CN106362722A - Method for preparing photocatalyst - Google Patents
Method for preparing photocatalyst Download PDFInfo
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- CN106362722A CN106362722A CN201610777314.1A CN201610777314A CN106362722A CN 106362722 A CN106362722 A CN 106362722A CN 201610777314 A CN201610777314 A CN 201610777314A CN 106362722 A CN106362722 A CN 106362722A
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- zno
- tio
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- vacuum drying
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title abstract description 3
- 238000001291 vacuum drying Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 5
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims description 7
- 238000002372 labelling Methods 0.000 claims description 7
- 238000010791 quenching Methods 0.000 claims description 7
- 230000000171 quenching effect Effects 0.000 claims description 7
- 238000012546 transfer Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000002242 deionisation method Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 5
- 238000011160 research Methods 0.000 abstract description 3
- 239000004408 titanium dioxide Substances 0.000 abstract description 2
- 229960004011 methenamine Drugs 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000002135 nanosheet Substances 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 238000000967 suction filtration Methods 0.000 abstract 1
- 238000006555 catalytic reaction Methods 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 6
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000005977 Ethylene Substances 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 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 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008450 motivation Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 230000001235 sensitizing effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention provides a method for preparing a photocatalyst. Weighed Zn(SO)2.6H2O and hexamethylene tetramine are dissolved in a 100 mL beaker containing magnets, deionized water is added, then the mixture is placed in oil bath at 90 DEG C to react for 8 h, then cooled to room temperature and subjected to suction filtration in a vacuum drying box at 60 DEG C to be dried for 24 h, and ZnO nanosheets are obtained. ZnO and TiO2 with a close band gap (Eg=3.37 eV) are used, and compared with TiO2, ZnO has a direct band gap and high electron mobility. Researches show that when ZnO degrades organic pollutants, the photocatalytic effect is better than that of TiO2, titanium dioxide grows on ZnO by preparing a heterojunction, and accordingly the sizes of two substances in the formed heterojunction happen to be a proper size.
Description
Technical field
The present invention relates to a kind of catalyst, more particularly, to a kind of preparation method of photocatalyst.
Background technology
Photocatalyst, as a kind of green catalyst, achieves huge progress in recent years.Promote light-catalyzed reaction research
Enormous motivation derives from the strong request of clean manufacturing energy crisis environmental conservation, and the potential exploration of photocatalyst itself
It is worth and application potential.Photocatalyst of zinc oxide can be exhibited one's skill to the full in environmental conservation, and its powerful catalytic degradation ability can
To allow overwhelming majority pollution turn materially innocuous substance, it is that water conservation contributes, country and enterprise row can be solved in the lump
Put the problem of sewage.Using zno, noxious substance cn- is degraded to innocuous substance co2, n2, no3-.Because light-catalyzed reaction meets
Low energy consumption, the environmentally friendly favor having obtained numerous scholars, in the last few years, scientist deeply grinds to light-catalyzed reaction
Study carefully, achieved with encouraging success, thus light-catalyzed reaction has become as an important method of catalytic reaction.
Surface sensitization is that photolytic activity sensitizer is adsorbed in zno surface, and under illumination, sensitizing molecules absorb photon and are produced from
By electronics, free electron transfers to zno surface, and the valence band of photosensitizer is then transferred in the hole producing after zno is excited simultaneously, makes
Its absorption spectrum moves to visible light direction, thus extending the scope of zno absorbing wavelength, improves visible light photocatalysis efficiency.Half
Conductor be combined be using two kinds of quasiconductor components between conduction band and valence band difference, so that photo-generated carrier is sufficiently separated, and extend multiple
The spectral response range of fit system, reaches the purpose of lifting photocatalysis efficiency.
By having consulted substantial amounts of scientific literature, to zno/tio2Photocatalyst photocatalyst has carried out deep discussion.
Also ratio is larger for the impact of nanoparticle size, and activity can change with the change of granular size.When this hetero-junctions is subject to more than it
After the photon irradiation of forbidden band wide band energy, produce photohole and light induced electron on its surface, light induced electron is given birth to oxygen reaction
Become superoxipe ion o2−, a lot of difficult Organic substances decomposing can be resolved into co2, h2The inorganic matters such as o.Preferably special based on these
Property, we only need to find a kind of preferable preparation method and preferably be combined zinc oxide and titanium dioxide, and we are with regard to permissible
Produce the photocatalyst of function admirable..
Content of the invention
It is an object of the invention to provide a kind of preparation method of photocatalyst, the present invention is using the preparation of high temperature hydro-thermal method
zno/tio2Photocatalyst, and the preparation scheme of this photocatalyst is improved.Carry out after being successfully prepared, to zno/tio2Light
Catalyst carries out the test of catalytic performance, using this catalyst degradating organic dye, measures its catalytic efficiency size, and
Allow it to be compared with other photocatalysts, its photocatalysis efficiency is evaluated and tested, find deficiency therein, then it is carried out
Modification or improvement preparation method, by multiple comparison, prepare the catalyst of more excellent performance so as to possess higher catalysis
Performance.
