CN113908822A - (BiO)2OHCl/La(OH)3Preparation method and application of composite visible-light-driven photocatalyst - Google Patents
(BiO)2OHCl/La(OH)3Preparation method and application of composite visible-light-driven photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims description 41
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- 239000008367 deionised water Substances 0.000 claims abstract description 70
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- 238000000967 suction filtration Methods 0.000 claims abstract description 63
- 238000003756 stirring Methods 0.000 claims abstract description 57
- 239000003054 catalyst Substances 0.000 claims abstract description 51
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 238000002360 preparation method Methods 0.000 claims abstract description 43
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 37
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- 238000001035 drying Methods 0.000 claims abstract description 36
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- 238000001914 filtration Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 67
- -1 polytetrafluoroethylene Polymers 0.000 claims description 35
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 34
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 34
- 238000005406 washing Methods 0.000 claims description 34
- 230000008569 process Effects 0.000 claims description 31
- 230000007935 neutral effect Effects 0.000 claims description 28
- 239000002351 wastewater Substances 0.000 claims description 20
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- XMEVHPAGJVLHIG-FMZCEJRJSA-N chembl454950 Chemical compound [Cl-].C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H]([NH+](C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O XMEVHPAGJVLHIG-FMZCEJRJSA-N 0.000 claims description 12
- 229960004989 tetracycline hydrochloride Drugs 0.000 claims description 12
- 230000003115 biocidal effect Effects 0.000 claims description 8
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- 230000001699 photocatalysis Effects 0.000 description 8
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 description 6
- 238000000926 separation method Methods 0.000 description 5
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- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
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- 229940073609 bismuth oxychloride Drugs 0.000 description 2
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/18—Arsenic, antimony or bismuth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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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
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Abstract
The invention provides a (BiO)2OHCl/La(OH)3The preparation method and the application of the composite visible-light-driven photocatalyst comprise the following steps: to La (NO)3)3Adding deionized water into the solid, adding concentrated ammonia water to adjust pH to 10, transferring the stirred solution into a reaction kettle, keeping at high temperature for 12h, naturally cooling to room temperature, performing suction filtration, taking out a sample, and drying to obtain La (OH)3A sample; to Bi (NO)3)3Adding deionized water and KCl into the solid, adding concentrated ammonia water to adjust pH to 10, stirring, adding La (OH)3Transferring the stirred solution into a reaction kettle, keeping at high temperature for 12h, naturally cooling to room temperature, filtering, taking out the sample, and drying to obtain (BiO)2OHCl/La(OH)3And compounding the visible light catalyst. Hair brushThe pressure of waste treatment and environmental pollution can be obviously reduced, and the high-efficiency catalytic degradation of the industrial wastewater is realized.
Description
Technical Field
The invention relates to the technical field of photocatalysis, in particular to a (BiO)2OHCl/La(OH)3A preparation method and application of the composite visible-light-driven photocatalyst.
Background
With the rapid development of industry, the discharge amount of various industrial waste water is rapidly increased, so that the problems of water environment and water resource pollution are severe, and the health and safety of human beings are threatened. Among them, organic pollutants in wastewater have characteristics of high toxicity, chemical stability, difficulty in biodegradation and the like, and can absorb and reflect sunlight entering water to interfere growth of organisms such as bacteria and the like, thereby causing serious harm to ecological environment. Therefore, how to efficiently treat organic pollutants in industrial wastewater becomes a difficult problem to be solved urgently in the technical field of domestic and foreign environmental protection.
The photocatalysis technology has the advantages of low cost, simple operation, mild reaction conditions, no secondary pollution and the like, is a green environment-friendly technology, and shows great potential in the degradation of organic pollutants in wastewater. However, the degradation efficiency of the traditional photocatalyst on the organic pollutants in the actual wastewater under the condition of visible light is far from satisfactory, and the preparation of a novel high-efficiency catalyst with visible light catalytic activity is still the focus of the current researchers.
