CN105749898B - A kind of nanometer Zinc oxide powder photochemical catalyst and preparation method thereof - Google Patents
A kind of nanometer Zinc oxide powder photochemical catalyst and preparation method thereof Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000003054 catalyst Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000001704 evaporation Methods 0.000 claims abstract description 8
- 230000008020 evaporation Effects 0.000 claims abstract description 8
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 8
- 238000007146 photocatalysis Methods 0.000 claims abstract description 7
- 230000001699 photocatalysis Effects 0.000 claims abstract description 7
- 239000011787 zinc oxide Substances 0.000 claims abstract description 5
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 9
- 239000000084 colloidal system Substances 0.000 claims description 7
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- 239000013557 residual solvent Substances 0.000 claims description 6
- 239000012265 solid product Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical compound [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 239000008236 heating water Substances 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- 239000002826 coolant Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 239000011941 photocatalyst Substances 0.000 abstract description 14
- 239000011858 nanopowder Substances 0.000 abstract description 8
- 238000001816 cooling Methods 0.000 abstract description 7
- 239000000843 powder Substances 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000000227 grinding Methods 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000005204 segregation Methods 0.000 abstract description 2
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 239000003125 aqueous solvent Substances 0.000 description 10
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 8
- 229940012189 methyl orange Drugs 0.000 description 8
- 230000000593 degrading effect Effects 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 239000006260 foam Substances 0.000 description 5
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000011686 zinc sulphate Substances 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000005562 fading Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/10—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation
- A62D3/17—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation to electromagnetic radiation, e.g. emitted by a laser
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/26—Organic substances containing nitrogen or phosphorus
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/28—Organic substances containing oxygen, sulfur, selenium or tellurium, i.e. chalcogen
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Abstract
The invention discloses a kind of nanometer Zinc oxide powder photochemical catalysts and preparation method thereof, the molecular formula of the nano powder photocatalyst is ZnO, it is mainly characterized by using soluble zinc sulfate for raw material, it is dissolved in that colourless transparent solution is made in deionized water, precursor powder will be made after mixed solution evaporation, dry, grinding；Nanometer Zinc oxide powder photochemical catalyst is being obtained after high-temperature calcination and natural cooling.The granularity of this nano powder photocatalyst has the advantages such as uniform tiny, good dispersion, purity are high, photocatalysis performance is good in 5~20nm, almost spherical.The raw material of the present invention is single to be easy to get, the problems such as not being related to the uniformity and component segregation of predecessor, preparation process is simple, reproducible, calcination temperature is low, and short preparation period, at low cost, it is easy to produce in enormous quantities, product has broad application prospects in fields such as light catalytic purifying treatment technologies.
Description
Technical field
The present invention relates to photocatalyst technology field, especially a kind of nanometer Zinc oxide powder photochemical catalyst and its preparation side
Method.
Background technology
With the increasingly raising of people's living standard, environmental pollution and energy shortage are that the current whole mankind faces and be badly in need of solution
Two significant problems certainly, and light catalytic purifying treatment technology is expected to one of effective solution route as these problems.Wherein,
Be most widely used is semi-conducting material photochemical catalyst, such as TiO2、ZnO、WO3、Fe2O3Deng.Time in the past few decades
In, TiO2Photochemical catalyst because it is active it is high, stability is good, the nontoxic and characteristics such as of low cost due to cause the very big pass of people
Note, but its energy gap（3.8eV）Wider, absorbable light wave is predominantly located at ultra-violet (UV) band, and to the absorption of visible light compared with
Few, this severely limits TiO2The application of catalysis material.ZnO is also a kind of important raw material of industry, in coating, rubber, pottery
Many fields such as porcelain and glass have wide application prospect.Nano zine oxide because particle size is small, large specific surface area due to have it is small
Dimensional effect, skin effect and quantum size effect etc., show good photocatalysis performance, piezoelectric property, high conductivity with
And the ability of scattering and absorption ultraviolet light.With TiO2It compares, the energy gap of nano zine oxide（3.2eV）It is relatively narrow, photoresponse model
It encloses more extensively, is a kind of sewage purification photochemical catalyst with potential using value.
Currently, the document report in relation to nanometer Zinc oxide powder preparation method has very much, such as：It is traditional solid phase method, molten
Glue-gel method, directly（Uniformly）The precipitation method, chemical vapour deposition technique and hydrothermal synthesis method etc..From the performance of photochemical catalyst and
From the aspect of synthesis technology, these preparation methods have its shortcoming.Such as：Traditional solid phase method needs higher sintering temperature
Degree, is unevenly distributed with product cut size, the shortcomings of easily reunion；Powder quality made from sol-gel method is preferable, but colloidal sol-
The preparation process of gel is easily influenced by factors such as solution PH, concentration and temperature, is taken longer；Chemical vapour deposition technique prepares
Though powder quality it is high, its yield is not high, production equipment is expensive, is not suitable for industrialized production；And hydro-thermal method is to experimental facilities
It is more demanding, the powder of synthesis limits photocatalysis efficiency because particle is larger.Therefore, seek a kind of more economical and convenient
Method is evenly dispersed to prepare, and the high nanometer Zinc oxide powder photochemical catalyst of photocatalysis efficiency has positive realistic meaning.
