CN102872853A - Three-dimensional ordered macroporous InVO4 visible light-responsive photocatalyst, preparation and application - Google Patents
Three-dimensional ordered macroporous InVO4 visible light-responsive photocatalyst, preparation and application Download PDFInfo
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- CN102872853A CN102872853A CN2012103641179A CN201210364117A CN102872853A CN 102872853 A CN102872853 A CN 102872853A CN 2012103641179 A CN2012103641179 A CN 2012103641179A CN 201210364117 A CN201210364117 A CN 201210364117A CN 102872853 A CN102872853 A CN 102872853A
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Abstract
A three-dimensional ordered macroporous InVO4 visible light-responsive photocatalyst, preparation and application belong to the technical field of photoresponsive catalysts. The preparation method comprises the following steps: under a stirring condition, dissolving indium nitrate, ammonium metavanadate and a complexing agent with an equal mol ratio in a mixed solution of water, anhydrous methanol, and glycol, uniformly stirring, weighing a PMMA template, soaking in a precursor solution, performing vacuum filtration and drying at room temperature, heating from room temperature to 300 DEG C with a speed of 1-2 DEG C/min in a tubular furnace in nitrogen atmosphere, holding the temperature for 3 hours, cooling the furnace to room temperature, heating from room temperature to 500 DEG C with a speed of 1-2 DEG C/min in air atmosphere, and holding the temperature for 4 hours. The indium vanadate photocatalyst with a three-dimensional ordered macroporous structure and mesopores on pore walls has degradation efficiency on methylene blue of up to 92-98% when irradiated by visible light for 1 hour. The preparation method of the invention is simple in operation, and low in raw material price.
Description
Technical field
The present invention relates to a kind of visible light-responded three-dimensional ordered macroporous material that has, relate in particular under radiation of visible light can the efficient degradation methylene blue etc. catalysis material, preparation and the application of organic dyestuff, belong to photoresponse type catalyst technical field.
Background technology
InVO
4Belong to orthovanadate (MVO
4) compound of a class, have two kinds of crystallographic systems of quadrature and monocline.The vanadic acid indium can be used as the anode material of rechargeable lithium-ion battery because of its good electrochemical properties.Aspect clean energy resource, owing to having visible light-responded characteristic, the vanadic acid indium not only can be at photocatalysis degradation organic contaminant under the radiation of visible light, and therefore all right photocatalytic hydrogen production by water decomposition had caused in recent years that the scholar paid close attention to widely.
InVO
4Synthetic solid-phase synthesis, sol-gel process and the hydro-thermal method etc. of mainly containing.Ye etc. (J.Ye, et al., J.Chem.Phys.Lett.2002,356:221) have prepared by high-temperature solid phase reaction method can be at the novel photocatalyst I of hydrogen production by water decomposition under radiation of visible light nMO
4(M=V, Nb, Ta), their energy gap is respectively 1.9eV, 2.5eV and 2.6eV.Yet high temperature solid-state method has, and temperature requirement is high, the reaction time long and generate the shortcomings such as product is uncontrollable, size is inhomogeneous.Xu Li wait first (Xu Lixian etc., the catalysis journal, 2006,27:100-102) adopt the template hydrothermal synthesis method to prepare the mesoporous InVO of bigger serface
4Photochemical catalyst obtains monocline type and oblique square structure by changing temperature.Hydrogen production by water decomposition speed can be up to 1836 μ mol/ (g h) under UV-irradiation at 700 ℃ of roasting gained samples.Zhang etc. (L.Zhang, et al., J.Solid State Chem.2006,179:804) adopt sol-gel process, will necessarily measure the In (OH) of ratio
3And V
2O
5Be dissolved in generation colloidal sol matter in diethylene triamine pentacetic acid (DTPA) (DTPA) solution, 600 ℃ of roastings make orthogonal type InVO
4, average grain diameter is 80nm.Xiao etc. (G.C.Xiao, et al., Chinese J.Inorg.Chem.2004,20:195) utilize hydro-thermal method, with InCl
3And NaVO
3Be source metal, make InVO through 180 ℃ of hydro-thermal reaction 4h
4, particle diameter is 20-40nm.Huang and Yu(Q.M.Huang, J.C.Yu, Chinese J.Struct.Chem.2005,24:1242 1248) with InCl
3And NaVO
3Be source metal, the In/V mol ratio is 1/2, at 150-210 ℃ of lower hydrothermal treatment consists 4h, obtains the pure phase InVO that particle diameter is 20-40nm
4Catalyst.