The present invention is realized by following steps:
1st, the preparation of zno nanometer sheet:
By the zn(so weighing4)2·6h2O and hexamethylenetetramine are dissolved in the 100 ml beakers being placed with Magnetitum, add deionization
Water, wherein zn(so4)2·6h2The mol ratio of o, hexamethylenetetramine and deionized water is 1:1-1.1:1, puts into 90 DEG C afterwards
Oil bath pan reacts 8 h, is cooled to room temperature, and sucking filtration is dried 24 h in 60 DEG C of vacuum drying oven, obtains zno nanometer sheet;
2、zno/tio2Preparation:
Take a beaker all to add isopropanol in beaker, add above-mentioned obtain zno, beaker is placed in ultrasonic machine, ultrasonic molten
Solution, after the completion of dissolving, then Deca metatitanic acid second butyl ester (tip) and diethylenetriamine (deta) continue ultrasonic dissolution 40 min respectively,
Transfer to 50 ml autoclaves, be then placed in 200 DEG C of baking ovens, heat 24 h, after having reacted cooling, pour the big examination of centrifugation into
Carry out labelling in pipe, and be centrifuged, in respectively deionized water and washing with alcohol three times, be centrifuged 8000 r/min, obtain product and put
Enter 60 DEG C of vacuum drying, vacuum drying time 24 h in vacuum drying oven, final product puts into Muffle furnace 400 DEG C/2 h, speed
The general 1 DEG C/min of rate carries out Quenching Treatment of annealing, thus preparing zno:tio2Mass percent is the zno/tio of 20%-80%2Urge
Agent.
The solution have the advantages that: the present invention utilizes zno and tio2There is close energy gap (eg=3.37 ev),
With tio2Compare, zno has direct band gap, high electron mobility, research shows, zno, in the organic pollution of degraded, has
Compare tio2Preferably photocatalysis effect, the preparation of hetero-junctions allows titania growth so that the hetero-junctions being formed on zno
In two kinds of matter dimensions reach a kind of size being just suitable for, by sem collection of illustrative plates can be seen that 40 % proportioning groups are formed different
Matter is tied, and form is good, and hetero-junctions surface is uniformly regular.The bright 40 % proportioning groups of chart of degraded methyl orange have fabulous for methyl orange
Photocatalysis effect.
Brief description
Fig. 1 is the result test chart of the zno product sem of case study on implementation 1 preparation.
Fig. 2 is 40 %zno/tio of case study on implementation 3 preparation2The result test chart of product sem.
Fig. 3 is the tio of case study on implementation 6 preparation2The result test chart of product sem.
Fig. 4 prepares the result test chart of product degraded methyl orange for case study on implementation 1-6.
Specific embodiment
To describe the present invention in detail below in conjunction with embodiment 1-5 to be had the advantage that it is intended to help reader more
Understand well the essence of the present invention, but any restriction can not be constituted to the enforcement of the present invention and protection domain.
Case study on implementation 1:
Weigh 5.3548 g zn(so4)2·6h2O and 2.5234 g hexamethylenetetramines.Alleged acquirement medicine is dissolved in 100 ml
In beaker, inside there are 60 ml deionized waters.Add Magnetitum, put into 90 DEG C of oil bath pans and react 8 h.It is cooled to room temperature, sucking filtration is 60
DEG C vacuum drying oven in be dried 24 h.
Case study on implementation 2:
Take a beaker to add 55 ml isopropanols in beaker, add the zno that 0.5 gzno(is prepared by case study on implementation 1), will
Beaker is placed in ultrasonic machine, ultrasonic dissolution, after the completion of dissolving, then Deca 0.18 ml metatitanic acid second butyl ester (tip) and 0.03 ml bis-
Ethylene triamine (deta) continues ultrasonic 40 min, transfers to 50 ml autoclaves, is then placed in 200 DEG C of baking ovens, heating
24 h.After having reacted cooling, pour in centrifugation Boiling tube and carry out labelling, and be centrifuged, in deionized water and washing with alcohol respectively
Three times, it is centrifuged 8000 r/min.Obtain product and put into 60 DEG C of vacuum drying, 24 h in vacuum drying oven.Final product puts into horse
Not stove 400 DEG C/2 h, the general 1 DEG C/min of speed carry out Quenching Treatment of annealing.Prepare tio2Doping content is 20 %zno/
tio2Catalyst.
Case study on implementation 3:
Take a beaker to add 55 ml isopropanols in beaker, add the zno that 0.5 gzno(is prepared by case study on implementation 1), will
Beaker is placed in ultrasonic machine, ultrasonic dissolution, after the completion of dissolving, then Deca 0.36 ml metatitanic acid second butyl ester (tip) and 0.06 ml bis-
Ethylene triamine (deta) continues ultrasonic 40 min, transfers to 50 ml autoclaves, is then placed in 200 DEG C of baking ovens, heating
24 h.After having reacted cooling, pour in centrifugation Boiling tube and carry out labelling, and be centrifuged, in deionized water and washing with alcohol respectively
Three times, it is centrifuged 8000 r/min.Obtain product and put into 60 DEG C of vacuum drying, 24 h in vacuum drying oven.Final product puts into horse
Not stove 400 DEG C/2 h, the general 1 DEG C/min of speed carry out Quenching Treatment of annealing.Prepare tio2Doping content is 40 %zno/
tio2Catalyst.
