CN103691418A - Preparation of mesoporous indium sesquioxide/reduced oxidized graphene compound photocatalyst - Google Patents
Preparation of mesoporous indium sesquioxide/reduced oxidized graphene compound photocatalyst Download PDFInfo
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- CN103691418A CN103691418A CN201310709326.7A CN201310709326A CN103691418A CN 103691418 A CN103691418 A CN 103691418A CN 201310709326 A CN201310709326 A CN 201310709326A CN 103691418 A CN103691418 A CN 103691418A
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Abstract
The invention discloses a preparation method of mesoporous indium sesquioxide/reduced oxidized graphene compound photocatalyst. The preparation method comprises the following steps: (1) the preparation of mesoporous indium sesquioxide; (2) the preparation of oxidized graphene; and (3) the preparation of mesoporous indium sesquioxide/reduced oxidized graphene compound. The mesoporous indium sesquioxide prepared by the method disclosed by the invention has a regular mesoporous passage structure, great specific surface area and good crystal form. The compounding of the mesoporous indium sesquioxide and the reduced oxidized graphene is capable of effectively inhibiting the compound possibility of photoelectrons-hole pairs, and the performance of photocatalytically degrading the organic pollutant of the indium sesquioxide is improved.
Description
Technical field
The present invention relates to conductor photocatalysis field, be specifically related to a kind of preparation method of mesoporous indium sesquioxide/redox graphene composite photo-catalyst.
Background technology
Quantity research shows greatly, and photocatalytic method can be effectively by organic pollutant degradations such as hydro carbons, halogenated organic matters, dyestuff, agricultural chemicals, phenols, aromatic hydrocarbons, and final mineralising is CO
2and H
2o.Therefore, photocatalysis technology has condition and coincide, and eliminates organic pollution thorough, the features such as non-secondary pollution.Along with the development of photocatalysis technology, the preparation of photochemical catalyst more and more receives the concern of scientists.Indium sesquioxide (In
2o
3, be Eg=2.8eV) one of the photochemical catalyst of recent scientists broad research, yet simple nanometer indium sesquioxide photocatalytic activity is lower, therefore can not be effectively by pollutant mineralising.In order to improve the catalytic activity of indium sesquioxide, must improve himself appearance structure, reduce its energy gap.Based on above-mentioned consideration, a kind of preparation method of mesoporous indium sesquioxide/redox graphene composite photo-catalyst is proposed, be intended to improve the photocatalytic activity of indium sesquioxide, effectively degradable organic pollutant.
Summary of the invention
Goal of the invention: the present invention, in order to solve the deficiencies in the prior art, provides a kind of preparation method of mesoporous indium sesquioxide/redox graphene composite photo-catalyst.Be mainly to solve the low problem of indium sesquioxide photocatalysis efficiency, improve the catalytic activity of indium sesquioxide, and expand the range of application of indium sesquioxide.
Technical scheme: a kind of preparation method of mesoporous indium sesquioxide/redox graphene composite photo-catalyst, comprises the following steps:
1) mesoporous indium sesquioxide, uses m-In
2o
3represent
Getting 1.0gKIT-6 is dissolved in 15mL ethanol as silica-based template, strong agitation 30min, in above-mentioned solution, add 2.0g indium nitrate again, continue to stir 2h, it is mixed, then with Rotary Evaporators, at 40 ℃, solvent evaporate to dryness is obtained to white powder, by the white powder obtaining roasting 5h under 550 ℃ of conditions, with the NaOH of 2M, at 60 ℃, go down except silicon substrate KIT-6, filter and obtain product, with deionized water and alcohol mixeding liquid, wash 2-3 time again, at 100 ℃ of dry 1h, obtain product m-In
2o
3, prepare stand-by.
