CN109305668A - A kind of preparation method of titanium dioxide-graphene nanocomposite material - Google Patents
A kind of preparation method of titanium dioxide-graphene nanocomposite material Download PDFInfo
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- CN109305668A CN109305668A CN201710631694.2A CN201710631694A CN109305668A CN 109305668 A CN109305668 A CN 109305668A CN 201710631694 A CN201710631694 A CN 201710631694A CN 109305668 A CN109305668 A CN 109305668A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The invention discloses a kind of preparation methods of titanium dioxide-graphene nanocomposite material, include: that (1) 40mL dehydrated alcohol is added into 5mL graphene oxide suspension, after ultrasonic disperse is uniform, titanium source, lye is added, 60~90min of magnetic agitation obtains mixed solution；(2) mixed solution is transferred in autoclave under the conditions of 90~220 DEG C reaction 12~for 24 hours, then 1~2h of heated at constant temperature, cooled to room temperature obtain mixture suspension under the conditions of 60~80 DEG C in drying box；(3) mixture suspension is centrifugated, sample is collected, uses deionized water, washes of absolute alcohol sample respectively, the dry drying under the conditions of 50~60 DEG C, 1.5h is calcined in 400~450 DEG C of Muffle furnace, obtains titanium dioxide-graphene nanocomposite material.In the present invention, the specific surface area by using composite material made from the method that graphene is added is 185m2/ g increases the contact area of titanium dioxide and pollutant in composite material, while titania nanoparticles are uniformly dispersed, to facilitate the photocatalysis effect of enhancing titanium dioxide.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of system of titanium dioxide-graphene nanocomposite material
Preparation Method.
Background technique
Photoelectric conversion technology is reacted at room temperature using it and can be directly unique come drive response etc. using solar energy as light source
Can, and become a kind of ideal environmental pollution treatment technology and clear energy sources production technology.On the one hand, it is desirable to apply photoelectricity
Transformation technology is developed efficiently, free of contamination clean energy resource, rationally and effectively utilizes solar energy, this not only can solve current energy
The shortage problem in source, it is often more important that can mitigate and largely be polluted at present using fossil fuel to environment bring；And another party
Face, people wish that photoelectric conversion method also can play the part of useful role in the processing of harmful waste again.Therefore, photoelectric conversion
Research be of great immediate significance for solving the energy, pollution problem.Wherein, it is about semiconductor that people, which study more,
The photoelectric property of nano material, the photoelectric property that it is shown make it either in terms of photoelectric conversion, or in waste
There is good actual application prospect in degradation treatment.
In numerous semiconductor nano materials, TiO2Nano particle is because it is with unique photoelectrochemical behaviour, excellent
Thermal stability, biologically inert, nontoxic and preparation simplicity etc., attracted wide public concern in fields such as optical electro-chemistry.But
Due to TiO2Nano particle forbidden band itself is wide, and not only the easily compound but also service life is shorter for the electron-hole pair of generation, photoresponse model
It encloses relatively narrow, its optical electro-chemistry activity is made to receive certain limitation.Therefore, how to improve TiO2The optical electro-chemistry of nano particle
It can, it has also become TiO2Important a research direction and research hotspot in optical electro-chemistry field.
But the preparation of existing titanium dioxide optical catalyst there are nanotube lengths short and easy to reunite problem, while stone
Black alkene lamella has been accumulated, and photocatalysis performance has been seriously affected.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation side of titanium dioxide-graphene nanocomposite material
Method is able to solve problems of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of titanium dioxide-graphene nanocomposite material, to overcome
Deficiency in the prior art.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of titanium dioxide-graphene nanocomposite material, comprising:
(1) 40mL dehydrated alcohol is added into 5mL graphene oxide suspension, after ultrasonic disperse is uniform, titanium source, alkali is added
Liquid, 60~90min of magnetic agitation obtain mixed solution；
(2) mixed solution is transferred in autoclave under the conditions of 90~220 DEG C reaction 12~for 24 hours, then in drying
1~2h of heated at constant temperature, cooled to room temperature obtain mixture suspension under the conditions of 60~80 DEG C in case；
(3) mixture suspension is centrifugated, collects sample, use deionized water, washes of absolute alcohol sample respectively, in
Dry drying, calcines 1.5h in 400~450 DEG C of Muffle furnace under the conditions of 50~60 DEG C, obtains titanium dioxide-graphene nano
Composite material.
