CN106861678A - It is a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation method of catalysis material - Google Patents
It is a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation method of catalysis material Download PDFInfo
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- CN106861678A CN106861678A CN201611196884.8A CN201611196884A CN106861678A CN 106861678 A CN106861678 A CN 106861678A CN 201611196884 A CN201611196884 A CN 201611196884A CN 106861678 A CN106861678 A CN 106861678A
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- ammonium molybdate
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- 239000000463 material Substances 0.000 title claims abstract description 20
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000004094 surface-active agent Substances 0.000 title claims abstract description 11
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 claims abstract description 16
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 claims abstract description 16
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 29
- 239000011259 mixed solution Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical compound O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 229910002900 Bi2MoO6 Inorganic materials 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 abstract description 4
- 239000004202 carbamide Substances 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 4
- 229940043267 rhodamine b Drugs 0.000 abstract description 4
- 238000001338 self-assembly Methods 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 11
- 238000001035 drying Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- -1 Ammonium Molybdate Tetrahydrates Chemical class 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 3
- 235000018660 ammonium molybdate Nutrition 0.000 description 3
- 229940010552 ammonium molybdate Drugs 0.000 description 3
- 239000011609 ammonium molybdate Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 241001198704 Aurivillius Species 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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—
-
- B01J35/39—
-
- 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
- C02F2101/38—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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation method of catalysis material, the present invention prepares urea catalysis material as primary raw material with five nitric hydrate bismuths, Ammonium Molybdate Tetrahydrate, urea, concentrated nitric acid, sodium acid carbonate using the method that water-bath flows back.And the test of photocatalysis performance is carried out to the material prepared using simulated solar irradiation, the superior photocatalysis performance of the material is proved by degradation biological persistent organic pollutants rhodamine B.The method does not have any surfactant and template material of addition in preparation process, and preparation process is simply novel.The composite belongs to inorganic catalysis material, flower-shaped Bi2MoO6It is by a large amount of super-thin sheet-shaped Bi2MoO6Self assembly is formed, and photocatalytic activity is higher, there is good application prospect in terms of environmental protection.
Description
Technical field
The present invention relates to a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation method of catalysis material,
Belong to optic catalytic composite material preparation field.
Background technology
In recent years, along with the development of China's rough formula of industry, problem of environmental pollution is also increasingly severe, water and air
Pollution has seriously threatened the existence and procreation of the mankind.Contain substantial amounts of toxic organic pollutant in some chemical emissions,
These pollutants can be enriched with the person, and the health to the mankind causes huge injury.In recent years, people always search for solution
The certainly method of environmental pollution, the sight of correlative study person has gradually been placed on sight using this unlimited regenerative resource of solar energy
Photocatalitic Technique of Semiconductor on.Can be by the efficient purifying water body of photocatalysis technology by sunshine.Traditional light
Catalyst TiO2Have the advantages that photocatalytic activity is high, inexpensive nontoxic, anti-light burn into stable chemical nature photocatalysis technology research
Active material.But TiO2Forbidden band energy gap be 3.2 eV, the ultraviolet light of short wavelength can only be absorbed and excited, and ultraviolet
The energy of line only accounts for total 5 percent or so of sunlight, so TiO2Light utilization ratio is relatively low.
Bi2MoO6It is a kind of conductor photocatalysis material with visible light catalysis activity higher, it can be used in waste water
The treatment of organic pollution, can decompose part in air harmful inorganic substances and almost all harmful organic substance
Matter, very important effect is served to purify air environment purification.Bi2MoO6Maximum absorption wavelength is about 491nm, is a kind of
There is the photochemical catalyst of response to visible ray well, it all shows excellent in terms of solar energy conversion and environmental pollution improvement
Different visible light catalysis activity.Bi2MoO6Structure be simplest Aurivillius types oxide, its pattern, size etc. are
The key factor of its chemical property is influenceed, therefore, study Bi2MoO6The controlledly synthesis of pattern and its visible light catalytic performance have
There are most important theories meaning and practical value.
The content of the invention
It is an object of the invention to provide a kind of without surfactant and the flower-shaped Bi of template2MoO6Catalysis material system
Preparation Method, is flowed back as primary raw material with five nitric hydrate bismuths, Ammonium Molybdate Tetrahydrate, urea, concentrated nitric acid, sodium acid carbonate using water-bath
Method prepare urea catalysis material.And the survey of photocatalysis performance is carried out to the material prepared using simulated solar irradiation
Examination, the superior photocatalysis performance of the material is proved by degradation biological persistent organic pollutants rhodamine B.The method is in system
There is no addition any surfactant and template material during standby, preparation process is simply novel.The composite belongs to nothing
Machine catalysis material, flower-shaped Bi2MoO6It is by a large amount of super-thin sheet-shaped Bi2MoO6Self assembly is formed, and photocatalytic activity is higher, in ring
Border protection aspect has good application prospect.
