CN113522232B - Passive NOxAdsorbent and preparation method and application thereof - Google Patents
Passive NOxAdsorbent and preparation method and application thereof Download PDFInfo
- Publication number
- CN113522232B CN113522232B CN202110719371.5A CN202110719371A CN113522232B CN 113522232 B CN113522232 B CN 113522232B CN 202110719371 A CN202110719371 A CN 202110719371A CN 113522232 B CN113522232 B CN 113522232B
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- sapo
- adsorbent
- passive
- molecular sieve
- drying
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000003463 adsorbent Substances 0.000 claims abstract description 129
- 238000000034 method Methods 0.000 claims abstract description 64
- 239000002184 metal Substances 0.000 claims abstract description 30
- 229910052751 metal Inorganic materials 0.000 claims abstract description 29
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 9
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 7
- 239000002808 molecular sieve Substances 0.000 claims description 74
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 74
- 238000001035 drying Methods 0.000 claims description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 61
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 60
- 239000008367 deionised water Substances 0.000 claims description 59
- 229910021641 deionized water Inorganic materials 0.000 claims description 59
- 238000005406 washing Methods 0.000 claims description 46
- 238000001354 calcination Methods 0.000 claims description 39
- 238000000967 suction filtration Methods 0.000 claims description 38
- 239000007787 solid Substances 0.000 claims description 21
- 238000005342 ion exchange Methods 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 11
- 238000005229 chemical vapour deposition Methods 0.000 claims description 8
- 238000000231 atomic layer deposition Methods 0.000 claims description 6
- 238000005470 impregnation Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052717 sulfur Inorganic materials 0.000 abstract description 10
- 239000011593 sulfur Substances 0.000 abstract description 10
- 239000003054 catalyst Substances 0.000 abstract description 8
- 229910052684 Cerium Inorganic materials 0.000 abstract description 5
- 230000018537 nitric oxide storage Effects 0.000 abstract description 5
- 229910052763 palladium Inorganic materials 0.000 abstract description 5
- 229910052697 platinum Inorganic materials 0.000 abstract description 5
- 229910052772 Samarium Inorganic materials 0.000 abstract description 3
- 229910052746 lanthanum Inorganic materials 0.000 abstract description 3
- 239000002594 sorbent Substances 0.000 abstract description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 113
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 35
- 238000009210 therapy by ultrasound Methods 0.000 description 17
- 229910002666 PdCl2 Inorganic materials 0.000 description 16
- 229910002651 NO3 Inorganic materials 0.000 description 13
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 13
- 238000003860 storage Methods 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- 230000009467 reduction Effects 0.000 description 10
- 238000006722 reduction reaction Methods 0.000 description 10
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 9
- 238000001179 sorption measurement Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- YWECOPREQNXXBZ-UHFFFAOYSA-N praseodymium(3+);trinitrate Chemical compound [Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YWECOPREQNXXBZ-UHFFFAOYSA-N 0.000 description 6
- JGFZNNIVVJXRND-UHFFFAOYSA-N N,N-Diisopropylethylamine (DIPEA) Chemical compound CCN(C(C)C)C(C)C JGFZNNIVVJXRND-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000003795 desorption Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000001307 helium Substances 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000010457 zeolite Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 231100001143 noxa Toxicity 0.000 description 3
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 3
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 description 3
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical group [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- BLVQZLMLJMPOIU-UHFFFAOYSA-N [Pm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O Chemical compound [Pm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BLVQZLMLJMPOIU-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 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 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 2
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical compound [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 150000002940 palladium Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000011007 phosphoric acid Nutrition 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- DFCYEXJMCFQPPA-UHFFFAOYSA-N scandium(3+);trinitrate Chemical compound [Sc+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O DFCYEXJMCFQPPA-UHFFFAOYSA-N 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910052773 Promethium Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- YZDZYSPAJSPJQJ-UHFFFAOYSA-N samarium(3+);trinitrate Chemical compound [Sm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YZDZYSPAJSPJQJ-UHFFFAOYSA-N 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/183—Physical conditioning without chemical treatment, e.g. drying, granulating, coating, irradiation
-
- 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
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3071—Washing or leaching
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
-
- 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
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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
- F01N3/0807—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by using absorbents or adsorbents
- F01N3/0828—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by using absorbents or adsorbents characterised by the absorbed or adsorbed substances
- F01N3/0842—Nitrogen oxides
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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
- F01N3/2066—Selective catalytic reduction [SCR]
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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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Biomedical Technology (AREA)
- Environmental & Geological Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Catalysts (AREA)
Abstract
The invention relates to a passive NOxAdsorbent, preparation method and application thereof, and passive NOxThe adsorbent comprises a carrier and an active component, wherein the carrier is SAPO-18, the active component is Pd or Pt, and the passive NOxThe adsorbent can also be doped with an auxiliary metal, and the auxiliary metal is at least one of La, Ce, Pr, Nd and Sm. The passive NO provided by the inventionxThe sorbent has good sulfur resistance and low temperature NO storage efficiency. The passive NO provided by the inventionxThe preparation method of the adsorbent can improve the passive NOxAdsorbent for storing NOxThe method is simple and effective to improve the performance of the original PNA catalyst, and has the advantages of sulfur resistance and easy repetition and operation.
