CN108365201A - A kind of TiO2Carbon-based graphene composite material and its preparation method and application - Google Patents
A kind of TiO2Carbon-based graphene composite material and its preparation method and application Download PDFInfo
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Abstract
The invention belongs to optic catalytic composite material fields, and in particular to a kind of TiO2Carbon-based graphene composite material and its preparation method and application.The composite material is first using porous carbon materials as matrix, using phenol resin solution as raw material, by hydro-thermal method on matrix growth in situ graphene, obtain carbon-based graphene, then use sol method in carbon-based graphene surface composite Ti O2Nano particle is prepared.The preparation process is simple, at low cost, environmentally protective.The composite material large specific surface area, and graphene growth in situ is on the carbon material, increases TiO2, stability and synergistic effect between graphene and porous carbon base body, to greatly improve the photocatalysis performance of material.By the composite material for the remains of pesticide in photocatalytic degradation vegetables, the degradation of pesticide rate after 2 hours is i.e. up to 90% or more, and the composite material is easy recycling in the process, therefore can repeatedly use.
Description
Technical field
The invention belongs to optic catalytic composite material fields, and in particular to a kind of TiO2Carbon-based graphene composite material and its
Preparation method and application.
Background technology
Excessive pesticide residues are an important factor for influencing public health, and long-term consumption can be produced by the vegetables of pollution by pesticides
Raw slow poisoning, even results in death etc..How to reduce the residual level of pesticide residues in vegetables medicine is current urgent problem to be solved.Mesh
Before, the residual method of removal agriculture has oxidizing process, microbial degradation method, lower temperature plasma technology etc., these methods often process
The journey used time is longer, causes vegetables stale, and cost is higher, and removal effect is undesirable, and some even can also bring secondary pollution.
The Photocatalyst to grow up in the past 20 years provides good approach, wherein nano-TiO for the removal of remains of pesticide2
Become most popular photocatalytic activity material because activity is high, stability is good for it.But by its energy gap (about 3.20eV)
Influence, TiO2To the absorption of light be only limitted to ultra-violet (UV) band (<400nm), and ultraviolet light contained in sunlight is less than 5%, this
Just significantly limit TiO2To the utilization ratio of solar energy.TiO simultaneously2The electrons and holes that light excitation generates easily occur
Compound, quantum efficiency is low (being usually no more than 10%), influences its photocatalysis efficiency, greatly limits TiO2Practical application.
New carbon graphene becomes people's concern due to its special planar structure and special property
Hot spot.By TiO2It is compound with graphene, it is expected to improve TiO2Defect, expand its photoresponse range.However existing research is far
The requirement of practical application cannot be reached.First, the method system that the graphene used at present is mainly restored by graphite initial oxidation
, which is generated a large amount of waste water and waste liquid, secondary pollution is caused to environment using a large amount of dense strong acid and strong oxidizer；Two
It is nano level graphene and TiO2Dusty material is not only easy to happen reunion in application process, seriously affects using effect,
And be distributed in aqueous systems after use and be difficult to separate, it is unfavorable for the control of practical cost.
Chinese patent (CN107362788A) discloses a kind of graphene oxide/titanium dioxide-activated carbon three-dimensional composite wood
Material and preparation method thereof is used for air purification.This method makes graphene oxide and titanium dioxide granule by way of ultrasonic disperse
It is attached to activated carbon surface, graphene oxide and TiO can be solved2The problem of powder is reunited, and using activated carbon to pollutant
Suction-operated improves the service efficiency of catalyst.However, this composite material acted on by mechanical mixture, each component
Between be physical absorption, therefore the stability between each component and act synergistically it is relatively poor.In addition, graphene oxide is not only made
A large amount of strong oxidizers and strong acid are needed during standby, and its surface has the functional groups such as a large amount of carboxyls, hydroxyl, epoxy group, this
A little functional groups there are severe jamming sp2Bond hybridization network is unfavorable for the migration of electronics, causes graphene oxide to TiO2Light
The improvement of catalysis is extremely limited.
Invention content
The shortcomings that overcome the prior art and deficiency, primary and foremost purpose of the invention are to provide a kind of TiO2Carbon-based graphene
The preparation method of composite material.
It is a further object to provide a kind of TiO being prepared by the above method2Carbon-based graphene composite wood
Material.
