CN107376990A - Preparation method with loose porous SCR catalyst - Google Patents
Preparation method with loose porous SCR catalyst Download PDFInfo
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- CN107376990A CN107376990A CN201710503094.8A CN201710503094A CN107376990A CN 107376990 A CN107376990 A CN 107376990A CN 201710503094 A CN201710503094 A CN 201710503094A CN 107376990 A CN107376990 A CN 107376990A
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- China
- Prior art keywords
- scr catalyst
- preparation
- loose porous
- metal
- catalyst
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- 239000003054 catalyst Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 230000000694 effects Effects 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims description 35
- 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 30
- 239000002808 molecular sieve Substances 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 19
- 238000000227 grinding Methods 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 19
- 229910052751 metal Inorganic materials 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 11
- YOWAEZWWQFSEJD-UHFFFAOYSA-N quinoxalin-2-amine Chemical class C1=CC=CC2=NC(N)=CN=C21 YOWAEZWWQFSEJD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 8
- 229910052684 Cerium Inorganic materials 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000001099 ammonium carbonate Substances 0.000 claims description 6
- 239000000969 carrier Substances 0.000 claims description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 229910052723 transition metal Inorganic materials 0.000 claims description 5
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 4
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- -1 transition metal acetates Chemical class 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 235000013877 carbamide Nutrition 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 102000019034 Chemokines Human genes 0.000 claims 1
- 108010012236 Chemokines Proteins 0.000 claims 1
- 239000012752 auxiliary agent Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052717 sulfur Inorganic materials 0.000 abstract description 5
- 239000011593 sulfur Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000010949 copper Substances 0.000 description 9
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 8
- 238000009740 moulding (composite fabrication) Methods 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 229910052720 vanadium Inorganic materials 0.000 description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 5
- 229910001868 water Inorganic materials 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 125000005909 ethyl alcohol group Chemical group 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 150000002823 nitrates Chemical class 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- BVCZEBOGSOYJJT-UHFFFAOYSA-N ammonium carbamate Chemical compound [NH4+].NC([O-])=O BVCZEBOGSOYJJT-UHFFFAOYSA-N 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical class [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 2
- 229940071125 manganese acetate Drugs 0.000 description 2
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- DUFCMRCMPHIFTR-UHFFFAOYSA-N 5-(dimethylsulfamoyl)-2-methylfuran-3-carboxylic acid Chemical compound CN(C)S(=O)(=O)C1=CC(C(O)=O)=C(C)O1 DUFCMRCMPHIFTR-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910017827 Cu—Fe Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- PRKQVKDSMLBJBJ-UHFFFAOYSA-N ammonium carbonate Chemical class N.N.OC(O)=O PRKQVKDSMLBJBJ-UHFFFAOYSA-N 0.000 description 1
- 235000011162 ammonium carbonates Nutrition 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 description 1
- WYYQVWLEPYFFLP-UHFFFAOYSA-K chromium(3+);triacetate Chemical compound [Cr+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WYYQVWLEPYFFLP-UHFFFAOYSA-K 0.000 description 1
- 229940011182 cobalt acetate Drugs 0.000 description 1
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 150000003948 formamides Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical class [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical class [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/78—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J29/7815—Zeolite Beta
-
- 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
- B01D53/46—Removing components of defined structure
- B01D53/54—Nitrogen compounds
- B01D53/56—Nitrogen oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/88—Handling or mounting catalysts
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- 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
- B01D53/9418—Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
- B01J29/42—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively containing iron group metals, noble metals or copper
- B01J29/46—Iron group metals or copper
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
- B01J29/48—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively containing arsenic, antimony, bismuth, vanadium, niobium tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/78—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J29/783—CHA-type, e.g. Chabazite, LZ-218
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/82—Phosphates
- B01J29/84—Aluminophosphates containing other elements, e.g. metals, boron
- B01J29/85—Silicoaluminophosphates [SAPO compounds]
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/01—Engine exhaust gases
- B01D2258/012—Diesel engines and lean burn gasoline engines
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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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- 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
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/10—Internal combustion engine [ICE] based vehicles
- Y02T10/12—Improving ICE efficiencies
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- Organic Chemistry (AREA)
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- Environmental & Geological Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of preparation method with loose porous SCR catalyst, preparation has loose porous SCR catalyst in the range of 150~500 DEG C, NOXHigh conversion rate is up to more than 70%, 150 DEG C up to 78%, 200 DEG C is 98%, wide temperature window, outstanding cryogenic property, preferable sulfur resistive effect are illustrated, can effectively solve the problem that vehicle is chronically at NO under low-speed running state, winter cold start-up or the state that loitersXThe problem of activity is low, has stronger actual application value.In addition, this invention simplifies preparation flow, synthesis condition is easy to control, is easy to industrial applications.
