CN114558561B - Preparation method and application of zinc titanate oxygen-containing defect photocatalyst - Google Patents
Preparation method and application of zinc titanate oxygen-containing defect photocatalyst Download PDFInfo
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- CN114558561B CN114558561B CN202210253453.XA CN202210253453A CN114558561B CN 114558561 B CN114558561 B CN 114558561B CN 202210253453 A CN202210253453 A CN 202210253453A CN 114558561 B CN114558561 B CN 114558561B
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000001301 oxygen Substances 0.000 title claims abstract description 44
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 44
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 42
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000011701 zinc Substances 0.000 title claims abstract description 37
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 35
- 230000007547 defect Effects 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 230000015556 catabolic process Effects 0.000 claims description 6
- 230000003197 catalytic effect Effects 0.000 claims description 6
- 238000006731 degradation reaction Methods 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000003344 environmental pollutant Substances 0.000 claims description 4
- 231100000719 pollutant Toxicity 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 4
- 150000003609 titanium compounds Chemical class 0.000 abstract description 4
- 150000003751 zinc Chemical class 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000011261 inert gas Substances 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 230000000593 degrading effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 230000002950 deficient Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The application belongs to the technical field of photocatalytic materials, and particularly discloses a preparation method and application of a zinc titanate oxygen-containing defect photocatalyst. Adding zinc salt into absolute ethyl alcohol, magnetically stirring, adding weak acid, then adding organic titanium compound into the solution, and stirring the obtained solution for 30 minutes; and (3) drying overnight, calcining at high temperature in an inert gas environment, and naturally cooling to obtain the zinc titanate oxygen-containing defect photocatalyst. The zinc titanate material prepared by the method can activate lattice oxygen to participate in catalytic reaction, and can adsorb and degrade organic pollutants, so that the photocatalytic activity is improved.
Description
Technical Field
The application belongs to the technical field of photocatalytic materials, and particularly relates to a zinc titanate photocatalyst with oxygen-containing defects, and a preparation method and application thereof.
Background
In recent years, environmental pollution problems have become one of the major global concerns, with gaseous pollution being always considered one of the most serious environmental problems threatening human survival. Among the many environmental purification methods, various environmental catalytic technologies such as photocatalysis and electrocatalysis have been attracting attention. The photocatalysis technology is an environment-friendly technology, realizes degradation of gaseous pollutants by utilizing sunlight, and has the characteristics of no secondary pollution, recycling and the like.
Zinc titanate (Zn) 2 TiO 4 ) The spinel type soft magnetic material has a spinel type crystal structure, is a soft magnetic material with excellent performance, has the outstanding advantages of extremely high resistivity and good magnetic spectrum characteristics, and is extremely suitable for being applied to high frequency and ultrahigh frequency. These characteristics determine the recyclability of the material, and in the aspect of catalysis, the prepared zinc titanate nano particles have the remarkable characteristics of fine and uniform particle size. And the narrow bandgap semiconductor can absorb most of visible light in sunlight. Related theoretical calculations and experiments also confirm that oxygen vacancies may be the surface reactive sites of the material. Thus, the introduction of oxygen vacancies will affect the physicochemical properties of the material, including the electronic structure of the systemThe geometry, the material absorption properties, the surface adsorption properties, etc. Oxygen defects may also increase catalytic activity. The introduction of oxygen vacancies can also affect the light absorption and surface adsorption properties of the material, and generally, the metal atoms of the metal oxide have the characteristic of coordination saturation, and oxygen molecules cannot be activated by chemisorption. The construction of oxygen vacancy defects overcomes the defects and promotes efficient transfer of photogenerated electrons from the oxide catalyst to the oxygen molecules.
Disclosure of Invention
The application aims to provide a zinc titanate oxygen-containing defect photocatalyst and a preparation method thereof, and the method is simple, convenient, low in cost, mild in condition and beneficial to mass production.
In order to achieve the above purpose, the application adopts the following technical scheme: the preparation method of the zinc titanate oxygen-containing defect photocatalyst comprises the following steps:
1) Adding zinc salt into absolute ethyl alcohol, magnetically stirring for 30 minutes, dropwise adding acid, stirring for 30 minutes again, dropwise adding an organic titanium compound, and drying overnight to obtain a precursor;
2) Grinding the precursor, calcining at high temperature in an inert gas environment, and naturally cooling to obtain the zinc titanate oxygen-containing defect photocatalyst.
Preferably, in the preparation method of the zinc titanate oxygen-containing defect photocatalyst in step 1), the zinc salt is zinc nitrate hexahydrate.
Preferably, in the preparation method of the zinc titanate oxygen-containing defect photocatalyst in step 1), the acid is glacial acetic acid.
Preferably, in the preparation method of the zinc titanate oxygen-containing defect photocatalyst in step 1), the organic titanium compound is tetra-n-butyl titanate.
