CN103691420A - Mesoporous niobium pentoxide/graphene compound photocatalyst prepared by one-step self-assembly method - Google Patents
Mesoporous niobium pentoxide/graphene compound photocatalyst prepared by one-step self-assembly method Download PDFInfo
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- CN103691420A CN103691420A CN201310709272.4A CN201310709272A CN103691420A CN 103691420 A CN103691420 A CN 103691420A CN 201310709272 A CN201310709272 A CN 201310709272A CN 103691420 A CN103691420 A CN 103691420A
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Abstract
The invention discloses a mesoporous niobium pentoxide/graphene compound photocatalyst prepared by a one-step self-assembly method. The preparation method comprises the following steps: (1) preparation of oxidized graphene; and (2) preparation of a mesoporous niobium pentoxide/graphene compound. The mesoporous niobium pentoxide/graphene compound is prepared by the one-step self-assembly method disclosed by the invention, and the prepared compound has a good open-framework structure, an intact crystal form and a large specific surface area. The graphene in the compound has the effects of increasing the specific surface area, improving the electrical conductivity and serving as a carrier. The mesoporous niobium pentoxide and the graphene are effectively combined, so that the photocatalytic performance of niobium pentoxide is remarkably improved, and the photocatalyst has an attractive prospect in the field of organic pollutant degradation and solar-energy conversion.
Description
Technical field
The present invention relates to conductor photocatalysis field, be specifically related to a kind of preparation method of mesoporous niobium pentaoxide/graphene composite photocatalyst.
Background technology
Niobium pentaoxide (Nb
2o
5) as a kind of typical N-shaped semi-conducting material, have that catalytic activity is high, chemical stability good and the advantage such as nontoxic, be widely used in photolysis water hydrogen field.Yet, Nb
2o
5energy gap be 3.4 eV, its corresponding absorbing wavelength is 364.7 nm, absorption bands is confined to ultraviolet region, can only utilize the ultraviolet light of 3%-5% in sunshine, has also limited Nb simultaneously
2o
5photocatalytic applications scope.The composite that semiconductor light-catalyst and material with carbon element form, is considered to one of catalysis material type of tool potentiality to be exploited.Be used at present the material with carbon element compound with semiconductor and mainly contain graphite, carbon black, active carbon, carbon fiber, CNT, fullerene etc.Graphene is the New Two Dimensional carbon nanomaterial of discovered in recent years, the monoatomic layer being connected with sp2 hydridization by carbon atom forms, its basic structural unit is benzene hexatomic ring the most stable in organic material, thickness in monolayer is only 0.35 nm, there is excellent conduction property, mechanical performance and chemical stability, in conjunction with its special monoatomic layer planar structure and high-specific surface area thereof, thereby become carrier material that performance is more excellent and the multifunctional material of electronics or hole-transfer.In recent years, various semiconductor/graphene composite materials are successfully synthesized by scientists.The main method of synthesized semiconductor/graphene composite material has hydro-thermal method, and ultraviolet light is assisted reducing process, ion-exchange etc., however the unexposed step self-assembly method of prior art is prepared mesoporous niobium pentaoxide/graphene composite photocatalyst.
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 niobium pentaoxide/graphene composite photocatalyst.Mainly to solve niobium pentaoxide as the photochemical catalyst problem low to solar energy utilization ratio.
Technical scheme: a kind of preparation method of mesoporous niobium pentaoxide/graphene composite photocatalyst, comprises the following steps:
1) 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.
2) preparation of mesoporous niobium pentaoxide/graphene composite photocatalyst, uses m-Nb
2o
5/ GR represents
Adopt a step self-assembly method legal system for mesoporous niobium pentaoxide/graphene composite photocatalyst; 1g F127 solution is added in 20g absolute ethyl alcohol, stir to clarify, slowly add 5.5mmol NbCl simultaneously
5, stir 30min, then take ratio that mass ratio is 1:0.01-0.1 and add the 0.5mg mL of above-mentioned preparation
-1gO solution, ultrasonic 20min, continues to stir after 30min, then reaction solution is transferred in teflon-lined reactor, 60 ℃ of baking oven ageings 3 days, after ageing finishes, make reactor naturally cooling, take out gained liquid, add appropriate hydrazine hydrate solution to stir 24h at 40 ℃, make graphene oxide be reduced to Graphene, filter, and repeatedly rinse products therefrom 3-5 time by deionized water, finally sample is placed on to anaerobic calcining 5h under 450 ℃ of ar gas environments and, to remove F127 template, obtains m-Nb
2o
5/ GR.