Invention content
It is insufficient existing for existing powder synthetic technology it is an object of the invention to overcome, it provides a kind of with high efficiency photocatalysis
Performance, uniformly tiny, good dispersion and purity height, raw material is simple and easy to get, short preparation period, low energy consumption, has easily to operate
Nano powder photocatalyst of zincblende lattce structure and preparation method thereof.
To reach above-mentioned technical problem, the present invention adopts the following technical scheme that：
There is zincblende lattce structure, spheric granules to use by a kind of nanometer Zinc oxide powder photochemical catalyst, molecular formula ZnO
Following methods are prepared：
1. the configuration of solution
By dissolution of raw material in deionized water, the solution A of a concentration of 0.2-0.5M is obtained；Wherein raw material is soluble Zn
Sulfate；
2. evaporation and drying
The method for first using heating water bath, solvent in the solution A is evaporated at 80 DEG C to solution/colloid critical condition,
Obtain mixture B；Then it uses the method for microwave heating to continue to evaporate the solvent in the mixture B at 80 DEG C, continues 4h, obtain
To gluey transparent presoma C；The presoma C is heat-treated to 1~5h under conditions of 150~300 DEG C again, removal is remaining molten
Agent water, and five crystallizations water are lost, obtain solid product；It is about 50nm Precursor Powders the solid product to be ground, grain size is made
D；
3. being heat-treated
The Precursor Powder D is calcined into 1~5h at 800~1000 DEG C, it is about 5~20nm's to obtain grain size after natural cooling
Nanometer Zinc oxide powder photochemical catalyst.
Preferably, step 2. described in presoma C heat treatment conditions be 200 DEG C heat preservation 2h.
Preferably, step 3. described in Precursor Powder D calcination condition be 900 DEG C heat preservation 3h.
Preferably, raw material is zinc sulfate.
Preferably, a concentration of 0.26M of the solution A.
Compared with prior art, advantageous effects of the invention：
1, the preparation method of nanometer Zinc oxide powder photochemical catalyst provided by the invention, raw material is simple, auxiliary using microwave
It helps and prepares presoma, conducive to the nano-powder of good dispersion is obtained, calcination temperature is relatively low, short preparation period, reproducible, prepares
Method is simple, is easy to produce in enormous quantities；
2, required raw material only has one kind, avoids phenomena such as raw material mixes uneven or component segregation；Uniformly divide conducive to producing
Scattered nano powder photocatalyst；
3, high by the nano powder photocatalyst purity prepared by technical solution of the present invention, good dispersion, particle size point
Cloth is uniform, and photocatalysis efficiency is high.
Description of the drawings
Fig. 1 is the X-ray powder diffraction pattern of nanometer Zinc oxide powder photochemical catalyst prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM of nanometer Zinc oxide powder photochemical catalyst prepared by the embodiment of the present invention 1；
Fig. 3 is the TEM of nanometer Zinc oxide powder photochemical catalyst prepared by the embodiment of the present invention 1；
Fig. 4 is the uv drs absorption spectrum of nanometer Zinc oxide powder photochemical catalyst prepared by the embodiment of the present invention 1, is inserted
Figure is that its energy gap calculates collection of illustrative plates；
It is dye during nanometer Zinc oxide powder photocatalyst for degrading methyl orange prepared by the embodiment of the present invention 1 that a is schemed in Fig. 5
Expect colour fading photo；
It is nanometer Zinc oxide powder photocatalyst for degrading methyl orange process prepared by the embodiment of the present invention 1 that b is schemed in Fig. 5（C/
C0）Collection of illustrative plates, wherein C0For the original concentration of methyl orange solution, C is the methyl orange solution concentration of different moments；
Fig. 6 is the kinetic profile of nanometer Zinc oxide powder photocatalyst for degrading methyl orange prepared by the embodiment of the present invention 1,
Abscissa is light application time in figure, and ordinate is ln (C0/C)。
Specific implementation mode
Embodiment 1：
Weigh 1.50g ZnSO4·7H2O is dissolved in the deionized water of 20ML, and stirring at room temperature forms colourless transparent solution
A；Then solution A is placed on about 3h in 80 DEG C of water-baths, evaporation aqueous solvent obtains mixture B to solution/colloid critical condition；
Then B is put into 80 DEG C of heating about 4h in micro-wave oven, continues to evaporate wherein most aqueous solvent, obtain gluey transparent presoma
C；Presoma C is put into 150 DEG C of heat preservation 2h in an oven, residual solvent water is removed and loses 5 crystallizations water；The white bubble that will be obtained
Precursor Powder D is made in the grinding of foam shape object；Precursor Powder D is packed into alumina crucible, 900 DEG C of temperature lower calcinations in Muffle furnace
3h obtains nanometer Zinc oxide powder photochemical catalyst after furnace cooling.The granularity of this nano powder photocatalyst is in 5~20nm.
