CN114029090B - 一种去除污水重金属的光催化剂的制备方法 - Google Patents
一种去除污水重金属的光催化剂的制备方法 Download PDFInfo
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- CN114029090B CN114029090B CN202111560651.2A CN202111560651A CN114029090B CN 114029090 B CN114029090 B CN 114029090B CN 202111560651 A CN202111560651 A CN 202111560651A CN 114029090 B CN114029090 B CN 114029090B
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- bismuth
- photocatalyst
- metal oxide
- based multi
- heavy metals
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 28
- 239000010865 sewage Substances 0.000 title claims abstract description 15
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 34
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000013299 conductive metal organic framework Substances 0.000 claims abstract description 28
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 23
- 229910052751 metal Chemical class 0.000 claims abstract description 16
- 239000002184 metal Chemical class 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 150000001621 bismuth Chemical class 0.000 claims abstract description 7
- 239000013110 organic ligand Substances 0.000 claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000012702 metal oxide precursor Substances 0.000 claims abstract description 6
- 239000000654 additive Substances 0.000 claims abstract description 3
- 230000000996 additive effect Effects 0.000 claims abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 8
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 4
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- OWSZUKMVEBFJMZ-UHFFFAOYSA-N benzene-1,2,3,4,5,6-hexamine Chemical compound NC1=C(N)C(N)=C(N)C(N)=C1N OWSZUKMVEBFJMZ-UHFFFAOYSA-N 0.000 claims description 4
- ANUAIBBBDSEVKN-UHFFFAOYSA-N benzene-1,2,4,5-tetramine Chemical compound NC1=CC(N)=C(N)C=C1N ANUAIBBBDSEVKN-UHFFFAOYSA-N 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 3
- IHIXIJGXTJIKRB-UHFFFAOYSA-N trisodium vanadate Chemical compound [Na+].[Na+].[Na+].[O-][V]([O-])([O-])=O IHIXIJGXTJIKRB-UHFFFAOYSA-N 0.000 claims description 3
- SATWKVZGMWCXOJ-UHFFFAOYSA-N 4-[3,5-bis(4-carboxyphenyl)phenyl]benzoic acid Chemical compound C1=CC(C(=O)O)=CC=C1C1=CC(C=2C=CC(=CC=2)C(O)=O)=CC(C=2C=CC(=CC=2)C(O)=O)=C1 SATWKVZGMWCXOJ-UHFFFAOYSA-N 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- HJCNSOVRAZFJLK-UHFFFAOYSA-N C1=CC(C(=O)O)=CC=C1C1=CC2=CC([N]3)=CC=C3C=C(C=C3)NC3=CC([N]3)=CC=C3C=C1N2 Chemical compound C1=CC(C(=O)O)=CC=C1C1=CC2=CC([N]3)=CC=C3C=C(C=C3)NC3=CC([N]3)=CC=C3C=C1N2 HJCNSOVRAZFJLK-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 2
