CN103028387B - Preparation method of graphene/titanium dioxide photocatalyst - Google Patents
Preparation method of graphene/titanium dioxide photocatalyst Download PDFInfo
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- CN103028387B CN103028387B CN201210582986.9A CN201210582986A CN103028387B CN 103028387 B CN103028387 B CN 103028387B CN 201210582986 A CN201210582986 A CN 201210582986A CN 103028387 B CN103028387 B CN 103028387B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a 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, due to the optical, electrical performance of its excellence, has been subjected to scientific research personnel's extensive concern.It can be used as performance wild 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 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 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 it is nontoxic, low cost and other advantages, is widely used in the fields such as sewage disposal as photochemical catalyst.By 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.In preparation process, adopt the methods such as hydrazine that graphene oxide is reduced, and then compound with titanium dioxide.Although graphene oxide has good dispersiveness in the aqueous solution, but in composite preparation process, when graphene oxide is reduced to after 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 is to provide a kind of preparation method of Graphene/titanium dioxide optical catalyst.Adopt the prepared Graphene/titanium dioxide optical catalyst of the method to there is excellent Photocatalytic Degradation Property to organic dyestuff, can be widely used in the field of Environment Protections such as sewage disposal.
A preparation method for Graphene/titanium dioxide optical catalyst, step is as follows:
(1) obtain solution A: butyl titanate is slowly added in 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 solution A while stirring, stirs, obtain mixed liquor;
(4) mixed liquor is packed in water heating kettle, after hydro-thermal, naturally cool to after room temperature, separating, washing, obtains Graphene/titanium dioxide optical catalyst.
Foregoing preparation method, preferred scheme is 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 is that during step (2) preparation mixed liquid B, graphene oxide used is for using the standby graphene oxide of Hummers legal system.
Foregoing preparation method, preferred scheme is 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 chloroform, obtain the solution that butyl titanate concentration is 0.8-4.5g/L; 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, gained mixed liquor is packed in water heating kettle into hydro-thermal 5-20 hour at 160-200 ℃.Naturally cool to after room temperature, separating, washing, must have the Graphene/titanium dioxide optical catalyst of excellent photocatalysis performance.The method of the invention is the transfer between water and chloroform by product, can effectively prevent the reunion of photochemical catalyst, 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 on two-phase interface with disperseing the butyl titanate in chloroform; After graphene oxide is Graphene by hydro-thermal, the Graphene/composite titania material of the hydrophobicity of generation will be transferred in chloroform from water, thereby avoid the reunion situation in single water, thereby improve specific area and the performance of photochemical catalyst.Adopt the prepared Graphene/titanium dioxide optical catalyst of the method to there is excellent Photocatalytic Degradation Property to organic dyestuff.
The present invention has following beneficial effect:
(1) process is simple, 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 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 there is excellent Photocatalytic Degradation Property, can be widely used in the field of Environment Protections such as sewage disposal.
Accompanying drawing explanation
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, the photocatalysis effect figure to methyl orange under ultraviolet irradiation.
The specific embodiment
In order to show substantive distinguishing features of the present invention and marked improvement, with following non-limiting embodiment, further illustrate embodiment and effect.
embodiment 1
A preparation method for Graphene/titanium dioxide optical catalyst, comprises the steps:
(1) obtain solution A, slowly joins 0.07 g butyl titanate in 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 solution A while stirring, stirs, obtain the mixed solution of A and B.
(2) mixed solution of A and B is packed in water heating kettle, at 180 ℃, be incubated 12 hours; Naturally cool to after room temperature, separating, washing obtains the Graphene/titanium dioxide optical catalyst with excellent photocatalysis performance.
