CN104275176A - Visible light responding photocatalyst Ca3Nb3V5O23 and preparation method thereof - Google Patents

Visible light responding photocatalyst Ca3Nb3V5O23 and preparation method thereof Download PDF

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Publication number
CN104275176A
CN104275176A CN201410537369.6A CN201410537369A CN104275176A CN 104275176 A CN104275176 A CN 104275176A CN 201410537369 A CN201410537369 A CN 201410537369A CN 104275176 A CN104275176 A CN 104275176A
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visible light
photochemical catalyst
preparation
photocatalyst
powder
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CN104275176B (en
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罗昊
苏和平
李洁
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Guangzhou Boyi Intellectual Property Operation Co ltd
Shandong Xingqiang Chemical Industry Technology Research Institute Co ltd
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Guilin University of Technology
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Abstract

The invention discloses a visible light responding photocatalyst Ca3Nb3V5O23 and a preparation method thereof. The photocatalyst has the following chemical formula: Ca3Nb3V5O23. The invention also discloses the preparation method of the visible light responding photocatalyst Ca3Nb3V5O23. The photocatalyst obtained by the invention has the advantages of wide spectral response range, high light conversion rate, good stability and the like, and has the effects of decomposing harmful chemical substances and organic biomasses and sterilizing under the irradiation of visible light; in addition, the preparation method is simple, low in synthesis temperature and cost and suitable for industrial production and application.

Description

Visible light-responded photochemical catalyst Ca 3nb 3v 5o 23and preparation method thereof
Technical field
The present invention relates to a kind of visible light-responded photochemical catalyst Ca 3nb 3v 5o 23and preparation method thereof, belong to inorganic field of photocatalytic material.
Background technology
Along with socioeconomic development, people more and more pay close attention to for the energy and ecological environment, solve energy shortage and problem of environmental pollution be realize sustainable development, improve people's living standard and safeguard national security in the urgent need to.
From phase late 1970s, there has been proposed and to utilize in photochemical catalyst decomposition water and the organic matter such as agricultural chemicals in air and odorant, and scribble the application example such as self-cleaning of the surface of solids of photochemical catalyst.The principle of light-catalyzed reaction is that photochemical catalyst is after absorbing the photon higher than its band-gap energy, generate hole and electronics, these holes and electronics carry out oxidation reaction and reduction reaction respectively, reach the object of decomposing harmful chemical, organic-biological matter and sterilization.Photochemical catalyst has many kinds, and wherein most representative is titanium dioxide (TiO 2), titanium dioxide has been utilized to decompose organic matters such as the agricultural chemicals in water and in air and odorants, but the band gap of titanium dioxide is 3.2eV, only under the ultraviolet irradiation shorter than 400nm, just activity can be shown, can only at indoor or the local work having uviol lamp, almost can not utilize visible ray, this limits the use of titanium dioxide optical catalyst greatly.
Consider the practicality of photochemical catalyst in decomposing harmful substances, utilize sunshine to be indispensable as light source.Irradiate maximum to sunshine medium wavelength intensity of visible ray near 500nm on earth's surface, wavelength is the energy of the visible region of 400nm ~ 750nm is approximately 43% of sunshine gross energy, so in order to efficient utilization, the R and D of bismuth series photocatalyst have achieved a series of great achievement, and bismuthous compound is as BiVO 4, Bi 2moO 6, Bi 2mo 2o 9, Bi 2mo 3o 12and Bi 2wO 4be in the news and there is good absorption under visible light.A series of niobium (tantalum) hydrochlorate photochemical catalyst is widely studied owing to having higher photocatalytic activity.Such as, niobate photocatalyst Pb 3nb 4o 13, BiNbO 4and Bi 2mNbO 7(M=Al, Ga, In, Y, rare earth element and Fe) etc. with niobium potassium compound oxide photocatalyst as KNbO 3, KNb 3o 8, K 4nb 6o 17and K 6nb 10.6o 30deng all, there is good photocatalysis performance, but its intrinsic photocatalytic effect is very weak or do not have activity in visible-range.
Although photocatalysis research has carried out the several years, but at present report to have visible light-responded photochemical catalyst kind still very limited, still also exist that light conversion efficiency is low, poor stability and the problem such as spectral response range is narrow, so it is very necessary for researching and developing the new visible light-responded high efficiency photocatalyst that has.We are to consisting of Ca 3nb 3v 5o 23, Ba 3nb 3v 5o 23, Pb 3nb 3v 5o 23, Sr 3nb 3v 5o 23compound carried out Photocatalytic Performance Study, found that Ca 3nb 3v 5o 23band gap be 2.72 eV, have excellent visible light-responded photocatalysis performance, the band gap width of other sample is all greater than 3.2eV, just can only can show activity under ultraviolet irradiation.
 
