CN109759039A - A kind of loaded photocatalyst and preparation method thereof - Google Patents
A kind of loaded photocatalyst and preparation method thereof Download PDFInfo
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- CN109759039A CN109759039A CN201711097682.2A CN201711097682A CN109759039A CN 109759039 A CN109759039 A CN 109759039A CN 201711097682 A CN201711097682 A CN 201711097682A CN 109759039 A CN109759039 A CN 109759039A
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Abstract
The present invention provides a kind of loaded photocatalyst, the loaded photocatalyst includes: carrier layer, middle layer and catalyst layer;The carrier layer is porous aluminium foil, and the middle layer is metal powder layer, and the catalyst layer is TiO2Layer.On the other hand, the present invention provides a kind of method for preparing above-mentioned loaded photocatalyst, comprising the following steps: punches aluminium foil, forms porous aluminium foil;Metal dust slurry is coated on carrying layer surface, forms metal powder layer, after first time drying, sintering, anodic oxidation, becomes middle layer;The porous aluminium foil for being coated with middle layer is impregnated in Catalyst precursor solutions, after taking-up after second of drying, sintering, anodic oxidation, forms catalyst layer.Loaded photocatalyst of the invention has the characteristics that include the carrier of high surface area, carrier and catalyst layer compatibility are good, the load capacity and effective surface area, the long-life for enhancing photocatalysis efficiency of photochemical catalyst can be improved.
Description
Technical field
The present invention relates to catalyst technical fields, specifically, the present invention relates to a kind of loaded photocatalyst and its preparations
Method.
Technical background
Photocatalysis is usually to drop the catalytic organism being in contact with it using the photocatalyst that visible/ultraviolet light is catalyzed
Solution.In recent years, the light absorption pollutant issued using sunlight or artificial light sources is decomposed the photochemical catalyst of removal in energy
Source environmental area plays the effect to become more and more important, has obtained extensive research.It is usually used in photocatalysis Decomposition pollutant at present
Catalyst is mainly N-type semiconductor, such as TiO2、ZnO、CdS、SnO2、Fe2O3Deng wherein TiO2Because its is cheap and easy to get, chemical stabilization
Property it is good, photocatalysis effect is high, in terms of pollution degradation using at most, be also widely studied.
TiO2The structure and preparation method of catalyst also all become research topic concerned by people, in previous research
In, suspended phase semiconductor photocatalytic oxidation is mainly used, the defect of the method is that in actual use, photochemical catalyst is easy solidifying
It is poly-, catalytic activity is lost, and then reduce catalytic efficiency.
Currently, also there are numerous studies about fixed semiconductor catalyst oxidizing process, wherein for loading TiO2Catalyst
Carrier, main active carbon, ceramics, light, glass, quartz, zeolite etc. at present, for loading TiO2The method of catalyst,
It is main at present that TiO is made by sintering2Catalyst is attached to carrier surface, however these carriers and TiO2Catalyst surface compatibility
It is poor, easily occur falling off and deactivation phenomenom, reduces photocatalysis efficiency, while surface area is small, the catalytic amount of load is limited, comparison
Suspended phase semiconductor photocatalytic oxidation, photocatalysis efficiency improve limited.
Summary of the invention
Aiming at the shortcomings in the prior art, one of the objects of the present invention is to provide a kind of loaded photocatalyst, this hairs
It includes the carrier of high surface area that bright loaded photocatalyst, which has, carrier and catalyst layer compatibility are good, photocatalysis can be improved
The load capacity and effective surface area of agent enhance the features such as long-life of photocatalysis efficiency, can overcome in the prior art carrier with
TiO2The problems such as catalyst poor compatibility, limited catalytic amount easy to fall off, load.
For this purpose, the present invention adopts the following technical scheme that:
On the one hand, the present invention provides a kind of loaded photocatalyst, the loaded photocatalyst include: carrier layer,
Middle layer and catalyst layer;The carrier layer is connect with the middle layer, and the middle layer is located at the carrying layer surface, described
Middle layer is connect with the catalyst layer, and the catalyst layer is located at the interlayer surfaces, and the middle layer is located at the load
Between body layer and the catalyst layer.
Preferably, the carrier layer is porous aluminium foil.
Preferably, the porous aluminium foil is with a thickness of 15-80 microns.
