CN108114718A - A kind of Ce-Zr-M overall structures combustion catalyst and preparation method - Google Patents
A kind of Ce-Zr-M overall structures combustion catalyst and preparation method Download PDFInfo
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- CN108114718A CN108114718A CN201611088281.6A CN201611088281A CN108114718A CN 108114718 A CN108114718 A CN 108114718A CN 201611088281 A CN201611088281 A CN 201611088281A CN 108114718 A CN108114718 A CN 108114718A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 73
- 238000002485 combustion reaction Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000000576 coating method Methods 0.000 claims abstract description 57
- 239000011248 coating agent Substances 0.000 claims abstract description 35
- 239000007789 gas Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 13
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 13
- 239000011593 sulfur Substances 0.000 claims abstract description 13
- 239000000919 ceramic Substances 0.000 claims abstract description 12
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 12
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 11
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- 239000012855 volatile organic compound Substances 0.000 claims abstract description 4
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 3
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 3
- 239000003034 coal gas Substances 0.000 claims abstract 2
- 239000003345 natural gas Substances 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 64
- 238000001035 drying Methods 0.000 claims description 24
- 239000006255 coating slurry Substances 0.000 claims description 21
- 230000001413 cellular effect Effects 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 14
- 230000009467 reduction Effects 0.000 claims description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 13
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 11
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 11
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 4
- 229910052878 cordierite Inorganic materials 0.000 claims description 4
- 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 claims description 4
- 229910018879 Pt—Pd Inorganic materials 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims 2
- 229910021641 deionized water Inorganic materials 0.000 claims 2
- 239000000567 combustion gas Substances 0.000 claims 1
- 238000007598 dipping method Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract 2
- 238000010304 firing Methods 0.000 abstract 1
- 239000000446 fuel Substances 0.000 abstract 1
- 241000264877 Hippospongia communis Species 0.000 description 28
- 239000003643 water by type Substances 0.000 description 18
- 238000000034 method Methods 0.000 description 12
- 238000006722 reduction reaction Methods 0.000 description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 9
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical class O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 description 9
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical class [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 206010019233 Headaches Diseases 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 210000003169 central nervous system Anatomy 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical class O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 231100000869 headache Toxicity 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 208000024891 symptom Diseases 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910001122 Mischmetal Inorganic materials 0.000 description 1
- 208000005374 Poisoning Diseases 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 229910003158 γ-Al2O3 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
- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/648—Vanadium, niobium or tantalum or polonium
- B01J23/6482—Vanadium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8993—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with chromium, molybdenum or tungsten
-
- B01J35/56—
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
-
- 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
Abstract
The invention discloses a kind of Ce Zr M overall structures combustion catalysts and preparation methods.The matrix of catalyst uses integral honeycomb, and in the oxide and oxide M of matrix surface coating Ce, Zr, wherein oxide M is made of by a certain percentage one or more of Ti, Si, Al, V, W, Co oxide;Then on the carrier for coating the mixed oxide coatings, active component Pt, Pd is impregnated.Ce, Zr, M ratio are 1 in the oxide coating:0.1~4:1~50, on the basis of integral honeycomb ceramics weight, Ce, Zr oxide and the ratio shared by M are 0 30wt%, and active component Pt, Pd or ratio shared by Pt Pd are 0.01wt% 0.2wt%.Overall structure catalyst disclosed by the invention has high activity and stability, and firing point is low, and resistance drop is small, and catalyst preparation process is simple, at low cost.Suitable for being purified by the water heater of fuel or the combustion tail gas of gas fired-boiler of natural gas, oil liquefied gas or coal gas, it can also be used to which sulfur-bearing VOCs gases efficient removal purifies.
Description
Technical field
The invention belongs to be catalyzed burning situation protection field, and in particular to a kind of Ce-Zr-M overall structures combustion catalyst
And preparation method..
