CN103691421A - CeVO4 micro-sphere photocatalyst and preparation method thereof - Google Patents
CeVO4 micro-sphere photocatalyst and preparation method thereof Download PDFInfo
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- CN103691421A CN103691421A CN201310751520.1A CN201310751520A CN103691421A CN 103691421 A CN103691421 A CN 103691421A CN 201310751520 A CN201310751520 A CN 201310751520A CN 103691421 A CN103691421 A CN 103691421A
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Abstract
The invention discloses a CeVO4 micro-sphere photocatalyst and a preparation method thereof, and belongs to the field of nano-micron material preparation. The preparation method comprises the following steps: dissolving Ce(NO3)3.6H2O and NH4VO3 in deionized water according to a molar ratio of 1 to 1 to form a solution A; weighing EDTA (ethylene diamine tetraacetic acid) and dissolving in the deionized water to form a solution B, wherein the molar ratio of Ce(NO3)3.6H2O to EDTA is 1 to 1; pouring the solution B into the solution A, mixing and magnetically stirring; putting the stirred solution into a stainless steel reaction kettle, putting the reaction kettle into an oven, heating to 180 DEG C, and preserving heat for 6-24 hours; performing furnace cooling on a hydrothermal product, washing by the deionized water and ethanol in sequence, and drying. CeVO4 micro-spheres are square single crystals and have space groups 141/amd [141]; in addition, the CeVO4 micro-spheres are spherical and have the diameters of 2-4 microns and the spherical walls of 100 nm. The preparation method is simple and the particle size distribution is uniform.
Description
Technical field
The present invention relates to the preparation field of nano and micro materials, more particularly, relate to a kind of CeVO
4micron ball photochemical catalyst and preparation method thereof.
Background technology
Novel inorganic nonmetal nano material is owing to having the focus that unique physical character and chemical property are Recent study.Cerium vanadate (the CeVO of tetragonal phase
4, hereinafter to be referred as CVO) and as a kind of composite metal oxide, the optics of tool uniqueness, electricity, magnetics and redox property, be widely used in the fields such as photoelectricity, catalysis, biology.For example as traditional fluorescent material, be widely used in polarizer, el light emitting device and main laser material, catalytic oxidation of propane dehydrogenation is propylene, can be used as the element of formation of solid polycomplex anode of oxide fuel cell etc.Having in addition its energy gap of report is 2.7eV left and right, can be used as photochemical catalyst catalytic degradation dyestuff and organic matter under radiation of visible light.
The method of synthetic CVO nano material generally includes liquid phase synthetic technology, vapour deposition (CVD), microwave-assisted synthesis and traditional solid sintering technology etc.With respect to gas phase and solid phase method, the advantage such as liquid phase method has that method is simple, energy-conserving and environment-protective, temperature are lower, is widely used at present.Liquid phase preparation process comprises hydro-thermal solvent-thermal method, sol-gel process, low-temperature molten salt method, self-propagating combustion, coprecipitation, ultrasonic synthetic and polyalcohol method etc.
Document 1(Nuengruethai Ekthammathat, Titipun Thongtem, Anukorn Phuruangrat, and Somchai Thongtem, Journal of Nanomaterials, 2013,7,1-7) Ce (NO for Nuengruethai Ekthammathat etc.
3)
36H
2o and NH
4vO
3for raw material, by the different pH values of HCl and NaOH regulator solution, microwave reaction 180W, 120min makes flower-shaped and shaft-like CVO.
Document 2(Hong Deng, Chenmin Liu, Shihe Yang, Si Xiao, Zhang-Kai Zhou, and Qu-Quan Wang, Crystal Growth & Design, 2008,8,12,4432-4439) Ce (NO for Hong Deng etc.
3)
36H
2o, Na
3vO
4with EDTA be raw material, the different pH values with ammoniacal liquor regulator solution are heated to 180 ℃ in reactor, react 24h, according to the proportioning difference of reactant made CVO nano rod, nano wire and careless pencil, flower-shaped CVO is nanocrystalline.
Document 3(Cuicui Yu, Min Yu, Chunxia Li, Cuimiao Zhang, Piaoping Yang, and Jun Lin, Crystal Growth & Design, 2009,9,2,783-791) Ce (NO for Cuicui Yu etc.
3)
36H
2o, NH
4vO
3with rare HNO
3for raw material, by the different pH values of ammoniacal liquor regulator solution, ultrasonic reaction 1h, has made fusiform CVO nanocrystalline.
