CN106076316A - A kind of with method that metatitanic acid is the raw material wide operating temperature denitrating catalyst of preparation - Google Patents
A kind of with method that metatitanic acid is the raw material wide operating temperature denitrating catalyst of preparation Download PDFInfo
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- CN106076316A CN106076316A CN201610443697.9A CN201610443697A CN106076316A CN 106076316 A CN106076316 A CN 106076316A CN 201610443697 A CN201610443697 A CN 201610443697A CN 106076316 A CN106076316 A CN 106076316A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 64
- 239000002253 acid Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000002994 raw material Substances 0.000 title claims abstract description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 48
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 48
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 23
- 239000006185 dispersion Substances 0.000 claims abstract description 18
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 16
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 11
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 7
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 7
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 6
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 6
- 239000010937 tungsten Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000010009 beating Methods 0.000 claims abstract description 4
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 8
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 5
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 5
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 5
- 229910000333 cerium(III) sulfate Inorganic materials 0.000 claims description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 4
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 3
- 239000012695 Ce precursor Substances 0.000 claims description 2
- DLUREXGYLIQGCG-UHFFFAOYSA-I [NH4+].[V+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O Chemical compound [NH4+].[V+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O DLUREXGYLIQGCG-UHFFFAOYSA-I 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical group [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims 1
- 241000143437 Aciculosporium take Species 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 7
- 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 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- ODPUKHWKHYKMRK-UHFFFAOYSA-N cerium;nitric acid Chemical compound [Ce].O[N+]([O-])=O ODPUKHWKHYKMRK-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000003546 flue gas Substances 0.000 description 3
- LXASOGUHMSNFCR-UHFFFAOYSA-D [V+5].[V+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O Chemical compound [V+5].[V+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O LXASOGUHMSNFCR-UHFFFAOYSA-D 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000001802 infusion Methods 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- GGKNTGJPGZQNID-UHFFFAOYSA-N (1-$l^{1}-oxidanyl-2,2,6,6-tetramethylpiperidin-4-yl)-trimethylazanium Chemical compound CC1(C)CC([N+](C)(C)C)CC(C)(C)N1[O] GGKNTGJPGZQNID-UHFFFAOYSA-N 0.000 description 1
- 101710194905 ARF GTPase-activating protein GIT1 Proteins 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 102100035959 Cationic amino acid transporter 2 Human genes 0.000 description 1
- 102100021391 Cationic amino acid transporter 3 Human genes 0.000 description 1
- 102100021392 Cationic amino acid transporter 4 Human genes 0.000 description 1
- 101710195194 Cationic amino acid transporter 4 Proteins 0.000 description 1
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 102100029217 High affinity cationic amino acid transporter 1 Human genes 0.000 description 1
- 101710081758 High affinity cationic amino acid transporter 1 Proteins 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 108091006231 SLC7A2 Proteins 0.000 description 1
- 108091006230 SLC7A3 Proteins 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910000004 White lead Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229940071125 manganese acetate Drugs 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
-
- 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
- B01D53/90—Injecting reactants
-
- 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
- B01J23/30—Tungsten
-
- 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
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
-
- 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
- B01J35/396—Distribution of the active metal ingredient
- B01J35/399—Distribution of the active metal ingredient homogeneously throughout the support particle
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of method being the wide operating temperature denitrating catalyst of raw material preparation with metatitanic acid, specifically comprise the following steps that metatitanic acid is added to the water making beating by a., ammonium salt dispersion is added and with ammonia regulation pH value to 3 ~ 6 in serosity, add cerium and tungsten presoma, addition ammonia regulation pH value, to 6 ~ 10, is prepared as CeO after filtration, drying, roasting2‑WO3/TiO2Powder body；B. vanadium presoma is dissolved in oxalic acid aqueous solution, adds described CeO2‑WO3/TiO2Powder body, stirring, it is prepared as V after drying, roasting2O5‑CeO2‑WO3/TiO2Catalyst.With existing industry V2O5‑WO3/TiO2Catalyst is compared, and denitrating catalyst prepared by the present invention has operating temperature width, denitration efficiency height, water resistant and anti-SO2The features such as ability is strong.
Description
Technical field
The present invention relates to a kind of method being the wide operating temperature denitrating catalyst of raw material preparation with metatitanic acid.
