CN106975496A - 抑菌催化还原多孔材料及其制备和在生产还原水上的应用 - Google Patents
抑菌催化还原多孔材料及其制备和在生产还原水上的应用 Download PDFInfo
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- CN106975496A CN106975496A CN201710233192.4A CN201710233192A CN106975496A CN 106975496 A CN106975496 A CN 106975496A CN 201710233192 A CN201710233192 A CN 201710233192A CN 106975496 A CN106975496 A CN 106975496A
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- palladium
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- reduction
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 60
- 239000011148 porous material Substances 0.000 title claims abstract description 51
- 230000009467 reduction Effects 0.000 title claims abstract description 44
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 41
- 230000002829 reductive effect Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title abstract description 11
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 43
- 238000006722 reduction reaction Methods 0.000 claims abstract description 43
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000004332 silver Substances 0.000 claims abstract description 21
- 229910052709 silver Inorganic materials 0.000 claims abstract description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000010531 catalytic reduction reaction Methods 0.000 claims abstract description 20
- 238000011065 in-situ storage Methods 0.000 claims abstract description 19
- 230000003115 biocidal effect Effects 0.000 claims abstract description 11
- 230000001603 reducing effect Effects 0.000 claims abstract description 11
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 10
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 230000010757 Reduction Activity Effects 0.000 claims abstract description 9
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000000694 effects Effects 0.000 claims abstract description 9
- 230000008021 deposition Effects 0.000 claims abstract description 7
- 238000011049 filling Methods 0.000 claims abstract description 7
- 238000007540 photo-reduction reaction Methods 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000001257 hydrogen Substances 0.000 claims description 50
- 229910052739 hydrogen Inorganic materials 0.000 claims description 50
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 46
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 14