Preferably, it is described it is porous be through hole, it is further preferred that the porous shape be round hole, square hole or
Diamond hole.
Preferably, the porous aperture is 0.5-5 microns.
Preferably, the middle layer is metal powder layer.Adhere to the metal powder layer in the porous aluminium foil surface, it can
To improve the surface area of carrier, to improve the load capacity and effective surface area of catalyst, enhance photocatalysis efficiency.
Preferably, the metal powder layer is the mixed layer of aluminium powder layer, titanium valve layer or aluminium powder and titanium valve.
Preferably, the metal powder layer is with a thickness of 5-30 microns.
Preferably, the partial size of the metal powder is 1-20 microns.
Preferably, the catalyst layer is TiO2Layer.
Another object of the present invention is to provide a kind of methods for preparing above-mentioned loaded photocatalyst, for this purpose,
The invention adopts the following technical scheme:
A method of preparing above-mentioned loaded photocatalyst, comprising the following steps:
S11: carrier layer is provided: aluminium foil being punched, porous aluminium foil is formed, becomes carrier layer;
Preferably, the hole knockout is that mechanical stamping punching or electrochemical etching punch.
Preferably, described porous for through hole.It is formed and runs through aluminium foil, on the one hand can increase the surface area of aluminium foil, improved
Catalyst loading, on the other hand, perforated holes enhance light pass-through, improve light source utilization rate;Aluminium foil conduct simultaneously
Metal base has good ductility, easy to process, meets the requirement of different catalytic devices.
It is further preferred that the porous shape is round hole, square hole or diamond hole.
Preferably, the porous aperture is 0.5-5 microns.
S12: preparation middle layer: metal dust slurry is coated on carrying layer surface, metal powder layer is formed, by first
After secondary drying, first sintering, first time anodic oxidation, metal powder layer is formed, middle layer is become;
Preferably, the metal dust slurry is coated on carrying layer surface two sides.Apply the upper and lower surface of porous aluminium foil
It is furnished with metal dust slurry, the surface area of carrier can be made to further increase.
Preferably, the metal dust slurry includes metal powder, adhesive and solvent.
Preferably, the metal powder is aluminium powder, titanium valve or combinations thereof.
Preferably, the partial size of the metal powder is 1-20 microns.
Preferably, the adhesive is carboxymethyl cellulose, polyvinyl alcohol, carboxyethyl cellulose, epoxy resin, acrylic acid
Any one in resin or two kinds.
Preferably, the solvent is water, acetone, toluene, ethyl acetate, any one in epoxy resin.
Preferably, the temperature of the first time drying is room temperature.The room temperature refers to 25-30 DEG C.
Preferably, the temperature of the first sintering is 400-650 DEG C.
Preferably, the time of the first sintering is 4-12h.
Preferably, the atmosphere of the first sintering is nitrogen atmosphere, argon atmosphere or vacuum atmosphere.
Preferably, the anodizing solution of the first time anodic oxidation is the mixed aqueous solution of boric acid and oxalic acid.
It is further preferred that the concentration of the boric acid is 3-15wt%, the concentration of the oxalic acid is 2-6wt%.
Preferably, the oxidation voltage of the first time anodic oxidation is 10-80V.
Preferably, the oxidizing temperature of the first time anodic oxidation is 50-90 DEG C.
The first time anodic oxidation is that porous aluminium foil is placed in anodizing solution, applies voltage to it, and electrification occurs
Anodic oxidation is learned, the oxidization of metal powder on its surface is made, generates aluminium oxide or titanium oxide.
By drying for the first time, first sintering, after first time anodic oxidation, knot that metal dust slurry can be made to consolidate
It closes in porous aluminium foil surface, while improving the weatherability of carrier material.
Use metal powder layer as middle layer, catalyst layer can be made and carrier layer is more preferable, stronger combination, because with
Other nonmetallic materials are compared, and metal powder has lower hot melt and ductility and easily oxidizable energy, are sintered Shi Nengyu
Catalyst TiO2It is easier to fuse, furthermore metal powder is sphere material, has high surface area, can increase catalyst TiO2Load
Carrying capacity;On the other hand, metal powder is aluminium powder, titanium valve or combinations thereof, because aluminium and titanium are congeners, what when anodic oxidation generated
Aluminium oxide or titanium oxide and catalyst TiO2Compatibility is fine, while it is vesicular texture, can also be improved catalyst
TiO2Loading.
