CN102139220A - Photocatalyst as well as preparation method and application thereof - Google Patents

Photocatalyst as well as preparation method and application thereof Download PDF

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CN102139220A
CN102139220A CN2010101067867A CN201010106786A CN102139220A CN 102139220 A CN102139220 A CN 102139220A CN 2010101067867 A CN2010101067867 A CN 2010101067867A CN 201010106786 A CN201010106786 A CN 201010106786A CN 102139220 A CN102139220 A CN 102139220A
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cdx
catalyst
film material
porous ceramic
ceramic film
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孟庆波
范玉尊
李冬梅
邓明晖
张全新
罗艳红
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Institute of Physics of CAS
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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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/542—Dye sensitized solar cells
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

The invention provides an improved photocatalyst which contains calcined CdX or a complex containing the CdX, wherein X is S, Se or Te. The invention further provides a method for preparing the improved photocatalyst provided by the invention, which comprises the step of: a, calcining the CdX or the complex containing the CdX at 300-500 DEG C under an oxygen-containing atmosphere for 5-180 minutes to obtain the improved photocatalyst. The catalyst provided by the invention can be used for the photodegradation of organic pollutants, the photocatalytic decomposition of water and the dye sensitization of a solar cell, and is greatly improved in catalytic property compared with the traditional catalysts.

Description

A kind of photochemical catalyst and its production and use
Technical field
The present invention relates to a kind of photochemical catalyst, this Preparation of catalysts method and uses thereof.
Background technology
Utilizing the curb environmental pollution key of problem (degraded and mineralising organic pollution) and solution energy problem of photocatalysis technology is to develop the visible-light-responsive photocatalyst of high catalytic activity, thereby maximally utilise solar energy, this also is the focus in the present catalysis material research.The energy gap of CdX (X=S, Se and Te) and solar spectrum are finely overlapping, therefore, can effectively utilize sunshine as the visible-light response type catalyst, and be used to photocatalysis degradation organic contaminant and photocatalytic hydrogen production by water decomposition.But, at " Prog.Inorg.Chem. " magazine 1994,41:21-144 and " J.Electrochem.Soc. " magazine 1983,130:28-33 have disclosed because there is serious photoetch phenomenon in CdX (X=S, Se and Te), promptly along with the carrying out of light-catalyzed reaction, X 2-(X=S, Se and Te) is oxidized to simple substance X (X=S, Se and Te) by photohole, hindered further carrying out of reaction, makes and the very fast decline of catalytic performance therefore, limited it separately as Application of Catalyst.At present, at " J.Phys.Chem.B " magazine 1997,101:5010-5017 and " J.Phys.Chem. " magazine 1985,89:1327-1329 disclose to adopt by add the electron donor method in reaction system and have suppressed photoetch; At " J.Phys.Chem.C " magazine 2009,113:6327-6359 and " Chem.Commun. " magazine 2009,3452-3454 discloses the method with the compound inhibition photoetch of the photochemical catalyst of other broad-band gap; At " Int.J.HydrogenEnergy " magazine 1998,23:427-4383 discloses that (Te) method such as surface deposition metal platinum suppresses photoetch for X=S, Se, thereby improves the method for photocatalysis performance at CdX.CdS can be used for DSSC as sensitizer simultaneously." Appl.Phys.Lett " magazine 2007,91:053503 and " Electrochem.Commun " magazine 2010,12:327-330 has reported the quantum dot sensitized TiO with CdS 2The light anode, and got electricity conversion preferably.
The present invention proposes a kind of modified photochemical catalyst, this Preparation of catalysts method and application, and this modified photochemical catalyst can suppress the photoetch effect.
Summary of the invention
An object of the present invention is to provide a kind of photochemical catalyst, this catalyst can resist the photoetch effect, catalytic performance height in light-catalyzed reaction.
Another object of the present invention provides the preparation method of photochemical catalyst of the present invention.
A further object of the present invention provides a kind of method of degradable organic pollutant, and this method is used photochemical catalyst of the present invention.
