CN103638959B - The preparation method of the bar-shaped niobium pentaoxide photochemical catalyst of N doping - Google Patents

The preparation method of the bar-shaped niobium pentaoxide photochemical catalyst of N doping Download PDF

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CN103638959B
CN103638959B CN201310692528.5A CN201310692528A CN103638959B CN 103638959 B CN103638959 B CN 103638959B CN 201310692528 A CN201310692528 A CN 201310692528A CN 103638959 B CN103638959 B CN 103638959B
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bar
niobium pentaoxide
preparation
doping
photochemical catalyst
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CN103638959A (en
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丁敏娟
李亚
蒋云霞
李蓉
金洁蓉
闫生荣
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NANTONG AGRICULTURAL COLLEGE
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Abstract

The invention discloses the preparation method of the bar-shaped niobium pentaoxide photochemical catalyst of a kind of N doping.1) preparation of bar-shaped niobium pentaoxide; 2) preparation of the bar-shaped niobium pentaoxide photochemical catalyst of N doping.This preparation method with metal niobium powder and urea for the bar-shaped niobium pentaoxide of N doping prepared by raw material.The present invention can significantly improve the photocatalytic activity of niobium pentaoxide, effectively strengthens its utilization rate to sunshine, expands the range of application of niobium pentaoxide photochemical catalyst further.Organic pollution mineralising in water can be CO by N doping bar-shaped niobium pentaoxide photochemical catalyst quickly and efficiently 2and H 2o, catalyst recycling rate of waterused is high, and has good application prospect and economic benefit, is a kind of environmentally friendly photochemical catalyst.

