CN112138658B - Preparation method of integral catalyst for purifying tank tail gas - Google Patents
Preparation method of integral catalyst for purifying tank tail gas Download PDFInfo
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- CN112138658B CN112138658B CN202011057834.8A CN202011057834A CN112138658B CN 112138658 B CN112138658 B CN 112138658B CN 202011057834 A CN202011057834 A CN 202011057834A CN 112138658 B CN112138658 B CN 112138658B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 43
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 41
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000000919 ceramic Substances 0.000 claims abstract description 36
- 239000011248 coating agent Substances 0.000 claims abstract description 35
- 238000000576 coating method Methods 0.000 claims abstract description 35
- WLLURKMCNUGIRG-UHFFFAOYSA-N alumane;cerium Chemical group [AlH3].[Ce] WLLURKMCNUGIRG-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000013543 active substance Substances 0.000 claims abstract description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 46
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 32
- 239000008367 deionised water Substances 0.000 claims description 26
- 229910021641 deionized water Inorganic materials 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 24
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 17
- 229960000583 acetic acid Drugs 0.000 claims description 16
- 239000012362 glacial acetic acid Substances 0.000 claims description 16
- 238000011068 loading method Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 239000011268 mixed slurry Substances 0.000 claims description 14
- 230000032683 aging Effects 0.000 claims description 13
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 12
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 235000006408 oxalic acid Nutrition 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 6
- 229910052878 cordierite Inorganic materials 0.000 claims description 5
- 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 group [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 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- 238000007654 immersion Methods 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 11
- 239000000779 smoke Substances 0.000 abstract description 9
- 238000000746 purification Methods 0.000 abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 239000004071 soot Substances 0.000 description 10
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 5
- 150000002430 hydrocarbons Chemical class 0.000 description 5
- 229910052863 mullite Inorganic materials 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007781 pre-processing Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 241000353097 Molva molva Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 210000001508 eye Anatomy 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 208000019622 heart disease Diseases 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 210000003456 pulmonary alveoli Anatomy 0.000 description 1
- 230000002685 pulmonary effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 208000023504 respiratory system disease Diseases 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—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
- B01J23/63—Platinum group metals with rare earths or actinides
-
- 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
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9445—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC]
-
- 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
-
- B01J35/56—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0207—Pretreatment of the support
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
- B01J37/0217—Pretreatment of the substrate before coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/024—Multiple impregnation or coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/038—Precipitation; Co-precipitation to form slurries or suspensions, e.g. a washcoat
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
Abstract
The invention discloses a preparation method of an integral catalyst for purifying tank tail gas, which comprises a carrier, a bonding coating and an active substance, wherein the carrier is a pretreated honeycomb ceramic filter body, the bonding coating is an aluminum sol coating, and the active substance is cerium-aluminum mixed oxide loaded with noble metal Pt; the preparation steps of the catalyst are as follows: (1) preparing a carrier, (2) preparing an alumina sol, (3) preparing an active substance, (4) preparing a slurry, and (5) preparing a monolithic catalyst. The monolithic catalyst prepared by the invention not only has good carbon smoke particle oxidation removal capability, but also can realize effective purification of CO, HCs and NOx in tail gas.
Description
Technical Field
The invention relates to a tank tail gas purifying catalyst technology, in particular to a preparation method of an integral catalyst for tank tail gas purification.
Background
The tank is a crawler-type armored combat vehicle with direct fire, cross-country capability and armored protection, is one of main weapons of modern land combat, and has the American name of 'the King of land combat'. The tank generally adopts a high-power diesel engine as a power system, and has the characteristics of low rotation speed, large torque, wide torque range, long continuous high-load operation time and the like, and can be normally used under da Leng thermal temperature difference. Tank tail gas is a mixture of components, mainly comprising Hydrocarbon Compounds (HC) and oxynitride (NO) x ) Soot particulate (soot). Wherein NO x Can cause permanent damage to eyes, respiratory system, central nervous system and the like of human body, and NO x Is also the main cause of acid rain; HC is the incomplete combustion product of fuel oil, has the characteristics of toxicity, inflammability, explosiveness, carcinogenesis and the like, and is extremely easy to be combined with NO under the sunshine condition x The photochemical reaction is the main cause of secondary pollution of photochemical smog; the diameter of the carbon smoke particles is usually 0.01-10 microns, the carbon smoke particles are long in residence time and long in transportation distance in the atmosphere, and easily cause large-scale pollution, in addition, the carbon smoke particles also have a strong carcinogenic effect, and the carbon smoke particles are extremely easy to gather at the pulmonary alveoli and other parts of a human body after entering the pulmonary part of the human body along with respiration, so that respiratory diseases, heart diseases and even cancers are caused.
