CN103028387A - Preparation method of graphene/titanium dioxide photocatalyst - Google Patents
Preparation method of graphene/titanium dioxide photocatalyst Download PDFInfo
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- CN103028387A CN103028387A CN2012105829869A CN201210582986A CN103028387A CN 103028387 A CN103028387 A CN 103028387A CN 2012105829869 A CN2012105829869 A CN 2012105829869A CN 201210582986 A CN201210582986 A CN 201210582986A CN 103028387 A CN103028387 A CN 103028387A
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Abstract
The invention discloses a preparation method of a graphene/titanium dioxide photocatalyst, which comprises the following steps of (1) preparing a solution A, slowly adding tetrabutyl titanate into chloroform, and obtaining the solution A, (2) preparing a mixed solution B, adding oxidized graphene into a mixed solution of deionized water and ethanol, and obtaining the mixed solution B, (3) stirring the mixed solution B, adding the mixed solution B into the solution A simultaneously, stirring uniformly, and obtaining a mixed solution, and (4) placing the mixed solution into a hydrothermal kettle, conducting the hydrothermal treatment, naturally cooling to a room temperature, separating and washing, and obtaining the graphene/titanium dioxide photocatalyst. The graphene/titanium dioxide photocatalyst prepared by the method has an excellent photocatalytic degradation property for organic dye.
Description
Technical field
The present invention relates to the inorganic synthesis technical field of Photocatalysis Function Material, especially relate to a kind of preparation method of Graphene/titanium dioxide optical catalyst.
Background technology
Graphene has been subjected to scientific research personnel's extensive concern owing to its excellent light, electrical property.It can be used as property enhancement phase and other nano semiconductor material carry out compound, prepare excellent performance composite.By Graphene and semiconductor nano material is compound, when material is irradiated by light, light induced electron can be transferred to the Graphene from semiconductor grain, effectively stop the compound of light induced electron and hole, improve the life-span in light induced electron and hole, thereby the raising photocatalysis efficiency significantly improves the performance of catalysis material.This composite has potential application in fields such as solar energy, electrode material of lithium battery and sewage disposals.
Titanium dioxide is a kind of semi-conducting material, because its nontoxic, low cost and other advantages is widely used in the fields such as sewage disposal as photochemical catalyst.With titanium dioxide and the compound photocatalysis performance that will improve titanium dioxide of Graphene, obtain the catalysis material of excellent performance.
The preparation method who reports at present has the methods such as hydro-thermal, solvent heat, chemical deposition.Adopt the method such as hydrazine that graphene oxide is reduced in the preparation process, and then compound with titanium dioxide.Although graphene oxide has good dispersiveness in the aqueous solution, but in the composite preparation process, after graphene oxide is reduced to Graphene, because Graphene has very strong hydrophobicity, cause gained Graphene/titanium dioxide optical catalyst to be reunited serious, be difficult for disperseing.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method of Graphene/titanium dioxide optical catalyst.Adopt the prepared Graphene/titanium dioxide optical catalyst of the method that organic dyestuff is had excellent Photocatalytic Degradation Property, can be widely used in the field of Environment Protections such as sewage disposal.
A kind of preparation method of Graphene/titanium dioxide optical catalyst, step is as follows:
(1) obtain solution A: butyl titanate is slowly added in the chloroform, obtain solution A;
(2) preparation mixed liquid B: graphene oxide is joined in the mixed solution of deionized water and ethanol, obtain mixed liquid B;
(3) mixed liquid B is added drop-wise in the solution A while stirring, stirs, get mixed liquor;
(4) mixed liquor is packed in the water heating kettle, after the hydro-thermal, naturally cool to room temperature after, separating, washing namely obtains Graphene/titanium dioxide optical catalyst.
Foregoing preparation method, preferred scheme are that the solution A of step (1) preparation is that butyl titanate concentration is the solution of 0.8-4.5g/L.
Foregoing preparation method, preferred scheme are that used graphene oxide is for using the standby graphene oxide of Hummers legal system during step (2) preparation mixed liquid B.
Foregoing preparation method, preferred scheme are that the mixed liquid B of step (2) preparation is that graphene oxide concentration is the mixed liquor of 0.02-1.0 g/L.