Background technology
Nitrogen oxides (NOx) can cause acid rain, photochemical fog etc. to affect the pollutant of environment, and it is also current air
The emphasis of environmental conservation and difficult point.According to incompletely statistics, the atmosphere pollution of China there is the NOx of more than 90% come from coal, stone
The combustion process of oil, natural gas etc..In numerous gas denitrifying technologies, SCR denitration technology is a kind of efficient denitrating flue gas
Technology, it is the history of existing more than 30 year for coal-burning power plant, has the advantages such as denitration efficiency height, moderate cost.Anti-according to catalysis
The kind of temperature and catalyst, SCR technique is answered to be divided into high temperature, middle gentle low temperature three kinds.Generally higher than 400 DEG C is high temperature, 300 ~
400 DEG C is middle temperature, is low temperature less than 300 DEG C.At present, to SCR denitration technology the most ripe be middle temperature catalyst, generally
For V2O5-WO3/TiO2Catalyst.But V2O5-WO3/TiO2Catalyst temperature window narrow (320 ~ 420 DEG C), largely affects
The application of catalyst.Therefore, the denitrating catalyst research carrying out wide operating temperature is extremely important.
In terms of wide operating temperature denitrating catalyst, have some scholars both at home and abroad and carried out research work:
CN103894182A discloses interval catalyst for denitrating flue gas of a kind of wide active temperature and preparation method thereof, and inventor adopts
With ball-milling method by variable valency metal oxide and V2O5-WO3/TiO2The common ball milling of catalyst so that it is mechanical mixture is uniform.But, should
Method is industrially difficult to.
CN104001497A discloses a kind of wide temperature window denitrating catalyst and preparation method thereof, and catalyst is by carrier
Forming with active component two parts, carrier is particle diameter 20 ~ 40nmCeO2And ZrO2Mixing is constituted, and active component is V2O5、V3O5、
VO2、V2O3In one or more, use coprecipitation and infusion process to combine and prepare.Catalyst is at the cigarette of 250 ~ 450 DEG C
Gas has preferable denitration effect, but the not detailed examination such as the denitration efficiency of catalyst and water resistant sulfur resistance.
CN104258872A discloses the denitration catalyst material preparation method of a kind of low temperature wide active temperature windows, with inclined titanium
Acid is support precursor, and Mn oxide is active component, adds nickel oxide auxiliary agent, uses coprecipitation to prepare.Urging of preparation
Agent low-temperature denitration rate is high, and active temperature windows width, 120 ~ 260 DEG C of denitration rates up to more than 90%.But, manganese-based catalyst
Water resistant sulfur resistance unsatisfactory.
CN104525216A discloses a kind of denitrating catalyst under the conditions of wide temperature window high-sulfur and preparation side thereof
Method.Preparation method is in business V2O5-WO3/TiO2Catalyst preparation process is added ferric nitrate, iron sulfate, manganese acetate or nitric acid
Cerium, obtains in wider high temperature interval 260 ~ 420 DEG C, 1000ppmSO2Under the conditions of, there is good anti-SO2Performance, denitration rate
The catalyst of more than 80%.But, the denitration efficiency of catalyst is on the low side.
In sum, domestic and international patent is about wide temperature denitrating catalyst preparation method, and majority is in existing commercial catalysts
V2O5-WO3/TiO2On the basis of, introducing transition metal oxide or rare-earth oxide realize, the catalyst of preparation
Widen the operating temperature of catalyst to a certain extent.But owing to using physical method mixing, active component and catalyst promoter
, there is the problems such as accumulation or embedding in dispersion heterogeneity, active component and auxiliary agent are difficult to collaborative playing a role, and operating temperature window
Mouth expanded scope is limited.
Summary of the invention
The invention provides a kind of method being the wide operating temperature denitrating catalyst of raw material preparation with metatitanic acid.
The present invention is with metatitanic acid as raw material, through making beating dispersion, adds ammonium salt and disperses and regulate pH value, add Ce in serosity
With W presoma, add ammonia regulation pH value, after filtration, drying, roasting, be prepared as CeO2-WO3/TiO2Powder body, then load
V2O5, it is prepared as V2O5-CeO2-WO3/TiO2Catalyst.
A kind of with method that metatitanic acid is the raw material wide operating temperature denitrating catalyst of preparation, it is characterised in that concrete steps are such as
Under:
A. be added to the water making beating by metatitanic acid, adds ammonium salt dispersion and with ammonia regulation pH value to 3 ~ 6, add in serosity
Cerium and tungsten presoma, addition ammonia regulation pH value, to 6 ~ 10, is prepared as CeO after filtration, drying, roasting2-WO3/TiO2Powder body；
B. vanadium presoma is dissolved in oxalic acid aqueous solution, adds described CeO2-WO3/TiO2Powder body, stirring, after drying, roasting
It is prepared as V2O5-CeO2-WO3/TiO2Catalyst.