Background technology
CO is the unburnt product of the carbonaceous materials such as coal, oil, is a kind of colourless, odorless, nonirritant toxic
Gas, is practically insoluble in water, is not easy to generate chemical reaction with other substances in air, CO is not easy to spread, stop in surface air
Stay the time longer.Time length will generate anoxic and damage the central nervous system of people after human contact CO, when CO concentration reaches
30mg/m3When, so that it may cause weak, lip of having a headache that will generate anoxic in symptoms, time length such as bright cherry-red, palpitating speeds and damage
The central nervous system of victimization causes the symptoms such as giddy, headache, physiology discomfort, fatigue, excessively high CO concentration or is connect when serious
Death can all be caused for a long time by touching, and China is every year because gas heater CO poisonings happen occasionally.Therefore, the discharge pair of CO
The health of the mankind has very serious consequence, causes the common concern of people.
The removing method of CO includes physical absorption null method and chemical conversion null method.Physical absorption null method is mainly profit
CO is adsorbed with the porous material (such as porous carbon, activated carbon) of large specific surface area.But physics null method has shortcomings:It inhales
Attached efficiency is low, equipment volume is big, frequently replaces.Chemical conversion null method mainly includes catalytic reduction method and catalytic oxidation.It urges
It is the C being reduced to CO by active hydrogen atom etc. with more utility value to change reduction methodxHyOzType compound, but at present should
Method only rests on laboratory theoretical research level, and according to promoting and applying, also there are larger gaps;It is normal that big volume low-concentration CO is eliminated at present
Method is catalytic oxidation.It is described in Chinese patent 101474566 by honeycomb ceramic carrier in coated on γ-Al2O3It applies
The catalyst and preparation method that layer and base metal copper/manganese/silver composite oxides form, using equi-volume impregnating by forerunner
Somaplasm material is carried on cordierite honeycomb ceramic carrier, and monolithic catalyst is made through dry and calcination process.The catalyst preparation
It is at low cost, but sulfur tolerance and stability are unknown.Chinese patent 102407130 discloses a kind of catalysis burning composition metal oxygen
The preparation method of compound integral catalyzer, using Co, Mn, Ce salt and carbonate as raw material, using coprecipitation prepares coating material
Expect CeO2, then Co, Mn salting liquid loaded into coating material CeO by different mol ratio2In, Co/Mn/ is made after drying, roasting
CeO2Composite oxide power catalyst is coated to using ball milling, soaking paste on ceramic honey comb, is most made afterwards through drying, roasting
Integral catalyzer, which has the features such as at low cost, catalytic activity is high, but sulfur tolerance is unknown.Chinese patent
A kind of preparation method that noble metal active component Pt-Pd is supported on to cordierite monolithic catalyst is introduced in 103831104A,
The component of coating is Al2O3、SiO2, cerium-rich mischmetal oxide, the mixture of K, although mixed coating material effect can be with,
But preparation process is comparatively laborious.For this purpose, the object of the present invention is to provide a kind of preparation process is simple, catalytic activity is high, resistant to sulfur
The good combustion catalyst preparation process of property.
The content of the invention
For presently disclosed resistant to sulfur combustion catalyst preparation process it is complicated, of high cost, the Sulfur tolerance of resistance to hydro-thermal is poor the features such as,
The present invention proposes a kind of overall structure combustion catalyst simple for process, manufacture is at low cost, mithridatism is good and preparation method.
The present invention provides a kind of Ce-Zr-M overall structures combustion catalyst, and the preparation of the catalyst uses following technology
Scheme:
A kind of Ce-Zr-M overall structures combustion catalyst provided by the invention, using integral honeycomb ceramics as carrier, in its table
Face coats Ce, Zr and M oxide, and wherein M is by one or more of Ti, Si, Al, V, W, Co oxide group by a certain percentage
Into;Then on the carrier for loading the composite oxide coating, active component Pt, Pd is impregnated;With integral honeycomb ceramics weight
On the basis of, ratio shared by all oxides of Ce, Zr, M is 0-30wt%, active component Pt, Pd or the ratio shared by Pt-Pd
For 0.01wt%-0.2wt%,
Ce, Zr, M molar ratio are 1 in the oxide coating:0.5~4:1~50, mole of active component Pd and Pt
Than for 0.25~4:1.