2) preparation of graphene oxide, represents with GO
Get 1.0g graphite powder (<30 μ m) and add in 100mL water, then add respectively 0.5g NaNO
3, 24.0mL H
2sO
4with 3.0g KMnO
4, ultrasonic concussion 10min, is placed in ice bath by reactant liquor, and strong agitation 30min takes out and at 25 ℃, continues to stir 30min, adds 46mL deionized water dilute reaction solution, is heated to 98 ℃ and continues to stir 10min, then in reactant liquor, add 10mL H
2o
2with 140mL H
2o, filtering reacting liquid, rinses gained reactant 3-5 time repeatedly by 5% HCl and deionized water respectively, and products therefrom is placed in to dry 10h at 80 ℃, makes graphene oxide (GO), before use, gets a certain amount of GO, is dissolved in deionized water, is made into 0.5mg mL
-1solution, ultrasonic concussion 2h, then use the rotating speed centrifugation 10min of 11000rpm, pipettes supernatant liquor stand-by.
3) preparation of mesoporous indium sesquioxide/redox graphene compound, uses m-In
2o
3/ RGO represents
The m-In that above-mentioned steps is prepared
2o
3with 0.5mg mL
-1gO solution take mass ratio 1:0.1-0.5 as proportioning, be added in the beaker of 100mL, then add 50mL ethanolic solution, stir 30min, then by the ultrasonic processing of mixture 30min, under the interior 120 ℃ of conditions of immigration 100mL autoclave, ageing is 2 days, taking-up is cooled to room temperature, and the composite of filtered and recycled gained cleans 3-5 time with deionized water and ethanol respectively, and dry at 40 ℃, the product labelling obtaining is m-In
2o
3/ RGO.
Beneficial effect: the present invention compares with existing technology, has successfully prepared well-regulated mesopore orbit structure, larger specific area and the m-In of crystalline structure preferably by hydro-thermal method
2o
3/ RGO composite photo-catalyst.The effective compound of mesoporous indium sesquioxide and redox graphene can reduce the right compound probability in light induced electron-hole, improves the performance of the photocatalysis degradation organic contaminant of indium sesquioxide.
The specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail.
Specific embodiment 1:
A preparation method for mesoporous indium sesquioxide/redox graphene composite photo-catalyst, comprises the following steps:
1) mesoporous indium sesquioxide, uses m-In
2o
3represent
Getting 1.0gKIT-6 is dissolved in 15mL ethanol as silica-based template, strong agitation 30min, in above-mentioned solution, add 2.0g indium nitrate again, continue to stir 2h, it is mixed, then with Rotary Evaporators, at 40 ℃, solvent evaporate to dryness is obtained to white powder, by the white powder obtaining roasting 5h under 550 ℃ of conditions, with the NaOH of 2M, at 60 ℃, go down except silicon substrate KIT-6, filter and obtain product, with deionized water and alcohol mixeding liquid, wash 2-3 time again, at 100 ℃ of dry 1h, obtain product m-In
2o
3, prepare stand-by.
2) preparation of graphene oxide, represents with GO
Get 1.0g graphite powder (<30 μ m) and add in 100mL water, then add respectively 0.5g NaNO
3, 24.0mL H
2sO
4with 3.0g KMnO
4, ultrasonic concussion 10min, is placed in ice bath by reactant liquor, and strong agitation 30min takes out and at 25 ℃, continues to stir 30min, adds 46mL deionized water dilute reaction solution, is heated to 98 ℃ and continues to stir 10min, then in reactant liquor, add 10mL H
2o
2with 140mL H
2o, filtering reacting liquid, rinses gained reactant 3-5 time repeatedly by 5% HCl and deionized water respectively, and products therefrom is placed in to dry 10h at 80 ℃, makes graphene oxide (GO), before use, gets a certain amount of GO, is dissolved in deionized water, is made into 0.5mg mL
-1solution, ultrasonic concussion 2h, then use the rotating speed centrifugation 10min of 11000rpm, pipettes supernatant liquor stand-by.
3) preparation of mesoporous indium sesquioxide/redox graphene compound, uses m-In
2o
3/ RGO represents
The m-In that above-mentioned steps is prepared
2o
3with 0.5mg mL
-1gO solution take mass ratio 1:0.1 as proportioning, be added in the beaker of 100mL, then add 50mL ethanolic solution, stir 30min, then by the ultrasonic processing of mixture 30min, under the interior 120 ℃ of conditions of immigration 100mL autoclave, ageing is 2 days, taking-up is cooled to room temperature, and the composite of filtered and recycled gained cleans 3-5 time with deionized water and ethanol respectively, and dry at 40 ℃, the product labelling obtaining is m-In
2o
3/ RGO.