A further object of the present invention provides a kind of method of photochemical catalyzing, and this method is used photochemical catalyst of the present invention.
A further object of the present invention provides the application of described photochemical catalyst in the preparation DSSC.
One aspect of the present invention provides a kind of photochemical catalyst, the consisting of through the CdX of calcination processing or contain the compound of CdX of this catalyst, and wherein X is S, Se or Te.Photochemical catalyst CdX is that commercially available reagent is analyzed pure or analyzed pure above or adopt chemical method synthetic.
Preferably, the compound of the described CdX of containing is the compound that CdX and porous ceramic film material form.
Preferably, described porous ceramic film material is molecular sieve, Woelm Alumina or titanium dioxide.
The present invention also provides a kind of method for preparing photochemical catalyst of the present invention on the other hand, the method comprising the steps of a: CdX or the compound that contains CdX containing under the atmosphere of oxygen 300-500 ℃ of calcining 5-180 minute, are obtained described photochemical catalyst.
Preferably, 350-450 ℃ of calcining 30-120 minute.
Most preferably, 400 ℃ of calcinings 60 minutes.
Preferably, the gas flow rate that contains under the oxygen atmosphere is 5-800mL/min.
Preferably, at first CdX is mixed also fully grinding with solvent flashing and carry out step a again.
More preferably, described solvent flashing is an ethanol.
Preferably, at first CdX is loaded on the porous ceramic film material, form the compound that contains CdX, carry out step a again.
Preferably, the mass ratio of CdX and porous ceramic film material is 1: 5-20.
More preferably, the mass ratio of CdX and porous ceramic film material is 1: 5-10.
Most preferably, the mass ratio of CdX and porous ceramic film material is 1: 10.
Further aspect of the present invention also provides a kind of method of degradable organic pollutant, and this method is used photochemical catalyst of the present invention.
Preferably, described organic pollution comprises one or more in methylene blue, methyl orange, rhodamine B and the methyl red.
Most preferably, described organic pollution is a methylene blue.
Further aspect of the present invention also provides the method for photochemical catalyzing, and this method is used photochemical catalyst of the present invention.
Further aspect of the present invention also provides the application of photochemical catalyst of the present invention in the preparation DSSC.CdX (X=S, Se and Te) as sensitizer can the sensitization broad-band gap semi-conducting material (as TiO 2, ZnO etc.), when being used for DSSC, can earlier CdX be loaded on the wide bandgap semiconductor materials of porous, carry out the method for step a again and handle.
The application of the photochemical catalyst that the present invention relates on the light degradation organic pollution comprises:
Photochemical catalyst according to the inventive method preparation;
According to the conventional method that is applicable to this area photochemical catalyst, the solution that contains organic pollution and illumination apparatus are assembled light-catalyzed reaction.
Compare with existing photochemical catalyst and treatment process technology, the photochemical catalyst that this type of was handled and the characteristics of treatment process are:
(1) surface of photochemical catalyst of the present invention has formed skim CdO, helps continuing in light-catalyzed reaction and carries out.The CdS of calcination processing of the present invention is in the reaction of catalytic degradation methylene blue, and the degradation rate of 5 hours methylene blues reaches more than 95%; The CdSe of calcination processing of the present invention is in the reaction of catalytic degradation methylene blue, and the degradation rate of 5 hours methylene blues reaches more than 94%; The CdTe of calcination processing of the present invention is in the reaction of catalytic degradation methylene blue, and the degradation rate of 5 hours methylene blues reaches more than 95%; The CdS-molecular sieve based catalyst of calcination processing of the present invention is in the reaction of catalytic degradation methylene blue, and the degradation rate of 5 hours methylene blues reaches more than 95%; The CdSe-Woelm Alumina of calcination processing of the present invention is catalyst based, and the degradation rate of 5 hours methylene blues reaches more than 94%; The CdTe-poriferous titanium dioxide based composite catalyst of calcination processing of the present invention, the degradation rate of 5 hours methylene blues reaches more than 94%.