Another object of the present invention is to provide above-mentioned TiO2The application of carbon-based graphene composite material.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of TiO2The preparation method of carbon-based graphene composite material, includes the following steps：
(1) porous carbon materials are dipped in phenol resin solution, hydro-thermal reaction is carried out at 120~200 DEG C, it then will be anti-
It answers product to filter and clean, is calcined in inert atmosphere at 900~1100 DEG C, carbon-based graphene is made；
(2) solid sulphuric acid oxygen titanium is dissolved in deionized water, adjusts pH value of solution to 10~11, generates white precipitate, will give birth to
At white precipitate filter out and clean to neutrality, then precipitation is added in peptizing agent and is made it dissolve, precursor sol is obtained；
(3) carbon-based graphene is added into precursor sol, is heated to reflux and is reacted, it is heavy then to generate reaction
Starch is filtered and is cleaned, and is finally sintered sediment in inert atmosphere at 300~600 DEG C, is obtained TiO2Carbon-based graphene is multiple
Condensation material.
Porous carbon materials described in step (1) be preferably one or both of bamboo charcoal, activated carbon or porous carbon fiber with
On.
The solid-to-liquid ratio of carbon-based graphene and precursor sol described in step (3) is preferably 1:50~1:10g/mL.
The solid-to-liquid ratio of carbon-based graphene and precursor sol described in step (3) is most preferably 1:20g/mL.
The solid-to-liquid ratio of porous carbon materials and phenol resin solution described in step (1) is preferably 1:10~3:5g/mL.
Hydro-thermal reaction duration described in step (1) is preferably 10~24 hours.
Inert atmosphere described in step (1) is nitrogen or argon gas, and calcining duration is preferably 3~5 hours.
The solid-to-liquid ratio of titanyl sulfate and deionized water described in step (2) is preferably 1:20~1:12.5g/mL.
The solid-to-liquid ratio of white precipitate described in step (2) and peptization agent solution is preferably 3:50~4:25g/mL.
Peptizing agent is preferably hydrogenperoxide steam generator described in step (2).
It is preferably 5~12 hours that duration is heated to reflux described in step (3).
Inert atmosphere described in step (3) is nitrogen or argon gas, and sintering duration is preferably 2~4 hours.
The present invention further provides a kind of TiO2Carbon-based graphene composite material, the composite material is by above method system
Standby and obtain, which has abundant hole, graphene and TiO2Nano particle is evenly distributed on hole surface, TiO2It receives
Rice grain particle size range is 5~45nm.
The present invention further provides above-mentioned TiO2The application of carbon-based graphene composite material, by the TiO2Carbon-based graphite
Alkene composite material is in the cleaning equipment of Researches on Photocatalytic Degradation of Pesticide Using or pesticide.
Compared with prior art, the present invention having the following advantages that and advantageous effect：
(1) in TiO2In the preparation process of carbon-based graphene composite material, the preparation of graphene is without the use of traditional elder generation
Oxidation restores technique, thus is without the use of a large amount of strong oxidizers and dense strong acid, only uses phenol resin solution as raw material, method
Simply, at low cost and environmentally protective, it is easy to industrial applications.
(2) TiO prepared in the present invention2In carbon-based graphene composite material, using graphene rather than graphene oxide with
TiO2It is compound, avoid interference of the surface of graphene oxide functional group to hybridization network, and graphene growth in situ and it is non-physical
It is adsorbed on porous carbon materials matrix, makes TiO2, stability between graphene and porous carbon base body and synergistic effect substantially carry
Height, the TiO of acquisition2Carbon-based graphene composite material is to visible absorption intensity compared with TiO2It can be improved 1.5~5 times.
(3) TiO prepared2Carbon-based graphene composite material is using porous carbon materials as matrix, and growth in situ is in matrix
On, stability is strong, can not only solve graphene and TiO2The problem of powder is easily reunited in use, and it is used
TiO2Carbon-based graphene composite material can reuse after simple drying, and reusable 20 times or more.
(4) by the TiO of preparation2Carbon-based graphene composite material is used to be difficult to the residual degraded in photocatalytic degradation vegetables
Pesticide, for the degradation of pesticide rate after 2 hours i.e. up to 90% or more, this has very important meaning for solving food-safety problem
Justice.
Description of the drawings
Fig. 1 is the TiO prepared in embodiment 12Carbon-based graphene composite material electron scanning micrograph.
Fig. 2 is the TiO prepared in embodiment 12TiO on carbon-based graphene composite material2The scanning electron of nano particle
Microscope photo.
Fig. 3 is the TiO prepared in embodiment 1, embodiment 2, embodiment 32The solid violet of carbon-based graphene composite material
Outside-visible diffusing reflection spectrum.
Fig. 4 is the TiO prepared in embodiment 12Degradation property curve graph of the carbon-based graphene composite material to pesticide.
