CN101966452A - Method for preparing visible light-responded LaVO4 and TiO2 composite nanotube - Google Patents
Method for preparing visible light-responded LaVO4 and TiO2 composite nanotube Download PDFInfo
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- CN101966452A CN101966452A CN 201010531067 CN201010531067A CN101966452A CN 101966452 A CN101966452 A CN 101966452A CN 201010531067 CN201010531067 CN 201010531067 CN 201010531067 A CN201010531067 A CN 201010531067A CN 101966452 A CN101966452 A CN 101966452A
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- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 239000002071 nanotube Substances 0.000 title claims abstract description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract description 10
- 238000000034 method Methods 0.000 title abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 49
- 239000000243 solution Substances 0.000 claims description 33
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 239000002114 nanocomposite Substances 0.000 abstract description 2
- 239000011941 photocatalyst Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 238000003980 solgel method Methods 0.000 abstract description 2
- 229910002339 La(NO3)3 Inorganic materials 0.000 abstract 1
- 229910019501 NaVO3 Inorganic materials 0.000 abstract 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 abstract 1
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 10
- 239000004065 semiconductor Substances 0.000 description 9
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing a visible light-responded LaVO4 and TiO2 nano composite photocatalyst and belongs to the technical field of environmental pollution abatement. The method is characterized by: firstly preparing LaVO4 by performing hydrothermal reaction on La(NO3)3 and NaVO3 under an alkaline condition; secondly, preparing LaVO4/TiO2 composite nano particles by taking tetrabutyl titanate as a titanium resource and ethanol as a solvent by a sol-gel method; and finally, preparing a composite nanotube by performing hydrothermal reaction on the LaVO4/TiO2 composite nano particles under the alkaline condition by a hydrothermal method. The preparation method of the invention has the advantages of stable performances, no other pollutants generated in the preparation process and the like, is convenient to operate and has very high practical value and application prospect.
Description
Technical field
The invention belongs to the environmental pollution treatment technology field, relate to a kind of powder TiO
2The preparation method of nano-composite catalyst specially refers to a kind of employing combination of sol-gel hydrothermal method and prepares powder LaVO
4/ TiO
2The method of composite nano tube.
Background technology
Along with the progress of human society, problem of environmental pollution is more and more serious, and the removal of these environmental contaminants need consume a large amount of energy, and this proposes stern challenge for the exhausted day by day energy.How problem of environmental pollution is effectively controlled and solved to the limited resources of reasonable use occurring in nature, becomes the hot issue of the present world and numerous domestic scholar's research.In recent years, the conductor photocatalysis oxidation technology was as one of high-level oxidation technology, just be subjected to the broad research of Chinese scholars, this technology can effectively be utilized solar energy with solar energy as degrade pollutant in the environment of the energy, reduces people's using energy source.
Find to be subjected to the TiO of light irradiation since Japanese scientist Fujishima and Honda
2The monocrystalline electrode can be with H
2O decomposes, and utilizes TiO
2Semiconductor light-catalyst is converted into the research focus that electric energy and chemical energy just become the conductor photocatalysis field with luminous energy.Recently, utilize TiO
2The research report of aspects such as semiconductor light-catalyst degradable organic pollutant, deodorizing, sterilization, automatically cleaning constantly increases.Yet, Detitanium-ore-type TiO
2Energy gap be 3.2eV, its excitation wavelength is 387.5nm, belongs to the ultraviolet light range in the sunshine.And for solar energy, its main concentration of energy is in the visible-range of 400nm-600nm, and this has significantly reduced TiO
2How therefore the efficient of semiconductor light-catalyst, realize TiO
2The visible light activity of semiconductor light-catalyst, efficiently utilizing the visible light in the sunshine is TiO
2One of key content of Study on photocatalyst.