In document 1, adopt the different pH values of HCl and NaOH regulator solution, in document 2 and document 3, all adopt the different pH values of ammoniacal liquor regulator solution, make whole reaction system present alkalescent.Applicant tests discovery, pH is very large to the pattern effect of crystal growth, that document 1 obtains is flower-shaped and shaft-like CVO, document 2 obtains is that CVO nano rod, nano wire and careless pencil, flower-shaped CVO are nanocrystalline, what document 3 obtained is that fusiform CVO is nanocrystalline, all the three-dimensional spherulite of unsuccessful acquisition.In addition, in document 2, adopt Na
3vO
4do vanadium source, relative price is expensive, and does not obtain three-dimensional spherulite.
Document 4(Hong Deng, Shihe Yang, Si Xiao, Hong-Mei Gong, and Qu-Quan Wang, J.AM.CHEM.SOC.2008,130,2032-2040) Ce (NO for Hong Deng etc.
3)
36H
2o, Na
3vO
4, NaOH, octadecylene and oleic acid, oleyl amine be raw material, after processing early stage, heats 180 ℃ in reactor, reaction 24h, the CVO that has made box-shaped is nanocrystalline, its diameter is about 40nm.
Document 5(Thanh-Dinh Nguyen, Cao-Thang Dinh, and Trong-On Do, Langmuir, 2009,25 (18), 11142 – 11148) Ce (NO such as Thanh-Dinh Nguyen
3)
36H
2o, toluene, acetic acid, potassium oleate are raw material stirring reaction 1h at 70 ℃, make Ce (OA)
3compound, uses V
2o
5, NaOH, TOABr, toluene is that mixed raw material obtains VO
4(TOA)
3compound, then the two is mixed, adds oleyl amine, heat 180 ℃ in reactor, reaction 16h, and the CVO that to have made diameter be 15nm is nanocrystalline.
Document 1~document 5 has prepared CeVO by diverse ways respectively
4nano and micro materials, but problems and the deficiency such as these methods still exist complex process, environmental pollution, organic matter amount is large, particle is inhomogeneous.In sum, the CeVO that prepared by existing bibliographical information
4crystal mostly is common nanocrystalline and one-dimensional nano line or nano rod, few three-dimensional chondritic also want high-temperature calcination after Hydrothermal Synthesis, and synthetic particle size distribution is inhomogeneous, poor-performing.
Summary of the invention
1. the technical problem that invention will solve
The object of the invention is to overcome and in prior art, cannot by suitable method, prepare particle diameter and be evenly distributed, and be the CeVO of three-dimensional chondritic
4the problem of micron ball, provides a kind of CeVO
4micron ball photochemical catalyst and preparation method thereof, adopts technical scheme of the present invention, and technique is simple, be convenient to industrialization produces, and the product of preparation has, and specific area is large, particle diameter is evenly distributed, degree of crystallinity high.
2. technical scheme
For achieving the above object, technical scheme provided by the invention is:
A kind of CeVO of the present invention
4micron ball photochemical catalyst, this CeVO
4micron ball photochemical catalyst has following character: (1), this CeVO
4micron ball is cubic monocrystalline, and space group is: 14
1/ amd[141]; (2), this CeVO
4micron ball is spherical, and its diameter is 2~4 μ m, and ball wall is 100nm.
A kind of CeVO of the present invention
4the preparation method of micron ball photochemical catalyst, its step is as follows:
Step 1, the Ce (NO that is 1:1 by mol ratio
3)
36H
2o and NH
4vO
3be dissolved in deionized water, be stirred to whole dissolvings, form solution A;
Step 3, the solution B that step 2 is obtained are poured in the solution A that step 1 obtains, and the two mixes, and carries out magnetic agitation;
Step 4, the solution after step 3 stirs is packed into and had in teflon-lined stainless steel cauldron, adding deionized water makes liquor capacity to 70%~80% of reactor volume, above-mentioned reactor is put into baking oven, be heated to 180 ℃, and insulation reaction 6~24 hours;
A kind of CeVO of the present invention
4the preparation method of micron ball photochemical catalyst, in step 3, the temperature of magnetic agitation is room temperature, mixing time is 0.5~1 hour.
A kind of CeVO of the present invention
4the preparation method of micron ball photochemical catalyst, in step 5, baking temperature is 60~80 ℃, be 5~6 hours drying time.