The integral honeycomb ceramics are cordierite honeycomb ceramic or metal beehive.
The present invention provides a kind of preparation method of Ce-Zr-M overall structures combustion catalyst, is as follows:
(1) prepared by coating slurry:First, it is 1 according to molar ratio by the nitrate of Ce, Zr:0.1~4 is added to deionization
In water, the solution A of 0.1-2.0mol/L is made;The water-soluble precursor of M oxide and oxide sol are added to deionization
In water, the solution B that concentration is 0.1-1.5mol/L is made;In mass ratio 1:A, B solution are added to ball milling by 0.33~2 ratio
In tank, by the mixture under 500 revs/min of rotating speed, when ball milling 1-4 is small, coating slurry is obtained;
(2) prepared by coating:Integral honeycomb carrier is immersed in slurry made from step (1), honeycomb is blown out with compressed air
Extra coating solution in carrier hole;Then, the honeycomb substrate of oxide coating will be coated with after microwave drying 1-15 minutes, in
When 300-1000 DEG C of roasting 1-7 is small, when preferably 400-800 DEG C roasting 2-5 is small, obtain scribbling the carrier of mixed oxide coatings;
(3) active component loads:The carrier for scribbling mixed oxide coatings is immersed into palladium nitrate solution (concentration range successively
Between 1-15mg/ml) or platinum nitrate solution (concentration range is between 1-15mg/ml) or once it is immersed in palladium nitrate and nitre
(for Pd, Pt concentration range between 1-15mg/ml, wherein palladium and platinum molar ratio range is 0.25~4 for the mixed solution of sour platinum:1
Between), solution extra in cellular set body opening is blown out with compressed air;After microwave drying 1-15 minutes, in 300-700 DEG C of roasting
When burning 1-7 is small, when preferably 400-600 DEG C roasting 2-4 is small, so as to which overall structure catalyst be made.
(4) reduction of catalyst:By catalyst made from step (3) in 10vol.%H2- 90vol.%N2Under atmosphere, 450
DEG C reduction 1-4 it is small when, be made reduction after overall structure catalyst, for use.
A kind of application of Ce-Zr-M overall structures combustion catalyst provided by the present invention, the catalyst are applied to
Sulfur-bearing carbon monoxide, methane or the removing of sulfur-bearing VOCs gas catalysis.
A kind of application of Ce-Zr-M overall structures combustion catalyst provided by the present invention is removed applied to carbon monoxide
Reaction, reaction velocity 2,000-100,000h-1, unstripped gas CO contents 100-200ppm, SO2Content 20ppm, catalyst can be
Realize that CO is converted completely at 200 DEG C.
The Ce-Zr-M overall structure combustion catalysts of the present invention have the following advantages that:
1. the Ce-Zr-M overall structure combustion catalysts of the present invention under higher space velocities, there is high catalysis to live
Property and stability;
2. the Ce-Zr-M overall structure combustion catalysts of the present invention, have the characteristics that its initiation temperature is low, resistance drop is small;
3. the Ce-Zr-M overall structure combustion catalysts of the present invention, the sulfur tolerance of resistance to hydro-thermal is good, is applicable not only to sulfur-bearing combustion
Tail gas removal of carbon monoxide is burnt, applies also for sulfur-bearing VOCs gas purifications;
4. the Ce-Zr-M overall structure combustion catalysts of the present invention, preparation process is simple, and manufacture is at low cost.
Specific embodiment
Below to the detailed description of the invention, only presently preferred embodiments of the present invention below, it is impossible to limit the present invention's with this
Scope.I.e. all equivalent changes and modifications done according to scope of the present invention patent should all belong to the scope that the present invention is covered.