Summary of the invention
The object of the present invention is to provide have three-dimensional ordered macroporous structure and can be at the InVO of visible light-responded lower efficient degradation methylene blue (MB) a kind of preparation
4Catalyst, preparation method.This catalyst has and has on three-dimensional ordered macroporous structure and the hole wall that mesoporous its specific area of vanadic acid indium catalyst is large, voidage is high, and catalytic activity is more superior.Up to now, there is no document and patent report utilizes template successfully to synthesize the InVO with three-dimensional ordered macroporous structure
4Catalyst.
A kind of three-dimensional ordered macroporous InVO
4Visible-light-responsive photocatalyst is characterized in that, this catalyst is to have to have mesoporous vanadic acid indium catalyst on three-dimensional ordered macroporous structure and the hole wall, and average pore size is 130 ~ 170nm, and the mesoporous aperture of hole wall is 2 ~ 10nm, and band-gap energy is 2 ~ 3eV.
Above-mentioned three-dimensional ordered macroporous InVO
4The preparation method of visible-light-responsive photocatalyst is characterized in that, adopts polymethyl methacrylate (PMMA) microsphere template legal system standby, specifically may further comprise the steps:
(1) under stirring condition, with the indium nitrate (In (NO of equimolar ratio
3)
34.5H
2O), ammonium metavanadate and complexing agent (citric acid, tartaric acid or ascorbic acid) are dissolved in the mixed solution of the absolute methanol of deionized water and different proportionings and ethylene glycol, stir 1h to fully dissolving, the corresponding 7ml deionized water of every 10mmol indium nitrate wherein, the corresponding absolute methanol of every 10mmol indium nitrate and ethylene glycol is 9ml altogether, and the volume ratio of absolute methanol and ethylene glycol is 7.5:1.5-1.5:7.5;
(2) take by weighing the orderly hard template polymethyl methacrylate (PMMA) of arrangement and in precursor solution, flood drying at room temperature behind vacuum filtration; The corresponding 4g polymethyl methacrylate of the indium nitrate of every 10mmol in the preferred steps (1), the preferred 3h of dip time;
(3) in tube furnace in rising to 300 ℃ and under this temperature, keep 3h from room temperature with the speed of 1-2 ℃/min under the nitrogen atmosphere, after furnace temperature is cooled to room temperature, under air atmosphere, rise to 500 ℃ and under this temperature, keep 4h with 1-2 ℃/min heating rate from room temperature, obtain the InVO of monoclinic phase three-dimensional ordered macroporous structure
4Catalyst.
Three-dimensional ordered macroporous InVO of the present invention
4Visible-light-responsive photocatalyst is used for photocatalytic degradation methylene blue (MB).
Wherein take ascorbic acid as complexing agent, absolute methanol/ethylene glycol volume ratio is the InVO that 7.5/1.5 makes
4The catalyst three-dimensional order is best, and average pore size is 138nm, and the mesoporous aperture of hole wall is 2 ~ 10nm, and band-gap energy is 2.50eV, has visible light-responded property, and the degradation efficiency of illumination MB after 1 hour is 98%; Take tartaric acid as complexing agent, absolute methanol/ethylene glycol volume ratio is 6/3 InVO that makes
4Catalyst has ordered 3 D structure, and average pore size is 142nm, and the mesoporous aperture of hole wall is 2 ~ 10nm, and its band-gap energy is 2.68eV, has preferably visible light-responded property, and the degradation efficiency of illumination MB after 1 hour is 95%; Take citric acid as complexing agent, absolute methanol/ethylene glycol volume ratio is 6/3 InVO that makes
4Catalyst has ordered 3 D structure, and the part duct caves in, and average pore size is 166nm, and the mesoporous aperture of hole wall is 2 ~ 10nm, and band-gap energy is 2.75eV, has visible light-responded property, and the degradation efficiency of illumination MB after 1 hour is 92%.
