CN106179367A - A kind of cerium modified titanium deoxide catalyst of copper and its preparation method and application - Google Patents
A kind of cerium modified titanium deoxide catalyst of copper and its preparation method and application Download PDFInfo
- Publication number
- CN106179367A CN106179367A CN201610534473.9A CN201610534473A CN106179367A CN 106179367 A CN106179367 A CN 106179367A CN 201610534473 A CN201610534473 A CN 201610534473A CN 106179367 A CN106179367 A CN 106179367A
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- China
- Prior art keywords
- copper
- parts
- cerium
- catalyst
- haydite
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- 239000003054 catalyst Substances 0.000 title claims abstract description 30
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 21
- 239000010949 copper Substances 0.000 title claims abstract description 21
- -1 cerium modified titanium Chemical class 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002351 wastewater Substances 0.000 claims abstract description 17
- 239000010802 sludge Substances 0.000 claims abstract description 16
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920000642 polymer Polymers 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 10
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 150000000703 Cerium Chemical class 0.000 claims abstract description 5
- 235000011054 acetic acid Nutrition 0.000 claims abstract description 3
- 150000001243 acetic acids Chemical class 0.000 claims abstract description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims abstract description 3
- 150000001879 copper Chemical class 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 12
- 239000000919 ceramic Substances 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 239000005995 Aluminium silicate Substances 0.000 claims description 5
- 235000012211 aluminium silicate Nutrition 0.000 claims description 5
- 235000013339 cereals Nutrition 0.000 claims description 5
- 239000004927 clay Substances 0.000 claims description 5
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- 239000002360 explosive Substances 0.000 claims description 4
- 239000010881 fly ash Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 235000019353 potassium silicate Nutrition 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical group [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 235000013312 flour Nutrition 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical group [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 239000005416 organic matter Substances 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims 1
- 229910000859 α-Fe Inorganic materials 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 239000002910 solid waste Substances 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 230000003647 oxidation Effects 0.000 description 10
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- 238000002386 leaching Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 229910052593 corundum Inorganic materials 0.000 description 6
- 229910021645 metal ion Inorganic materials 0.000 description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- 229910052681 coesite Inorganic materials 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 239000008187 granular material Substances 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 229910052573 porcelain Inorganic materials 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 229910002012 Aerosil® Inorganic materials 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000012876 carrier material Substances 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000003361 porogen Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- SPSSULHKWOKEEL-UHFFFAOYSA-N 2,4,6-trinitrotoluene Chemical compound CC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O SPSSULHKWOKEEL-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012458 free base Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 235000019394 potassium persulphate Nutrition 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910001428 transition metal ion Inorganic materials 0.000 description 2
- 239000000015 trinitrotoluene Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 241001300078 Vitrea Species 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- XQJHRCVXRAJIDY-UHFFFAOYSA-N aminophosphine Chemical compound PN XQJHRCVXRAJIDY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 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 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000002153 concerted effect Effects 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003721 gunpowder Substances 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 125000003258 trimethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 210000004127 vitreous body Anatomy 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
-
- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
-
- 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
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
-
- 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)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of cerium modified titanium deoxide catalyst of copper and its preparation method and application, described catalyst is doped with copper and cerium in titanium dioxide, and copper, the doping of cerium are respectively the 5 ~ 10% of titania weight, 10 ~ 20%.Its preparation method is 300 ~ 400 parts of dehydrated alcohol of addition, 5 ~ 8 parts of acetylacetone,2,4-pentanediones, mix homogeneously after 3 ~ 6 parts of glacial acetic acids in reaction vessel, adds 20 ~ 50 parts of butyl titanates, and stirring mixes to obtain solution A；(2) in 20 ~ 30 parts of dehydrated alcohol, add the solubility cerium salt 1 ~ 3 part of 0.1 ~ 0.5M, the soluble copper salt 2 ~ 3 parts of 0.2 ~ 1M, after mix homogeneously, then be mixed to get solution B with solution A；(3) solution B is heated to 60 ~ 90 DEG C, adds 1 ~ 4 part of template, react 0.5 ~ 2h, obtain performed polymer；(4) being soaked in by haydite in described performed polymer 5 ~ 20 seconds, taking-up drains, and after drying, calcines 0.5 ~ 2h in 400 ~ 500 DEG C, obtains the cerium modified titanium deoxide catalyst of copper.This catalyst is effective to the catalytic treatment of waste water；The preparation of catalyst simultaneously can also utilize solid waste municipal sludge.