- 150000000703 Cerium Chemical class 0.000 claims description 10
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 230000033116 oxidation-reduction process Effects 0.000 claims description 9
- 150000002940 palladium Chemical class 0.000 claims description 8
- 230000003385 bacteriostatic effect Effects 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
- ZGMCLEXFYGHRTK-UHFFFAOYSA-N [Fe].[Ce] Chemical compound [Fe].[Ce] ZGMCLEXFYGHRTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004480 active ingredient Substances 0.000 claims description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- 238000002604 ultrasonography Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 230000007423 decrease Effects 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 239000011260 aqueous acid Substances 0.000 claims description 4
- 239000002152 aqueous-organic solution Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 210000000988 bone and bone Anatomy 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000969 carrier Substances 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 2
- 238000007872 degassing Methods 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical group [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 2
- 229940071536 silver acetate Drugs 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims 1
- 239000011790 ferrous sulphate Substances 0.000 claims 1
- LITYQKYYGUGQLY-UHFFFAOYSA-N iron nitric acid Chemical group [Fe].O[N+]([O-])=O LITYQKYYGUGQLY-UHFFFAOYSA-N 0.000 claims 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- JKDRQYIYVJVOPF-FDGPNNRMSA-L palladium(ii) acetylacetonate Chemical compound [Pd+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O JKDRQYIYVJVOPF-FDGPNNRMSA-L 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- 235000021419 vinegar Nutrition 0.000 claims 1
- 239000000052 vinegar Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000000151 deposition Methods 0.000 abstract description 6
- 230000001408 fungistatic effect Effects 0.000 abstract description 4
- 238000007598 dipping method Methods 0.000 abstract description 3
- 238000004321 preservation Methods 0.000 abstract description 2
- 238000012859 sterile filling Methods 0.000 abstract 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 11
