CN110237853B - Gadolinium chromate/silver phosphate composite photocatalyst and application thereof in VOCs purification - Google Patents
Gadolinium chromate/silver phosphate composite photocatalyst and application thereof in VOCs purification Download PDFInfo
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- CN110237853B CN110237853B CN201910615439.8A CN201910615439A CN110237853B CN 110237853 B CN110237853 B CN 110237853B CN 201910615439 A CN201910615439 A CN 201910615439A CN 110237853 B CN110237853 B CN 110237853B
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- gadolinium
- chromate
- silver
- silver phosphate
- phosphate
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- OFNHMKFJXLGYNW-UHFFFAOYSA-N dioxido(dioxo)chromium gadolinium(3+) Chemical compound [Cr](=O)(=O)([O-])[O-].[Gd+3].[Cr](=O)(=O)([O-])[O-].[Cr](=O)(=O)([O-])[O-].[Gd+3] OFNHMKFJXLGYNW-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910000161 silver phosphate Inorganic materials 0.000 title claims abstract description 61
- 229940019931 silver phosphate Drugs 0.000 title claims abstract description 51
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 19
- 238000000746 purification Methods 0.000 title claims abstract description 7
- 239000012855 volatile organic compound Substances 0.000 title claims abstract description 7
- 239000004332 silver Substances 0.000 claims abstract description 19
- 229910052709 silver Inorganic materials 0.000 claims abstract description 19
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 17
- -1 silver phosphate compound Chemical class 0.000 claims abstract description 16
- 150000003379 silver compounds Chemical class 0.000 claims abstract description 15
- 229940100890 silver compound Drugs 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004202 carbamide Substances 0.000 claims abstract description 8
- 238000011068 loading method Methods 0.000 claims abstract description 8
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 21
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims description 16
- 239000003054 catalyst Substances 0.000 claims description 9
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 239000007791 liquid phase Substances 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000012071 phase Substances 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract description 27
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 27
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 abstract description 9
- 239000008096 xylene Substances 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 229910052688 Gadolinium Inorganic materials 0.000 abstract description 4
- 239000003344 environmental pollutant Substances 0.000 abstract description 4
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 abstract description 4
- 231100000719 pollutant Toxicity 0.000 abstract description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052804 chromium Inorganic materials 0.000 abstract description 3
- 239000011651 chromium Substances 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 230000005284 excitation Effects 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 229910001316 Ag alloy Inorganic materials 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 239000004065 semiconductor Substances 0.000 abstract 1
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 26
- 239000007864 aqueous solution Substances 0.000 description 21
- 238000003756 stirring Methods 0.000 description 14
- 229910001961 silver nitrate Inorganic materials 0.000 description 13
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 6
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000008103 glucose Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000013329 compounding Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 229910021555 Chromium Chloride Inorganic materials 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 description 1
- XHFVDZNDZCNTLT-UHFFFAOYSA-H chromium(3+);tricarbonate Chemical compound [Cr+3].[Cr+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O XHFVDZNDZCNTLT-UHFFFAOYSA-H 0.000 description 1
- 229910000151 chromium(III) phosphate Inorganic materials 0.000 description 1
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 description 1
- IKZBVTPSNGOVRJ-UHFFFAOYSA-K chromium(iii) phosphate Chemical compound [Cr+3].[O-]P([O-])([O-])=O IKZBVTPSNGOVRJ-UHFFFAOYSA-K 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- MEANOSLIBWSCIT-UHFFFAOYSA-K gadolinium trichloride Chemical compound Cl[Gd](Cl)Cl MEANOSLIBWSCIT-UHFFFAOYSA-K 0.000 description 1
- JAOZQVJVXQKQAD-UHFFFAOYSA-K gadolinium(3+);phosphate Chemical compound [Gd+3].[O-]P([O-])([O-])=O JAOZQVJVXQKQAD-UHFFFAOYSA-K 0.000 description 1
- RQXZRSYWGRRGCD-UHFFFAOYSA-H gadolinium(3+);tricarbonate Chemical compound [Gd+3].[Gd+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O RQXZRSYWGRRGCD-UHFFFAOYSA-H 0.000 description 1