(2) adopt the catalytic performance of photochemical catalyst of the present invention to be greatly enhanced.
(3) calcining heat, time range, calcination atmosphere have bigger selectivity in the processing method of modified photochemical catalyst catalytic performance of the present invention.
(4) method of modified photochemical catalyst catalytic performance of the present invention has easy, the with low cost advantage of treatment process.
Description of drawings
Fig. 1 represents the X-ray powder diffraction spectrogram through the CdS sample of 400 ℃ of calcining different times.Wherein mark # number diffraction maximum is CdO, and other is the CdS of six side's phases.
Fig. 2 represents the x-ray photoelectron spectroscopy spectrogram through 30 minutes CdS sample of 400 ℃ of calcinings.
The specific embodiment
Further describe the present invention below with reference to embodiment, following examples only are used to explain the present invention, are not used in restriction the present invention, and the appropriate combination of following examples technical scheme and variation are all in protection scope of the present invention.
Before describing the specific embodiment of the present invention, at first introduce photocatalysis performance method of testing of the present invention:
Light source is a halogen lamp, carries out under the visible light condition in order to guarantee the catalysis experiment, adopts the cut-off type optical filter to remove the following light of 420nm wavelength fully.Catalyst joined contain in the certain density organic pollution solution, constantly stir, in the illumination process, every sampling at regular intervals.Adopt ultraviolet-uisible spectrophotometer to measure solution absorbency, to define the degradation rate of organic pollutants.
Organic pollution comprises methylene blue, methyl orange, rhodamine B, methyl red etc.Mainly be that target contaminant is illustrated in the specific embodiments below with the methylene blue.
In following examples, the calcining atmosphere can adopt oxygen atmosphere, and gas flow is 5-800ml/ minute, no longer further enumerates in following examples.
Embodiment 1
(1) CdS with the 1g commodity places agate mortar, and the abundant ground and mixed of interpolation ethanol is even;
(2) raw material with mixing places crucible, carries out calcination processing (calcining heat and time see the following form) under air atmosphere, naturally cooling;
(3) light source of photocatalysis experiment employing is the 500W halogen lamp, adopts the cut-off type optical filter to remove the following light of 420nm wavelength fully, and the assurance experiment is carried out under visible light.Catalyst consumption is 0.5g/L, and the concentration of methylene blue solution is 3 * 10 -5M, in the illumination reaction process, every sampling is at regular intervals measured solution absorbency with ultraviolet-uisible spectrophotometer, to determine the degradation rate of methylene blue.
The experimental result of above-mentioned catalyst photocatalytic degradation methylene blue sees Table 1.
Table 1 is through the performance of the CdS of the commodity of calcination processing catalyst photocatalytic degradation methylene blue
Figure GSA00000016568400051
Embodiment 2
Embodiment 2 usefulness and embodiment 1 identical method experimentizes, but with the CdSe replaced C dS of commodity.The experimental result of above-mentioned catalyst photocatalytic degradation methylene blue sees Table 2.
Table 2 is through the performance of the CdSe of the commodity of calcination processing catalyst photocatalytic degradation methylene blue
Figure GSA00000016568400052
Figure GSA00000016568400061
Embodiment 3
Embodiment 3 usefulness and embodiment 1 identical method experimentizes, but with the CdTe replaced C dS of commodity.The experimental result of above-mentioned catalyst photocatalytic degradation methylene blue sees Table 3.
Table 3 is through the performance of the CdTe of the commodity of calcination processing catalyst photocatalytic degradation methylene blue
Figure GSA00000016568400071
Embodiment 4
(1) measures the 90mM Cd (NO of equal volume amounts 3) 24H 2O, 90mM (NH 2) 2CS transfers in the reactor that volume is 80ml, and filling degree is 80%, in 200 ℃ of hydro-thermal reaction 4h, and cooling naturally, filtration washing.