- 230000001954 sterilising effect Effects 0.000 description 7
- 238000004659 sterilization and disinfection Methods 0.000 description 7
- 150000002431 hydrogen Chemical class 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 229910052613 tourmaline Inorganic materials 0.000 description 3
- 229940070527 tourmaline Drugs 0.000 description 3
- 239000011032 tourmaline Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- 208000017667 Chronic Disease Diseases 0.000 description 2
- 241000305071 Enterobacterales Species 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000005030 aluminium foil Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical group [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- -1 stirring 15min Chemical compound 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 208000000913 Kidney Calculi Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 206010029148 Nephrolithiasis Diseases 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- LXNAVEXFUKBNMK-UHFFFAOYSA-N acetic acid;palladium Chemical compound [Pd].CC(O)=O.CC(O)=O LXNAVEXFUKBNMK-UHFFFAOYSA-N 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 201000001883 cholelithiasis Diseases 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 230000037452 priming Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 208000019553 vascular disease Diseases 0.000 description 1
- 238000010792 warming 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/894—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/64—Pore diameter
- B01J35/657—Pore diameter larger than 1000 nm
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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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/68—Treatment of water, waste water, or sewage by addition of specified substances, e.g. trace elements, for ameliorating potable water
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- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/04—Oxidation reduction potential [ORP]
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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
本发明属于新材料技术领域,涉及一种抑菌催化还原多孔材料及其制备方法和在生产还原水上的应用。本发明多孔材料为载体,金属铁、铈、钯为催化还原活性组分,纳米银为抑菌组分,采用浸渍、煅烧、原位催化还原沉积、原位光还原沉积等工艺制备出的催化材料,钯和银均匀分散地负载于多孔载体的孔壁和外层等与水气接触充分的位置,最大限度发挥催化还原功效的同时保证抑菌效果。本发明解决还原水的抑菌性和还原性之间的矛盾,在普通灌装(相对于无菌灌装)条件下实现抑菌保鲜,简化还原水生产工艺,降低成本。由于该材料和器件在强还原性条件下工作,银主要以单质形式存在,不仅损耗少、寿命长,而且不会在水中引入过量的银离子,安全性高。
