CN105562015A - Visible light responding photocatalyst Ca3Fe2GeO8 and preparation method thereof - Google Patents

Visible light responding photocatalyst Ca3Fe2GeO8 and preparation method thereof Download PDF

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CN105562015A
CN105562015A CN201510935747.0A CN201510935747A CN105562015A CN 105562015 A CN105562015 A CN 105562015A CN 201510935747 A CN201510935747 A CN 201510935747A CN 105562015 A CN105562015 A CN 105562015A
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visible light
ca3fe2geo8
geo
preparation
photochemical catalyst
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程柳
唐莹
李洁
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Guilin University of Technology
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Guilin University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/835—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with germanium, tin or lead
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts

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Abstract

The invention discloses a broadband and efficient visible light responding photocatalyst Ca3Fe2GeO8 and a preparation method of the visible light responding photocatalyst Ca3Fe2GeO8. A chemical composition formula of the visible light responding photocatalyst Ca3Fe2GeO8 is Ca3Fe2GeO8.The invention also discloses the preparation method of the visible light responding photocatalyst Ca3Fe2GeO8. The visible light responding photocatalyst Ca3Fe2GeO8 obtained through the preparation method has the advantages of wide spectral response range, high light conversion efficiency, high stability and the like. The visible light responding photocatalyst Ca3Fe2GeO8 has the functions of decomposing harmful chemical substances and organic biomass and sterilizing under the irradiation of visible light; in addition, the preparation method is simple, the synthetic temperature is low, and the cost is low, so that the visible light responding photocatalyst Ca3Fe2GeO8 is suitable for industrial production and application.

Description

Visible light-responded photochemical catalyst Ca 3fe 2geO 8and preparation method thereof
Technical field
The present invention relates to a kind of visible light-responded photochemical catalyst Ca 3fe 2geO 8and 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, the current exploration to visible light-responded photochemical catalyst is the summary of experience drawn by great many of experiments with exploitation major part, in theory also cannot from the crystal structure of compound, composition, the physicochemical properties such as molecular weight are predicted its photocatalysis performance, therefore at present report to have visible light-responded photochemical catalyst kind still very limited, and it is low to there is light conversion efficiency, synthesis difficulty, poor stability and the problem such as spectral response range is narrow, research and develop that new preparation method is simple and to have the visible light-responded high efficiency photocatalyst of wideband be that this area scientific and technical personnel thirst for solving always but are difficult to the difficult problem that succeeds all the time, which greatly limits extensive use and the development of photochemical catalyst.We are to consisting of Ca 3fe 2geO 8, Ba 3fe 2geO 8and Sr 3fe 2geO 8sample carried out Photocatalytic Performance Study.Found that Ca 3fe 2geO 8band gap width is 2.65eV, has excellent visible light-responded photocatalysis performance; Ba 3fe 2geO 8and Sr 3fe 2geO 8for insulator, under ultraviolet irradiation, also do not show activity.
Summary of the invention
The object of this invention is to provide and a kind of there is visible light-responded photochemical catalyst Ca 3fe 2geO 8and preparation method thereof.
The chemical constitution formula with visible light-responded photochemical catalyst that the present invention relates to is: Ca 3fe 2geO 8.
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, Fe 2o 3and GeO 2powder press Ca 3fe 2geO 8composition weigh batching.
(2) raw material mixing step (1) prepared, put into ball grinder, add zirconia ball and absolute ethyl alcohol, ball milling 8 hours, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
(3) powder step (2) mixed 800 ~ 850 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 3fe 2geO 8powder.
Advantage of the present invention: Ca 3fe 2geO 8the visible light-responded wide frequency range of photochemical catalyst, 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 3fe 2geO 8addition 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, then irradiate photochemical catalyst by wave filter; Catalysis time is set as 60 minutes.
Embodiment 1:
(1) pure chemistry raw materials of Ca CO will be analyzed 3, Fe 2o 3and GeO 2powder press Ca 3fe 2geO 8composition weigh batching.
(2) raw material mixing step (1) prepared, put into ball grinder, add zirconia ball and absolute ethyl alcohol, ball milling 8 hours, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
(3) powder step (2) mixed 800 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 3fe 2geO 8powder.
Prepared photochemical catalyst, under being greater than the radiation of visible light of 420nm, reaches 97.9% to methyl orange clearance in 60 minutes at wavelength.
Embodiment 2:
(1) pure chemistry raw materials of Ca CO will be analyzed 3, Fe 2o 3and GeO 2powder press Ca 3fe 2geO 8composition weigh batching.
(2) raw material mixing step (1) prepared, put into ball grinder, add zirconia ball and absolute ethyl alcohol, ball milling 8 hours, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
(3) powder step (2) mixed 825 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 3fe 2geO 8powder.
Prepared photochemical catalyst, under being greater than the radiation of visible light of 420nm, reaches 98.7% to methyl orange clearance in 60 minutes at wavelength.
Embodiment 3:
(1) pure chemistry raw materials of Ca CO will be analyzed 3, Fe 2o 3and GeO 2powder press Ca 3fe 2geO 8composition weigh batching.
(2) raw material mixing step (1) prepared, put into ball grinder, add zirconia ball and absolute ethyl alcohol, ball milling 8 hours, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves.
(3) powder step (2) mixed 850 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 3fe 2geO 8powder.
Prepared photochemical catalyst, be greater than the radiation of visible light of 420nm at wavelength under, 60min reaches 98.1% 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 3fe 2geO 8;
Preparation method's concrete steps of described photochemical catalyst are:
(1) pure chemistry raw materials of Ca CO will be analyzed 3, Fe 2o 3and GeO 2powder press Ca 3fe 2geO 8composition weigh batching;
(2) raw material mixing step (1) prepared, put into ball grinder, add zirconia ball and absolute ethyl alcohol, ball milling 8 hours, is mixed and finely ground, and takes out and dries, and crosses 200 mesh sieves;
(3) powder step (2) mixed 800 ~ 850 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 3fe 2geO 8powder.
CN201510935747.0A 2015-12-15 2015-12-15 Visible light responding photocatalyst Ca3Fe2GeO8 and preparation method thereof Pending CN105562015A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102068954A (en) * 2009-11-24 2011-05-25 中国科学院物理研究所 Method and device for photocatalytic reaction
CN103418389A (en) * 2013-08-20 2013-12-04 桂林理工大学 Visible-light-response photocatalyst BaFe4Ti2O11 and preparation method thereof
CN103706352A (en) * 2013-11-17 2014-04-09 桂林理工大学 Visible light response photocatalyst SrLa10V4O26 and preparation method thereof
US20140235736A1 (en) * 2011-10-24 2014-08-21 Sogang University Research Foundation Apparatus and method for reducing carbon dioxide using solar light
CN104190400A (en) * 2014-09-27 2014-12-10 桂林理工大学 Visible light responding photocatalyst Ca3La4V2O14 and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102068954A (en) * 2009-11-24 2011-05-25 中国科学院物理研究所 Method and device for photocatalytic reaction
US20140235736A1 (en) * 2011-10-24 2014-08-21 Sogang University Research Foundation Apparatus and method for reducing carbon dioxide using solar light
CN103418389A (en) * 2013-08-20 2013-12-04 桂林理工大学 Visible-light-response photocatalyst BaFe4Ti2O11 and preparation method thereof
CN103706352A (en) * 2013-11-17 2014-04-09 桂林理工大学 Visible light response photocatalyst SrLa10V4O26 and preparation method thereof
CN104190400A (en) * 2014-09-27 2014-12-10 桂林理工大学 Visible light responding photocatalyst Ca3La4V2O14 and preparation method thereof

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