CN110694603A - Preparation method of novel porous structure photocatalyst - Google Patents
Preparation method of novel porous structure photocatalyst Download PDFInfo
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- CN110694603A CN110694603A CN201910844815.0A CN201910844815A CN110694603A CN 110694603 A CN110694603 A CN 110694603A CN 201910844815 A CN201910844815 A CN 201910844815A CN 110694603 A CN110694603 A CN 110694603A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 80
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 37
- 239000004005 microsphere Substances 0.000 claims abstract description 25
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000005530 etching Methods 0.000 claims abstract description 7
- 239000003365 glass fiber Substances 0.000 claims abstract description 7
- 239000012528 membrane Substances 0.000 claims abstract description 7
- 239000010453 quartz Substances 0.000 claims abstract description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000012159 carrier gas Substances 0.000 claims abstract description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- 239000010936 titanium Substances 0.000 claims abstract description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 6
- 239000005543 nano-size silicon particle Substances 0.000 claims description 4
- 239000002159 nanocrystal Substances 0.000 claims description 2
- 238000005118 spray pyrolysis Methods 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 8
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 239000003960 organic solvent Substances 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 7
- 238000000197 pyrolysis Methods 0.000 description 5
- 229910003074 TiCl4 Inorganic materials 0.000 description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000001782 photodegradation Methods 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- 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
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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- 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
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- 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
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- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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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- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
The invention belongs to the technical field of new materials, and particularly relates to a preparation method of a novel porous structure photocatalyst, which comprises the following steps: the method comprises the following steps: dissolving a titanium precursor in deionized water to prepare a 0.5M aqueous solution; step two: adding silica sol into the solution to serve as a precursor solution, atomizing the solution into micrometer-sized liquid drops through an ultrasonic atomizer, and taking silica microspheres with different sizes as hard templates; step three: then the liquid drops enter a high-temperature quartz tube type reactor under the assistance of carrier gas, and products are collected by adopting a glass fiber filter membrane; step four: calcining at 450 ℃ for 1 hour and etching with 10 wt% hydrofluoric acid at room temperature to obtain the titanium dioxide microsphere photocatalyst with a porous structure. The invention realizes the separation and reutilization of nano-sized titanium dioxide, has high catalytic efficiency, and can realize the comprehensive effect of industrial application by using the organic solvent and the template agent.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to a preparation method of a novel porous structure photocatalyst.
Background
As global economy continues to increase at a high rate, environmental pollution and energy shortage problems become more and more serious. The treatment of harmful organic pollutants in water resources is one of the current research hotspots. The photocatalysis technology is a novel green and environment-friendly sewage treatment technology because the organic pollutants are converted into harmless water and carbon dioxide by utilizing solar energy. Since 1972, the pioneering work of japanese scientists Fujishima and Honda on the photocatalytic performance of titanium dioxide semiconductor oxides, much attention has been paid to research surrounding the photocatalysis of nano-titanium dioxide. However, commercial nano-sized titanium dioxide particles have the problems of high cost, small size, difficulty in separation and reuse and the like, and the exertion of the photocatalytic performance of the nano-sized titanium dioxide and the application of the nano-sized titanium dioxide in environmental management are limited to a certain extent.
In addition, Kikuo Okuyama et al prepared a titanium dioxide microsphere with a macroporous structure by using a polystyrene sphere as a template and a commercial titanium dioxide nanoparticle as a precursor, wherein the pore structure and morphology of the titanium dioxide microsphere can be finely controlled by the amount of the polystyrene sphere, but the photocatalytic performance of the titanium dioxide microsphere is general. On the other hand, organic templating agents such as P123 and F127 have also been used to design and prepare titania-based mesoporous microsphere materials. However, these methods inevitably require an organic solvent and an organic phase surfactant, and have problems such as emission limitation in industrial production.
In the preparation method of the novel porous photocatalyst in the prior art, the problems that nano-sized titanium dioxide is difficult to separate and reuse, the catalytic efficiency is low, an organic solvent and a template agent are used and the like exist, and therefore, the research and development of the preparation method of the novel porous photocatalyst are urgently needed.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above and/or the problems occurring in the existing preparation methods of the novel porous structure photocatalyst.