S13: it prepares catalyst layer: the porous aluminium foil Jing Guo S12 step process is impregnated in Catalyst precursor solutions,
After taking-up after second of drying, second sintering, second of anodic oxidation, catalyst layer is formed.
Preferably, the Catalyst precursor solutions are TiO2Precursor solution.
Preferably, the TiO2Precursor solution includes lactic acid, acetic acid and butyl titanate.
It is further preferred that in the solvent, with molar ratio computing, lactic acid: acetic acid: butyl titanate=5:5:1.
Preferably, second of dry temperature is room temperature.The room temperature refers to 25-30 DEG C.
Preferably, the temperature of second of sintering is 200-400 DEG C.
Preferably, the time of second of sintering is 4-12h.
Preferably, the atmosphere of second of sintering is air atmosphere.
Preferably, the anodizing solution of second of anodic oxidation is the mixed aqueous solution of boric acid and oxalic acid.
It is further preferred that the concentration of the boric acid is 3-15wt%, the concentration of the oxalic acid is 2-6wt%.
Preferably, the oxidation voltage of second of anodic oxidation is 10-80V.
Preferably, the temperature of second of anodic oxidation is 50-90 DEG C.
Second of anodic oxidation is that porous aluminium foil is placed in anodizing solution, applies voltage to it, send out metal
Raw electrochemical anodic oxidation generates aluminium ion or titanium ion to catalyst TiO2Layer migration, keeps carrier layer chimeric with catalyst layer,
Enhance the adhesive force of catalyst layer.
The invention has the benefit that
(1) loaded photocatalyst provided by the invention is using porous aluminium foil as carrier, and in carrier surface adhesion metal powder
Last layer makes carrier surface area with higher, can improve the load capacity and effective surface area of catalyst, enhances photocatalysis efficiency;
(2) loaded photocatalyst provided by the invention makes catalyst layer adhesion-tight using metal powder layer as middle layer,
Extend the service life of catalyst;
(3) loaded photocatalyst preparation process provided by the invention passes through anodic oxidation twice, first time anodic oxidation
Metal powder layer can be made to aoxidize, improve the compatibility of metal powder layer and catalyst layer, second of anodic oxidation can make to carry
Body layer is chimeric with catalyst layer generation, improves the adhesive force of catalyst layer.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of loaded photocatalyst provided by the invention.
Fig. 2 is the preparation flow figure of loaded photocatalyst provided by the invention.
In figure: carrier layer 100, middle layer 200, catalyst layer 300.
Specific embodiment
To keep the technical problems solved, the adopted technical scheme and the technical effect achieved by the invention clearer, below
It will the technical scheme of the embodiment of the invention will be described in further detail in conjunction with attached drawing, it is clear that described embodiment is only
It is a part of the embodiment of the present invention, instead of all the embodiments.
Embodiment 1
(1) 15 microns of thick aluminium foils are passed through into mechanical punching, formation is porous to run through aluminium foil, and aperture is 1 micron.
(2) by weight, the aluminium powder for being 6 microns in partial size: polyvinyl alcohol: water=15:5:80 ratio is configured to metal
Metal dust slurry is coated on porous two surfaces through aluminium foil by powder slurries, and single side coating layer thickness is 5 microns.
(3) high under 550 DEG C, argon atmosphere by the porous aluminium foil after coating metal powder slurry after drying at room temperature
Temperature sintering 8h.
(4) by the mixing of the sintered porous oxalic acid for being placed in boric acid and 2wt% that concentration is 10wt% through aluminium foil
In aqueous solution, it is 65 DEG C, under 30V voltage in temperature, carries out first time anodic oxidation.
(5) the porous aluminium foil that runs through after first time anodic oxidation is impregnated in TiO2Precursor solution (each component in solution
Molar ratio is lactic acid: acetic acid: butyl titanate=5:5:1) in, then drying at room temperature, high temperature is burnt under 200 DEG C, air atmosphere
Tie 8h.
(6) finally by the sintered porous oxalic acid for being placed in boric acid and 2wt% that concentration is 10wt% through aluminium foil
In mixed aqueous solution, it is 65 DEG C, under 30V voltage in temperature, carries out second of anodic oxidation, obtain loaded photocatalyst.