Description

The preparation method of the bar-shaped niobium pentaoxide photochemical catalyst of N doping
Technical field
The present invention relates to semiconductor light-catalyst preparation field, be specifically related to the preparation method of the bar-shaped niobium pentaoxide photochemical catalyst of a kind of N doping.
Background technology
Along with expanding economy; energy crisis is on the rise: the consumption of fossil energy; pollution of air, water resource etc. becomes the bottleneck of sustainable development, and therefore, the means of seeking a kind of environmental protection solve problems has become the extremely urgent task in countries in the world.Photocatalysis is because having the plurality of advantages such as clean, efficient, safe and receiving very large concern.
Semiconductor TiO is found from Fujishima in 1972 2can by since photoelectrocatalysis decomposition water, the research of conductor photocatalysis material just becomes the focus of scientists study.Recently, niobium pentaoxide (Nb 2o 5) receive very large concern as a kind of typical n-type semiconductor photochemical catalyst.But reunite because niobium pentoxide nano particle specific surface area little Yi causes, the wider (E of energy gap g=3.4eV) and light induced electron and hole are easy to compound in its body, limit the application of niobium pentaoxide in photocatalysis field.Therefore, prepare the high activity niobium pentaoxide photochemical catalyst with visible-light response type and become the important research direction in this field.Large quantity research shows, by preparing the method that the semiconductor (nanometer rods, nanosphere, nano wire etc.) with nanometer new look structure is the photocatalytic activity improving photochemical catalyst.Wherein, scientists is rather extensive to the research of the photochemical catalyst of nanometer rods class, mainly has relatively large specific area due to nano bar-shape structure and has good draw ratio.Large specific area can increase active sites and the reaction center of catalyst surface, and simultaneously preferably draw ratio effectively can suppress the right compound again of light induced electron and hole, thus significantly strengthens the catalytic activity of photochemical catalyst.In addition, nonmetal doping modification is utilized to be a kind of main method making the photoactive semiconductor light-catalyst of ultraviolet realize Visible-light Irradiation.Nonmetal (as C, N, S etc.) doping can make the absorption spectrum generation red shift of semiconductor light-catalyst, expands its photoresponse scope, thus improves photocatalytic activity further.But prior art not yet discloses the preparation method of the bar-shaped niobium pentaoxide photochemical catalyst of N doping.
Summary of the invention
Goal of the invention: the present invention, in order to solve the deficiencies in the prior art, has the preparation method of the bar-shaped niobium pentaoxide photochemical catalyst of N doping of high catalytic activity under providing a kind of effective sunshine.Mainly solve the niobium pentaoxide photochemical catalyst serious Complex Problem that in low and body, photo-generate electron-hole is right to sunshine utilization rate, improve the catalytic activity of photochemical catalyst, and expand the range of application of photochemical catalyst.
Technical scheme: the preparation method of the bar-shaped niobium pentaoxide photochemical catalyst of a kind of N doping, comprises the following steps:
1) preparation of bar-shaped niobium pentaoxide, uses Nb 2o 5nR represents
Getting 0.2g metal niobium powder is dissolved in 80mL deionized water, with the rotating speed stir process 30min of 1000rpm, above-mentioned solution is transferred in 100mL autoclave, ageing 7 days under 200 DEG C of conditions, filtration obtains product, wash 2-3 time with deionized water and alcohol mixeding liquid again, filter, obtain product Nb at 60 DEG C of dry 1h 2o 5nR, prepares stand-by.
2) preparation of the bar-shaped niobium pentaoxide of N doping, uses N-Nb 2o 5nR represents
Take 1gNb 2o 5the urea of NR and different quality, urea and Nb 2o 5the mass ratio of NR is 1 ~ 4:1, and the sample obtained is at 400 DEG C of calcining 2h, and by gained sample dust technology and deionized water washing, suction filtration, is then placed in 70 DEG C of baking ovens and dries 12h, the sample N-Nb obtained 2o 5nR.
Beneficial effect: the present invention compares with existing technology, successfully synthesize the bar-shaped niobium pentaoxide photochemical catalyst of visible-light response type N doping with bigger serface, more excellent draw ratio, efficiently solve the difficult problem that niobium pentaoxide photochemical catalyst catalytic activity is low, improve the light energy use efficiency of photochemical catalyst, expand the range of application of niobium pentaoxide further.Organic pollution mineralising in water can be CO by N doping bar-shaped niobium pentaoxide photochemical catalyst quickly and efficiently 2and H 2o, catalyst recycling rate of waterused is high, and has good application prospect and economic benefit, is a kind of environmentally friendly photochemical catalyst.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be described in detail.
Specific embodiment 1:
A preparation method for the bar-shaped niobium pentaoxide photochemical catalyst of N doping, comprises the following steps:
1) preparation of bar-shaped niobium pentaoxide, uses Nb 2o 5nR represents
Getting 0.2g metal niobium powder is dissolved in 80mL deionized water, with the rotating speed stir process 30min of 1000rpm, above-mentioned solution is transferred in 100mL autoclave, ageing 7 days under 200 DEG C of conditions, filtration obtains product, wash 2-3 time with deionized water and alcohol mixeding liquid again, filter, obtain product Nb at 60 DEG C of dry 1h 2o 5nR;
2) preparation of the bar-shaped niobium pentaoxide of N doping, uses N-Nb 2o 5nR represents
Above-mentioned steps is prepared Nb 2o 5nR mixes with the mass ratio of 1:1 with urea, even with mortar grinder, and the sample obtained is at 400 DEG C of calcining 2h, and by gained sample dust technology and deionized water washing, suction filtration, is then placed in 70 DEG C of baking ovens and dries 12h, obtain sample N-Nb 2o 5nR.
Specific embodiment 2:
A preparation method for the bar-shaped niobium pentaoxide photochemical catalyst of N doping, comprises the following steps:
1) preparation of bar-shaped niobium pentaoxide, uses Nb 2o 5nR represents
Getting 0.4g metal niobium powder is dissolved in 80mL deionized water, with the rotating speed stir process 30min of 1000rpm, above-mentioned solution is transferred in 100mL autoclave, ageing 7 days under 200 DEG C of conditions, filtration obtains product, wash 2-3 time with deionized water and alcohol mixeding liquid again, filter, obtain product Nb at 60 DEG C of dry 1h 2o 5nR, prepares stand-by;
2) preparation of the bar-shaped niobium pentaoxide of N doping, uses N-Nb 2o 5nR represents
Above-mentioned steps is prepared Nb 2o 5nR mixes with the mass ratio of 2:1 with urea, even with mortar grinder, and the sample obtained is at 400 DEG C of calcining 2h, and by gained sample dust technology and deionized water washing, suction filtration, dries 12h under being then placed on 70 DEG C of baking ovens, the sample N-Nb obtained 2o 5nR;
Specific embodiment 3:
A preparation method for the bar-shaped niobium pentaoxide photochemical catalyst of N doping, comprises the following steps:
1) preparation of bar-shaped niobium pentaoxide, uses Nb 2o 5nR represents
Getting 0.6g metal niobium powder is dissolved in 80mL deionized water, with the rotating speed stir process 30min of 1000rpm, above-mentioned solution is transferred in 100mL autoclave, ageing 7 days under 200 DEG C of conditions, filtration obtains product, wash 2-3 time with deionized water and alcohol mixeding liquid again, filter, obtain product Nb at 60 DEG C of dry 1h 2o 5nR, prepares stand-by;
2) preparation of the bar-shaped niobium pentaoxide of N doping, uses N-Nb 2o 5nR represents
Above-mentioned steps is prepared Nb 2o 5nR mixes with the mass ratio of 3:1 with urea, even with mortar grinder, and the sample obtained is at 400 DEG C of calcining 2h, and by gained sample dust technology and deionized water washing, suction filtration, dries 12h under being then placed on 70 DEG C of baking ovens, obtain sample N-Nb 2o 5nR;
Specific embodiment 4:
A preparation method for the bar-shaped niobium pentaoxide photochemical catalyst of N doping, comprises the following steps:
1) preparation of bar-shaped niobium pentaoxide, uses Nb 2o 5nR represents
Getting 0.8g metal niobium powder is dissolved in 80mL deionized water, with the rotating speed stir process 30min of 1000rpm, above-mentioned solution is transferred in 100mL autoclave, ageing 7 days under 200 DEG C of conditions, filtration obtains product, wash 2-3 time with deionized water and alcohol mixeding liquid again, filter, obtain product Nb at 60 DEG C of dry 1h 2o 5nR, prepares stand-by;
2) preparation of the bar-shaped niobium pentaoxide of N doping, uses N-Nb 2o 5nR represents
Above-mentioned steps is prepared Nb 2o 5nR mixes with the mass ratio of 4:1 with urea, even with mortar grinder, and the sample obtained is at 400 DEG C of calcining 2h, and by gained sample dust technology and deionized water washing, suction filtration, dries 12h under being then placed on 70 DEG C of baking ovens, the sample N-Nb obtained 2o 5nR.