Fig. 5 is the TiO prepared in embodiment 12Carbon-based graphene composite material repeatedly uses degradation orthene
Degradation rate variation diagram.
Specific implementation mode
Specific embodiments of the present invention will be described in further detail below in conjunction with the accompanying drawings, but the embodiment party of the present invention
Formula is without being limited thereto.For not specifically specified technological parameter, routine techniques progress can refer to.
Embodiment 1
TiO2The preparation method of carbon-based graphene composite material, includes the following steps：
(1) it takes 10mL phenol resin solutions to pour into water heating kettle, 3g bamboo charcoals and deionized water is added, 24 are kept the temperature in 120 DEG C
Hour, product is filtered, is washed respectively with deionized water and ethyl alcohol, is calcined 3 hours in nitrogen atmosphere at 1000 DEG C, is made
Carbon-based graphene.
(2) 8g titanyl sulfates and 100mL deionized waters are mixed, adjusts pH to 11 with ammonium hydroxide, white precipitate is filtered simultaneously
It is washed with deionized water to neutrality, 40mL hydrogenperoxide steam generators is added and dissolve precipitation, obtain precursor colloidal sol.
(3) 100mL precursor sols are taken, the carbon-based graphenes of 5g are added, are heated to reflux 10 hours, obtained sediment mistake
Filter, with deionized water and ethyl alcohol washing precipitate, is sintered 2 hours in nitrogen atmosphere at 500 DEG C, obtains TiO2Carbon-based stone
Black alkene composite material TiO2- 5%BG.
Fig. 1 is the scanning electron microscope (SEM) photograph of the sample, which shows the TiO of preparation2Carbon-based graphene composite material has abundant
Hole, a large amount of graphene and TiO2Channel surfaces Fig. 2 that particle is equably supported on bamboo charcoal is TiO on the sample2Nanometer
The scanning electron microscope (SEM) photograph of particle, the figure show TiO on the sample2Nano particle diameter ranging from 10~15nm.
Curve c is the solid ultraviolet-visible diffuse reflectance spectrum of the sample in Fig. 3.It can be seen that TiO2Carbon-based graphene composite wood
Expect to dramatically increase in the absorption intensity of visible region, and it is compound after material have a little red shift, illustrate composite material to ultraviolet
The absorbability of light and visible light enhances.
Embodiment 2
TiO2The preparation method of carbon-based graphene composite material, includes the following steps：
(1) it takes 10mL phenol resin solutions to pour into water heating kettle, 6g bamboo charcoals and deionized water is added, 17 are kept the temperature in 160 DEG C
Hour, product is filtered, is washed respectively with deionized water and ethyl alcohol, is calcined 5 hours in nitrogen atmosphere at 950 DEG C, is made
Carbon-based graphene.
(2) 6g titanyl sulfates and 100mL deionized waters are mixed, adjusts pH to 10 with ammonium hydroxide, white precipitate is filtered simultaneously
It is washed with deionized water to neutrality, 22.5mL hydrogenperoxide steam generators is added and dissolve precipitation, obtain precursor colloidal sol.
(3) 100mL precursor sols are taken, the carbon-based graphenes of 8g are added, are heated to reflux 12 hours, obtained sediment mistake
Filter, with deionized water and ethyl alcohol washing precipitate, is sintered 4 hours in nitrogen atmosphere at 450 DEG C, obtains TiO2Carbon-based stone
Black alkene composite material TiO2- 8%BG.
The TiO prepared in the present embodiment2Carbon-based graphene composite material has abundant hole, graphene and TiO2Particle
Equably it is supported on hole surface, TiO2Nano particle diameter ranging from 30~40nm.
Curve b is the solid ultraviolet-visible diffuse reflectance spectrum of the sample in Fig. 3.It can be seen that TiO2Carbon-based graphene composite wood
Expect to dramatically increase in the absorption intensity of visible region, and it is compound after material have a little red shift, illustrate composite material to ultraviolet
The absorbability of light and visible light enhances.
Embodiment 3
TiO2The preparation method of carbon-based graphene composite material, includes the following steps：
(1) it takes 10mL phenol resin solutions to pour into water heating kettle, 2g activated carbons and deionized water is added, in 200 DEG C of heat preservations
24 hours, product is filtered, washed respectively with deionized water and ethyl alcohol, calcined 4 hours in nitrogen atmosphere at 1100 DEG C, made
Obtain carbon-based graphene.