Method provided by the present invention is simple to operate, and cost of material is cheap, and products therefrom pattern, specific area are controlled.
The three-dimensional ordered macroporous InVO of the present invention's preparation
4Catalyst has visible light-responded property, can at efficient degradation MB under the radiation of visible light, have good application prospect in photocatalysis field.
Utilize crystal structure, the particle morphology of the instrumental characterizing gained target products such as D8ADVANCE type X-ray diffractometer (XRD), ZEISS SUPRA 55 type high resolution scanning electron microscopes (HRSEM), JEOL-2010 type high resolution transmission electron microscopy (HRTEM) and SHIMADAZU-UV-2450 type ultraviolet-visible spectrometer (UV-Vis), pore structure, photo absorption performance.Utilize photo catalysis reactor to measure three-dimensional ordered macroporous InVO
4Under radiation of visible light, the degrade efficient of MB of catalyst.The result shows, according to the prepared InVO of the inventive method
4Catalyst has three-dimensional ordered macroporous structure also can be at efficient degradation MB under the radiation of visible light.
Compound concentration be the 100mL MB solution of 10mg/L in the photocatalysis quartz reactor, add 0.1gInVO
4The ultrasonic 15min of catalyst lucifuge passes into air, adds behind the condensing unit dark place and stirs 20min.Get the 6ml blank sample, (wavelength 〉=400nm) get the equal-volume sample every 20min afterwards is used for the analysis of MB concentration to open the visible light device.
Description of drawings
Fig. 1 is obtained InVO
4The XRD spectra of sample, wherein curve (a), (b), (c) are respectively the XRD spectra of embodiment 1, embodiment 2, embodiment 3 samples;
Fig. 2 is prepared InVO
4The HRSEM photo of sample, wherein figure (a) with (b), (c) with (d), (e) and the HRSEM photo that (f) is respectively embodiment 1, embodiment 2 and embodiment 3 samples;
Fig. 3 is prepared InVO
4The HRTEM photo of sample, wherein figure (a) with (b), (c) with (d), (e) and the HRTEM photo that (f) is respectively embodiment 1, embodiment 2 and embodiment 3 samples;
Fig. 4 is the prepared InVO of embodiment
4The ultraviolet-visible light spectrogram of sample and band-gap energy figure
Wherein scheme (a), (b) and (c) respectively corresponding embodiment 1, embodiment 2 and embodiment 3;
Fig. 5 is prepared InVO
4Under radiation of visible light, degrade efficient (the initial concentration C of MB of sample
0=10mg/L), wherein scheme (1), (2) and (3) (marking in the drawings 1.2.3) respectively corresponding embodiment 1, embodiment 2 and embodiment 3;
Fig. 6 is degrade under the visible light degradation efficiencies of different initial concentration MB of embodiment 2 samples.