Embodiment 2
(1) 30 microns of thick aluminium foils are beaten in the electrolyte of 15% hydrochloric acid and 0.5% sulfuric acid by electrochemical etching
Hole, formation is porous to run through aluminium foil, and aperture is 0.5-1 microns.
(2) by weight, the aluminium powder for being 1-3 microns in partial size: carboxymethyl cellulose: water=10:5:85 ratio, configuration
At metal dust slurry, metal dust slurry is coated on porous two surfaces through aluminium foil, single side coating layer thickness is 15 micro-
Rice.
(3) by the porous aluminium foil that runs through after coating metal powder slurry after drying at room temperature, in 600 DEG C, argon atmosphere
Lower high temperature sintering 4h.
(4) by the sintered porous oxalic acid mixing water for being placed in boric acid and 2wt% that concentration is 10wt% through aluminium foil
In solution, it is 75 DEG C, under 30V voltage in temperature, carries out first time anodic oxidation.
(5) the porous aluminium foil after first time anodic oxidation is impregnated in TiO2Precursor solution (each component mole in solution
Than for lactic acid: acetic acid: butyl titanate=5:5:1) in, then drying at room temperature, the high temperature sintering 8h under 400 DEG C, air atmosphere.
(6) finally the sintered porous oxalic acid that boric acid and 2wt% that concentration is 10wt% are placed in through aluminium foil is mixed
In Heshui solution, it is 75 DEG C, under 30V voltage in temperature, carries out second of anodic oxidation, obtain loaded photocatalyst.
Embodiment 3
(1) 45 microns of thick aluminium foils are passed through into mechanical punching, formation is porous to run through aluminium foil, and aperture is 3 microns.
(2) by weight, the aluminium powder for being 6-8 microns by partial size: 4-5 microns of titanium valve: epoxy resin=5:5:90 ratio
Example, is configured to metal dust slurry, metal dust slurry is coated on porous two surfaces through aluminium foil, single side coating layer thickness
It is 5 microns.
(3) by the porous aluminium foil that runs through after coating metal powder slurry after drying at room temperature, in 660 DEG C, nitrogen atmosphere
Lower high temperature sintering 12h.
(4) by the mixing water of the sintered porous oxalic acid for being placed in boric acid and 5wt% that concentration is 8wt% through aluminium foil
In solution, it is 50 DEG C, under 70V voltage in temperature, carries out first time anodic oxidation.
(5) the porous aluminium foil that runs through after first time anodic oxidation is impregnated in TiO2Precursor solution (each component in solution
Molar ratio is lactic acid: acetic acid: butyl titanate=5:5:1) in, then drying at room temperature, at 350 DEG C, high temperature is burnt under argon atmosphere
Tie 4h.
(6) finally by it is sintered it is porous through aluminium foil be placed in concentration be 8wt% boric acid mixed with the oxalic acid of 5wt%
In aqueous solution, it is 50 DEG C, under 70V voltage in temperature, carries out second of anodic oxidation, obtain loaded photocatalyst.
Embodiment 4
(1) 60 microns of thick aluminium foils are passed through into mechanical punching, formation is porous to run through aluminium foil, and aperture is 3 microns.
(2) by weight, the titanium valve for being 10-12 microns in partial size: acrylic resin: toluene=15:15:70 ratio,
It is configured to metal dust slurry, metal dust slurry is coated on porous two surfaces through aluminium foil, single side coating layer thickness is
10 microns.
(3) by porous after coating metal powder slurry through aluminium foil after drying at room temperature, at 600 DEG C, vacuum atmosphere
Lower high temperature sintering 10h.
(4) by the sintered porous oxalic acid mixing water for being placed in boric acid and 6wt% that concentration is 15wt% through aluminium foil
In solution, it is 65 DEG C, under 50V voltage in temperature, carries out first time anodic oxidation.
(5) the porous aluminium foil that runs through after first time anodic oxidation is impregnated in TiO2Precursor solution (each component in solution
Molar ratio is lactic acid: acetic acid: butyl titanate=5:5:1) in, then drying at room temperature, high temperature is burnt under 350 DEG C, air atmosphere
Tie 6h.