Foregoing preparation method, preferred scheme is that the consumption of step (3) solution A and mixed liquid B is equal-volume.
Foregoing preparation method, preferred scheme is that step (4) hydrothermal temperature is 160-200 ℃.
Foregoing preparation method, preferred scheme is that step (4) the hydro-thermal time is 5-20 hour.
The present invention is to provide a kind of preparation method of Graphene/titanium dioxide optical catalyst, comprise the steps: (1) obtain solution A, butyl titanate is slowly added in the chloroform, obtain the solution that butyl titanate concentration is 0.8-4.5g/L; The preparation mixed liquid B will join in the mixed solution of deionized water and ethanol with the standby graphene oxide of Hummers legal system in right amount, obtains the mixed liquor that graphene oxide concentration is 0.02-1.0 g/L.The mixed liquid B of certain volume is added drop-wise in isopyknic solution A while stirring, stirs.(2) last, the gained mixed liquor is packed in the water heating kettle, at 160-200 ℃ of lower hydro-thermal 5-20 hour.After naturally cooling to room temperature, separating, washing namely gets the Graphene/titanium dioxide optical catalyst with excellent photocatalysis performance.The method of the invention can effectively prevent the reunion of photochemical catalyst by the transfer of product between water and chloroform, significantly improves specific area and the photocatalysis performance of photochemical catalyst.
The present invention has adopted a kind of water and chloroform two-phase hydro-thermal method to prepare the Graphene/photocatalysis material of titanium dioxide of good dispersion.In the method, before graphene oxide is by hydro-thermal, can be dispersed in water well, react at two-phase interface with disperseing the butyl titanate in the chloroform; After graphene oxide is Graphene by hydro-thermal, the Graphene/composite titania material of the hydrophobicity of generation will be transferred in the chloroform from water, thereby avoid the reunion situation at single aqueous phase, thereby improve specific area and the performance of photochemical catalyst.Adopt the prepared Graphene/titanium dioxide optical catalyst of the method that organic dyestuff is had excellent Photocatalytic Degradation Property.
The present invention has following beneficial effect:
(1) process is simple, and is easy to implement, can reduce the chance of introducing impurity, thereby can not affect the purity of product.
(2) preparation process is gentle, does not need the special atmosphere protection, and equipment needed thereby is simple, and reaction speed is fast, is suitable for large-scale production.
(3) avoid the reunion of composite, made gained Graphene/titanium dioxide optical catalyst have excellent Photocatalytic Degradation Property, can be widely used in the field of Environment Protections such as sewage disposal.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the prepared Graphene/titanium dioxide optical catalyst of example 1;
Fig. 2 is the prepared Graphene/titanium dioxide optical catalyst of example 1, under ultraviolet irradiation to the photocatalysis effect figure of methyl orange.
The specific embodiment
In order to show substantive distinguishing features of the present invention and marked improvement, further specify embodiment and effect with following non-limiting embodiment.
Embodiment 1
A kind of preparation method of Graphene/titanium dioxide optical catalyst comprises the steps:
(1) obtain solution A slowly joins 0.07 g butyl titanate in the 40 mL chloroforms, and concentration is 1.75 g/L; Obtain solution B joins 0.024 g in the mixed liquor of 40 mL deionized waters and ethanol with the standby graphene oxide of Hummers legal system, the concentration of graphene oxide is 0.6 g/L.Resulting mixed solution B is added drop-wise in the solution A while stirring, stirs, obtain the mixed solution of A and B.
(2) mixed solution of A and B is packed in the water heating kettle, 180 ℃ of lower insulations 12 hours; After naturally cooling to room temperature, separating, washing namely gets the Graphene/titanium dioxide optical catalyst with excellent photocatalysis performance.
Can find out that through tem study titania nanoparticles is dispersed on the graphene sheet layer, as shown in Figure 1.Fig. 2 has provided the catalytic effect figure of the catalyst of example 1 prepared composite under UV-irradiation to methyl orange.The result shows, UV-irradiation lower 40 minutes can be that the methyl orange solution of 20 mg/L is degradable with concentration, illustrates that the gained catalyst has excellent photocatalysis performance.