- QLAFITOLRQQGTE-UHFFFAOYSA-H gadolinium(3+);trisulfate Chemical compound [Gd+3].[Gd+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O QLAFITOLRQQGTE-UHFFFAOYSA-H 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 1
- 229910000367 silver sulfate Inorganic materials 0.000 description 1
- HTRJDXQPCKIFIU-UHFFFAOYSA-N silver;ethanol;nitrate Chemical compound [Ag+].CCO.[O-][N+]([O-])=O HTRJDXQPCKIFIU-UHFFFAOYSA-N 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/864—Removing carbon monoxide or hydrocarbons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8678—Removing components of undefined structure
- B01D53/8687—Organic components
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
-
- B01J35/39—
Abstract
The invention discloses a gadolinium chromate/silver phosphate composite photocatalyst and application thereof in VOCs purification, wherein the composite is expressed in a GdCrO mode3/Ag/Ag3PO4. The preparation method comprises the following steps: 1) taking a gadolinium source and a chromium source in a mortar according to the proportion of 1:1, adding a proper amount of urea, uniformly grinding, and then placing in a specific atmosphere for roasting at a high temperature to obtain gadolinium chromate; 2) loading silver particles on the gadolinium chromate to obtain a gadolinium chromate/silver compound; 3) and loading silver phosphate on the gadolinium chromate/silver to obtain a gadolinium chromate/silver phosphate compound. GdCrO prepared by the invention3/Ag/Ag3PO4The simple substance Ag in the silver alloy generates plasma resonance under the excitation of visible light to generate hot electron-hole pairs. Semiconductor GdCrO with band gap separation connected by hot electron-hole pair3And Ag3PO4Without sacrificing their oxidation or reduction potential, thereby enhancing the photocatalytic redox capability of the composite. GdCrO3/Ag/Ag3PO4Is used for photocatalytic degradation of organic pollutants. It is under the irradiation of visible light and mild reaction conditions, such as 90oAnd C, completely catalyzing and purifying typical organic gas pollutants such as toluene, xylene and benzene.
Description
Technical Field
The invention relates to a gadolinium chromate/silver phosphate composite photocatalyst and application thereof in purification of VOCs, and belongs to the technical field of photocatalytic materials and environmental protection.
Background
The photocatalytic pollutant degradation technology has the characteristics of mild conditions, low reaction energy consumption and the like, and is one of the technologies with the most application prospect. But conventional photocatalysts, e.g. TiO2There are problems of rapid recombination of photo-generated electron-hole pairs, low quantum yield, low purification efficiency, and the like. The construction of complex heterosystems is considered to be an effective method for reducing the recombination rate of photogenerated electron-hole pairs, for example by constructing Z-type heterojunctions In2O3-Ag-Ag3PO4（Chemical Engineering Journal2017, 320, 644-2S/Ag3PO4 （Applied Catalysis B: Environmental2017, 209, 566-3PO4Photo-generated electron-hole pairsThe separation efficiency of (1). However, the existing heterogeneous system construction ideas and technologies generally sacrifice the original oxidation or reduction potential of the monomer of the heterogeneous system, and the performance of photocatalytic purification of organic pollutants cannot be effectively improved.
Disclosure of Invention
Aiming at the problems faced by a compound heterogeneous system in the field of photocatalysis, the invention provides a gadolinium chromate/silver phosphate compound photocatalyst (GdCrO)3/Ag/Ag3PO4) And a preparation method and application thereof. In the composite catalyst, the weight fraction of the simple substance Ag is 0.1-20% and the weight fraction of the silver phosphate is 1-40.0% based on 100% of the weight of the catalyst. Elementary Ag in the compound generates plasma resonance under the excitation of visible light to generate hot electron-hole pairs to receive Ag3PO4The generated photo-generated electrons are transferred to GdCrO3On the photo-generated hole, the energy gap is separated from the GdCrO3And Ag3PO4Connected and fully utilizes respective oxidation or reduction potential to prepare the high-efficiency GdCrO3/Ag/Ag3PO4A composite photocatalytic material.
The preparation method of the gadolinium chromate/silver phosphate composite photocatalyst comprises the following steps:
(1) taking a gadolinium source and a chromium source in a mortar according to the proportion of 1:1, adding a proper amount of urea, uniformly grinding, and then placing in a specific atmosphere for high-temperature roasting to obtain gadolinium chromate;
(2) loading silver particles on the gadolinium chromate to obtain a gadolinium chromate/silver compound;
(3) and loading silver phosphate on the gadolinium chromate/silver to obtain a gadolinium chromate/silver phosphate compound.