(6) finally by the mixed of the oxalic acid for being placed in boric acid and 6wt% that concentration is 15wt% through aluminium foil porous after sintering
In Heshui solution, it is 65 DEG C, under 50V voltage in temperature, carries out second of anodic oxidation, obtain loaded photocatalyst.
Embodiment 5
(1) 80 microns of thick aluminium foils are passed through into mechanical punching, formation is porous to run through aluminium foil, and aperture is 5 microns.
(2) by weight, the titanium valve for being 15 microns by partial size: 5-6 microns of aluminium powder: carboxymethyl cellulose: water=10:3:
The proportional arrangement of 7:80 is coated on porous two surfaces through aluminium foil at metal dust slurry, and single side coating layer thickness is 30 micro-
Rice.
(3) by the porous aluminium foil that runs through after coating metal powder slurry after drying at room temperature, in 660 DEG C, nitrogen atmosphere
Lower high temperature sintering 10h.
(4) by the mixing of the sintered porous oxalic acid for being placed in boric acid and 5wt% that concentration is 10wt% through aluminium foil
In aqueous solution, it is 90 DEG C, under 80V voltage in temperature, carries out first time anodic oxidation.
(5) the porous aluminium foil that runs through after first time anodic oxidation is impregnated in TiO2Precursor solution (each component in solution
Molar ratio is lactic acid: acetic acid: butyl titanate=5:5:1) in, then drying at room temperature, high temperature is burnt under 250 DEG C, air atmosphere
Tie 12h.
(6) finally by the sintered porous oxalic acid for being placed in boric acid and 5wt% that concentration is 10wt% through aluminium foil
In mixed aqueous solution, in the case where temperature is 90 DEG C, oxidation voltage is 80V voltage, second of anodic oxidation is carried out, support type light is obtained
Catalyst.
Comparative example 1
Commercially available absorbent charcoal carrier, is impregnated in TiO2(each component molar ratio is lactic acid: acetic acid: titanium to precursor solution in solution
Acid four butyl esters=5:5:1) in, after drying at room temperature, 5h is handled under 300 DEG C, air atmosphere.
Comparative example 2
Commercial zeolite carrier, is impregnated in TiO2(each component molar ratio is lactic acid: acetic acid: metatitanic acid to precursor solution in solution
Four butyl esters=5:5:1) in, after drying at room temperature, 5h is handled under 300 DEG C, air atmosphere.
The catalyst of preparation is placed in micro fixed-bed reactor device according to same loading, respectively in sunlight
Under ultraviolet source, degradation experiment is carried out to methyl orange.By using visible spectrophotometer test methyl orange solution in wave
Absorption peak at a length of 462nm is strong and weak, to judge the degradation rate of the methyl orange after different time illumination.Test data such as 1 institute of table
Show.
Methyl orange degradation rate under 1 different catalysts system of table
It can be seen that by the test data of table 1, on the one hand, the degradation rate of embodiment 1-5 is greater than the degradation of comparative example 1-2
Rate shows that the catalyst of support type of the invention, the catalyst of relative usage routine carrier largely improve methyl orange drop
Solution rate;On the other hand, in embodiment 1-5, with the increase of metal powder partial size, the thickness of coating is bigger, the surface provided
Product is more, and under same catalyst loading, catalyst has higher effective surface area, and catalytic efficiency is higher.
The technical principle of the invention is described above in combination with a specific embodiment.These descriptions are intended merely to explain of the invention
Principle, and shall not be construed in any way as a limitation of the scope of protection of the invention.Based on the explanation herein, the technology of this field
Personnel can associate with other specific embodiments of the invention without creative labor, these modes are fallen within
Within protection scope of the present invention.
Claims (10)
1. a kind of loaded photocatalyst, which is characterized in that the loaded photocatalyst includes carrier layer, middle layer and catalysis
Oxidant layer, the carrier layer are connect with the middle layer, and the middle layer is located at the carrying layer surface, the middle layer with it is described
Catalyst layer connection, the catalyst layer are located at the interlayer surfaces, and the middle layer is located at the carrier layer and urges with described
Between agent layer;Wherein, the carrier layer is porous aluminium foil;The middle layer is metal powder layer;The catalyst layer is
TiO2Layer.
