CN102744091B - Porous inorganic ceramic membrane-graphene-N modified TiO2 photocatalyst material and preparation method thereof - Google Patents
Porous inorganic ceramic membrane-graphene-N modified TiO2 photocatalyst material and preparation method thereof Download PDFInfo
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- CN102744091B CN102744091B CN201210212423.0A CN201210212423A CN102744091B CN 102744091 B CN102744091 B CN 102744091B CN 201210212423 A CN201210212423 A CN 201210212423A CN 102744091 B CN102744091 B CN 102744091B
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- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/208—Off-grid powered water treatment
- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a porous inorganic ceramic membrane-graphene-N modified TiO2 photocatalyst material and a preparation method thereof, and belongs to the technical field of photocatalytic materials. The porous inorganic ceramic membrane-graphene-N modified TiO2 photocatalyst material is characterized in that a porous inorganic ceramic membrane is used as a carrier and a compound of N-modified TiO2 and graphene is loaded on the surface of the carrier; the porous inorganic ceramic membrane-graphene-N modified TiO2 photocatalyst material comprises: by mass, 50 to 80% of the porous inorganic ceramic membrane and 20 to 50% of the compound of N-modified TiO2 and graphene; and the compound of N-modified TiO2 and graphene comprises: by mass, 8 to 10% of graphene and 90 to 92% of N-modified TiO2, and an atomic ratio of N to Ti is 2: 1. The porous inorganic ceramic membrane utilizes thermal power plant coal ash as a raw material and sawdust as a foaming agent so that a preparation cost is low. The porous inorganic ceramic membrane is used as a carrier so that mass transfer on the surface is promoted; a surface adsorption reaction is accelerated; and an organic matter conversion ratio is increased because of a very large specific surface area. Graphene has excellent electron transport properties, mechanical properties and surface chemical properties. N-modified TiO2 has a high light absorption threshold so that photocatalytic properties can be utilized effectively.
Description
Technical field:
The invention belongs to catalysis material technical field, be specifically related to a kind of porous, inorganic ceramic membrane-Graphene-N modification TiO
2photocatalyst material and preparation method thereof.
Background technology:
As a kind of photocatalyst material being most widely used, TiO
2at aspects such as environmental pollution improvement and solar energy utilizations, played the part of key player.At present, at TiO
2the aspect such as preparation had very large breakthrough, but because its energy gap is 3.2 eV(anatases, Anatase), can only absorbing wavelength be less than the ultraviolet light of 400 nm, photocatalysis efficiency is very low.Therefore, a lot of scientists concentrate on TiO by the emphasis of research
2visible ray modification and improve on catalytic efficiency.
The present invention adopts sol-gel process, the synthetic pure inoranic membrane/Graphene/TiO that mixes N of the uniform high activity of particle size dispersion take tetrabutyl titanate as precursor
2enrichment organic pollutants photocatalyst material.After mixing nonmetalloid N, improved TiO
2photoresponse scope, and expand to visible light wave range, reduce the compound of electronics and hole, its photocatalytic activity further improves.Simple titanium dioxide is as catalyst, and the organic matter in sewage is low in its surface concentration, low its catalytic efficiency that also affected of mass transfer rate.By titanium dichloride load in the surface of inorganic ceramic membrane, inoranic membrane, with its greatly specific area and porosity, can promote the mass transport process that it is surperficial, accelerates adsorption reaction, and then reach the organic object of enrichment, thereby increase the catalytic efficiency of titanium dioxide.In addition, Graphene has excellent electronic transport performance, mechanical performance and surface chemistry performance, and this is greatly improved the adsorption efficiency of its composite in photocatalytic process, separative efficiency and the photocatalysis efficiency of photo-generated carrier.
Summary of the invention:
The object of the invention is to overcome the defect of existing photocatalyst catalyst, utilize enrichment, the electronic transport performance of Graphene uniqueness and the doping vario-property of N element of inorganic ceramic membrane, provide that a kind of light absorption wavelength threshold value is large, catalytic efficiency is high, corrosion-resistant, resistance to cleaning, mechanical strength is large, Stability Analysis of Structures is indeformable and porous, inorganic ceramic membrane-Graphene-N modification TiO of the enrichment organic pollutants of long service life
2photocatalyst material and preparation method thereof.
The technical solution adopted in the present invention is:
This photocatalyst material is take porous, inorganic ceramic membrane as carrier, by N modification TiO
2be carried on carrier surface with the compound of Graphene; In this photocatalyst material, the mass percent of porous, inorganic ceramic membrane is 50% ~ 80%, N modification TiO
2with the mass percent of graphene complex be 20% ~ 50%; N modification TiO
2in graphene complex, Graphene and N modification TiO
2mass percent be respectively 8% ~ 10% and the atomic ratio of 90% ~ 92%, N and Ti be 2:1.
