CN115007137A - Catalyst for purifying dioxin and preparation method thereof - Google Patents
Catalyst for purifying dioxin and preparation method thereof Download PDFInfo
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- CN115007137A CN115007137A CN202210825095.5A CN202210825095A CN115007137A CN 115007137 A CN115007137 A CN 115007137A CN 202210825095 A CN202210825095 A CN 202210825095A CN 115007137 A CN115007137 A CN 115007137A
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- metal oxide
- bivo
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- dioxin
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- 239000003054 catalyst Substances 0.000 title claims abstract description 135
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 title claims abstract 12
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 86
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 85
- 239000002131 composite material Substances 0.000 claims abstract description 41
- 239000000919 ceramic Substances 0.000 claims abstract description 25
- 238000000498 ball milling Methods 0.000 claims abstract description 23
- 238000010304 firing Methods 0.000 claims abstract description 22
- 238000000746 purification Methods 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 239000002002 slurry Substances 0.000 claims abstract description 13
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 6
- QGWDKKHSDXWPET-UHFFFAOYSA-E pentabismuth;oxygen(2-);nonahydroxide;tetranitrate Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[O-2].[Bi+3].[Bi+3].[Bi+3].[Bi+3].[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QGWDKKHSDXWPET-UHFFFAOYSA-E 0.000 claims abstract description 6
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- 238000002791 soaking Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 26
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 5
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 5
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 5
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000003801 milling Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 51
- KVGZZAHHUNAVKZ-UHFFFAOYSA-N 1,4-Dioxin Chemical compound O1C=COC=C1 KVGZZAHHUNAVKZ-UHFFFAOYSA-N 0.000 description 48
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 24
- 238000010926 purge Methods 0.000 description 10
- 239000002912 waste gas Substances 0.000 description 9
- 229910052878 cordierite Inorganic materials 0.000 description 8
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 8
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 6
- 150000002013 dioxins Chemical group 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000005338 heat storage Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000004827 dibenzo-1,4-dioxins Chemical class 0.000 description 1
- 150000004826 dibenzofurans Chemical class 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
Images
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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
- B01J23/76—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
- B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8659—Removing halogens or halogen compounds
- B01D53/8662—Organic halogen compounds
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
The invention discloses a catalyst for purifying dioxin and a preparation method thereof, wherein the preparation method comprises the following steps: step one, firing basic bismuth nitrate and ammonium metavanadate to generate Bi 2 O 3 And V 2 O 5 (ii) a Adding Bi 2 O 3 And V 2 O 5 Ball milling and firing to obtain BiVO 4 A catalyst; step two, burning the precursor of the hexavalent metal oxide to obtain a hexavalent metal oxide cocatalyst; step three, firing the precursor of the divalent metal oxide to obtain a divalent metal oxide cocatalyst; step four, BiVO 4 Catalyst and hexavalent metal oxide promoter and divalent metal oxide promoterBall milling and firing to obtain BiVO 4 ‑AO 3 -a BO composite catalyst; or adding a template agent and deionized water during ball milling to obtain catalyst slurry; then soaking the honeycomb ceramic carrier into the catalyst slurry for uniform coating, and then firing to obtain BiVO 4 ‑AO 3 -a ceramic supported composite catalyst for BO. The invention has the advantages of simple preparation method, environmental protection and high purification efficiency.
Description
Technical Field
The invention belongs to the technical field of environmental protection, relates to a catalyst, and particularly relates to a catalyst for purifying dioxin and a preparation method thereof.
Background
Industrial enterprises, especially the pharmaceutical industry, generally use a large amount of dichloromethane as a solvent, and since dichloromethane has the advantages of low toxicity, strong volatility, non-flammability and the like, the dichloromethane is difficult to replace by other raw and auxiliary materials at present. Therefore, the volatile organic waste gases (VOCs) of pharmaceutical enterprises often contain dichloromethane components, and the dichloromethane waste gases are difficult to condense, insoluble in water, poor in biodegradability and absorbability, so that the dichloromethane waste gases become difficult and complicated diseases in VOCs treatment.