(2) above-mentioned synthetic CdS is placed agate mortar, the abundant ground and mixed of interpolation ethanol is even;
(3) raw material with mixing places crucible, carries out calcination processing (calcining heat and time see the following form) under air atmosphere, naturally cooling;
(4) light source of photocatalysis experiment employing is the 500W halogen lamp, adopts the cut-off type optical filter to remove the following light of 420nm wavelength fully, and the assurance experiment is carried out under visible light.Catalyst consumption is 0.5g/L, and the concentration of methylene blue solution is 3 * 10 -5M, in the illumination reaction process, every sampling is at regular intervals measured solution absorbency with ultraviolet-uisible spectrophotometer, to determine the degradation rate of methylene blue.The experimental result of above-mentioned catalyst photocatalytic degradation methylene blue sees Table 4.
Table 4 is through the performance of the synthetic CdS catalyst photocatalytic degradation methylene blue of calcination processing
Figure GSA00000016568400081
Embodiment 5
Embodiment 5 usefulness and embodiment 4 identical methods experimentize, but use Na 2SeO 3Replace (NH 2) 2CS.The experimental result of above-mentioned catalyst photocatalytic degradation methylene blue sees Table 5.
Table 5 is through the performance of the synthetic CdSe catalyst photocatalytic degradation methylene blue of calcination processing
Figure GSA00000016568400092
Figure GSA00000016568400101
Embodiment 6
Embodiment 6 usefulness and embodiment 4 identical methods experimentize, but use Na 2TeO 3Replace (NH 2) 2CS.The experimental result of above-mentioned catalyst photocatalytic degradation methylene blue sees Table 6.
Table 6 is through the performance of the synthetic catalyst based photocatalytic degradation methylene blue of CdTe of calcination processing
Figure GSA00000016568400102
Figure GSA00000016568400111
Embodiment 7
(1) takes by weighing isopyknic 90mM Cd (NO 3) 24H 2O, 90mM (NH 2) 2CS transfers in the reactor that volume is 80ml, and filling degree is 80%, and the apparent mass ratio certain according to CdS and molecular sieve M adds molecular sieve, in 200 ℃ of hydro-thermal reaction 4h, and cooling naturally, filtration washing.
(2) above-mentioned synthetic CdS-M is placed crucible, under air atmosphere, carry out calcination processing (calcining heat and time see the following form), naturally cooling.
(3) light source of photocatalysis experiment employing is the 500W halogen lamp, adopts the cut-off type optical filter to remove the following light of 420nm wavelength fully, and the assurance experiment is carried out under visible light.Catalyst consumption is 0.5g/L, and the concentration of methylene blue solution is 3 * 10 -5M, in the illumination reaction process, every sampling is at regular intervals measured solution absorbency with ultraviolet-uisible spectrophotometer, to determine the degradation rate of methylene blue.The experimental result of above-mentioned catalyst photocatalytic degradation methylene blue sees Table 7.
Table 7 is through the performance of the synthetic CdS-molecular sieve based catalyst photocatalytic degradation methylene blue of calcination processing
Figure GSA00000016568400112
Figure GSA00000016568400121
Figure GSA00000016568400131
Figure GSA00000016568400141
Embodiment 8
Embodiment 8 usefulness and embodiment 7 identical methods experimentize, but use Na 2SeO 3Replace (NH 2) 2CS is with Woelm Alumina substituted molecule sieve.
The experimental result of above-mentioned catalyst photocatalytic degradation methylene blue sees Table 8.
Table 8 is through the performance of the synthetic catalyst based photocatalytic degradation methylene blue of CdSe-Woelm Alumina of calcination processing
Figure GSA00000016568400142
Figure GSA00000016568400151
Figure GSA00000016568400161
Embodiment 9
Embodiment 9 usefulness and embodiment 7 identical methods experimentize, but use Na 2TeO 3Replace (NH 2) 2CS is with poriferous titanium dioxide substituted molecule sieve.
The experimental result of above-mentioned catalyst photocatalytic degradation methylene blue sees Table 9.