In order to improve TiO
2Semiconductor light-catalyst is in the spectral response and the photocatalysis quantum efficiency thereof of visible-range, and scientist is to TiO both at home and abroad
2Semiconductor light-catalyst has carried out various modifications, and is compound comprising noble metal loading, metal ion mixing, nonmetallic ion-doped, optical semiconductor sensitization and semiconductor.Semiconductor composite Ti O
2Can improve TiO
2The separation of charge effect, expand visible light-responded scope.In recent years, and people such as Benjaram M.Reddy (B.M.Reddy, I.Ganesh, Journal of Molecular Catalysis A:Chemical, 2001,169,207-223) utilize coprecipitation method to prepare La
2O
3-TiO
2And V
2O
5/ La
2O
3-TiO
2Composite.People such as Huang (H.J.Huang, D.Z.Li, Q.Lin, W.J.Zhang, Y.Shao, Y.B.Chen, M.Sun, X.Z.Fu, Environ.Sci.Technol.2009,43,4164-4168) use sol-gel process to prepare LaVO
4/ TiO
2Composite nanometer particle, and be used to the benzene of degrading, discover through LaVO
4TiO after the modification
2Its photochemical properties of nano particle is greatly improved.TiO
2Nanotube is as TiO
2A kind of form owing to have bigger specific area, thereby have stronger absorption property, help further to improve TiO
2Photocatalysis performance, and, photo-generated carrier than graininess easier from the ion internal migration to the surface, thereby improved the separative efficiency in light induced electron-hole, therefore, the preparation LaVO
4/ TiO
2Composite nano tube will improve TiO
2Photocatalysis efficiency and visible light-responded scope.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method and application thereof of photochemical catalyst, and this catalyst can improve TiO
2To the response of visible light, reduce the compound of light induced electron-hole, effectively improved degraded to organic pollution.
Preparation method of the present invention is as follows:
1) LaVO
4Preparation: with 6.5mmol NH
4VO
3Be dissolved in the 0.65M NaOH solution, form NaVO
3Solution.Then, with 0.5M La (NO
3)
3Drips of solution adds NaVO
3Solution after stirring a period of time, changes above-mentioned solution in the reactor of polytetrafluoroethylene (PTFE), at 200 ℃ of following hydro-thermal reaction 48h.After the reaction, sediment is cleaned respectively, filters with deionized water and ethanol, drying.
2) LaVO
4/ TiO
2The preparation of composite nanometer particle: at first, butyl titanate is added dropwise in the ethanol solution, forms a solution.Secondly, with the mixing (volume ratio is 40: 3: 15) of absolute ethyl alcohol, nitric acid and water, form b solution.Then the b drips of solution is added in a solution, after the stirring, form TiO
2Colloidal sol.At last, with LaVO
4Join TiO
2In the colloidal sol, ultrasonic after, leave standstill 24h, dry then, obtain LaVO
4/ TiO
2Composite nanometer particle.LaVO wherein
4With respect to TiO
2The adding mass ratio can be chosen as 1-20.
3) LaVO
4/ TiO
2The preparation of composite nano tube: with LaVO
4/ TiO
2Composite nanometer particle is put into alkaline solution, ultrasonic after, above-mentioned solution is changed in the reactor of polytetrafluoroethylene (PTFE), at 180 ℃ of following hydro-thermal reaction 48h.After the reaction, sediment is cleaned respectively with rare nitric acid and ethanol, drying is calcined 6h down at 100 ℃-800 ℃ again, finally obtains composite nano tube.
The invention has the beneficial effects as follows that technology is fairly simple, easy operating can be applicable to industrial production simultaneously again.The LaVO for preparing by the method for the invention
4/ TiO
2Composite nano materials has tubular form, has big adsorption capacity.The raw material that preparation is used is cheap and easy to get, need not expensive device.
Description of drawings
Fig. 1 a is LaVO
4/ TiO
2The sem photograph that the composite nano tube multiplication factor is 10000 times (SEM).
Fig. 1 b is LaVO
4/ TiO
2The sem photograph that the composite nano tube multiplication factor is 30000 times (SEM).
Fig. 2 is LaVO
4/ TiO
2The x-ray diffraction pattern of composite nano tube (XRD).Abscissa is the angle of diffraction (2 θ) of twice, and ordinate is the intensity (cps) of diffraction maximum.
Surface photovoltaic spectroscopy among Fig. 3 (SPV) has characterized the LaVO of preparation
4/ TiO
2Composite nano tube visible light-responded.Abscissa is wavelength (wavelength), and ordinate is energy (μ V).
The specific embodiment
Be described in detail specific embodiments of the invention below in conjunction with technical scheme and accompanying drawing.