At present, the exhaust emission standards of industrial enterprises in various regions are gradually tightened, taking the unified standard of pharmaceutical industry atmospheric pollutant emission standard in the delta area of Yangtze river as an example, the emission limit concentration of non-methane total hydrocarbon is 60mg/m 3 The limit concentration of dichloromethane emission is 20mg/m 3 . In order to stably discharge after reaching standards, the purification efficiency of a VOCs waste gas treatment system in the general pharmaceutical industry needs to reach more than 90%, and the current mainstream treatment process is a Regenerative Thermal Oxidizer (RTO) aiming at VOCs waste gas containing dichloromethane.
The waste gas containing chlorine VOCs generates secondary pollution of dioxin during incineration, and the concentration of the dioxin even exceeds the relevant emission limit value. Dioxin is a general term for polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans, has extremely strong toxicity, is difficult to decompose in nature, and can enter human bodies through food chains due to lipophilic characteristics, thereby causing serious harm to health. In order to ensure the health of plant workers and surrounding residents and the sustainable development of the environmental bearing capacity, the dioxin generated by the RTO needs to be effectively treated.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a catalyst for purifying dioxin and a preparation method thereof, and BiVO is prepared by adopting a solid phase method 4 -AO 3 The preparation method of the-BO composite catalyst is simple and suitable for mass production, and BiVO is obtained 4 -AO 3 BiVO prepared by loading-BO composite catalyst on honeycomb ceramic 4 -AO 3 -BO supported cordierite ceramic composite catalysts, which can be used for the decomposition of dioxins produced during the combustion of VOCs.
In order to achieve the above object, the present invention provides a method for preparing a catalyst for purifying dioxin, which has the following characteristics: the method comprises the following steps:
step one, burning the basic bismuth nitrate to generate Bi 2 O 3 (ii) a Burning ammonium metavanadate to generate V 2 O 5 (ii) a Adding Bi 2 O 3 And V 2 O 5 Ball milling, and firing to obtain BiVO 4 A catalyst;
step two, burning the precursor of the hexavalent metal oxide to obtain a hexavalent metal oxide cocatalyst; precursors of the hexavalent metal oxide are ammonium paramolybdate or/and ammonium paratungstate, and the hexavalent metal oxide promoters obtained by burning are MoO 3 、WO 3 ；
Step three, firing the precursor of the divalent metal oxide to obtain a divalent metal oxide cocatalyst; the precursor of the divalent metal oxide is one or more of copper nitrate, nickel nitrate, zinc nitrate or cobalt nitrate, and the promoters of the divalent metal oxide obtained by firing are CuO, NiO, ZnO and CoO respectively;
step four, BiVO obtained in the step three 4 Catalyst, hexavalent metal oxide cocatalyst obtained in step two and stepBall milling the divalent metal oxide cocatalyst obtained in the third step, and then firing to obtain BiVO 4 -AO 3 -a BO composite catalyst; BiVO 4 -AO 3 BiVO in-BO composite catalyst 4 As a main active component, a composite hexavalent metal oxide cocatalyst AO 3 (MoO 3 、WO 3 ) And a divalent metal oxide promoter BO (CuO, NiO, ZnO, CoO).
Or, BiVO obtained in the third step 4 Mixing a catalyst, the hexavalent metal oxide cocatalyst obtained in the step two and the divalent metal oxide cocatalyst obtained in the step three, adding a template agent and deionized water, and performing ball milling to obtain catalyst slurry; then soaking the honeycomb ceramic carrier into the catalyst slurry for uniform coating, and then firing to obtain BiVO 4 -AO 3 -a ceramic supported composite catalyst for BO.
Further, the present invention provides a method for preparing a catalyst for purifying dioxin, which may further have the following characteristics: in the first step, the basic bismuth nitrate is placed in a muffle furnace to be burnt, the burning temperature is 400-600 ℃, and the burning time is 2-5 h; the ammonium metavanadate is placed in a muffle furnace for ignition, the ignition temperature is 300-600 ℃, and the ignition time is 2-5 h; the Bi 2 O 3 And V 2 O 5 Ball milling is carried out according to the stoichiometric ratio of 1: 1, the ball milling time is 2-5h, then the ball milling is placed in a muffle furnace for burning, the burning temperature is 600-700 ℃, and the burning time is 5-10 h.