Specific embodiment 2:
A preparation method for mesoporous indium sesquioxide/redox graphene composite photo-catalyst, comprises the following steps:
1) mesoporous indium sesquioxide, uses m-In
2o
3represent
Getting 1.0gKIT-6 is dissolved in 15mL ethanol as silica-based template, strong agitation 30min, in above-mentioned solution, add 2.0g indium nitrate again, continue to stir 2h, it is mixed, then with Rotary Evaporators, at 40 ℃, solvent evaporate to dryness is obtained to white powder, by the white powder obtaining roasting 5h under 550 ℃ of conditions, with the NaOH of 2M, at 60 ℃, go down except silicon substrate KIT-6, filter and obtain product, with deionized water and alcohol mixeding liquid, wash 2-3 time again, at 100 ℃ of dry 1h, obtain product m-In
2o
3, prepare stand-by.
2) preparation of graphene oxide, represents with GO
Get 1.0g graphite powder (<30 μ m) and add in 100mL water, then add respectively 0.5g NaNO
3, 24.0mL H
2sO
4with 3.0g KMnO
4, ultrasonic concussion 10min, is placed in ice bath by reactant liquor, and strong agitation 30min takes out and at 25 ℃, continues to stir 30min, adds 46mL deionized water dilute reaction solution, is heated to 98 ℃ and continues to stir 10min, then in reactant liquor, add 10mL H
2o
2with 140mL H
2o, filtering reacting liquid, rinses gained reactant 3-5 time repeatedly by 5% HCl and deionized water respectively, and products therefrom is placed in to dry 10h at 80 ℃, makes graphene oxide (GO), before use, gets a certain amount of GO, is dissolved in deionized water, is made into 0.5mg mL
-1solution, ultrasonic concussion 2h, then use the rotating speed centrifugation 10min of 11000rpm, pipettes supernatant liquor stand-by.
3) preparation of mesoporous indium sesquioxide/redox graphene compound, uses m-In
2o
3/ RGO represents
The m-In that above-mentioned steps is prepared
2o
3with 0.5mg mL
-1gO solution take mass ratio 1:0.2 as proportioning, be added in the beaker of 100mL, then add 50mL ethanolic solution, stir 30min, then by the ultrasonic processing of mixture 30min, under the interior 120 ℃ of conditions of immigration 100mL autoclave, ageing is 2 days, taking-up is cooled to room temperature, and the composite of filtered and recycled gained cleans 3-5 time with deionized water and ethanol respectively, and dry at 40 ℃, the product labelling obtaining is m-In
2o
3/ RGO.
Specific embodiment 3:
A preparation method for mesoporous indium sesquioxide/redox graphene composite photo-catalyst, comprises the following steps:
1) mesoporous indium sesquioxide, uses m-In
2o
3represent
Getting 1.0gKIT-6 is dissolved in 15mL ethanol as silica-based template, strong agitation 30min, in above-mentioned solution, add 2.0g indium nitrate again, continue to stir 2h, it is mixed, then with Rotary Evaporators, at 40 ℃, solvent evaporate to dryness is obtained to white powder, by the white powder obtaining roasting 5h under 550 ℃ of conditions, with the NaOH of 2M, at 60 ℃, go down except silicon substrate KIT-6, filter and obtain product, with deionized water and alcohol mixeding liquid, wash 2-3 time again, at 100 ℃ of dry 1h, obtain product m-In
2o
3, prepare stand-by.
2) preparation of graphene oxide, represents with GO
Get 1.0g graphite powder (<30 μ m) and add in 100mL water, then add respectively 0.5g NaNO
3, 24.0mL H
2sO
4with 3.0g KMnO
4, ultrasonic concussion 10min, is placed in ice bath by reactant liquor, and strong agitation 30min takes out and at 25 ℃, continues to stir 30min, adds 46mL deionized water dilute reaction solution, is heated to 98 ℃ and continues to stir 10min, then in reactant liquor, add 10mL H
2o
2with 140mL H
2o, filtering reacting liquid, rinses gained reactant 3-5 time repeatedly by 5% HCl and deionized water respectively, and products therefrom is placed in to dry 10h at 80 ℃, makes graphene oxide (GO), before use, gets a certain amount of GO, is dissolved in deionized water, is made into 0.5mg mL
-1solution, ultrasonic concussion 2h, then use the rotating speed centrifugation 10min of 11000rpm, pipettes supernatant liquor stand-by.
