molar ratio is 1:3 are added later, stir 1 h;It will
Acquired solution moves into autoclave and carries out hydro-thermal reaction, 120o20 h are reacted under the conditions of C, finally by reacted product
Washed, drying to obtain TiO2/ graphene composite photocatalyst.
By measurement, TiO2Graphene content is 9% in/graphene composite photocatalyst.
A kind of embodiment 2: TiO2The preparation method of/graphene composite photocatalyst, TiO2For main active component, graphite
Alkene is as catalyst carrier, and graphene content is 30 mg.
Its preparation process the following steps are included:
Ultrasound 30min in 10 mL ethyl alcohol is added in the graphite oxide of 30 mg;Then 10 mL aqueous isopropanols are added, and stir 1
h;The ammonium titanium fluoride (0.05 mol/L) and 25 mL of boric acid mixed solution that molar ratio is 1:3 are added later, stir 1 h;By institute
It obtains in solution immigration autoclave and carries out hydro-thermal reaction, 140o20 h are reacted under the conditions of C, finally pass through reacted product
Washing, drying to obtain TiO2/ graphene composite photocatalyst.
By measurement, TiO2Graphene content is 23% in/graphene composite photocatalyst.
A kind of embodiment 3: TiO2The preparation method of/graphene composite photocatalyst, TiO2For main active component, graphite
Alkene is as catalyst carrier, and graphene content is 50 mg.
Its preparation process the following steps are included:
Ultrasound 30min in 10 mL ethyl alcohol is added in the graphite oxide of 50 mg;Then 10 mL aqueous isopropanols are added, and stir 1
h;The ammonium titanium fluoride (0.05 mol/L) and 25 mL of boric acid mixed solution that molar ratio is 1:3 are added later, stir 1 h;By institute
It obtains in solution immigration autoclave and carries out hydro-thermal reaction, 140o16h is reacted under the conditions of C, finally passes through reacted product
Washing, drying to obtain TiO2/ graphene composite photocatalyst.
By measurement, TiO2Graphene content is 33% in/graphene composite photocatalyst.
Catalyst performance evaluation
The catalyst for taking example 1 ~ 3 to prepare respectively, and the business TiO of purchase2Catalyst amounts to 4 samples, takes 10mg respectively
Prepared photochemical catalyst is added in the rhodamine B solution of 10 mg/L of 50 mL, puts it into dark field and secretly adsorbs 30 min, reaches
It is balanced to De contamination;Sampling is primary at this time;25 min of ultraviolet lamp illumination radiation suspension is reused, every 5 min sampling is primary,
3 min are centrifuged using 5500 r/min of centrifuge, 3 mL of Aspirate supernatant is put into quartz cell, using UV-vis spectroscopy light
Degree meter obtains the concentration of rhodamine B in supernatant to measure the absorption spectrum of the solution.After experiment, different hydrothermal conditions are to light
Fig. 1 is shown in the influence of catalytic effect.
In Fig. 1, abscissa is reaction time, the ratio of concentration and initial concentration that ordinate is inscribed when being a certain.
As seen from the figure, compared to individual TiO2, TiO prepared by the present invention2The photocatalysis of/graphene composite photocatalyst
Effect, which has, to be obviously improved, and is better than pure TiO to the degradation effect of rhodamine B solution2(control group degradation efficiency is only sample
74.6%) the final efficiency for the catalyst sample that, example 1 ~ 3 obtains has respectively reached 98.2%, 98.8%, 96.7%.It is reacting
In 5min to 10min this period, rate of catalysis reaction has rapid growth, the reaction speed for the catalyst that wherein example 3 obtains
Rate is most fast.
Can also take as following formula with control condition TiO2/ graphene composite photocatalyst is implemented referring specifically to table 1
TiO is prepared in example 4-102The method of/graphene composite photocatalyst is identical as 1-3 is implemented, and obstructed place is only that each step
In parameter selection.
