CN103084198A - Preparation method of efficient photocatalyst nitrogen doped meso-porous niobium pentoxide - Google Patents

Preparation method of efficient photocatalyst nitrogen doped meso-porous niobium pentoxide Download PDF

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CN103084198A
CN103084198A CN2013100438581A CN201310043858A CN103084198A CN 103084198 A CN103084198 A CN 103084198A CN 2013100438581 A CN2013100438581 A CN 2013100438581A CN 201310043858 A CN201310043858 A CN 201310043858A CN 103084198 A CN103084198 A CN 103084198A
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preparation
weight portion
photocatalyst
niobium pentoxide
porous niobium
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黄徽
何晓春
王成
刘瑞霞
严进
孙强
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Nantong Vocational College
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Nantong Vocational College
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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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

The invention discloses a preparation method of an efficient photocatalyst nitrogen doped meso-porous niobium pentoxide. The preparation method comprises a step of the preparation of meso-porous niobium pentoxide and a step of the preparation of nitrogen doped meso-porous niobium pentoxide. The preparation method can effectively develop the light response range of a niobium pentoxide photocatalyst, substantially enhance the catalytic activity of a photocatalyst under the condition of the sunlight, and further enlarge the application field of the niobium pentoxide photocatalyst. The efficient photocatalyst nitrogen doped meso-porous niobium pentoxide has the characteristics of rapid and effective decomposition of water, high recovery rate and no secondary pollution, and is an environmentally-friendly photocatalyst.