The specific embodiment
Embodiment 1:
Measure respectively the 7ml deionized water, the 6ml absolute methanol, 3ml ethylene glycol is in the 50ml small beaker, add respectively the 10mmol indium nitrate under the stirring condition, 10mmol citric acid and 10mmol ammonium metavanadate, magnetic agitation 1h is to fully dissolving, take by weighing 4g PMMA template and impregnated in 3h in the above-mentioned precursor solution, drying at room temperature 12h behind the vacuum filtration, in tube furnace in rising to 300 ℃ and under this temperature, keep 3h from room temperature with the speed of 1 ℃/min under the nitrogen atmosphere, after furnace temperature is cooled to room temperature, under air atmosphere, rise to 500 ℃ and under this temperature, keep 4h with the speed of 1 ℃/min from room temperature, make the InVO of monoclinic phase three-dimensional ordered macroporous structure
4Catalyst.The aperture is about 166nm, and the mesoporous aperture of hole wall is 2 ~ 10nm.Preparation 100ml concentration be the MB solution of 10mg/L in quartz reactor, add 0.1g InVO
4The ultrasonic 15min of lucifuge passes into air behind the catalyst, adds behind the condensing unit dark place and stirs 20min.Get the 6ml blank sample, get the equal-volume sample every 20min after opening the visible light device, get altogether 4 samples.The band-gap energy that makes sample is 2.75eV, and the degradation efficiency of MB is 92% after 1 hour under radiation of visible light.
Embodiment 2:
Measure respectively the 7ml deionized water, the 6ml absolute methanol, 3ml ethylene glycol is in the 50ml small beaker, add respectively the 10mmol indium nitrate under the stirring condition, 10mmol tartaric acid and 10mmol ammonium metavanadate, magnetic agitation 1h is to fully dissolving, take by weighing 4g PMMA template and impregnated in 3h in the above-mentioned precursor solution, drying at room temperature 12h behind the vacuum filtration, in tube furnace in rising to 300 ℃ and under this temperature, keep 3h from room temperature with the speed of 1 ℃/min under the nitrogen atmosphere, after furnace temperature is cooled to room temperature, under air atmosphere, rise to 500 ℃ and under this temperature, keep 4h with the speed of 1 ℃/min from room temperature, make the InVO of monoclinic phase three-dimensional ordered macroporous structure
4Catalyst.The aperture is about 142nm, and the mesoporous aperture of hole wall is 2 ~ 10nm.Preparation 100ml concentration be the MB solution of 10mg/L in quartz reactor, add 0.1g InVO
4The ultrasonic 15mi n of lucifuge passes into air behind the catalyst, adds behind the condensing unit dark place and stirs 20min.Get the 6ml blank sample, get the equal-volume sample every 20min after opening the visible light device, get altogether 4 samples.The band-gap energy that makes sample is 2.68eV, and the degradation efficiency of MB is 95% after 1 hour under radiation of visible light.
Embodiment 3:
Measure respectively the 7ml deionized water, 7.5ml absolute methanol, 1.5ml ethylene glycol is in the 50ml small beaker, add respectively the 10mmol indium nitrate under the stirring condition, 10mmol ascorbic acid and 10mmol ammonium metavanadate, magnetic agitation 1h is to fully dissolving, take by weighing 4g PMMA template and impregnated in 3h in the above-mentioned precursor solution, drying at room temperature 12h behind the vacuum filtration, in tube furnace in rising to 300 ℃ and under this temperature, keep 3h from room temperature with the speed of 1 ℃/min under the nitrogen atmosphere, after furnace temperature is cooled to room temperature, under air atmosphere, rise to 500 ℃ and under this temperature, keep 4h with the speed of 1 ℃/min from room temperature, make the InVO of monoclinic phase three-dimensional ordered macroporous structure
4Catalyst.The aperture is about 138nm, and the mesoporous aperture of hole wall is 2 ~ 10nm.Preparation 100ml concentration be the MB solution of 10mg/L in quartz reactor, add 0.1g InVO
4The ultrasonic 15min of lucifuge passes into air behind the catalyst, adds behind the condensing unit dark place and stirs 20min.Get the 6ml blank sample, get the equal-volume sample every 20min after opening the visible light device, get altogether 4 samples.The band-gap energy that makes sample is 2.50eV, and the degradation efficiency of MB is 98% after 1 hour under visible light.
Claims (7)
1. three-dimensional ordered macroporous InVO
4Visible-light-responsive photocatalyst is characterized in that, this catalyst is to have to have mesoporous vanadic acid indium catalyst on three-dimensional ordered macroporous structure and the hole wall, and average pore size is 130 ~ 170nm, and the mesoporous aperture of hole wall is 2 ~ 10nm, and band-gap energy is 2 ~ 3eV.