Embodiment 2
A kind of preparation method of Graphene/titanium dioxide optical catalyst comprises the steps:
(1) obtain solution A slowly joins 0.17 g butyl titanate in the 40 mL chloroforms, and concentration is 4.2 g/L; The preparation mixed liquid B joins 0.008 g in the mixed liquor of 40 mL deionized waters and ethanol with the standby graphene oxide of Hummers legal system, the concentration of graphene oxide is 0.02 g/L.Mixed liquid B is added drop-wise in the solution A while stirring, continues to mix, obtain the mixed solution of A and B.
(2) mixed solution of A and B is packed in the water heating kettle, 160 ℃ of lower insulations 20 hours; After naturally cooling to room temperature, separating, washing namely gets the Graphene/titanium dioxide optical catalyst with excellent photocatalysis performance.
Embodiment 3
A kind of preparation method of Graphene/titanium dioxide optical catalyst comprises the steps:
(1) obtain solution A slowly joins 0.034 g butyl titanate in the 40 mL chloroforms, and concentration is 0.85 g/L; The preparation mixed liquid B joins 0.032 g in the mixed liquor of 40 mL deionized waters and ethanol with the standby graphene oxide of Hummers legal system, the concentration of graphene oxide is 0.8 g/L.Resulting mixed solution B is added drop-wise in the solution A while stirring, stirs, obtain the mixed solution of A and B.
(2) mixed solution of A and B is packed in the water heating kettle, 200 ℃ of lower insulations 5 hours; After naturally cooling to room temperature, separating, washing namely gets the Graphene/titanium dioxide optical catalyst with excellent photocatalysis performance.
Obviously, the above embodiment of the present invention is only for clearly illustrating example of the present invention, and is not to be restriction to embodiments of the present invention.For those of ordinary skill in the field, on above-mentioned basis of giving an example, can also do other multi-form variation or changes.Here can't give all embodiments exhaustive.Everyly belong to the row that apparent variation that technical scheme of the present invention amplifies out or change still are in protection scope of the present invention.
This patent application is subject to the fund of project of national nature science fund project (51002069) and subsidizes.
Claims (7)
1. the preparation method of a Graphene/titanium dioxide optical catalyst is characterized in that, step is as follows:
(1) obtain solution A: butyl titanate is slowly added in the chloroform, obtain solution A;
(2) preparation mixed liquid B: graphene oxide is joined in the mixed solution of deionized water and ethanol, obtain mixed liquid B;
(3) mixed liquid B is added drop-wise in the solution A while stirring, stirs, get mixed liquor;
(4) mixed liquor is packed in the water heating kettle, after the hydro-thermal, naturally cool to room temperature after, separating, washing namely obtains Graphene/titanium dioxide optical catalyst.
2. preparation method according to claim 1 is characterized in that, the solution A of step (1) preparation is that butyl titanate concentration is the solution of 0.8-4.5g/L.
3. preparation method according to claim 1 is characterized in that, used graphene oxide is for using the standby graphene oxide of Hummers legal system during step (2) preparation mixed liquid B.
4. preparation method according to claim 1 is characterized in that, the mixed liquid B of step (2) preparation is that graphene oxide concentration is the mixed liquor of 0.02-1.0 g/L.
5. preparation method according to claim 1 is characterized in that, the consumption of step (3) solution A and mixed liquid B is equal-volume.
6. preparation method according to claim 1 is characterized in that, step (4) hydrothermal temperature is 160-200 ℃.
7. preparation method according to claim 1 is characterized in that, step (4) the hydro-thermal time is 5-20 hour.
