CN110711594A - Ag3PO4/AlPO4Composite high-efficiency photocatalyst and preparation method thereof - Google Patents
Ag3PO4/AlPO4Composite high-efficiency photocatalyst and preparation method thereof Download PDFInfo
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- CN110711594A CN110711594A CN201911008822.3A CN201911008822A CN110711594A CN 110711594 A CN110711594 A CN 110711594A CN 201911008822 A CN201911008822 A CN 201911008822A CN 110711594 A CN110711594 A CN 110711594A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 45
- 229910000161 silver phosphate Inorganic materials 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 96
- 239000007864 aqueous solution Substances 0.000 claims abstract description 70
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 52
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000002131 composite material Substances 0.000 claims abstract description 38
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 33
- 239000012065 filter cake Substances 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 15
- 239000002244 precipitate Substances 0.000 claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 15
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 7
- 239000010452 phosphate Substances 0.000 claims abstract description 7
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000004793 Polystyrene Substances 0.000 claims description 17
- 239000000839 emulsion Substances 0.000 claims description 17
- 229920002223 polystyrene Polymers 0.000 claims description 17
- 239000007787 solid Substances 0.000 claims description 16
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 6
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical group [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 5
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 5
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 4
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 4
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 4
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 4
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 4
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 4
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 239000001488 sodium phosphate Substances 0.000 claims description 4
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 4
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 4
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 3
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 3
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 3
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 3
- 235000011008 sodium phosphates Nutrition 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000001354 calcination Methods 0.000 abstract description 13
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 abstract description 6
- 229940019931 silver phosphate Drugs 0.000 abstract description 6
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 3
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 3
- 229940043267 rhodamine b Drugs 0.000 abstract description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract 1
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Inorganic materials [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 5
- 239000005696 Diammonium phosphate Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 235000019797 dipotassium phosphate Nutrition 0.000 description 2
- 229910000396 dipotassium phosphate Inorganic materials 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 229910001437 manganese ion Inorganic materials 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- OCKGFTQIICXDQW-ZEQRLZLVSA-N 5-[(1r)-1-hydroxy-2-[4-[(2r)-2-hydroxy-2-(4-methyl-1-oxo-3h-2-benzofuran-5-yl)ethyl]piperazin-1-yl]ethyl]-4-methyl-3h-2-benzofuran-1-one Chemical compound C1=C2C(=O)OCC2=C(C)C([C@@H](O)CN2CCN(CC2)C[C@H](O)C2=CC=C3C(=O)OCC3=C2C)=C1 OCKGFTQIICXDQW-ZEQRLZLVSA-N 0.000 description 1
- 101710134784 Agnoprotein Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- ZMFWDTJZHRDHNW-UHFFFAOYSA-N indium;trihydrate Chemical compound O.O.O.[In] ZMFWDTJZHRDHNW-UHFFFAOYSA-N 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229940071125 manganese acetate Drugs 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
Classifications
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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
- 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
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1817—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with copper, silver or gold
-
- 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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/36—Aluminium phosphates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- 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
- C02F2101/40—Organic compounds containing sulfur
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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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Abstract
The invention provides Ag3PO4/AlPO4A composite photocatalyst and a preparation method thereof. The technical scheme is as follows: adding aluminum nitrate aqueous solution, silver nitrate aqueous solution and phosphate aqueous solution with certain concentration into a reactor with stirring, adjusting the pH value of the solution to 1.0 by using nitric acid, then dropwise adding sodium hydroxide aqueous solution under stirring to generate yellow precipitate, and continuously dropwise adding sodium hydroxide solution until the pH value of the solution reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake with deionized water for three times, calcining the filter cake in a tubular furnace at 300-500 ℃ for 0.5-3 hours, and cooling to obtain golden yellow Ag3PO4/AlPO4Composite photocatalysisAnd (3) preparing. The prepared composite photocatalyst is strip-shaped, the length is 3-5 micrometers, the length-diameter ratio is 5-10, and the photocatalytic effect on methylene blue aqueous solution and rhodamine B aqueous solution is superior to that of pure silver phosphate.