3) preparation of mesoporous indium sesquioxide/redox graphene compound, uses m-In
2o
3/ RGO represents
The m-In that above-mentioned steps is prepared
2o
3with 0.5mg mL
-1gO solution take mass ratio 1:0.3 as proportioning, be added in the beaker of 100mL, then add 50mL ethanolic solution, stir 30min, then by the ultrasonic processing of mixture 30min, under the interior 120 ℃ of conditions of immigration 100mL autoclave, ageing is 2 days, taking-up is cooled to room temperature, and the composite of filtered and recycled gained cleans 3-5 time with deionized water and ethanol respectively, and dry at 40 ℃, the product labelling obtaining is m-In
2o
3/ RGO.
Specific embodiment 4:
A preparation method for mesoporous indium sesquioxide/redox graphene composite photo-catalyst, comprises the following steps:
1) mesoporous indium sesquioxide, uses m-In
2o
3represent
Getting 1.0gKIT-6 is dissolved in 15mL ethanol as silica-based template, strong agitation 30min, in above-mentioned solution, add 2.0g indium nitrate again, continue to stir 2h, it is mixed, then with Rotary Evaporators, at 40 ℃, solvent evaporate to dryness is obtained to white powder, by the white powder obtaining roasting 5h under 550 ℃ of conditions, with the NaOH of 2M, at 60 ℃, go down except silicon substrate KIT-6, filter and obtain product, with deionized water and alcohol mixeding liquid, wash 2-3 time again, at 100 ℃ of dry 1h, obtain product m-In
2o
3, prepare stand-by.
2) preparation of graphene oxide, represents with GO
Get 1.0g graphite powder (<30 μ m) and add in 100mL water, then add respectively 0.5g NaNO
3, 24.0mL H
2sO
4with 3.0g KMnO
4, ultrasonic concussion 10min, is placed in ice bath by reactant liquor, and strong agitation 30min takes out and at 25 ℃, continues to stir 30min, adds 46mL deionized water dilute reaction solution, is heated to 98 ℃ and continues to stir 10min, then in reactant liquor, add 10mL H
2o
2with 140mL H
2o, filtering reacting liquid, rinses gained reactant 3-5 time repeatedly by 5% HCl and deionized water respectively, and products therefrom is placed in to dry 10h at 80 ℃, makes graphene oxide (GO), before use, gets a certain amount of GO, is dissolved in deionized water, is made into 0.5mg mL
-1solution, ultrasonic concussion 2h, then use the rotating speed centrifugation 10min of 11000rpm, pipettes supernatant liquor stand-by.
3) preparation of mesoporous indium sesquioxide/redox graphene compound, uses m-In
2o
3/ RGO represents
The m-In that above-mentioned steps is prepared
2o
3with 0.5mg mL
-1gO solution take mass ratio 1:0.5 as proportioning, be added in the beaker of 100mL, then add 50mL ethanolic solution, stir 30min, then by the ultrasonic processing of mixture 30min, under the interior 120 ℃ of conditions of immigration 100mL autoclave, ageing is 2 days, taking-up is cooled to room temperature, and the composite of filtered and recycled gained cleans 3-5 time with deionized water and ethanol respectively, and dry at 40 ℃, the product obtaining is designated as m-In
2o
3/ RGO.