Embodiment 1
Weigh 26.05g cerium nitrate hexahydrates, five water zirconium nitrates of 25.76g are dissolved in 200ml deionized waters, obtained solution A;Claim
9.36g ammonium metavanadates is taken to be added in 200ml deionized waters, boil dissolving, it is molten then to add in 16g titaniums colloidal sol, 10g silicon wherein
Glue obtained solution B;A, B solution are added in ball grinder again, by the mixture under 500 revs/min of rotating speed, when ball milling 2 is small, obtained
To coating slurry;Integral honeycomb carrier is immersed in coating slurry, with extra in compressed air blowout cellular set body opening after taking-up
Coating solution;Then the honeycomb substrate of oxide coating will be coated with through microwave drying after ten minutes, when 650 DEG C of roastings 3 are small,
Obtain scribbling the carrier of mixed oxide coatings;The carrier for scribbling mixed oxide coatings is impregnated into palladium nitrate and platinum nitrate successively
Solution blows out solution extra in cellular set body opening with compressed air;Through microwave drying after five minutes, when 550 DEG C of roastings 4 are small,
So as to which overall structure catalyst be made.By catalyst obtained in 10vol.%H2- 90vol.%N2Under atmosphere, 450 DEG C of reductase 12s
Hour, the overall structure catalyst after reduction is made.
Embodiment 2
Weigh 17.36g cerium nitrate hexahydrates, five water zirconium nitrates of 17.17g are dissolved in 300ml deionized waters, obtained solution A;Again
It weighs 23.4g ammonium metavanadates to be added in 400ml deionized waters, boils dissolving, then add in 16g titaniums colloidal sol, 10g aluminium wherein
Colloidal sol obtained solution B;A, B solution are added in ball grinder, by the mixture under 500 revs/min of rotating speed, when ball milling 3 is small, obtained
To coating slurry;Integral honeycomb carrier is immersed in coating slurry, with extra in compressed air blowout cellular set body opening after taking-up
Coating solution;Then the honeycomb substrate of oxide coating will be coated with through microwave drying after ten minutes, when 650 DEG C of roastings 2 are small,
Obtain scribbling the carrier of mixed oxide coatings;The carrier for scribbling mixed oxide coatings is immersed into palladium nitrate and platinum nitrate successively
Solution blows out solution extra in cellular set body opening with compressed air;Through microwave drying after five minutes, when 600 DEG C of roastings 3 are small,
So as to which overall structure catalyst be made.By catalyst obtained in 10vol.%H2- 90vol.%N2Under atmosphere, 450 DEG C of reductase 12s
Hour, the overall structure catalyst after reduction is made.
Embodiment 3
Weigh 14.33g cerium nitrate hexahydrates, five water zirconium nitrates of 28.34g are dissolved in 300ml deionized waters, obtained solution A;Again
Weigh 17.55g ammonium metavanadates to be added in 300ml deionized waters, boil dissolving, then add in wherein 27.93g titaniums colloidal sol,
20g Ludox, obtained solution B;A, B solution are added in ball grinder, by the mixture under 500 revs/min of rotating speed, ball milling 2
Hour, obtain coating slurry;Integral honeycomb carrier is immersed in coating slurry, cellular set body opening is blown out with compressed air after taking-up
In extra coating solution;Then the honeycomb substrate of oxide coating will be coated with through microwave drying after ten minutes, in 650 DEG C of roastings
3 it is small when, obtain scribbling the carriers of mixed oxide coatings;By the carrier for scribbling mixed oxide coatings immerse successively palladium nitrate and
Platinum nitrate solution blows out solution extra in cellular set body opening with compressed air;Through microwave drying after five minutes, in 550 DEG C of roastings
4 it is small when, so as to which overall structure catalyst be made.By catalyst obtained in 10vol.%H2- 90vol.%N2Under atmosphere, 450 DEG C
When reductase 12 is small, the overall structure catalyst after reduction is made.