Description
Technical field
The present invention relates to the preparation method with loose porous SCR catalyst, belongs to motor vehicle emission technical field, especially belongs to
In the field of catalyst preparation of SCR denitration.
Background technology
To meet Abgasgesetz, Urea-SCR technologies have turned into the preferred reduction NO of medium and heavy-duty engines enterpriseXTechnology path,
And increasingly received by people and turn into diesel engine vent gas NOXPost-process mainstream research direction.The core of Urea-SCR technologies
It is catalyst, Urea-SCR catalyst includes metal oxide catalyst, noble metal catalyst and Zeolite molecular sieve catalysis at present
Agent.Wherein noble metal catalyst cost is too high and easily forms sulfate with the sulfide in tail gas and causes catalyst inactivation.
Domestic use is more universal at present for catalytic component based on vanadium, has the advantages that application experience is abundant, technology maturation, but because vanadium system is catalyzed
Agent temperature window is narrow, and catalytic component based on vanadium can decompose during high temperature, caused V2O5Belong to highly toxic substance, health and environment are endangered
Evil is larger, thus it can only be a kind of temporary transient transitional technology, it is impossible to meets tightened up discharge standard requirement, Europe, the United States, day etc.
Developed country clearly prohibits the use of vanadium catalyst.
Transition metal supporting molecular sieve catalyst has the heat endurance higher than catalytic component based on vanadium and broader in recent years
Temperature window and receive significant attention.It is used for low-temperature SCR denitration as the A patents of application number CN 103599813 disclose one kind
Molecular sieve based catalyst and preparation method thereof, including the molecular sieve carriers that are modified of Cu and in tri- kinds of elements of Ce, Zr, Mn
One or more oxides.The catalyst in the range of 100~250 DEG C, reach 62 to the removal effect of nitrogen oxides~
100%, and there is good sulfur resistive ability；Application number CN102029178 A patents disclose copper-based molecular sieve catalyst and its
Preparation method, the mixed liquor of copper acetate and ammonium ceric nitrate is configured first, then add molecular sieve carrier ZSM-5 into mixed liquor and stir
Mix, finally obtain copper-based molecular sieve catalyst, the copper-based molecular sieve catalyst of gained by drying roasting, its molecular formula is expressed as
Cu-Ce-ZSM-5, its component are：Copper accounts for the 3-12% of total catalyst weight, and cerium accounts for the 5-8% of total catalyst weight, and ZSM-5 is accounted for
The 80-92% of total catalyst weight, the catalyst react very efficient at 200~500 DEG C to NH3-SCR, and with good
Water resistant sulfur resistance and stability, adapt to tightened up emission regulation demands, and reach reduce cost and improve use
The purpose of security；The A patents of application number CN 103008002 disclose the preparation method of Fe and Cu composite molecular sieve catalysts
And application, using Fe or Cu as active component, ZSM-5, SSZ-13, SAPO-34, MOR or Beta molecular sieve are catalyst carrier, are adopted
Catalyst is prepared with ion-exchange, then, the Fe molecular sieve catalysts and Cu molecular sieve catalytics prepared using mechanical series connection
Agent, the operating temperature window of molecular sieve catalyst is widened, in the range of 200~500 DEG C, the purification efficiency of nitrogen oxides reaches
More than 95%.
Though the molecular sieve catalyst that the Cu bases of above-mentioned preparation, Fe bases or Cu-Fe bases are modified improves NO to varying degreesX
Activity, widened temperature window, there is certain resistance to hydrothermal stability, but be in practical application we have found that：（1）Ion is handed over
Method is changed, program is cumbersome, can not realize industrial production；（2）For 200~500 DEG C of catalyst being prepared, the row of can solve the problem that
Temperature degree is more than 200 DEG C of uses, but the catalyst be in that winter cold start-up, idling be low and the worst cold case such as loiter under,
NOXActivity is very low, and even zero；（3）For with preferable low temperature NOXCatalyst, but in 300~500 DEG C of high temperature sections
NOXActivity it is relatively low.