The exhaust purification device is installed on the tank exhaust pipeline, is an effective and economical post-treatment technology, and usually adopts means such as a filter to intercept and trap soot particles in the tank exhaust so as to gather the soot particles in the purification device, but when the soot particles are accumulated to a certain degree, the increase of exhaust back pressure can be caused, the normal exhaust of an engine is influenced, and the soot particles must be removed by means such as combustion so as to keep the normal back pressure of the exhaust, thereby realizing the regeneration of the purification device. If the catalyst is coated on the surface of the filter, HC can be oxidized into non-toxic CO through catalysis 2 And can oxidize NO to NO 2 And go intoStep of utilizing NO 2 The oxidation of the collected soot particles can be realized at low temperature by the strong oxidation capability, so that the effective purification of the tank tail gas pollutants can be realized. Therefore, the development of an economical and efficient tank tail gas purifying catalyst is of great significance, and no report on related documents exists at present.
Disclosure of Invention
In order to solve the problems, the invention provides the integral catalyst for purifying the tank tail gas, which is safe in raw materials, simple in preparation steps, good in economy and good in purifying effect, and the preparation method.
In order to achieve the above object, the present invention is realized by the following technical scheme:
the invention relates to a preparation method of an integral catalyst for purifying tank tail gas, which comprises a carrier, a bonding coating and an active substance, wherein the carrier is a pretreated honeycomb ceramic filter body, the bonding coating is an aluminum sol coating, and the active substance is cerium-aluminum mixed oxide loaded with noble metal Pt; the preparation steps of the catalyst are as follows:
(1) Preparing a carrier: placing the honeycomb ceramic filter body in oxalic acid solution with the mass fraction of 5% -15%, heating to 85-95 ℃, preprocessing for 6-24 hours, and then drying to obtain a preprocessed honeycomb ceramic filter body;
(2) Preparing aluminum sol; dissolving pseudo-boehmite in deionized water by taking the pseudo-boehmite as an aluminum source and glacial acetic acid as a dispergator, and adding the glacial acetic acid for fully stirring to obtain aluminum sol;
(3) Preparing an active substance: grinding and mixing aluminum oxide powder and cerium oxide powder to obtain mixed oxide powder; proper amount of platinum nitrate Pt (NO) is immersed by an isovolumetric method 3 ) 4 Or chloroplatinic acid H 2 PtCl 6 Loading the mixed oxide powder to obtain a precursor sample; drying the obtained precursor sample at 120 ℃ for 1 hour, and calcining at 500 ℃ for 2 hours to obtain cerium-aluminum mixed oxide loaded with noble metal Pt;
(4) Preparing slurry: adding the cerium-aluminum mixed oxide loaded with the noble metal Pt prepared in the step (3) into the aluminum sol prepared in the step (2), stirring and mixing uniformly, adding deionized water, and aging at room temperature to obtain mixed slurry;
(5) Preparing a monolithic catalyst: the mixed slurry is coated on the surface of the pretreated honeycomb ceramic filter body by adopting a vacuum extraction method or an immersion method, the honeycomb ceramic filter body coated with the mixed slurry is dried at 120 ℃, calcined at 500 ℃ for 2 hours, and the coating, drying and roasting processes are repeated until the coating amount reaches more than 50g/L, thus obtaining the integral catalyst.