Further, the present invention provides a method for preparing a catalyst for purifying dioxin, which may further have the following characteristics: in the second step, the precursor of the hexavalent metal oxide is placed in a muffle furnace to be burned; the burning temperature of the ammonium paramolybdate is 500-600 ℃, and the burning time is 2-5 h; the burning temperature of the ammonium paratungstate is 400-600 ℃, and the burning time is 2-5 h.
Further, the present invention provides a method for preparing a catalyst for purifying dioxin, which may further have the following characteristics: in the third step, the precursor of the divalent metal oxide is placed in a muffle furnace to be burned; the burning temperature of the copper nitrate, the nickel nitrate, the zinc nitrate and the cobalt nitrate is 200-500 ℃, and the burning time is 2-5 h.
Further, the present invention provides a method for preparing a catalyst for purifying dioxin, which can also have the following characteristics: wherein BiVO is prepared 4 -AO 3 In step four of the-BO composite catalyst, the BiVO 4 The weight ratio of the catalyst, the hexavalent metal oxide cocatalyst and the divalent metal oxide cocatalyst is 1: 0.1-0.5; the ball milling time is 2-5 h; placing the mixture in a muffle furnace for burning at the temperature of 700 ℃ and 800 ℃ for 5-10 h.
Further, the present invention provides a method for preparing a catalyst for purifying dioxin, which may further have the following characteristics: wherein BiVO is prepared 4 -AO 3 In the fourth step of the BO supported ceramic composite catalyst, the weight ratio of the BiVO4 catalyst to the hexavalent metal oxide cocatalyst to the divalent metal oxide cocatalyst is 1: 0.1-0.5; the weight ratio of the catalyst, the template agent and the deionized water in the catalyst slurry is 1: 1-5: 5-10; the template agent is glycerol or citric acid, and mainly has the functions of improving the dispersibility and viscosity of the catalyst in water and facilitating loading; the ball milling time is 2-5 h; placing the mixture in a muffle furnace for burning at the temperature of 600-700 ℃ for 5-10 h.
Further, the present invention provides a method for preparing a catalyst for purifying dioxin, which may further have the following characteristics: wherein BiVO is prepared 4 -AO 3 In the fourth step of the-BO ceramic-loaded composite catalyst, the honeycomb ceramic carrier is impregnated with the catalyst slurry for multiple times and is burned to obtain the composite catalyst with the active component content of 10% -30%. The purification efficiency of the catalyst for dioxin generally improves along with the increase of the content of active components, but when the content of the components is too high, the overall strength and the heat conduction performance of the catalyst are affected, and the economic efficiency is not good.
Further, the present invention provides a method for preparing a catalyst for purifying dioxin, which may further have the following characteristics: wherein, in the steps one to four, the temperature rise rate in the burning process is 5-10 ℃/min.
Further, the present invention provides a method for preparing a catalyst for purifying dioxin, which may further have the following characteristics: wherein, in the first step and the fourth step, the ball milling device is a planetary ball mill, the grinding balls are stainless steel balls or alumina ceramic balls with the diameter of 5mm-10mm, the ball-material ratio is 10-20: 1, and the revolution is 100 plus materials at 500 rpm/min.
The invention also provides a catalyst for purifying dioxin prepared by the preparation method.
Wherein, BiVO 4 -AO 3 The BO loaded ceramic composite catalyst can be directly used in RTO equipment to replace bottom heat storage ceramic, and the waste heat of RTO is utilized to efficiently decompose dioxin. The BiVO 4 -AO 3 The BO ceramic-loaded composite catalyst can efficiently decompose the secondary pollutant dioxin generated by burning chlorine-containing organic matters by RTO at the temperature range of 150 ℃ and 300 ℃.
The invention has the beneficial effects that:
the solid phase method is adopted to prepare the catalyst for purifying dioxin, so that the preparation cost is low, and the method is suitable for large-scale industrial production; and no organic solvent is used in the preparation process, so that the preparation method is environment-friendly and meets the requirements of energy conservation, environmental protection and green development.
The preparation method provided by the invention can effectively prevent the loss of active species, can prepare the catalyst with expected components and crystal forms, has good dispersibility, is favorable for obtaining metal oxide with large specific surface area by nitrogen oxide, ammonia gas and other gases generated in the reaction process, and has higher activity.
