CN102423702A - Graphene oxide/titanium dioxide composite photocatalysis material and preparation method thereof - Google Patents
Graphene oxide/titanium dioxide composite photocatalysis material and preparation method thereof Download PDFInfo
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- CN102423702A CN102423702A CN2011104560278A CN201110456027A CN102423702A CN 102423702 A CN102423702 A CN 102423702A CN 2011104560278 A CN2011104560278 A CN 2011104560278A CN 201110456027 A CN201110456027 A CN 201110456027A CN 102423702 A CN102423702 A CN 102423702A
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Abstract
The invention relates to a graphene oxide/titanium dioxide composite photocatalysis material and a preparation method thereof, and belongs to the technical field of photocatalysis. The material of the present invention is applicable for catalytic degradation of pollutants. With the present invention, the problem of low photocatalysis efficiency of the catalyst is solved. The structure of the composite photocatalysis material is that: nano-scale titanium dioxide is uniformly dispersed in micron graphene oxide lamellas to form the composite photocatalysis material. The preparation method for the composite photocatalysis material comprises: 1, preparing the graphene oxide into an aqueous suspension; 2, sequentially and slowly adding polyethylene glycol, glacial acetic acid and tetrabutyl titanate to dehydrated alcohol under a stirring condition to prepare into a mixing solution; 3, adding the prepared graphene oxide aqueous suspension from the step 1 to the prepared mixing solution from the step 2 in a dropwise manner, stirring at a uniform speed at a room temperature to form a mixed solution; 4, drying the mixed solution from the step 3 to obtain the solid mixture; 5, placing the obtained solid mixture from the step 4 to a container, carrying out calcination under the protection of inert gas to obtain the graphene oxide/titanium dioxide composite photocatalyst.
Description
Technical field
The present invention relates to a kind of optic catalytic composite material and preparation method thereof, belong to the photocatalysis technology field, be applicable to catalytic degradation inorganic, organic pollution.
Background technology
In recent years, problems such as energy crisis and environmental pollution are increasingly serious, and all pay much attention to energy savings and protection environment countries in the world.Photocatalysis is with its normal-temperature reaction and can directly utilize solar energy to carry out characteristics such as catalytic degradation, is considered to a kind of environmental pollution purification techniques that has wide application prospect.Since Fujishima in 1972 and Honda found that anatase phase titanium dioxide can effectively be purified waste water, titanium dioxide received people's attention and obtains broad research as a kind of environmental type catalyst.Yet titanium dioxide photoproduction carrier is compound very easily again in the photocatalytic process, causes photo-quantum efficiency very low, thereby influences its photocatalysis efficiency, can improve photocatalysis efficiency so reduce the compound of photo-generated carrier.
Graphene is a kind of carbonaceous new material of the tightly packed one-tenth individual layer of a kind of carbon atom bi-dimensional cellular shape lattice structure.Unique mechanical, calorifics, optics and the electrical properties more excellent than CNT are arranged.Graphene oxide is the important growth of Graphene, and structure is identical substantially with Graphene.The graphene oxide sheet has the big and strong characteristics of ion-exchange capacity of specific area.With graphite is that a kind of lyophobic dust is different; Graphene oxide has a large amount of oxy radicals such as C-O-C, C-OH, C=O; The groups such as hydroxyl, carboxyl that link to each other with the graphite linings covalency such as COOH; Be a kind of hydroaropic substance, can in pure water, form steady suspension, these characteristics are all given itself and the good compound ability of titanium dioxide.
Summary of the invention
Technical problem to be solved by this invention is the low problem of environmental type catalyst photocatalysis efficiency.A kind of graphene oxide/titanic oxide composite photochemical catalyst material and preparation method thereof is provided.
Technical scheme of the present invention:
A kind of graphene oxide/titanic oxide composite photochemical catalyst material; This composite photocatalyst material structure: titanium dioxide is distributed in the upper and lower surfaces and the fringe region of graphene oxide material, forms the composite photocatalyst material that a kind of Nano titanium dioxide is dispersed in micron order graphene oxide lamella.