Description
Technical Field
The invention belongs to passive NOxThe field of adsorbers (PNA), and relates to a passive NOxAn adsorbent and a preparation method and application thereof.
Background
Nitrogen Oxides (NO) emitted from diesel vehiclesx) Can adversely affect human health and environment, thereby reducing NOxBecomes an important social problem. Currently, Selective Catalytic Reduction (SCR) and NOxStorage Reduction (NSR) technology has been successfully used to reduce NO in diesel vehiclesxAnd (5) discharging. Both techniques are effective in reducing NO once the operating temperature (above 200 ℃) is reachedx. However, during cold start of vehicle operation, exhaust temperatures are well below 200 ℃, and these systems can fail. For example, at such low temperatures, current NSR catalysts are unable to oxidize NO to NO2And this is NOxA key step of storage; also, urea cannot be completely decomposed to NH in the SCR system3To convert NOx。
To control NO during cold startxEmission of, passive NOxThe adsorber (PNA), the NO of which is of great interestxThe adsorbent material can adsorb NO at low temperaturexAnd NO is converted into a gas at a high temperature when SCR and NSR normally operatexAnd releasing. Current research indicates metal oxides as NOxOne of the adsorbent materials has considerable potential. Crocker et Al (applied. Catal. B environ, 2015, 170-171, 283-292) reported Pt/Al2O3Has NO adsorption at 80-160 deg.CxThe ability of the cell to perform. And in Pt/Al2O3The addition of proper La can improve the adsorption of NOxThe ability of the cell to perform. Pd on CeO2The above temperature range of 80-200 ℃ can adsorb NO (US patent 8,105559), and the desorption temperature of NO is above 200 ℃. However, Pd-CeO2Exhibits low NO trapping efficiency and readily adsorbs SO2This severely limits NO storage in practical applications. Therefore, further development of Ce-based materials is required in practical applications.
Pd supported zeolite asIs an alternative material of PNA catalyst, which has good resistance to sulfur and Hydrocarbon (HC) poisoning. Recently, Chen et al (Catal. Lett.,2016,146, 1706-1711) reported that various zeolites such as BEA, MFI and CHA using Pd loading had high NO storage efficiency. Pd/zeolite as passive NOxThe unique behavior of the adsorbent depends on the nature of the Pd adsorption sites, and the framework structure of the zeolite affects not only the NO storage capacity but also the NO desorption temperature.
Disclosure of Invention
In order to solve the problem of lack of passive NO in the prior artxProblem of adsorbent, the present invention provides a passive NOxAn adsorbent and a preparation method and application thereof.
The technical scheme provided by the invention is as follows:
in a first aspect, there is provided a passive NOxThe adsorbent comprises a carrier and an active component, wherein the carrier is SAPO-18, and the active component is Pd or Pt.
Preferably, the doping amount of the active component in the carrier is 0.5wt.% to 5 wt.%.