Beneficial effect: the present invention compares with existing technology, has prepared mesoporous niobium pentaoxide/graphene composite photocatalyst by a step self-assembly method.Prepared compound has good pore passage structure, complete crystal formation and larger specific area.Graphene has played increase specific area in this compound, improves the effect of electric conductivity and carrier.Effective combination of mesoporous niobium pentaoxide and Graphene has significantly improved the photocatalysis performance of niobium pentaoxide, at organic pollutant degradation and field of solar energy conversion, has tempting prospect.
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 niobium pentaoxide/graphene composite photocatalyst, comprises the following steps:
1) 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.
2) preparation of mesoporous niobium pentaoxide/graphene composite photocatalyst, uses m-Nb
2o
5/ GR represents
Adopt a step self-assembly method legal system for mesoporous niobium pentaoxide/graphene composite photocatalyst; 1g F127 solution is added in 20g absolute ethyl alcohol, stir to clarify, slowly add 5.5mmol NbCl simultaneously
5, stir 30min, then take ratio that mass ratio is 1:0.01 and add the 0.5mg mL of above-mentioned preparation
-1gO solution, ultrasonic 20min, continues to stir after 30min, then reaction solution is transferred in teflon-lined reactor, 60 ℃ of baking oven ageings 3 days, after ageing finishes, make reactor naturally cooling, take out gained liquid, add appropriate hydrazine hydrate solution to stir 24h at 40 ℃, make graphene oxide be reduced to Graphene, filter, and repeatedly rinse products therefrom 3-5 time by deionized water, finally sample is placed on to anaerobic calcining 5h under 450 ℃ of ar gas environments and, to remove F127 template, obtains m-Nb
2o
5/ GR.
Specific embodiment 2:
A preparation method for mesoporous niobium pentaoxide/graphene composite photocatalyst, comprises the following steps:
1) 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.
2) preparation of mesoporous niobium pentaoxide/graphene composite photocatalyst, uses m-Nb
2o
5/ GR represents
Adopt a step self-assembly method legal system for mesoporous niobium pentaoxide/graphene composite photocatalyst; 1g F127 solution is added in 20g absolute ethyl alcohol, stir to clarify, slowly add 5.5mmol NbCl simultaneously
5, stir 30min, then take ratio that mass ratio is 1:0.02 and add the 0.5mg mL of above-mentioned preparation
-1gO solution, ultrasonic 20min, continues to stir after 30min, then reaction solution is transferred in teflon-lined reactor, 60 ℃ of baking oven ageings 3 days, after ageing finishes, make reactor naturally cooling, take out gained liquid, add appropriate hydrazine hydrate solution to stir 24h at 40 ℃, make graphene oxide be reduced to Graphene, filter, and repeatedly rinse products therefrom 3-5 time by deionized water, finally sample is placed on to anaerobic calcining 5h under 450 ℃ of ar gas environments and, to remove F127 template, obtains m-Nb
2o
5/ GR.
Specific embodiment 3:
A preparation method for mesoporous indium sesquioxide/redox graphene composite photo-catalyst, comprises the following steps:
1) 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.
2) preparation of mesoporous niobium pentaoxide/graphene composite photocatalyst, uses m-Nb
2o
5/ GR represents
Adopt a step self-assembly method legal system for mesoporous niobium pentaoxide/graphene composite photocatalyst; 1g F127 solution is added in 20g absolute ethyl alcohol, stir to clarify, slowly add 5.5mmol NbCl simultaneously
5, stir 30min, then take ratio that mass ratio is 1:0.03 and add the 0.5mg mL of above-mentioned preparation
-1gO solution, ultrasonic 20min, continues to stir after 30min, then reaction solution is transferred in teflon-lined reactor, 60 ℃ of baking oven ageings 3 days, after ageing finishes, make reactor naturally cooling, take out gained liquid, add appropriate hydrazine hydrate solution to stir 24h at 40 ℃, make graphene oxide be reduced to Graphene, filter, and repeatedly rinse products therefrom 3-5 time by deionized water, finally sample is placed on to anaerobic calcining 5h under 450 ℃ of ar gas environments and, to remove F127 template, obtains m-Nb
2o
5/ GR.