Description

The preparation method of the doped meso-porous niobium pentaoxide high efficiency photocatalyst of nitrogen
Technical field
The present invention relates to the semiconductor light-catalyst preparation field, but be specifically related to a kind of preparation method of the doped meso-porous niobium pentaoxide high efficiency photocatalyst of nitrogen of decomposition water.
Background technology
Hydrogen Energy is a kind of energy of green non-pollution, is the energy that is widely adopted of a new generation after the non-renewable energies such as coal, oil and natural gas, has cleaning, energy storage is high, the source is abundant, the service efficiency advantages of higher.So human society demands seeking a kind of hydrogen producing technology that can realize suitability for industrialized production urgently.
Photochemical catalyzing is that a kind of catalysis material that utilizes absorbs solar energy, converts solar energy into chemical energy and then is used for the emerging technology of water-splitting hydrogen production.Its advantage is: (1) utilizes solar energy cheap, that reserves enrich and clean.(2) directly solar energy is converted into chemical energy, does not need to provide the more energy.(3) hydrogen is reduced to water after energy is emitted in oxidation as the energy, be a kind of harmless benign cycle, and tellurian water resource is very abundant.Semiconductor catalyst photolysis water hydrogen method has advantages of practicality, cleaning, economy.
Realize with TiO from nineteen forty-two Fujishima etc. 2Since the semi-conducting electrode hydrogen production by water decomposition, all obtained great development in the resonable application of touching upon of photoelectrocatalysis hydrogen manufacturing.From the angle of environment, TiO 2Have inexpensive, nontoxic, good stability, be easy to the characteristics such as recovery and be widely used.But, TiO 2Can be with greater band gap (being about 3.2ev), need just to show photocatalytic activity under UV-irradiation, and ultraviolet light only accounts for 6.5% left and right of sunshine total energy spectrum, lower to the utilization rate of sunshine.In addition, the compound quantum yield that also causes of light induced electron and electron hole is low.Along with the application of multiphase photocatalysis hydrogen manufacturing and the raising of photocatalysis efficiency, the development of new photochemical catalyst is expanded the study hotspot that its photoresponse scope becomes the photocatalysis hydrogen production field.
Research is found, Nb 2O 5Can band gap be 3.4eV, with TiO 2Can band gap (being about 3.2ev) close, advantage is to compare TiO 2Have more stable photocatalysis performance, but need to just show higher photocatalytic activity under UV-irradiation.Can make Nb by nonmetal doping 2O 5Can band gap narrow down, more effective absorption sunshine is expanded its photoresponse scope.In addition, the specific surface area size of catalyst and crystallization degree are also the key factors that affects the conductor photocatalysis activity, mesoporous Nb 2O 5Have the advantages that specific area is large, degree of crystallinity is high, the duct is regular, can effectively suppress the compound of light induced electron and hole in its surface light catalytic process, greatly increased catalytic active site, further improved photocatalysis performance.
Summary of the invention
Goal of the invention: the present invention provides in order to solve the deficiencies in the prior art the preparation method who has the doped meso-porous niobium pentaoxide of nitrogen of high catalytic activity under a kind of effective sunshine.
Technical scheme: the preparation method of the doped meso-porous niobium pentaoxide high efficiency photocatalyst of a kind of nitrogen comprises the following steps:
1) preparation of mesoporous niobium pentaoxide, use m-Nb 2O 5Represent
A) adopt the synthetic m-Nb of self-assembly method 2O 5
The F127 that takes the 0.1-2.0 weight portion is dissolved in 1.0-20.0 weight portion absolute ethyl alcohol with the magnetic stirring apparatus of the rotating speed of 500-1000rpm and processes 10min, after F127 dissolves fully, add 0.1-1.5 weight portion columbium pentachloride strong agitation 20min, the color of the solution becomes colorless transparently by faint yellow, dropwise adds the CaCl of 0.5mol/L 2Solution 0.5-1.0ml, and make Nb after continuing to stir 10min 2O 5Colloidal sol;
B) with Nb 2O 5Colloidal sol is placed in autoclave, ageing 72h under 60 ℃ of conditions, and 40 ℃ of dry 5h put into Muffle furnace and heat-treat, and are warming up to 450 ℃ with the speed of 5 ℃/min, keep naturally being down to room temperature after 5h, make m-Nb 2O 5Product;
2) preparation of the doped meso-porous niobium pentaoxide of nitrogen, use N-m-Nb 2O 5Represent
Take respectively the m-Nb of 0.5-5.0 weight portion 2O 5With 0.05-1.0 weight portion ammonium chloride, be dissolved in 1-10ml water, process 5h with the magnetic stirring apparatus of the rotating speed of 500-1000rpm, filter and obtain N-m-Nb 2O 5Thick product, with rare nitric acid and deionized water washing 3 times, dry 12h under 70 ℃ of conditions puts into Muffle furnace and heat-treats respectively, is warming up to 400 ℃ with the speed of 5 ℃/min, naturally is down to room temperature after maintenance 2h, makes N-m-Nb 2O 5Product.
Beneficial effect: the present invention compares with existing technology, successfully synthesized the doped meso-porous niobium pentaoxide photochemical catalyst of nitrogen with bigger serface and orderly duct, solve the low difficult problem of niobium pentaoxide photocatalyst activity, can effectively expand the photoresponse scope of niobium pentaoxide, improve the catalytic activity of photochemical catalyst under sunlight conditions, further enlarge the suitable application area of niobium pentaoxide photochemical catalyst.Decomposition water quickly and efficiently, catalyst recovery yield is high, does not cause secondary pollution, is a kind of photochemical catalyst of green.
The specific embodiment
The present invention will be described in detail below in conjunction with specific embodiment.
Specific embodiment 1:
The preparation method of the doped meso-porous niobium pentaoxide high efficiency photocatalyst of a kind of nitrogen comprises the following steps:
1) preparation of mesoporous niobium pentaoxide, use m-Nb 2O 5Represent
A) adopt the synthetic m-Nb of self-assembly method 2O 5
The F127 that takes 0.1g is dissolved in the 1.0g absolute ethyl alcohol with the magnetic stirring apparatus of the rotating speed of 500-1000rpm and processes 10min, after F127 dissolves fully, add 0.1g columbium pentachloride strong agitation 20min, the color of the solution becomes colorless well-illuminatedly by faint yellow, dropwise adds the CaCl of 0.5mol/L 2Solution 0.5ml, and continuation stirring 10min makes Nb 2O 5Colloidal sol;
B) with Nb 2O 5Colloidal sol is placed in autoclave, ageing 72h under 60 ℃ of conditions, and 40 ℃ of dry 5h put into Muffle furnace and heat-treat, and are warming up to 450 ℃ with the speed of 5 ℃/min, keep naturally being down to room temperature after 5h, make m-Nb 2O 5Product;
2) preparation of the doped meso-porous niobium pentaoxide of nitrogen, use N-m-Nb 2O 5Represent
Take respectively the m-Nb of 0.5g 2O 5With 0.05g ammonium chloride, be dissolved in 10ml water, process 5h with the magnetic stirring apparatus of the rotating speed of 500-1000rpm and filter and obtain N-m-Nb 2O 5Thick product, with rare nitric acid and deionized water washing 3 times, dry 12h under 70 ℃ of conditions puts into Muffle furnace and heat-treats respectively, is warming up to 400 ℃ with the speed of 5 ℃/min, naturally is down to room temperature after maintenance 2h, makes N-m-Nb 2O 5Product.
Specific embodiment 2:
The preparation method of the doped meso-porous niobium pentaoxide high efficiency photocatalyst of a kind of nitrogen comprises the following steps:
A) adopt the synthetic m-Nb of self-assembly method 2O 5
The F127 that takes 2.0g is dissolved in the 20.0g absolute ethyl alcohol with the magnetic stirring apparatus of the rotating speed of 500rpm and processes 10min, after F127 dissolves fully, add 1.5g columbium pentachloride strong agitation 20min, the color of the solution becomes colorless well-illuminatedly by faint yellow, dropwise adds the CaCl of 0.5mol/L 2Solution 1.0ml, and continuation stirring 10min makes Nb 2O 5Colloidal sol;
B) with Nb 2O 5Colloidal sol is placed in autoclave, ageing 72h under 60 ℃ of conditions, and 40 ℃ of dry 5h put into Muffle furnace and heat-treat, and are warming up to 450 ℃ with the speed of 5 ℃/min, keep naturally being down to room temperature after 5h, make m-Nb 2O 5Product;
2) preparation of the doped meso-porous niobium pentaoxide of nitrogen, use N-m-Nb 2O 5Represent
Take respectively the m-Nb of 5.0g 2O 5With 1.0g ammonium chloride, be dissolved in 1ml water, process 5h with the magnetic stirring apparatus of the rotating speed of 500-1000rpm and filter and obtain N-m-Nb 2O 5Thick product, with rare nitric acid and deionized water washing 3 times, dry 12h under 70 ℃ of conditions puts into Muffle furnace and heat-treats respectively, is warming up to 400 ℃ with the speed of 5 ℃/min, naturally is down to room temperature after maintenance 2h, makes N-m-Nb 2O 5Product.
Specific embodiment 3:
The preparation method of the doped meso-porous niobium pentaoxide high efficiency photocatalyst of a kind of nitrogen comprises the following steps:
1) preparation of mesoporous niobium pentaoxide, use m-Nb 2O 5Represent
A) adopt the synthetic m-Nb of self-assembly method 2O 5
The F127 that takes 1.0g is dissolved in the 10.0g absolute ethyl alcohol with the magnetic stirring apparatus of the rotating speed of 1000rpm and processes 10min, after F127 dissolves fully, add 1.0g columbium pentachloride strong agitation 20min, the color of the solution becomes colorless transparently by faint yellow, dropwise adds the CaCl of 0.5mol/L 2Solution 0.5ml, and continuation stirring 10min makes Nb 2O 5Colloidal sol;
B) with Nb 2O 5Colloidal sol is placed in autoclave, ageing 72h under 60 ℃ of conditions, and 40 ℃ of dry 5h put into Muffle furnace and heat-treat, and are warming up to 450 ℃ with the speed of 5 ℃/min, keep naturally being down to room temperature after 5h, make m-Nb 2O 5Product;
2) preparation of the doped meso-porous niobium pentaoxide of nitrogen, use N-m-Nb 2O 5Represent
Take respectively the m-Nb of 4.0g 2O 5With 0.5g ammonium chloride, be dissolved in 5ml water, process 5h with the magnetic stirring apparatus of the rotating speed of 500-1000rpm and filter and obtain N-m-Nb 2O 5Thick product, with rare nitric acid and deionized water washing 3 times, dry 12h under 70 ℃ of conditions puts into Muffle furnace and heat-treats respectively, is warming up to 400 ℃ with the speed of 5 ℃/min, naturally is down to room temperature after maintenance 2h, makes N-m-Nb 2O 5Product.
Specific embodiment 4:
The preparation method of the doped meso-porous niobium pentaoxide high efficiency photocatalyst of a kind of nitrogen comprises the following steps:
1) preparation of mesoporous niobium pentaoxide, use m-Nb 2O 5Represent
A) adopt the synthetic m-Nb of self-assembly method 2O 5
The F127 that takes 1.5g is dissolved in the 15.0g absolute ethyl alcohol with the magnetic stirring apparatus of the rotating speed of 900rpm and processes 10min, after F127 dissolves fully, add 1.2g columbium pentachloride strong agitation 20min, the color of the solution becomes colorless transparently by faint yellow, dropwise adds the CaCl of 0.5mol/L 2Solution 0.6ml, and continuation stirring 10min makes Nb 2O 5Colloidal sol;
B) with Nb 2O 5Colloidal sol is placed in autoclave, ageing 72h under 60 ℃ of conditions, and 40 ℃ of dry 5h put into Muffle furnace and heat-treat, and are warming up to 450 ℃ with the speed of 5 ℃/min, keep naturally being down to room temperature after 5h, make m-Nb 2O 5Product;
2) preparation of the doped meso-porous niobium pentaoxide of nitrogen, use N-m-Nb 2O 5Represent
Take respectively the m-Nb of 5.0g 2O 5With 0.6g ammonium chloride, be dissolved in 7ml water, process 5h with the magnetic stirring apparatus of the rotating speed of 500-1000rpm and filter and obtain N-m-Nb 2O 5Thick product, with rare nitric acid and deionized water washing 3 times, dry 12h under 70 ℃ of conditions puts into Muffle furnace and heat-treats respectively, is warming up to 400 ℃ with the speed of 5 ℃/min, naturally is down to room temperature after maintenance 2h, makes N-m-Nb 2O 5Product.