Description
Technical field
The present invention relates to a kind of cerium modified titanium deoxide catalyst of copper and its preparation method and application, belong to process Industry Waste
Catalyst material technical field in water.
Background technology
Persulfate advanced oxidation is a kind of effective ways processing organic wastewater with difficult degradation thereby grown up in recent years, its
Oxidation mechanism is under catalyst action, produces more higher SO than OH oxidizing potential4 -Peroxy, main catalytic way has
Thermocatalytic, photocatalysis and chemical catalysis.Chemical catalysis is mainly with metal or transition metal ions such as Fe0、Fe2+、Co2+、Ce2+
Deng activation SO4 -.Zhang Shenghan etc. are at " ferrous sulfate/potassium peroxydisulfate system advanced treatment of dyeing wastewater " (Donghua University's journal
Vol.39N6.P814), ten thousand little tender etc. at " persulfate treating technology rubbish percolation liquid membrane concentrated solution ", (non-ferrous metal sets
Meter and research Vol.35No.1P33) and the patent of invention of Zhang Naidong et al.: 201110149719.8 describe chemical catalytic oxidation
Progress.Shen Xunwei etc. are at " impact of persulphate on photocatalysis of phenol in aqueous TiO_2 suspensions " (environment
Science journal Vol.25No.5P631), husky pretty roc etc. is at " nano-TiO2/ mesoporous ZSM-5 works in coordination with persulfate photocatalytic degradation nitre
Base phenolic waste water " in terms of (Anhui University of Technology journal Vol.30No.1P32) describe persulfate cooperative photocatalysis oxidation
Progress.
From the point of view of above-mentioned introduction, transition metal-catalyzed, it is directly to excite SO by the variation of valence of transition metal4 -Product
Raw, Titanium Dioxide is then to excite titanium dioxide to produce conduction band electron and valence band hole by light, and photohole moves to
Surface and ADSORPTION STATE hydroxyl and water react generation hydroxyl radical free radical；And light induced electron produces O with electron acceptor- 2Free radical, enters
And excite persulfate to produce SO4 -.Catalyst effect during persulfate oxidation it is critical that.
Data shows, when metal and metal ion catalysis persulfate oxidation, metal ion is to be dissolved in ionic state to treat
In disposing waste liquid, not only cause the loss of metal ion, and need the separation circuit increasing metal ion with waste water.If will
Metal ion loads on solid carrier, so that it may solve the problems referred to above.When carrying out optically catalytic TiO 2 reaction, there is people by two
Titania oxide supported on carrier, such as: the patent of invention " modification processing method of a kind of ZSM-5 zeolite " at model peak et al. (patent No.:
20111092779.8), the patent of invention " MCM-41 molecular sieve and titanium nanometer composite material and preparation method thereof " of Zhai Qingzhou et al.
(patent No.: 200410096181.9).
Transition metal ions excites the catalysis oxidation of persulfate jointly to act on difficulty with the photochemical catalytic oxidation of titanium dioxide
The degraded of degradation of organic waste water can play the coordinating effect of superposition.
Summary of the invention
Present invention solves the technical problem that and be to provide the catalyst that a kind of catalytic effect is good, may be used for processing industry
Waste water, particularly explosive waste water；Meanwhile, the preparation method of this catalyst is easy, it is also possible to utilize municipal sludge, the pottery obtained
Ceramic carrier dissolution rate is low.
The technical scheme is that, it is provided that a kind of cerium modified titanium deoxide catalyst of copper, in titanium dioxide doped with
Copper and cerium, copper, the doping of cerium are respectively the 5～10%, 10～20% of titania weight.
The doping of the present invention is doping in the solution, and the material after doping is homogeneous in microstructure, i.e. micro-
Seeing on yardstick, the distribution of foreign atom is also uniform；This has substantially with common physical doping (such as: two kinds of powder mix)
Difference.Thus, this doping belongs to homogeneous doping.