Preferably, the passive NO isxThe adsorbent is further doped with an auxiliary metal, wherein the auxiliary metal is at least one of scandium (Sc), yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), manganese (Mn), nickel (Ni), and copper (Cu).
Preferably, the metal of the auxiliary agent is Ce, Pr or Nd.
Preferably, in the above technical solution, the doping amount of the promoter metal in the carrier is 0.5wt.% to 5wt.%, more preferably 0.5wt.% to 3wt.%, and even more preferably 2 wt.%.
Preferably, the passive NO isxThe adsorbent is prepared by any one of an impregnation method, an ion exchange method, an atomic layer deposition method and a chemical vapor deposition method.
In a second aspect, there is provided a method of preparing a passive NO as described abovexA method of making an adsorbent comprising the steps of:
(1) dissolving ammonium nitrate in deionized waterForming an ammonium nitrate solution; slowly adding the H-SAPO-18 molecular sieve into the ammonium nitrate solution, stirring for 10H at 80 ℃, and sequentially performing suction filtration, washing and drying to obtain NH4-SAPO-18 molecular sieve;
(2) dissolving an active component Pd or Pt in deionized water to obtain a precursor solution; and reacting NH4Slowly adding the SAPO-18 molecular sieve into the precursor solution, exchanging for 6h at 70 ℃, performing suction filtration, washing and drying to obtain a solid, and calcining for 5h at 550 ℃ to obtain Pd-SAPO-18 powder;
(3) and doping the assistant metal into the Pd-SAPO-18 powder by using an impregnation method, wherein the metal doping amount is 0.5-5.0 wt% of the mass of the powder.
In a third aspect, there is provided a passive NO comprising the above-mentionedxA particulate filter for diesel engine of adsorbent.
In a fourth aspect, a diesel exhaust gas treatment system is provided that includes the particulate filter for a diesel engine described above.
In a fifth aspect, a vehicle comprising the diesel exhaust treatment system is provided.
Compared with the prior art, the invention has the following beneficial effects:
(1) the passive NO provided by the inventionxThe sorbent has good sulfur resistance and low temperature NO storage efficiency.
(2) The passive NO provided by the inventionxThe preparation method of the adsorbent can improve the passive NOxAdsorbent for storing NOxThe method is simple and effective to improve the performance of the original PNA catalyst, and has the advantages of sulfur resistance and easy repetition and operation.
(3) The synthesis method has the advantages of low cost, simple process, environmental protection, molecular sieve, active component copper content and adjustable and controllable coordination environment surface acid concentration and acid strength of silicon atoms in the molecular sieve structure, and overcomes the defects of high cost, low raw material utilization rate and the like of the traditional one-step synthesis method.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is an XRD pattern for a Pd-SAPO-18 adsorbent with a promoter metal doping level of 2 wt.%;
FIG. 2 shows NO for different promoter-doped Pd-SAPO-18 adsorbents at 160 ℃ with a content of 2.0 wt.%xThe storage efficiency;
FIG. 3 shows NO for different amounts of Pr-doped PdPr-SAPO-18 adsorbents at 160 deg.CxThe storage efficiency;
FIG. 4 shows NO for Pd-SAPO-18 adsorbents that are undoped at 160 ℃ and doped with 2.0 wt.% Pr after sulfur exposurexThe storage efficiency.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The present invention provides a passive NOxThe adsorbent comprises a carrier and an active component, wherein the carrier is SAPO-18, and the active component is Pd or Pt. The passive NOxUse of adsorbents for NO control during cold start of a vehiclexAnd (4) discharging. Preferably, the doping amount of the active component in the carrier is 0.5wt.% to 5 wt.%. The above-mentioned passive NOxThe adsorbent can be doped with an assistant metal, wherein the assistant metal can be a rare earth element, the rare earth element is at least one of La, Ce, Pr, Nd and Sm, preferably, the doped rare earth element is Ce, Pr or Nd, and the doping amount of the doped rare earth element in the carrier is 0.5-5 wt.%.
Preferably, the above technical means isMoving NOxThe adsorbent is prepared by any one of an impregnation method, an ion exchange method, an atomic layer deposition method, a chemical vapor deposition method and a one-step method.