- 229930195725 Mannitol Natural products 0.000 claims description 2
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 2
- NVGVNJDFTHQFQR-UHFFFAOYSA-N benzene-1,2,3,4,5,6-hexathiol Chemical compound SC1=C(S)C(S)=C(S)C(S)=C1S NVGVNJDFTHQFQR-UHFFFAOYSA-N 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- RBTKNAXYKSUFRK-UHFFFAOYSA-N heliogen blue Chemical compound [Cu].[N-]1C2=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=NC([N-]1)=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=N2 RBTKNAXYKSUFRK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 239000000594 mannitol Substances 0.000 claims description 2
- 235000010355 mannitol Nutrition 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- PNYYBUOBTVHFDN-UHFFFAOYSA-N sodium bismuthate Chemical compound [Na+].[O-][Bi](=O)=O PNYYBUOBTVHFDN-UHFFFAOYSA-N 0.000 claims description 2
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
- NAFSMMJPUQZBRJ-UHFFFAOYSA-N Cl.[Bi] Chemical compound Cl.[Bi] NAFSMMJPUQZBRJ-UHFFFAOYSA-N 0.000 claims 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims 1
- AZOOXWWPWARTFV-UHFFFAOYSA-N zirconium hydrochloride Chemical compound Cl.[Zr] AZOOXWWPWARTFV-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 15
- 239000012621 metal-organic framework Substances 0.000 abstract description 6
- 239000000969 carrier Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 238000013329 compounding Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 25
- 230000001699 photocatalysis Effects 0.000 description 15
- 239000003054 catalyst Substances 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 239000012921 cobalt-based metal-organic framework Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- DKUYEPUUXLQPPX-UHFFFAOYSA-N dibismuth;molybdenum;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mo].[Mo].[Bi+3].[Bi+3] DKUYEPUUXLQPPX-UHFFFAOYSA-N 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910000380 bismuth sulfate Inorganic materials 0.000 description 2
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- BEQZMQXCOWIHRY-UHFFFAOYSA-H dibismuth;trisulfate Chemical compound [Bi+3].[Bi+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BEQZMQXCOWIHRY-UHFFFAOYSA-H 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 2