Thirdly, the preparation method provided by the invention firstly prepares the main active component BiVO 4 Then compounding hexavalent metal oxide cocatalyst and divalent metal oxide cocatalyst to prepare BiVO 4 -AO 3 The BO composite catalyst has a crystal structure and a solid solution form which are convenient to control, and can avoid the formation of heterogeneous low-activity substances compared with a common liquid phase method.
And fourthly, the composite catalyst is loaded on the cordierite honeycomb ceramic through an impregnation method and is applied to RTO equipment to replace a small amount of heat accumulators on the bottom layer of the regenerator, the structure of the RTO equipment does not need to be changed, the residual temperature in the RTO equipment can be fully utilized, the dioxin can be rapidly decomposed within the range of 150 plus one year of 300 ℃, and the investment and the operating cost for treating the dioxin are obviously saved.
Drawings
FIG. 1 is a schematic diagram of a catalyst for purification of dioxin;
FIG. 2 shows BiVO as a catalyst for purifying dioxin in example 4 4 -WO 3 -SEM picture of CoO composite catalyst;
FIG. 3 is a schematic view of the application of the catalyst for purification of dioxin in example 5 to RTO;
wherein the reference numerals are: the device comprises a flame arrester, a 2-RTO main fan, a 3-air inlet pipeline, a 4-air inlet valve, a 5-dioxin catalyst layer, a 6-regenerator, a 7-combustor, an 8-combustor, a 9-thermal bypass valve, a 10-thermal bypass pipeline, an 11-mixed flow box, a 12-exhaust valve, a 13-exhaust pipeline, a 14-RTO purging fan, a 15-purging pipeline, a 16-purging valve and a 17-exhaust barrel.
Detailed Description
The present invention is further illustrated by the following specific examples.
Comparative example 1
This comparative example provides a BiVO 4 The preparation method of the catalyst comprises the following steps: putting the basic bismuth nitrate into a muffle furnace to be burnt for 3 hours at 500 ℃ to generate Bi 2 O 3 (ii) a Putting ammonium metavanadate in a muffle furnace, and burning for 3h at 450 ℃ to generate V 2 O 5 (ii) a Adding Bi 2 O 3 And V 2 O 5 Ball-milling for 4h according to the stoichiometric ratio of 1: 1, placing the mixture in a muffle furnace for firing for 7h at 650 ℃, and grinding to obtain BiVO 4 A catalyst.
Comparative example 2
This comparative example provides a hexavalent metal oxide cocatalyst MoO 3 The preparation method comprises the following steps: placing ammonium paramolybdate in a muffle furnace, igniting for 3h at 550 ℃, and grinding to obtain hexavalent metal oxide cocatalyst MoO 3 。
Comparative example 3
This comparative example provides a hexavalent metal oxide cocatalyst WO 3 Method for preparing the sameComprises the following steps: placing ammonium paratungstate in a muffle furnace, igniting for 3h at 500 ℃, and grinding to obtain hexavalent metal oxide cocatalyst WO 3 。
Comparative example 4
The comparative example provides a divalent metal oxide promoter CuO, the preparation method of which is: and (3) putting copper nitrate into a muffle furnace, burning for 2h at 400 ℃, and grinding to obtain a divalent metal oxide cocatalyst CuO.
Comparative example 5
The comparative example provides a divalent metal oxide promoter NiO, and the preparation method comprises the following steps: and (3) putting the nickel nitrate into a muffle furnace, burning for 2h at 400 ℃, and grinding to obtain the divalent metal oxide cocatalyst NiO.
Comparative example 6
The comparative example provides a divalent metal oxide promoter ZnO, and the preparation method comprises the following steps: and (3) putting zinc nitrate into a muffle furnace, burning for 2h at 400 ℃, and grinding to obtain the divalent metal oxide cocatalyst ZnO.
Comparative example 7
The comparative example provides a divalent metal oxide cocatalyst CoO, and the preparation method comprises the following steps: and (3) placing the cobalt nitrate in a muffle furnace, burning for 2h at 400 ℃, and grinding to obtain a divalent metal oxide cocatalyst CoO.