Wherein, the gadolinium source in the step (1) can be gadolinium nitrate, gadolinium chloride, gadolinium phosphate, gadolinium carbonate, gadolinium sulfate and the like, and gadolinium nitrate is preferred; the chromium source can be selected from chromium nitrate, chromium chloride, chromium phosphate, chromium carbonate, chromium sulfate, etc., preferably chromium nitrate. The roasting atmosphere is air, or can be replaced by mixed gas consisting of oxygen and inert gas in different proportions, and the roasting temperature is 150-1100%oAnd C, roasting for 0.1-24 hours. Preferably by bakingThe burning temperature is 700-900 DEG CoAnd C, roasting for 3-6 hours.
In the step (2), the silver source can be silver nitrate, silver chloride, silver phosphate, silver sulfate and the like, preferably silver nitrate and prepared into precursor solution. And reducing and loading silver on the gadolinium chromate by adopting a liquid phase reduction method and selecting a glucose solution as a reducing agent. NaBH may also be used4Or other reducing agents, or other reducing methods such as a light reduction method, a calcination reduction method and the like are selected to load the Ag particles on the gadolinium chromate.
The method for compounding silver phosphate with gadolinium chromate/silver in the step (3) is a liquid phase deposition method. And (3) selecting a disodium hydrogen phosphate aqueous solution and a silver nitrate aqueous solution as precursor solutions, and carrying out liquid phase reaction on gadolinium chromate/silver to deposit silver phosphate. The silver/gadolinium chromate may also be compounded with silver phosphate by solid phase grinding compounding.
Preparation of perovskite GdCrO by roasting method3It has been reported thatApplied Catalysis B: Environmental2018, 232, 124-134.) reports that the roasting method prepares pure-phase GdCrO3The method of (1). In the liquid phase reduction method, glucose is used as a reducing agent to reduce silver ions to prepare simple substance silver, and the method has been reported, for example, Bi and (b)Chemistry-A European Journal2012, 18, 14272-) -cubic Ag using glucose solution3PO4And (3) preparing the simple substance silver by selective reduction. The calcination and liquid phase reduction methods described above are also common experimental conditions for those skilled in the art. But the invention firstly obtains the gadolinium chromate/silver phosphate compound by accurately controlling the proportion of the components of the compound material, the adding amount of the silver source and the reduction condition, the in-situ partial corrosion of gadolinium chromate/silver by phosphate radical, the in-situ deposition of silver phosphate and other working procedures.
It is a further object of the present invention to provide the use of a gadolinium chromate/silver phosphate complex.
The application of the gadolinium chromate/silver phosphate compound provided by the invention is the application of the gadolinium chromate/silver phosphate compound in photocatalytic degradation of volatile organic gas pollutants (or VOCs) in air, such as gas pollutants of toluene, xylene, benzene and the like.
Compared with the prior art, the invention has the following advantages thatThe beneficial effects are that: (1) the preparation process of the gadolinium chromate/silver phosphate compound is simple, the experimental period is short, except that the gadolinium chromate is related to high-temperature synthesis, the rest steps can be carried out at room temperature, and industrial large-scale production is facilitated. (2) The gadolinium chromate/silver phosphate compound prepared by the invention can be irradiated by visible light and reacted under mild reaction conditions, such as 90 DEGoAnd C, completely catalyzing and purifying typical VOCs such as toluene, xylene and benzene.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited to the specific operation manner described in the examples, and other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and they are included in the scope of the present invention.
Example 1
A gadolinium chromate/silver phosphate composite photocatalyst: (1) weighing gadolinium nitrate and chromium nitrate with a molar ratio of 1:1, uniformly grinding in a mortar containing a proper amount of urea, transferring to a muffle furnace, and roasting at 850 ℃ for 3 h under an air atmosphere to obtain gadolinium chromate; (2) adding 0.6 g of gadolinium chromate into a silver-ammonia solution prepared from 30mL of 42.47 g/L silver nitrate aqueous solution and 0.5mol/L diluted ammonia water, stirring for 30 min, then adding 20 mL of 297.25 g/L glucose aqueous solution, and continuously stirring for 5 min to obtain a gadolinium chromate/silver compound; (3) adding 0.3 g of gadolinium chromate/silver compound into 30mL of 9.47 g/L disodium hydrogen phosphate aqueous solution, stirring for 30 min, then dropwise adding 15 mL of 5.67 g/L silver nitrate aqueous solution, and continuously stirring for 30 min to obtain the gadolinium chromate/silver phosphate compound, wherein the mass fraction of the simple substance Ag is 4.2% and the mass fraction of the silver phosphate is 25.9% based on 100% of the weight of the catalyst.