Embodiment 4
Weigh 28.65g cerium nitrate hexahydrates, five water zirconium nitrates of 14.17g are dissolved in 300ml deionized waters, obtained solution A;Again
11.7g ammonium metavanadates is taken to be added in 200ml deionized waters, boil dissolving, then add in wherein again 31.92g titaniums colloidal sol,
15g Ludox, obtained solution B;A, B solution are added in ball grinder again, then added, by the mixture in rotating speed 500
Under rev/min, when ball milling 2 is small, coating slurry is obtained;Integral honeycomb carrier is immersed in coating slurry, compressed air is used after taking-up
Blow out coating solution extra in cellular set body opening;Then the honeycomb substrate of oxide coating will be coated with through microwave drying 10 minutes
Afterwards, when 650 DEG C of roastings 3 are small, obtain scribbling the carrier of mixed oxide coatings;To scribble the carriers of mixed oxide coatings according to
Secondary immersion palladium nitrate and platinum nitrate solution, solution extra in cellular set body opening is blown out with compressed air;Through microwave drying 5 minutes
Afterwards, when 550 DEG C of roastings 4 are small, so as to which overall structure catalyst be made.By catalyst obtained in 10vol.%H2-
90vol.%N2Under atmosphere, when 450 DEG C of reductase 12s are small, the overall structure catalyst after reduction is made.
Embodiment 5
Weigh 13.03g cerium nitrate hexahydrates, five water zirconium nitrates of 12.88g are dissolved in 100ml deionized waters, obtained solution A;Again
It weighs 4.68g ammonium metavanadates to be added in 100ml deionized waters, boils dissolving, add 8g titaniums colloidal sol, 5g Ludox wherein
Obtained solution B;A, B solution are added in ball grinder again, by the mixture under 500 revs/min of rotating speed, when ball milling 2 is small, obtained
Coating slurry;Integral honeycomb carrier is immersed in coating slurry, coating solution extra in cellular set body opening is blown out with compressed air;
Then the honeycomb substrate of oxide coating will be coated with through microwave drying after ten minutes, when 650 DEG C of roastings 3 are small, is scribbled
The carrier of mixed oxide coatings;The carrier for scribbling mixed oxide coatings is once immersed into palladium nitrate and platinum nitrate mixing is molten
Liquid blows out solution extra in cellular set body opening with compressed air;Through microwave drying after five minutes, when 600 DEG C of roastings 4 are small, from
And overall structure catalyst is made.By catalyst obtained in 10vol.%H2- 90vol.%N2Under atmosphere, 450 DEG C of reductase 12s are small
When, the overall structure catalyst after reduction is made.
Embodiment 6
Weigh 39.09g cerium nitrate hexahydrates, five water zirconium nitrates of 38.64g are dissolved in 300ml deionized waters, obtained solution A;Again
It weighs 14.04g ammonium metavanadates to be added in 300ml deionized waters, boils dissolving, add 24g titaniums colloidal sol, 15g silicon wherein
Colloidal sol obtained solution B;A, B solution are added in ball grinder, by the mixture under 500 revs/min of rotating speed, when ball milling 2 is small,
Obtain coating slurry;Integral honeycomb carrier is immersed in coating slurry, painting extra in cellular set body opening is blown out with compressed air
Layer liquid;Then the honeycomb substrate of oxide coating will be coated with through microwave drying after ten minutes, when 650 DEG C of roastings 3 are small, obtained
Scribble the carrier of mixed oxide coatings;The carrier for scribbling mixed oxide coatings is immersed into palladium nitrate solution, uses compressed air
Blow out solution extra in cellular set body opening;Through microwave drying after five minutes, when 550 DEG C of roastings 2 are small, tied so as to be made whole
Structure catalyst.By catalyst obtained in 10vol.%H2- 90vol.%N2Under atmosphere, when 450 DEG C of reductase 12s are small, after reduction is made
Overall structure catalyst.
