CN116044544A - Method for preparing integral cDPF for filtering soot particles in vehicle tail gas and integral cDPF - Google Patents
Method for preparing integral cDPF for filtering soot particles in vehicle tail gas and integral cDPF Download PDFInfo
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- CN116044544A CN116044544A CN202211580207.1A CN202211580207A CN116044544A CN 116044544 A CN116044544 A CN 116044544A CN 202211580207 A CN202211580207 A CN 202211580207A CN 116044544 A CN116044544 A CN 116044544A
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- cdpf
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- nitrate
- impregnating solution
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- 239000002245 particle Substances 0.000 title claims abstract description 59
- 239000004071 soot Substances 0.000 title claims abstract description 56
- 238000001914 filtration Methods 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000000243 solution Substances 0.000 claims abstract description 68
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 52
- 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 abstract description 45
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 43
- 238000002360 preparation method Methods 0.000 claims abstract description 40
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 37
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000919 ceramic Substances 0.000 claims abstract description 25
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 25
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 24
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 23
- 239000011664 nicotinic acid Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000005470 impregnation Methods 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 12
- 239000012153 distilled water Substances 0.000 claims abstract description 9
- 238000007710 freezing Methods 0.000 claims abstract description 9
- 230000008014 freezing Effects 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003980 solgel method Methods 0.000 claims abstract description 5
- 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 claims description 19
- 239000007788 liquid Substances 0.000 claims description 15
- 239000000126 substance Substances 0.000 claims description 15
- 229910052863 mullite Inorganic materials 0.000 claims description 13
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- 239000006104 solid solution Substances 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims description 4
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 235000010333 potassium nitrate Nutrition 0.000 claims description 4
- 239000004323 potassium nitrate Substances 0.000 claims description 4
- 210000002345 respiratory system Anatomy 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims 4
- 238000002485 combustion reaction Methods 0.000 abstract description 8
- 238000011069 regeneration method Methods 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- 238000007598 dipping method Methods 0.000 abstract description 7
- 230000008929 regeneration Effects 0.000 abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052593 corundum Inorganic materials 0.000 abstract description 5
- 239000010431 corundum Substances 0.000 abstract description 5
- 239000000779 smoke Substances 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 26
- 230000003197 catalytic effect Effects 0.000 description 15
- 239000003054 catalyst Substances 0.000 description 14
- 239000006229 carbon black Substances 0.000 description 12
- 239000012071 phase Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- 238000013112 stability test Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000001947 vapour-phase growth Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 210000004081 cilia Anatomy 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 230000008646 thermal stress Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- RCFVMJKOEJFGTM-UHFFFAOYSA-N cerium zirconium Chemical compound [Zr].[Ce] RCFVMJKOEJFGTM-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 210000002615 epidermis Anatomy 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910004625 Ce—Zr Inorganic materials 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003592 biomimetic effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000007676 flexural strength test Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 235000001968 nicotinic acid Nutrition 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Images
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
- F01N3/022—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N13/00—Exhaust or silencing apparatus characterised by constructional features ; Exhaust or silencing apparatus, or parts thereof, having pertinent characteristics not provided for in, or of interest apart from, groups F01N1/00 - F01N5/00, F01N9/00, F01N11/00
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
- F01N3/023—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters using means for regenerating the filters, e.g. by burning trapped particles
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
- F01N3/023—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters using means for regenerating the filters, e.g. by burning trapped particles
- F01N3/0232—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters using means for regenerating the filters, e.g. by burning trapped particles removing incombustible material from a particle filter, e.g. ash
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
- F01N3/033—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices
- F01N3/035—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices with catalytic reactors, e.g. catalysed diesel particulate filters
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/18—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control
- F01N3/20—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control specially adapted for catalytic conversion ; Methods of operation or control of catalytic converters
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
- F01N3/2803—Construction of catalytic reactors characterised by structure, by material or by manufacturing of catalyst support
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
- F01N3/2803—Construction of catalytic reactors characterised by structure, by material or by manufacturing of catalyst support
- F01N3/2825—Ceramics
- F01N3/2828—Ceramic multi-channel monoliths, e.g. honeycombs
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Materials Engineering (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention discloses a preparation method of an integral cDPF for filtering soot particles in vehicle tail gas and the integral cDPF. The preparation method is characterized in that the integral cDPF is prepared by a gas phase growth method, a sol-gel method and an impregnation method, and the integral cDPF has a bionic structure. The preparation method comprises the following steps: preparing silica sol impregnating solution, aluminum nitrate impregnating solution and ammonium fluoride impregnating solution according to a proportion; sequentially dipping, freezing and drying cordierite honeycomb ceramics; placing cordierite honeycomb ceramics in a corundum crucible, and placing the corundum crucible in a muffle furnace for heating and maintaining; weighing cobalt nitrate, cerium nitrate and zirconium nitrate, then adding citric acid and distilled water to prepare a mixed solution, vacuumizing, standing and drying the cordierite with the surface modified; the sample is placed in a muffle furnace to be heated and baked. The integral cDPF can greatly improve the trapping performance of the carbon smoke particles, and can reduce the ignition temperature and the maximum combustion temperature of the carbon smoke particles at the same time, thereby realizing good regeneration of the DPF.