Description
Technical Field
The invention relates to Ag3PO4/AlPO4A composite high-efficiency photocatalyst and a preparation method thereof belong to the field of photocatalytic materials.
Background
Silver phosphate (Ag)3PO4) Is a novel high-efficiency photocatalytic material and has high photocatalytic performance under the irradiation of natural light. The preparation is simple and environment-friendly, so that the photocatalyst is one of the materials with the greatest application prospect in the field of photocatalytic degradation photoelectrochemistry. But Ag3PO4Has poor self-stability and is easy to self-corrode in photocatalysis, namely Ag under photocatalysis conditions3PO4Gradually becomes simple substance Ag, and finally becomes the simple substance Ag completely. In addition, Ag3PO4The production cost is also higher. For increasing Ag3PO4Stability of (2), many researchers have synthesized Ag3PO4/AgX(X＝Cl，Br，I)，Ag3PO4/TiO2，Ag3PO4/SnO2，Ag3PO4/CeO2，Ag3PO4/C3N4，Ag/Ag3PO4/TiO2，Ag3PO4/In(OH)3，A3PO4Graphene oxide and Ag3PO4/TiO2Graphene/and other composite photocatalysts, and Ag of the composite photocatalysts is improved to a certain extent3PO4The doped components are expensive, so the raw material cost is still high. The cheap ferric trichloride such as the chenchenyang and the like is firstly reacted in a high-pressure reaction kettle at the temperature of 200 ℃ for 20 hours to prepare the ferroferric oxide (Fe)3O4) Then dispersing ferroferric oxide in the reaction solution of silver nitrate and potassium dihydrogen phosphate to prepare Fe3O4/Ag3PO4Composite photocatalyst [ chenchenyang and the like, visible light catalytic performance of ferroferric oxide coated silver phosphate composite photocatalyst, chemical research, 2012, 23 (5): 61-65]. Manganese ions (Mn) are prepared from manganese acetate, silver nitrate and disodium hydrogen phosphate by a hydrothermal method2+) Doped Ag3PO4Photocatalysts [ such as Domnaun, hydrothermally synthesized manganese ion doped silver phosphate and photocatalytic performance thereof, inorganic salt industry, 2017, 49 (6): 90-93]. Although the raw material cost of the composite photocatalyst doped with iron or manganese is reduced, the preparation needs to be carried out in a high-pressure reaction kettle or a hydrothermal kettle, has higher requirements on equipment and reaction conditions, and is compatible with pure Ag3PO4In contrast, the photocatalytic performance is also reduced.
The invention provides an Ag composite photocatalyst for overcoming the defects of silver phosphate composite photocatalysts reported in the prior literature and a preparation method thereof3PO4/AlPO4Composite photocatalyst and preparation method thereof. The innovation point of the invention is that aluminum phosphate and silver phosphate are coprecipitated by a liquid phase precipitation method to form a heterostructure Ag3PO4/AlPO4The compound not only reduces the cost of the photocatalyst, but also simplifies the preparation process and simultaneously improves the catalytic activity of the photocatalyst. The reaction system comprises the following components: aluminum nitrate [ Al (NO)3)3]Silver nitrate (AgNO)3) Phosphate, nitric acid (HNO)3) Sodium hydroxide (NaOH), polystyrene emulsion. The adopted technical scheme is as follows: adding an aluminum nitrate aqueous solution, a silver nitrate aqueous solution, a phosphate aqueous solution and a certain amount of polystyrene emulsion with a solid content of 10% into a reactor with a stirrer, adjusting the pH value of the solution to 1.0 by using nitric acid, gradually dropwise adding a sodium hydroxide aqueous solution under stirring to gradually increase the pH value of the solution until yellow precipitates are generated in the solution, and continuously dropwise adding an excessive sodium hydroxide aqueous solution until the pH value of the solution reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake with deionized water for 3 times, calcining the filter cake in a tubular furnace at 300-500 ℃ for 0.5-3 hours, and cooling to obtain golden yellow Ag3PO4/AlPO4A composite photocatalyst is provided. According to Ag3PO4And AlPO4The prepared composite photocatalyst is marked as (Ag)3)x(Al)yPO4Wherein x is Ag3PO4Y is AlPO4The amount fraction of substance(s) of (c).