Description
技术领域
本发明属于新材料技术领域,涉及一种抑菌催化还原多孔材料及其制备方法和在生产还原水上的应用。
背景技术
水是生命之源,水的质量决定了人的生活质量,并对人体健康起着决定性作用。随着生活水平提高,人们对健康饮水的重视程度越来越高,获得更为健康的水成为迫切需要。自2007年日本Ohsawa教授发现氢气可选择性清除人体内的恶性自由基并产生抗氧化作用以来,有关富氢水对人体慢性疾病的防治作用已经成为研究热点,关于氢气在糖尿病、心脑血管疾病、肿瘤防治和美容抗衰老等方面的报道相继出现。氢分子被认为将开创慢性疾病预防治新途径,富氢水也很快被消费者认识并接受,相关的产业和市场具有旺盛的生命力,被称为“氢产业”。
目前制取富氢水的方法主要有富氢镁棒法、电解法、气液混合法、托玛琳杯等。富氢镁棒法是利用镁与水反应生成氢气,电解法是利用阴极还原产生氢气,气液混合法是利用专门的装置使氢气与水混合而制取富氢水。这三种方法均可制取富氢水,但存在各自的不足。富氢镁棒法和电解法分别需要加热装置和电解装置,只适宜家用或定点使用,不便携带,制取的水不能长时间储存,只能现制现饮。不仅如此,以上两种方法一般会使水的硬度升高,既影响口感,也不适合部分人群(如:肾结石、胆结石患者)。气液混合法也存在自身的问题,由于纯净水和矿泉水在灌装之前一般需臭氧杀菌,然后在有臭氧残余的状态下灌装密封,如果在臭氧杀菌之前向水中引入氢,会因绝大部分氢在杀菌时溢出而失去还原功效,如果在臭氧杀菌之后引入活性氢,则难以保证产品的抑菌效果,其可储存性和安全性会出现问题。此外,气液混合法制取富氢水需要较长的时间,水的还原活性也较低,因为氢气在水中的溶解度很低,不易达到有效浓度,而且非新生态氢分子的还原活性也不高;托玛琳杯是利用放置于杯中的电气石、锗石与水发生微弱反应生成少量的氢分子来产生还原性,其缺点是氢气产生量少,水的还原性弱,其电位一般只能达到-100mV左右,不能很好地起到去除人体内有害氧化性物质的功效。
发明内容
本发明的目的在于提供一种抑菌催化还原多孔材料及其制备方法和在生产还原水上的应用,材料上的活性成分均匀分散,具有很好的催化还原功能,可将氢气分解为新生态氢原子存在于水中,使水的氧化还原电位降低到-600mV以下。由于银的存在,材料具有很好的抑菌效果,可在去除水中氧化性成分(主要是臭氧)、引入氢原子的同时,保持水的抑菌性能。与此同时,作为主要催化还原活性组分的钯和作为抑菌活性组分的银可以在还原水生产设备上原位负载,方便在长期运行导致性能降低后进行恢复。
本发明的技术方案是:
一种抑菌催化还原多孔材料,由多元活性组分和多孔载体组成;多元活性组分包括催化还原活性成分和抑菌活性成分,催化还原活性成分为钯、铁、铈的单质、固溶体或氧化物中的至少一种,抑菌活性成分为单质银或银的氧化物;多孔载体为多孔钛骨、多孔钛棒、多孔钛板、多孔镁、多孔锆、多孔锡、活性炭滤芯、陶瓷滤芯、膨胀石墨或活性氧化铝颗粒;催化还原活性成分中,钯的重量百分比为0.01~5wt%,铁的重量百分比为0.1~10wt%,铈的重量百分比为0.05~5wt%;抑菌活性成分中,银的重量百分比为0.01~2wt%。
所述的抑菌催化还原多孔材料,多孔载体的孔隙率为30~90%,平均孔径为0.01~10μm。
所述的抑菌催化还原多孔材料的制备方法,包括如下步骤:
(1)配制含有铁盐或(和)铈盐的含酸水溶液或有机溶液,铁盐浓度为1g/L~50g/L,铈盐浓度为1g/L~30g/L,超声或搅拌溶解;
(2)配制钯盐的含酸水溶液或有机溶液,钯盐浓度为0.01g/L~1g/L,超声或搅拌溶解;
(3)将用去离子水清洗并于80~130℃烘干的多孔载体浸渍在铁盐或(和)铈盐的混合溶液中,超声或抽真空除气5~30min,以利于溶液进入微孔并润湿;
(4)将浸渍有铁盐或(和)铈盐的多孔载体在80~130℃烘干,然后在空气或氧气气氛下煅烧,温度为300℃~600℃,时间为0.5~3小时;
(5)将煅烧后的含铁氧化物或(和)铈氧化物的多孔载体在去离子水中浸洗干净,然后填充到固定床中,用浓度为0.01g/L~1g/L的钯盐溶液循环流过,并采用下面两种方法中的至少一种实现钯在多孔载体上的负载:
(a)利用气液混合装置向固定床进水口加入氢气,氢气与水体积比控制在0.2~1:1,反应时间为5~120min;(b)采用紫外光或可见光使钯在多孔载体表面光还原沉积,光的波长为184~450nm,光强为50~500mW/cm2,光还原时间为5~120min;
(6)将步骤(5)中负载钯的多孔材料用清水清洗干净,然后用浓度为0.05g/L~5g/L的硝酸银或醋酸银水溶液循环流过,并用气液混合装置向固定床进水口加入氢气,利用钯的催化还原作用原位沉积纳米银;氢气与水体积比控制在0.1~1:1,反应时间为5~60min;
(7)将步骤(6)得到的材料取出清洗,然后在60~120℃烘干,得到具有抑菌性能和催化还原性能的多孔材料;或者,步骤(6)得到的材料不取出烘干,所述材料和固定床整体直接作为处理器使用。
所述的抑菌催化还原多孔材料的制备方法,铁盐为硝酸铁、醋酸铁、氯化铁或硫酸亚铁,铈盐为硝酸铈、氯化铈或2-甲基乙醇铈,钯盐为硝酸钯、醋酸钯、氯化钯或乙酰丙酮钯。
所述的抑菌催化还原多孔材料的制备方法,步骤(7)之后,当抑菌催化还原多孔材料长期使用后,催化还原性和抑菌性能下降时,分别用步骤(5)和步骤(6)中的方法进行恢复。