Description
Technical Field
The invention relates to the technical field of diesel vehicle tail gas treatment, in particular to a preparation method of an integral cDPF for filtering soot particles in vehicle tail gas and the integral cDPF.
Background
Generally, a Diesel Particulate Filter (DPF) is a wall-flow type honeycomb ceramic material having a cylindrical structure formed by extrusion, and is composed of hundreds of small wall-flow type parallel channels along the height direction of the cylindrical structure. The wall-flow channels are made from ceramic sintered with a controlled higher, more precise porosity, with numerous pores in the wall having a pore size of a few microns. Adjacent channels in the wall-flow ceramic honeycomb filter are alternately plugged at both ends as a filter medium, forcing the gasoline and diesel exhaust to flow through the porous structure of the wall-flow ceramic. Soot particles that are too large to pass through the porous surface may be physically collected and accumulated in the channels. The DPF wall flow channels are designed to have optimal porosity, enable exhaust gas to pass through the channel walls without significant obstruction, and have good selectivity for trapping particulate matter.
A key component of diesel filtration systems is the DPF, and the substrate material of the DPF affects its performance and durability. Advances in material science have also prompted the development of substrate materials for DPFs. In general, DPF substrate materials are characterized by higher filtration efficiency, lower pressure drop, good high temperature resistance, low thermal expansion rate, thermal stress resistance, and chemical resistance to ash (e.g., sulfate, etc.) contained in exhaust particulates.
It must be emphasized that depending on the regeneration method, the diesel particulate trap may be exposed to very high temperatures, even in excess of 1000 ℃, and rapid temperature changes. These conditions are mainly caused by the heat released by the soot particles accumulated in the filter during the rapid oxidation. Thermal stresses tend to have localized characteristics because the distribution of soot particles throughout the filter is not necessarily uniform. Both high temperature and thermal stresses are the main causes of filter damage, failure, such as melting or cracking. Therefore, the accumulated soot particles are timely catalytically combusted and discharged, and the method has great significance on the service life of the DPF.
All DPFs are intended to capture and contain a certain amount of soot particles. When too many soot particles are trapped, they can cause obstruction to the flow of gas and ultimately result in too high a pressure drop of the exhaust gas through the DPF, which can not only result in insufficient combustion to cause the filter itself to become plugged more severely, but can also negatively impact the operation of the engine.
Therefore, it is necessary to provide a reliable method for a motor vehicle exhaust system to remove the soot particles accumulated in the DPF to restore its soot trapping capability and ensure trouble-free operation.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention provides a preparation method of an integral cDPF for filtering soot particles in vehicle tail gas and the integral cDPF, and overcomes the defects that the existing vehicle DPF is difficult to regenerate and soot particle pollutants are difficult to effectively remove.
In particular, the vehicle exhaust gas may be a gasoline vehicle exhaust gas or a diesel vehicle exhaust gas. The monolithic cDPF has a biomimetic structure.
The removal of the soot, the so-called combustion soot regeneration of the filter, may be carried out continuously during normal operation of the DPF (passive regeneration) or after reaching a predetermined soot accumulation amount (active regeneration). By loading a proper catalyst to continuously catalyze the combustion of soot particles, the method is a form of passive regeneration, and the research emphasis and breakthrough point of DPF regeneration are realized by searching for a high-performance catalyst and reducing the combustion temperature of carbon particles to eliminate the carbon particles in the exhaust gas of a diesel engine.