The preparation method of the photocatalyst material of described enrichment organic pollutants, concrete steps are as follows:
Step (1): be SiO by main component
2, Al
2o
3, CaO, MgO, TiO
2, K
2o and Na
2the cinder of O grinds evenly, and adding particle diameter is the blowing agent of 0.02 mm, adopts the condition dip mold moulding of semidry method at briquetting pressure 38 MPa on forcing press, is pressed into thin slice; The thin slice of compacting is calcined in Muffle furnace to 2 h under 1100 oC and obtained pulverized coal-ash-based porous potsherd, and ground, obtain porous, inorganic ceramic membrane;
Step (2): under room temperature, Graphene is put into absolute ethyl alcohol, carry out ultrasonic wave for the first time and add tetrabutyl titanate after processing, carry out again ultrasonic processing for the second time, and successively by ammonium chloride and acetic acid mixed solution and porous, inorganic ceramic membrane joining in above-mentioned solution in ultrasonic processing procedure for the second time; Ultrasonic processing until the appearance of colloidal sol stop, and under room temperature condition aging a couple of days;
Step (3): the aged samples that step (2) is obtained is dried, roasting, obtains described photocatalyst material, and in the photocatalyst material obtaining, the mass percent of porous, inorganic ceramic membrane is 50% ~ 80%, N modification TiO
2with the mass percent of graphene complex be 20% ~ 50%; N modification TiO
2in graphene complex, Graphene and N modification TiO
2mass percent be respectively 8% ~ 10% and the atomic ratio of 90% ~ 92%, N and Ti be 2:1.
The grinding particle diameter of the flyash in described step (1) is 0.06 mm ~ 0.09 mm; Blowing agent be wood chip and consumption account for cinder and blowing agent gross mass 10%; After calcining, the grinding particle diameter of thin slice is 0.1 mm ~ 0.3 mm.
In described step (2), the ultrasonic processing time is 15 min for the first time, and secondary ultrasonic processing time is 30 min.
Being dried as common air dry oven in described step (3) is dry, and baking temperature is 80 oC, and be 10 h drying time; Roasting is carried out under nitrogen atmosphere, and sintering temperature is 550 oC, and roasting time is 1.5 h.
Beneficial effect of the present invention is:
Porous, inorganic ceramic membrane take thermal power plant's flyash as raw material, wood chip is blowing agent, preparation cost is low, and can recycle refuse.The photocatalyst material of preparing take porous, inorganic ceramic membrane as carrier, its loose structure can promote surperficial mass transport process, has accelerated adsorption reaction, and its great specific area, can make the organic matter in water body be enriched in its surface, thereby increase organic conversion ratio.Graphene possesses excellent electronic transport performance, mechanical performance and surface chemistry performance, and this is greatly improved the adsorption efficiency of its composite in photocatalytic process, separative efficiency and the photocatalysis efficiency of photo-generated carrier.In addition,, after mixing nonmetalloid N, improved TiO
2photoresponse scope, and expand to visible light wave range, reduce the compound of electronics and hole, its photocatalytic activity further improves.
The specific embodiment:
The invention provides a kind of porous, inorganic ceramic membrane-Graphene-N modification TiO
2photocatalyst material and preparation method thereof, is further elaborated the present invention below by specific embodiment.
Percentage composition in following example is weight percentage if no special instructions.
Embodiment 1
A kind of porous, inorganic ceramic membrane-Graphene-N modification TiO
2photocatalyst material, its preparation method is as follows:
Step (1): be SiO by main component
2, Al
2o
3, CaO, MgO, TiO
2, K
2o and Na
2the cinder of O is ground to 0.06 mm ~ 0.09 mm, and adding 10 wt.% particle diameters is the wood chip of 0.02 mm, and on forcing press, adopting semidry method is the condition dip mold moulding of 38 MPa in briquetting pressure, is pressed into the thin slice of φ 10 × 5 mm; The thin slice of compacting is calcined in Muffle furnace to 2 h under 1100 oC and obtained pulverized coal-ash-based porous potsherd, and be ground to particle diameter 0.1 mm ~ 0.3 mm.
Step (2): under room temperature, 0.80 g Graphene is put into absolute ethyl alcohol, add 38.38 g tetrabutyl titanates after ultrasonic processing 15 min, again ultrasonic processing 30 min.Successively by appropriate acetic acid and 12.07 g NH
4cl mixed solution and 10.00 g inoranic membranes join in above-mentioned solution in ultrasonic processing.Ultrasonic processing is until the appearance of colloidal sol.Aging a couple of days under room temperature condition.