Al (NO) as described above3)3The concentration of (A) is as follows: 0.01 to 0.3 mol.L-1，AgNO3The concentration of (A) is as follows: 0.01 to 0.54 mol.L-1。
Ag as described above3PO4/AlPO4In the composite photocatalyst, Ag3PO4And AlPO4The ratio of the amount fraction of the substance(s) is 9: 1 to 5: 5.
The phosphate salt is, as mentioned above, diammonium hydrogen phosphate [ (NH)4)2HPO4]Ammonium dihydrogen phosphate [ NH ]4H2PO4]Disodium hydrogen phosphate [ Na ]2HPO4]Phosphorus, phosphorusSodium dihydrogen acid [ NaH ]2PO4]Dipotassium hydrogen phosphate [ K ]2HPO4]Potassium dihydrogen phosphate [ KH ]2PO4]Sodium phosphate [ Na ]3PO4]Or mixtures thereof, and the like.
The usage amount of the polystyrene emulsion with the solid content of 10% is 0.5-1.0% of the total volume of the aluminum nitrate aqueous solution, the silver nitrate aqueous solution and the phosphate aqueous solution.
Ag prepared by the invention3PO4/AlPO4The shape of the composite photocatalyst particles is strip, the length is 3-5 micrometers, and the length-diameter ratio is 5-10.
Ag prepared by the invention3PO4/AlPO4The composite photocatalyst has excellent photocatalytic performance. When the solid-liquid ratio (namely the mass of the photocatalyst/the volume of the aqueous solution) is 50mg/100mL, the aqueous solution with the concentration of 10mg/L methylene blue or rhodamine B is irradiated by visible light with the wavelength of more than 400nm for 3min, the decolorization rate reaches more than 90 percent, and the composite photocatalyst can be recycled for 4 times. When an aqueous solution with the concentration of 30mg/L methylene blue or rhodamine B is irradiated, Ag3PO4/AlPO4The photocatalysis effect of the composite photocatalyst is obviously better than that of pure Ag3PO4A photocatalyst.
Detailed Description
The invention is further illustrated by the following examples, but is not limited thereto.
Example 1A stirred reactor was charged with 0.01 mol. L-1Al(NO3)30.27 mol. L of an aqueous solution- 1AgNO30.1 mol. L of an aqueous solution-1100mL of diammonium phosphate aqueous solution is added, 1.5mL of polystyrene emulsion with 10% of solid content is added, the pH value of the solution is adjusted to 1.0 by nitric acid, then sodium hydroxide aqueous solution is dropwise added under stirring until yellow precipitate is generated, and the excessive sodium hydroxide aqueous solution is continuously dropwise added until the pH value reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake with deionized water for 3 times, finally calcining the filter cake in a tubular furnace at 300-500 ℃ for 3 hours, and cooling to obtain the golden yellowAg with strip-shaped color appearance3PO4/AlPO4Composite photocatalyst [ marked as (Ag)3)0.9(Al)0.1PO4】。
Example 2A stirred reactor was charged with 0.02 mol. L-1Al(NO3)30.24 mol. L of an aqueous solution- 1AgNO30.1 mol. L of an aqueous solution-1100mL of each disodium hydrogen phosphate aqueous solution is added with 3.0mL of polystyrene emulsion with the solid content of 10 percent, the pH value of the solution is adjusted to 1.0 by nitric acid, then sodium hydroxide aqueous solution is dropwise added under stirring until yellow precipitate is generated, and excessive sodium hydroxide aqueous solution is continuously dropwise added until the pH value reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake with deionized water for 3 times, finally calcining the filter cake in a tubular furnace at 300-500 ℃ for 3 hours, and cooling to obtain golden yellow Ag in the shape of a strip3PO4/AlPO4Composite photocatalyst [ marked as (Ag)3)0.8(Al)0.2PO4】。