Summary of the invention
The object of this invention is to provide and a kind of there is visible light-responded photochemical catalyst Ca 3nb 3v 5o 23and preparation method thereof.
The chemical constitution formula with visible light-responded photochemical catalyst that the present invention relates to is: Ca 3nb 3v 5o 23.
Preparation method's concrete steps of above-mentioned visible light-responded photochemical catalyst are:
(1) by 99.9% analytically pure chemical raw material CaCO 3, Nb 2o 5and V 2o 5starting powder press Ca 3nb 3v 5o 23composition weigh batching.
(2) raw material mixing step (1) prepared, put into ball grinder, add zirconia ball and distilled water, ball milling 8 hours, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
(3) powder step (2) mixed 700 ~ 750 DEG C of pre-burnings, and is incubated 6 hours, naturally cools to room temperature, is then pulverized by ball mill and average diameter of particles is diminished, lower than 2 μm, namely obtain Ca 3nb 3v 5o 23powder.
The spectral response range of the photochemical catalyst that the present invention obtains is wide, the high and good stability of light conversion efficiency, has the effect of decomposing harmful chemical, organic-biological matter and sterilization under visible light illumination; Preparation method is simple in addition, synthesis temperature is low, and cost is low, is applicable to industrial production and application.
Detailed description of the invention
To be specifically described the present invention below:
1, in order to obtain the composite oxides used in the present invention, first use solid-phase synthesis to prepare powder, namely using as the various oxide of raw material or carbonate according to the metering of target constitutional chemistry than mixing, then to synthesize in air atmosphere at ambient pressure.
2, in order to effectively utilize light, the size of the photochemical catalyst in the present invention is preferably in micron level, or even nano particle, and specific area is larger.With oxide powder prepared by solid-phase synthesis, its particle is comparatively large and surface area is less, but can pulverize means by ball mill makes particle diameter diminish.
3, photocatalysis experiment of the present invention is using methyl orange as simulation organic pollution, and its concentration is 20mg/L; Photochemical catalyst Ca 3nb 3v 5o 23addition be 1g/L; Light source uses the xenon lamp of 300W, the vessel that reactive tank uses pyrex to make, and obtains the light that wavelength is greater than 420nm long wavelength, then irradiate photochemical catalyst by wave filter; Catalysis time is set as 60 minutes.
Embodiment 1:
(1) by 99.9% analytically pure chemical raw material CaCO 3, Nb 2o 5and V 2o 5starting powder press Ca 3nb 3v 5o 23composition weigh batching.
(2) raw material mixing step (1) prepared, put into ball grinder, add zirconia ball and distilled water, ball milling 8 hours, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
(3) powder step (2) mixed 700 DEG C of pre-burnings, and is incubated 6 hours, naturally cools to room temperature, is then pulverized by ball mill and average diameter of particles is diminished, lower than 2 μm, namely obtain Ca 3nb 3v 5o 23powder.
Prepared photochemical catalyst, under being greater than the radiation of visible light of 420nm, reaches 97.6% to methyl orange clearance in 60 minutes at wavelength.
Embodiment 2:
(1) by 99.9% analytically pure chemical raw material CaCO 3, Nb 2o 5and V 2o 5starting powder press Ca 3nb 3v 5o 23composition weigh batching.
(2) raw material mixing step (1) prepared, put into ball grinder, add zirconia ball and distilled water, ball milling 8 hours, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
(3) powder step (2) mixed 720 DEG C of pre-burnings, and is incubated 6 hours, naturally cools to room temperature, is then pulverized by ball mill and average diameter of particles is diminished, lower than 2 μm, namely obtain Ca 3nb 3v 5o 23powder.
Prepared photochemical catalyst, under being greater than the radiation of visible light of 420nm, reaches 97.8% to methyl orange clearance in 60 minutes at wavelength.
Embodiment 3:
(1) by 99.9% analytically pure chemical raw material CaCO 3, Nb 2o 5and V 2o 5starting powder press Ca 3nb 3v 5o 23composition weigh batching.
(2) raw material mixing step (1) prepared, put into ball grinder, add zirconia ball and distilled water, ball milling 8 hours, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
(3) powder step (2) mixed 750 DEG C of pre-burnings, and is incubated 6 hours, naturally cools to room temperature, is then pulverized by ball mill and average diameter of particles is diminished, lower than 2 μm, namely obtain Ca 3nb 3v 5o 23powder.
Prepared photochemical catalyst, be greater than the radiation of visible light of 420nm at wavelength under, 60min reaches 98.2% to methyl orange clearance.
The present invention is never limited to above embodiment.Bound, the interval value of each temperature can realize the present invention, do not enumerate embodiment at this.
The made photocatalyst powder of above inventive embodiments can be carried on multiple matrix surface.Matrix can be glass, pottery, active carbon or quartz sand etc., and photochemical catalyst can be carried on matrix surface in the form of a film.