In order to achieve the above purpose, the invention adopts the following technical scheme:
according to one aspect of the present invention, there is provided a method for preparing an integral cDPF for soot particle filtration in vehicle exhaust, the raw materials used in the preparation method including aluminum nitrate, ethyl orthosilicate, potassium nitrate, cobalt nitrate, cerium nitrate and zirconium nitrate, the preparation method preparing an integral cDPF for soot particle filtration in vehicle exhaust by a vapor phase growth method, a sol gel method and an impregnation method, the integral cDPF having a bionic structure;
wherein the preparation method comprises the following steps:
step one, preparing a silica sol impregnating solution, an aluminum nitrate impregnating solution and an ammonium fluoride impregnating solution according to a proportion, wherein the preparation method of the silica sol impregnating solution comprises the following steps: measuring absolute ethyl alcohol in a first container, measuring ethyl orthosilicate, adding distilled water into the container, putting the container into a magnetic stirrer for continuous stirring, dripping 2-3 drops of ammonia water to catalyze the hydrolysis of the ethyl orthosilicate, and stirring overnight to prepare silica sol; the preparation method of the aluminum nitrate impregnating solution comprises the steps of weighing aluminum nitrate to prepare an aluminum nitrate impregnating solution; the preparation method of the ammonium fluoride impregnating solution comprises the steps of weighing ammonium fluoride to prepare an ammonium fluoride solution;
step two, sequentially soaking, freezing and drying the cordierite honeycomb ceramic in the silica sol soaking liquid, the aluminum nitrate soaking liquid and the ammonium fluoride soaking liquid which are obtained in the step one;
step three, placing the cordierite honeycomb ceramic obtained in the step two into a muffle furnace, heating and maintaining, wherein the silica sol impregnating solution, the aluminum nitrate impregnating solution and the ammonium fluoride impregnating solution generate gas-phase atmosphere under the high-temperature condition, and continuously depositing atoms or molecules in the gas phase on a crystallization interface to realize mullite whisker growth;
weighing cobalt nitrate, cerium nitrate and zirconium nitrate, and then adding citric acid and distilled water to prepare a mixed solution;
step five, placing the mixed solution in a second container, placing the cordierite with the surface modified obtained in the step three in the second container, ensuring that the solution is over the sample, transferring the second container into a vacuum drying dish, vacuumizing, standing, taking out the sample, drying in an oven, and repeating the process once;
and step six, placing the sample obtained in the step five into a muffle furnace, heating and roasting to obtain the integral cDPF.
In some embodiments, the monolithic cDPF prepared by the preparation method is cordierite-mullite-cerium-zirconium solid solution composite oxide, and the monolithic cDPF has a bionic structure similar to the structure of human respiratory system and bronchial epithelial cilium cells.
In some embodiments, the concentration ratio of the silica sol impregnating solution, the aluminum nitrate impregnating solution and the ammonium fluoride impregnating solution is 1:2:9, and the concentration of the aluminum nitrate impregnating solution is 1.98 mol.L -1 。
In some embodiments, the freezing temperature in step two is-6 ℃, the drying temperature in step two is 50-80 ℃, and the drying temperature in step two is 55 ℃.
In some embodiments, in the second and third steps, cordierite honeycomb ceramics are respectively immersed in silica sol impregnating solution, aluminum nitrate impregnating solution and ammonium fluoride impregnating solution for 6 hours, then frozen for 6 hours, finally dried at 90 ℃, placed in a muffle furnace and baked at 120 ℃ for 12 hours, the impregnating solution generates gas-phase atmosphere under high temperature condition, and the mullite whisker growth is realized by utilizing the continuous deposition of atoms or molecules in the gas phase on a crystallization interface.
In some embodiments, the temperature is raised and maintained in step three to 1000 ℃ at a temperature rise rate of 2 ℃/min for 2 hours; the first container of the first step and the second container of the fifth step are beakers.
In some embodiments, the molar ratio of cobalt nitrate, cerium nitrate, zirconium nitrate is 21:4:4, 3:1:1, 2:1:1, 1:1:1, 21:3:3, 21:2:2, or 21:1:1, the warm firing in step six is firing at a warm rate of 2 ℃/min to 600 ℃ for 2 hours;
the amount of the substance added with the citric acid is the sum of the amount of the substance of cobalt nitrate 2 times, the amount of the substance of cerium nitrate 3 times and the amount of the substance of zirconium nitrate 4 times.
In some embodiments, the rest time after evacuation in step five is 10-30min and the drying temperature in step five is 100-175 ℃.
In some embodiments, the post-evacuation rest time in step five is 15min and the drying temperature in step five is 110 ℃.
According to another aspect of the present invention there is provided a monolithic cDPF for soot particulate filtration in vehicle exhaust gas, said monolithic cDPF being prepared by the aforementioned preparation method.
Compared with the prior art, the invention has the beneficial technical effects that:
the integral cDPF prepared by the preparation method is a brand new integral cDPF, mullite whiskers are grown on the surface of the DPF by a gas phase growth method by utilizing a bionics idea, and the integral cDPF with a bionical structure similar to that of a human respiratory system and a bronchial upper epidermis cilium cell structure is constructed by benefiting from the inspiration of the human respiratory system and the bronchial upper epidermis cilium cell structure. Preparing mullite whiskers on the surface of the wall-flow cordierite honeycomb ceramic by using a vapor phase growth method so as to play a role in efficient filtration; loading a high-efficiency cerium-zirconium solid solution catalyst on the surface of the whisker by using an impregnation method so as to achieve a self-cleaning function; thereby constructing an integral cDPF with bionic structure and performance.
At present, the invention utilizes the four raw materials to prepare the integral cDPF by a three-step method for filtering and catalyzing soot particles in the tail gas of the diesel vehicle. And the integral cDPF has excellent catalytic performance and great application value. Through experimental tests, the integrated cDPF can greatly filter soot particles in the automobile exhaust, and can realize the regeneration of the cDPF at the normal temperature of the automobile exhaust emission, namely, the filtered exhaust is catalyzed.