Example 3 to a stirred reactor, 0.03 mol. L-1Al(NO3)30.21 mol. L of an aqueous solution- 1AgNO30.1 mol. L of an aqueous solution-1100mL of each dipotassium phosphate aqueous solution is added with 3.0mL of polystyrene emulsion with the solid content of 10 percent, the pH value of the solution is adjusted to 1.0 by nitric acid, then sodium hydroxide aqueous solution is dropwise added under stirring until yellow precipitate is generated, and the dropwise addition of excessive sodium hydroxide aqueous solution is continued until the pH value reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake with deionized water for 3 times, finally calcining the filter cake in a tubular furnace at 300-500 ℃ for 3 hours, and cooling to obtain golden yellow Ag in the shape of a strip3PO4/AlPO4Composite photocatalyst [ marked as (Ag)3)0.7(Al)0.3PO4】。
Example 4A stirred reactor was charged with 0.04 mol. L-1Al(NO3)30.18 mol. L of an aqueous solution- 1AgNO30.1 mol. L of an aqueous solution-1100mL of ammonium dihydrogen phosphate aqueous solution is added, 2.0mL of polystyrene emulsion with the solid content of 10% is added, the pH value of the solution is adjusted to 1.0 by nitric acid, then sodium hydroxide aqueous solution is dropwise added under stirring until yellow precipitate is generated, and the dropwise addition of excessive sodium hydroxide aqueous solution is continued until the pH value of the solution reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake with deionized water for 3 times, finally calcining the filter cake in a tubular furnace at 300-500 ℃ for 3 hours, and cooling to obtain golden yellow Ag in the shape of a strip3PO4/AlPO4Composite photocatalyst [ marked as (Ag)3)0.6(Al)0.4PO4】。
Example 5A stirred reactor was charged with 0.05 mol. L-1Al(NO3)30.15 mol. L of an aqueous solution- 1AgNO30.1 mol. L of an aqueous solution-1100mL of each sodium dihydrogen phosphate aqueous solution is added with 2.5mL of polystyrene emulsion with the solid content of 10 percent, the pH value of the solution is adjusted to 1.0 by nitric acid, then sodium hydroxide aqueous solution is dropwise added under stirring until yellow precipitate is generated, and the excessive sodium hydroxide aqueous solution is continuously dropwise added until the pH value of the solution reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake with deionized water for 3 times, finally calcining the filter cake in a tubular furnace at 300-500 ℃ for 3 hours, and cooling to obtain golden yellow Ag in the shape of a strip3PO4/AlPO4Composite photocatalyst [ marked as (Ag)3)0.5(Al)0.5PO4】。
Example 6A stirred reactor was charged with 0.01 mol. L-1Al(NO3)30.27 mol. L of an aqueous solution- 1AgNO30.1 mol. L of an aqueous solution-1100mL of potassium dihydrogen phosphate aqueous solution is added, 1.5mL of polystyrene emulsion with the solid content of 10% is added, the pH value of the solution is adjusted to 1.0 by nitric acid, then sodium hydroxide aqueous solution is dropwise added under stirring until yellow precipitate is generated, and the dropwise addition of excessive sodium hydroxide aqueous solution is continued until the pH value of the solution reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake for 3 times by using deionized water, and finally, washing the filter cakeCalcining the filter cake in a tubular furnace at 300-500 ℃ for 3 hours, and cooling to obtain golden yellow strip-shaped Ag3PO4/AlPO4Composite photocatalyst [ marked as (Ag)3)0.9(Al)0.1PO4】。