V in described catalyst2O5、CeO2、WO3、TiO2Content be followed successively by 0.5 ~ 1.5wt.%, 0.1 ~ 10wt.%, 1 ~
8wt.%、80~95wt.%。
The concentration of described metatitanic acid serosity is 100 ~ 600g/L.
Described ammonium salt one in ammonium carbonate, ammonium sulfate, ammonium citrate.
Described cerium precursor one in cerous nitrate, cerous sulfate, ammonium ceric nitrate.
Described tungsten presoma one in ammonium tungstate, ammonium metatungstate, ammonium paratungstate.
Drying temperature described in step a is 80 ~ 120 DEG C, and sintering temperature is 500 ~ 600 DEG C, and roasting time is 2 ~ 5h.
Vanadium presoma described in step b is 5-20g/L with the mass volume ratio of oxalic acid aqueous solution.
The concentration of described oxalic acid aqueous solution is 1.18mol/L.
Described vanadium presoma one in ammonium metavanadate, vanadium oxalate ammonium.
The denitrating catalyst prepared by the present invention has operating temperature width, denitration efficiency height, water resistant and anti-SO2Ability is strong
Feature.Catalyst is 220 ~ 450 DEG C, 500ppmSO in wider temperature range2Under conditions of, denitration rate can reach more than 90%.
Metatitanic acid, with metatitanic acid as raw material, is first disperseed by the present invention with ammonium salt and ammonia, under charge ion effect,
Metatitanic acid is in high Dispersion on surface state.Cerium and tungsten presoma are precipitated in surface and the duct of metatitanic acid simultaneously, are formed
CeO2And WO3Crystallite, utilizes the synergism between Ce-W simultaneously, improves the activity of catalyst.On this basis, draw further
Enter active component V2O5, utilize V2O5-CeO2-WO3Interaction, improve the activity of catalyst, sulfur resistive water resistant ability.
Catalyst prepared by the present invention has carrier TiO2Crystal grain is little, V2O5、CeO2、WO3Active component particle diameter is little and disperses
The feature such as uniformly.
It is relatively easy that the technology of preparing of catalyst of the present invention also has production process, it is easy to the features such as enforcement.
Detailed description of the invention
The assay method of various embodiments of the present invention and comparative example is:
The assessing terms of activity rating: screening 20 ~ 40 mesh beaded catalyst loading amounts 0.4g, reaction temperature is 180 ~ 500 DEG C, gas
Condition is: 500ppmNH3+500ppmNO+ 500ppSO2+5%O2, N2Balance, pressure is normal pressure, and air speed is 30000mlmg-1h-1,
Conversion ratio with NO measures the reactivity of catalyst, and product KM9106 flue gas analyzer is analyzed.
Embodiment 1
A. take 20g metatitanic acid and join in 43.2g water, dispersion of pulling an oar at normal temperatures, in serosity, add 0.30g ammonium citrate
Dispersion, stirred in water bath 1h of 70 DEG C, progressively drips ammonia and regulates pH value to 5.Weigh 0.32g ammonium tungstate and 1.27g nitre
Acid cerium is dissolved in 10mL water together, and dropwise adds in above-mentioned solution.Add ammonia regulation pH value to 8, through filter, 100 DEG C
It is prepared as CeO after drying, 550 DEG C of roasting 2h2-WO3/TiO2Powder body.
B. weigh 0.13g ammonium metavanadate and add in 10mL oxalic acid aqueous solution, 40 DEG C of stirred in water bath 2h to the most molten
Solve, take the powder body of preparation in 9.87g step a and add, stirring, it is prepared as V after drying, 600 DEG C of roasting 2h2O5-CeO2-WO3/
TiO2Catalyst.Catalyst is designated as CAT-1.
Embodiment 2
A. take 20g metatitanic acid and join in 35.0g water, dispersion of pulling an oar at normal temperatures, in serosity, add 0.48g ammonium carbonate divide
Dissipate, stirred in water bath 1h of 70 DEG C, progressively drip ammonia and regulate pH value to 5.5.Weigh 0.16g ammonium paratungstate and 1.62g
Cerous sulfate is dissolved in 10mL water together, and dropwise adds in above-mentioned solution.Add ammonia regulation pH value to 9, through filter, 100
DEG C dry, be prepared as CeO after 600 DEG C of roasting 2h2-WO3/TiO2Powder body.