2. prepare a kind of three-dimensional ordered macroporous InVO claimed in claim 1
4The method of visible-light-responsive photocatalyst is characterized in that, adopts the poly (methyl methacrylate) micro-sphere template synthesis, specifically may further comprise the steps:
(1) under stirring condition, indium nitrate, ammonium metavanadate and the complexing agent of equimolar ratio is dissolved in the mixed solution of the absolute methanol of deionized water and different proportionings and ethylene glycol, stir 1h to fully dissolving, the corresponding 7ml deionized water of every 10mmol indium nitrate wherein, the corresponding absolute methanol of every 10mmol indium nitrate and ethylene glycol is 9ml altogether, and the volume ratio of absolute methanol and ethylene glycol is 7.5:1.5-1.5:7.5, and complexing agent is citric acid, tartaric acid or ascorbic acid;
(2) take by weighing the orderly hard template polymethyl methacrylate of arrangement and in precursor solution, flood drying at room temperature behind vacuum filtration;
(3) in tube furnace in rising to 300 ℃ and under this temperature, keep 3h from room temperature with the speed of 1-2 ℃/min under the nitrogen atmosphere, after furnace temperature is cooled to room temperature, under air atmosphere, rise to 500 ℃ and under this temperature, keep 4h with 1-2 ℃/min heating rate from room temperature, obtain the InVO of monoclinic phase three-dimensional ordered macroporous structure
4Catalyst.
3. according to the method for claim 2, it is characterized in that, the corresponding 4g polymethyl methacrylate of the indium nitrate of every 10mmol in the step (1), dip time is 3h.
4. according to the method for claim 2, it is characterized in that, wherein take ascorbic acid as complexing agent, absolute methanol/ethylene glycol volume ratio is the InVO that 7.5/1.5 makes
4The catalyst three-dimensional order is best, and average pore size is 138nm, and the mesoporous aperture of hole wall is 2 ~ 10nm, and band-gap energy is 2.50eV.
5. according to the method for claim 2, it is characterized in that, take tartaric acid as complexing agent, absolute methanol/ethylene glycol volume ratio is 6/3 InVO that makes
4Catalyst has ordered 3 D structure, and average pore size is 142nm, and the mesoporous aperture of hole wall is 2 ~ 10nm, and its band-gap energy is 2.68eV.
6. according to the method for claim 2, it is characterized in that, take citric acid as complexing agent, absolute methanol/ethylene glycol volume ratio is 6/3 InVO that makes
4Catalyst has ordered 3 D structure, and the part duct caves in, and average pore size is 166nm, and the mesoporous aperture of hole wall is 2 ~ 10nm, and band-gap energy is 2.75eV.
7. a kind of three-dimensional ordered macroporous InVO claimed in claim 1
4Visible-light-responsive photocatalyst is used for the photocatalytic degradation methylene blue.