Through tem study, can find out that titania nanoparticles is dispersed on graphene sheet layer, as shown in Figure 1.Fig. 2 has provided the catalytic effect figure of the catalyst of the prepared composite of example 1 under UV-irradiation to methyl orange.Result shows, UV-irradiation lower 40 minutes can be that the methyl orange solution of 20 mg/L is degradable by concentration, illustrates that gained catalyst has excellent photocatalysis performance.
embodiment 2
A preparation method for Graphene/titanium dioxide optical catalyst, comprises the steps:
(1) obtain solution A, slowly joins 0.17 g butyl titanate in 40 mL chloroforms, and concentration is 4.2 g/L; 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 solution A while stirring, continues to be uniformly mixed, obtain the mixed solution of A and B.
(2) mixed solution of A and B is packed in water heating kettle, at 160 ℃, be incubated 20 hours; Naturally cool to after room temperature, separating, washing obtains the Graphene/titanium dioxide optical catalyst with excellent photocatalysis performance.
embodiment 3
A preparation method for Graphene/titanium dioxide optical catalyst, comprises the steps:
(1) obtain solution A, slowly joins 0.034 g butyl titanate in 40 mL chloroforms, and concentration is 0.85 g/L; 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 solution A while stirring, stirs, obtain the mixed solution of A and B.
(2) mixed solution of A and B is packed in water heating kettle, at 200 ℃, be incubated 5 hours; Naturally cool to after room temperature, separating, washing obtains the Graphene/titanium dioxide optical catalyst with excellent photocatalysis performance.
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the 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 cannot give all embodiments exhaustive.Every still row in protection scope of the present invention of apparent variation that technical scheme of the present invention amplifies out or change that belong to.
This patent application is subject to the fund of project of national nature science fund project (51002069) and subsidizes.
Claims (1)
1. a preparation method for Graphene/titanium dioxide optical catalyst, is characterized in that, step is as follows:
(1) obtain solution A: butyl titanate is slowly added in chloroform, obtain the solution A that butyl titanate concentration is 0.8-4.5g/L;
(2) preparation mixed liquid B: will join in the mixed solution of deionized water and ethanol with the standby graphene oxide of Hummers legal system, obtain the mixed liquid B that graphene oxide concentration is 0.02-1.0g/L;
(3) mixed liquid B is added drop-wise in isopyknic solution A while stirring, stirs, obtain mixed liquor;
(4) mixed liquor is packed in water heating kettle, 160-200 ℃ of hydro-thermal 5-20 hour, naturally cools to after room temperature, and separating, washing obtains Graphene/titanium dioxide optical 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 |
| 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 |
| CN104907018B (en) * | 2015-05-25 | 2017-03-01 | 齐鲁工业大学 | A kind of three-dimensional metatitanic acid/graphene oxide pluralgel 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 |
| 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 |
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| CN108722386B (en) * | 2017-04-14 | 2021-04-16 | 中国科学院理化技术研究所 | Polymer-induced graphene growth multi-morphology TiO2Method for preparing 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 |
| CN108704635A (en) * | 2018-05-25 | 2018-10-26 | 东北大学 | Graphene titanium dioxide composite nano material and preparation method thereof |
| CN111186874B (en) * | 2020-01-17 | 2021-05-18 | 厦门大学 | Silanization reduction graphene oxide titanium dioxide composite material and preparation method and application thereof |
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| WO2011085122A2 (en) * | 2010-01-06 | 2011-07-14 | Graphicpak Corporation | Hybrid polymer compositions with enhanced bio-degradability |
| CN101890344B (en) * | 2010-07-27 | 2012-06-13 | 华东理工大学 | Preparation method of graphene/titanium dioxide composite photocatalyst |
| CN102350334B (en) * | 2011-08-08 | 2013-08-21 | 江苏大学 | Graphene/mesoporous titanium dioxide visible light catalyst and preparation method |
| CN102489284B (en) * | 2011-11-22 | 2013-09-11 | 浙江大学 | Graphene composite titanium dioxide photocatalyst capable of magnetic separation and recovery, and preparation method thereof |
| CN102496700B (en) * | 2011-12-20 | 2014-03-05 | 中国科学院新疆理化技术研究所 | Graphene-titanium dioxide nanotube composite material and preparation method thereof |
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