In recent years, doping of hydroxyl groups into bismuth oxychloride (BiOCl) to form (BiO)2OHCl has attracted considerable interest to researchers as a new photocatalytic material and has been the focus of research. Specifically, (BiO)2OHCL is an indirect bandgap semiconductor with a highly anisotropic layer structure (i.e., a layer of [ Bi ]2O2]2+Sandwiched between two layers [ Cl2]2-In crystals) and both of these advantages contribute to the effective separation of the photo-generated electron-hole (e-h +) pairs, so that the photo-catalytic activity is outstanding. The research finds that: (BiO)2The degradation activity of OHCl to organic pollutants is better than that of TiO2(P25, Degussa); meanwhile, (BiO)2OHCl has the advantages of being non-toxic, low in cost, and the like, and thus has attracted much attention in the field of photocatalysis.
(BiO)2OHCl band gap (Eg) is around 3.5eV, which can only be excited by UV light. Researchers try to expand the photoresponse range of the solar cell by adopting various modification means, such as precious metal deposition, cocatalyst loading, rare earth ion doping and the like, so that the solar utilization rate of the solar cell is improved. However, the above modification methods generally have the disadvantages of high cost, complicated preparation process, and the like. Based on this, there is a need to develop a new visible light response type (BiO) with low cost, simple preparation process and no environmental pollution2OHCl composite photocatalytic material.
Disclosure of Invention
Based on this, the object of the invention is to propose a (BiO)2OHCl/La(OH)3Preparation method of composite visible light catalyst to prepare novel (BiO)2OHCl/La(OH)3The composite visible light catalyst meets the application requirement of actual photocatalytic degradation.
The invention provides a (BiO)2OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst comprises the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding deionized water into the solid, adding concentrated ammonia water to adjust pH to 10, transferring the solution after continuous stirring into a polytetrafluoroethylene reaction kettle, keeping the solution at high temperature for 12h, naturally cooling the product to room temperature, performing suction filtration, repeatedly washing the product with deionized water and ethanol to neutrality in the suction filtration process, taking out the sample, and drying the sample at 60 ℃ for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to Bi (NO)3)3Adding deionized water and KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring, and adding the La (OH) prepared in the step one3Transferring the solution obtained after continuous stirring into a polytetrafluoroethylene reaction kettle, keeping for 12h at high temperature, performing suction filtration after the product is naturally cooled to room temperature, and performing suction filtration by using deionized water and BRepeatedly washing with alcohol to neutral, taking out sample, and drying at 60 deg.C to obtain (BiO)2OHCl/La(OH)3And compounding the visible light catalyst.
The invention provides a (BiO)2OHCl/La(OH)3The preparation method of the composite visible light catalyst comprises the steps of firstly preparing La (OH)3Sample, in particular, to La (NO)3)3Adding deionized water into the solid, adding concentrated ammonia water to adjust pH to 10, transferring the solution after continuous stirring into a polytetrafluoroethylene reaction kettle, keeping the solution at high temperature for 12h, naturally cooling the product to room temperature, performing suction filtration, repeatedly washing the product with deionized water and ethanol to neutrality in the suction filtration process, taking out the sample, and drying the sample at 60 ℃ for 12h to obtain La (OH)3A sample; then preparing to obtain (BiO)2OHCl/La(OH)3Composite visible light catalyst, in particular, to Bi (NO)3)3Adding deionized water and KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring, and adding the La (OH) prepared in the step one3Transferring the solution obtained after continuous stirring into a polytetrafluoroethylene reaction kettle, keeping the solution at high temperature for 12 hours, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing the product to be neutral by deionized water and ethanol in the suction filtration process, taking out the sample, and drying the sample at 60 ℃ to obtain (BiO)2OHCl/La(OH)3And compounding the visible light catalyst. Prepared by the invention (BiO)2OHCl/La(OH)3The composite visible light catalyst has low cost, simple preparation process and no environmental pollution, and has good degradation effect on tetracycline hydrochloride-containing antibiotic wastewater and organic pollutant-containing industrial wastewater.
The (BiO)2OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst comprises the step one and the step two, wherein the concentration of the added concentrated ammonia water is 10-14 mol/L.