Comparative example 1
A gadolinium chromate/silver phosphate composite photocatalyst was compared. 0.3 g of gadolinium chromate in example 1 is added into 30mL of 9.47 g/L disodium hydrogen phosphate aqueous solution and stirred for 30 min, then 30mL of 5.67 g/L silver nitrate aqueous solution is added dropwise, and stirring is continued for 30 min to obtain a gadolinium chromate/silver phosphate compound.
Comparative example 2
A gadolinium chromate/silver phosphate composite photocatalyst was compared. Weighing gadolinium nitrate and chromium nitrate with a molar ratio of 1:1, uniformly grinding in a mortar containing a proper amount of urea, transferring to a muffle furnace, and roasting at 850 ℃ for 3 h under an air atmosphere to obtain gadolinium chromate; (2) adding 0.6 g of gadolinium chromate into a silver-ammonia solution prepared from 30mL of 42.47 g/L silver nitrate aqueous solution and 0.5mol/L diluted ammonia water, stirring for 30 min, adding 20 mL of 297.25 g/L glucose aqueous solution, and continuously stirring for 5 min to obtain the gadolinium chromate/silver compound.
Comparative example 3
A gadolinium chromate/silver phosphate composite photocatalyst was compared. (1) Dripping 30mL of 14.2 g/L disodium hydrogen phosphate aqueous solution into 30mL of 42.47 g/L silver nitrate aqueous solution, and stirring for 30 min to obtain silver phosphate; (2) adding 0.3 g of silver phosphate into a silver ammonia solution prepared from 30mL of 21.23 g/L silver nitrate aqueous solution and 0.5mol/L diluted ammonia water, stirring for 30 min, adding 20 mL of 148.63 g/L glucose aqueous solution, and continuously stirring for 5 min to obtain the silver phosphate/silver compound.
Example 2
A gadolinium chromate/silver phosphate composite photocatalyst: (1) weighing gadolinium nitrate and chromium nitrate with a molar ratio of 1:1, uniformly grinding in a mortar containing a proper amount of urea, transferring to a muffle furnace, and roasting at 700 ℃ for 6 hours in an air atmosphere to obtain gadolinium chromate; (2) 0.6 g of gadolinium chromate is added into 30mL of 15.0 g/L silver nitrate aqueous solution, stirred for 30 min, and then 10 mL of 5.0 g/L NaBH is added4The aqueous solution is stirred for 10 min to obtain a gadolinium chromate/silver compound; (3) 0.3 g of gadolinium chromate/silver compound and 0.05 g of silver phosphate are mixed, ground and mixed evenly in a nitrogen atmosphere for 500 goCalcining for 2 h to obtain a gadolinium chromate/silver phosphate compound, wherein the mass fraction of the simple substance Ag is 11.1% and the mass fraction of the silver phosphate is 14.3% based on 100% of the weight of the catalyst.
Example 3
A gadolinium chromate/silver phosphate composite photocatalyst: (1) weighing gadolinium nitrate and chromium nitrate with a molar ratio of 1:1, uniformly grinding in a mortar containing a proper amount of urea, transferring to a muffle furnace, and roasting at 800 ℃ for 4.5 hours in an air atmosphere to obtain gadolinium chromate; (2) adding 0.6 g of gadolinium chromate into 30mL of 24.0 g/L silver nitrate water-ethanol mixed solution, and illuminating for 30 min under an Xe lamp to obtain a gadolinium chromate/silver compound; (3) adding 0.3 g of gadolinium chromate/silver compound into 30mL of 14.21 g/L disodium hydrogen phosphate aqueous solution, stirring for 30 min, then dropwise adding 15 mL of 8.51 g/L silver nitrate aqueous solution, and continuously stirring for 30 min to obtain the gadolinium chromate/silver phosphate compound, wherein the mass fraction of the simple substance Ag is 0.4% and the mass fraction of the silver phosphate is 33.3% by taking the weight of the catalyst as 100%.