Preferably, in the preparation method of the zinc titanate oxygen-containing defect photocatalyst in the step 1), zinc atoms are titanium atoms=1:1 according to the mole ratio.
Preferably, in the preparation method of the zinc titanate oxygen-containing defect photocatalyst in the step 2), the high-temperature calcination is carried out at a calcination temperature of 450-650 ℃ for 2 hours.
Preferably, in the preparation method of the zinc titanate oxygen-containing defect photocatalyst in step 2), the inert gas is nitrogen.
The zinc titanate oxygen-containing defect photocatalyst provided by the application is applied to low-temperature catalytic degradation of gas pollutants.
Preferably, the gaseous contaminant is isopropanol.
Preferably, the method is as follows: and (3) adding a zinc titanate oxygen-containing defect photocatalyst into a sealed reaction container, adding isopropanol, and carrying out catalytic degradation under a xenon lamp.
The beneficial effects of the application are as follows: the zinc titanate catalyst is prepared by zinc salt and organic titanium compound, a large number of oxygen defect structures are constructed, and oxygen defects can activate lattice oxygen and adsorb organic pollutants, so that the photocatalytic activity is improved. The preparation method provided by the application has the advantages of low raw materials, simplicity in operation, great reduction in cost, no pollution to the environment, realization of green chemistry and effective degradation of gas pollutants.
Drawings
FIG. 1 is an XRD pattern of zinc titanate oxygen-deficient photocatalysts prepared in examples 1-4 of the present application.
FIG. 2 is a graph showing the comparison of the activities of zinc titanate oxygen-containing defect photocatalysts prepared in examples 1-4 of the present application for degrading isopropanol gas.
Detailed Description
EXAMPLE 1 Zinc titanate oxygen-containing Defect photocatalyst
The preparation method comprises the following steps:
1) 0.874g of zinc nitrate hexahydrate is dissolved in 10ml of absolute ethyl alcohol, after magnetic stirring for 30 minutes, 2ml of glacial acetic acid is dropwise added, stirring is carried out at room temperature for 30 minutes, 1ml of tetra-n-butyl titanate is dropwise added slowly, stirring is carried out for 30 minutes, the obtained mixed solution is aged for 24 hours, and drying is carried out at 80 ℃ overnight, thus obtaining the precursor.
2) Grinding the precursor, calcining for 2 hours at 450 ℃ in a nitrogen environment, heating at a rate of 5 ℃/min, and naturally cooling to obtain the zinc titanate oxygen-containing defect photocatalyst, wherein the photocatalyst is marked as OVs-ZTO-450.
EXAMPLE 2 Zinc titanate oxygen-deficient photocatalyst
The preparation method comprises the following steps:
1) 0.874g of zinc nitrate hexahydrate is dissolved in 10ml of absolute ethyl alcohol, after magnetic stirring for 30 minutes, 2ml of glacial acetic acid is dropwise added, stirring is carried out at room temperature for 30 minutes, 1ml of tetra-n-butyl titanate is dropwise added slowly, stirring is carried out for 30 minutes, the obtained mixed solution is aged for 24 hours, and drying is carried out at 80 ℃ overnight, thus obtaining the precursor.
2) Grinding the precursor, calcining at 550 ℃ for 2 hours in a nitrogen environment, heating at a rate of 5 ℃/min, and naturally cooling to obtain the zinc titanate oxygen-containing defect photocatalyst, which is marked as OVs-ZTO-550.
EXAMPLE 3 Zinc titanate oxygen-containing Defect photocatalyst
The preparation method comprises the following steps:
1) 0.874g of zinc nitrate hexahydrate is dissolved in 10ml of absolute ethyl alcohol, after magnetic stirring for 30 minutes, 2ml of glacial acetic acid is dropwise added, stirring is carried out at room temperature for 30 minutes, 1ml of tetra-n-butyl titanate is dropwise added slowly, stirring is carried out for 30 minutes, the obtained mixed solution is aged for 24 hours, and drying is carried out at 80 ℃ overnight, thus obtaining the precursor.
2) Grinding the precursor, calcining for 2 hours at 650 ℃ in a nitrogen environment, heating at a rate of 5 ℃/min, and naturally cooling to obtain the zinc titanate oxygen-containing defect photocatalyst, which is marked as OVs-ZTO-650.
EXAMPLE 4 Zinc titanate oxygen-defective photocatalyst
The preparation method comprises the following steps:
1) 0.874g of zinc nitrate hexahydrate is dissolved in 10ml of absolute ethyl alcohol, after magnetic stirring for 30 minutes, 2ml of glacial acetic acid is dropwise added, stirring is carried out at room temperature for 30 minutes, 1ml of tetra-n-butyl titanate is dropwise added slowly, stirring is carried out for 30 minutes, the obtained mixed solution is aged for 24 hours, and drying is carried out at 80 ℃ overnight, thus obtaining the precursor.