B. weigh 0.11g vanadium oxalate and add in 10mL oxalic acid aqueous solution, 40 DEG C of stirred in water bath 2h to being completely dissolved,
Take the powder body of preparation in 9.89g step a to add, stirring, after drying, 600 DEG C of roasting 2h, be prepared as V2O5-CeO2-WO3/TiO2
Catalyst.Catalyst is designated as CAT-2.
Embodiment 3
A. take 20g metatitanic acid and join in 49.6g water, dispersion of pulling an oar at normal temperatures, in serosity, add 0.29g ammonium sulfate divide
Dissipate, stirred in water bath 1h of 70 DEG C, progressively drip ammonia and regulate pH value to 4.5.Weigh 0.50g ammonium metatungstate and 0.64g
Cerous sulfate is dissolved in 10mL water together, and dropwise adds in above-mentioned solution.Add ammonia regulation pH value to 7, through filter, 80 DEG C
It is prepared as CeO after drying, 580 DEG C of roasting 3h2-WO3/TiO2Powder body.
B. weigh 0.16g ammonium metavanadate and add in 10mL oxalic acid aqueous solution, 40 DEG C of stirred in water bath 2h to the most molten
Solve, take the powder body of preparation in 9.84g step a and add, stirring, it is prepared as V after drying, 600 DEG C of roasting 2h2O5-CeO2-WO3/
TiO2Catalyst.Catalyst is designated as CAT-3.
Embodiment 4
A. take 20g metatitanic acid and join in 41.5g water, dispersion of pulling an oar at normal temperatures, in serosity, add 0.36g carbon lemon acid ammonium
Dispersion, stirred in water bath 1h of 70 DEG C, progressively drips ammonia and regulates pH value to 4.Weigh 0.55g ammonium paratungstate and 0.15g
Ammonium ceric nitrate is dissolved in 10mL water together, and dropwise adds in above-mentioned solution.Add ammonia regulation pH value to 6.5, through filter,
It is prepared as CeO after 120 DEG C of drying, 520 DEG C of roasting 4h2-WO3/TiO2Powder body.
B. weigh 0.11g ammonium metavanadate and add in 10mL oxalic acid aqueous solution, 40 DEG C of stirred in water bath 2h to the most molten
Solve, take the powder body of preparation in 9.89g step a and add, stirring, it is prepared as V after drying, 600 DEG C of roasting 2h2O5-CeO2-WO3/
TiO2Catalyst.Catalyst is designated as CAT-4.
Embodiment 5
A. take 20g metatitanic acid and join in 38.2g water, dispersion of pulling an oar at normal temperatures, in serosity, add 0.40g ammonium citrate
Dispersion, stirred in water bath 1h of 70 DEG C, progressively drips ammonia and regulates pH value to 4.5.Weigh 0.40g ammonium paratungstate and
1.00g cerous nitrate is dissolved in 10mL water together, and dropwise adds in above-mentioned solution.Addition ammonia regulation pH value, to 7.5, passes through
It is prepared as CeO after filter, 100 DEG C of drying, 580 DEG C of roasting 1h2-WO3/TiO2Powder body.
B. weigh 0.15g vanadium oxalate and add in 10mL oxalic acid aqueous solution, 40 DEG C of stirred in water bath 2h to being completely dissolved,
Take the powder body of preparation in 9.85g step a to add, stirring, after drying, 600 DEG C of roasting 2h, be prepared as V2O5-CeO2-WO3/TiO2
Catalyst.Catalyst is designated as CAT-5.
Embodiment 6
A. take 20g metatitanic acid and join in 45.6g water, dispersion of pulling an oar at normal temperatures, in serosity, add 0.45g ammonium sulfate divide
Dissipate, stirred in water bath 1h of 70 DEG C, progressively drip ammonia and regulate pH value to 5.5.Weigh 0.45g ammonium paratungstate and 0.85g
Cerous sulfate is dissolved in 10mL water together, and dropwise adds in above-mentioned solution.Add ammonia regulation pH value to 8, through filter, 100
DEG C dry, be prepared as CeO after 590 DEG C of roasting 2h2-WO3/TiO2Powder body.
B. weigh 0.16g ammonium metavanadate and add in 10mL oxalic acid aqueous solution, 40 DEG C of stirred in water bath 2h to the most molten
Solve, take the powder body of preparation in 9.84g step a and add, stirring, it is prepared as V after drying, 600 DEG C of roasting 2h2O5-CeO2-WO3/
TiO2Catalyst.Catalyst is designated as CAT-6.