It is a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation method of catalysis material, step is as follows:
Step one:
Two kinds of solids of five nitric hydrate bismuths and Ammonium Molybdate Tetrahydrate are weighed, the nitric acid that 15ml concentration is 2mol/L is dissolved in respectively molten
In liquid, stirring makes it form five nitric hydrate bismuth solution and Ammonium Molybdate Tetrahydrate solution respectively;
Step 2:
Ammonium Molybdate Tetrahydrate solution is added drop-wise in five nitric hydrate bismuth solution, ultrasound 10min again after stirring 30min is mixed
Close solution;
Step 3:
Sodium bicarbonate powder is added in the mixed solution obtained in step 2, and mixed solution is continued to monitor with pH meter
PH, between the pH of mixed solution reaches 6-7;
Step 4:
The mixed solution that pH will be mixed up is transferred in round-bottomed flask, is centrifuged after the 18h that flowed back at 80 DEG C and is precipitated;
Step 5:
The precipitation deionized water and ethanol of acquisition are washed twice respectively, the product that will have been washed is put into 60 in vacuum drying chamber
Degree dries 12 hours, obtains final products.
In described step one, the ratio between molal quantity of bismuth element and molybdenum element in five nitric hydrate bismuths and Ammonium Molybdate Tetrahydrate
It is 2:1.
It is an advantage of the invention that:
The present invention relates to a kind of Bi with floriform appearance by super-thin sheet-shaped self assembly2MoO6The preparation of catalysis material
Method, without any surfactant and template in preparation process, it is to avoid the trouble of removal additive, and addition
Agent is possible to the problems such as removing unclean, and reduces synthesis cost.The plain mode that reaction is flowed back using water-bath, is a kind of
Simple and effective synthetic method.50mg this products are in visible ray(λ>420nm)Lower degraded 50ml concentration is the rhodamine B of 10PPm
Solution, degradation rate reaches 45% within 90 minutes.
Brief description of the drawings
Fig. 1 is to weigh the flower-shaped Bi of 50mg2MoO6Product is in visible ray(λ>420nm)Lower degraded 50ml concentration is sieve of 10PPm
The degradation curve of red bright B solution.
Fig. 2 is the SEM scanning electron microscope (SEM) photographs of product.
Specific embodiment
Below by embodiment 1-3, the invention will be further described.
Embodiment 1
Step one:Two kinds of solids of the nitric hydrate bismuths of 1.2121g five and 0.2207g Ammonium Molybdate Tetrahydrates accurately are weighed, is dissolved respectively
In 15ml concentration in the salpeter solution of 2mol/L, stirring forms it into five nitric hydrate bismuth solution and Ammonium Molybdate Tetrahydrate is molten
Liquid;
Step 2:Ammonium Molybdate Tetrahydrate solution is added drop-wise in five nitric hydrate bismuth solution, ultrasound 10min again after stirring 30min,
Obtain mixed solution;
Step 3:Sodium bicarbonate powder is added in the mixed solution obtained in step 2, and mixing is continued to monitor with pH meter
The pH of solution, until the Ph of mixed solution reaches 6.5.
Step 4:The mixed solution that pH will be mixed up is transferred in round-bottomed flask, is centrifuged after the 18h that flowed back at 80 DEG C and obtained
Precipitation.
Step 5:The precipitation deionized water and ethanol of acquisition are washed twice respectively.The product that will have been washed is put into very
12 hours of 60 degree of dryings in empty drying box, obtain final products.
Embodiment 2
Step one:Two kinds of solids of the nitric hydrate bismuths of 1.2121g five and 0.2207g Ammonium Molybdate Tetrahydrates accurately are weighed, is dissolved respectively
In 15ml concentration in the salpeter solution of 2mol/L, stirring forms it into five nitric hydrate bismuth solution and Ammonium Molybdate Tetrahydrate is molten
Liquid;
Step 2:Ammonium Molybdate Tetrahydrate solution is added drop-wise in five nitric hydrate bismuth solution, ultrasound 10min again after stirring 30min,
Obtain mixed solution;
Step 3:Sodium bicarbonate powder is added in the mixed solution obtained in step 2, and mixing is continued to monitor with pH meter
The pH of solution, until the pH of mixed solution reaches 7.