The invention further improves that: the honeycomb ceramic filter body in the step (1) has a wall-flow structure, wherein one of cordierite and mullite is a main component of the honeycomb ceramic filter body.
The invention further improves that: the mass of the deionized water added in the step (2) is 10-20 times of the mass of the pseudo-boehmite, and the mass of the glacial acetic acid added is 1-1.5 times of the mass of the pseudo-boehmite.
The invention further improves that: in the step (3), the mass ratio of the alumina powder to the cerium oxide powder is 3:1-5:1, and the loading amount of the noble metal Pt is 0.5-2% of the total mass of the mixed oxide.
The invention further improves that: in the step (4), the mass ratio of the cerium-aluminum mixed oxide loaded with the noble metal Pt to the aluminum sol is 5:1-20:1, the mass of the added deionized water is 5-20 times of the total mass of the cerium-aluminum mixed oxide loaded with the noble metal Pt and the aluminum sol, and the aging time is 6-12 hours.
The beneficial effects of the invention are as follows: the monolithic catalyst prepared by the invention not only has good carbon smoke particle oxidation removal capability, but also can realize CO and HC in tail gas s And NO x Is effective in purifying.
Drawings
FIG. 1 is a schematic cross-sectional view of a tank exhaust gas purifying monolithic catalyst prepared by the present invention.
Detailed Description
The invention is further described below. The following examples are only for more clearly illustrating the technical aspects of the present invention, and are not intended to limit the scope of the present invention.
The invention relates to a preparation method of an integral catalyst for purifying tank tail gas, which comprises a carrier 1, a bonding coating 2 and an active substance 3, wherein the carrier 1 is a pretreated honeycomb ceramic filter body, the bonding coating 2 is an aluminum sol coating, and the active substance 3 is cerium-aluminum mixed oxide loaded with noble metal Pt; the preparation steps of the catalyst are as follows:
(1) Preparing a carrier: placing the honeycomb ceramic filter body in oxalic acid solution with the mass fraction of 5% -15%, heating to 85-95 ℃, preprocessing for 6-24 hours, and then drying to obtain a preprocessed honeycomb ceramic filter body; wherein the honeycomb ceramic filter body has a wall-flow structure, and one of cordierite and mullite is a main component of the honeycomb ceramic filter body:
(2) Preparing aluminum sol; dissolving pseudo-boehmite in deionized water by taking the pseudo-boehmite as an aluminum source and glacial acetic acid as a dispergator, and adding the glacial acetic acid for fully stirring to obtain aluminum sol; wherein the mass of the deionized water is 10-20 times of that of the pseudo-boehmite, and the mass of the glacial acetic acid is 1-1.5 times of that of the pseudo-boehmite;
(3) Preparing an active substance: grinding and mixing aluminum oxide powder and cerium oxide powder to obtain mixed oxide powder; proper amount of platinum nitrate Pt (NO) is immersed by an isovolumetric method 3 ) 4 Or chloroplatinic acid H 2 PtCl 6 Loading the mixed oxide powder to obtain a precursor sample; drying the obtained precursor sample at 120 ℃ for 1 hour, and calcining at 500 ℃ for 2 hours to obtain cerium-aluminum mixed oxide loaded with noble metal Pt; wherein the mass ratio of the alumina powder to the cerium oxide powder is 5:1-3:1, and the noble metal Pt loading amount is 0.5% -2% of the total mass of the mixed oxide;
(4) Preparing slurry: adding the cerium-aluminum mixed oxide loaded with the noble metal Pt prepared in the step (3) into the aluminum sol prepared in the step (2), stirring and mixing uniformly, adding deionized water, and aging for 6 hours at room temperature to obtain mixed slurry; wherein the mass ratio of the cerium-aluminum mixed oxide loaded with the noble metal Pt to the aluminum sol is 20:1-5:1, the mass of the added deionized water is 5-20 times of the total mass of the cerium-aluminum mixed oxide loaded with the noble metal Pt and the aluminum sol, and the aging time is 6-12 hours.