The (BiO)2OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst comprises the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding 20ml of deionized water into the solid, adding concentrated ammonia water to adjust the pH value to 10, transferring the solution after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing the product to be neutral by using the deionized water and ethanol in the suction filtration process, taking out a sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to 0.97g of Bi (NO)3)3Adding 20mL of deionized water and 2mmol of KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring for 5min, and adding 0.05g of La (OH) prepared in the first step3Transferring the solution obtained after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to the room temperature, repeatedly washing the product to be neutral by deionized water and ethanol in the suction filtration process, taking out the sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain (BiO)2OHCl/La(OH)3And compounding the visible light catalyst.
The (BiO)2OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst comprises the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding 20ml of deionized water into the solid, adding concentrated ammonia water to adjust the pH value to 10, transferring the solution after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing the product to be neutral by using the deionized water and ethanol in the suction filtration process, taking out a sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to 0.97g of Bi (NO)3)3Adding in solidAdding 20mL of deionized water and 2mmol of KCl, adding concentrated ammonia water to adjust the pH to 10, stirring for 5min, and adding 0.1g of La (OH) prepared in the first step3Transferring the solution obtained after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to the room temperature, repeatedly washing the product to be neutral by deionized water and ethanol in the suction filtration process, taking out the sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain (BiO)2OHCl/La(OH)3And compounding the visible light catalyst.
The (BiO)2OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst comprises the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding 20ml of deionized water into the solid, adding concentrated ammonia water to adjust the pH value to 10, transferring the solution after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing the product to be neutral by using the deionized water and ethanol in the suction filtration process, taking out a sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to 0.97g of Bi (NO)3)3Adding 20mL of deionized water and 2mmol of KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring for 5min, and adding 0.15g of La (OH) prepared in the step one3Transferring the solution obtained after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to the room temperature, repeatedly washing the product to be neutral by deionized water and ethanol in the suction filtration process, taking out the sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain (BiO)2OHCl/La(OH)3And compounding the visible light catalyst.
The (BiO)2OHCl/La(OH)3The preparation method of the composite visible light catalyst comprises the following stepsThe following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding 20ml of deionized water into the solid, adding concentrated ammonia water to adjust the pH value to 10, transferring the solution after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing the product to be neutral by using the deionized water and ethanol in the suction filtration process, taking out a sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to 0.97g of Bi (NO)3)3Adding 20mL of deionized water and 2mmol of KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring for 5min, and adding 0.2g of La (OH) prepared in the first step3Transferring the solution obtained after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to the room temperature, repeatedly washing the product to be neutral by deionized water and ethanol in the suction filtration process, taking out the sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain (BiO)2OHCl/La(OH)3And compounding the visible light catalyst.
One kind (BiO)2OHCl/La(OH)3Use of a composite visible light catalyst, said (BiO)2OHCl/La(OH)3The composite visible-light-induced photocatalyst is the composite visible-light-induced photocatalyst as described above, wherein the (BiO) is used2OHCl/La(OH)3The composite visible light catalyst is used for degrading antibiotic wastewater containing tetracycline hydrochloride or industrial wastewater containing organic pollutants.
One kind (BiO)2OHCl/La(OH)3Use of a composite visible light catalyst, wherein the (BiO) is used2OHCl/La(OH)3The method for degrading the antibiotic wastewater containing tetracycline hydrochloride by the composite visible-light-driven photocatalyst comprises the following steps:
will (BiO)2OHCl/La(OH)3Composite visible light catalystAdding the tetracycline hydrochloride-containing antibiotic wastewater into the reactor, stirring the mixture for 30-60 min under a dark condition until adsorption balance is achieved, then turning on visible light irradiation to perform photocatalytic degradation reaction, controlling the reaction temperature to be 15-35 ℃, and stirring the mixture; wherein the wavelength of the visible light is more than 420 nm.