BiVO obtained in comparative examples 1 to 7 4 Catalyst, hexavalent Metal oxide cocatalyst (MoO) 3 、WO 3 And divalent metal oxide promoters (CuO, NiO, ZnO, CoO) for purifying dioxins. Generating dioxin by adopting a trace amount dioxin generating system, and controlling the initial toxicity equivalent mass concentration of the dioxin to be 5(ng TEQ/Nm) 3 ) Left and right; the catalytic reaction device is a tubular quartz reactor, comprises a heating device and can control the temperature to be between room temperature and 400 ℃; the space velocity of the catalytic reaction is 10000 - 1 h. At the beginning of the experiment, a catalyst is added into a tubular quartz reactor, dioxin gas is introduced, when the concentration of dioxin at an inlet and an outlet is stable (adsorption action is eliminated), the temperature is raised to 300 ℃ and is stably maintained, the concentration of the inlet and the outlet is tested, and the performance test results are shown in table 1.
TABLE 1
| Kind of catalyst | Dioxin purification efficiency (%) |
| Comparative example 1BiVO 4 Catalyst and process for preparing same | 44 |
| Comparative example 2 hexavalent Metal |
11 |
| Comparative example 3 hexavalent Metal |
13 |
| Comparative example 4 divalent Metal oxide promoter CuO | ＜5％ |
| Comparative example 5 divalent Metal oxide promoter NiO | ＜5％ |
| Comparative example 6 divalent Metal oxide Co-catalyst ZnO | ＜5％ |
| Comparative example 7 divalent Metal oxide promoter CoO | ＜5％ |
As can be seen from Table 1, BiVO alone 4 The catalyst has poor purifying efficiency on dioxin, namely 44%; sheetHexavalent metallic oxide cocatalyst MoO 3 And WO 3 The purification efficiency of dioxin is lower than 15 percent; the single divalent metal oxide promoters, CuO, NiO, ZnO and CoO, have substantially no effect on dioxins.
Comparative example 8
This comparative example provides a BiVO 4 -MoO 3 The catalyst is prepared by mixing BiVO in comparative example 1 4 Catalyst and hexavalent Metal oxide cocatalyst MoO of comparative example 2 3 Ball-milling for 4h according to the weight ratio of 1: 0.2, and then placing the mixture in a muffle furnace for firing for 5h at 700 ℃ to obtain BiVO 4 -MoO 3 And (3) compounding a catalyst.
Comparative example 9
This comparative example provides a BiVO 4 -WO 3 The catalyst is prepared by mixing BiVO in comparative example 1 4 Catalyst and hexavalent Metal oxide cocatalyst WO in comparative example 3 3 Ball-milling for 4h according to the weight ratio of 1: 0.2, and then placing the mixture in a muffle furnace for firing for 5h at 700 ℃ to obtain BiVO 4 -WO 3 And (3) compounding a catalyst.
Example 1
This embodiment provides a BiVO 4 -WO 3 A CuO catalyst prepared by reacting BiVO of comparative example 1 4 Catalyst, hexavalent Metal oxide cocatalyst WO in comparative example 3 3 And a divalent metal oxide cocatalyst CuO in the comparative example 4 according to the weight ratio of 1: 0.2: 0.1, placing the mixture in a muffle furnace for firing at 700 ℃ for 5 hours to obtain BiVO 4 -WO 3 -a CuO composite catalyst.
Example 2
This embodiment provides a BiVO 4 -WO 3 -NiO catalyst prepared by reacting BiVO of comparative example 1 4 Catalyst, hexavalent Metal oxide cocatalyst WO in comparative example 3 3 And the divalent metal oxide cocatalyst NiO in the comparative example 5 are mixed and ball-milled for 4h according to the weight ratio of 1: 0.2: 0.1, and then are placed in a muffle furnace for firing at 700 ℃ for 5h to obtain BiVO 4 -WO 3 -NiO composite catalyst.
Example 3
This comparative example provides a BiVO 4 -WO 3 -ZnO catalyst prepared by mixing BiVO of comparative example 1 4 Catalyst, hexavalent Metal oxide cocatalyst WO in comparative example 3 3 And the divalent metal oxide cocatalyst ZnO in the comparative example 6 are mixed and ball-milled for 4h according to the weight ratio of 1: 0.2: 0.1, and then are placed in a muffle furnace for firing at 700 ℃ for 5h to obtain BiVO 4 -WO 3 -ZnO composite catalyst.