The present invention further provides the preparation method of the cerium modified titanium deoxide catalyst of copper, comprise the following steps, each step
In material the most by volume part calculate:
(1) in reaction vessel, 300～400 parts of dehydrated alcohol are added, 5～8 parts of acetylacetone,2,4-pentanediones, mixed after 3～6 parts of glacial acetic acids
Closing uniformly, add 20～50 parts of butyl titanates, stirring mixes to obtain solution A；
(2) in 20～30 parts of dehydrated alcohol, add 0.1～0.5M solubility cerium salt 1～3 parts, 0.2～1M solvable
Property mantoquita 2～3 parts, after mix homogeneously, then be mixed to get solution B with solution A；
(3) solution B is heated to 60～90 DEG C, adds 1～4 part of template, react 0.5～2h, obtain performed polymer；
(4) being soaked in by haydite in described performed polymer 5～20 seconds, taking-up drains, after drying, in 400～500 DEG C of calcinings
0.5～2h, obtain the cerium modified titanium deoxide catalyst of copper.
Further, in described step (2), solubility cerium salt is ammonium ceric nitrate.
Further, in described step (2), soluble copper salt is copper sulfate.
Further, in described step (3), template is Polyethylene Glycol.
Further, described haydite is prepared by following methods:
(1) by weight, with municipal sludge 20-60 part, clay 10-20 part, Kaolin 10-20 part, flyash 10-20
Part, silicon source 2-5 part are raw material；Each component in raw material is mixed, then through extruding to obtain haydite blank；Described silicon source be waterglass,
One or more in aerosil and silica flour；
(2) described haydite blank is sintered after drying, cooling, obtain porous ceramic grain carrier；Described sintering is by after drying
Haydite blank be first warming up to 300-600 DEG C at pre-burning 10-40min, then be warming up to 950-1150 DEG C, be incubated 10-40min.
Further, the moisture content of described municipal sludge is not higher than 85%, and contents on dry basis organic in municipal sludge is
50～60%, the contents on dry basis of inanimate matter is 40～50%.Being mainly composed of of inanimate matter: aluminium sesquioxide, silicon dioxide and
Ferrum oxide, calcium oxide, magnesium oxide etc..
Further, the comprcssive strength of described haydite is 20～30MPa
Further, the porosity of described haydite is 45～55%, and specific surface area is 200～400m2/g。
The present invention provides above-mentioned catalyst to process at waste water further, the particularly application in terms of explosive waste water process.
Anatase titanium dioxide, under visible/action of ultraviolet light, can excite generation photoelectron, and then produce hydroxyl free
Base, by being entrained in titanium dioxide lattice artificial manufacturing defect, utilizes the variation of valence of cerium ion, produces under action of ultraviolet light
Third contact of a total solar or lunar eclipse electron-hole, makes the speed of burying in oblivion of the hydroxyl radical free radical of generation reduce, and the concentration of effective free radical increases, oxidation efficiency
Improve.The lattice defect that cerium causes is different, plays the effect of concerted catalysis, and the effect of copper ion is to reduce free energy of reaction, makes
Oxidation reaction is easier to make for.
Cerium ion directly can also produce SO by catalytic decomposition persulfate4Free radical, sulphuric acid free radical compares hydroxyl free
Base has higher oxidizing potential, and the Organic substance being more difficult to degraded can be made to degrade oxidized decomposition.
The titanium dioxide performed polymer prepared is coated in haydite surface, obtains anatase titanium dioxide by calcining brilliant
Body.
Mud prepares haydite more use underwater mud or sludge with low moisture content, the viscosity of aqueous municipal sludge at present
Greatly, the mixing with material is relatively difficult, uses fewer.And it is the highest to prepare haydite percent opening at present, uses as building materials
Added value is relatively low.For this situation, the present invention utilizes and prepares porous carrier rich in organic municipal sludge as porogen
Material.The municipal sludge addition of the present invention is big, and up to 60%, the content of organic matter is high, can account for the 15-20% in solid content, no
Need to additionally add porogen, municipal sludge, without being dried directly use, can save the energy.