(5) Preparing a monolithic catalyst: the mixed slurry is coated on the surface of the pretreated honeycomb ceramic filter body by adopting a vacuum extraction method or an immersion method, the honeycomb ceramic filter body coated with the mixed slurry is dried at 120 ℃, calcined at 500 ℃ for 2 hours, and the coating, drying and roasting processes are repeated until the coating amount reaches more than 50g/L, thus obtaining the integral catalyst.
Example 1
The invention relates to a preparation method of an integral catalyst for purifying tank tail gas, which comprises a carrier, a bonding coating and an active substance, wherein the carrier is a pretreated honeycomb ceramic filter body, the bonding coating is an aluminum sol coating, and the active substance is cerium-aluminum mixed oxide loaded with noble metal Pt; the preparation steps of the catalyst are as follows:
(1) Preparing a carrier: the honeycomb ceramic filter body is of a wall flow structure, cordierite is used as a main component, the honeycomb ceramic filter body is placed in oxalic acid solution with the mass fraction of 5%, heated to 85 ℃, pretreated for 6 hours, and then dried, so that the pretreated honeycomb ceramic filter body is obtained;
(2) Preparing aluminum sol: dissolving pseudo-boehmite in deionized water by taking the pseudo-boehmite as an aluminum source and glacial acetic acid as a dispergator, and adding the glacial acetic acid for fully stirring to obtain aluminum sol; wherein the mass of the added deionized water is 10 times of that of the pseudo-boehmite, and the mass of the added glacial acetic acid is 1 time of that of the pseudo-boehmite;
(3) Preparing an active substance: grinding and mixing aluminum oxide powder and cerium oxide powder to obtain mixed oxide powder; proper amount of platinum nitrate Pt (NO) is immersed by an isovolumetric method 3 ) 4 Or chloroplatinic acid H 2 PtCl 6 Loading the mixed oxide powder to obtain a precursor sample; drying the obtained precursor sample at 120 ℃ for 1 hour, and calcining at 500 ℃ for 2 hours to obtain cerium-aluminum mixed oxide loaded with noble metal Pt; wherein the mass ratio of the alumina powder to the cerium oxide powder is 5:1, and the loading amount of the noble metal Pt is 0.5% of the total mass of the mixed oxide;
(4) Preparing slurry: adding the cerium-aluminum mixed oxide loaded with the noble metal Pt prepared in the step (3) into the aluminum sol prepared in the step (2), stirring and mixing uniformly, adding deionized water, wherein the mass of the added deionized water is 10 times of the total mass of the cerium-aluminum mixed oxide loaded with the noble metal Pt and the aluminum sol, and aging for 6 hours at room temperature to obtain mixed slurry; wherein, the mass ratio of cerium-aluminum mixed oxide loaded with noble metal Pt to aluminum sol is 20:1;
(5) Preparing a monolithic catalyst: and (3) coating the mixed slurry on the surface of the pretreated honeycomb ceramic filter body by adopting a vacuum extraction method, drying the honeycomb ceramic filter body coated with the mixed slurry at 120 ℃, calcining for 2 hours at 500 ℃, and repeating the coating, drying and calcining processes for 3 times with the coating amount of 52g/L to obtain the monolithic catalyst.
Example 2
The difference from example 1 is that: the main component of the honeycomb ceramic filter body in the preparation step (1) is mullite; the loading amount of the noble metal Pt in the step (3) is 0.75% of the total mass of the mixed oxide; in the step (4), the mass ratio of the cerium-aluminum mixed oxide loaded with the noble metal Pt to the aluminum sol is 15:1, the mass of the added deionized water is 5 times of the total mass of the cerium-aluminum mixed oxide loaded with the noble metal Pt and the aluminum sol, and the room-temperature aging time is 6 hours; and (5) coating the mixed slurry on the surface of the pretreated honeycomb ceramic filter body by adopting a vacuum extraction method, drying the honeycomb ceramic filter body coated with the mixed slurry at 120 ℃, calcining for 2 hours at 500 ℃, and repeating the coating, drying and roasting processes for 3 times, wherein the coating amount is 53g/L.