Embodiment 1
6.5mmol NH
4VO
3Be dissolved in the 0.65M NaOH solution, form NaVO
3Solution.Then, with 0.5M La (NO
3)
3Drips of solution adds NaVO
3Solution after stirring a period of time, changes above-mentioned solution in the reactor of polytetrafluoroethylene (PTFE), at 200 ℃ of following hydro-thermal reaction 48h.After the reaction, sediment is cleaned respectively 3 times with deionized water and ethanol, drying obtains being jade-green LaVO
4Then, preparation LaVO
4/ TiO
2Composite nanometer particle, its synthesis step is as follows: at first, butyl titanate is added dropwise in the ethanol solution, forms a solution.Secondly, with the mixing (volume ratio is 40: 3: 15) of absolute ethyl alcohol, nitric acid and water, form b solution.Then the b drips of solution is added in a solution, stir 30min, form TiO
2Colloidal sol.At last, with the LaVO of 0.02g
4Join TiO
2In the colloidal sol, behind the ultrasonic 30min, leave standstill 24h, dry then, obtain LaVO
4/ TiO
2Composite nanometer particle.At last, with LaVO
4/ TiO
2Composite nanometer particle is put into alkaline solution, behind the ultrasonic 30min, above-mentioned solution is changed in the reactor of polytetrafluoroethylene (PTFE), at 180 ℃ of following hydro-thermal reaction 48h.After the reaction, sediment is cleaned respectively 3 times with rare nitric acid and ethanol, drying with the heating rate of 2 ℃/min, is calcined 6h down at 300 ℃ then, finally obtains composite nano tube.The LaVO that makes
4/ TiO
2The environmental scanning electronic microscope photo of composite nano tube is shown in Fig. 1 (a) and (b).Fig. 1 (a) is 10000 times a electromicroscopic photograph, from this low multiple Electronic Speculum, composite nano tube is prepared in a large number as can be seen, Fig. 1 (b) is 30000 times a electromicroscopic photograph, from this high multiple Electronic Speculum, the about 50nm-350nm of the diameter of composite nano tube as can be seen, the about 15nm of thickness of pipe wall, pipe range can reach several μ m.X-ray diffractogram as shown in Figure 2, as can be seen from Figure 2, under different calcining heats, composite nano tube just along with the rising of temperature, begins to occur the rutile phase mainly based on anatase mutually gradually.SPV by Fig. 3 characterizes, and composite nano tube can produce electronics-hole separation under the wavelength greater than 400nm as can be seen, illustrates that it has response to visible light.
Embodiment 2
According to the preparation method of the present invention of embodiment 1, just do not add LaVO
4, make pure TiO
2Nano pipe light catalyst.
Embodiment 3
According to the preparation method of the present invention of embodiment 1, just with LaVO
4Amount is increased to 0.4g, under 300 ℃ of calcinings, makes 20% LaVO
4/ TiO
2The compound nanotube photocatalytic agent.
According to the preparation method of the present invention of embodiment 1, with LaVO
4Amount is increased to the LaVO of 0.1g
4/ TiO
2The composite nano tube calcining heat is increased to 600 ℃, makes LaVO
4/ TiO
2The compound nanotube photocatalytic agent.
Claims (2)
1. visible light-responded LaVO
4With TiO
2The preparation method of composite nano tube is characterized in that following steps:
1) LaVO
4Preparation: with 6.5mmol NH
4VO
3Be dissolved in the 0.65M NaOH solution, form NaVO
3Solution; Then, with 0.5M La (NO
3)
3Drips of solution adds NaVO
3Solution changes above-mentioned solution in the reactor of polytetrafluoroethylene (PTFE) over to after the stirring, at 200 ℃ of following hydro-thermal reaction 48h; After the reaction, sediment is cleaned respectively, filters with deionized water and ethanol, drying;
2) LaVO
4With TiO
2The preparation of composite nanometer particle: at first, butyl titanate is added dropwise in the ethanol solution, forms a solution; Secondly, be that 40: 3: 15 absolute ethyl alcohol, nitric acid and water mixes with volume ratio, form b solution; Then the b drips of solution is added in a solution, after the stirring, form TiO
2Colloidal sol; At last, with LaVO
4Join TiO
2In the colloidal sol, ultrasonic after, leave standstill 24h, dry then, obtain LaVO
4With TiO
2Composite nanometer particle;
3) LaVO
4With TiO
2The preparation of composite nano tube: with LaVO
4With TiO
2Composite nanometer particle is put into alkaline solution, ultrasonic after, above-mentioned solution is changed in the reactor of polytetrafluoroethylene (PTFE), at 180 ℃ of following hydro-thermal reaction 48h; After the reaction, with sediment with rare nitric acid and ethanol clean respectively, drying, at 100 ℃-800 ℃ following calcining 6h, finally obtain composite nano tube again.
2. preparation method according to claim 1 is characterized in that step 2) middle LaVO
4With respect to TiO
2The adding mass ratio be 1-20.
