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 PDF

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CN109985614A
CN109985614A CN201910305666.0A CN201910305666A CN109985614A CN 109985614 A CN109985614 A CN 109985614A CN 201910305666 A CN201910305666 A CN 201910305666A CN 109985614 A CN109985614 A CN 109985614A
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tio
composite photocatalyst
graphene composite
mixed solution
graphene
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杨剑
柴玉涛
胡广
郎油东
黎学剑
李英
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Chongqing University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18Carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • B01J37/10Heat treatment in the presence of water, e.g. steam
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • C02F1/32Treatment of water, waste water, or sewage by irradiation with ultraviolet light
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/36Organic compounds containing halogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

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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

A kind of TiO2/ graphene composite photocatalyst and preparation method thereof
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.
CN201910305666.0A 2019-04-16 2019-04-16 A kind of TiO2/ graphene composite photocatalyst and preparation method thereof Pending CN109985614A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020147108A1 (en) * 1997-12-18 2002-10-10 Koji Sato Methods for producing oxides or composites thereof
CN101439873A (en) * 2008-12-16 2009-05-27 济南大学 Method for titania film growth in fluorine-based aqueous solution
CN102500287A (en) * 2011-09-28 2012-06-20 重庆大学 Graphene/modified titanium dioxide nano sol composite material and preparation method thereof
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020147108A1 (en) * 1997-12-18 2002-10-10 Koji Sato Methods for producing oxides or composites thereof
CN101439873A (en) * 2008-12-16 2009-05-27 济南大学 Method for titania film growth in fluorine-based aqueous solution
CN102500287A (en) * 2011-09-28 2012-06-20 重庆大学 Graphene/modified titanium dioxide nano sol composite material and preparation method thereof
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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
HU, GUANG ET AL.,: ""Research on Photocatalytic Properties of TiO2-Graphene Composites with Different Morphologies"", 《JOURNAL OF MATERIALS ENGINEERING AND PERFORMANCE》 *

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