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Cited By (10)
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| CN103877969A (en) * | 2014-04-08 | 2014-06-25 | 中南大学 | In 2 O 3 ·InVO 4 Heterostructure composites and methods of making and using same |
| CN104084188A (en) * | 2014-06-26 | 2014-10-08 | 北京工业大学 | Visible-light response photo-catalyst with three-dimensional orderly macropore InVO4-BiVO4 heterojunction, as well as preparation and application of photo-catalyst |
| CN106345465A (en) * | 2015-04-08 | 2017-01-25 | 天津大学 | Application of three-dimensional macroporous molybdenum dioxide loaded palladium particle material to electrocatalysis material |
| CN108251917A (en) * | 2018-01-29 | 2018-07-06 | 湘潭大学 | A kind of preparation method and applications of titanium dioxide/vanadic acid indium heterogeneous structural nano fiber |
| CN108855202A (en) * | 2018-06-05 | 2018-11-23 | 上海交通大学 | For photocatalytic water and the composite photo-catalyst of contaminant degradation and preparation method thereof |
| CN110299540A (en) * | 2019-07-02 | 2019-10-01 | 陕西科技大学 | A kind of NiCo of three-dimensional netted hierarchical porous structure2O4The preparation method of elctro-catalyst |
| CN110302739A (en) * | 2019-06-12 | 2019-10-08 | 三峡大学 | The InVO of the nitrogenous organic dyestuff of selective absorption4The preparation method and applications of adsorbent |
| CN112495411A (en) * | 2020-09-09 | 2021-03-16 | 同济大学 | Carbon nitride nanosheet loaded indium vanadate quantum dot photocatalyst and preparation and application thereof |
| CN113070056A (en) * | 2021-03-22 | 2021-07-06 | 南昌大学 | General synthesis method of tantalum pentoxide photocatalytic material with three-dimensional ordered network structure |
| CN113649026A (en) * | 2021-07-27 | 2021-11-16 | 南昌大学 | General synthesis method of three-dimensional ordered macroporous cadmium sulfide photocatalytic material |
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| CN103877969A (en) * | 2014-04-08 | 2014-06-25 | 中南大学 | In 2 O 3 ·InVO 4 Heterostructure composites and methods of making and using same |
| CN104084188A (en) * | 2014-06-26 | 2014-10-08 | 北京工业大学 | Visible-light response photo-catalyst with three-dimensional orderly macropore InVO4-BiVO4 heterojunction, as well as preparation and application of photo-catalyst |
| CN106345465A (en) * | 2015-04-08 | 2017-01-25 | 天津大学 | Application of three-dimensional macroporous molybdenum dioxide loaded palladium particle material to electrocatalysis material |
| CN106345465B (en) * | 2015-04-08 | 2018-08-31 | 天津大学 | Application of the three-dimensional macroporous structure molybdenum dioxide supported palladium granular materials as electrocatalysis material |
| CN108251917A (en) * | 2018-01-29 | 2018-07-06 | 湘潭大学 | A kind of preparation method and applications of titanium dioxide/vanadic acid indium heterogeneous structural nano fiber |
| CN108855202A (en) * | 2018-06-05 | 2018-11-23 | 上海交通大学 | For photocatalytic water and the composite photo-catalyst of contaminant degradation and preparation method thereof |
| CN110302739B (en) * | 2019-06-12 | 2021-08-24 | 三峡大学 | InVO for selectively adsorbing nitrogen-containing organic dye4Preparation method and application of adsorbent |
| CN110302739A (en) * | 2019-06-12 | 2019-10-08 | 三峡大学 | The InVO of the nitrogenous organic dyestuff of selective absorption4The preparation method and applications of adsorbent |
| CN110299540A (en) * | 2019-07-02 | 2019-10-01 | 陕西科技大学 | A kind of NiCo of three-dimensional netted hierarchical porous structure2O4The preparation method of elctro-catalyst |
| CN112495411A (en) * | 2020-09-09 | 2021-03-16 | 同济大学 | Carbon nitride nanosheet loaded indium vanadate quantum dot photocatalyst and preparation and application thereof |
| CN112495411B (en) * | 2020-09-09 | 2022-08-05 | 同济大学 | Carbon nitride nanosheet loaded indium vanadate quantum dot photocatalyst and preparation and application thereof |
| CN113070056A (en) * | 2021-03-22 | 2021-07-06 | 南昌大学 | General synthesis method of tantalum pentoxide photocatalytic material with three-dimensional ordered network structure |
| CN113070056B (en) * | 2021-03-22 | 2022-11-08 | 南昌大学 | General synthesis method of three-dimensional ordered net-shaped tantalum pentoxide photocatalytic material |
| CN113649026A (en) * | 2021-07-27 | 2021-11-16 | 南昌大学 | General synthesis method of three-dimensional ordered macroporous cadmium sulfide photocatalytic material |
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Application publication date: 20130116 |