Drawings
These and/or other aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the preferred embodiments, taken in conjunction with the accompanying drawings, in which:
FIG. 1 is an XRD pattern of an as-received, modified mullite whisker/cordierite sample of the monolithic cDPFs of examples 1 and 2 of the present invention;
FIG. 2 is a graph of the catalytic performance test of soot particles for monolithic cDPFs of examples 1 and 2 and for as-received, modified mullite whisker/cordierite samples of the present invention;
FIG. 3 is a graph of the cycle stable catalytic performance test of the monolithic cDPF of example 2 of the present invention.
Detailed Description
The technical scheme of the invention is further specifically described below through examples and with reference to the accompanying drawings. In the specification, the same or similar reference numerals denote the same or similar components. The following description of embodiments of the present invention with reference to the accompanying drawings is intended to illustrate the general inventive concept and should not be taken as limiting the invention.
The embodiment of the invention provides a preparation method of an integral cDPF for filtering soot particles in vehicle tail gas.
The integral cDPF prepared by the preparation method is a cordierite-mullite-cerium zirconium solid solution composite oxide. The cDPF has good catalytic performance on soot particles in vehicle tail gas such as diesel vehicles or gasoline vehicles, can effectively reduce the ignition temperature of the soot particles, and has good application in the trapping work of the soot particles in the diesel vehicles and the automobile tail gas.
In one embodiment of the invention, a method for preparing an integral cDPF with a bionic structure for soot particle filtration in vehicle exhaust is provided. The preparation method comprises the following raw materials of aluminum nitrate, tetraethoxysilane, ammonium fluoride, potassium nitrate, cobalt nitrate, cerium nitrate and zirconium nitrate with preset amounts, and the integral cDPF with a bionic structure for filtering soot particles in the tail gas of the vehicle is prepared through three steps of a vapor phase growth method, a sol-gel method and an impregnation method.
The preparation method comprises the following steps:
step one, preparing silica sol impregnating solution, aluminum nitrate impregnating solution and ammonium fluoride impregnating solution according to a certain concentration proportion. The preparation method of the silica sol impregnating solution comprises the following steps: measuring a certain amount of absolute ethyl alcohol in a first container (such as a beaker), measuring a certain amount of ethyl orthosilicate, adding a proper amount of distilled water into the first container, putting the first container into a magnetic stirrer for continuous stirring, dropwise adding 2-3 drops of ammonia water to catalyze the hydrolysis of the ethyl orthosilicate, and stirring overnight to prepare silica sol; preparing an aluminum nitrate dipping solution; the preparation method of the aluminum nitrate impregnating solution comprises the following steps of; a certain amount of aluminum nitrate is weighed to prepare an aluminum nitrate impregnating solution (for example, the concentration is 1.98 mol.L) -1 ) The method comprises the steps of carrying out a first treatment on the surface of the The preparation method of the ammonium fluoride impregnating solution comprises the following steps: weighing a certain amount of ammonium fluoride to prepare an ammonium fluoride solution.
And step two, sequentially soaking the cordierite honeycomb ceramic in the soaking liquid obtained in the step one, freezing and drying.
And thirdly, placing the cordierite honeycomb ceramic package obtained in the step two (for example, in a corundum crucible) into a muffle furnace (for example, at the heating rate of 2 ℃/min), heating to a certain temperature and maintaining for a certain time (for example, heating to 1000 ℃ for 2 hours (h)).
And step four, weighing cobalt nitrate, cerium nitrate and zirconium nitrate, and then adding citric acid and distilled water to prepare a mixed solution.
And fifthly, placing the mixed solution into a second container (such as a beaker with proper size), placing the cordierite with the modified surface obtained in the third step into the second container, ensuring that the solution is over the sample, transferring the container into a vacuum drying device (such as a vacuum drying dish), vacuumizing, standing for a period of time, taking out the sample, drying in a baking device (such as an oven), and repeating the process once.
And step six, placing the sample obtained in the step five into a muffle furnace (for example, at a heating rate of 2 ℃/min) to a preset temperature, and roasting for a preset time (for example, roasting for 2 hours at 600 ℃) to obtain the integral cDPF.
In some embodiments, the silica sol impregnation fluid, aluminum nitrate impregnation fluid, ammonium fluoride impregnation fluid concentration ratio is 1:2:9.
In some embodiments, the molar ratio of cobalt nitrate, cerium nitrate, zirconium nitrate is: 21:4:4, 3:1:1, 2:1:1, 1:1:1, 21:3:3, 21:2:2, or 21:1:1.
The preferred molar ratios of cobalt nitrate, cerium nitrate and zirconium nitrate are: 21:4:4.
The drying temperature in the second step is 50-80 ℃, preferably 55 ℃.
The rest time after the vacuumizing in the fifth step is 10-30 minutes (min), and preferably, the rest time after the vacuumizing in the fifth step is 15min.
The drying temperature in the fifth step is 100-175 ℃, preferably the drying temperature in the fifth step is 110 ℃.
