CN102744091A - 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 PDF

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CN102744091A
CN102744091A CN2012102124230A CN201210212423A CN102744091A CN 102744091 A CN102744091 A CN 102744091A CN 2012102124230 A CN2012102124230 A CN 2012102124230A CN 201210212423 A CN201210212423 A CN 201210212423A CN 102744091 A CN102744091 A CN 102744091A
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graphene
ceramic membrane
inorganic ceramic
porous
photocatalyst material
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CN102744091B (en
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覃吴
董长青
石司默
张媛媛
杨勇平
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North China Electric Power University
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North China Electric Power University
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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
    • 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

Porous, inorganic ceramic membrane-Graphene-N modification TiO 2Photocatalyst material and preparation method thereof
Technical field:
The invention belongs to the 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 application photocatalyst material the most widely, TiO 2Played the part of the key player at aspects such as environmental pollution improvement and solar energy utilizations.At present, at TiO 2Aspects such as preparation very big breakthrough has been arranged, but since its energy gap be 3.2 eV (anatase, Anatase), can only absorbing wavelength less than the ultraviolet light of 400 nm, photocatalysis efficiency is very low.Therefore, a lot of scientists concentrate on TiO with the emphasis of research 2The visible light modification with improve on the catalytic efficiency.
The present invention adopts sol-gel process, is synthetic pure inoranic membrane/Graphene of the mixing N/TiO of the uniform high activity of particle size dispersion of precursor with the tetrabutyl titanate 2Organic pollution photocatalyst material in the water-enriched.Mix after the nonmetalloid N, improved TiO 2The photoresponse 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 the sewage is low in its surface concentration, low its catalytic efficiency that also influenced of mass transfer rate.With the surface of titanium dichloride load in inorganic ceramic membrane; Inoranic membrane can promote the mass transport process that it is surperficial with its greatly specific area and porosity, accelerates the surface adsorption reaction; And then reach the organic purpose 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 makes the adsorption efficiency of its composite in photocatalytic process, the separative efficiency and the photocatalysis efficiency of photo-generated carrier be greatly improved.
Summary of the invention:
The objective of the invention is to overcome the defective of existing photocatalyst catalyst; Utilize the unique electronic transport performance of the enrichment, Graphene of inorganic ceramic membrane and the doping vario-property of N element, provide that a kind of light absorption wavelength threshold value is big, catalytic efficiency is high, corrosion-resistant, anti-cleaning, mechanical strength is big, Stability Analysis of Structures is indeformable and the water-enriched of long service life in the porous, inorganic ceramic membrane-Graphene-N modification TiO of organic pollution 2Photocatalyst material and preparation method thereof.
The technical scheme that the present invention adopted is:
This photocatalyst material is a carrier with the porous, inorganic ceramic membrane, with 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 90% ~ 92%, the atomic ratio of N and Ti is 2:1.
The preparation method of the photocatalyst material of organic pollution in the described water-enriched, concrete steps are following:
Step (1): with main component is SiO 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, on forcing press, adopts the condition dip mold moulding of semidry method at briquetting pressure 38 MPa, is pressed into thin slice; The thin slice of compacting is calcined 2 h under 1100 oC promptly obtain the fly ash base porous ceramics piece in Muffle furnace, and, obtain the porous, inorganic ceramic membrane its grinding;
Step (2): under the room temperature; Graphene is put into absolute ethyl alcohol; Carry out adding tetrabutyl titanate after the ultrasonic Treatment first time; Carry out the sonicated second time again, and in sonicated process join in above-mentioned solution in the second time ammonium chloride and acetic acid mixed solution and porous, inorganic ceramic membrane successively; Sonicated stops until the appearance of colloidal sol, and wears out a couple of days down in room temperature condition;
Step (3): the aged samples to step (2) obtains is carried out drying, roasting, promptly obtains said photocatalyst material, and in the photocatalyst material that obtains, 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 90% ~ 92%, the atomic ratio of N and Ti is 2:1.
The grinding particle diameter of the flyash in the said 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%; The grinding particle diameter of calcining back thin slice is 0.1 mm ~ 0.3 mm.
The sonicated time first time is 15 min in the said step (2), and secondary sonicated time is 30 min.
Drying in the said step (3) is that common air dry oven 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:
The porous, inorganic ceramic membrane is that raw material, wood chip are blowing agent with thermal power plant's flyash, and preparation cost is low, and can recycle refuse.With the porous, inorganic ceramic membrane is the photocatalyst material of preparing carriers; Its loose structure can promote surperficial mass transport process, has accelerated the surface adsorption reaction, and its great specific area; Can make the organic matter in the 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 makes the adsorption efficiency of its composite in photocatalytic process, the separative efficiency and the photocatalysis efficiency of photo-generated carrier be greatly improved.In addition, mix after the nonmetalloid N, improved TiO 2The photoresponse 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 done further elaboration through specific embodiment to the present invention below.
Percentage composition in the following instance is weight percentage like no specified otherwise.
Embodiment 1
A kind of porous, inorganic ceramic membrane-Graphene-N modification TiO 2Photocatalyst material, its preparation method is following:
Step (1): with main component is SiO 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 2 h under 1100 oC promptly obtain the fly ash base porous ceramics piece in Muffle furnace, and it is ground to particle diameter 0.1 mm ~ 0.3 mm.
Step (2): under the room temperature, 0.80 g Graphene is put into absolute ethyl alcohol, add 38.38 g tetrabutyl titanates, sonicated 30 min once more behind sonicated 15 min.Successively with an amount of acetate and 12.07 g NH 4Cl mixed solution and 10.00 g inoranic membranes join in sonicated in the above-mentioned solution.Sonicated is until the appearance of colloidal sol.Room temperature condition wears out a couple of days down.
Step (3): the aged samples that step (2) is obtained places under common air dry oven 80 oC 550 oC roastings, 1.5 h under dry 10 h, the Muffle furnace nitrogen atmosphere, promptly 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/the graphene complex, Graphene and TiO 2Mass percent be respectively 8% and 92%, the atomic ratio of N and Ti is 2:1).
Adopting organophosphorus pesticide is the target degradation product, is that light source has been investigated N modified inorganic film/Graphene/TiO with ultraviolet ray (wavelength: 254 nm, 365 nm), visible light respectively 2The photocatalytic activity of photocatalyst material.The result shows: under air and the nitrogen atmosphere, under this catalyst action, the conversion ratio of organophosphorus pesticide is all higher, and the result shows and mix after the nonmetalloid N that its catalytic rate is also higher in the visible light wave range.
Embodiment 2
A kind of porous, inorganic ceramic membrane-Graphene-N modification TiO 2Photocatalyst material, its preparation method is following:
Step (1): with main component is SiO 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 2 h under 1100 oC promptly obtain the fly ash base porous ceramics piece in Muffle furnace, and it is ground to particle diameter 0.1 mm ~ 0.3 mm.
Step (2): under the room temperature, 0.72 g Graphene is put into absolute ethyl alcohol, add 30.37 g tetrabutyl titanates, sonicated 30 min once more behind sonicated 15 min.Successively with an amount of acetate and 9.56 g NH 4Cl mixed solution and 12.00 g inoranic membranes join in sonicated in the above-mentioned solution.Sonicated is until the appearance of colloidal sol.Room temperature condition wears out a couple of days down.
Step (3): the aged samples that step (2) is obtained places under common air dry oven 80 oC 550 oC roastings, 1.5 h under dry 10 h, the Muffle furnace nitrogen atmosphere, promptly 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/the graphene complex, Graphene and TiO 2Mass percent be respectively 9% and 91%, the atomic ratio of N and Ti is 2:1).
Adopting organophosphorus pesticide is the target degradation product, is that light source has been investigated N modified inorganic film/Graphene/TiO with ultraviolet ray (wavelength: 254 nm, 365 nm), visible light respectively 2The photocatalytic activity of photocatalyst material.The result shows: under air and the nitrogen atmosphere, under this catalyst action, the conversion ratio of organophosphorus pesticide is all higher, and the result shows and mix after the nonmetalloid N that its catalytic rate is also higher in the visible light wave range.
Embodiment 3
A kind of porous, inorganic ceramic membrane-Graphene-N modification TiO 2Photocatalyst material, its preparation method is following:
Step (1): with main component is SiO 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 2 h under 1100 oC promptly obtain the fly ash base porous ceramics piece in Muffle furnace, and it is ground to particle diameter 0.1 mm ~ 0.3 mm.
Step (2): under the room temperature, 0.60 g Graphene is put into absolute ethyl alcohol, add 22.53 g tetrabutyl titanates, sonicated 30 min once more behind sonicated 15 min.Successively with an amount of acetate and 7.09 g NH 4Cl mixed solution and 14.00 g inoranic membranes join in sonicated in the above-mentioned solution.Sonicated is until the appearance of colloidal sol.Room temperature condition wears out a couple of days down.
Step (3): the aged samples that step (2) is obtained places under common air dry oven 80 oC 550 oC roastings, 1.5 h under dry 10 h, the Muffle furnace nitrogen atmosphere, promptly 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/the graphene complex, Graphene and TiO 2Mass percent be respectively 10% and 90%, the atomic ratio of N and Ti is 2:1).
Adopting organophosphorus pesticide is the target degradation product, is that light source has been investigated N modified inorganic film/Graphene/TiO with ultraviolet ray (wavelength: 254 nm, 365 nm), visible light respectively 2The photocatalytic activity of photocatalyst material.The result shows: under air and the nitrogen atmosphere, under this catalyst action, the conversion ratio of organophosphorus pesticide is all higher, and the result shows and mix after the nonmetalloid N that its catalytic rate is also higher in the visible light wave range.