Embodiment 7
Weigh 13.03g cerium nitrate hexahydrates, five water zirconium nitrates of 12.88g are dissolved in 100ml deionized waters, obtained solution A;Claim
4.68g ammonium metavanadates is taken to be added in 100ml deionized waters, boil dissolving, add 8g titaniums colloidal sol, 5g Ludox systems wherein
Obtain solution B;A, B solution are added in ball grinder again, by the mixture under 500 revs/min of rotating speed, when ball milling 2 is small, applied
Cover slurry;Integral honeycomb carrier is immersed in coating slurry, coating solution extra in cellular set body opening is blown out with compressed air;So
The honeycomb substrate of oxide coating will be coated with afterwards through microwave drying after ten minutes, when 650 DEG C of roastings 3 are small, obtain scribbling mixed
Close the carrier of oxide coating;The carrier for scribbling mixed oxide coatings is immersed into platinum nitrate solution, bee is blown out with compressed air
Extra solution in nest carrier hole;Through microwave drying after five minutes, when 600 DEG C of roastings 4 are small, it is catalyzed so as to which overall structure be made
Agent.By catalyst obtained in 10vol.%H2- 90vol.%N2Under atmosphere, when 450 DEG C of reductase 12s are small, the entirety after reduction is made
Structure catalyst.
Embodiment 8
Weigh 13.03g cerium nitrate hexahydrates, five water zirconium nitrates of 12.88g are dissolved in 100ml deionized waters, obtained solution A;Claim
2.68g ammonium paratungstates, 2g cobalt nitrate hexahydrates is taken to be added in 100ml deionized waters, boils dissolving, it is molten to add 8g titaniums wherein
Glue, 5g Ludox obtained solutions B;A, B solution are added in ball grinder again, by the mixture under 500 revs/min of rotating speed, ball
Grind 2 it is small when, obtain coating slurry;Integral honeycomb carrier is immersed in coating slurry, is blown out with compressed air in cellular set body opening
Extra coating solution;Then the honeycomb substrate of oxide coating will be coated with through microwave drying after ten minutes, 3 is roasted in 650 DEG C
Hour obtains scribbling the carrier of mixed oxide coatings;The carrier for scribbling mixed oxide coatings is immersed into palladium nitrate solution, is used
Extra solution in compressed air blowout cellular set body opening;Through microwave drying after five minutes, when 600 DEG C of roastings 4 are small, so as to make
Obtain overall structure catalyst.By catalyst obtained in 10vol.%H2- 90vol.%N2Under atmosphere, when 450 DEG C of reductase 12s are small, system
Overall structure catalyst after must reducing.
Embodiment 9
Weigh 13.03g cerium nitrate hexahydrates, five water zirconium nitrates of 12.88g are dissolved in 100ml deionized waters, obtained solution A;Claim
2.68g ammonium paratungstates, 2g cobalt nitrate hexahydrates is taken to be added in 100ml deionized waters, boils dissolving, it is molten to add 8g titaniums wherein
Glue, 5g Ludox obtained solutions B;A, B solution are added in ball grinder again, by the mixture under 500 revs/min of rotating speed, ball
Grind 2 it is small when, obtain coating slurry;Integral honeycomb carrier is immersed in coating slurry, is blown out with compressed air in cellular set body opening
Extra coating solution;Then the honeycomb substrate of oxide coating will be coated with through microwave drying after ten minutes, 3 is roasted in 650 DEG C
Hour obtains scribbling the carrier of mixed oxide coatings;By the carrier for scribbling mixed oxide coatings immerse successively palladium nitrate and
Platinum nitrate solution blows out solution extra in cellular set body opening with compressed air;Through microwave drying after five minutes, in 500 DEG C of roastings
4 it is small when, so as to which overall structure catalyst be made.By catalyst obtained in 10vol.%H2- 90vol.%N2Under atmosphere, 450 DEG C
When reductase 12 is small, the overall structure catalyst after reduction is made.