Claims (1)

1. a visible light-responded photochemical catalyst, is characterized in that the chemical constitution formula of described photochemical catalyst is Ca 3nb 3v 5o 23;
Preparation method's concrete steps of described photochemical catalyst are:
(1) by 99.9% analytically pure chemical raw material CaCO 3, Nb 2o 5and V 2o 5starting powder press Ca 3nb 3v 5o 23composition weigh batching;
(2) raw material mixing step (1) prepared, put into ball grinder, add zirconia ball and distilled water, ball milling 8 hours, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves;
(3) powder step (2) mixed 700 ~ 750 DEG C of pre-burnings, and is incubated 6 hours, naturally cools to room temperature, is then pulverized by ball mill and makes average diameter of particles lower than 2 μm, namely obtain Ca 3nb 3v 5o 23powder.
CN201410537369.6A 2014-10-13 2014-10-13 Visible light-responded photocatalyst Ca3Nb3V5O23And preparation method thereof Active CN104275176B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104772135A (en) * 2015-04-08 2015-07-15 三峡大学 Wide-frequency high-efficiency visible light response photocatalyst CaNb2V2O11 and method for preparing wide-frequency high-efficiency visible light response photocatalyst
CN105289577A (en) * 2015-10-31 2016-02-03 江苏师范大学 Vanadium tantalum/niobate photocatalyst and preparation method and application of vanadium tantalum/niobate photocatalyst

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CN1951557A (en) * 2006-11-03 2007-04-25 中国科学院上海硅酸盐研究所 Hydrothermal method for preparing superstructure visible light responsive Bi2WO6 photcatalyst
CN101264934A (en) * 2008-04-11 2008-09-17 浙江大学 Visible light response method for preparing Bi2WO6 photocatalyst fused salt
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104772135A (en) * 2015-04-08 2015-07-15 三峡大学 Wide-frequency high-efficiency visible light response photocatalyst CaNb2V2O11 and method for preparing wide-frequency high-efficiency visible light response photocatalyst
CN105289577A (en) * 2015-10-31 2016-02-03 江苏师范大学 Vanadium tantalum/niobate photocatalyst and preparation method and application of vanadium tantalum/niobate photocatalyst

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Effective date of registration: 20201208

Address after: No.25-1, Gangcheng Road, dongyinggang Economic Development Zone, Hekou District, Dongying City, Shandong Province

Patentee after: Shandong Xingqiang Chemical Industry Technology Research Institute Co.,Ltd.

Address before: Room 502, building 1, No. 40, xiayuangang East Street, Tianhe District, Guangzhou City, Guangdong Province

Patentee before: Guangzhou Boyi Intellectual Property Operation Co.,Ltd.

Effective date of registration: 20201208

Address after: Room 502, building 1, No. 40, xiayuangang East Street, Tianhe District, Guangzhou City, Guangdong Province

Patentee after: Guangzhou Boyi Intellectual Property Operation Co.,Ltd.

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Patentee before: GUILIN University OF TECHNOLOGY