Claims (1)

1. the preparation method of the doped meso-porous niobium pentaoxide high efficiency photocatalyst of nitrogen, is characterized in that: comprise the following steps:
1) preparation of mesoporous niobium pentaoxide, use m-Nb 2O 5Represent
A) adopt the synthetic m-Nb of self-assembly method 2O 5
The F127 that takes the 0.1-2.0 weight portion is dissolved in 1.0-20.0 weight portion absolute ethyl alcohol with the magnetic stirring apparatus of the rotating speed of 500-1000rpm and processes 10min, after F127 dissolves fully, add 0.1-1.5 weight portion columbium pentachloride strong agitation 20min, the color of the solution becomes colorless transparently by faint yellow, dropwise adds the CaCl of 0.5mol/L 2Solution 0.5-1.0ml, and make Nb after continuing to stir 10min 2O 5Colloidal sol;
B) with Nb 2O 5Colloidal sol is placed in autoclave, ageing 72h under 60 ℃ of conditions, and 40 ℃ of dry 5h put into Muffle furnace and heat-treat, and are warming up to 450 ℃ with the speed of 5 ℃/min, keep naturally being down to room temperature after 5h, make m-Nb 2O 5Product;
2) preparation of the doped meso-porous niobium pentaoxide of nitrogen, use N-m-Nb 2O 5Represent
Take respectively the m-Nb of 0.5-5.0 weight portion 2O 5With 0.05-1.0 weight portion ammonium chloride, be dissolved in 1-10ml water, process 5h with the magnetic stirring apparatus of the rotating speed of 500-1000rpm, filter and obtain N-m-Nb 2O 5Thick product, with rare nitric acid and deionized water washing 3 times, dry 12h under 70 ℃ of conditions puts into Muffle furnace and heat-treats respectively, is warming up to 400 ℃ with the speed of 5 ℃/min, naturally is down to room temperature after maintenance 2h, makes N-m-Nb 2O 5Product.
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CN103638959A (en) * 2013-12-16 2014-03-19 南通农业职业技术学院 Preparation method of rodlike N-doped niobium pentoxide photocatalyst
CN105688965A (en) * 2016-01-12 2016-06-22 南通职业大学 Preparation method of mesoporous niobium pentoxide/nitrogen-doped graphene efficient composite photocatalyst
CN106115781A (en) * 2016-06-23 2016-11-16 南阳师范学院 A kind of Hemicentrotus seu Strongylocentrotus shape Nb2o5electrode material and preparation method thereof
CN106334553A (en) * 2015-09-16 2017-01-18 哈尔滨工业大学 High-efficiency doping method of doped NbOx platinum-based catalyst used for fuel cell catalysts
CN107626338A (en) * 2017-10-11 2018-01-26 南通科技职业学院 The preparation method of the mesoporous niobium pentaoxide of molybdenum sulfide Nanoparticle Modified/nitrogen-doped graphene composite photo-catalyst
CN109167002A (en) * 2018-08-15 2019-01-08 合肥国轩高科动力能源有限公司 A kind of preparation method of lithium-sulfur cell composite diaphragm
CN110606508A (en) * 2018-06-17 2019-12-24 深圳格林德能源有限公司 Novel negative electrode material preparation method and solid-state lithium ion battery thereof
CN114369846A (en) * 2021-12-24 2022-04-19 复旦大学 Nitrogen-doped mesoporous metal oxide film and preparation method thereof
CN116443927A (en) * 2023-02-24 2023-07-18 浙江农林大学 Method for synthesizing mesoporous niobium pentoxide with high specific surface area by one-pot method