One kind (BiO)2OHCl/La(OH)3Use of a composite visible light catalyst, wherein the (BiO) is used2OHCl/La(OH)3The method for degrading the industrial wastewater containing the organic pollutants by using the composite visible-light-driven photocatalyst comprises the following steps:
will (BiO)2OHCl/La(OH)3The composite visible-light-driven photocatalyst is put into industrial wastewater containing organic pollutants, stirred for 30-60 min under the dark condition until adsorption balance is achieved, then visible light irradiation is turned on, photocatalytic degradation reaction is carried out, the reaction temperature is controlled to be 15-35 ℃, and stirring is carried out; wherein, the visible light adopts visible light with the wavelength of more than 420 nm.
Additional features and advantages of the disclosure will be set forth in the description which follows, or in part may be learned by the practice of the above-described techniques of the disclosure, or may be learned by practice of the disclosure.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
FIG. 1 is pure (BiO) as prepared in example 12SEM image of OHCl;
FIG. 2 shows pure La (OH) prepared in example 13SEM picture of (1);
FIG. 3 is (BiO) prepared in example 22OHCl/La(OH)3SEM picture of the composite photocatalyst;
FIG. 4 is (BiO) prepared in example 22OHCl/La(OH)3TEM image (100nm) of the composite photocatalyst;
FIG. 5 is (BiO) prepared in example 22OHCl/La(OH)3TEM image (50nm) of the composite photocatalyst;
FIG. 6 is (BiO) prepared in example 22OHCl/La(OH)3TEM image (10nm) of the composite photocatalyst;
FIG. 7 shows La (OH) alone3Pure (BiO)2OHCL reaction with (BiO) prepared in example 32OHCl/La(OH)3An XRD spectrum of the composite photocatalyst;
FIG. 8 shows La (OH) alone3Pure (BiO)2OHCL reaction with (BiO) prepared in example 32OHCl/La(OH)3Ultraviolet diffuse reflection spectrum of the composite photocatalyst;
FIG. 9 is (BiO) prepared in examples 1-52OHCl/La(OH)3Composite photocatalyst, pure (BiO)2Degradation graph of OHCl to antibiotic wastewater containing tetracycline hydrochloride;
FIG. 10 is (BiO) prepared in examples 1-52OHCl/La(OH)3Composite photocatalyst, pure (BiO)2Degradation pattern of OHCl on waste water containing o-nitrophenol.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The first embodiment is as follows:
pure sample (BiO)2Preparation of OHCl:
to 0.97g Bi (NO)3)3Adding 20mL of deionized water and 2mmol of KCl into the solid, and adding concentrated ammonia waterAdjusting pH to 10, transferring the solution after continuously stirring for 60min into 50ml polytetrafluoroethylene reaction kettle, maintaining at 180 deg.C for 12h, waiting for the product to naturally cool to room temperature, vacuum filtering, repeatedly washing with deionized water and ethanol to neutrality during the vacuum filtering process, taking out sample, and drying (60 deg.C, 12h) to obtain (BiO)2OHCl. Wherein the pure sample (BiO) is prepared2The SEM image of OHCl is shown in FIG. 1.
Pure La (OH)3The preparation of (1):
to La (NO)3)3Adding 20mL of deionized water into the solid, adding concentrated ammonia water to adjust the pH value to 10, transferring the solution which is continuously stirred for 60min into a 50mL polytetrafluoroethylene reaction kettle, keeping the solution at 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing the product to be neutral by using the deionized water and ethanol in the suction filtration process, taking out a sample, drying the sample at 60 ℃ for 12h to obtain La (OH)3. Wherein, the pure sample La (OH) is obtained3Is shown in fig. 2.