Example 4
This comparative example provides a BiVO 4 -WO 3 CoO catalyst prepared by reacting BiVO of comparative example 1 4 Catalyst, hexavalent Metal oxide cocatalyst WO in comparative example 3 3 And the divalent metal oxide cocatalyst CoO in the comparative example 7 are mixed and ball-milled for 4h according to the weight ratio of 1: 0.2: 0.1, and then are placed in a muffle furnace for firing at 700 ℃ for 5h to obtain BiVO 4 -WO 3 -a CoO composite catalyst. BiVO 4 -WO 3 The SEM image of the-CoO composite catalyst is shown in FIG. 2, and the good dispersibility of each component can be seen from the SEM image.
BiVO obtained in comparative examples 8 to 9 4 -AO 3 Composite catalyst and BiVO obtained in examples 1 to 4 4 -AO 3 The performance of the BO composite catalyst for purifying dioxin was tested. The test methods were the same as above, and the results of the performance tests are shown in table 2.
TABLE 2
| Kind of catalyst | Dioxin purification efficiency (%) |
| Comparative example 1BiVO 4 Catalyst and process for preparing same | 44 |
| Comparative example 8BiVO 4 -MoO 3 Catalyst and process for preparing same | 74 |
| Comparative example 9BiVO 4 -WO 3 Catalyst and process for preparing same | 78 |
| Example 1BiVO 4 -WO 3 -CuO catalyst | 86 |
| Example 2BiVO 4 -WO 3 -NiO catalyst | 85 |
| Example 3BiVO 4 -WO 3 -ZnO catalyst | 89 |
| Example 4BiVO 4 -WO 3 catalyst-CoO | 92 |
As can be seen from Table 2, BiVO 4 After the hexavalent metal oxide cocatalyst is compounded, the purification efficiency of the dioxin is improved to more than 70 percent from 44 percent, wherein BiVO 4 -WO 3 Can reach 78%; BiVO 4 After the hexavalent metal oxide cocatalyst and the divalent metal oxide cocatalyst are compounded, the purification efficiency of dioxin is further improved to more than 85 percent, wherein BiVO 4 -WO 3 The purification efficiency of the-CoO composite catalyst to dioxin is the highest and reaches 92 percent.
Meanwhile, it can be seen from a combination of tables 1 and 2 that BiVO 4 -WO 3 BiVO in-CoO composite catalyst 4 The catalyst, the composite hexavalent metal oxide cocatalyst and the divalent metal oxide cocatalyst have a synergistic effect, so that the purifying efficiency of the catalyst on dioxin is further improved。
BiVO with optimal performance 4 -WO 3 The purification efficiency of the CoO composite catalyst for dioxins at different temperatures is detailed in the following table, and the test temperatures are 150 ℃, 200 ℃, 250 ℃, 300 ℃ and 350 ℃.
| BiVO 4 -WO 3 CoO catalyst test temperature | Dioxin purification efficiency (%) |
| 150℃ | 84 |
| 200℃ | 88 |
| 250℃ | 91 |
| 300℃ | 92 |
| 350℃ | 90 |
As can be seen from the above table, BiVO 4 -WO 3 The purification efficiency of the-CoO composite catalyst to dioxin can reach more than 80 percent in the temperature range of 150-350 ℃, the low-temperature catalytic activity is good, and the purification efficiency is optimal and reaches 92 percent at about 300 ℃.
Example 5
This embodiment provides a BiVO 4 -WO 3 The composite catalyst of-CoO supported cordierite ceramic is prepared byBiVO in comparative example 1 4 Catalyst, hexavalent Metal oxide cocatalyst WO in comparative example 3 3 And the divalent metal oxide cocatalyst CoO in the comparative example 7, in a weight ratio of 1: 0.2: 0.1, adding a citric acid template and deionized water at the same time, and ball-milling for 4h to prepare catalyst slurry, wherein the weight ratio of the catalyst, the citric acid template and the deionized water is 1: 4: 8; impregnating a cordierite honeycomb ceramic carrier into the catalyst slurry, uniformly coating, and then placing the catalyst slurry into a muffle furnace to be fired at 700 ℃ for 6 hours to obtain BiVO 4 -WO 3 -a composite catalyst of CoO-supported cordierite ceramic. Repeating the steps of dipping and burning for three times to obtain BiVO with the active component content of about 12 percent 4 -WO 3 -a composite catalyst of a CoO-supported cordierite ceramic.