Step (3): the aged samples that step (2) is obtained is placed under common air dry oven 80 oC and is dried 550 oC roasting 1.5 h under 10 h, Muffle furnace nitrogen atmosphere, obtains N modified inorganic film/Graphene/TiO
2photocatalyst material (inoranic membrane and N modified inorganic film/Graphene/TiO
2the mass percent of compound is respectively 50% and 50%.N modification TiO
2in/graphene complex, Graphene and TiO
2mass percent be respectively 8% and the atomic ratio of 92%, N and Ti be 2:1).
Adopting organophosphorus pesticide is target degradation product, is that light source has been investigated N modified inorganic film/Graphene/TiO respectively with ultraviolet ray (wavelength: 254 nm, 365 nm), visible ray
2the photocatalytic activity of photocatalyst material.Result shows: under air and nitrogen atmosphere, under this catalyst action, the conversion ratio of organophosphorus pesticide is all higher, and after result shows to mix nonmetalloid N, in visible light wave range, its catalytic rate is also higher.
Embodiment 2
A kind of porous, inorganic ceramic membrane-Graphene-N modification TiO
2photocatalyst material, its preparation method is as follows:
Step (1): be SiO by main component
2, Al
2o
3, CaO, MgO, TiO
2, K
2o and Na
2the cinder of O is ground to 0.06 mm ~ 0.09 mm, and adding 10 wt.% particle diameters is the wood chip of 0.02 mm, and on forcing press, adopting semidry method is the condition dip mold moulding of 38 MPa in briquetting pressure, is pressed into the thin slice of φ 10 × 5 mm; The thin slice of compacting is calcined in Muffle furnace to 2 h under 1100 oC and obtained pulverized coal-ash-based porous potsherd, and be ground to particle diameter 0.1 mm ~ 0.3 mm.
Step (2): under room temperature, 0.72 g Graphene is put into absolute ethyl alcohol, add 30.37 g tetrabutyl titanates after ultrasonic processing 15 min, again ultrasonic processing 30 min.Successively by appropriate acetic acid and 9.56 g NH
4cl mixed solution and 12.00 g inoranic membranes join in above-mentioned solution in ultrasonic processing.Ultrasonic processing is until the appearance of colloidal sol.Aging a couple of days under room temperature condition.
Step (3): the aged samples that step (2) is obtained is placed under common air dry oven 80 oC and is dried 550 oC roasting 1.5 h under 10 h, Muffle furnace nitrogen atmosphere, obtains N modified inorganic film/Graphene/TiO
2photocatalyst material (inoranic membrane and N modified inorganic film/Graphene/TiO
2the mass percent of compound is respectively 60% and 40%.N modification TiO
2in/graphene complex, Graphene and TiO
2mass percent be respectively 9% and the atomic ratio of 91%, N and Ti be 2:1).
Adopting organophosphorus pesticide is target degradation product, is that light source has been investigated N modified inorganic film/Graphene/TiO respectively with ultraviolet ray (wavelength: 254 nm, 365 nm), visible ray
2the photocatalytic activity of photocatalyst material.Result shows: under air and nitrogen atmosphere, under this catalyst action, the conversion ratio of organophosphorus pesticide is all higher, and after result shows to mix nonmetalloid N, in visible light wave range, its catalytic rate is also higher.
Embodiment 3
A kind of porous, inorganic ceramic membrane-Graphene-N modification TiO
2photocatalyst material, its preparation method is as follows:
Step (1): be SiO by main component
2, Al
2o
3, CaO, MgO, TiO
2, K
2o, Na
2the cinder of O is ground to 0.06 mm ~ 0.09 mm, and adding 10 wt.% particle diameters is the wood chip of 0.02 mm, and on forcing press, adopting semidry method is the condition dip mold moulding of 38 MPa in briquetting pressure, is pressed into the thin slice of φ 10 × 5 mm; The thin slice of compacting is calcined in Muffle furnace to 2 h under 1100 oC and obtained pulverized coal-ash-based porous potsherd, and be ground to particle diameter 0.1 mm ~ 0.3 mm.
Step (2): under room temperature, 0.60 g Graphene is put into absolute ethyl alcohol, add 22.53 g tetrabutyl titanates after ultrasonic processing 15 min, again ultrasonic processing 30 min.Successively by appropriate acetic acid and 7.09 g NH
4cl mixed solution and 14.00 g inoranic membranes join in above-mentioned solution in ultrasonic processing.Ultrasonic processing is until the appearance of colloidal sol.Aging a couple of days under room temperature condition.
Step (3): the aged samples that step (2) is obtained is placed under common air dry oven 80 oC and is dried 550 oC roasting 1.5 h under 10 h, Muffle furnace nitrogen atmosphere, obtains N modified inorganic film/Graphene/TiO
2photocatalyst material (inoranic membrane and N modified inorganic film/Graphene/TiO
2the mass percent of compound is respectively 70% and 30%.N modification TiO
2in/graphene complex, Graphene and TiO
2mass percent be respectively 10% and the atomic ratio of 90%, N and Ti be 2:1).