In the second step and the third step, cordierite honeycomb ceramics are respectively immersed in silica sol impregnating solution, aluminum nitrate impregnating solution and ammonium fluoride impregnating solution for 6 hours, then freezing treatment is carried out for 6 hours, finally drying is carried out at 90 ℃, then the materials are put into a muffle furnace for roasting at 120 ℃ for 12 hours, the impregnating solution generates gas-phase atmosphere at the high temperature of 120 ℃, and the growth of mullite whiskers is realized by utilizing the continuous deposition of atoms or molecules in the gas phase on a crystallization interface.
The embodiment of the invention also provides an integral cPDF for filtering soot particles in vehicle exhaust. The monolithic cppdf was prepared according to the preparation method of the above examples.
Example 1:
the embodiment provides a preparation method of an integral cDPF with a bionic structure for filtering soot particles in vehicle tail gas, which comprises the following steps of preparing the integral cDPF with the bionic structure for filtering soot particles in the diesel vehicle tail gas by a gas phase growth method and a sol-gel method, wherein the raw materials of the integral cDPF comprise aluminum nitrate, ethyl orthosilicate, ammonium fluoride, potassium nitrate, cobalt nitrate, cerium nitrate and zirconium nitrate. The method comprises the following steps:
step one, preparing a silica sol impregnating solution, an aluminum nitrate impregnating solution and an ammonium fluoride impregnating solution according to the concentration ratio of 1:2:9. The preparation method of the silica sol impregnating solution comprises the following steps: measuring a certain amount of absolute ethyl alcohol in a beaker, measuring a certain amount of ethyl orthosilicate, adding a proper amount of distilled water in the beaker, putting the beaker into a magnetic stirrer for continuous stirring, dropwise adding 2-3 drops of ammonia water to catalyze the hydrolysis of the ethyl orthosilicate, and stirring overnight to prepare silica sol; preparing an aluminum nitrate dipping solution; the preparation method of the aluminum nitrate impregnating solution comprises the following steps: weighing a certain amount of aluminum nitrate to prepare an aluminum nitrate impregnating solution (the concentration is 1.98 mol.L) -1 ) The method comprises the steps of carrying out a first treatment on the surface of the The preparation method of the ammonium fluoride impregnating solution comprises the following steps: weighing a certain amount of ammonium fluoride to prepare an ammonium fluoride solution.
And step two, sequentially soaking the cordierite honeycomb ceramic in the soaking liquid obtained in the step one, freezing and drying. The dipping sequence in the second step is silica sol dipping solution, aluminum nitrate dipping solution and ammonium fluoride dipping solution. The freezing time was 30 minutes and the drying conditions were 55℃for 15 hours.
And thirdly, placing the cordierite honeycomb ceramic obtained in the second step in a corundum crucible, and placing the corundum crucible into a muffle furnace, wherein the temperature rising rate of the muffle furnace is 2 ℃/min, and the temperature is raised to 1000 ℃ and kept for 2 hours, so that the surface-modified cordierite ceramic can be obtained.
And step four, weighing cobalt nitrate, cerium nitrate and zirconium nitrate, then adding citric acid and distilled water to prepare a mixed solution, wherein the molar ratio of the cobalt nitrate to the cerium nitrate to the zirconium nitrate in the step four is 21:4:4, and the amount of substances added by the citric acid is the sum of the amount of cobalt nitrate substances, the amount of cerium nitrate substances and the amount of cerium nitrate substances which are 2 times, the amount of cerium nitrate substances which are 3 times and the amount of cerium nitrate substances which are 4 times.
And fifthly, placing the mixed solution into a beaker with proper size, placing the cordierite with the surface modified obtained in the step three into the beaker, ensuring that the solution is over the sample, transferring the beaker into a vacuum drying dish, vacuumizing, standing for a period of time, taking out the sample, drying in an oven, and repeating the process once. And step five, vacuumizing and standing for 15 minutes, and drying at 110 ℃ for 15 hours.
And step six, placing the sample obtained in the step five into a muffle furnace for heating to obtain the integral cDPF. And step six, heating the muffle furnace to a temperature of 600 ℃ at a heating rate of 2 ℃/min for 2 hours.
Example 2:
the embodiment provides a preparation method of an integral cDPF with a bionic structure for filtering soot particles in vehicle exhaust, and the embodiment is different from the embodiment 1 in that the molar ratio of cobalt nitrate, cerium nitrate and zirconium nitrate is 3:1:1.
Example 3:
the embodiment provides a preparation method of an integral cDPF with a bionic structure for filtering soot particles in vehicle exhaust, and the embodiment is different from the embodiment 1 in that the molar ratio of cobalt nitrate, cerium nitrate and zirconium nitrate is 2:1:1.
Example 4:
the embodiment provides a preparation method of an integral cDPF with a bionic structure for filtering soot particles in vehicle exhaust, and the embodiment is different from the embodiment 1 in that the molar ratio of cobalt nitrate, cerium nitrate and zirconium nitrate is 1:1:1.