Claims (1)
1. a preparation method for mesoporous indium sesquioxide/redox graphene composite photo-catalyst, is characterized in that: comprise the following steps:
1) mesoporous indium sesquioxide, uses m-In
2o
3represent
Getting 1.0gKIT-6 is dissolved in 15mL ethanol as silica-based template, strong agitation 30min, in above-mentioned solution, add 2.0g indium nitrate again, continue to stir 2h, it is mixed, then with Rotary Evaporators, at 40 ℃, solvent evaporate to dryness is obtained to white powder, by the white powder obtaining roasting 5h under 550 ℃ of conditions, with the NaOH of 2M, at 60 ℃, go down except silicon substrate KIT-6, filter and obtain product, with deionized water and alcohol mixeding liquid, wash 2-3 time again, at 100 ℃ of dry 1h, obtain product m-In
2o
3, prepare stand-by;
2) preparation of graphene oxide, represents with GO
Get 1.0g graphite powder (<30 μ m) and add in 100mL water, then add respectively 0.5g NaNO
3, 24.0mL H
2sO
4with 3.0g KMnO
4, ultrasonic concussion 10min, is placed in ice bath by reactant liquor, and strong agitation 30min takes out and at 25 ℃, continues to stir 30min, adds 46mL deionized water dilute reaction solution, is heated to 98 ℃ and continues to stir 10min, then in reactant liquor, add 10mL H
2o
2with 140mL H
2o, filtering reacting liquid, rinses gained reactant 3-5 time repeatedly by 5% HCl and deionized water respectively, and products therefrom is placed in to dry 10h at 80 ℃, makes graphene oxide (GO), before use, gets a certain amount of GO, is dissolved in deionized water, is made into 0.5mg mL
-1solution, ultrasonic concussion 2h, then use the rotating speed centrifugation 10min of 11000rpm, pipettes supernatant liquor stand-by;
3) preparation of mesoporous indium sesquioxide/redox graphene compound, uses m-In
2o
3/ RGO represents
The m-In that above-mentioned steps is prepared
2o
3with 0.5mg mL
-1gO solution take mass ratio 1:0.1-0.5 as proportioning, be added in the beaker of 100mL, then add 50mL ethanolic solution, stir 30min, then by the ultrasonic processing of mixture 30min, under the interior 120 ℃ of conditions of immigration 100mL autoclave, ageing is 2 days, taking-up is cooled to room temperature, and the composite of filtered and recycled gained cleans 3-5 time with deionized water and ethanol respectively, and dry at 40 ℃, the product labelling obtaining is m-In
2o
3/ RGO.
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Cited By (7)
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| CN103934014A (en) * | 2014-04-25 | 2014-07-23 | 苏州大学 | Method for preparing nitrogen-doped indium oxide nanorod/graphene oxide composite photocatalyst |
| CN104495811A (en) * | 2014-12-12 | 2015-04-08 | 盐城市新能源化学储能与动力电源研究中心 | Graphene composite material and preparation method thereof |
| CN107340367A (en) * | 2017-07-11 | 2017-11-10 | 济南大学 | A kind of preparation method of three-dimensional rGO/In2O3 composite room temperature gas sensitive |
| CN110215916A (en) * | 2019-04-24 | 2019-09-10 | 中国科学技术大学 | A kind of indium oxide nanocatalyst, preparation method and its application grown on rGO |
| CN112774659A (en) * | 2021-01-25 | 2021-05-11 | 中国计量大学 | Graphene/indium oxide hydride composite photocatalyst and preparation method thereof |
| CN113092545A (en) * | 2021-04-13 | 2021-07-09 | 哈尔滨理工大学 | Based on CuO/In2O3Preparation method of modified graphene MEMS gas sensor |
| CN113842906A (en) * | 2020-06-25 | 2021-12-28 | 现代自动车株式会社 | Catalyst for converting carbon dioxide into methanol by hydrogenation and method for preparing same |
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| CN103934014A (en) * | 2014-04-25 | 2014-07-23 | 苏州大学 | Method for preparing nitrogen-doped indium oxide nanorod/graphene oxide composite photocatalyst |
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| CN113842906A (en) * | 2020-06-25 | 2021-12-28 | 现代自动车株式会社 | Catalyst for converting carbon dioxide into methanol by hydrogenation and method for preparing same |
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| CN113092545A (en) * | 2021-04-13 | 2021-07-09 | 哈尔滨理工大学 | Based on CuO/In2O3Preparation method of modified graphene MEMS gas sensor |
| CN113092545B (en) * | 2021-04-13 | 2022-12-09 | 哈尔滨理工大学 | Based on CuO/In 2 O 3 Preparation method of modified graphene MEMS gas sensor |
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Application publication date: 20140402 |