Specific embodiment 4:
A preparation method for mesoporous niobium pentaoxide/graphene composite photocatalyst, comprises the following steps:
1) 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.
2) preparation of mesoporous niobium pentaoxide/graphene composite photocatalyst, uses m-Nb
2o
5/ GR represents
Adopt a step self-assembly method legal system for mesoporous niobium pentaoxide/graphene composite photocatalyst; 1g F127 solution is added in 20g absolute ethyl alcohol, stir to clarify, slowly add 5.5mmol NbCl simultaneously
5, stir 30min, then take ratio that mass ratio is 1:0.05 and add the 0.5mg mL of above-mentioned preparation
-1gO solution, ultrasonic 20min, continues to stir after 30min, then reaction solution is transferred in teflon-lined reactor, 60 ℃ of baking oven ageings 3 days, after ageing finishes, make reactor naturally cooling, take out gained liquid, add appropriate hydrazine hydrate solution to stir 24h at 40 ℃, make graphene oxide be reduced to Graphene, filter, and repeatedly rinse products therefrom 3-5 time by deionized water, finally sample is placed on to anaerobic calcining 5h under 450 ℃ of ar gas environments and, to remove F127 template, obtains m-Nb
2o
5/ GR.
Claims (1)
1. a preparation method for mesoporous niobium pentaoxide/graphene composite photocatalyst, is characterized in that: comprise the following steps:
1) 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;
2) preparation of mesoporous niobium pentaoxide/graphene composite photocatalyst, uses m-Nb
2o
5/ GR represents
Adopt a step self-assembly method legal system for mesoporous niobium pentaoxide/graphene composite photocatalyst; 1g F127 solution is added in 20g absolute ethyl alcohol, stir to clarify, slowly add 5.5mmol NbCl simultaneously
5, stir 30min, then take ratio that mass ratio is 1:0.01-0.1 and add the 0.5mg mL of above-mentioned preparation
-1gO solution, ultrasonic 20min, continues to stir after 30min, then reaction solution is transferred in teflon-lined reactor, 60 ℃ of baking oven ageings 3 days, after ageing finishes, make reactor naturally cooling, take out gained liquid, add appropriate hydrazine hydrate solution to stir 24h at 40 ℃, make graphene oxide be reduced to Graphene, filter, and repeatedly rinse products therefrom 3-5 time by deionized water, finally sample is placed on to anaerobic calcining 5h under 450 ℃ of ar gas environments and, to remove F127 template, obtains m-Nb
2o
5/ GR.
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| CN106809879A (en) * | 2017-02-27 | 2017-06-09 | 湖南工业大学 | A kind of niobium pentoxide nano stick material with regular hollow quadratic box-like and its preparation method and application |
| CN109830660A (en) * | 2019-01-15 | 2019-05-31 | 广州特种承压设备检测研究院 | Graphene/niobium pentaoxide combination electrode material and preparation method thereof |
| CN109980210A (en) * | 2019-04-19 | 2019-07-05 | 陕西科技大学 | A kind of niobium pentaoxide three-dimensional doped graphene composite material and preparation method and application |
| CN110323429A (en) * | 2019-07-08 | 2019-10-11 | 中南大学 | Niobium pentaoxide/redox graphene composite negative pole material preparation method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105457633A (en) * | 2014-10-05 | 2016-04-06 | 青岛鑫润土苗木专业合作社 | Preparation method of highly-active mesoporous photocatalyst |
| CN106809879A (en) * | 2017-02-27 | 2017-06-09 | 湖南工业大学 | A kind of niobium pentoxide nano stick material with regular hollow quadratic box-like and its preparation method and application |
| CN109830660A (en) * | 2019-01-15 | 2019-05-31 | 广州特种承压设备检测研究院 | Graphene/niobium pentaoxide combination electrode material and preparation method thereof |
| CN109980210A (en) * | 2019-04-19 | 2019-07-05 | 陕西科技大学 | A kind of niobium pentaoxide three-dimensional doped graphene composite material and preparation method and application |
| CN109980210B (en) * | 2019-04-19 | 2021-01-29 | 陕西科技大学 | Niobium pentoxide three-dimensional doped graphene composite material and preparation method and application thereof |
| CN110323429A (en) * | 2019-07-08 | 2019-10-11 | 中南大学 | Niobium pentaoxide/redox graphene composite negative pole material preparation method |
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Application publication date: 20140402 |