Example 3
The difference from example 1 is that: step (1), placing the honeycomb ceramic filter body in oxalic acid solution with the mass fraction of 8%, heating to 90 ℃, and pre-treating for 12 hours; the mass of deionized water added in the step (2) is 12 times of that of pseudo-boehmite, and the mass of glacial acetic acid added is 1.2 times of that of the pseudo-boehmite; the loading amount of the noble metal Pt in the step (3) is 1% of the total mass of the mixed oxide; in the step (4), the mass ratio of the cerium-aluminum mixed oxide loaded with the noble metal Pt to the aluminum sol is 12:1, the mass of the added deionized water is 8 times of the total mass of the cerium-aluminum mixed oxide loaded with the noble metal Pt and the aluminum sol, and the room-temperature aging time is 8 hours; and (5) repeating the coating, drying and roasting processes for 3 times by adopting a vacuum extraction method, wherein the coating amount is 55g/L.
Example 4
The difference from example 3 is that: the main component of the honeycomb ceramic filter body in the step (1) is mullite; in the step (3), the mass ratio of the alumina powder to the cerium oxide powder is 4.5:1, and the loading amount of the noble metal Pt is 1.25% of the total mass of the mixed oxide; in the step (4), the mass ratio of the cerium-aluminum mixed oxide loaded with the noble metal Pt to the aluminum sol is 10:1, the mass of the added deionized water is 12 times of the total mass of the cerium-aluminum mixed oxide loaded with the noble metal Pt and the aluminum sol, and the room-temperature aging time is 8 hours; and (5) repeating the coating, drying and roasting processes for 3 times, wherein the coating amount is 58g/L.
Example 5
The difference from example 3 is that: step (1), placing the honeycomb ceramic filter body in oxalic acid solution with the mass fraction of 10%, heating to 90 ℃, and pre-treating for 18 hours; the mass of deionized water added in the step (2) is 15 times of that of pseudo-boehmite, and the mass of glacial acetic acid added is 1.3 times of that of the pseudo-boehmite; in the step (3), the mass ratio of the alumina powder to the cerium oxide powder is 4:1, and the loading amount of the noble metal Pt is 1.5% of the total mass of the mixed oxide; in the step (4), the mass ratio of the cerium-aluminum mixed oxide loaded with the noble metal Pt to the aluminum sol is 8:1, the mass of the added deionized water is 15 times of the total mass of the cerium-aluminum mixed oxide loaded with the noble metal Pt and the aluminum sol, and the room-temperature aging time is 10 hours; the coating amount of the bond coat in the step (5) was 59g/L.
Example 6
The difference from example 5 is that: the main component of the honeycomb ceramic filter body in the step (1) is mullite, the mass of deionized water added in the step (2) is 15 times that of pseudo-boehmite, and the mass of glacial acetic acid added is 1.4 times that of the pseudo-boehmite; in the step (3), the mass ratio of the alumina powder to the cerium oxide powder is 3.5:1, and the loading amount of the noble metal Pt is 1.75% of the total mass of the mixed oxide; in the step (4), the mass ratio of the cerium-aluminum mixed oxide loaded with the noble metal Pt to the aluminum sol is 7:1, the mass of the added deionized water is 18 times of the total mass of the cerium-aluminum mixed oxide loaded with the noble metal Pt and the aluminum sol, and the room-temperature aging time is 10 hours.
Example 7
Compared with the example 6, the main component of the honeycomb ceramic filter body in the step (1) is cordierite, the honeycomb ceramic filter body is placed in oxalic acid solution with the mass fraction of 15%, and is heated to 95 ℃ and is pretreated for 24 hours; the mass of deionized water added in the step (2) is 20 times of that of pseudo-boehmite, and the mass of glacial acetic acid added is 1.5 times of that of the pseudo-boehmite; in the step (3), the mass ratio of the alumina powder to the cerium oxide powder is 3:1, and the loading amount of the noble metal Pt is 2% of the total mass of the mixed oxide; the mass ratio of the cerium-aluminum mixed oxide loaded with the noble metal Pt to the aluminum sol is 5:1, the mass of the added deionized water is 20 times of the total mass of the cerium-aluminum mixed oxide loaded with the noble metal Pt and the aluminum sol, and the room-temperature aging time is 12 hours; the coating amount of the bonding coating in the step (5) is 64g/L.