The BiVO is prepared 4 -WO 3 The CoO supported cordierite ceramic composite catalyst was used in a certain pharmaceutical plant RTO plant, see figure 3. RTO equipment be three room RTO, the regenerator is numbered from left to right 1#, 2# and 3# in proper order, wherein waste gas passes through spark arrester 1, gets into regenerator 6 through admission line 3 under the effect of RTO main air blower 2, is filled with heat accumulation pottery in regenerator 6, is equipped with dioxin decomposition catalyst 5 (being about to BiVO) in bottom heat accumulation pottery below 4 -WO 3 The composite catalyst of the CoO load cordierite ceramic replaces part of heat storage ceramic (bottom)), the air inlet pipeline 3 is connected with the heat storage chamber 6 through an air inlet valve 4, waste gas enters the combustion chamber 7 after being preheated by the heat storage chamber 6 and is heated to the combustion temperature for complete decomposition, the temperature of the combustion chamber 7 is provided by the burner 8, a thermal bypass valve 9 is opened when the combustion chamber 7 is over-heated, the excessive heat is introduced into a mixed flow box 11 through a thermal bypass pipeline 10, the waste gas enters the mixed flow box 11 through an exhaust valve 12 and an exhaust pipeline 13 after being decomposed by the combustion chamber and is mixed with the excessive temperature exhaust gas, and then enters an exhaust funnel 17; during purging, the RTO purge fan 14 is turned on, and clean air enters the regenerator through the purge line 15 and the purge valve 16 to purge. Only one of the inlet valve 4, the exhaust valve 12 and the purge valve 16 corresponding to the same regenerator is opened, for example, the inlet valve of the 1# regenerator is opened in the 1-stage operation state; discharging the combusted waste gas through the No. 2 regenerator, and opening an exhaust valve of the No. 2 regenerator at the moment; blowing in No. 3 regeneratorPurge, at this point, the # 3 regenerator purge valve is open.
The temperature of the heat accumulating type dioxin catalysis layer opened by the exhaust valve is generally 150-300 ℃, so that the dioxin generated by processing chlorine-containing organic matters by RTO can be effectively decomposed. Testing the concentration of the dioxin at the RTO outlet before and after replacement under the same working condition, wherein the concentration of the dioxin at the RTO outlet before replacement is 0.6ng TEQ/Nm 3 After replacement, the concentration of RTO outlet dioxin is 0.08ng TEQ/Nm 3 And the actual application purification efficiency reaches 87%.
Claims (10)
1. A preparation method of a catalyst for purifying dioxin is characterized by comprising the following steps:
the method comprises the following steps:
step one, burning the basic bismuth nitrate to generate Bi 2 O 3 ；
Burning ammonium metavanadate to generate V 2 O 5 ；
Adding Bi 2 O 3 And V 2 O 5 Ball milling, and firing to obtain BiVO 4 A catalyst;
step two, burning the precursor of the hexavalent metal oxide to obtain a hexavalent metal oxide cocatalyst; precursors of the hexavalent metal oxide are ammonium paramolybdate or/and ammonium paratungstate, and the hexavalent metal oxide promoters obtained by burning are MoO 3 、WO 3 ；
Step three, firing the precursor of the divalent metal oxide to obtain a divalent metal oxide cocatalyst; the precursor of the divalent metal oxide is one or more of copper nitrate, nickel nitrate, zinc nitrate or cobalt nitrate, and the promoters of the divalent metal oxide obtained by firing are CuO, NiO, ZnO and CoO respectively;
step four, BiVO obtained in the step three 4 Ball-milling the catalyst, the hexavalent metal oxide cocatalyst obtained in the step two and the divalent metal oxide cocatalyst obtained in the step three, and then firing to obtain BiVO 4 -AO 3 -a BO composite catalyst;
or, BiVO obtained in the third step 4 Catalyst andmixing the hexavalent metal oxide cocatalyst obtained in the step two and the divalent metal oxide cocatalyst obtained in the step three, adding a template agent and deionized water, and performing ball milling to obtain catalyst slurry; then soaking the honeycomb ceramic carrier into the catalyst slurry for uniform coating, and then firing to obtain BiVO 4 -AO 3 -a ceramic supported composite catalyst for BO.