所述的抑菌催化还原多孔材料的应用,将抑菌催化还原多孔材料应用于固定床催化体系,在普通灌装条件下,用于生产可储存的富氢还原水,富氢还原水中的氢浓度1~3ppm;生产还原水时,水的氧化还原电位降至-100mV~-700mV,水流量为5至300个床层体积/小时,氢气流量为水流量的1/2~1/30;如需高浓度的含氢水,氢浓度3~5ppm,使水循环流过固定床。
所述的抑菌催化还原多孔材料的应用,利用活性钯的催化还原作用原位生成纳米银,纳米银缓慢释放出微量银离子,从而产生持续稳定的抑菌性。
所述的抑菌催化还原多孔材料的应用,利用铁铈负载的多孔材料的催化还原作用或光催化还原作用原位生成纳米钯,形成具有催化还原能力的钯活性位。
所述的抑菌催化还原多孔材料的应用,当抑菌催化还原多孔材料长期使用导致钯和银逐渐消耗,该材料的催化还原性能和抑菌性能下降时,直接在设备上进行钯和银的原位负载,使材料的性能得到恢复。
本发明的设计思想是:
本发明主要设计一种具有催化还原性和抑菌性的多孔材料,并将其应用于固定床处理器中,用以制取具有富氢的还原水。赋予水还原性和赋予其抑菌性存在一定的矛盾,因为抑菌通常利用强氧化性的臭氧来实现。要解决这一问题,需要寻找新的抑菌方法。本发明以安全、稳定、无毒的多孔材料为载体,金属铁、铈、钯为催化还原活性组分,纳米银为抑菌组分,采用浸渍、煅烧、原位催化还原沉积、原位光还原沉积等工艺制备出的催化材料,钯和银均匀分散地负载于多孔载体的孔壁和外层等与水气接触充分的位置,最大限度发挥催化还原功效的同时保证抑菌效果。
不同于传统的浸渍法和喷雾法,贵金属活性组分钯和银采用原位沉积的方法进行负载,所负载的纳米钯主要沉积在与水和氢气接触充分的区域,可提高贵金属盐的利用率和接触效率。利用该催化材料制备的富氢还原水既有很好的还原性,也有很好的抑菌性。由于该催化材料在还原条件下使用,银离子不会过快地释放到水中,安全无害且可保证其使用寿命。与此同时,钯和银的负载工艺与还原水的生产工艺完全吻合,这使得材料的催化还原性和抑菌性的原位恢复变得方便可行。
本发明的优点及有益效果如下:
1、本发明采用催化还原或光(催化)还原使活性成分钯和银均匀分散地分布于多孔载体内孔壁和外表面等与水气接触充分的地方,可最大限度发挥其功效。
2、本发明所选用的载体疏松多孔,透水性好,且活性催化成分均匀分散,抑菌催化还原多孔材料具有优异的催化还原性能,可高效还原去除杀菌后残留在水中的臭氧,并将氢气分解为高活性的新生态原子存在于水中,可使水的氧化还原电位降低到-600mV以下。
3、本发明中的材料利用负载有铁铈的多孔载体的催化还原作用和光(催化)还原作用原位负载高分散性的活性钯,然后利用活性钯的催化还原作用原位生成均匀分散的纳米银,在使用过程中纳米银可缓慢释放出微量银离子,从而产生持续稳定的抑菌性。由于该材料可以在强还原条件下工作使用,银主要以单质存在,银离子释放缓慢、不会过量释放,不仅损耗少、使用寿命长,而且不会在水中引入过量的银离子,安全性高。如长期使用后催化还原性能和抑菌性下降,可用本发明中的方法进行原位恢复。
4、本发明很好地解决还原性和抑菌性之间的矛盾,可用于生产罐装、瓶装或袋装的富氢还原水,产品可储存,且使用方便、易携带。
具体实施方式
在具体实施过程中,本发明采用多孔钛骨、活性炭滤芯等多孔材料作为载体,首先通过浸渍、煅烧工艺在载体上均匀负载具有催化还原活性的铁铈复合氧化物组分,然后利用铁铈复合氧化物负载的多孔材料的催化还原作用或光(催化)还原作用原位生成纳米钯,形成原位负载具有高效催化还原作用的钯活性位。最后利用活性钯组分的催化还原作用,原位生成具有抑菌性能的纳米银,使材料同时具有很好的催化还原性能和抑菌性能。由于该材料和器件一般在强还原性条件下工作,银主要以单质形式存在,不仅损耗少、寿命长,而且不会在水中引入过量的银离子,安全性高。当长期使用导致材料的催化还原性能和抑菌性能下降时,可直接在设备上进行钯和银的原位负载,使其性能得到恢复。使用本发明中的材料,可迅速分解杀菌后水中残余的臭氧,并使水的氧化还原电位降至-600mV以下。由于材料的抑菌作用,生产的还原水可储存6个月以上。因此,本发明可在普通灌装(相对于无菌灌装)条件下实现抑菌保鲜,简化还原水生产工艺,降低生产成本。
下面结合实施例对本发明进一步详细描述。
实施例1
本实施例中,在5L水中加入60g九水硝酸铁和20克六水硝酸铈,搅拌15min后,铁盐和铈盐全部溶解。将长度为40cm、直径为50mm、平均孔径为1μm、孔隙率为35%的多孔钛棒,用体积浓度为2%的硝酸清洗,然后浸入铁盐和铈盐的混合溶液,超声30min后,取出多孔钛棒,在恒温烘箱中120℃干燥3h。将干燥后的含盐多孔钛棒放入箱式热处理炉,在空气气氛下以5℃/min的速率升温至600℃并保温60min,随炉冷却后用二次去离子水清洗2次,然后安装到固定床反应器中。将65g醋酸钯溶于5L冰醋酸与水的体积比为1:1的溶液,得到醋酸钯含酸溶液,然后使醋酸钯含酸溶液循环流过负载有铁铈的多孔钛棒,用射流器在进液口以500mL/min的流量通入氢气,120min后排出醋酸钯溶液,得到钯负载的多孔钛棒。最后,用10L浓度为0.5g/L的硝酸银水溶液循环流过钯负载的多孔钛棒,并在进水口以300mL/min的流量通入氢气,60min后取出多孔钛棒在80℃烘干,得到同时负载铁铈复合氧化物和钯、银纳米颗粒的抑菌催化还原多孔材料。
本实施例所得抑菌催化还原多孔材料中,钯的重量百分比为0.68wt%,铁的重量百分比为1.1wt%,铈的重量百分比为0.35wt%,银的重量百分比为0.22wt%。