3. beneficial effect
Adopt technical scheme provided by the invention, compare with existing known technology, there is following remarkable result:
(1) a kind of CeVO of the present invention
4the preparation method of micron ball photochemical catalyst, its raw material adopts Ce (NO
3)
36H
2o, NH
4vO
3and EDTA, adopt simple gentleness, eco-friendly hydrothermal method, utilize EDTA for complexant and template direction agent, and and NH
4vO
3in NH
4 +the pH value of the whole reaction system of co-controlling is faintly acid, and the growth that gentle reaction system is nano and micro materials provides suitable environment, thereby is that diameter is the spherical CeVO of 2~4 μ m by controlling the addition control products therefrom pattern of EDTA
4micron ball, and particle diameter is evenly distributed.But, CeVO prepared by existing bibliographical information
4crystal mostly is common nanocrystalline and one-dimensional nano line or nano rod, few three-dimensional chondritic also to want after Hydrothermal Synthesis high-temperature calcination and its particle diameter to distribute also inhomogeneous, the present invention passes through control Ce (NO
3)
36H
2o, NH
4vO
3with the mol ratio of EDTA be 1:1:1, successfully realized the spherical CeVO that obtains three-dimensional appearance under the condition of low temperature
4crystal, ball wall is thinner, and diameter is about 2~4 μ m, is the monocrystalline of complete crystallization, and this is in prior art, not yet to have bibliographical information.CeVO of the present invention
4micron ball photochemical catalyst, because its hollow ball-type structural material has the features such as specific area is large, density is low, good stability, and the photocatalytic activity of photochemical catalyst and the degree of crystallinity of catalyst, size, pattern etc. are because have substantial connection, photocatalysis performance test experiments proved invention CeVO
4micron ball and one-dimentional structure CeVO
4material is compared, and has good photocatalysis performance.Experiment confirms: synthetic CeVO
4the energy gap of micron ball is 2.73eV, has response in visible-range, and to dyestuff rhodamine B, at simulation radiation of visible light, the degradation rate after 4 hours can reach 96.15%.
(2) a kind of CeVO of the present invention
4the preparation method of micron ball photochemical catalyst, usings EDTA as complexant and template direction agent, and environmental protection is easy to control, and avoids using toxicity large, dangerous large organic solvent and complexant; Course of reaction is without adding surfactant or other any organic matters, and experimental technique route is simple, operation is convenient, environmental friendliness.
Accompanying drawing explanation
Fig. 1 is a kind of CeVO of the present invention
4the preparation method's of micron ball photochemical catalyst schematic flow sheet.
Fig. 2 is the CeVO of embodiment 1 preparation
4the XRD spectra of micron ball.
Fig. 3 is the CeVO of embodiment 1 preparation
4the SEM figure of micron ball.
Fig. 4 is the CeVO of embodiment 1 preparation
4the TEM figure of micron ball.
Fig. 5 is the CeVO of embodiment 1 preparation
4the HRTEM figure of micron ball.
The specific embodiment
For further understanding content of the present invention, the present invention is described in detail in conjunction with the accompanying drawings and embodiments.
Embodiment 1
In conjunction with Fig. 1, a kind of CeVO of the present embodiment
4the preparation method of micron ball photochemical catalyst, its step is as follows:
Step 1, the Ce (NO that is 1:1 by mol ratio
3)
36H
2o and NH
4vO
3be dissolved in 20mL deionized water, Ce (NO in the present embodiment
3)
36H
2o and NH
4vO
3take each 5mmol, be stirred to whole dissolvings, form colourless solution A;
Step 3, the solution B that step 2 is obtained are poured in the solution A that step 1 obtains, and the two mixes, and carries out magnetic agitation, the temperature of magnetic agitation is room temperature, mixing time be 0.5~1 hour all can, in the present embodiment, mixing time is 0.7 hour, and reactant is mixed;
Step 4, the solution after step 3 stirs is packed into and had in teflon-lined stainless steel cauldron, adding deionized water makes liquor capacity to 70%~80% of reactor volume, above-mentioned reactor is put into baking oven, be heated to 180 ℃, and insulation reaction 6~24 hours all can, in the present embodiment, insulation reaction is 12 hours;
The CeVO that the method for employing the present embodiment prepares
4micron ball photochemical catalyst has following character: (1), this CeVO
4micron ball is cubic monocrystalline, and space group is: 14
1/ amd[141]; (2), this CeVO
4micron ball is spherical, and its diameter is 2~4 μ m, and ball wall is 100nm.Fig. 2 is the prepared CeVO of the present embodiment
4nanocrystalline XRD spectra, in figure, all diffraction maximums can index be Emission in Cubic CeVO
4standard powder diffraction data [referring to Joint Committee on Powder Diffraction Standards (JCPDS), File No.12-0757], do not find the diffraction maximum of any impurity.Fig. 3, Fig. 4, Fig. 5 are the prepared CeVO of the present embodiment
4the SEM figure of micron ball, TEM figure and HRTEM figure, can find the CeVO making
4micron crystalline substance is spherical, diameter 2~4 μ m.HRTEM figure gained interplanar distance is 0.260nm, corresponding to the index CeVO of institute
4(220) crystal face.
Comparative example 1
This comparative example be a kind of CeVO
4the preparation method of nano and micro materials, its step is with embodiment 1, and difference is: in this comparative example, in step 2, take the amount 0mmol of EDTA, find the CeVO finally obtaining through test
4the pattern of powder is the mixture of irregular bulk and stub.