Claims (5)

1. porous, inorganic ceramic membrane-Graphene-N modification TiO 2Photocatalyst material is characterized in that, is carrier with the porous, inorganic ceramic membrane, with 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 90% ~ 92%, the atomic ratio of N and Ti is 2:1.
2. the described porous, inorganic ceramic membrane-Graphene of claim 1-N modification TiO 2The preparation method of photocatalyst material is characterized in that, concrete steps are following:
Step (1): with main component is SiO 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, on forcing press, adopts the condition dip mold moulding of semidry method at briquetting pressure 38 MPa, is pressed into thin slice; The thin slice of compacting is calcined 2 h under 1100 oC promptly obtain the fly ash base porous ceramics piece in Muffle furnace, and, obtain the porous, inorganic ceramic membrane its grinding;
Step (2): under the room temperature; Graphene is put into absolute ethyl alcohol; Carry out adding tetrabutyl titanate after the ultrasonic Treatment first time; Carry out the sonicated second time again, and in sonicated process join in above-mentioned solution in the second time ammonium chloride and acetic acid mixed solution and porous, inorganic ceramic membrane successively; Sonicated stops until the appearance of colloidal sol, and wears out a couple of days down in room temperature condition;
Step (3): the aged samples to step (2) obtains is carried out drying, roasting, promptly obtains said photocatalyst material, and in the photocatalyst material that obtains, 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 90% ~ 92%, the atomic ratio of N and Ti is 2:1.
3. porous, inorganic ceramic membrane-Graphene according to claim 2-N modification TiO 2The preparation method of photocatalyst material is characterized in that, the grinding particle diameter of the flyash in the said 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%; The grinding particle diameter of calcining back thin slice is 0.1 mm ~ 0.3 mm.
4. porous, inorganic ceramic membrane-Graphene according to claim 2-N modification TiO 2The preparation method of photocatalyst material is characterized in that, the sonicated time first time is 15 min in the said step (2), and secondary sonicated time is 30 min.
5. porous, inorganic ceramic membrane-Graphene according to claim 2-N modification TiO 2The preparation method of photocatalyst material is characterized in that, the drying in the said step (3) is that common air dry oven 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.
CN201210212423.0A 2012-06-21 2012-06-21 Porous inorganic ceramic membrane-graphene-N modified TiO2 photocatalyst material and preparation method thereof Expired - Fee Related CN102744091B (en)

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CN110980681A (en) * 2019-11-07 2020-04-10 河北科技大学 Na3Mg3(PO4)3MgO photocatalytic material, preparation method and application

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Cited By (5)

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CN110980681A (en) * 2019-11-07 2020-04-10 河北科技大学 Na3Mg3(PO4)3MgO photocatalytic material, preparation method and application

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