- YMKHJSXMVZVZNU-UHFFFAOYSA-N manganese(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YMKHJSXMVZVZNU-UHFFFAOYSA-N 0.000 description 2
- 239000013239 manganese-based metal-organic framework Substances 0.000 description 2
- 239000013099 nickel-based metal-organic framework Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 241001198704 Aurivillius Species 0.000 description 1
- 239000013255 MILs Substances 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012924 metal-organic framework composite Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 230000001443 photoexcitation Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
- B01J31/181—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine
- B01J31/1815—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine with more than one complexing nitrogen atom, e.g. bipyridyl, 2-aminopyridine
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2213—At least two complexing oxygen atoms present in an at least bidentate or bridging ligand
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/34—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of chromium, molybdenum or tungsten
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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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/70—Complexes comprising metals of Group VII (VIIB) as the central metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/845—Cobalt
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- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/847—Nickel
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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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
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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Abstract
本发明公开了一种去除污水重金属的光催化剂的制备方法，其包括以下步骤：S1：将铋盐和金属盐加入到溶剂A中，充分搅拌溶解，形成铋基多金属氧化物前驱体溶液；S2：将铋基多金属氧化物前驱体溶液放入高压反应釜中，在120‑200度下水热反应6‑48h，过滤后再清洗干燥，得到铋基多金属氧化物；S3：将金属源、有机配体和添加剂加入到溶剂B中，充分搅拌溶解，形成导电MOF前驱体溶液；S4：将步骤S2制得的铋基多金属氧化物加入到导电MOF前驱体溶液中，搅拌充分溶解，然后在25‑150度下反应2‑48h，过滤清洗干燥，得到铋基多金属氧化物/导电MOF复合光催化剂。本发明可以解决采用MOF材料为载体，复合其他半导体材料形成的光催化剂活性差的问题。
Description
技术领域
本发明涉及光催化材料技术领域，尤其涉及一种去除污水重金属的光催化剂的制备方法。
背景技术
生活中用的自来水中常常含有重金属(如Cr、Cd、Pb等)，对人体及动植物的健康造成严重威胁。目前，光催化处理污水被认为是一种有前途的方法，具有Aurivillius层状特征的铋基多金属氧化物(BiMOx)，具有优异的物化性质、独特的铁电性能、催化性能等，是一类很好的可见光催化剂，在光催化中展示出较大的优势。但BiMOx的光量子效率低、电子空穴易复合，通过形貌、结构、组分的优化，调控带隙结构、抑制光生载流子的复合，是提高其光催化性能的关键。导电金属有机骨架(MOF)材料不仅具有传统MOF材料的超高比表面积，多孔性和可调控结构等性质，有利于污染物和产物的吸附扩散，形成光催化的理想反应平台；而且导电MOF材料还具有较高的导电率，利于提高光催化剂的光生载流子分离效率。