(2) 8g titanyl sulfates and 100mL deionized waters are mixed, adjusts pH to 11 with ammonium hydroxide, white precipitate is filtered simultaneously
It is washed with deionized water to neutrality, 80mL hydrogenperoxide steam generators is added and dissolve precipitation, obtain precursor colloidal sol.
(3) 100mL precursor sols are taken, the carbon-based graphenes of 2g are added, are heated to reflux 8 hours, obtained sediment filtering,
With deionized water and ethyl alcohol washing precipitate, it is sintered 3 hours in nitrogen atmosphere at 500 DEG C, obtains TiO2Carbon-based graphene
Composite material TiO2- 2%BG.
The TiO prepared in the present embodiment2Carbon-based graphene composite material has abundant hole, graphene and TiO2Particle
Equably it is supported on hole surface, TiO2Nano particle diameter ranging from 22~30nm.
Curve a is the solid ultraviolet-visible diffuse reflectance spectrum of the sample in Fig. 3.It can be seen that TiO2Carbon-based graphene composite wood
Expect to dramatically increase in the absorption intensity of visible region, and it is compound after material have a little red shift, illustrate composite material to ultraviolet
The absorbability of light and visible light enhances.
Embodiment 4
TiO2The preparation method of carbon-based graphene composite material, includes the following steps：
(1) it takes 5mL phenol resin solutions to pour into water heating kettle, 1g carbon fibers and deionized water is added, 24 are kept the temperature in 200 DEG C
Hour, product is filtered, is washed respectively with deionized water and ethyl alcohol, is calcined 5 hours in nitrogen atmosphere at 1100 DEG C, is made
Carbon-based graphene.
(2) 7g titanyl sulfates and 100mL deionized waters are mixed, adjusts pH to 11 with ammonium hydroxide, white precipitate is filtered simultaneously
It is washed with deionized water to neutrality, 30mL hydrogenperoxide steam generators is added and dissolve precipitation, obtain precursor colloidal sol.
(3) 100mL precursor sols are taken, the carbon-based graphenes of 2g are added, are heated to reflux 10 hours, obtained sediment mistake
Filter, with deionized water and ethyl alcohol washing precipitate, is sintered 2 hours in nitrogen atmosphere at 300 DEG C, obtains TiO2Carbon-based stone
Black alkene composite material.
The TiO prepared in the present embodiment2Carbon-based graphene composite material has abundant hole, graphene and TiO2Particle
Equably it is supported on hole surface, TiO2Nano particle diameter ranging from 5~14nm.
Embodiment 5
TiO2The preparation method of carbon-based graphene composite material, includes the following steps：
(1) it takes 10mL phenol resin solutions to pour into water heating kettle, 1g bamboo charcoals and deionized water is added, 10 are kept the temperature in 120 DEG C
Hour, product is filtered, is washed respectively with deionized water and ethyl alcohol, is calcined 3 hours in nitrogen atmosphere at 900 DEG C, is made
Carbon-based graphene.
(2) 5g titanyl sulfates and 100mL deionized waters are mixed, adjusts pH to 10 with ammonium hydroxide, white precipitate is filtered simultaneously
It is washed with deionized water to neutrality, 30mL hydrogenperoxide steam generators is added and dissolve precipitation, obtain precursor colloidal sol.
(3) 100mL precursor sols are taken, the carbon-based graphenes of 10g are added, are heated to reflux 5 hours, obtained sediment mistake
Filter, with deionized water and ethyl alcohol washing precipitate, is sintered 3 hours in nitrogen atmosphere at 600 DEG C, obtains TiO2Carbon-based stone
Black alkene composite material.
The TiO prepared in the present embodiment2Carbon-based graphene composite material has abundant hole, graphene and TiO2Particle
Equably it is supported on hole surface, TiO2Nano particle diameter ranging from 38~45nm.
Embodiment 6
TiO2The application of carbon-based graphene composite material：
By TiO made from embodiment 12Carbon-based graphene composite material is applied to the residual agriculture in photocatalytic degradation vegetables
Medicine：It takes fresh pakchoi to be impregnated 1 hour in Rogor, malathion, orthene, isocarbophos respectively, then takes out
Natural air drying, the pakchoi after respectively taking 100g to air-dry, is separately added into 400mg TiO2Carbon-based graphene composite material and
1000ml deionized waters are degraded under 300W xenon lamps, and timing sampling detection calculates the degradation rate of remains of pesticide.
By the TiO after using2Carbon-based graphene composite material is recovered by filtration, and is heated 1 hour in 60 DEG C of baking ovens.Then
It is degradation object with orthene, repeats above-mentioned degradation of pesticide and test 5 times.