Example 4
A gadolinium chromate/silver phosphate composite photocatalyst and a preparation method thereof are disclosed: (1) weighing gadolinium nitrate and chromium nitrate with a molar ratio of 1:1, uniformly grinding in a mortar containing a proper amount of urea, transferring to a muffle furnace in an air atmosphere, and calcining at 900 ℃ for 2 h to obtain gadolinium chromate; (2) 0.6 g of gadolinium chromate is added to 30mL of 30.0 g/L silver nitrate ethanol aqueous solution to dry, and then the mixture is dried at 500oCalcining in air for 2 h under C to obtain a gadolinium chromate/silver compound; (3) adding 0.3 g of gadolinium chromate/silver compound into 30mL of 18.94 g/L disodium hydrogen phosphate aqueous solution, stirring for 30 min, then dropwise adding 15 mL of 11.34 g/L silver nitrate aqueous solution, and continuously stirring for 30 min to obtain the gadolinium chromate/silver phosphate compound, wherein the mass fraction of the simple substance Ag is 12.3% and the mass fraction of the silver phosphate is 40.0% by taking the weight of the catalyst as 100%.
0.2 g of each of the catalysts described in examples 1 to 4 and comparative examples 1 to 3 was uniformly coated on a film of 7.0 cm2On a surface vessel, and is arranged at the bottom of a reaction kettle, and mixed gas (O) is used2:N2=1: 3) purging for 30 min to remove CO in the reaction kettle2. Toluene, xylene or benzene visible light catalytic reaction experimental conditions: toluene gas was bubbled through mixed gas (O)2:N2=1: 3), xylene and benzene were fed from outside the reactor by a pipette. The initial concentration of the toluene, the xylene or the benzene in the reaction kettle is 700 ppm, and the reaction kettle is treated in a dark place for 30 min at room temperature before illumination, so that the toluene, the xylene or the benzene can achieve adsorption-desorption balance on the surface of the catalyst. A300W xenon lamp provided with a UVIR-cut400 filter is used as a simulated visible light source (lambda = 400-780 nm, and the light intensity is 100 mw)·cm-2) At 90 oCReacting for 2 h under the conditions of toluene, xylene or benzene concentration detection by gas chromatography (GC 7900, FID) and CO detection by gas chromatography (GC2060, FID)2The yields were used to convert to elimination of toluene, xylene or benzene.
TABLE 1 evaluation results of activity of gadolinium chromate/silver phosphate composite photocatalyst under visible light irradiation
Claims (6)
1. A gadolinium chromate/silver phosphate composite photocatalyst is characterized in that: the weight of the catalyst is 100 percent, the weight fraction of the simple substance silver is 0.1 to 20 percent, and the weight fraction of the silver phosphate is 1 to 40.0 percent.
2. The method of preparing a gadolinium chromate/silver phosphate composite photocatalyst as claimed in claim 1, wherein: the method comprises the following steps:
(1) taking gadolinium nitrate and chromium nitrate in a mortar according to the proportion of 1:1, adding a proper amount of urea, uniformly grinding, and then placing in an oxygen-containing atmosphere for high-temperature roasting to obtain gadolinium chromate;
(2) loading silver particles on gadolinium chromate to obtain a gadolinium chromate/silver compound;
(3) and loading silver phosphate on the gadolinium chromate/silver to obtain a gadolinium chromate/silver phosphate compound.
3. The method according to claim 2, wherein the calcination temperature in the step (1) is 700 to 1100 ℃ and the calcination time is 2 to 24 hours.
4. The preparation method according to claim 2, wherein the silver ions are reduced and loaded on the gadolinium chromate by a liquid-phase reduction method, a light reduction method or a gas-phase reduction method in the step (2).
5. The preparation method according to claim 2, wherein the method of loading silver phosphate on the gadolinium chromate/silver in the step (3) is a liquid phase deposition method or a solid phase grinding composite method.
6. Use of a gadolinium chromate/silver phosphate composite photocatalyst according to claim 1 or a gadolinium chromate/silver phosphate composite photocatalyst prepared by a preparation method according to any one of claims 2 to 5 for the purification of VOCs.
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