2) Grinding the precursor, calcining at 550 ℃ for 2 hours in an air environment, heating at a rate of 5 ℃/min, and naturally cooling to obtain the zinc titanate oxygen-containing defect photocatalyst, which is marked as ZTO-550.
FIG. 1 is an XRD test pattern of the zinc titanate oxygen-deficient photocatalyst prepared in examples 1-4. As can be seen from FIG. 1, comparing it with a standard card, it is demonstrated that Zn was successfully synthesized 2 TiO 4 A material.
Example 5 application
The photocatalysts prepared in examples 1 to 4 were placed at 4cm, respectively 2 In the glass tank, the glass tank loaded with the photocatalyst is respectively placed in a 224ml reactor containing air with atmospheric pressure, finally 5ul isopropanol liquid is injected into the reactor, the reactor is heated by illumination through a 300W xenon lamp, timing is started after 10min, and a needle is extracted every 20 min from a sample for testing. The acetone produced was subjected to gas chromatography using a FID detector (GC 1690, shortcut technologies). After the reaction was completed, the reactor was cooled to room temperature and the catalyst was collected for further characterization.
Fig. 2 is a graph showing that the activities of the photocatalysts prepared in examples 1-4 for degrading isopropanol gas are compared, and it is obvious that the photocatalysts prepared in example 2 have the highest photocatalytic activity, which is about 2.16 times the isopropanol degrading rate of the photocatalysts OVs-ZTO-450 prepared in example 1, the photocatalysts OVs-ZTO-550 prepared in example 2 are about 3.39 times the isopropanol degrading rate of the photocatalysts OVs-ZTO-650 prepared in example 3, and the photocatalysts OVs-ZTO-550 prepared in example 2 are about 3.6 times the isopropanol degrading rate of the photocatalysts ZTO-550 prepared in example 4, because the photocatalysts prepared in the application contain a large amount of oxygen defects, the oxygen defects not only can activate lattice oxygen and participate in catalytic reaction, but also can adsorb degraded organic matters, thereby improving the photocatalytic activity.
Claims (2)
1. The application of the zinc titanate oxygen-containing defect photocatalyst in low-temperature catalytic degradation of gas pollutants is characterized by comprising the following steps: adding zinc titanate oxygen-containing defect photocatalyst into a sealed reaction container, adding isopropanol, and carrying out catalytic degradation under a xenon lamp; the preparation method of the zinc titanate oxygen-containing defect photocatalyst comprises the following steps:
1) Adding zinc nitrate hexahydrate into absolute ethyl alcohol, magnetically stirring for 30 minutes, dropwise adding glacial acetic acid, stirring for 30 minutes again, dropwise adding tetra-n-butyl titanate, and drying overnight to obtain a precursor;
2) Grinding the precursor, calcining at 550 ℃ for 2 hours in a nitrogen environment, and naturally cooling to obtain the zinc titanate oxygen-containing defect photocatalyst.
2. The use according to claim 1, wherein in step 1), the molar ratio of zinc atoms to titanium atoms=1:1.
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| CN114558561B true CN114558561B (en) | 2023-12-08 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108786780A (en) * | 2018-06-03 | 2018-11-13 | 常州德维勒新材料科技有限公司 | A kind of nano combined Zn2TiO4The preparation method of functional material and its dispersion liquid |
| CN111468096A (en) * | 2020-04-09 | 2020-07-31 | 浙江工业大学 | Zn2TiO4/TiO2Composite material and preparation method and application thereof |
| CN112958093A (en) * | 2021-02-05 | 2021-06-15 | 辽宁大学 | Cobalt ferrite photocatalyst with oxygen-containing defect and preparation method and application thereof |
| CN114042471A (en) * | 2021-12-03 | 2022-02-15 | 辽宁大学 | Visible light response type Zn2TiO4/g-C3N4Heterojunction material and application thereof |
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- 2022-03-15 CN CN202210253453.XA patent/CN114558561B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108786780A (en) * | 2018-06-03 | 2018-11-13 | 常州德维勒新材料科技有限公司 | A kind of nano combined Zn2TiO4The preparation method of functional material and its dispersion liquid |
| CN111468096A (en) * | 2020-04-09 | 2020-07-31 | 浙江工业大学 | Zn2TiO4/TiO2Composite material and preparation method and application thereof |
| CN112958093A (en) * | 2021-02-05 | 2021-06-15 | 辽宁大学 | Cobalt ferrite photocatalyst with oxygen-containing defect and preparation method and application thereof |
| CN114042471A (en) * | 2021-12-03 | 2022-02-15 | 辽宁大学 | Visible light response type Zn2TiO4/g-C3N4Heterojunction material and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| Alima Mebrek et al..Preparation and characterization of spinel type Zn2TiO4 nanocomposite.《Ceramics International》.2018,第44卷10921-10928. * |
| 万利远等.Zn2TiO4纳米线的合成及其应用于丙酮的光催化降解.《第六届全国环境催化与环境材料学术会议论文集》.2009,第38页. * |
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