Example 5:
the embodiment provides a preparation method of an integral cDPF with a bionic structure for filtering soot particles in vehicle exhaust, and the embodiment is different from the embodiment 1 in that the molar ratio of cobalt nitrate, cerium nitrate and zirconium nitrate is 21:3:3.
Example 6:
the embodiment provides a preparation method of an integral cDPF with a bionic structure for filtering soot particles in vehicle exhaust, and the embodiment is different from the embodiment 1 in that the molar ratio of cobalt nitrate, cerium nitrate and zirconium nitrate is 21:2:2.
Example 7:
the embodiment provides a preparation method of an integral cDPF with a bionic structure for filtering soot particles in vehicle exhaust, and the embodiment is different from the embodiment 1 in that the molar ratio of cobalt nitrate, cerium nitrate and zirconium nitrate is 21:1:1.
The vapor phase growth mullite whisker of the invention comprises the following steps: the cordierite honeycomb ceramic is respectively immersed in a silica sol impregnating solution, an aluminum nitrate impregnating solution and an ammonium fluoride impregnating solution for 6 hours, then frozen for 6 hours, finally dried at 90 ℃, placed in a muffle furnace and baked at 120 ℃ for 12 hours, the impregnating solution generates a gas-phase atmosphere under a high-temperature condition, and atoms or molecules in the gas-phase are continuously deposited on a crystallization interface to realize mullite whisker growth.
XRD test
Fig. 1 is an XRD pattern of the cDPF and cordierite as-received, modified mullite whisker/cordierite samples of examples 1 and 2 of the present invention. As can be seen from fig. 1, the prepared cDPF has better crystallinity, and diffraction peaks at 10.460 °, 18.052 °, 18.988 °, 21.711 °, 26.338 °, 28.475 °, 29.405 ° and 33.875 ° are characteristic diffraction peaks of cordierite; diffraction peaks at 16.432 °, 26.267 °, 30.960 °, 35.278 °, 40.874 ° are characteristic diffraction peaks of mullite; at 29.878 °, 49.606 °, 58.506 ° (Zr) 0.84 Ce 0.16 O 2 ) And 28.870 °, 48.049 °, 57.012 °, 70.357 ° (Ce 0.75 Zr 0.15 O 2 ) The diffraction peak of (2) is a characteristic diffraction peak of cerium-zirconium solid solution; co (Co) 3 O 4 Characteristic diffraction peaks of (2) can be observed at 31.271 °, 36.852 ° and 44.808 °.
(II) flexural Strength test
Table 1 shows the flexural strength of the cDPF and cordierite as received and modified mullite whisker/cordierite samples of examples 1 and 2. As can be seen from table 1, the wall-flow cordierite honeycomb ceramics modified by the vapor-phase growth method did not significantly change the flexural strength as compared with the original samples, and the vapor-phase growth method did not cause structural damage to the wall-flow cordierite honeycomb ceramics, resulting in lower flexural strength of the samples. It can also be seen that the flexural strength of the catalyst loaded samples by impregnation was 10.18MPa and 10.17MPa, respectively, with only a slight drop of 0.39% to 0.49% compared to wall-flow cordierite honeycomb ceramics and surface-modified cordierite, and still be within acceptable limits.
TABLE 1 flexural Strength of samples
(III) test of Capture Performance for soot
Table 2 shows the filtration performance of the cdfs of examples 1 and 2, as-received, modified mullite whisker/cordierite samples. As can be seen from Table 2, the original cordierite delta M value before modification is 0.0115g, the blocking effect of the modified sample on carbon black particles is obviously improved, and the M/C of the sample is improved by 82.6%. Whereas the two samples with coated catalyst had only a slight increase in filtration efficiency compared to the M/C sample with uncoated catalyst, example 1 increased the filtration efficiency by 97.4% as compared to the wall flow cordierite honeycomb ceramic, and example 2 increased the filtration efficiency by a factor of 100.1% compared to the wall flow cordierite honeycomb ceramic sample. Sample M/C was improved to a different extent from that of example 2 in example 1.
TABLE 2 cordierite honeycomb ceramics and monolithic cDPF sample filtration performance
* Filtration efficiency: finger means: (sample. DELTA.M/cordierite. DELTA.M-1) by 100%.