Therefore, the invention aims to provide a preparation method of a novel porous structure photocatalyst, which can realize the separation and reuse of nano-sized titanium dioxide, has high catalytic efficiency, and can realize industrial application by using an organic solvent and a template agent.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions:
a preparation method of a novel porous structure photocatalyst comprises the following steps:
the preparation method of the novel porous structure photocatalyst comprises the following steps:
the method comprises the following steps: dissolving a titanium precursor in deionized water to prepare a 0.5M aqueous solution;
step two: adding silica sol into the solution to serve as a precursor solution, atomizing the solution into micrometer-sized liquid drops through an ultrasonic atomizer, and taking silica microspheres with different sizes as hard templates;
step three: then the liquid drops enter a high-temperature quartz tube type reactor under the assistance of carrier gas, and products are collected by adopting a glass fiber filter membrane;
step four: calcining at 450 ℃ for 1 hour and etching with 10 wt% hydrofluoric acid at room temperature to obtain the titanium dioxide microsphere photocatalyst with a porous structure.
As a preferable embodiment of the preparation method of the novel porous structure photocatalyst of the present invention, wherein: the titanium dioxide porous microspheres are composed of 5-10nm anatase phase titanium dioxide nanocrystals, and the specific surface area of the product is 40-120m2/g。
As a preferable embodiment of the preparation method of the novel porous structure photocatalyst of the present invention, wherein: the particle size of the adopted nano silicon dioxide microsphere hard template is 5-120 nanometers, and the addition amount is 10% -70%.
As a preferable embodiment of the preparation method of the novel porous structure photocatalyst of the present invention, wherein: the temperature of the ultrasonic-assisted spray pyrolysis is 400-800 ℃.
As a preferable embodiment of the preparation method of the novel porous structure photocatalyst of the present invention, wherein: the concentration of hydrofluoric acid used for etching the nano silicon dioxide template is 5-30%.
Compared with the prior art: the preparation method of the novel porous structure photocatalyst in the prior art has excellent photocatalytic activity, is used for photodegradation of methylene blue, has the degradation rate of 99 percent within 1 hour, is simple to operate and low in cost, realizes separation and reutilization of nano-sized titanium dioxide in a continuous modification mode, has high catalytic efficiency, and can realize industrial application by using an organic solvent and a template agent.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the present invention will be described in detail below with reference to the accompanying drawings and detailed embodiments, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise. Wherein:
FIG. 1 is a schematic diagram of a process for preparing porous titanium dioxide microspheres by ultrasonic atomization and pyrolysis;
fig. 2 is an XRD spectrum of titanium dioxide microspheres, wherein: a is a titanium dioxide microsphere with a solid structure, b is a mixture of titanium dioxide and silicon dioxide, and c is a titanium dioxide microsphere with a porous structure;
FIG. 3 is SEM images of different porous titanium dioxide microspheres, wherein a is a pure titanium dioxide microsphere, b is a titanium dioxide microsphere prepared by adding 20 nm silicon oxide as a template, c is a titanium dioxide microsphere prepared by adding 60 nm silicon oxide as a template, and d is a titanium dioxide microsphere prepared by adding 110 nm silicon oxide as a template;
fig. 4 is a TEM image and a high resolution TEM image of the porous titania microspheres.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described herein, and it will be apparent to those of ordinary skill in the art that the present invention may be practiced without departing from the spirit and scope of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below.
The invention provides a preparation method of a novel porous structure photocatalyst, which comprises the following steps:
embodiment mode 1
TiCl4 was dissolved in 100ml deionized water and prepared as a 0.5M aqueous solution. Adding the finally generated silicon dioxide with the mass ratio of 20 percent and the particle size of 110 nanometers into the titanium dioxide as a precursor, and atomizing the silicon dioxide into micrometer-sized liquid drops by an ultrasonic atomizer. Then the liquid drops enter a high-temperature quartz tube type reactor under the assistance of 500L/h of air, the pyrolysis temperature is 800 ℃, and products are collected by adopting a glass fiber filter membrane. Calcining at 450 deg.C for 1 hour and 10 wt% hydrogenEtching with hydrofluoric acid at room temperature to obtain the titanium dioxide microsphere with porous structure and specific surface area of 46.1m2/g。