In a second aspect, there is provided a method of preparing a passive NO as described abovexA method of making an adsorbent comprising the steps of:
(1) dissolving ammonium nitrate in deionized water to form an ammonium nitrate solution; slowly adding the H-SAPO-18 molecular sieve into the ammonium nitrate solution, stirring for 10 hours at the temperature of 80 ℃, and sequentially performing suction filtration, washing and drying to obtain NH4-SAPO-18 molecular sieve;
(2) dissolving an active component Pd or Pt in deionized water to obtain a precursor solution; and reacting NH4Slowly adding the SAPO-18 molecular sieve into the precursor solution, exchanging for 6h at 70 ℃, performing suction filtration, washing and drying to obtain a solid, and calcining for 5h at 550 ℃ to obtain Pd-SAPO-18 powder;
(3) and doping the assistant metal into the Pd-SAPO-18 powder by using an impregnation method, wherein the metal doping amount is 0.5-5.0 wt% of the mass of the powder.
The invention also provides an in-situ preparation method of the passive NOxA method of making an adsorbent comprising the steps of:
sequentially adding an aluminum source, orthophosphoric acid, a silicon source, tertiary phosphorus, a palladium salt and an organic template agent N, N-diisopropylethylamine into deionized water, and fully stirring to obtain initial gel; and (3) placing the completely stirred gel in a hydrothermal reaction kettle, crystallizing for 1-7 days at 150-220 ℃, cooling at room temperature, centrifugally filtering, washing, drying, and calcining for 5 hours at 500-850 ℃ to obtain the Pd-SAPO-18 molecular sieve based catalyst.
In a third aspect, there is provided a passive NO comprising the above-mentionedxThe invention relates to a diesel particulate filter of adsorbent, which uses the passive NOxSorbent coated on particulate Filter (Filter or DPF) with low temperature NOxThe multifunctional functions of adsorption, oil smoke capture and catalytic combustion can realize NO in the cold start stage of the diesel enginexAnd eliminating the pollutants discharged by the oil smoke at the same time. The present invention can also use the passive NO mentioned abovexThe adsorbent is arranged in front of the SCR, thereby not only avoiding NH during SCR3Over-oxidation of and preventing rapid SCR of NO2Competition for oxidation of soot.
In a fourth aspect, a diesel exhaust gas treatment system is provided that includes the particulate filter for a diesel engine described above.
In a fifth aspect, a vehicle comprising the diesel exhaust treatment system is provided.
The framework structure of the Pd-SAPO-18 adsorbent doped with the auxiliary metal is not changed, and the characteristic peak of the auxiliary metal oxide does not appear in an XRD (X-ray diffraction) diagram after the content of the auxiliary metal is optimized, so that the uniform distribution of the auxiliary metal oxide on the surface of the catalyst or the small particle size of the formed oxide is shown. When the preferred promoter metal is Pr and its content is 2.0 wt.%, the PNA adsorbent has a higher storage efficiency and a better sulfur resistance.
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
Example 1
The embodiment provides a method for preparing a PdPr-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form an ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) 0.123g of Pr (NO)3)4·6H2Dissolving O in 2mL of deionized water to form a praseodymium nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the praseodymium nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, calcining the obtained solid at 550 ℃ for 5h, and thus obtaining the PdPr-SAPO-18 adsorbent with the Pr doping amount of 2.0 wt.%.
Example 2
The embodiment provides a method for preparing a PdLa-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4SAPO-18 molecular sieves.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) 0.125g of La (NO)3)3·6H2Dissolving O in 2mL of deionized water to form a lanthanum nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the lanthanum nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, calcining the obtained solid at 550 ℃ for 5h, and obtaining the PdLa-SAPO-18 adsorbent with the La doping amount of 2.0 wt.%.
Example 3
The embodiment provides a method for preparing a PdCe-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) 0.124g of Ce (NO)3)3·6H2O is dissolved in 2mL of deionized water to formAdding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the cerium nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, calcining the obtained solid at 550 ℃ for 5h, and respectively obtaining the PdCe-SAPO-18 adsorbent with the Ce doping amount of 2.0 wt.%.