Example 7A stirred reactor was charged with 0.02 mol. L-1Al(NO3)30.24 mol. L of an aqueous solution- 1AgNO30.1 mol. L of an aqueous solution-1100mL of each sodium phosphate aqueous solution, then adding 3.0mL of polystyrene emulsion with the solid content of 10%, adjusting the pH value of the solution to 1.0 by using nitric acid, then dropwise adding a sodium hydroxide aqueous solution under stirring until yellow precipitate is generated, and continuously dropwise adding an excessive sodium hydroxide aqueous solution until the pH value of the solution reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake with deionized water for 3 times, finally calcining the filter cake in a tubular furnace at 300-500 ℃ for 3 hours, and cooling to obtain golden yellow Ag in the shape of a strip3PO4/AlPO4Composite photocatalyst [ marked as (Ag)3)0.8(Al)0.2PO4】。
Example 8 charging of 100ml 0.02mol. L into a stirred reactor-1Al(NO3)3Aqueous solution, 100 mL0.24mol. L-1AgNO3Aqueous solution, 50 mL0.1mol. L-1Diammonium phosphate and 50 mL0.1mol.L-1Adding 3.0mL of polystyrene emulsion with the solid content of 10% into the aqueous solution of ammonium dihydrogen phosphate, adjusting the pH value of the solution to 1.0 by using nitric acid, then dropwise adding an aqueous solution of sodium hydroxide under stirring until yellow precipitate is generated, and continuously dropwise adding an excessive aqueous solution of sodium hydroxide until the pH value of the solution reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake with deionized water for 3 times, finally calcining the filter cake in a tubular furnace at 300-500 ℃ for 3 hours, and cooling to obtain golden yellow Ag in the shape of a strip3PO4/AlPO4Composite photocatalyst [ marked as (Ag)3)0.8(Al)0.2PO4】。
Example 9 charging of 100ml 0.03mol. cndot. in a stirred reactorL-1Al(NO3)3Aqueous solution, 100 mL0.21mol. L-1AgNO3Aqueous solution, 50 mL0.1mol. L-1Diammonium phosphate and 50 mL0.1mol.L-1Adding 3.0mL of polystyrene emulsion with the solid content of 10% into an aqueous solution of disodium hydrogen phosphate, adjusting the pH value of the solution to 1.0 by using nitric acid, then dropwise adding an aqueous solution of sodium hydroxide under stirring until yellow precipitate is generated, and continuously dropwise adding an excessive aqueous solution of sodium hydroxide until the pH value of the solution reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake with deionized water for 3 times, finally calcining the filter cake in a tubular furnace at 300-500 ℃ for 3 hours, and cooling to obtain golden yellow Ag in the shape of a strip3PO4/AlPO4Composite photocatalyst [ marked as (Ag)3)0.7(Al)0.3PO4】。
Example 10 charging of 100ml 0.04mol. L into a stirred reactor-1Al(NO3)3Aqueous solution, 100 mL0.18mol. L-1AgNO3Aqueous solution, 50 mL0.1mol. L-1Disodium hydrogen phosphate and 50 mL0.1mol.L-1Adding 3.0mL of polystyrene emulsion with the solid content of 10% into aqueous solution of dipotassium phosphate, adjusting the pH value of the solution to 1.0 by using nitric acid, then dropwise adding aqueous solution of sodium hydroxide under stirring until yellow precipitate is generated, and continuously dropwise adding excessive aqueous solution of sodium hydroxide until the pH value of the solution reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake with deionized water for 3 times, finally calcining the filter cake in a tubular furnace at 300-500 ℃ for 3 hours, and cooling to obtain golden yellow Ag in the shape of a strip3PO4/AlPO4Composite photocatalyst [ marked as (Ag)3)0.7(Al)0.3PO4】。
Example 11 charging of 100ml 0.02mol. L into a stirred reactor-1Al(NO3)3Aqueous solution, 100 mL0.54mol. L-1AgNO3Aqueous solution, 50 mL0.2mol.L-1Disodium hydrogen phosphate and 50 mL0.2mol.L-1Sodium phosphate in water, then 3.0mL of a 10% solids polystyrene emulsion was added and the solution was adjusted with nitric acidThe pH value is 1.0, then sodium hydroxide aqueous solution is dropwise added under stirring until yellow precipitate is generated, and excessive sodium hydroxide aqueous solution is continuously dropwise added until the pH value of the solution reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake with deionized water for 3 times, finally calcining the filter cake in a tubular furnace at 300-500 ℃ for 3 hours, and cooling to obtain golden yellow Ag in the shape of a strip3PO4/AlPO4Composite photocatalyst [ marked as (Ag)3)0.9(Al)0.1PO4】。