Adopting organophosphorus pesticide is target degradation product, is that light source has been investigated N modified inorganic film/Graphene/TiO respectively with ultraviolet ray (wavelength: 254 nm, 365 nm), visible ray
2the photocatalytic activity of photocatalyst material.Result shows: under air and nitrogen atmosphere, under this catalyst action, the conversion ratio of organophosphorus pesticide is all higher, and after result shows to mix nonmetalloid N, in visible light wave range, its catalytic rate is also higher.
Claims (4)
1. porous, inorganic ceramic membrane-Graphene-N modification TiO
2the preparation method of photocatalyst material, this material is take porous, inorganic ceramic membrane as carrier, by N modification TiO
2be carried on carrier surface with the compound of Graphene; In this photocatalyst material, the mass percent of porous, inorganic ceramic membrane is 50%～80%, N modification TiO
2with the mass percent of graphene complex be 20%～50%; N modification TiO
2in graphene complex, Graphene and N modification TiO
2mass percent be respectively 8%～10% and the atomic ratio of 90%～92%, N and Ti be 2:1;
It is characterized in that, concrete preparation process is as follows:
Step (1): be SiO by main component
2, Al
2o
3, CaO, MgO, TiO
2, K
2o and Na
2the cinder of O grinds evenly, and adding particle diameter is the blowing agent of 0.02mm, adopts the condition dip mold moulding of semidry method at briquetting pressure 38MPa on forcing press, is pressed into thin slice; The thin slice of compacting is calcined in Muffle furnace to 2h at 1100 ℃ and obtained pulverized coal-ash-based porous potsherd, and ground, obtain porous, inorganic ceramic membrane;
Step (2): under room temperature, Graphene is put into absolute ethyl alcohol, carry out ultrasonic wave for the first time and add tetrabutyl titanate after processing, carry out again ultrasonic processing for the second time, and successively by ammonium chloride and acetic acid mixed solution and porous, inorganic ceramic membrane joining in above-mentioned solution in ultrasonic processing procedure for the second time; Ultrasonic processing until the appearance of colloidal sol stop, and under room temperature condition aging a couple of days;
Step (3): the aged samples that step (2) is obtained is dried, roasting, obtains described photocatalyst material, and in the photocatalyst material obtaining, the mass percent of porous, inorganic ceramic membrane is 50%～80%, N modification TiO
2with the mass percent of graphene complex be 20%～50%; N modification TiO
2in graphene complex, Graphene and N modification TiO
2mass percent be respectively 8%～10% and the atomic ratio of 90%～92%, N and Ti be 2:1.
2. porous, inorganic ceramic membrane-Graphene-N modification TiO according to claim 1
2the preparation method of photocatalyst material, is characterized in that, the grinding particle diameter of the flyash in described step (1) is 0.06mm～0.09mm; Blowing agent be wood chip and consumption account for cinder and blowing agent gross mass 10%; After calcining, the grinding particle diameter of thin slice is 0.1mm～0.3mm.
3. porous, inorganic ceramic membrane-Graphene-N modification TiO according to claim 1
2the preparation method of photocatalyst material, is characterized in that, in described step (2), the ultrasonic processing time is 15min for the first time, and secondary ultrasonic processing time is 30min.
4. porous, inorganic ceramic membrane-Graphene-N modification TiO according to claim 1
2the preparation method of photocatalyst material, is characterized in that, being dried as common air dry oven in described step (3) is dry, and baking temperature is 80 ℃, and be 10h drying time; Roasting is carried out under nitrogen atmosphere, and sintering temperature is 550 ℃, and roasting time is 1.5h.
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| CN104944794B (en) * | 2015-06-04 | 2018-04-17 | 华东理工大学 | One kind prepares graphene SiO2The method of anti-reflection film |
| CN108249655B (en) * | 2018-02-02 | 2021-07-06 | 上海师范大学 | Rotary type photocatalysis-adsorption-membrane separation synergistic reaction device |
| CN110980681B (en) * | 2019-11-07 | 2021-06-01 | 河北科技大学 | Na3Mg3(PO4)3MgO photocatalytic material, preparation method and application |
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| CN101890344A (en) * | 2010-07-27 | 2010-11-24 | 华东理工大学 | Preparation method of graphene/titanium dioxide composite photocatalyst |
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| CN101890344A (en) * | 2010-07-27 | 2010-11-24 | 华东理工大学 | Preparation method of graphene/titanium dioxide composite photocatalyst |
| CN102127750A (en) * | 2011-03-01 | 2011-07-20 | 哈尔滨工程大学 | Method for preparing graphene material based on chemical deposition |
| CN102225330A (en) * | 2011-04-20 | 2011-10-26 | 东南大学 | Method for preparing photochemical catalyst/graphene one-dimensional nuclear shell compound structure by using photochemical catalysis method |
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