(IV) test of catalytic Performance on soot particles
FIG. 2 shows the cDPF of example 1 and example 2 and a modified mullite whisker/cordierite sample vs. carbon as receivedCatalytic performance test chart of smoke. The test uses simulated exhaust conditions similar to DOCs (diesel oxidation catalyst) test conditions as the experimental gas in the experiment. Analysis of FIG. 2 shows that the initial firing temperature of the carbon black particles reaches a maximum CO in the untreated cordierite as it is at about 200.5C 2 The concentration temperature was 478.5 ℃, and the curve tended to be 0 after 600 ℃. The curve of the sample of mullite whisker grown by modifying the cordierite surface shows that the soot particles start to ignite at 154.9 c and the maximum CO is detected at 305.8 c 2 Concentration of CO 2 The concentration tends to be 0. The result is superior to the known one because the presence of whiskers during loading of the soot particles partially intercepts the soot particles during their passage through parallel channels and holes, and the soot particles are dispersed throughout the process so as to be in sufficient contact with the oxygen and heat in the exhaust gas, thus the light-off temperature and the maximum CO 2 The concentration temperature is reduced. In cordierite, carbon black particles are finally gathered together to form large particles, and the carbon in the cordierite cannot be fully contacted with oxygen, so that the carbon black cannot be fully heat-exchanged, and the maximum CO is achieved 2 Is higher.
For examples 1 and 2, the light-off temperature of the carbon black particles was significantly reduced. For sample example 1, the carbon black particles had a light-off temperature of 124.9℃and a maximum CO 2 The concentration temperature was 328.9 ℃. For sample example 2, there was good catalytic performance. It can be seen that a small portion of CO can be detected at a temperature of around 60℃ 2 With increasing temperature, CO 2 The concentration continues to rise and peaks at 236.7 ℃ and then tends to be 0. Notably, the two curves of example 1 and example 2 are in the range of 450-600 ℃, CO 2 There is a small increase in concentration, and it is presumed that this portion should be CO released by combustion of the carbon black particles accumulated in the bottom 2 . Thus, by calculating two COs 2 The percentage of peak area can be used to obtain the catalytic efficiency of the catalyst, i.e. the percentage of carbon black particles that the catalyst can catalyze and oxidize in the exhaust temperature range. As shown in the figure, the left side of the division point of the catalytic efficiency is calculatedThe percentage of the curve area was calculated to be that example 2 was able to catalyze about 86.23% of the carbon black particles under exhaust conditions, while example 1 was able to catalyze about 87.04% of the carbon black particles.
The data for the combustion of the catalytic carbon black particles in this test (O 2 Concentration, light-off temperature (T) i ) Maximum CO 2 Concentration temperature (T) max ) Etc.). In simulating the exhaust conditions (O) 2 10%) of the materials in example 2 had the lowest light-off temperature of 55.8deg.C and the lowest maximum combustion efficiency temperature, T max At 236.7℃the catalytic efficiency of sample example 2 was 86.23%. In the research, experimental test results prove that the embodiment 1 and the embodiment 2 have good performance and application prospect.
TABLE 3 catalytic performance of monolithic cDPF samples on soot particles
Example 2 has excellent catalytic performance as compared with example 1. With reference to the commercial cDPF, noble metals such as Pt, pd, etc. are used as the coating layer of the catalyst, and the equilibrium temperature is 320 ℃, which is not only expensive, costly to use, but also higher than that of example 2 measured in the laboratory. The monolithic cDPF coated with the cobalt-doped Ce-Zr solid solution catalyst on mullite whisker/cordierite has better catalytic effect than other catalysts, and has wide application prospect due to the high-efficiency and economical characteristics.
(V) catalytic stability test of sample
FIG. 3 is a graph of the cycle stability test of example 2, and it can be seen from FIG. 3 that T is the first cycle stability test i (55.8 ℃ C.) and T max (236.7 ℃) is lower than several subsequent cycle tests. A reasonable explanation is that mullite whisker/cordierite is coated by impregnationThe fresh catalyst Co/CZ has more adsorbed oxygen on the surface, and the adsorbed oxygen has stronger low-temperature oxidation activity, so that the active sites can accelerate the catalytic combustion of carbon black particles at lower temperature. However, after the first cycle stability test, the surface adsorption oxygen sites are consumed and the catalyst is stabilized, so that T is from the start of the second cycle stability test to the end of the fifth cycle stability test i And T max The value of (2) tends to be almost stable. The experiment of the cycle stability test proves that the integral cDPF prepared in the embodiment 2 has good structural stability and catalytic performance stability, and has important application value in the field of integral cDPF.
The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner without contradiction. The various possible combinations of the invention are not described in detail in order to avoid unnecessary repetition.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Although a few embodiments of the present general inventive concept have been shown and described, it would be appreciated by those skilled in the art that changes may be made in these embodiments without departing from the principles and spirit of the general inventive concept, the scope of which is defined in the claims and their equivalents.