2. loaded photocatalyst according to claim 1, which is characterized in that the porous aluminium foil is micro- with a thickness of 15-80
Rice, aperture are 0.5-5 microns.
3. loaded photocatalyst according to claim 1, which is characterized in that the metal powder layer is aluminium powder layer, titanium
The mixed layer of bisque or aluminium powder and titanium valve.
4. loaded photocatalyst according to claim 1, which is characterized in that the metal powder layer is micro- with a thickness of 5-30
Rice, the partial size of the metal powder are 1-20 microns.
5. according to claim 1 to the preparation method of loaded photocatalyst as claimed in claim 4, which is characterized in that including
Following steps:
S11: carrier layer is provided: aluminium foil being punched, porous aluminium foil is formed, becomes carrier layer;
S12: preparation middle layer: being coated on carrying layer surface for metal dust slurry, form metal powder layer, dry by first time
After dry, first sintering, first time anodic oxidation, metal powder layer is formed, middle layer is become;
S13: it prepares catalyst layer: the porous aluminium foil Jing Guo S12 step process is impregnated in Catalyst precursor solutions, take out
Afterwards after second of drying, second sintering, second of anodic oxidation, catalyst layer is formed.
6. the preparation method of loaded photocatalyst according to claim 5, which is characterized in that the catalyst precursor
Solution is TiO2Precursor solution, the TiO2Precursor solution includes lactic acid, acetic acid and butyl titanate.
7. the preparation method of loaded photocatalyst according to claim 6, which is characterized in that with molar ratio computing, lactic acid:
Acetic acid: butyl titanate=5:5:1.
8. the preparation method of loaded photocatalyst according to claim 5, which is characterized in that the metal dust slurry
Including metal powder, adhesive and solvent, metal powder is aluminium powder, titanium valve or combinations thereof, and the adhesive is carboxymethyl cellulose
Element, polyvinyl alcohol, carboxyethyl cellulose, epoxy resin, any one or two kinds in acrylic resin, the solvent be water,
Acetone, toluene, ethyl acetate, any one in epoxy resin.
9. the preparation method of loaded photocatalyst according to claim 5, which is characterized in that the first sintering
Temperature is 400-650 DEG C, and the time of the first sintering is 4-12h, and the atmosphere of the first sintering is nitrogen atmosphere, argon
Gas atmosphere or vacuum atmosphere.
10. the preparation method of loaded photocatalyst according to claim 5, which is characterized in that second of anode
The anodizing solution of oxidation is the mixed aqueous solution of boric acid and oxalic acid, and the oxidation voltage of second of anodic oxidation is 10-
80V, the temperature of second of anodic oxidation are 50-90 DEG C.
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WO2024027122A1 (en) * | 2022-08-02 | 2024-02-08 | 南通海星电子股份有限公司 | Preparation method for high-dielectric composite powder sintered foil |
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JP2000265297A (en) * | 1999-03-12 | 2000-09-26 | Toyota Central Res & Dev Lab Inc | Metallic material having photocatalytic activity and its production |
CN1410158A (en) * | 2002-11-12 | 2003-04-16 | 中国地质大学(武汉) | Method of loading titanium dioxide photo catalyst on metal surface |
CN1712131A (en) * | 2005-06-09 | 2005-12-28 | 上海交通大学 | Production of TiO2 naometer light catalyzing net from foam metal carrier |
CN102274710A (en) * | 2011-05-19 | 2011-12-14 | 浙江大学 | Method for preparing zeolite socony mobile-5 (ZSM-5) molecular sieve membrane reactor loaded with Cu/stainless steel screen mesh catalyst |
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JPH10174883A (en) * | 1996-12-18 | 1998-06-30 | Sumitomo Light Metal Ind Ltd | Aluminum material having photocatalytic function and its production |
JP2000265297A (en) * | 1999-03-12 | 2000-09-26 | Toyota Central Res & Dev Lab Inc | Metallic material having photocatalytic activity and its production |
CN1410158A (en) * | 2002-11-12 | 2003-04-16 | 中国地质大学(武汉) | Method of loading titanium dioxide photo catalyst on metal surface |
CN1712131A (en) * | 2005-06-09 | 2005-12-28 | 上海交通大学 | Production of TiO2 naometer light catalyzing net from foam metal carrier |
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