Common porous ceramic be mainly composed of aluminosilicate, raw material includes Kaolin, kieselguhr, clay etc., pore former
The material of gas can be at high temperature evaporated into for carbonate, Organic substance etc..Interpolation municipal sludge prepares haydite utilization wherein to be had
Machine thing is as porogen, and inorganic matter is as haydite composition；Organic substance is oxidation Decomposition when 300-600 DEG C (pre-burning), and volatilization produces
Gas, overflows and forms hole；And inorganic substances are with SiO in mud2、Al2O3、CaO、Fe2O3Element is main, is alumino silicate ceramic
The raw material fired.The raw material of haydite is with SiO2And Al2O3For bulk composition, form intensity and the primary structure of structure for haydite
Basis, Al2O3Account for 10-25%, SiO2Account for 40-79%, the present invention is properly added silicon source (waterglass, aerosil and silicon
Powder), to increase SiO2Content, adjust Al2O3With SiO2Ratio；The silicon source of the present invention is also used as binding agent, for haydite
The formation of stock provides structural strength, makes the intensity of stock improve, it is easy to molding.
During sludge ceramsite fires building porcelain granule, decompose during Organic substance pre-burning, be internally formed trickle through hole at haydite,
After temperature rises to a certain degree, SiO in raw material2、Al2O3、CaO、Fe2O3Start mutually to melt (ore deposit after cooling, to be formed
Thing), when after sintering temperature arrives 1200 DEG C or when sintering time extends, form certain thickness glass at particle surface and melt mutually
Melt body, becomes closed pore haydite after cooling, this haydite density is little, intensity is high.During firing porous carrier haydite (perforate), it is impossible to
Form vitreous body at particle surface, cause closed pore；Require that the most again internal each component is the most melted, have enough physical strengths,
Therefore the assurance to sintering temperature and sintering time is more accurate.CaO、Fe2O3Etc. can be as SiO2、Al2O3High-temperature Liquefaction
Flux (need not individually add other cosolvent, such as Borax), reduces and forms Vitrea temperature, opens according in this research
The material composition of hole haydite, firing temperature is at 950-1150 DEG C, and firing temperature is 10-40min.Sintering procedure needs control
Heating rate and cool speed, programming rate is too fast makes particle surface and inside be heated inequality, and surface easily melts, easily
Form closed pore；The physical property making granule is changed by cooling rate soon, easily forms crack.
In sum, carrier haydite is with the maximum difference of building porcelain granule: building porcelain granule desired strength is high, light weight, interior
Portion's porous, surface-closed, without penetrability space, to aperture not requirement.Carrier haydite requires that there is penetrability micropore on surface, compares table
Area is big, and uniform pore diameter is relatively low to requirement of strength, and therefore, the control to temperature is more accurate, needs through substantial amounts of examination
Test and mass data analysis including Phase Diagram Analysis can determine.The composition of raw material constituted is not had by building porcelain granule
It is strict with, and carrier haydite is strict to raw-material component requirements, needs additional silicon source to carry out composition adjustment, small composition
The mass data such as difference all can affect its performance, needs by great many of experiments and includes surface scan, inside diameter measurement, structural analysis
Analyze and application test can determine.
Porous ceramic grain carrier prepared by the present invention has a following characteristics: rough surface, loose porous, and particle porosity is up to
45-55%, specific surface area reaches 200-400m2/g；Stable chemical nature, 1+1 hydrochloric acid dissolution rate ＜ 1%；Leaching of Heavy Metals amount exists
Secondary pollution that is below the mark, that cause without Leaching；Mechanical strength is high, and comprcssive strength reaches 20-30MPa, the highest.Can
Substitute traditional natural porous material or artificial porous material, the catalyst in processing and the carrier material of adsorbent as waste water
Material.The present invention utilizes mud to prepare porous ceramic grain material, and raw material is simple, low price, excellent performance, easy to use.
The invention has the beneficial effects as follows, the treatment of Organic Wastewater for difficult degradation is effective；Especially for containing amino, phosphine
The organic wastewater degraded rate of the difficult degradations such as acidic group, phenyl ring, condensed ring is higher, it is also possible to utilize municipal sludge to prepare haydite, it is achieved useless
Thing utilizes.