Preferably, in step (1), the preparation method of the graphene oxide suspension includes: 1) to set 1000mL beaker
In ice-water bath, the 300ml concentrated sulfuric acid, 8g graphite are sequentially added, 6g sodium nitrate stirs 1~2h；Temperature is being kept to be lower than 10 DEG C
Under the conditions of, 30g potassium permanganate is slowly added in beaker, 1~2h is stirred, removes ice-water bath, magnetic force under the conditions of 20~30 DEG C
72~120h is stirred, thick liquid is obtained；2) sulfuric acid of 500mL5wt% is added while stirring into thick liquid, continues to stir
1~2h, the hydrogen peroxide and deionized water for adding 20g30wt% continue 1~2h of stirring, stand 12~for 24 hours, obtain product；3)
Product is used to 3% dilute hydrochloric acid, distillation washing, centrifugation respectively, removal precipitating obtains graphene oxide suspension.
Preferably, the titanium source is selected from one of butyl titanate and titanium dioxide.
Preferably, the lye is selected from sodium hydrate aqueous solution and/or potassium hydroxide aqueous solution.
Preferably, in step (2), the autoclave is the enclosed high pressure reaction kettle of polytetrafluoroethylene (PTFE) stainless steel.
Compared with the prior art, the advantages of the present invention are as follows: in the present invention, it is made by using the method that graphene is added
Composite material specific surface area be 185m2/ g increases the contact area of titanium dioxide and pollutant in composite material, simultaneously
Titania nanoparticles are uniformly dispersed, to facilitate the photocatalysis effect of enhancing titanium dioxide.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of titanium dioxide-graphene nanocomposite material, comprising:
(1) 40mL dehydrated alcohol is added into 5mL graphene oxide suspension, after ultrasonic disperse is uniform, titanium source, alkali is added
Liquid, 60~90min of magnetic agitation obtain mixed solution；
(2) mixed solution is transferred in autoclave under the conditions of 90~220 DEG C reaction 12~for 24 hours, then in drying
1~2h of heated at constant temperature, cooled to room temperature obtain mixture suspension under the conditions of 60~80 DEG C in case；
(3) mixture suspension is centrifugated, collects sample, use deionized water, washes of absolute alcohol sample respectively, in
Dry drying, calcines 1.5h in 400~450 DEG C of Muffle furnace under the conditions of 50~60 DEG C, obtains titanium dioxide-graphene nano
Composite material.
In above-mentioned steps (1), the titanium source is selected from one of butyl titanate and titanium dioxide, and the lye is selected from hydrogen-oxygen
Change sodium water solution and/or potassium hydroxide aqueous solution.
In above-mentioned steps (2), the autoclave is the enclosed high pressure reaction kettle of polytetrafluoroethylene (PTFE) stainless steel.
In one embodiment, the preparation method of the graphene oxide suspension includes:
1) 1000mL beaker is placed in ice-water bath, sequentially adds the 300ml concentrated sulfuric acid, 8g graphite, 6g sodium nitrate, stirring 1
~2h；Under conditions of keeping temperature to be lower than 10 DEG C, 30g potassium permanganate is slowly added in beaker, 1~2h is stirred, removes ice
Water-bath, 72~120h of magnetic agitation under the conditions of 20~30 DEG C obtain thick liquid；
2) sulfuric acid of 500mL5wt% is added while stirring into thick liquid, continues 1~2h of stirring, adds
The hydrogen peroxide and deionized water of 20g30wt% continues 1~2h of stirring, stand 12~for 24 hours, obtain product；
3) product is used to 3% dilute hydrochloric acid, distillation washing, centrifugation respectively, removal precipitating obtains graphene oxide and suspends
Liquid.
Embodiment
1, the preparation of graphene oxide suspension
1) 1000mL beaker is placed in ice-water bath, sequentially adds the 300ml concentrated sulfuric acid, 8g graphite, 6g sodium nitrate, stirring
2h；Under conditions of keeping temperature to be lower than 10 DEG C, 30g potassium permanganate is slowly added in beaker, 1h is stirred, removes ice-water bath,
Magnetic agitation 120h under the conditions of 250 DEG C obtains thick liquid；
2) sulfuric acid of 500mL5wt% is added while stirring into thick liquid, continues to stir 1.5h, add
The hydrogen peroxide and deionized water of 20g30wt% continues to stir 2h, stands 20h, obtains product；
3) product is used to 3% dilute hydrochloric acid, distillation washing, centrifugation respectively, removal precipitating obtains graphene oxide and suspends
Liquid.
2, titanium dioxide-graphene nanocomposite material preparation
(1) 40mL dehydrated alcohol is added into 5mL graphene oxide suspension, after ultrasonic disperse is uniform, metatitanic acid fourth is added
Ester, sodium hydrate aqueous solution, magnetic agitation 90min obtain mixed solution；
(2) mixed solution is transferred in autoclave under the conditions of 180 DEG C and reacts 16h, then in 80 in drying box
Heated at constant temperature 2h under the conditions of DEG C, cooled to room temperature obtain mixture suspension；
(3) mixture suspension is centrifugated, collects sample, use deionized water, washes of absolute alcohol sample respectively, in
Dry drying, calcines 1.5h in 400~450 DEG C of Muffle furnace under the conditions of 60 DEG C, and it is compound to obtain titanium dioxide-graphene nano
Material.