The preparation method of this composite photocatalyst material may further comprise the steps:
Step 1 is made into graphene oxide the water slurry of mass concentration 0.1～1g/L;
Step 3 is got the graphene oxide water slurry 2～8ml of step 1 preparation, is added drop-wise in 30～40ml mixed liquor of step 2 preparation, at the uniform velocity stirs under the room temperature 1～5 day, forms mixed liquor;
Step 4 is dry with the mixed liquor of gained in the step 3, obtains solid mixt;
Step 5 is put into container with gained solid mixt in the step 4, under inert gas shielding, in 400 ℃～450 ℃ calcinings 0.5～3 hour, after the cooling, obtains graphene oxide/titanium dioxide composite photocatalyst.
Mixing speed in the step 2 is 50～150r/min.
Graphene oxide water slurry rate of addition in the step 3 is 50～500 μ l/min.
The container that solid mixt is put in the step 5 comprises: quartz container, glass container, ceramic vessel;
Described inert gas comprises: volume fraction is greater than the argon gas of 99Vol.%, and volume fraction is greater than the nitrogen of 99Vol.%, and volume fraction is greater than the argon hydrogen gaseous mixture of 99Vol.%.
The present invention compares the beneficial effect that is had with prior art:
Titanium dioxide is distributed in the upper and lower surfaces and the fringe region of graphene oxide material, forms the composite photocatalyst material that a kind of Nano titanium dioxide is dispersed in micron order graphene oxide lamella.
Graphene oxide and composite titania material through low temperature calcination, form more stable chemical bond under inert gas shielding.And because the unique structure of functional groups of graphene oxide, excitation electron can be transferred on the graphene oxide material fast on the titanium dioxide conduction band, and then improves light-catalyzed reaction speed.
Description of drawings
The sketch map of Fig. 1 graphene oxide/titanic oxide composite photochemical catalyst material.
The pure anatase phase of Fig. 2 TiO
2With make the photocatalytic degradation figure of graphene oxide/titanic oxide composite photochemical catalyst material to methyl orange.
The specific embodiment
A kind of graphene oxide/titanic oxide composite photochemical catalyst material; This composite photocatalyst material structure: titanium dioxide is distributed in the upper and lower surfaces and the fringe region of graphene oxide material, forms the composite photocatalyst material that a kind of Nano titanium dioxide is dispersed in micron order graphene oxide lamella.
The step of one of a kind of graphene oxide/titanic oxide composite photochemical catalyst material and preparation method thereof comprises:
Step 1 is made into graphene oxide the water slurry of mass concentration 0.1g/L;
The step 2 low whipping speed is slowly polyethylene glycol, glacial acetic acid and butyl titanate to be joined successively under the 50r/min condition to be made into mixed liquor in the absolute ethyl alcohol; Its mass concentration is followed successively by: polyethylene glycol 2.5g/L; Glacial acetic acid 0.3g/L, butyl titanate 0.1g/L;
Step 3 is got the graphene oxide water slurry 2ml of step 1 preparation, is that 50 μ l/min are added drop-wise in the 30ml mixed liquor of step 2 preparation with rate of addition, at the uniform velocity stirs 1 day under 15 ℃, forms mixed liquor;
Step 4 obtains solid mixt with the mixed liquor of gained in the step 3 after 60 ℃ of dryings;
Step 5 is put into container with gained solid mixt in the step 4, volume fraction greater than the nitrogen protection of 99Vol.% under in 400 ℃ the calcining 0.5 hour, obtain graphene oxide/titanium dioxide composite photocatalyst after the cooling.