Claims (2)

1. a preparation method for the bar-shaped niobium pentaoxide photochemical catalyst of N doping, is characterized in that: comprise the following steps:
1) preparation of bar-shaped niobium pentaoxide, uses Nb 2o 5nR represents
Getting 0.2g metal niobium powder is dissolved in 80mL deionized water, with the rotating speed stir process 30min of 1000rpm, above-mentioned solution is transferred in 100mL autoclave, ageing 7 days under 200 DEG C of conditions, filtration obtains product, wash 2-3 time with deionized water and alcohol mixeding liquid again, obtain product Nb at 60 DEG C of dry 1h 2o 5nR;
2) preparation of the bar-shaped niobium pentaoxide of N doping, uses N-Nb 2o 5nR represents
Take 1gNb 2o 5the urea of NR and different quality, urea and Nb 2o 5the mass ratio of NR is 1 ~ 4:1, uses mortar grinder Homogeneous phase mixing, and the sample obtained is at 400 DEG C of calcining 2h, and by gained sample dust technology and deionized water washing, suction filtration, is then placed in 70 DEG C of baking ovens and dries 12h, the sample N-Nb obtained 2o 5nR.
2. the bar-shaped niobium pentaoxide photocatalyst applications of N doping according to claim 1 is in photocatalysis field.
CN201310692528.5A 2013-12-16 2013-12-16 The preparation method of the bar-shaped niobium pentaoxide photochemical catalyst of N doping Expired - Fee Related CN103638959B (en)

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Citations (4)

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WO2011132036A1 (en) * 2010-04-22 2011-10-27 Universidade Do Porto Composite grapheno-metal oxide platelet method of preparation and applications
US20120205321A1 (en) * 2011-02-16 2012-08-16 City University Of Hong Kong Nitrogen doped a2nb4o11, process for preparation thereof, and method for degradation of organic pollutants
CN103084198A (en) * 2013-02-01 2013-05-08 南通职业大学 Preparation method of efficient photocatalyst nitrogen doped meso-porous niobium pentoxide

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CN101439883A (en) * 2008-11-18 2009-05-27 福州大学 Nb2O5 one-dimensional nano material and preparation thereof
WO2011132036A1 (en) * 2010-04-22 2011-10-27 Universidade Do Porto Composite grapheno-metal oxide platelet method of preparation and applications
US20120205321A1 (en) * 2011-02-16 2012-08-16 City University Of Hong Kong Nitrogen doped a2nb4o11, process for preparation thereof, and method for degradation of organic pollutants
CN103084198A (en) * 2013-02-01 2013-05-08 南通职业大学 Preparation method of efficient photocatalyst nitrogen doped meso-porous niobium pentoxide

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