TiCl4 was dissolved in 100ml deionized water and prepared as a 0.5M aqueous solution. Adding the finally generated silicon dioxide with the mass ratio of 20 percent and the particle size of 20 nanometers into the titanium dioxide as a precursor, and atomizing the silicon dioxide into micrometer-sized liquid drops by an ultrasonic atomizer. Then the liquid drops enter a high-temperature quartz tube type reactor under the assistance of 500L/h of air, the pyrolysis temperature is 600 ℃, and products are collected by adopting a glass fiber filter membrane. Calcining at 450 ℃ for 1 hour and etching with 10 wt% hydrofluoric acid at room temperature to obtain the titanium dioxide microsphere with porous structure and specific surface area of 87.2m2/g。
Embodiment 3
TiCl4 was dissolved in 100ml deionized water and prepared as a 0.5M aqueous solution. Adding silicon dioxide with the mass ratio of the finally generated titanium dioxide of 60 percent and the particle size of 20 nanometers into the titanium dioxide as a precursor, and atomizing the silicon dioxide into micrometer-sized liquid drops by an ultrasonic atomizer. Then the liquid drops enter a quartz tube type reactor under the assistance of 500L/h of air, the pyrolysis temperature is 400 ℃, and products are collected by adopting a glass fiber filter membrane. Calcining at 450 ℃ for 1 hour and etching with 10 wt% hydrofluoric acid at room temperature to obtain the titanium dioxide microsphere with porous structure and specific surface area of 112.3m2/g。
Comparative sample 1
TiCl4 was dissolved in 100ml deionized water and prepared as a 0.5M aqueous solution. And (3) atomizing into micrometer-sized liquid drops by an ultrasonic atomizer without adding a silica template. Then the liquid drops enter a high-temperature quartz tube type reactor under the assistance of 500L/h of air, the pyrolysis temperature is 800 ℃, and products are collected by adopting a glass fiber filter membrane. Calcining at 450 ℃ for 1 hour to obtain the solid titanium dioxide microspheres with the specific surface area of 13.5m2/g。
By combining the above embodiments, the preparation method of the novel porous structure photocatalyst has excellent photocatalytic activity, is used for photodegradation of methylene blue, and has a degradation rate of 99% within 1 hour. The method is simple to operate and low in cost, and the continuous modification mode can realize industrial application.
While the invention has been described above with reference to an embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the various features of the disclosed embodiments of the invention may be used in any combination, provided that no structural conflict exists, and the combinations are not exhaustively described in this specification merely for the sake of brevity and resource conservation. Therefore, it is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (5)
1. A preparation method of a novel porous structure photocatalyst is characterized by comprising the following steps: the preparation method of the novel porous structure photocatalyst comprises the following steps:
the method comprises the following steps: dissolving a titanium precursor in deionized water to prepare a 0.5M aqueous solution;
step two: adding silica sol into the solution to serve as a precursor solution, atomizing the solution into micrometer-sized liquid drops through an ultrasonic atomizer, and taking silica microspheres with different sizes as hard templates;
step three: then the liquid drops enter a high-temperature quartz tube type reactor under the assistance of carrier gas, and products are collected by adopting a glass fiber filter membrane;
step four: calcining at 450 ℃ for 1 hour and etching with 10 wt% hydrofluoric acid at room temperature to obtain the titanium dioxide microsphere photocatalyst with a porous structure.
2. The method for preparing the novel porous photocatalyst according to claim 1, wherein the method comprises the following steps: the titanium dioxide porous microspheres are composed of 5-10nm anatase phase titanium dioxide nanocrystals, and the specific surface area of the product is 40-120m2/g。
3. The method for preparing the novel porous photocatalyst according to claim 1, wherein the method comprises the following steps: the particle size of the adopted nano silicon dioxide microsphere hard template is 5-120 nanometers, and the addition amount is 10% -70%.
4. The method for preparing the novel porous photocatalyst according to claim 1, wherein the method comprises the following steps: the temperature of the ultrasonic-assisted spray pyrolysis is 400-800 ℃.
5. The method for preparing the novel porous photocatalyst according to claim 1, wherein the method comprises the following steps: the concentration of hydrofluoric acid used for etching the nano silicon dioxide template is 5-30%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116237062A (en) * | 2022-12-19 | 2023-06-09 | 莆田学院 | Method for preparing porous indium cadmium sulfide based on ultrasonic atomization |
| CN116832837A (en) * | 2023-03-21 | 2023-10-03 | 武汉理工大学 | Flower ball-shaped TiO 2 Heterojunction material with/BiOBr core-shell structure and preparation method and application thereof |
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2019
- 2019-09-07 CN CN201910844815.0A patent/CN110694603A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116237062A (en) * | 2022-12-19 | 2023-06-09 | 莆田学院 | Method for preparing porous indium cadmium sulfide based on ultrasonic atomization |
| CN116832837A (en) * | 2023-03-21 | 2023-10-03 | 武汉理工大学 | Flower ball-shaped TiO 2 Heterojunction material with/BiOBr core-shell structure and preparation method and application thereof |
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Application publication date: 20200117 |