Case study on implementation 4:
Take a beaker to add 55 ml isopropanols in beaker, add the zno that 0.5 gzno(is prepared by case study on implementation 1), will
Beaker is placed in ultrasonic machine, ultrasonic dissolution, after the completion of dissolving, then Deca 0.72 ml metatitanic acid second butyl ester (tip) and 0.12 ml bis-
Ethylene triamine (deta) continues ultrasonic 40 min, transfers to 50 ml autoclaves, is then placed in 200 DEG C of baking ovens, heating
24 h.After having reacted cooling, pour in centrifugation Boiling tube and carry out labelling, and be centrifuged, in deionized water and washing with alcohol respectively
Three times, it is centrifuged 8000 r/min.Obtain product and put into 60 DEG C of vacuum drying, 24 h in vacuum drying oven.Final product puts into horse
Not stove 400 DEG C/2 h, the general 1 DEG C/min of speed carry out Quenching Treatment of annealing.Prepare tio2Doping content is 60 %zno/
tio2Catalyst.
Case study on implementation 5:
Take a beaker to add 55 ml isopropanols in beaker, add the zno that 0.5 gzno(is prepared by case study on implementation 1), will
Beaker is placed in ultrasonic machine, ultrasonic dissolution, after the completion of dissolving, then Deca 1.44 ml metatitanic acid second butyl ester (tip) and 0.24 ml bis-
Ethylene triamine (deta) continues ultrasonic 40 min, transfers to 50 ml autoclaves, is then placed in 200 DEG C of baking ovens, heating
24 h.After having reacted cooling, pour in centrifugation Boiling tube and carry out labelling, and be centrifuged, in deionized water and washing with alcohol respectively
Three times, it is centrifuged 8000 r/min.Obtain product and put into 60 DEG C of vacuum drying, 24 h in vacuum drying oven.Final product puts into horse
Not stove 400 DEG C/2 h, the general 1 DEG C/min of speed carry out Quenching Treatment of annealing.Prepare tio2Doping content is 80 %zno/
tio2Catalyst.
Case study on implementation 6:
A beaker is taken to add 55 ml isopropanols, Deca 3 ml metatitanic acid second butyl ester (tip) and 0.5 ml diethylenetriamine in beaker
(deta) ultrasonic 40 min, transfer to 50 ml autoclaves, are then placed in 200 DEG C of baking ovens, heat 24 h.React cold
But after, pour in centrifugation Boiling tube and carry out labelling, and be centrifuged, in deionized water respectively and washing with alcohol three times, be centrifuged 8000
r/min.Obtain product and put into 60 DEG C of vacuum drying, 24 h in vacuum drying oven.Final product puts into Muffle furnace 400 DEG C/2
H, the general 1 DEG C/min of speed carry out Quenching Treatment of annealing.Prepare pure tio2Catalyst.
Embodiment described above is only that the preferred embodiment of the present invention is described, the not model to the present invention
Enclose and be defined, on the premise of without departing from design spirit of the present invention, the technical side to the present invention for the those of ordinary skill in the art
Various modifications and improvement that case is made, all should fall in the protection domain of claims of the present invention determination.
Claims (1)
1. a kind of preparation method of photocatalyst, the preparation of (1) zno nanometer sheet: by the zn(so weighing4)2·6h2O and six first
Urotropine is dissolved in the 100 ml beakers being placed with Magnetitum, adds deionized water, wherein zn(so4)2·6h2O, hexamethylenetetramine
It is 1:1-1.1:1 with the mol ratio of deionized water, puts into 90 DEG C of oil bath pans afterwards and react 8 h, be cooled to room temperature, sucking filtration is 60
DEG C vacuum drying oven in be dried 24 h, obtain zno nanometer sheet;(2) zno/tio2Preparation: take a beaker in beaker all plus
Enter isopropanol, add zno, beaker is placed in ultrasonic machine, ultrasonic dissolution, after the completion of dissolving, then Deca metatitanic acid second fourth respectively
Ester (tip) continues ultrasonic dissolution 40 min with diethylenetriamine (deta), transfers to 50 ml autoclaves, is then placed in 200
In DEG C baking oven, heat 24 h, after react cooling, pour into be centrifuged in Boiling tube and carry out labelling, and be centrifuged, using deionization respectively
Water and washing with alcohol three times, are centrifuged 8000 r/min, obtain product and put into 60 DEG C of vacuum drying in vacuum drying oven, vacuum is done
Dry time 24 h, final product puts into Muffle furnace 400 DEG C/2 h, and the general 1 DEG C/min of speed carries out Quenching Treatment of annealing, thus
Preparation zno:tio2Mass percent is the zno/tio of 20%-80%2Catalyst.
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CN106111107A (en) * | 2016-06-27 | 2016-11-16 | 南昌航空大学 | A kind of Zinc oxide nano sheet catalyst of titania additive |
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Application publication date: 20170201 |