Embodiment 7
A. take 20g metatitanic acid and join in 51.6g water, dispersion of pulling an oar at normal temperatures, in serosity, add 0.38g ammonium sulfate divide
Dissipate, stirred in water bath 1h of 70 DEG C, progressively drip ammonia and regulate pH value to 6.Weigh 0.55g ammonium paratungstate and 0.65g nitre
Acid cerium is dissolved in 10mL water together, and dropwise adds in above-mentioned solution.Add ammonia regulation pH value to 9.5, through filter, 100
DEG C dry, be prepared as CeO after 500 DEG C of roasting 4h2-WO3/TiO2Powder body.
B. weigh 0.16g ammonium metavanadate and add in 10mL oxalic acid aqueous solution, 40 DEG C of stirred in water bath 2h to the most molten
Solve, take the powder body of preparation in 9.84g step a and add, stirring, it is prepared as V after drying, 600 DEG C of roasting 2h2O5-CeO2-WO3/
TiO2Catalyst.Catalyst is designated as CAT-7.
Comparative example 1
Infusion process is used to prepare 1%V2O5-5%WO3/TiO2, take 10g commercial titanium white lead, add the ammonium metavanadate, partially measured
Ammonium tungstate, oxalic acid mixed solution, after being through impregnation with 2h, 100 DEG C of drying, 600 DEG C of roasting 2h.Catalyst is designated as DB-1.
Comparative example 2
A. take 20g metatitanic acid and join in 40g water, dispersion of pulling an oar at normal temperatures, in serosity, add the dispersion of 0.35g ammonium carbonate,
Stirred in water bath 1h of 70 DEG C, progressively drip ammonia and regulate pH value to 5.Weigh 0.32g ammonium tungstate to be dissolved in 10mL water,
And dropwise add in above-mentioned solution.Addition ammonia regulation pH value, to 8, is prepared as after filtration, 100 DEG C of drying, 550 DEG C of roasting 2h
WO3/TiO2Powder body.
B. weigh 0.15g ammonium metavanadate and add in 10mL oxalic acid aqueous solution, 40 DEG C of stirred in water bath 2h to the most molten
Solve, take the powder body of preparation in 9.85g step a and add, stirring, it is prepared as V after drying, 600 DEG C of roasting 2h2O5-WO3/TiO2Urge
Agent.Catalyst is designated as DB-2.
Catalyst performance after tested, such as following table.
。
Claims (10)
1. the method that a kind is the wide operating temperature denitrating catalyst of raw material preparation with metatitanic acid, it is characterised in that concrete steps are such as
Under:
A. be added to the water making beating by metatitanic acid, adds ammonium salt dispersion and with ammonia regulation pH value to 3 ~ 6, add in serosity
Cerium and tungsten presoma, addition ammonia regulation pH value, to 6 ~ 10, is prepared as CeO after filtration, drying, roasting2-WO3/TiO2Powder body；
B. vanadium presoma is dissolved in oxalic acid aqueous solution, adds described CeO2-WO3/TiO2Powder body, stirring, after drying, roasting
It is prepared as V2O5-CeO2-WO3/TiO2Catalyst.
2. the method for claim 1, it is characterised in that V in described catalyst2O5、CeO2、WO3、TiO2Content successively
It is 0.5 ~ 1.5wt.%, 0.1 ~ 10wt.%, 1 ~ 8wt.%, 80 ~ 95wt.%.
3. the method for claim 1, it is characterised in that the concentration of described metatitanic acid serosity is 100 ~ 600g/L.
4. the method for claim 1, it is characterised in that described ammonium salt is in ammonium carbonate, ammonium sulfate, ammonium citrate
A kind of.
5. the method for claim 1, it is characterised in that described cerium precursor is selected from cerous nitrate, cerous sulfate, ammonium ceric nitrate
In one.
6. the method for claim 1, it is characterised in that described tungsten presoma is selected from ammonium tungstate, ammonium metatungstate, para-tungstic acid
One in ammonium.
7. the method for claim 1, it is characterised in that drying temperature described in step a is 80 ~ 120 DEG C, sintering temperature
Being 500 ~ 600 DEG C, roasting time is 2 ~ 5h.
8. the method for claim 1, it is characterised in that vanadium presoma described in step b and the mass body of oxalic acid aqueous solution
Long-pending ratio is 5-20g/L.
9. the method as described in claim 1 or 8, it is characterised in that the concentration of described oxalic acid aqueous solution is 1.18mol/L.
10. the method as described in claim 1 or 8, it is characterised in that described vanadium presoma is in ammonium metavanadate, vanadium oxalate ammonium
One.
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