Two the step of a kind of graphene oxide/titanic oxide composite photochemical catalyst material and preparation method thereof comprises:
Step 1 is made into graphene oxide the water slurry of mass concentration 0.3g/L;
The step 2 low whipping speed is slowly polyethylene glycol, glacial acetic acid and butyl titanate to be joined successively under the condition of 100r/min to be made into mixed liquor in the absolute ethyl alcohol; Its mass concentration is followed successively by: polyethylene glycol 3g/L; Glacial acetic acid 0.25g/L, butyl titanate 0.15g/L;
Step 3 is got the graphene oxide water slurry 3ml of step 1 preparation, is that 100 μ l/min are added drop-wise in the 35ml mixed liquor of step 2 preparation with rate of addition, at the uniform velocity stirs 3 days under 20 ℃, forms mixed liquor;
Step 4 obtains solid mixt with the mixed liquor of gained in the step 3 after 65 ℃ of dryings;
Step 5 is put into container with gained solid mixt in the step 4, volume fraction greater than the nitrogen protection of 99Vol.% under in 450 ℃ the calcining 2 hours, obtain graphene oxide/titanium dioxide composite photocatalyst after the cooling.
Three the step of a kind of graphene oxide/titanic oxide composite photochemical catalyst material and preparation method thereof comprises:
Step 1 is made into graphene oxide the water slurry of mass concentration 0.6g/L;
The step 2 low whipping speed is slowly polyethylene glycol, glacial acetic acid and butyl titanate to be joined successively under the 120r/min condition to be made into mixed liquor in the absolute ethyl alcohol; Its mass concentration is followed successively by: polyethylene glycol 2.8g/L; Glacial acetic acid 0.28g/L, butyl titanate 0.18g/L;
Step 3 is got the graphene oxide water slurry 5ml of step 1 preparation, is that 200 μ l/min are added drop-wise in the 38ml mixed liquor of step 2 preparation with rate of addition, at the uniform velocity stirs 4 days under 22 ℃, forms mixed liquor;
Step 4 obtains solid mixt with the mixed liquor of gained in the step 3 after 60 ℃ of dryings;
Step 5 is put into container with gained solid mixt in the step 4, volume fraction greater than the argon shield of 99Vol.% under in 430 ℃ the calcining 2.5 hours, obtain graphene oxide/titanium dioxide composite photocatalyst after the cooling.
Four the step of a kind of graphene oxide/titanic oxide composite photochemical catalyst material and preparation method thereof comprises:
Step 1 is made into graphene oxide the water slurry of mass concentration 1g/L;
The step 2 low whipping speed is slowly polyethylene glycol, glacial acetic acid and butyl titanate to be joined successively under the 150r/min condition to be made into mixed liquor in the absolute ethyl alcohol; Its mass concentration is followed successively by: polyethylene glycol 3.5g/L; Glacial acetic acid 0.2g/L, butyl titanate 0.2g/L;
Step 3 is got the graphene oxide water slurry 8ml of step 1 preparation, is that 500 μ l/min are added drop-wise in the 40ml mixed liquor of step 2 preparation with rate of addition, at the uniform velocity stirs 5 days under 25 ℃, forms mixed liquor;
Step 4 obtains solid mixt with the mixed liquor of gained in the step 3 after 60 ℃ of dryings;
Step 5 is put into container with gained solid mixt in the step 4, under volume fraction is protected greater than the argon hydrogen gaseous mixture of 99Vol.%, in 450 ℃ of calcinings 3 hours, obtains graphene oxide/titanium dioxide composite photocatalyst after the cooling.
The sketch map of Fig. 1 graphene oxide/titanic oxide composite photochemical catalyst material.
Because the structure of functional groups that graphene oxide is unique; Make on the titanium dioxide conduction band excitation electron can transfer on the graphene oxide material fast; Reduce the recombination reaction between titanium dioxide current-carrying, prolong Carrier Recombination, thereby effectively improve photocatalysis efficiency.
The pure anatase phase of Fig. 2 TiO
2With make the photocatalytic degradation figure of graphene oxide/titanic oxide composite photochemical catalyst material to methyl orange.Visible gained composite catalyzing agent material catalytic efficiency is far above pure anatase phase titanium dioxide from the curve.
Claims (5)
1. graphene oxide/titanic oxide composite photochemical catalyst material is characterized in that:
This composite photocatalyst material structure: titanium dioxide is distributed in the upper and lower surfaces and the fringe region of graphene oxide material, forms the composite photocatalyst material that a kind of Nano titanium dioxide is dispersed in micron order graphene oxide lamella.