Simulated tail gas purification test
The prepared integral catalyst is placed on a simulated soot regeneration generator for soot uploading, the loading amount is 10g/L, and the catalyst is used for soot uploading under the condition of simulating tank tail gas (under 10% O) 2 +1000ppmNO+800ppmC 3 H 6 Balance gas N 2 Space velocity of 100000h -1 ) The tail gas purification test was performed with the following results:
exhaust smoke test for real vehicle
The prepared integral catalytic example 7 is packaged and then is arranged on the top of a certain tank vehicle, and according to the requirements of the non-road mobile diesel engine exhaust smoke limit value and measuring method (GB 36886-2018), the actual vehicle exhaust smoke test is carried out, and the result is as follows:
the foregoing is merely a preferred embodiment of the present invention, and it should be noted that modifications and variations could be made by those skilled in the art without departing from the technical principles of the present invention, and such modifications and variations should also be regarded as being within the scope of the invention.
Claims (1)
1. A preparation method of an integral catalyst for purifying tank tail gas is characterized by comprising the following steps of: the catalyst comprises a carrier, a bonding coating and an active substance, wherein the carrier is a pretreated honeycomb ceramic filter body, and the main component of the honeycomb ceramic filter body is cordierite; the bonding coating is an aluminum sol coating, and the active substance is cerium-aluminum mixed oxide loaded with noble metal Pt; the preparation steps of the catalyst are as follows:
(1) Preparing a carrier: placing the honeycomb ceramic filter body in oxalic acid solution with the mass fraction of 15%, heating to 95 ℃, pre-treating for 24 hours, and then drying to obtain a pretreated honeycomb ceramic filter body;
(2) Preparing aluminum sol; dissolving pseudo-boehmite in deionized water by taking the pseudo-boehmite as an aluminum source and glacial acetic acid as a dispergator, and adding the glacial acetic acid for fully stirring to obtain aluminum sol;
(3) Preparing an active substance: grinding and mixing aluminum oxide powder and cerium oxide powder to obtain mixed oxide powder; platinum nitrate Pt (NO) by adopting an isovolumetric impregnation method 3 ) 4 Or chloroplatinic acid H 2 PtCl 6 Loading the mixed oxide powder to obtain a precursor sample; drying the obtained precursor sample at 120 ℃ for 1 hour, and calcining at 500 ℃ for 2 hours to obtain cerium-aluminum mixed oxide loaded with noble metal Pt;
(4) Preparing slurry: adding the cerium-aluminum mixed oxide loaded with the noble metal Pt prepared in the step (3) into the aluminum sol prepared in the step (2), stirring and mixing uniformly, adding deionized water, and aging at room temperature to obtain mixed slurry;
(5) Preparing a monolithic catalyst: coating the mixed slurry on the surface of the pretreated honeycomb ceramic filter body by adopting a vacuum extraction method or an immersion method, drying the honeycomb ceramic filter body coated with the mixed slurry at 120 ℃, calcining for 2 hours at 500 ℃, and repeating the coating, drying and roasting processes until the coating amount reaches 64g/L to obtain the integral catalyst;
the mass of deionized water added in the step (2) is 20 times of that of pseudo-boehmite, and the mass of glacial acetic acid added is 1.5 times of that of the pseudo-boehmite;
the mass ratio of the alumina powder to the cerium oxide powder in the step (3) is 3:1, and the noble metal Pt loading amount is 2% of the total mass of the mixed oxide;
in the step (4), the mass ratio of the cerium-aluminum mixed oxide loaded with the noble metal Pt to the aluminum sol is 5:1, the mass of the added deionized water is 20 times of the total mass of the cerium-aluminum mixed oxide loaded with the noble metal Pt and the aluminum sol, and the aging time is 12 hours.
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