In the present invention, the specific surface area by using composite material made from the method that graphene is added is 185m2/ g increases
The contact area of titanium dioxide and pollutant in big composite material, while titania nanoparticles are uniformly dispersed, to have
Help enhance the photocatalysis effect of titanium dioxide.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Claims (5)
1. a kind of preparation method of titanium dioxide-graphene nanocomposite material characterized by comprising
(1) 40mL dehydrated alcohol is added into 5mL graphene oxide suspension, after ultrasonic disperse is uniform, titanium source, lye is added,
60~90min of magnetic agitation obtains mixed solution；
(2) mixed solution is transferred in autoclave under the conditions of 90~220 DEG C reaction 12~for 24 hours, then in drying box
1~2h of heated at constant temperature under the conditions of 60~80 DEG C, cooled to room temperature obtain mixture suspension；
(3) mixture suspension is centrifugated, collects sample, use deionized water, washes of absolute alcohol sample respectively, in 50~
Dry drying, calcines 1.5h in 400~450 DEG C of Muffle furnace under the conditions of 60 DEG C, and it is compound to obtain titanium dioxide-graphene nano
Material.
2. the preparation method of titanium dioxide-graphene nanocomposite material according to claim 1, which is characterized in that step
Suddenly in (1), the preparation method of the graphene oxide suspension includes: that 1) 1000mL beaker is placed in ice-water bath, successively plus
Enter the 300ml concentrated sulfuric acid, 8g graphite, 6g sodium nitrate stirs 1~2h；Under conditions of keeping temperature to be lower than 10 DEG C, by 30g Gao Meng
Sour potassium is slowly added in beaker, is stirred 1~2h, is removed ice-water bath, and 72~120h of magnetic agitation under the conditions of 20~30 DEG C is obtained
Thick liquid；2) sulfuric acid of 500mL5wt% is added while stirring into thick liquid, continues 1~2h of stirring, adds
The hydrogen peroxide and deionized water of 20g30wt% continues 1~2h of stirring, stand 12~for 24 hours, obtain product；3) product is used respectively
3% dilute hydrochloric acid distills washing, centrifugation, removal precipitating, acquisition graphene oxide suspension.
3. the preparation method of titanium dioxide-graphene nanocomposite material according to claim 1, which is characterized in that institute
It states titanium source and is selected from one of butyl titanate and titanium dioxide.
4. the preparation method of titanium dioxide-graphene nanocomposite material according to claim 1, which is characterized in that institute
It states lye and is selected from sodium hydrate aqueous solution and/or potassium hydroxide aqueous solution.
5. the preparation method of titanium dioxide-graphene nanocomposite material according to claim 1, which is characterized in that step
Suddenly in (2), the autoclave is the enclosed high pressure reaction kettle of polytetrafluoroethylene (PTFE) stainless steel.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110373891A (en) * | 2019-07-16 | 2019-10-25 | 东华大学 | Load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene and preparation method thereof |
| CN113120890A (en) * | 2021-03-10 | 2021-07-16 | 苏州兴华高新材料科技有限公司 | Preparation method and application of graphene and titanium oxide nanocomposite |
| CN113753946A (en) * | 2021-09-01 | 2021-12-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of titanium dioxide @ graphene @ titanium dioxide anode material, product and application |
| CN114014308A (en) * | 2021-12-13 | 2022-02-08 | 中科悦达(上海)材料科技有限公司 | Preparation method of graphene composite material and graphene composite material |
| CN115532248A (en) * | 2022-03-29 | 2022-12-30 | 徐玲霞 | Preparation method of graphene titanium dioxide compound |
-
2017
- 2017-07-28 CN CN201710631694.2A patent/CN109305668A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110373891A (en) * | 2019-07-16 | 2019-10-25 | 东华大学 | Load bismuth tungstate/visible light-responded composite antibacterial fabric of titanium dioxide/redox graphene and preparation method thereof |
| CN113120890A (en) * | 2021-03-10 | 2021-07-16 | 苏州兴华高新材料科技有限公司 | Preparation method and application of graphene and titanium oxide nanocomposite |
| CN113753946A (en) * | 2021-09-01 | 2021-12-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of titanium dioxide @ graphene @ titanium dioxide anode material, product and application |
| CN114014308A (en) * | 2021-12-13 | 2022-02-08 | 中科悦达(上海)材料科技有限公司 | Preparation method of graphene composite material and graphene composite material |
| CN115532248A (en) * | 2022-03-29 | 2022-12-30 | 徐玲霞 | Preparation method of graphene titanium dioxide compound |
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