Example 12 charging of 100ml0.1 mol. L into a stirred reactor-1Al(NO3)3Aqueous solution, 100 mL0.3mol. L-1AgNO3Aqueous solution, 50 mL0.2mol.L-1Disodium hydrogen phosphate and 50 mL0.2mol.L-1Adding 3.0mL of polystyrene emulsion with the solid content of 10% into aqueous solution of sodium dihydrogen phosphate, adjusting the pH value of the solution to 1.0 by using nitric acid, then dropwise adding aqueous solution of sodium hydroxide under stirring until yellow precipitate is generated, and continuously dropwise adding excessive aqueous solution of sodium hydroxide until the pH value of the solution reaches 4.0; standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake with deionized water for 3 times, finally calcining the filter cake in a tubular furnace at 300-500 ℃ for 3 hours, and cooling to obtain golden yellow Ag in the shape of a strip3PO4/AlPO4Composite photocatalyst [ marked as (Ag)3)0.5(Al)0.5PO4】。
Claims (5)
1. Ag3PO4/AlPO4The composite photocatalyst and the preparation method thereof are characterized in that: adding an aluminum nitrate aqueous solution, a silver nitrate aqueous solution, a phosphate aqueous solution and a certain amount of polystyrene emulsion with a solid content of 10% into a reactor with stirring, adjusting the pH value of the solution to 1.0 by using nitric acid, gradually dropwise adding a sodium hydroxide aqueous solution under stirring to gradually increase the pH value of the solution until yellow precipitates are generated in the solution, and continuously dropwise adding an excessive sodium hydroxide aqueous solution until the pH value of the solution reaches 4.0. Standing the slurry obtained by the reaction for 30 minutes, filtering, washing the filter cake for 3 times by using deionized water, and thenCalcining the filter cake in a tubular furnace at 300-500 ℃ for 0.5-3 hours, and cooling to obtain golden yellow Ag3PO4/AlPO4A composite photocatalyst is provided.
2. Ag according to claim 13PO4/AlPO4The composite photocatalyst and the preparation method thereof are characterized in that: said Al (NO)3)3The concentration of (A) is as follows: 0.01 to 0.3 mol.L-1，AgNO3The concentration of (A) is as follows: 0.01 to 0.54 mol.L-1。
3. Ag according to claim 13PO4/AlPO4The composite photocatalyst and the preparation method thereof are characterized in that: the Ag is3PO4/AlPO4In the composite photocatalyst, Ag3PO4And AlPO4The ratio of the amount fraction of the substance(s) is 9: 1 to 5: 5.
4. Ag according to claim 13PO4/AlPO4The composite photocatalyst and the preparation method thereof are characterized in that: the phosphate is diammonium hydrogen phosphate [ (NH)4)2HPO4]Ammonium dihydrogen phosphate [ NH ]4H2PO4]Disodium hydrogen phosphate [ Na ]2HPO4]Sodium dihydrogen phosphate [ NaH ]2PO4]Dipotassium hydrogen phosphate [ K ]2HPO4]Potassium dihydrogen phosphate [ KH ]2PO4]Sodium phosphate [ Na ]3PO4]Or mixtures thereof, and the like.
5. Ag according to claim 13PO4/AlPO4The composite photocatalyst and the preparation method thereof are characterized in that: the usage amount of the polystyrene emulsion with the solid content of 10% is 0.5-1.0% of the total volume of the aluminum nitrate aqueous solution, the silver nitrate aqueous solution and the phosphate aqueous solution.
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| CN113244950A (en) * | 2021-05-26 | 2021-08-13 | 贵州省化工研究院 | Composite carrier photocatalyst and application thereof |
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