Table 1
It is tested through photocatalysis performance, the results showed that the TiO obtained under hydrothermal condition within the above range2/ graphene complex light is urged
Agent is to the degradation effect of rhodamine B solution compared to business TiO2, have certain promotion, this is attributed to TiO2In graphene table
Forming core is grown up on face, can have better dispersion, and make TiO2The chemical bond formd between graphene, the two contact area
It is bigger, it improves photocatalytic activity, shorten forbidden bandwidth;This also illustrates when graphene content is 9% ~ 33%, graphene
Presence can effectively improve photocatalytic degradation efficiency.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the scope of the claims of invention.
Claims (4)
1. a kind of TiO2The preparation method of/graphene composite photocatalyst, which comprises the steps of:
S1: it weighs graphite oxide and is dissolved in ethyl alcohol;
S2: the solution that S1 is obtained is placed in supersonic wave cleaning machine after processing, adds aqueous isopropanol;
S3: into the mixed solution that S2 is obtained, ammonium titanium fluoride and boric acid mixed solution are added, and stir;
S4: the mixed solution that S3 is obtained moves into the polytetrafluoroethyllining lining of autoclave, carries out hydro-thermal reaction;
S5: reacted product is washed, is drying to obtain TiO2/ graphene composite photocatalyst.
2. TiO as described in claim 12The preparation method of/graphene composite photocatalyst, it is characterised in that:
S1: it weighs graphite oxide and is dissolved in ethyl alcohol;
S2: the solution that S1 is obtained is placed in supersonic wave cleaning machine, and after being ultrasonically treated 30 ~ 120 min, aqueous isopropanol is added,
Wherein, the ratio between the quality of graphite oxide, the volume of ethyl alcohol and volume of isopropanol are as follows: 10 ~ 50mg: 10 ~ 25mL: 5 ~ 15mL;
S3: again into the mixed solution that S2 is obtained, 25 mL of ammonium titanium fluoride and boric acid mixed solution that molar ratio is 1:3, institute is added
The concentration for stating ammonium titanium fluoride is 0.05 mol/L, and stirs 1h;
S4: the mixed solution that S3 is obtained moves into the polytetrafluoroethyllining lining of autoclave, carries out hydro-thermal reaction;
In the reaction process, temperature condition is 100 ~ 150oC, hydro-thermal reaction 16 ~ for 24 hours;
S5: reacted product is washed, is drying to obtain TiO2/ graphene composite photocatalyst.
3. TiO as claimed in claim 22The preparation method of/graphene composite photocatalyst, it is characterised in that: including walking as follows
It is rapid:
S1: it weighs graphite oxide and is dissolved in ethyl alcohol;
S2: the solution that S1 is obtained is placed in supersonic wave cleaning machine, and after being ultrasonically treated 30 min, aqueous isopropanol is added;
Wherein, the ratio between the quality of graphite oxide, the volume of ethyl alcohol and volume of isopropanol are as follows: 50mg: 10mL: 10mL;
S3: again into the mixed solution that S2 is obtained, 25 mL of ammonium titanium fluoride and boric acid mixed solution that molar ratio is 1:3, institute is added
The concentration for stating ammonium titanium fluoride is 0.05 mol/L, and stirs 1h;
S4: the mixed solution that S3 is obtained moves into the polytetrafluoroethyllining lining of autoclave, carries out hydro-thermal reaction;
In the reaction process, temperature condition is 140oC, hydro-thermal reaction 16h;
S5: reacted product is washed, is drying to obtain TiO2/ graphene composite photocatalyst.
4. a kind of TiO2/ graphene composite photocatalyst, which is characterized in that institute is prepared using the method for claims 1 or 2 or 3
, the TiO2Graphene content 9% ~ 33% in/graphene composite photocatalyst.
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CN102728337A (en) * | 2012-06-08 | 2012-10-17 | 华北电力大学 | Graphite / titanium dioxide composite material and preparation method thereof |
CN108212160A (en) * | 2018-02-05 | 2018-06-29 | 北京欧美中科学技术研究院 | A kind of preparation method of the magnetic oxygenated graphene composite material of photocatalytic degradation |
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US20020147108A1 (en) * | 1997-12-18 | 2002-10-10 | Koji Sato | Methods for producing oxides or composites thereof |
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