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|---|---|---|---|
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|---|---|---|---|
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| CN101966452B CN101966452B (en) | 2012-09-05 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320659A (en) * | 2011-08-19 | 2012-01-18 | 河北联合大学 | A kind of method that adopts the synthetic vanadic acid lanthanum nano material of microwave irradiation |
| CN102744065A (en) * | 2012-07-19 | 2012-10-24 | 福州大学 | Catalyst with optothermal coupling effect and preparation method thereof |
| CN102786816A (en) * | 2012-08-22 | 2012-11-21 | 北京化工大学 | Preparation method of water-soluble rare earth luminous nanocrystallines with functionalized surfaces |
| CN103464135A (en) * | 2012-06-07 | 2013-12-25 | 中国人民解放军63971部队 | Preparation method of YVO4/TiO2 composite photocatalyst |
| CN103537302A (en) * | 2013-10-01 | 2014-01-29 | 大连理工大学 | Method for preparing compound nanometer photocatalyst by adopting CdSe quantum dot |
| CN105457621A (en) * | 2015-11-24 | 2016-04-06 | 李跃军 | Preparation method of heterojunction titanium dioxide/rare-earth doped vanadate composite nanofiber photocatalytic material |
| CN107597098A (en) * | 2017-09-27 | 2018-01-19 | 大连民族大学 | A kind of one pot process has visible light-responded photochemical catalyst LaVO4/WO3The preparation method of nanometer sheet |
| CN108786829A (en) * | 2018-04-04 | 2018-11-13 | 芜湖职业技术学院 | Photochemical catalyst of doped nano titanium dioxide and preparation method thereof |
| CN112387270A (en) * | 2020-12-07 | 2021-02-23 | 清华大学 | Photocatalytic material for eliminating VOCs and ozone and multilayer-hole-plate type photocatalytic reactor |
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2010
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Patent Citations (3)
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320659A (en) * | 2011-08-19 | 2012-01-18 | 河北联合大学 | A kind of method that adopts the synthetic vanadic acid lanthanum nano material of microwave irradiation |
| CN102320659B (en) * | 2011-08-19 | 2013-07-31 | 河北联合大学 | Method for synthesizing lanthanum-vanadate nano material by adopting microwave-radiation method |
| CN103464135A (en) * | 2012-06-07 | 2013-12-25 | 中国人民解放军63971部队 | Preparation method of YVO4/TiO2 composite photocatalyst |
| CN102744065A (en) * | 2012-07-19 | 2012-10-24 | 福州大学 | Catalyst with optothermal coupling effect and preparation method thereof |
| CN102744065B (en) * | 2012-07-19 | 2014-10-01 | 福州大学 | Catalyst with optothermal coupling effect and preparation method thereof |
| CN102786816B (en) * | 2012-08-22 | 2014-04-02 | 北京化工大学 | Preparation method of water-soluble rare earth luminous nanocrystallines with functionalized surfaces |
| CN102786816A (en) * | 2012-08-22 | 2012-11-21 | 北京化工大学 | Preparation method of water-soluble rare earth luminous nanocrystallines with functionalized surfaces |
| CN103537302A (en) * | 2013-10-01 | 2014-01-29 | 大连理工大学 | Method for preparing compound nanometer photocatalyst by adopting CdSe quantum dot |
| CN105457621A (en) * | 2015-11-24 | 2016-04-06 | 李跃军 | Preparation method of heterojunction titanium dioxide/rare-earth doped vanadate composite nanofiber photocatalytic material |
| CN107597098A (en) * | 2017-09-27 | 2018-01-19 | 大连民族大学 | A kind of one pot process has visible light-responded photochemical catalyst LaVO4/WO3The preparation method of nanometer sheet |
| CN107597098B (en) * | 2017-09-27 | 2020-08-14 | 大连民族大学 | One-pot synthesis of visible-light-responsive photocatalyst LaVO4/WO3Preparation method of nanosheet |
| CN108786829A (en) * | 2018-04-04 | 2018-11-13 | 芜湖职业技术学院 | Photochemical catalyst of doped nano titanium dioxide and preparation method thereof |
| CN108786829B (en) * | 2018-04-04 | 2021-05-11 | 芜湖职业技术学院 | Photocatalyst doped with nano titanium dioxide and preparation method thereof |
| CN112387270A (en) * | 2020-12-07 | 2021-02-23 | 清华大学 | Photocatalytic material for eliminating VOCs and ozone and multilayer-hole-plate type photocatalytic reactor |
| CN112387270B (en) * | 2020-12-07 | 2021-11-30 | 清华大学 | Photocatalytic material for eliminating VOCs and ozone and multilayer-hole-plate type photocatalytic reactor |
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| Publication number | Publication date |
|---|---|
| CN101966452B (en) | 2012-09-05 |
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