Example 4
The embodiment provides a method for preparing a PdNd-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) 0.122g of Nd (NO)3)2·6H2Dissolving O in 2mL of deionized water to form a neodymium nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the neodymium nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, calcining the obtained solid at 550 ℃ for 5h, and respectively obtaining the PdNd-SAPO-18 adsorbent with the Nd doping amount of 2.0 wt.%.
Example 5
The embodiment provides a method for preparing a PdSm-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4Slowly adding SAPO-18 molecular sieve to the palladium chloride solutionExchanging the solution at 70 ℃ for 6h, filtering, washing, drying at 100 ℃, and calcining at 550 ℃ for 5h to obtain the Pd-SAPO-18 adsorbent.
(3) 0.118g of Sm (NO)3)3·6H2Dissolving O in 2mL of deionized water to form a samarium nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, calcining the obtained solid at 550 ℃ for 5h, and respectively obtaining the PdSm-SAPO-18 adsorbent with Sm doping amount of 2.0 wt.%.
Example 6
The embodiment provides a method for preparing a PdPr-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) 0.031g of Pr (NO)3)4·6H2Dissolving O in 2mL of deionized water to form a Pr nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, calcining the obtained solid at 550 ℃ for 5h, and respectively obtaining the PdPr-SAPO-18 adsorbent with the Pr doping amount of 0.5 wt.%.
Example 7
The embodiment provides a method for preparing a PdPr-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) Mixing 0.062g of Pr (NO)3)4·6H2Dissolving O in 2mL of deionized water to form a Pr nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, calcining the obtained solid at 550 ℃ for 5h, and respectively obtaining the PdPr-SAPO-18 adsorbent with the Pr doping amount of 1.0 wt.%.
Example 8
The embodiment provides a method for preparing a PdPr-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) Adding 0.093g of Pr (NO)3)4·6H2Dissolving O in 2mL of deionized water to form a Pr nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, calcining the obtained solid at 550 ℃ for 5h, and respectively obtaining the PdPr-SAPO-18 adsorbent with the Pr doping amount of 1.5 wt.%.
Example 9
The embodiment provides a method for preparing a PdPr-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) 0.125g of Pr (NO)3)4·6H2Dissolving O in 2mL of deionized water to form a Pr nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, calcining the obtained solid at 550 ℃ for 5h, and respectively obtaining the PdPr-SAPO-18 adsorbent with the Pr doping amount of 2.0 wt.%.
Example 10
The embodiment provides a method for preparing a PdPr-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) 0.185g of Pr (NO)3)4·6H2Dissolving O in 2mL of deionized water to form a Pr nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, calcining the obtained solid at 550 ℃ for 5h, and respectively obtaining the Pr doping amount of3.0 wt.% of a PdPr-SAPO-18 adsorbent.
Example 11
The embodiment provides a method for preparing a PtPr-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) Dissolving 1g of platinum nitrate in 50mL of deionized water to form a platinum nitrate solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the platinum nitrate solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pt-SAPO-18 adsorbent.
(3) 0.185g of Pr (NO)3)4·6H2Dissolving O in 2mL of deionized water to form a Pr nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, calcining the obtained solid at 550 ℃ for 5h, and respectively obtaining the PtPr-SAPO-18 adsorbent with the Pr doping amount of 3.0 wt.%.
Example 12
The embodiment provides a method for preparing a PdSc-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form an ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) 0.1g of Sc (NO)3)4·6H2O solutionAnd (3) forming a scandium nitrate solution in 2mL of deionized water, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the scandium nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, and calcining the obtained solid at 550 ℃ for 5h to obtain the PdSc-SAPO-18 adsorbent.
Example 13
The embodiment provides a method for preparing a PdY-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form an ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) 0.1g of Y (NO)3)4·6H2Dissolving O in 2mL of deionized water to form yttrium nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the yttrium nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, calcining the obtained solid at 550 ℃ for 5h, and thus obtaining the PdY-SAPO-18 adsorbent.