2. The method for preparing a catalyst for purification of dioxin according to claim 1, characterized in that:
in the first step, the basic bismuth nitrate is placed in a muffle furnace to be burnt, the burning temperature is 400-600 ℃, and the burning time is 2-5 h;
the ammonium metavanadate is placed in a muffle furnace for ignition, the ignition temperature is 300-600 ℃, and the ignition time is 2-5 h;
the Bi 2 O 3 And V 2 O 5 Ball milling is carried out according to the stoichiometric ratio of 1: 1, the ball milling time is 2-5h, then the ball milling is placed in a muffle furnace for burning, the burning temperature is 600-700 ℃, and the burning time is 5-10 h.
3. The method for preparing a catalyst for purifying dioxin according to claim 1, characterized in that:
in the second step, the precursor of the hexavalent metal oxide is placed in a muffle furnace to be burned;
the burning temperature of the ammonium paramolybdate is 500-600 ℃, and the burning time is 2-5 h;
the burning temperature of the ammonium paratungstate is 400-600 ℃, and the burning time is 2-5 h.
4. The method for preparing a catalyst for purification of dioxin according to claim 1, characterized in that:
in the third step, the precursor of the divalent metal oxide is placed in a muffle furnace to be burned;
the burning temperature of the copper nitrate, the nickel nitrate, the zinc nitrate and the cobalt nitrate is 200-500 ℃, and the burning time is 2-5 h.
5. The method for preparing a catalyst for purifying dioxin according to claim 1, characterized in that:
wherein BiVO is prepared 4 -AO 3 In step four of the-BO composite catalyst, the BiVO 4 The weight ratio of the catalyst, the hexavalent metal oxide cocatalyst and the divalent metal oxide cocatalyst is 1: 0.1-0.5; the ball milling time is 2-5 h; placing the mixture in a muffle furnace for burning at the temperature of 700 ℃ and 800 ℃ for 5-10 h.
6. The method for preparing a catalyst for purifying dioxin according to claim 1, characterized in that:
wherein BiVO is prepared 4 -AO 3 In step four of the composite catalyst of BO supported ceramic, the BiVO 4 The weight ratio of the catalyst to the hexavalent metal oxide cocatalyst and the divalent metal oxide cocatalyst is 1: 0.1-0.5; the weight ratio of the catalyst, the template agent and the deionized water in the catalyst slurry is 1: 1-5: 5-10; the template agent is glycerol or citric acid; the ball milling time is 2-5 h; placing the mixture in a muffle furnace for burning at the temperature of 600-700 ℃ for 5-10 h.
7. The method for preparing a catalyst for purifying dioxin according to claim 1, characterized in that:
wherein BiVO is prepared 4 -AO 3 In the fourth step of the-BO ceramic-loaded composite catalyst, the honeycomb ceramic carrier is impregnated with the catalyst slurry for multiple times and is burned to obtain the composite catalyst with the active component content of 10% -30%.
8. The method for preparing a catalyst for purification of dioxin according to claim 1, characterized in that:
wherein, in the steps one to four, the temperature rise rate in the burning process is 5-10 ℃/min.
9. The method for preparing a catalyst for purifying dioxin according to claim 1, characterized in that:
wherein, in the first step and the fourth step, the ball milling device is a planetary ball mill, the grinding balls are stainless steel balls or alumina ceramic balls with the diameter of 5mm-10mm, the ball-material ratio is 10-20: 1, and the revolution is 100 plus materials at 500 rpm/min.
10. The catalyst for purification of dioxin produced by the production method according to any one of claims 1 to 9.
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Application publication date: 20220906 Assignee: Nanjing University environmental planning and Design Institute Group Co.,Ltd. Assignor: Nanda enjieyou Environmental Technology (Jiangsu) Co.,Ltd. Contract record no.: X2024980006432 Denomination of invention: A catalyst for dioxin purification and its preparation method Granted publication date: 20230728 License type: Common License Record date: 20240530 |