(BiO)2OHCl/La(OH)3The preparation method of the composite visible light catalyst comprises the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding deionized water into the solid, adding concentrated ammonia water to adjust pH to 10, transferring the solution after continuous stirring into a polytetrafluoroethylene reaction kettle, keeping the solution at high temperature for 12h, naturally cooling the product to room temperature, performing suction filtration, repeatedly washing the product with deionized water and ethanol to neutrality in the suction filtration process, taking out the sample, and drying the sample at 60 ℃ for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to Bi (NO)3)3Adding deionized water and KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring, and adding the La (OH) prepared in the step one3Transferring the solution obtained after continuously stirring into a polytetrafluoroethylene reaction kettle, keeping the solution at high temperature for 12 hours, naturally cooling the product to room temperature, then carrying out suction filtration,repeatedly washing with deionized water and ethanol to neutral during suction filtration, taking out sample, and drying at 60 deg.C to obtain (BiO)2OHCl/La(OH)3And compounding the visible light catalyst.
Wherein, in the first step and the second step, the concentration of the added strong ammonia water is 10-14 mol/L.
Example two:
second embodiment of the invention (BiO)2OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst specifically comprises the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding 20ml of deionized water into the solid, adding concentrated ammonia water to adjust the pH value to 10, transferring the solution after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing the product to be neutral by using the deionized water and ethanol in the suction filtration process, taking out a sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to 0.97g of Bi (NO)3)3Adding 20mL of deionized water and 2mmol of KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring for 5min, and adding 0.05g of La (OH) prepared in the first step3Transferring the solution obtained after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to the room temperature, repeatedly washing the product to be neutral by deionized water and ethanol in the suction filtration process, taking out the sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain (BiO)2OHCl/La(OH)3The composite visible light catalyst is marked as BOL-1.
Among them, the one prepared in this example (BiO)2OHCl/La(OH)3The SEM image of the composite visible light catalyst is shown in fig. 3. FIGS. 4 to 6 show (BiO) obtained in this example2OHCl/La(OH)3Composite visible light catalyst inTEM images at different scales. Prepared in this example (BiO)2OHCl/La(OH)3The composite visible light photocatalyst has a nano flaky shape, grows in a petal-shaped staggered manner, is beneficial to the exposure of active sites, and La (OH)3The nano-rods are uniformly modified on the surface of the nano-sheet, which is beneficial to the separation of photo-generated electrons and holes.
Example three:
the third embodiment of the present invention proposes (BiO)2OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst specifically comprises the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding 20ml of deionized water into the solid, adding concentrated ammonia water to adjust the pH value to 10, transferring the solution after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing the product to be neutral by using the deionized water and ethanol in the suction filtration process, taking out a sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to 0.97g of Bi (NO)3)3Adding 20mL of deionized water and 2mmol of KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring for 5min, and adding 0.1g of La (OH) prepared in the first step3Transferring the solution obtained after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to the room temperature, repeatedly washing the product to be neutral by deionized water and ethanol in the suction filtration process, taking out the sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain (BiO)2OHCl/La(OH)3The composite visible light catalyst is marked as BOL-2.
As shown in FIGS. 7 and 8, the carbonized egg membrane has a low content (BiO)2OHCl/La(OH)3The XRD pattern of the composite photocatalyst appears (BiO)2OHCL and La (OH)3Diffraction Peak of (BiO)2OHCl/La(OH)3Among the composite materials (BiO)2OHCL has good crystallinity and is relatively pure (BiO)2OHCl has a broadened light absorption range and a narrower band gap.
Example four
The fourth embodiment of the present invention proposes (BiO)2OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst specifically comprises the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding 20ml of deionized water into the solid, adding concentrated ammonia water to adjust the pH value to 10, transferring the solution after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing the product to be neutral by using the deionized water and ethanol in the suction filtration process, taking out a sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to 0.97g of Bi (NO)3)3Adding 20mL of deionized water and 2mmol of KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring for 5min, and adding 0.1g of La (OH) prepared in the first step3Transferring the solution obtained after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to the room temperature, repeatedly washing the product to be neutral by deionized water and ethanol in the suction filtration process, taking out the sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain (BiO)2OHCl/La(OH)3The composite visible light catalyst is marked as BOL-3.