2. the preparation method of a graphene oxide/titanic oxide composite photochemical catalyst material is characterized in that:
The preparation method of this composite photocatalyst material may further comprise the steps:
Step 1 is made into graphene oxide the water slurry of mass concentration 0.1～1g/L;
Step 2 slowly joins polyethylene glycol, glacial acetic acid and butyl titanate successively under stirring condition and is made into mixed liquor in the absolute ethyl alcohol; Its mass concentration is followed successively by: polyethylene glycol 2.5～3.5g/L; Glacial acetic acid 0.2～0.3g/L, butyl titanate 0.1～0.2g/L;
Step 3 is got the graphene oxide water slurry 2～8ml of step 1 preparation, is added drop-wise in 30～40ml mixed liquor of step 2 preparation, at the uniform velocity stirs under the room temperature 1～5 day, forms mixed liquor;
Step 4 is dry with the mixed liquor of gained in the step 3, obtains solid mixt;
Step 5 is put into container with gained solid mixt in the step 4, under inert gas shielding, in 400 ℃～450 ℃ calcinings 0.5～3 hour, after the cooling, obtains graphene oxide/titanium dioxide composite photocatalyst.
3. the preparation method of graphene oxide/titanic oxide composite photochemical catalyst material according to claim 2 is characterized in that:
Mixing speed in the step 2 is 50～150r/min.
4. the preparation method of graphene oxide/titanic oxide composite photochemical catalyst material according to claim 2 is characterized in that:
Graphene oxide water slurry rate of addition in the step 3 is 50～500 μ l/min.
5. the preparation method of graphene oxide/titanic oxide composite photochemical catalyst material according to claim 2 is characterized in that:
The container that solid mixt is put in the step 5 comprises: quartz container, glass container, ceramic vessel;
Described inert gas comprises: volume fraction is greater than the argon gas of 99Vol.%, and volume fraction is greater than the nitrogen of 99Vol.%, and volume fraction is greater than the argon hydrogen gaseous mixture of 99Vol.%.
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| CN103991903A (en) * | 2014-06-04 | 2014-08-20 | 江苏大学 | Method for preparing mixed-phase titanium dioxide nanosheet photocatalyst |
| CN104446594A (en) * | 2014-11-07 | 2015-03-25 | 河南理工大学 | Functional porous cement based composite material and preparation method thereof |
| CN104472542A (en) * | 2014-12-18 | 2015-04-01 | 中山大学 | Method for preparing graphene/silver/titanium dioxide composite material |
| CN105540733A (en) * | 2016-01-26 | 2016-05-04 | 浙江工商大学 | TiO2-reduced graphene composite and preparation method thereof and application of TiO2-reduced graphene composite to artificial sea water system |
| CN105964286A (en) * | 2016-05-18 | 2016-09-28 | 江苏理工学院 | Nitrogen-doped graphene quantum dot and graphite-phase carbon nitride composite photocatalyst and preparation method thereof |
| CN106140126A (en) * | 2015-05-15 | 2016-11-23 | 蓝石科技(开曼)有限公司 | A kind of powder composite photocatalyst material and preparation method thereof |
| CN106263261A (en) * | 2015-05-18 | 2017-01-04 | 宝峰时尚国际控股有限公司 | The application of composite photocatalyst material and bactericidal deodorant insole, footwear and preparation method |
| CN106423247A (en) * | 2016-11-10 | 2017-02-22 | 过冬 | Method for enhancing Cr<6+> photocatalysis of TiO2 |
| CN106799219A (en) * | 2016-12-22 | 2017-06-06 | 南昌航空大学 | A kind of preparation method of titania nanoparticles/Graphene composite photocatalyst material |
| CN107321340A (en) * | 2017-06-29 | 2017-11-07 | 南通大学 | A kind of graphene composite photocatalyst aeroge of hierarchical porous structure and preparation method thereof |
| CN110639611A (en) * | 2019-09-03 | 2020-01-03 | 浙江工商大学 | Polyethylene glycol thermal reduction grafting modified graphene photocatalyst and preparation and application 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 |