Example 14
The embodiment provides a method for preparing a PdPmP-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form an ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4Slowly adding SAPO-18 molecular sieve into the palladium chloride solution, exchanging at 70 deg.C for 6h, vacuum filtering, washing, and drying at 100 deg.CDrying and calcining at 550 ℃ for 5h to obtain the Pd-SAPO-18 adsorbent.
(3) 0.1g of Pm (NO)3)4·6H2Dissolving O in 2mL of deionized water to form a promethium nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the promethium nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, and calcining the obtained solid at 550 ℃ for 5h to obtain the PdPm-SAPO-18 adsorbent.
Example 15
The embodiment provides a method for preparing a PdCu-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form an ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) Adding Cu (NO)3)2·6H2Dissolving O in 2mL of deionized water to form a copper nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the copper nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, and calcining the obtained solid at 550 ℃ for 5h to obtain the PdCu-SAPO-18 adsorbent.
Example 16
The embodiment provides a method for preparing a PdMn-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form an ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the palladium chloride in 50mL of deionized water to form a palladium chloride solution3g of NH prepared in step (1) are added4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) 0.1g of Mn (NO)3)2Dissolving the Pd-SAPO-18 adsorbent prepared in the step (2) in 2mL of deionized water to form a manganese nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the manganese nitrate solution, carrying out ultrasonic treatment for 2 hours, drying at 80 ℃ for 12 hours, and calcining the obtained solid at 550 ℃ for 5 hours to obtain the PdMn-SAPO-18 adsorbent.
Example 17
The embodiment provides a method for preparing a PdNi-SAPO-18 adsorbent by an ion exchange method, which comprises the following steps:
(1) dissolving 10g of ammonium nitrate in 40mL of deionized water to form an ammonium nitrate solution, slowly adding 6g of H-SAPO-18 molecular sieve into the ammonium nitrate solution, exchanging for 10H at 80 ℃, performing suction filtration, washing, and drying at 100 ℃ to obtain NH4-SAPO-18 molecular sieve.
(2) 1g of PdCl2Dissolving the obtained solution in 50mL of deionized water to form a palladium chloride solution, and adding 3g of NH prepared in step (1)4And (3) slowly adding the SAPO-18 molecular sieve into the palladium chloride solution, exchanging for 6h at 70 ℃, performing suction filtration, washing, drying at 100 ℃, and calcining for 5h at 550 ℃ to obtain the Pd-SAPO-18 adsorbent.
(3) 0.1g of Ni (NO)3)2·6H2Dissolving O in 2mL of deionized water to form a nickel nitrate solution, adding 2g of the Pd-SAPO-18 adsorbent prepared in the step (2) into the nickel nitrate solution, carrying out ultrasonic treatment for 2h, drying at 80 ℃ for 12h, and calcining the obtained solid at 550 ℃ for 5h to obtain the PdNi-SAPO-18 adsorbent.
Example 18
This example provides a passive NOxThe preparation method of the adsorbent comprises the following steps:
weighing 100g H-SAPO-18 molecular sieve and 186g deionized water to prepare viscous slurry with solid content of 35 wt%; accurately weighing 0.176g of praseodymium nitrate solution with the concentration of 13.5 wt% and 0.08g of palladium nitrate solution with the concentration of 12.5 wt%, and slowly dropwise adding the praseodymium nitrate solution and the palladium nitrate solution into the slurry; and (2) putting the slurry into a ball mill, ball-milling the powder, controlling the D50 to be 6-10 mu m, drying the slurry in a 120 ℃ oven until the water is completely evaporated, and roasting in the air at 700 ℃ for 2h to obtain the PdPr-SAPO-18 adsorbent.
Example 19
This example provides a dip method for preparing passive NOxA method of making an adsorbent comprising the steps of:
(1) activating the SAPO-18 molecular sieve, and then alternately dipping the molecular sieve in praseodymium nitrate solution with the concentration of 1.35 wt% and palladium nitrate solution with the concentration of 1.25 wt% for 10 times; drying to remove excess liquid;
(2) roasting the SAPO-18 molecular sieve treated in the step (1) in air at 700 ℃ for 2H, and then roasting in H2And (3) carrying out reduction treatment in the atmosphere, wherein the reduction temperature is 600 ℃, and the reduction time is 1h, so as to obtain the PdPr-SAPO-18 adsorbent.