Detailed description of the invention
Below by several embodiments, the present invention being done concrete introduction, following instance does not constitute limitation of the invention.
Embodiment one
1, prepared by ceramsite carrier
Take mud 2.0kg, clay 1.0kg, Kaolin 1.0kg, flyash 1.0kg, waterglass 0.2kg, be sufficiently mixed all
Even, causeColumn haydite blank, is warming up to 500 DEG C with 10 DEG C of temperature in high temperature furnace, constant temperature pre-burning 30min,
Again with 5 DEG C/min ramp to 1100 DEG C, sinter 20min, be cooled to less than 300 DEG C with 10 DEG C/min speed, take out nature
Cooling, obtaining porous ceramsite carrier outward appearance is brick-red short cylinder solid particle.On inspection without Leaching material, have preferably
Apparent density and porosity, can be used as catalyst carrier material.
Preparing haydite ceramic surface coarse, loose porous, particle porosity is up to 55%, and specific surface area reaches 380m2/g；Change
Learn stable in properties, 1+1 hydrochloric acid dissolution rate ＜ 0.1%；Leaching of Heavy Metals amount, below the useless discharge standard of danger, causes without Leaching
Secondary pollution；Mechanical strength is high, and comprcssive strength reaches 27MPa.
2, titanium dioxide performed polymer synthesis
1) adding 350L dehydrated alcohol in reaction vessel, then be separately added into 7.8L acetylacetone,2,4-pentanedione, 4.5L glacial acetic acid mixes
Uniformly, 40L butyl titanate, stirring mixing are added.
2) additionally measure 27L dehydrated alcohol, add 0.1M ammonium ceric nitrate 1L；Add the copper sulfate 2L of 0.2M；Mix homogeneously
After, it is slowly added into step 1) in, stirring reaction.
3) heating in water bath is to 80 DEG C, claims 3L Polyethylene Glycol, reacts 1h, obtain the pre-polymerization of the cerium modified titanium dioxide of copper after dissolving
Body, cools down standby.
3, ceramic monolith step 1 obtained, is dipped in the performed polymer that step 2 obtains, and quickly removes, drain pre-polymerization
Body, after drying, calcines 2h in 450 DEG C, obtains the cerium modified titanium deoxide catalyst of copper.
Embodiment two
1, prepared by ceramsite carrier
Take mud 2.4kg, clay 0.5kg, Kaolin 0.5kg, flyash 0.4kg, aerosil 0.15kg, fully
Mix homogeneously, causesColumn haydite blank, is warming up to 500 DEG C with 10 DEG C of temperature, constant temperature pre-burning in high temperature furnace
40min, then with 5 DEG C/min ramp to 1100 DEG C, sinter 20min, be cooled to less than 300 DEG C with 10 DEG C/min speed, take
Go out natural cooling, burn porous ceramsite carrier outward appearance is micro-yellow short cylinder solid particle.On inspection without Leaching material, have
Preferably apparent density and porosity, can be used as catalyst carrier material.
Preparing haydite ceramic surface coarse, loose porous, particle porosity is up to 45%, and specific surface area reaches 220m2/g；Change
Learn stable in properties, 1+1 hydrochloric acid dissolution rate ＜ 0.1%；Leaching of Heavy Metals amount, below the useless discharge standard of danger, causes without Leaching
Secondary pollution；Mechanical strength is high, and comprcssive strength reaches 30MPa.
2, titanium dioxide performed polymer synthesis
1) adding 400L dehydrated alcohol in reaction vessel, then be separately added into 5.5L acetylacetone,2,4-pentanedione, the mixing of 4L glacial acetic acid is all
Even, add 30L butyl titanate, stirring mixing.
2) additionally measure 20L dehydrated alcohol, add the ammonium ceric nitrate 1L of 0.1M；Adding the copper sulfate 3L of 0.5M, mixing is all
After even, it is slowly added into step 1) in, stirring reaction.
3) heating in water bath is to 60 DEG C, claims 4L Polyethylene Glycol, reacts 2h, obtain the pre-polymerization of the cerium modified titanium dioxide of copper after dissolving
Body, cools down standby.