实施例2
本实施例中,将实施例1中的抑菌催化还原多孔材料固定在内径为63mm的PVC滤壳中,制成固定床处理器。氢气和二次反渗透水同时被吸入小型自吸泵后,先通过小型管道混合器进行气液混合,然后流经装有抑菌催化还原多孔材料的固定床处理器,以制取具有抑菌性的还原水。
在水流量为100L/h,氢气流量为200mL/min的条件下,出水中的银离子浓度未检出,氧化还原电位为-630mV。
上述还原水用铝箔袋封存,6个月后测得氧化还原电位为-615mV,水中未检测出大肠杆菌菌群。
实施例3
本实施例中,将实施例1中的抑菌催化还原多孔材料固定在内径为63mm的PVC滤壳中,制成固定床处理器。100L原水经臭氧杀菌后,残余的臭氧浓度为0.45mg/L。臭氧水以200L/h的流速循环流经装有抑菌催化还原多孔材料的固定床处理器,同时以500mL/min的流量通入氢气,循环2小时后,取样检测。水样的氧化还原电位为-645mV,臭氧和银离子未检出。
上述还原水用铝箔袋封存,6个月后测得氧化还原电位为-625mV,水中未检测出大肠杆菌菌群。
实施例结果表明,用本发明中的方法制备的抑菌催化还原多孔材料可制取兼具强还原性和抑菌性的还原水,且不产生其它危害,在生产商品还原水上具有明显的应用价值。
Claims (9)
1.一种抑菌催化还原多孔材料,其特征在于,由多元活性组分和多孔载体组成;多元活性组分包括催化还原活性成分和抑菌活性成分,催化还原活性成分为钯、铁、铈的单质、固溶体或氧化物中的至少一种,抑菌活性成分为单质银或银的氧化物;多孔载体为多孔钛骨、多孔钛棒、多孔钛板、多孔镁、多孔锆、多孔锡、活性炭滤芯、陶瓷滤芯、膨胀石墨或活性氧化铝颗粒;催化还原活性成分中,钯的重量百分比为0.01~5wt%,铁的重量百分比为0.1~10wt%,铈的重量百分比为0.05~5wt%;抑菌活性成分中,银的重量百分比为0.01~2wt%。
2.按照权利要求1所述的抑菌催化还原多孔材料,其特征在于,多孔载体的孔隙率为30~90%,平均孔径为0.01~10μm。
3.一种权利要求1所述的抑菌催化还原多孔材料的制备方法,其特征在于,包括如下步骤:
(1)配制含有铁盐或(和)铈盐的含酸水溶液或有机溶液,铁盐浓度为1g/L~50g/L,铈盐浓度为1g/L~30g/L,超声或搅拌溶解;
(2)配制钯盐的含酸水溶液或有机溶液,钯盐浓度为0.01g/L~1g/L,超声或搅拌溶解;
(3)将用去离子水清洗并于80~130℃烘干的多孔载体浸渍在铁盐或(和)铈盐的混合溶液中,超声或抽真空除气5~30min,以利于溶液进入微孔并润湿;
(4)将浸渍有铁盐或(和)铈盐的多孔载体在80~130℃烘干,然后在空气或氧气气氛下煅烧,温度为300℃~600℃,时间为0.5~3小时;
(5)将煅烧后的含铁氧化物或(和)铈氧化物的多孔载体在去离子水中浸洗干净,然后填充到固定床中,用浓度为0.01g/L~1g/L的钯盐溶液循环流过,并采用下面两种方法中的至少一种实现钯在多孔载体上的负载:
(a)利用气液混合装置向固定床进水口加入氢气,氢气与水体积比控制在0.2~1:1,反应时间为5~120min;(b)采用紫外光或可见光使钯在多孔载体表面光还原沉积,光的波长为184~450nm,光强为50~500mW/cm2,光还原时间为5~120min;
(6)将步骤(5)中负载钯的多孔材料用清水清洗干净,然后用浓度为0.05g/L~5g/L的硝酸银或醋酸银水溶液循环流过,并用气液混合装置向固定床进水口加入氢气,利用钯的催化还原作用原位沉积纳米银;氢气与水体积比控制在0.1~1:1,反应时间为5~60min;
(7)将步骤(6)得到的材料取出清洗,然后在60~120℃烘干,得到具有抑菌性能和催化还原性能的多孔材料;或者,步骤(6)得到的材料不取出烘干,所述材料和固定床整体直接作为处理器使用。
4.根据权利要求1所述的抑菌催化还原多孔材料的制备方法,其特征在于,铁盐为硝酸铁、醋酸铁、氯化铁或硫酸亚铁,铈盐为硝酸铈、氯化铈或2-甲基乙醇铈,钯盐为硝酸钯、醋酸钯、氯化钯或乙酰丙酮钯。
5.根据权利要求1所述的抑菌催化还原多孔材料的制备方法,其特征在于,步骤(7)之后,当抑菌催化还原多孔材料长期使用后,催化还原性和抑菌性能下降时,分别用步骤(5)和步骤(6)中的方法进行恢复。
6.一种权利要求1至5之一所述的抑菌催化还原多孔材料的应用,其特征在于,将抑菌催化还原多孔材料应用于固定床催化体系,在普通灌装条件下,用于生产可储存的富氢还原水,富氢还原水中的氢浓度1~3ppm;生产还原水时,水的氧化还原电位降至-100mV~-700mV,水流量为5至300个床层体积/小时,氢气流量为水流量的1/2~1/30;如需高浓度的含氢水,氢浓度3~5ppm,使水循环流过固定床。
7.根据权利要求6所述的抑菌催化还原多孔材料的应用,其特征在于,利用活性钯的催化还原作用原位生成纳米银,纳米银缓慢释放出微量银离子,从而产生持续稳定的抑菌性。
8.根据权利要求6所述的抑菌催化还原多孔材料的应用,其特征在于,利用铁铈负载的多孔材料的催化还原作用或光催化还原作用原位生成纳米钯,形成具有催化还原能力的钯活性位。
9.根据权利要求6所述的抑菌催化还原多孔材料的应用,其特征在于,当抑菌催化还原多孔材料长期使用导致钯和银逐渐消耗,该材料的催化还原性能和抑菌性能下降时,直接在设备上进行钯和银的原位负载,使材料的性能得到恢复。
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