Claims (10)
1. The preparation method is characterized in that raw materials used in the preparation method comprise aluminum nitrate, ethyl orthosilicate, potassium nitrate, cobalt nitrate, cerium nitrate and zirconium nitrate, and the preparation method is used for preparing the integral cDPF for filtering the soot particles in the vehicle tail gas through a gas phase growth method, a sol-gel method and an impregnation method, and the integral cDPF has a bionic structure;
wherein the preparation method comprises the following steps:
step one, preparing a silica sol impregnating solution, an aluminum nitrate impregnating solution and an ammonium fluoride impregnating solution according to a proportion, wherein the preparation method of the silica sol impregnating solution comprises the following steps: measuring absolute ethyl alcohol in a first container, measuring ethyl orthosilicate, adding distilled water into the container, putting the container into a magnetic stirrer for continuous stirring, dripping 2-3 drops of ammonia water to catalyze the hydrolysis of the ethyl orthosilicate, and stirring overnight to prepare silica sol; the preparation method of the aluminum nitrate impregnating solution comprises the steps of weighing aluminum nitrate to prepare an aluminum nitrate impregnating solution; the preparation method of the ammonium fluoride impregnating solution comprises the steps of weighing ammonium fluoride to prepare an ammonium fluoride solution;
step two, sequentially soaking, freezing and drying the cordierite honeycomb ceramic in the silica sol soaking liquid, the aluminum nitrate soaking liquid and the ammonium fluoride soaking liquid which are obtained in the step one;
step three, placing the cordierite honeycomb ceramic obtained in the step two into a muffle furnace, heating and maintaining, wherein the silica sol impregnating solution, the aluminum nitrate impregnating solution and the ammonium fluoride impregnating solution generate gas-phase atmosphere under the high-temperature condition, and continuously depositing atoms or molecules in the gas phase on a crystallization interface to realize mullite whisker growth;
weighing cobalt nitrate, cerium nitrate and zirconium nitrate, and then adding citric acid and distilled water to prepare a mixed solution;
step five, placing the mixed solution in a second container, placing the cordierite with the surface modified obtained in the step three in the second container, ensuring that the solution is over the sample, transferring the second container into a vacuum drying dish, vacuumizing, standing, taking out the sample, drying in an oven, and repeating the process once;
and step six, placing the sample obtained in the step five into a muffle furnace, heating and roasting to obtain the integral cDPF.
2. The method for preparing an integral cDPF for soot particle filtration in vehicle exhaust according to claim 1, wherein the integral cDPF prepared by the method is a cordierite-mullite-cerium-zirconium solid solution composite oxide, and has a bionic structure similar to the structure of human respiratory system and bronchial epimucosae cells.
3. The method for preparing an integral cDPF for soot particulate filtration in vehicle exhaust as claimed in claim 1, wherein the concentration ratio of the silica sol impregnation liquid, the aluminum nitrate impregnation liquid and the ammonium fluoride impregnation liquid is proportionally prepared as follows: 1:2:9, the concentration of the aluminum nitrate impregnating solution is 1.98 mol.L -1 。
4. The method for preparing an integral cDPF for soot particulate filtration in vehicle exhaust as claimed in claim 2, wherein the freezing temperature in the second step is-6 ℃, the drying temperature in the second step is 50-80 ℃, and the drying temperature in the second step is 55 ℃.
5. The method for preparing an integral cDPF for soot particle filtration in vehicle exhaust according to claim 4, wherein in the second and third steps, cordierite honeycomb ceramics are respectively immersed in silica sol immersion liquid, aluminum nitrate immersion liquid and ammonium fluoride immersion liquid for 6 hours, then frozen for 6 hours, finally dried at 90 ℃, placed in a muffle furnace and baked for 12 hours at 120 ℃, the immersion liquid generates gas phase atmosphere at high temperature, and mullite whisker growth is realized by continuous deposition of atoms or molecules in gas phase on a crystallization interface.
6. The method of preparing an integral cDPF for soot particulate filtration in vehicle exhaust as claimed in claim 5, wherein the temperature is raised and maintained in step three to 1000 ℃ at a temperature rise rate of 2 ℃/min for 2 hours;
the first container of the first step and the second container of the fifth step are beakers.
7. The method for preparing an integral cDPF for soot particulate filtration in vehicle exhaust as claimed in claim 2, wherein the molar ratio of cobalt nitrate, cerium nitrate, zirconium nitrate is 21:4:4, 3:1:1, 2:1:1, 1:1:1, 21:3:3, 21:2:2 or 21:1:1, and the heating firing in step six is to heat up to 600 ℃ at a heating rate of 2 ℃/min for 2 hours;
the amount of the substance added with the citric acid is the sum of the amount of the substance of cobalt nitrate 2 times, the amount of the substance of cerium nitrate 3 times and the amount of the substance of zirconium nitrate 4 times.
8. The method for preparing an integral cDPF for soot particulate filtration in vehicle exhaust as claimed in claim 2, wherein the rest time after evacuation in the fifth step is 10 to 30min and the drying temperature in the fifth step is 100 to 175 ℃.
9. The method for preparing an integral cDPF for soot particulate filtration in vehicle exhaust as claimed in claim 8, wherein the rest time after evacuation in said step five is 15min and the drying temperature in said step five is 110 ℃.
10. An integral cDPF for soot particulate filtration in vehicle exhaust, characterized in that it is prepared by the preparation method according to any one of claims 1 to 11.
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Application publication date: 20230502 |