中国专利CN 110047657A介绍了一种MIL系列MOF复合掺钼钒酸铋光阳极及其制备方法，通过掺钼的钒酸铋和MOF材料复合，提高光阳极的光电流。
中国专利CN 103657634 A采用石墨烯为载体，修饰钼酸铋纳米带，得到一种在太阳光下具有强吸附、高光催化活性的新型光催化剂。发明人认为石墨烯较强的电子传导能力和电子储存能力，能捕获和传导光激发电子，阻碍半导体催化剂中光生载流子的复合。
Zhu等(Selective Reduction of CO2 by Conductive MOF Nanosheets as anEfficient Co-catalyst under Visible Light Illumination)首次将导电MOF材料用于光催化CO2还原的助催化剂，发现导电MOF中二维共轭的π电子以及丰富的Ni-N4活性位，使其具备高导电性和高活性。
Zhao等(Carbon nitride assisted 2D conductive metal-organic frameworkscomposite photocatalyst for efficient visible light-driven H2O2 production)以C3N4为载体，负载二维导电MOF(Ni-CAT)，得到Ni-CAT/C3N4复合光催化剂，与单纯的C3N4或Ni-CAT相比，发现Ni-CAT/C3N4复合光催化剂在可将光下催化氧还原为H2O2的效率呈指数级提高。在可见光照射下，CN上产生的电子会转移到Ni-CAT上，从而抑制Ni-CAT的载流子复合，使Ni-CAT上有更多电子进行氧还原反应，CN上留下更多空穴可用于水氧化反应。
但是，目前大多采用传统的MOF材料为载体，复合其他半导体材料形成光催化剂，其催化性能、稳定性还有待进一步加强。
发明内容
本发明的目的在于：为了解决现有技术中采用MOF材料为载体，复合其他半导体材料形成的光催化剂活性差的问题，而提供的一种去除污水重金属的光催化剂的制备方法。
为了实现上述目的，本发明提供了一种去除污水重金属的光催化剂的制备方法，其包括以下步骤：
S1：将铋盐和金属盐加入到溶剂A中，并调节pH值为2～10，充分搅拌溶解，形成铋基多金属氧化物前驱体溶液；
S2：将所述铋基多金属氧化物前驱体溶液放入高压反应釜中，在120-200度下水热反应6-48h，过滤后再清洗干燥，得到铋基多金属氧化物；
S3：将金属源、有机配体和添加剂加入到溶剂B中，充分搅拌溶解，形成导电MOF前驱体溶液；
S4：将步骤S2制得的所述铋基多金属氧化物加入到所述导电MOF前驱体溶液中，搅拌使所述铋基多金属氧化物充分溶解，然后在25-150度下反应2-48h，过滤清洗干燥，得到铋基多金属氧化物/导电MOF复合光催化剂。
为上述技术方案的进一步描述：
所述步骤S1中铋盐为铋的盐酸盐、硫酸盐、硝酸盐或铋酸钠中的任一一种或至少两种的组合。
为上述技术方案的进一步描述：
所述步骤S1中的金属盐为钼酸钠、钼酸铵、钨酸钠、钨酸铵、正钒酸钠、偏钒酸铵或偏钒酸钠中的任一一种或至少两种的组合。
作为上述技术方案的进一步描述：
所述步骤S1中的溶剂A为水、乙醇、乙二醇、丙三醇或甘露醇中的任一一种或至少两种的组合。
作为上述技术方案的进一步描述：
所述步骤S1中的铋盐、金属盐和溶剂A的摩尔比为2∶1∶20～200。
作为上述技术方案的进一步描述：
所述步骤S3中的金属源为铁、钴、镍、铜、锰、锆的盐酸盐、硝酸盐、硫酸盐、醋酸盐中的任一一种或至少两种的组合。
作为上述技术方案的进一步描述：
所述步骤S3中的有机配体为六氨基苯、2，3，6，7，10，11-六亚氨基三苯、2，3，6，7，10，11-六羟基三苯、1，2，4，5-苯四胺、苯六硫醇、5，10，15，20-四(4-羧基苯基)卟啉、1，4-苯二吡唑酯、2，3，9，10，16，17，23，24-八氨基铜酞菁、或1，3，5-三(4-羧基苯基)苯中的任一一种或至少两种的组合。
作为上述技术方案的进一步描述：
所述步骤S3中的溶剂B为二甲基亚砜、N，N-二甲基甲酰胺或水中的任一一种或至少两种的组合，金属源与溶剂B的质量比为1∶50-200。
作为上述技术方案的进一步描述：
所述步骤S3中的金属源：有机配体的摩尔比为10∶1～1∶10。
作为上述技术方案的进一步描述：
所述步骤S4中的铋基多金属氧化物与导电MOF的质量比为0.1∶1～10∶1。
综上所述，由于采用了上述技术方案，本发明的有益效果是：本发明的铋基多金属氧化物/导电MOF复合材料，集合了导电MOF的高比表面积、高孔隙率、高导电性、高稳定性的特征，同时还可以调节铋基多金属氧化物的带隙宽度，有利于提高光生电子/空穴的分离效率，达到增强光催化效率的目的。
具体实施方式
下面将更详细地描述本公开的示例性实施例。虽然显示了本公开的示例性实施例，然而应当理解，可以以各种形式实现本公开而不应被这里阐述的实施例所限制。相反，提供这些实施例是为了能够更透彻地理解本公开，并且能够将本公开的范围完整的传达给本领域的技术人员。
实施例一：
称取1.0mmol的硝酸铋、0.5mmol的钼酸铵，加入到40ml的乙醇中，充分搅拌溶解，形成钼酸铋(Bi2MoO6)的前驱体溶液；在高压反应釜中，在160度下，反应24h，清洗干燥，得到Bi2MoO6；称取1.0mmol的四水合醋酸钴、6.0mmol的2，3，6，7，10，11-六羟基三苯，加入到50ml的N，N-二甲基甲酰胺/水(体积比为1∶4)混合溶液中，充分搅拌溶解，形成导电Co-MOF的前驱体溶液；在上述溶液中加入0.2g Bi2MoO6，搅拌使其充分分散；在110度下反应18h，清洗干燥，得到Bi2MoO6/导电Co-MOF复合催化剂。