Example 20
This example provides a Chemical Vapor Deposition (CVD) process for preparing PdPr-SAPO-18 adsorbent.
a. Activating a carrier:
and placing the SAPO-18 molecular sieve in reaction equipment of chemical vapor deposition equipment, sealing a reaction cavity, vacuumizing the chemical vapor deposition system, introducing high-purity helium to purge a system pipeline, heating to 600 ℃, and introducing oxygen gas to complete carrier activation and promote high dispersion of active components on the surface of the SAPO-18.
b. Active component deposition:
adjusting the outlet valve of the reaction chamber of the chemical vapor deposition equipment treated in the step a, and setting the deposition temperature to be 550 ℃; simultaneously introducing a palladium chloride solution with the concentration of 12.5 wt% and oxygen into the reaction cavity, and controlling the time to be 150 s; finally, introducing high-purity helium gas for washing, wherein the washing time is controlled to be 120 s;
c. b, circulating for 10 times;
d. roasting the SAPO-18 obtained in the step c in air at 700 ℃ for 2hAfter at H2And carrying out reduction treatment under the atmosphere, wherein the reduction temperature is 600 ℃, and the reduction time is 1h, so as to obtain the Pd-SAPO-18 adsorbent.
Example 21
The embodiment provides a method for preparing a Pd-SAPO-18 adsorbent by an atomic layer deposition method, which comprises the following steps:
a. activating a carrier:
and placing the SAPO-18 molecular sieve in reaction equipment of atomic layer deposition equipment, sealing a reaction cavity, vacuumizing the atomic layer deposition system, introducing high-purity helium to purge a system pipeline, heating to 600 ℃, and then introducing oxygen gas to complete carrier activation and promote high dispersion of active components on the surface of the SAPO-18 molecular sieve.
b. Deposition of active components:
adjusting the outlet valve of the reaction cavity of the atomic layer reaction equipment treated in the step a to enable the cavity to be in a negative pressure state, and setting the deposition temperature to be 550 ℃; sequentially introducing a praseodymium nitrate solution with the concentration of 13.5 wt% for 200s and a palladium chloride solution with the concentration of 12.5 wt% for 200s into the reaction cavity; then introducing oxygen for 150 s; finally, introducing high-purity helium gas for washing, wherein the washing time is controlled to be 120 s;
c. b, circulating for 10 times;
d. roasting the SAPO-18 molecular sieve obtained in the step c in the air at the temperature of 700 ℃ for 2H, and then roasting in H2And (3) carrying out reduction treatment in the atmosphere, wherein the reduction temperature is 600 ℃, and the reduction time is 1h, so as to obtain the PdPr-SAPO-18 adsorbent.
Example 22
The embodiment provides a method for preparing a Pd-SAPO-18 catalyst in situ by a dual-template one-step method, which comprises the following steps:
sequentially adding an aluminum source, orthophosphoric acid, a silicon source, tertiary phosphorus, a palladium salt and an organic template agent N, N-diisopropylethylamine into deionized water, and fully stirring to obtain initial gel; and (3) placing the completely stirred gel in a hydrothermal reaction kettle, crystallizing for 1-7d at 150-220 ℃, cooling at room temperature, performing centrifugal filtration, washing, drying, and calcining for 5h at 500-850 ℃ to obtain the Pd-SAPO-18 molecular sieve catalyst.
Passive NO of the inventionxThe following method was used for evaluation of the adsorbent:
200mg of powder passive NO is charged into the reactorxAdsorbent to study its NOxAdsorption and desorption properties of. Introducing 5% of O2、10％H2O and N2The reaction space velocity is 30000h-1Pretreating for 30min, introducing 300ppmNO at different temperaturesxCarrying out NOxAnd (4) storing. In NOxAfter a period of storage, NO is switched offxAnd (4) carrying out gas flow and temperature programmed desorption.