EXAMPLE five
The fifth embodiment of the present invention provides (BiO)2OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst specifically comprises the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)320ml of deionized water was added to the solid, andadding concentrated ammonia water to adjust pH to 10, transferring the solution after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing with deionized water and ethanol during the suction filtration process to be neutral, taking out the sample, drying at the temperature of 60 ℃ for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to 0.97g of Bi (NO)3)3Adding 20mL of deionized water and 2mmol of KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring for 5min, and adding 0.2g of La (OH) prepared in the first step3Transferring the solution obtained after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to the room temperature, repeatedly washing the product to be neutral by deionized water and ethanol in the suction filtration process, taking out the sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain (BiO)2OHCl/La(OH)3The composite visible light catalyst is marked as BOL-4.
EXAMPLE six
Evaluation of photocatalytic performance (for tetracycline hydrochloride-containing wastewater):
pure (BiO)2OHCL, pure La (OH)3And (BiO) prepared in examples 2 to 52OHCl/La(OH)3The composite photocatalyst is applied to the degradation of tetracycline hydrochloride (TC. HCl) containing wastewater. The method specifically comprises the following steps: using BOL-1, BOL-2, BOL-3, BOL-4, (BiO)2OHCL and La (OH)3The method is used for degrading tetracycline hydrochloride (TC & HCl) -containing wastewater, and comprises the following specific implementation steps:
50mg (BiO)2Putting OHCL composite photocatalyst into 80mL of wastewater containing 10ppm of TC & HCl, stirring for 30min under dark condition, taking a first sample as an initial value, opening a water cooling system to keep the reaction temperature at 25 ℃, and simulating visible light by using a xenon lamp light source added with a filter (the step (b) ((the step of adding the filter)>420nm), sampling once every 5min, stopping the catalytic reaction after 30min by turning off the light source, performing centrifugal separation on the obtained sample, and taking supernatant;
measuring the absorbance value of the obtained sample at the position of 375nm of the maximum absorption wavelength of the sample by using an ultraviolet-visible spectrophotometer, recording data, and respectively calculating and evaluating the degradation performance of the prepared sample on tetracycline hydrochloride (TC. HCl) in the wastewater. As shown in FIG. 9, the degradation effect of the prepared composite photocatalyst on TC & HCl is obviously higher than that of pure (BiO)2OHCl, wherein the degradation efficiency of the BOL-2 photocatalyst to TC & HCl within 100min can reach 92%.
EXAMPLE seven
Evaluation of photocatalytic performance (for industrial wastewater containing organic pollutants):
pure (BiO)2OHCL, pure La (OH)3And (BiO) prepared in examples 2 to 52OHCl/La(OH)3The composite photocatalyst is applied to degradation of industrial wastewater containing organic pollutants. The method specifically comprises the following steps: using BOL-1, BOL-2, BOL-3, BOL-4, (BiO)2OHCL and La (OH)3Degrading industrial waste water containing organic pollutants. The specific implementation steps are as follows:
50mg (BiO)2Putting the OHCL composite photocatalyst into 80mL of wastewater containing 10ppm of o-NP, stirring for 30min under the dark condition, taking a first sample as an initial value, opening a water cooling system to keep the reaction temperature at 25 ℃, and simulating visible light by using a xenon lamp light source added with a filter (wherein the xenon lamp light source is used for simulating visible light)>420nm), sampling once every 5min, stopping the catalytic reaction after 30min by turning off the light source, performing centrifugal separation on the obtained sample, and taking supernatant;
and measuring the absorbance value of the obtained sample at the maximum absorption wavelength of 280nm by using an ultraviolet-visible spectrophotometer, recording data, and respectively calculating and evaluating the degradation performance of the prepared sample on o-nitrophenol (o-NP) in the wastewater. As shown in FIG. 10, the degradation effect of the prepared composite photocatalyst on o-NP is obviously higher than that of pure (BiO)2OHCI, wherein the photocatalyst of BOL-2 can degrade o-NP with the efficiency of 88% in 100 min.