3, ceramic monolith step 1 obtained, is dipped in the performed polymer that step 2 obtains, and quickly removes, drain pre-polymerization
Body, after drying, calcines 2h in 400 DEG C, obtains the cerium modified titanium deoxide catalyst of copper.
Catalytic effect
Catalyst synthesized by embodiment one and embodiment two is used for explosive waste water produced by certain gunpowder manufacturing enterprise
Cleaning test, respectively obtains following experimental result:
Comparative example one: pure titinium dioxide makees catalyst, is not doped, and other are identical with embodiment one.
Comparative example two: be not added with catalyst, reacts under the conditions of equal-wattage uviol lamp and same amount of potassium peroxydisulfate, to fried
Medicine waste water aoxidizes, result such as following table
Comparative example three: be not added with copper ion modified in catalyst, other are identical with embodiment one.
Comparative example four: reduction cerous nitrate consumption is to 0.5L, and other are identical with embodiment one.
Wherein, COD represents COD；TN represents total nitrogen；TNT represents trinitrotoluene；RDX represents ring trimethylene
Trintriamine.
Claims (10)
1. the cerium modified titanium deoxide catalyst of copper, it is characterised in that doped with copper and cerium in titanium dioxide, copper, cerium
Doping is respectively the 5 ~ 10% of titania weight, 10 ~ 20%.
2. the method preparing the cerium modified titanium deoxide catalyst of copper described in claim 1, it is characterised in that include following step
Suddenly, the material the most by volume part in each step calculates:
(1) adding 300 ~ 400 parts of dehydrated alcohol in reaction vessel, 5 ~ 8 parts of acetylacetone,2,4-pentanediones, after 3 ~ 6 parts of glacial acetic acids, mixing is all
Even, add 20 ~ 50 parts of butyl titanates, stirring mixes to obtain solution A；
(2) add in 20 ~ 30 parts of dehydrated alcohol the solubility cerium salt 1 ~ 3 part of 0.1 ~ 0.5M, 0.2 ~ 1M soluble copper salt 2 ~
3 parts, after mix homogeneously, then it is mixed to get solution B with solution A；
(3) solution B is heated to 60 ~ 90 DEG C, adds 1 ~ 4 part of template, react 0.5 ~ 2h, obtain performed polymer；
(4) being soaked in by haydite in described performed polymer 5 ~ 20 seconds, taking-up drains, after drying, in 400 ~ 500 DEG C calcine 0.5 ~
2h, obtains the cerium modified titanium deoxide catalyst of copper.
3. method as claimed in claim 2, it is characterised in that in described step (2), solubility cerium salt is ammonium ceric nitrate, can
Dissolubility mantoquita is copper sulfate.
4. method as claimed in claim 2, it is characterised in that in described step (2), soluble ferrite is ferrous sulfate
Ammonium.
5. method as claimed in claim 2, it is characterised in that in described step (3), template is Polyethylene Glycol.
6. method as claimed in claim 2, it is characterised in that described haydite is prepared by following methods:
(1) by weight, with municipal sludge 20-60 part, clay 10-20 part, Kaolin 10-20 part, flyash 10-20 part, silicon
Source 2-5 part is raw material；Each component in raw material is mixed, then through extruding to obtain haydite blank；Described silicon source is waterglass, gas phase two
One or more in silicon oxide and silica flour；
(2) described haydite blank is sintered after drying, cooling, obtain porous ceramic grain carrier；Described sintering is by dried pottery
Grain blank be first warming up to 300-600 DEG C at pre-burning 10-40min, then be warming up to 950-1150 DEG C, be incubated 10-40min.
7. method as claimed in claim 6, it is characterised in that the moisture content of described municipal sludge is not higher than 85%, municipal sludge
The contents on dry basis of middle organic matter is 50 ~ 60%, and the contents on dry basis of inanimate matter is 40 ~ 50%.
8. method as claimed in claim 2, it is characterised in that the comprcssive strength of described haydite is 20 ~ 30MPa, and porosity is
45 ~ 55%, specific surface area is 200 ~ 400m2/g。
9. the application in terms of waste water process of the catalyst described in claim 1.
Applying the most as claimed in claim 9, described waste water is explosive waste water.
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