FIG. 1 shows passive NO after doping with different promoter metalsxThe XRD pattern of the adsorbent found that the characteristic peaks of the oxides of each of the promoter metals did not appear at 2wt.% exchange, indicating that the oxides of each of the promoter metals were uniformly dispersed or their particle size was small, thus indicating that the doping of the promoter metals did not affect the framework structure of the molecular sieve.
FIG. 2 is the NO of different promoter metal doped Pd-SAPO-18 adsorbents at 160 ℃ with a content of 2.0 wt.%xStorage efficiency, different promoter metals produce NO on molecular sievesxDifferent ability to adsorb vacancies, and thus to NOxShows different efficiencies, wherein the Pr-doped Pd-SAPO-18 adsorbent shows excellent NOxThe adsorption efficiency.
FIG. 3 is NO for different amounts of Pr-doped PdPr-SAPO-18 adsorbents at 160 deg.CxStorage efficiency, NO generated in the molecular sieve when the Pr doping amount is 2.0 wt%xMost adsorbed vacancies, and therefore NO, adsorbedxThe efficiency is highest.
FIG. 4 is NO for Pd-SAPO-18 adsorbents undoped and doped with 2.0 wt.% Pr at 160 ℃ after sulfur exposurexStorage efficiency, wherein Pr-doped Pd-SAPO-18 adsorbents exhibit excellent NOxAnd the storage efficiency shows that the PdPr-SAPO-18 adsorbent has better sulfur resistance. In conclusion, the introduction of Pr can improve the adsorption efficiency of the adsorbent and enhance the sulfur resistance of the PNA adsorbent on the basis of not influencing the skeleton structure of the original PNA adsorbent, and Pr doping is simpleA single effective method for improving the performance of PNA adsorbent.
The foregoing are merely exemplary embodiments of the present invention, which enable those skilled in the art to understand or practice the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. Passive NOxThe adsorbent comprises a carrier and an active component, and is also doped with an auxiliary metal, and is characterized in that: the carrier is SAPO-18, the active component is Pd, and the auxiliary metal is at least one of praseodymium and neodymium.
2. Passive NO according to claim 1xAn adsorbent characterized by: the doping amount of the auxiliary metal in the carrier is 0.5-5 wt.%.
3. Passive NO according to claim 2xAn adsorbent characterized by: the doping amount of the auxiliary metal in the carrier is 0.5-3 wt.%.
4. Passive NO according to claim 3xAn adsorbent characterized by: the doping amount of the promoter metal in the carrier is 2 wt.%.
5. Passive NO according to claim 1xAn adsorbent characterized by: said passive NOxThe adsorbent is prepared by any one of an impregnation method, a solid-state ion exchange method, an atomic layer deposition method and a chemical vapor deposition method.
6. Preparation of the passive NO of any one of claims 1 to 5xMethod for producing adsorbentThe method is characterized by comprising the following steps:
(1) dissolving ammonium nitrate in deionized water to form an ammonium nitrate solution; slowly adding the H-SAPO-18 molecular sieve into the ammonium nitrate solution, stirring for 10H at 80 ℃, and sequentially performing suction filtration, washing and drying to obtain NH4-SAPO-18 molecular sieve;
(2) dissolving an active component Pd in deionized water to obtain a precursor solution; and reacting NH4Slowly adding the SAPO-18 molecular sieve into the precursor solution, exchanging for 6h at 70 ℃, performing suction filtration, washing and drying to obtain a solid, and calcining for 5h at 550 ℃ to obtain Pd-SAPO-18 powder;
(3) doping an auxiliary metal into the Pd-SAPO-18 powder by using an impregnation method, wherein the metal doping amount is 0.5-5.0 wt% of the mass of the powder; the assistant metal is one or more of Pr and Nd.
7. A particulate filter for a diesel engine, characterized in that: comprising the passive NO of any one of claims 1 to 5xAn adsorbent.
8. A diesel engine tail gas processing system which characterized in that: a particulate filter for diesel engines, comprising the particulate filter for diesel engines according to claim 7.
9. A vehicle, characterized in that: comprising the diesel exhaust treatment system of claim 8.
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