实施例二：
称取1.0mmol的硫酸铋、0.5mmol的钨酸钠，加入到50ml的乙醇/乙二醇混合溶液(体积比为4∶1)中，充分搅拌溶解，形成钨酸铋(Bi2WO6)的前驱体溶液；在高压反应釜中，在180度下，反应12h，清洗干燥，得到Bi2WO6；称取1.0mmol的六水合氯化镍、1.0mmol的1，2，4，5-苯四胺，加入到120ml的去离子水中，充分搅拌溶解，形成导电Ni-MOF的前驱体溶液；在上述溶液中加入0.5gBi2WO6，搅拌使其充分分散；在60度下反应2h，清洗干燥，得到Bi2WO6/导电Ni-MOF复合催化剂。
实施例三：
称取1.0mmol的硫酸铋、0.5mmol的正钒酸钠，加入到100ml的去离子水中，充分搅拌溶解，形成钒酸铋(BiVO4)的前驱体溶液；在高压反应釜中，在200度下，反应6h，清洗干燥，得到BiVO4；称取1.0mmol的六水合硝酸锰、1.0mmol的六氨基苯，加入到60ml的二甲基亚砜中，再加入3ml浓氨水，充分搅拌溶解，形成导电Mn-MOF的前驱体溶液；在上述溶液中加入上述制得的0.1gBiVO4，搅拌使其充分分散，在60度下反应2h，清洗干燥，得到BiVO4/导电Mn-MOF复合催化剂。
对比例一：
称取1.0mmol的硝酸铋、0.5mmol的钼酸铵，加入到40ml的乙醇中，充分搅拌溶解，形成钼酸铋(Bi2MoO6)的前驱体溶液；在高压反应釜中，在160度下，反应24h，清洗干燥，得到Bi2MoO6。
对比例二：
称取1.0mmol的四水合醋酸钴、6.0mmol的2，3，6，7，10，11-六羟基三苯，加入到50ml的N，N-二甲基甲酰胺/水(体积比为1∶4)混合溶液中，充分搅拌溶解，形成导电Co-MOF的前驱体溶液；上述溶液在110度下反应18h，清洗干燥，得到导电Co-MOF。
利用光催化反应仪验证催化材料对于含Cr(VI)污水的光催化净化性能，具体为：
通过对比反应前后Cr(VI)的量来确定催化剂的催化效果，其中，Cr(VI)去除率(％)＝(Cr(VI)反应前-Cr(VI)反应后)÷Cr(VI)反应前×100。经过光催化反应的Cr(VI)的光催化净化效果如表1所示。
表1为实施例及对比实施例制备的催化剂光催化净化含Cr(VI)污水的性能。
由表1可以看出，在相同的反应条件下，铋基多金属氧化物/导电MOF复合光催化剂对Cr(VI)的去除效率的明显高于单纯的铋基多金属氧化物、单纯的导电MOF对Cr(VI)的去除效率，且铋基多金属氧化物/导电MOF复合光催化剂循环6次后的催化效率下降也不多，可以看出铋基多金属氧化物/导电MOF复合光催化的重复使用后的催化效率也很高。
本发明通过将铋基多金属氧化物与导电MOF复合，形成铋基多金属氧化物/导电MOF复合材料，集合了导电MOF的高比表面积、高孔隙率、高导电性、高稳定性的特征，同时还可以调节铋基多金属氧化物的带隙宽度，有利于提高光生电子/空穴的分离效率，达到增强光催化效率的目的。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。
Claims (7)
1.一种去除污水重金属的光催化剂的制备方法，其特征在于，包括以下步骤：
S1：将铋盐和金属盐加入到溶剂A中，并调节pH值为2～10，充分搅拌溶解，形成铋基多金属氧化物前驱体溶液,溶剂A为水、乙醇、乙二醇、丙三醇或甘露醇中的任一一种或至少两种的组合；
S2：将所述铋基多金属氧化物前驱体溶液放入高压反应釜中，在120-200度下水热反应6-48h，过滤后再清洗干燥，得到铋基多金属氧化物；
S3：将金属源、有机配体和添加剂加入到溶剂B中，充分搅拌溶解，形成导电MOF前驱体溶液,有机配体为六氨基苯、2,3,6,7,10,11-六亚氨基三苯、2,3,6,7,10,11-六羟基三苯、1,2,4,5-苯四胺、苯六硫醇、5,10,15,20-四(4-羧基苯基)卟啉、1,4-苯二吡唑酯、2,3,9,10,16,17,23,24-八氨基铜酞菁、或1,3,5-三(4-羧基苯基)苯中的任一一种或至少两种的组合,溶剂B为二甲基亚砜、N,N-二甲基甲酰胺或水中的任一一种或至少两种的组合，金属源与溶剂B的质量比为1：50-200；
S4：将步骤S2制得的所述铋基多金属氧化物加入到所述导电MOF前驱体溶液中，搅拌使所述铋基多金属氧化物充分溶解，然后在25-150度下反应2-48h，过滤清洗干燥，得到铋基多金属氧化物/导电MOF复合光催化剂。
2.根据权利要求1所述的一种去除污水重金属的光催化剂的制备方法，其特征在于，所述步骤S1中铋盐为铋的盐酸盐、硫酸盐、硝酸盐或铋酸钠中的任一一种或至少两种的组合。
3.根据权利要求1所述的一种去除污水重金属的光催化剂的制备方法，其特征在于，所述步骤S1中的金属盐为钼酸钠、钼酸铵、钨酸钠、钨酸铵、正钒酸钠、偏钒酸铵或偏钒酸钠中的任一一种或至少两种的组合。
4.根据权利要求1所述的一种去除污水重金属的光催化剂的制备方法，其特征在于，所述步骤S1中的铋盐、金属盐和溶剂A的摩尔比为2：1：20～200。
5.根据权利要求1所述的一种去除污水重金属的光催化剂的制备方法，其特征在于，所述步骤S3中的金属源为铁、钴、镍、铜、锰、锆的盐酸盐、硝酸盐、硫酸盐、醋酸盐中的任一一种或至少两种的组合。
6.根据权利要求1所述的一种去除污水重金属的光催化剂的制备方法，其特征在于，所述步骤S3中的金属源：有机配体的摩尔比为10：1～1：10。
7.根据权利要求1所述的一种去除污水重金属的光催化剂的制备方法，其特征在于，所述步骤S4中的铋基多金属氧化物与导电MOF的质量比为0.1:1～10:1。
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