| CN112044432A (en) * | 2020-09-07 | 2020-12-08 | 南京大学 | Rapid preparation method of titanium dioxide supported gold nanoparticles at normal temperature |
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| CN101890344A (en) * | 2010-07-27 | 2010-11-24 | 华东理工大学 | Preparation method of graphene/titanium dioxide composite photocatalyst |
| CN101947441A (en) * | 2010-09-07 | 2011-01-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Graphene composite photocatalyst, preparation method and application thereof |
| CN102266789A (en) * | 2010-06-07 | 2011-12-07 | 付文甫 | Renewable photocatalyst for decomposing hydrogen sulfide to prepare hydrogen |
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| CN102266789A (en) * | 2010-06-07 | 2011-12-07 | 付文甫 | Renewable photocatalyst for decomposing hydrogen sulfide to prepare hydrogen |
| CN101890344A (en) * | 2010-07-27 | 2010-11-24 | 华东理工大学 | Preparation method of graphene/titanium dioxide composite photocatalyst |
| CN101947441A (en) * | 2010-09-07 | 2011-01-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Graphene composite photocatalyst, preparation method and application thereof |
Cited By (17)
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| CN103991903A (en) * | 2014-06-04 | 2014-08-20 | 江苏大学 | Method for preparing mixed-phase titanium dioxide nanosheet photocatalyst |
| CN103991903B (en) * | 2014-06-04 | 2016-06-15 | 江苏大学 | A kind of preparation method of mixed phase titanium dioxide nanosheet photocatalyst |
| CN104446594A (en) * | 2014-11-07 | 2015-03-25 | 河南理工大学 | Functional porous cement based composite material and preparation method thereof |
| CN104446594B (en) * | 2014-11-07 | 2016-06-29 | 河南理工大学 | A kind of functional type honeycombed cement based composites and preparation method thereof |
| CN104472542A (en) * | 2014-12-18 | 2015-04-01 | 中山大学 | Method for preparing graphene/silver/titanium dioxide composite material |
| CN106140126A (en) * | 2015-05-15 | 2016-11-23 | 蓝石科技(开曼)有限公司 | A kind of powder composite photocatalyst material and preparation method thereof |
| CN106263261A (en) * | 2015-05-18 | 2017-01-04 | 宝峰时尚国际控股有限公司 | The application of composite photocatalyst material and bactericidal deodorant insole, footwear and preparation method |
| CN105540733A (en) * | 2016-01-26 | 2016-05-04 | 浙江工商大学 | TiO2-reduced graphene composite and preparation method thereof and application of TiO2-reduced graphene composite to artificial sea water system |
| CN105964286A (en) * | 2016-05-18 | 2016-09-28 | 江苏理工学院 | Nitrogen-doped graphene quantum dot and graphite-phase carbon nitride composite photocatalyst and preparation method thereof |
| CN105964286B (en) * | 2016-05-18 | 2019-07-09 | 江苏理工学院 | A kind of nitrogen-doped graphene quantum dot and graphite phase carbon nitride composite photo-catalyst and preparation method thereof |
| CN106423247A (en) * | 2016-11-10 | 2017-02-22 | 过冬 | Method for enhancing Cr<6+> photocatalysis of TiO2 |
| CN106799219A (en) * | 2016-12-22 | 2017-06-06 | 南昌航空大学 | A kind of preparation method of titania nanoparticles/Graphene composite photocatalyst material |
| CN107321340A (en) * | 2017-06-29 | 2017-11-07 | 南通大学 | A kind of graphene composite photocatalyst aeroge of hierarchical porous structure and preparation method thereof |
| CN110639611A (en) * | 2019-09-03 | 2020-01-03 | 浙江工商大学 | Polyethylene glycol thermal reduction grafting modified graphene photocatalyst and preparation and application 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 |
| CN112044432A (en) * | 2020-09-07 | 2020-12-08 | 南京大学 | Rapid preparation method of titanium dioxide supported gold nanoparticles at normal temperature |
| CN112044432B (en) * | 2020-09-07 | 2021-12-17 | 南京大学 | Rapid preparation method of titanium dioxide supported gold nanoparticles at normal temperature |
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Application publication date: 20120425 |