Referring to attached drawing 1, it is the XRD diffracting spectrums of nanometer Zinc oxide powder photochemical catalyst manufactured in the present embodiment, from Fig. 1
In as can be seen that diffraction peak intensity is high and sharp, illustrate synthesized by nano powder photocatalyst crystallinity it is good.
Referring to attached drawing 2, it is the pattern SEM pictures of nanometer Zinc oxide powder photochemical catalyst manufactured in the present embodiment, from Fig. 2
In as can be seen that powder granularity in 5~20nm, favorable dispersibility.
Referring to attached drawing 3, it is the pattern TEM pictures of nanometer Zinc oxide powder photochemical catalyst manufactured in the present embodiment, from Fig. 3
In as can be seen that particle has certain shape, even size distribution, crystallinity is good.
Referring to attached drawing 4, it is the uv drs absorption light of nanometer Zinc oxide powder photochemical catalyst manufactured in the present embodiment
Spectrum, illustration are that its energy gap calculates collection of illustrative plates.As seen from Figure 4, nanometer Zinc oxide powder is ultraviolet less than 400nm in wavelength
There is apparent light absorption in area, the direct bandwidth angle value 3.19eV being calculated with illustration（388nm）It is consistent.
Referring to attached drawing 5, it is nanometer Zinc oxide powder photochemical catalyst manufactured in the present embodiment（0.1g）In simulated solar irradiation
Dyestuff colour fading process photo during the lower degradation 50ML methyl oranges (10Mg/L) of irradiation；Fig. 5 b are receiving for preparation of the embodiment of the present invention
Rice Zinc oxide powder photocatalyst for degrading methyl orange process（C/C0）Collection of illustrative plates, wherein C0For the original concentration of methyl orange solution, C is
The methyl orange solution concentration of different moments.It can be seen from Fig. 5a that nanometer Zinc oxide powder has good simulated solar irradiation
Catalytic degradation methyl orange effect；From Fig. 5 b it is found that methyl orange degradation rate is 95% in 1 hour.
Referring to attached drawing 6, it is the dynamics of nanometer Zinc oxide powder photocatalyst for degrading methyl orange manufactured in the present embodiment
Collection of illustrative plates, abscissa is light application time in figure, and ordinate is ln (C0/C)。
From fig. 6 it can be seen that the process of nanometer Zinc oxide powder photocatalyst for degrading methyl orange meets pseudo- single order power
Relationship ln (C0/C)=kt+ ln(C0/C1), C1The concentration of methyl orange solution when to start illumination.Obviously, ln (C0/ C) and illumination
Time, t was in a linear relationship, degradation rate constant k=0.0489Min-1.
Embodiment 2：
Weigh 1.50g ZnSO4·7H2O is dissolved in the deionized water of 20ML, and stirring at room temperature forms colourless transparent solution
A；Then solution A is placed on about 3h in 80 DEG C of water-baths, evaporation aqueous solvent obtains mixture B to solution/colloid critical condition；
Then B is put into 80 DEG C of heating about 4h in micro-wave oven, continues to evaporate wherein most aqueous solvent, obtain gluey transparent presoma
C；Presoma C is put into 200 DEG C of heat preservation 2h in an oven, removes residual solvent water, and lose five crystallizations water；The white that will be obtained
Precursor Powder D is made in foam grinding；Precursor Powder D is packed into alumina crucible, 800 DEG C of temperature lower calcinations in Muffle furnace
3h obtains nanometer Zinc oxide powder photochemical catalyst after furnace cooling.
Embodiment 3：
Weigh 1.50g ZnSO4·7H2O is dissolved in the deionized water of 20ML, and stirring at room temperature forms colourless transparent solution
A；Then solution A is placed on about 3h in 80 DEG C of water-baths, evaporation aqueous solvent obtains mixture B to solution/colloid critical condition；
Then B is put into 80 DEG C of heating about 4h in micro-wave oven, continues to evaporate wherein most aqueous solvent, obtain gluey transparent presoma
C；Presoma C is put into 150 DEG C of heat preservation 2h in an oven, removes residual solvent water, and lose five crystallizations water；The white that will be obtained
Precursor Powder D is made in foam grinding；Precursor Powder D is packed into alumina crucible, 850 DEG C of temperature lower calcinations in Muffle furnace
3h obtains nanometer Zinc oxide powder photochemical catalyst after furnace cooling.