Detection is carried out according to standard method as defined in NY/T 761.
Fig. 4 is the degradation rate figure of the material light catalysis degrading pesticide, and the material is to Rogor, horse traction sulphur as can be seen from Figure
Fast degradation may be implemented in phosphorus, orthene, isocarbophos, and 2 hours degradation rates are up to respectively under simulated solar irradiation
92.3%, 95.6%, 96.7%, 90.1%.
Fig. 5 is the degradation rate variation diagram that the material repeatedly uses degradation orthene.It can be seen that the TiO of preparation2Carbon
Base graphene composite material still has very high Photocatalytic Degradation Property after being used for multiple times.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of TiO2The preparation method of carbon-based graphene composite material, which is characterized in that include the following steps：
(1) porous carbon materials are dipped in phenol resin solution, hydro-thermal reaction is carried out at 120~200 DEG C, then produce reaction
Object is filtered and is cleaned, and is calcined in inert atmosphere at 900~1100 DEG C, and carbon-based graphene is made；
(2) solid sulphuric acid oxygen titanium is dissolved in deionized water, adjusts pH value of solution to 10~11, white precipitate is generated, by generation
White precipitate is filtered out and is cleaned to neutrality, and then precipitation is added in peptizing agent and makes it dissolve, obtains precursor sol；
(3) carbon-based graphene is added into precursor sol, is heated to reflux and is reacted, the sediment for then generating reaction
It filters and cleans, finally sediment is sintered at 300~600 DEG C in inert atmosphere, obtains TiO2Carbon-based graphene composite wood
Material.
2. TiO according to claim 12The preparation method of carbon-based graphene composite material, it is characterised in that：In step (1)
The porous carbon materials are one or more of bamboo charcoal, activated carbon or porous carbon fiber.
3. TiO according to claim 12The preparation method of carbon-based graphene composite material, it is characterised in that：In step (3)
The solid-to-liquid ratio of the carbon-based graphene and precursor sol is 1:50~1:10g/mL.
4. TiO according to claim 32The preparation method of carbon-based graphene composite material, it is characterised in that：In step (3)
The solid-to-liquid ratio of the carbon-based graphene and precursor sol is 1:20g/mL.
5. according to any one of the claim 1-4 TiO2The preparation method of carbon-based graphene composite material, it is characterised in that：Step
Suddenly peptizing agent described in (2) is hydrogenperoxide steam generator.
6. according to any one of the claim 1-4 TiO2The preparation method of carbon-based graphene composite material, it is characterised in that：Step
Suddenly described in (1) a length of 10~24 hours when hydro-thermal reaction.
7. according to any one of the claim 1-4 TiO2The preparation method of carbon-based graphene composite material, it is characterised in that：
The solid-to-liquid ratio of titanyl sulfate and deionized water described in step (2) is 1:20~1:12.5g/mL；
The solid-to-liquid ratio of white precipitate described in step (2) and peptization agent solution is 3:50~4:25g/mL.
8. according to any one of the claim 1-4 TiO2The preparation method of carbon-based graphene composite material, it is characterised in that：Step
A length of 5~12 hours when being heated to reflux described in (3) suddenly.
9. a kind of TiO2Carbon-based graphene composite material, it is characterised in that：It is prepared by any one of claim 1-8 the methods
And obtain, which has abundant hole, graphene and TiO2Nano particle is evenly distributed on hole surface, TiO2Nanometer
Particle size range is 5~45nm.
10. TiO described in a kind of claim 92The application of carbon-based graphene composite material, it is characterised in that：By the TiO2Carbon
Base graphene composite material is in the cleaning equipment of Researches on Photocatalytic Degradation of Pesticide Using or pesticide.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114345318A (en) * | 2021-12-03 | 2022-04-15 | 中北大学 | graphene-SrTiO3Material and method for the production thereof |
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| CN104388923A (en) * | 2014-10-17 | 2015-03-04 | 山东科技大学 | Making method of graphene modified titanium oxide metal anticorrosion coating |
| CN105645393A (en) * | 2016-01-14 | 2016-06-08 | 山东科技大学 | Preparing method for in-situ growth of graphene on graphite fibers |
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| US20130163146A1 (en) * | 2011-12-23 | 2013-06-27 | Samsung Electro-Mechanics Co., Ltd. | Electrode active material-conductive agent composite, method for preparing the same, and electrochemical capacitor comprising the same |
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| CN114345318B (en) * | 2021-12-03 | 2024-06-11 | 中北大学 | Graphene-SrTiO3Material and preparation method thereof |
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