Step 4:The mixed solution that pH will be mixed up is transferred in round-bottomed flask, is centrifuged after the 18h that flowed back at 80 DEG C and obtained
Precipitation.
Step 5:The precipitation deionized water and ethanol of acquisition are washed twice respectively.The product that will have been washed is put into very
12 hours of 60 degree of dryings in empty drying box, obtain final products.
Embodiment 3
Step one:Two kinds of solids of the nitric hydrate bismuths of 1.2121g five and 0.2207g Ammonium Molybdate Tetrahydrates accurately are weighed, is dissolved respectively
In 15ml concentration in the salpeter solution of 2mol/L, stirring forms it into five nitric hydrate bismuth solution and Ammonium Molybdate Tetrahydrate is molten
Liquid;
Step 2:Ammonium Molybdate Tetrahydrate solution is added drop-wise in five nitric hydrate bismuth solution, ultrasound 10min again after stirring 30min,
Obtain mixed solution;
Step 3:Sodium bicarbonate powder is added in the mixed solution obtained in step 2, and mixing is continued to monitor with pH meter
The pH of solution, until the pH of mixed solution reaches 6.7.
Step 4:The mixed solution that pH will be mixed up is transferred in round-bottomed flask, is centrifuged after the 18h that flowed back at 80 DEG C and obtained
Precipitation.
Step 5:The precipitation deionized water and ethanol of acquisition are washed twice respectively.The product that will have been washed is put into very
12 hours of 60 degree of dryings in empty drying box, obtain final products.
By the flower-shaped Bi of final product2MoO650mg is under simulated solar irradiation for the rhodamine B solution of the 50ml 10PPm that degrade
Refer to accompanying drawing 1.
Fig. 2 be embodiment 1-2 obtained by product scanning electron microscope (SEM) photograph, from the figure, it can be seen that with a process for preparing
Flower-shaped Bi2MoO6It is by substantial amounts of super-thin sheet-shaped Bi2MoO6Self assembly is formed.
Claims (2)
1. a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation method of catalysis material, it is characterized by:Step
It is rapid as follows:
Step one:
Two kinds of solids of five nitric hydrate bismuths and Ammonium Molybdate Tetrahydrate are weighed, the nitric acid that 15ml concentration is 2mol/L is dissolved in respectively molten
In liquid, stirring makes it form five nitric hydrate bismuth solution and Ammonium Molybdate Tetrahydrate solution respectively;
Step 2:
Ammonium Molybdate Tetrahydrate solution is added drop-wise in five nitric hydrate bismuth solution, ultrasound 10min again after stirring 30min is mixed
Close solution;
Step 3:
Sodium bicarbonate powder is added in the mixed solution obtained in step 2, and mixed solution is continued to monitor with pH meter
PH, between the pH of mixed solution reaches 6-7;
Step 4:
The mixed solution that pH will be mixed up is transferred in round-bottomed flask, is centrifuged after the 18h that flowed back at 80 DEG C and is precipitated;
Step 5:
The precipitation deionized water and ethanol of acquisition are washed twice respectively, the product that will have been washed is put into 60 in vacuum drying chamber
Degree dries 12 hours, obtains final products.
2. as claimed in claim 1 a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation of catalysis material
Method, it is characterized by:In step one, the ratio between molal quantity of bismuth element and molybdenum element in five nitric hydrate bismuths and Ammonium Molybdate Tetrahydrate
It is 2:1.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101254463A (en) * | 2008-04-11 | 2008-09-03 | 南京大学 | Synthetic method of visible light catalyst Bi2MoO6 |
CN106076429A (en) * | 2016-06-06 | 2016-11-09 | 东华大学 | A kind of textile fabric/Graphene/Bi2moO6/ BiPO4the preparation method of combinational environment catalysis material |
-
2016
- 2016-12-22 CN CN201611196884.8A patent/CN106861678A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101254463A (en) * | 2008-04-11 | 2008-09-03 | 南京大学 | Synthetic method of visible light catalyst Bi2MoO6 |
CN106076429A (en) * | 2016-06-06 | 2016-11-09 | 东华大学 | A kind of textile fabric/Graphene/Bi2moO6/ BiPO4the preparation method of combinational environment catalysis material |
Non-Patent Citations (1)
Title |
---|
XUEMEI HOU, ET AL.: "Preparation and characterization of Fe3O4/SiO2/Bi2MoO6 composite as magnetically separable photocatalyst", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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