The Ce-Zr-M overall structures combustion catalyst of examples detailed above 1-7 is subjected to activity and estimation of stability, reaction gas mould
Intend sulfur-bearing combustion tail gas composition:H2O=9%, N2=76%, O2=10%, CO2=5%, the SO of CO=200ppm, 20ppm2, it is empty
Fast 100000h-1, catalyst activity and stability are as shown in the table.
Claims (7)
1. a kind of Ce-Zr-M overall structures combustion catalyst, it is characterised in that:The catalyst using integral honeycomb ceramics as carrier,
In the oxide and oxide M of its surface coating Ce, Zr, then on the carrier for loading the composite oxide coating, dipping
Active component Pt, Pd;
On the basis of integral honeycomb ceramics weight, Ce, Zr oxide and the mass ratio shared by M are 0-30wt.%, active component
Mass ratio shared by Pt, Pd or Pt-Pd is 0.01-0.2wt.%.
2. Ce-Zr-M overall structures combustion catalyst according to claim 1, it is characterised in that the M by Ti, Si, Al,
V, one or more of W, Co oxide forms by a certain percentage.
3. Ce-Zr-M overall structures combustion catalyst according to claim 1, it is characterised in that the integral honeycomb ceramics
For cordierite honeycomb ceramic or metal beehive.
4. Ce-Zr-M overall structures combustion catalyst according to claim 1, it is characterised in that active component Pd's and Pt
Molar ratio is 0.25~4:1.
5. Ce-Zr-M overall structures combustion catalyst according to claim 2, it is characterised in that Ce, Zr, M molar ratio is
1:0.5~4:1~50.
6. the preparation method of Ce-Zr-M overall structures combustion catalyst according to claim 1, it is characterised in that including as follows
Step:
(1) prepared by coating slurry:First, it is 1 according to molar ratio by the nitrate of Ce, Zr:0.1~4 is added in deionized water,
The solution A of 0.1-2.0mol/L is made;The water-soluble precursor of M oxide or oxide sol are added in deionized water,
The solution B that concentration is 0.1-1.5mol/L is made;In mass ratio 1:A, B solution are added in ball grinder by 0.33~2 ratio,
By the mixture under 500 revs/min of rotating speed, when ball milling 1-4 is small, coating slurry is obtained;
(2) prepared by coating:Integral honeycomb carrier is immersed in slurry made from step (1), honeycomb substrate is blown out with compressed air
Extra coating solution in hole;Then, the honeycomb substrate of oxide coating will be coated with after microwave drying 1-15 minutes, in 300-
When 1000 DEG C of roasting 1-7 are small, obtain scribbling the carrier of mixed oxide coatings;
(3) active component loads:The palladium nitrate that the carrier for scribbling mixed oxide coatings is immersed to concentration 1-15mg/ml successively is molten
The platinum nitrate solution of liquid and concentration 1-15mg/ml;Or concentration is once immersed in the palladium nitrate and platinum nitrate of 1-15mg/ml
Mixed solution, wherein palladium are with platinum molar ratio range 0.25~4:1, it is blown out with compressed air extra molten in cellular set body opening
Liquid;After microwave drying 1-15 minutes, when 300-700 DEG C of roasting 1-7 is small, so as to which overall structure catalyst before reduction be made;
(4) reduction of catalyst:By catalyst made from step (3) in 10vol.%H2- 90vol.%N2Under atmosphere, 450 DEG C also
When former 1-4 is small, Ce-Zr-M overall structure combustion catalysts are made.
7. the application of Ce-Zr-M overall structures combustion catalyst according to claim 1, it is characterised in that the catalyst should
For using natural gas, oil liquefied gas and coal gas and other are net as the gas heater of combustion gas or the combustion tail gas of gas fired-boiler
Change and purified for sulfur-bearing VOCs gases efficient removal.
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