Table 9 is through the performance of the synthetic CdTe-poriferous titanium dioxide based composite catalyst photocatalytic degradation methylene blue of calcination processing
Figure GSA00000016568400172
Figure GSA00000016568400181
Comparative example 1
(Te) experimental result of catalyst photocatalytic degradation methylene blue sees Table 10 for X=S, Se without the CdX of the commodity of calcination processing.
Table 10 is without CdX (X=S, Se, Te) performance of catalyst photocatalytic degradation methylene blue of the commodity of calcination processing
Figure GSA00000016568400201

Claims (10)

1. photochemical catalyst, the consisting of through the CdX of calcination processing or contain the compound of CdX of this catalyst, wherein X is S, Se or Te.
2. photochemical catalyst according to claim 1, the compound of the wherein said CdX of containing are the compound that CdX and porous ceramic film material form, and preferably, described porous ceramic film material is molecular sieve, Woelm Alumina or titanium dioxide.
3. method for preparing claim 1 or 2 described photochemical catalysts, the method comprising the steps of a: CdX or the compound that contains CdX are being contained under the atmosphere of oxygen 300-500 ℃ of calcining 5-180 minute, obtain described photochemical catalyst, preferably, 350-450 ℃ of calcining 30-120 minute, most preferably, 400 ℃ of calcinings 60 minutes.
4. method according to claim 3, the gas flow rate under the wherein said atmosphere that contains oxygen is 5-800mL/min.
5. according to claim 3 or 4 described methods, wherein at first CdX is mixed also fully grinding with solvent flashing and carry out step a again, preferably, described solvent flashing is an ethanol.
6. according to claim 3 or 4 described methods, wherein at first CdX is loaded on the porous ceramic film material, form the compound that contains CdX, carry out step a again.
7. method according to claim 6, wherein the mass ratio of CdX and porous ceramic film material is 1: 5-20, preferably, the mass ratio of CdX and porous ceramic film material is 1: 5-10, most preferably, the mass ratio of CdX and porous ceramic film material is 1: 10.
8. the method for a degradable organic pollutant, it is characterized in that, this method is used claim 1 or 2 described photochemical catalysts, preferably, described organic pollution comprises one or more in methylene blue, methyl orange, rhodamine B and the methyl red, most preferably, described organic pollution is a methylene blue.
9. the method for a photochemical catalyzing is characterized in that, this method is used claim 1 or 2 described photochemical catalysts.
10. claim 1 or the 2 described photochemical catalysts application in the preparation DSSC.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103055943A (en) * 2012-12-18 2013-04-24 华南理工大学 Dye-sensitization photocatalysis and application thereof in catalytic degradation of ionic liquid under the present of visible light
CN108914188A (en) * 2018-07-23 2018-11-30 西南大学 Nano-tube array/nanometer filament composite structure, preparation method, quantum dot sensitized composite construction and application
CN111621297A (en) * 2020-06-17 2020-09-04 南通创亿达新材料股份有限公司 Cadmium selenide quantum dot and solid-phase preparation method thereof
CN112038096A (en) * 2020-09-28 2020-12-04 湖南艾华集团股份有限公司 Ripple current resistant solid-state aluminum electrolytic capacitor and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103055943A (en) * 2012-12-18 2013-04-24 华南理工大学 Dye-sensitization photocatalysis and application thereof in catalytic degradation of ionic liquid under the present of visible light
CN103055943B (en) * 2012-12-18 2015-06-03 华南理工大学 Dye-sensitization photocatalysis and application thereof in catalytic degradation of ionic liquid under the present of visible light
CN108914188A (en) * 2018-07-23 2018-11-30 西南大学 Nano-tube array/nanometer filament composite structure, preparation method, quantum dot sensitized composite construction and application
CN111621297A (en) * 2020-06-17 2020-09-04 南通创亿达新材料股份有限公司 Cadmium selenide quantum dot and solid-phase preparation method thereof
CN112038096A (en) * 2020-09-28 2020-12-04 湖南艾华集团股份有限公司 Ripple current resistant solid-state aluminum electrolytic capacitor and preparation method thereof

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Application publication date: 20110803