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| CN103521270A (en) * | 2013-10-22 | 2014-01-22 | 天津大学 | Sulfonated coal loaded TiO2 photocatalyst and preparation method thereof |
| CN104148045A (en) * | 2014-08-15 | 2014-11-19 | 中国科学院青海盐湖研究所 | Arc process-based graphene/titanium dioxide composite material preparation method |
| CN104907018A (en) * | 2015-05-25 | 2015-09-16 | 齐鲁工业大学 | Three-dimensional titanic acid/graphene oxide composite gel, and preparation method thereof |
| CN105826515A (en) * | 2016-05-16 | 2016-08-03 | 北京师范大学 | Lithium ion battery cathode material and application thereof |
| CN106076337A (en) * | 2016-07-14 | 2016-11-09 | 中国科学院生态环境研究中心 | A kind of composite photocatalyst material and preparation method thereof |
| CN106311206A (en) * | 2016-09-09 | 2017-01-11 | 北京优碳环能科技有限公司 | Titanium dioxide/graphene composite nanometer photocatalyst, method for preparing same and application of titanium dioxide/graphene composite nanometer photocatalyst |
| CN106395800A (en) * | 2016-08-26 | 2017-02-15 | 南通大学 | Preparation method of TiO2 intercalated graphene oxide |
| CN106693946A (en) * | 2017-01-13 | 2017-05-24 | 江西德弘新材料有限公司 | Preparation method of graphene/titanium oxide composite visible light photocatalyst |
| CN107824173A (en) * | 2017-11-01 | 2018-03-23 | 南通纺织丝绸产业技术研究院 | A kind of titanous auto-dope titania nanoparticles partial reduction stannic oxide/graphene nano piece composite and preparation method thereof |
| CN108262032A (en) * | 2016-12-30 | 2018-07-10 | 海门市源美美术图案设计有限公司 | A kind of modified graphene composite material and its photocatalysis |
| CN108704635A (en) * | 2018-05-25 | 2018-10-26 | 东北大学 | Graphene titanium dioxide composite nano material and preparation method thereof |
| CN108722386A (en) * | 2017-04-14 | 2018-11-02 | 中国科学院理化技术研究所 | A kind of polymer induction graphene growth multiform looks TiO2The method of photochemical catalyst |
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| CN103521270A (en) * | 2013-10-22 | 2014-01-22 | 天津大学 | Sulfonated coal loaded TiO2 photocatalyst and preparation method thereof |
| CN104148045A (en) * | 2014-08-15 | 2014-11-19 | 中国科学院青海盐湖研究所 | Arc process-based graphene/titanium dioxide composite material preparation method |
| CN104148045B (en) * | 2014-08-15 | 2016-02-03 | 中国科学院青海盐湖研究所 | Based on the preparation method of the graphene/titania composite material of arc process |
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| CN105826515A (en) * | 2016-05-16 | 2016-08-03 | 北京师范大学 | Lithium ion battery cathode material and application thereof |
| CN106076337A (en) * | 2016-07-14 | 2016-11-09 | 中国科学院生态环境研究中心 | A kind of composite photocatalyst material and preparation method thereof |
| CN106395800A (en) * | 2016-08-26 | 2017-02-15 | 南通大学 | Preparation method of TiO2 intercalated graphene oxide |
| CN106395800B (en) * | 2016-08-26 | 2019-04-19 | 南通大学 | A kind of preparation method of TiO2 intercalation graphene oxide |
| CN106311206A (en) * | 2016-09-09 | 2017-01-11 | 北京优碳环能科技有限公司 | Titanium dioxide/graphene composite nanometer photocatalyst, method for preparing same and application of titanium dioxide/graphene composite nanometer photocatalyst |
| CN108262032A (en) * | 2016-12-30 | 2018-07-10 | 海门市源美美术图案设计有限公司 | A kind of modified graphene composite material and its photocatalysis |
| CN106693946A (en) * | 2017-01-13 | 2017-05-24 | 江西德弘新材料有限公司 | Preparation method of graphene/titanium oxide composite visible light photocatalyst |
| CN108722386A (en) * | 2017-04-14 | 2018-11-02 | 中国科学院理化技术研究所 | A kind of polymer induction graphene growth multiform looks TiO2The method of photochemical catalyst |
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| CN108704635A (en) * | 2018-05-25 | 2018-10-26 | 东北大学 | Graphene titanium dioxide composite nano material and preparation method thereof |
| CN111186874A (en) * | 2020-01-17 | 2020-05-22 | 厦门大学 | Silanization reduction graphene oxide titanium dioxide composite material and preparation method and application thereof |
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