1. The invention takes lanthanum nitrate as raw material, is cheap and easily available, and has one dimension of La (OH)3The nano-rod has unique electronic structure, morphological characteristics and excellent photoelectric property, and is prepared by taking the nano-rod as a raw materialNew pattern (BiO)2OHCl/La(OH)3The composite material can reduce the production cost; the nanorod structure can provide a space channel for electron transmission, and is beneficial to separation of photo-generated electrons and holes, so that the catalytic activity of the composite photocatalyst is promoted to be improved;
2. in the photocatalyst prepared by the invention (BiO)2OHCl3Nanoflower and rod-shaped La (OH)3In combination, the rod-shaped structure is inserted around the flower-shaped structure, so that the migration rate of current carriers is promoted, and the recombination of photo-generated electron pairs is effectively inhibited; at the same time, overcomes the defects caused by the common preparation method (BiO)2The OHCl nanosheets are easy to stack, so that the specific surface area is reduced, the problem of exposure of catalytic active sites is not facilitated, and the prepared photocatalyst has quick and efficient visible light photocatalytic degradation performance on organic pollutants and antibiotics in wastewater.
Finally, it should be noted that: the above-mentioned embodiments are only specific embodiments of the present invention, which are used for illustrating the technical solutions of the present invention and not for limiting the same, and the protection scope of the present invention is not limited thereto, although the present invention is described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: any person skilled in the art can modify or easily conceive the technical solutions described in the foregoing embodiments or equivalent substitutes for some technical features within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the embodiments of the present invention, and they should be construed as being included therein. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (9)
1. One kind (BiO)2OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst is characterized by comprising the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding deionized water to the solid, and addingAdding concentrated ammonia water to adjust pH to 10, transferring the solution after continuous stirring into a polytetrafluoroethylene reaction kettle, keeping at high temperature for 12h, naturally cooling the product to room temperature, performing suction filtration, repeatedly washing with deionized water and ethanol during suction filtration to neutrality, taking out the sample, drying at 60 deg.C for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to Bi (NO)3)3Adding deionized water and KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring, and adding the La (OH) prepared in the step one3Transferring the solution obtained after continuous stirring into a polytetrafluoroethylene reaction kettle, keeping the solution at high temperature for 12 hours, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing the product to be neutral by deionized water and ethanol in the suction filtration process, taking out the sample, and drying the sample at 60 ℃ to obtain (BiO)2OHCl/La(OH)3And compounding the visible light catalyst.
2. The (BiO) according to claim 12OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst is characterized in that in the first step and the second step, the concentration of the added concentrated ammonia water is 10-14 mol/L.
3. The (BiO) according to claim 12OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst is characterized by comprising the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding 20ml of deionized water into the solid, adding concentrated ammonia water to adjust the pH value to 10, transferring the solution after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing the product to be neutral by using the deionized water and ethanol in the suction filtration process, taking out a sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to 0.97g of Bi (NO)3)3Adding 20mL of deionized water and 2mmol of KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring for 5min, and adding 0.05g of La (OH) prepared in the first step3Transferring the solution obtained after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to the room temperature, repeatedly washing the product to be neutral by deionized water and ethanol in the suction filtration process, taking out the sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain (BiO)2OHCl/La(OH)3And compounding the visible light catalyst.
4. The (BiO) according to claim 12OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst is characterized by comprising the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding 20ml of deionized water into the solid, adding concentrated ammonia water to adjust the pH value to 10, transferring the solution after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing the product to be neutral by using the deionized water and ethanol in the suction filtration process, taking out a sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to 0.97g of Bi (NO)3)3Adding 20mL of deionized water and 2mmol of KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring for 5min, and adding 0.1g of La (OH) prepared in the first step3Transferring the solution obtained after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping at 180 deg.C for 12h, naturally cooling the product to room temperature, vacuum filtering, and repeatedly washing with deionized water and ethanol during vacuum filtrationTaking out the sample to be neutral, and drying the sample at the temperature of 60 ℃ for 12h to obtain (BiO)2OHCl/La(OH)3And compounding the visible light catalyst.