Comparative example 2
This comparative example be a kind of CeVO
4the preparation method of nano and micro materials, its step is with embodiment 1, and difference is: in this comparative example, step 2 takes the amount 2.5mmol of EDTA, Ce (NO
3)
36H
2o, NH
4vO
3with the mol ratio of EDTA be 1:1:0.5, through test, find the CeVO finally obtain
4the pattern of powder is irregular spherical, and diameter is 2~6 μ m, also has irregular block aggregate.
Comparative example 3
This comparative example be a kind of CeVO
4the preparation method of nano and micro materials, its step is with embodiment 1, and difference is: in this comparative example, step 2 takes the amount 7.5mmol of EDTA, Ce (NO
3)
36H
2o, NH
4vO
3with the mol ratio of EDTA be 1:1:1.5, through test, find the CeVO finally obtain
4the pattern of powder is irregular spherical and spherical agglomerated thing.
Comparative example 4
This comparative example be a kind of CeVO
4the preparation method of nano and micro materials, its step is with embodiment 1, and difference is: in this comparative example, step 2 takes the amount 10mmol of EDTA, Ce (NO
3)
36H
2o, NH
4vO
3with the mol ratio of EDTA be 1:1:2, through test, find the CeVO finally obtain
4the pattern of powder is for being irregular spherical, and diameter is about 1~2 μ m, and ball wall is thicker, reunites more serious.
Known according to comparative example 1~4 and embodiment 1, in order to obtain the uniform spherical CeVO of pattern
4micron is brilliant, and its key is exactly to select EDTA as complexant and template direction agent, and controls Ce (NO
3)
36H
2o, NH
4vO
3with the mol ratio of EDTA, this is the outstanding improvement of the present invention, although adopted EDTA as raw material in background technology Literature 1, adopts the pH value of ammoniacal liquor regulator solution to cause obtaining the CeVO of three-dimensional spherical structure in document 1
4powder.Except technical scheme of the present invention, all cannot obtain the uniform spherical CeVO of pattern
4micron is brilliant.
Claims (4)
1. a CeVO
4micron ball photochemical catalyst, is characterized in that, this CeVO
4micron ball photochemical catalyst has following character:
(1), this CeVO
4micron ball is cubic monocrystalline, and space group is: 14
1/ amd[141];
(2), this CeVO
4micron ball is spherical, and its diameter is 2~4 μ m, and ball wall is 100nm.
2. a CeVO
4the preparation method of micron ball photochemical catalyst, is characterized in that, its step is as follows:
Step 1, the Ce (NO that is 1:1 by mol ratio
3)
36H
2o and NH
4vO
3be dissolved in deionized water, be stirred to whole dissolvings, form solution A;
Step 2, take EDTA, wherein: Ce (NO
3)
36H
2the mol ratio of O and EDTA is 1:1, EDTA is dissolved in deionized water, and is stirred to whole dissolvings, forms solution B;
Step 3, the solution B that step 2 is obtained are poured in the solution A that step 1 obtains, and the two mixes, and carries out magnetic agitation;
Step 4, the solution after step 3 stirs is packed into and had in teflon-lined stainless steel cauldron, adding deionized water makes liquor capacity to 70%~80% of reactor volume, above-mentioned reactor is put into baking oven, be heated to 180 ℃, and insulation reaction 6~24 hours;
Step 5, the product after step 4 hydro-thermal is cooling with stove after, successively with deionized water and ethanol, clean, be then drying to obtain CeVO
4micron ball photochemical catalyst.
3. a kind of CeVO according to claim 2
4the preparation method of micron ball photochemical catalyst, is characterized in that: in step 3, the temperature of magnetic agitation is room temperature, and mixing time is 0.5~1 hour.
4. a kind of CeVO according to claim 2
4the preparation method of micron ball photochemical catalyst, is characterized in that: in step 5, baking temperature is 60~80 ℃, and be 5~6 hours drying time.
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CN201510657930.9A CN105126814B (en) | 2013-12-31 | 2013-12-31 | A kind of CeVO4The preparation method of micron ball photocatalyst |
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CN104445399A (en) * | 2014-11-30 | 2015-03-25 | 湘潭大学 | Preparation method of hexagonal cerium vanadate nanodisk and use thereof |
CN105253916A (en) * | 2015-08-25 | 2016-01-20 | 江西师范大学 | Preparation method for monoclinic phase Eu2O2SO4 microsphere |
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CN108620109A (en) * | 2018-06-12 | 2018-10-09 | 常州大学 | The preparation method and applications of heterojunction photocatalyst are converted on a kind of cerium vanadate/modified attapulgite |
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Also Published As
Publication number | Publication date |
---|---|
CN105126814A (en) | 2015-12-09 |
CN103691421B (en) | 2016-01-27 |
CN105126814B (en) | 2017-09-15 |
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