Embodiment 4：
Weigh 1.50g ZnSO4·7H2O is dissolved in the deionized water of 20ML, and stirring at room temperature forms colourless transparent solution
A；Then solution A is placed on about 3h in 80 DEG C of water-baths, evaporation aqueous solvent obtains mixture B to solution/colloid critical condition；
Then B is put into 80 DEG C of heating about 4h in micro-wave oven, continues to evaporate wherein most aqueous solvent, obtain gluey transparent presoma
C；Presoma C is put into 200 DEG C of heat preservation 2h in an oven, removes residual solvent water, and lose five crystallizations water；The white that will be obtained
Precursor Powder D is made in foam grinding；Precursor Powder D is packed into alumina crucible, 950 DEG C of temperature lower calcinations in Muffle furnace
3h obtains nanometer Zinc oxide powder photochemical catalyst after furnace cooling.
Embodiment 5：
Weigh 1.50g ZnSO4·7H2O is dissolved in the deionized water of 20ML, and stirring at room temperature forms colourless transparent solution
A；Then solution A is placed on about 3h in 80 DEG C of water-baths, evaporation aqueous solvent obtains mixture B to solution/colloid critical condition；
Then B is put into 80 DEG C of heating about 4h in micro-wave oven, continues to evaporate wherein most aqueous solvent, obtain gluey transparent presoma
C；Presoma C is put into 200 DEG C of heat preservation 2h in an oven, removes residual solvent water, and lose five crystallizations water；The white that will be obtained
Precursor Powder D is made in foam grinding；Precursor Powder D is packed into alumina crucible, is forged at a temperature of 1000 DEG C in Muffle furnace
3h is burnt, nanometer Zinc oxide powder photochemical catalyst is obtained after furnace cooling.
Embodiment described above is only that the preferred embodiment of the present invention is described, and is not carried out to the scope of the present invention
It limits, under the premise of not departing from design spirit of the present invention, those of ordinary skill in the art make technical scheme of the present invention
Various modifications and improvement, should all fall into claims of the present invention determination protection domain in.
Claims (5)
1. a kind of nanometer Zinc oxide powder photochemical catalyst, molecular formula ZnO, which is characterized in that its with zincblende lattce structure, and
Granularity is the spheric granules of 5~20nm, is prepared using the following method：
1. the configuration of solution
By dissolution of raw material in deionized water, the solution A of a concentration of 0.2-0.5M is obtained；Wherein raw material is the sulfuric acid of soluble Zn
Salt；
2. evaporation and drying
The method for first using heating water bath is evaporated the solvent in the solution A at 80 DEG C to solution/colloid critical condition, is obtained
Mixture B；Then it uses the method for microwave heating to continue to evaporate the solvent in the mixture B at 80 DEG C, continues 4 hours, obtain
To gluey transparent presoma C；The presoma C is heat-treated to 1~5h under conditions of 150~300 DEG C again, removes residual solvent
Water, and 5 crystallizations water are lost, obtain solid product；The solid product is ground, Precursor Powder D is made；
3. being heat-treated
The Precursor Powder D is calcined into 1~5h at 800~1000 DEG C, nanometer Zinc oxide powder photocatalysis is obtained after natural cooling
Agent.
2. nanometer Zinc oxide powder photochemical catalyst according to claim 1, which is characterized in that step 2. described in presoma
C heat treatment conditions are 200 DEG C of heat preservation 2h.
3. nanometer Zinc oxide powder photochemical catalyst according to claim 1, which is characterized in that step 3. described in front axle shell
The calcination condition of last D is 900 DEG C of heat preservation 3h.
4. nanometer Zinc oxide powder photochemical catalyst according to claim 1, which is characterized in that the raw material is soluble
Zinc sulfate.
5. nanometer Zinc oxide powder photochemical catalyst according to claim 1, which is characterized in that the solution A it is a concentration of
0.26M。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610191351.4A CN105749898B (en) | 2016-03-30 | 2016-03-30 | A kind of nanometer Zinc oxide powder photochemical catalyst and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610191351.4A CN105749898B (en) | 2016-03-30 | 2016-03-30 | A kind of nanometer Zinc oxide powder photochemical catalyst and preparation method thereof |
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| "碱式硫酸锌转化法制备ZnO多孔片及其光致发光性能";何朋等;《物理化学学报》;20131230;第29卷(第4期);第874页-880页 * |
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