5. The (BiO) according to claim 12OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst is characterized by comprising the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding 20ml of deionized water into the solid, adding concentrated ammonia water to adjust the pH value to 10, transferring the solution after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to room temperature, repeatedly washing the product to be neutral by using the deionized water and ethanol in the suction filtration process, taking out a sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to 0.97g of Bi (NO)3)3Adding 20mL of deionized water and 2mmol of KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring for 5min, and adding 0.15g of La (OH) prepared in the step one3Transferring the solution obtained after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to the room temperature, repeatedly washing the product to be neutral by deionized water and ethanol in the suction filtration process, taking out the sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain (BiO)2OHCl/La(OH)3And compounding the visible light catalyst.
6. The (BiO) according to claim 12OHCl/La(OH)3The preparation method of the composite visible-light-driven photocatalyst is characterized by comprising the following steps:
step one, preparing La (OH)3Sample preparation:
to La (NO)3)3Adding 20ml deionized water into the solid, and adding concentrated ammoniaAdjusting pH to 10 with water, transferring the solution after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping at 180 deg.C for 12h, naturally cooling the product to room temperature, vacuum-filtering, repeatedly washing with deionized water and ethanol to neutrality during vacuum-filtering, taking out the sample, drying at 60 deg.C for 12h to obtain La (OH)3A sample;
step two, preparing to obtain (BiO)2OHCl/La(OH)3Compounding visible light catalyst:
to 0.97g of Bi (NO)3)3Adding 20mL of deionized water and 2mmol of KCl into the solid, adding concentrated ammonia water to adjust the pH to 10, stirring for 5min, and adding 0.2g of La (OH) prepared in the first step3Transferring the solution obtained after continuously stirring for 60min into a 50ml polytetrafluoroethylene reaction kettle, keeping the solution at the high temperature of 180 ℃ for 12h, performing suction filtration after the product is naturally cooled to the room temperature, repeatedly washing the product to be neutral by deionized water and ethanol in the suction filtration process, taking out the sample, and drying the sample at the temperature of 60 ℃ for 12h to obtain (BiO)2OHCl/La(OH)3And compounding the visible light catalyst.
7. One kind (BiO)2OHCl/La(OH)3Use of a composite visible light catalyst, said (BiO)2OH Cl/La(OH)3Composite visible light catalyst according to any of claims 1 to 5, characterized in that said (BiO) is applied2OHCl/La(OH)3The composite visible light catalyst is used for degrading antibiotic wastewater containing tetracycline hydrochloride or industrial wastewater containing organic pollutants.
8. A process (BiO) according to claim 72OHCl/La(OH)3Use of a composite visible light catalyst, characterized in that the (BiO) is used2OHCl/La(OH)3The method for degrading the antibiotic wastewater containing tetracycline hydrochloride by the composite visible-light-driven photocatalyst comprises the following steps:
will (Bi0)2OHCl/La(OH)3Adding the tetracycline hydrochloride-containing antibiotic into a composite visible light catalystStirring the raw wastewater for 30-60 min under a dark condition until adsorption balance is achieved, then turning on visible light irradiation to perform photocatalytic degradation reaction, controlling the reaction temperature to be 15-35 ℃, and stirring; wherein the wavelength of the visible light is more than 420 nm.
9. A process (BiO) according to claim 72OHCl/La(OH)3Use of a composite visible light catalyst, characterized in that the (BiO) is used2OHCl/La(OH)3The method for degrading the industrial wastewater containing the organic pollutants by using the composite visible-light-driven photocatalyst comprises the following steps:
will (BiO)2OHCl/La(OH)3The composite visible-light-driven photocatalyst is put into industrial wastewater containing organic pollutants, stirred for 30-60 min under the dark condition until adsorption balance is achieved, then visible light irradiation is turned on, photocatalytic degradation reaction is carried out, the reaction temperature is controlled to be 15-35 ℃, and stirring is carried out; wherein, the visible light adopts visible light with the wavelength of more than 420 nm.
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| CA2359495A1 (en) * | 2000-10-20 | 2002-04-20 | Sumitomo Chemical Co., Ltd. | Photocatalyst, process for producing the same and photocatalyst coating composition using the same |
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