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CN103638959B (en) * 2013-12-16 2015-11-25 南通农业职业技术学院 The preparation method of the bar-shaped niobium pentaoxide photochemical catalyst of N doping
CN103638959A (en) * 2013-12-16 2014-03-19 南通农业职业技术学院 Preparation method of rodlike N-doped niobium pentoxide photocatalyst
CN106334553B (en) * 2015-09-16 2018-12-11 哈尔滨工业大学 A kind of NbO of fuel-cell catalyst dopingxThe efficient doping method of platinum based catalyst
CN106334553A (en) * 2015-09-16 2017-01-18 哈尔滨工业大学 High-efficiency doping method of doped NbOx platinum-based catalyst used for fuel cell catalysts
CN105688965A (en) * 2016-01-12 2016-06-22 南通职业大学 Preparation method of mesoporous niobium pentoxide/nitrogen-doped graphene efficient composite photocatalyst
CN105688965B (en) * 2016-01-12 2019-02-12 南通职业大学 Mesoporous niobium pentaoxide/nitrogen-doped graphene high-efficiency composite photocatalyst preparation method
CN106115781A (en) * 2016-06-23 2016-11-16 南阳师范学院 A kind of Hemicentrotus seu Strongylocentrotus shape Nb2o5electrode material and preparation method thereof
CN107626338A (en) * 2017-10-11 2018-01-26 南通科技职业学院 The preparation method of the mesoporous niobium pentaoxide of molybdenum sulfide Nanoparticle Modified/nitrogen-doped graphene composite photo-catalyst
CN110606508A (en) * 2018-06-17 2019-12-24 深圳格林德能源有限公司 Novel negative electrode material preparation method and solid-state lithium ion battery thereof
CN109167002A (en) * 2018-08-15 2019-01-08 合肥国轩高科动力能源有限公司 A kind of preparation method of lithium-sulfur cell composite diaphragm
CN114369846A (en) * 2021-12-24 2022-04-19 复旦大学 Nitrogen-doped mesoporous metal oxide film and preparation method thereof
CN114369846B (en) * 2021-12-24 2023-11-24 复旦大学 Nitrogen-doped mesoporous metal oxide film and preparation method thereof
CN116443927A (en) * 2023-02-24 2023-07-18 浙江农林大学 Method for synthesizing mesoporous niobium pentoxide with high specific surface area by one-pot method

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Application publication date: 20130508