The content of the invention
In view of the above in the prior art the shortcomings that, the purpose of the present invention are to be to provide to urge with loose porous SCR
The preparation method of agent, using modified molecular sieve catalyst as internal layer activated centre, by outer layer switching imported agent, by activity increase agent
Treated transition metal is supported on internal layer activated centre surface, and ectonexine active metal component passes through in calcination process
Chemically react, the effect of Synergistic is formed between ectonexine metal, while outer layer switching is led and also all volatilized in calcination process
Fall, flexible loose porous structure is finally formed on endothecium structure surface.Prepared by the present invention has loose porous SCR catalyst
In the range of 150~500 DEG C, NOXHigh conversion rate is 98% up to more than 70%, 150 DEG C up to 78%, 200 DEG C, illustrates wider temperature
Window, outstanding cryogenic property, preferable sulfur resistive effect are spent, can effectively solve the problem that vehicle is chronically at low-speed running state, winter
NO under its cold start-up or the state that loitersXThe problem of activity is low, has stronger actual application value.In addition, present invention letter
Preparation flow is changed, synthesis condition is easy to control, is easy to industrial applications.
The technical proposal of the invention is realized in this way：Preparation method with loose porous SCR catalyst, it is characterised in that tool
Body step is as follows：(1) by the one or more in 12.5~15.6 parts of mantoquita and 1.6~3.7 parts of metal promoters, be dissolved in from
In sub- water, stirring and dissolving, 34~47.6 parts of molecular sieve carriers are added, mix 2~4h；(2) 1.5~1.9 parts of amino are added
Ammonium formate, at 45~60 DEG C, 1~3h of stirring obtains mixed liquor；（3）Mixed liquor drying, high-temperature calcination, grinding obtain metal
Modified molecular screen powder；（4）10.8~16.2 parts of transition metal acetates are dissolved in deionized water wiring solution-forming, add 0.5
~0.9 part of activity increase agent, 12.5~15.6 especially layer switching imported agent and 1.5~2.6 parts of surface dispersants, 45~105 DEG C of strengths
Stir 2~5h；（5）Add 33.3~43.2 parts（3）Obtained metal-modified molecular sieve powder is strong at 60~115 DEG C
Power stirs 3~6h, obtains body of paste；（6）Body of paste is dried in 85~120 DEG C of baking ovens, crushed, 450~520 DEG C of calcining 4h
~6h, grinding, that is, obtain with flexible, porous double-decker SCR catalyst.
The metal promoter is the one or more in La, Ti, Cr, Mn and Ce.
Described transition acetate is the one or several kinds in Co, Zr, Cr, Mn and Ce metal.
The activity increase agent is one in ammonium formate, aminoquinoxaline, ammonium oxalate, formamide, ammonium carbonate, ammonium hydrogen carbonate and urea
Kind is several.
The outer layer switching imported agent is CMC（Mass fraction 1%）, the surface dispersant is one kind in ethanol, propyl alcohol
Or combination.
Good effect of the present invention is that it has loose porous SCR catalyst in the range of 150~500 DEG C, NOXHigh conversion rate
It is 98% up to more than 70%, 150 DEG C up to 78%, 200 DEG C, illustrates wide temperature window, outstanding cryogenic property, preferably resists
Sulphur effect, it can effectively solve the problem that vehicle is chronically at NO under low-speed running state, winter cold start-up or the state that loitersXActivity
The problem of low, there is stronger actual application value；In addition preparation flow is also simplify, synthesis condition is easy to control, is easy to industry
Change application.
Brief description of the drawings
Fig. 1 is the transmission TEM image that embodiment 1 prepares catalyst；
Fig. 2 is the NO of embodiment 1 and comparative example 1XConversion ratio test curve;
Fig. 3 is that the presulfurization of embodiment 1 handles NO after 24hXConversion ratio test curve.
Embodiment
In following specific example descriptions, a large amount of concrete details are given in order to more deep this hair of understanding
It is bright.It will be apparent, however, to one skilled in the art that the present invention can without one or more of these details and
It is carried out.
Embodiment 1
(1) by 900g copper nitrate and 100g cerous nitrates, it is dissolved in 2200g deionized waters, stirring and dissolving, adds
3000gBeta40 molecular sieve carriers, mix 2h；(2) 100g carbamic acid ammonia is added, at 45 DEG C, stirring 3h is mixed
Liquid；（3）Mixed liquor obtains metal modified molecular screen powder through 105 DEG C of drying, 450 DEG C of calcining 5h, grindings；（4）By 900g's
Manganese acetate is dissolved in 2900g deionized water wiring solution-formings, add 56g ammonium formates, 1000g mass fractions be 1%CMC and 150g without
Water-ethanol, 45 DEG C of strong stirring 5h；（5）Add 3000g（3）The metal-modified molecular sieve powder of middle acquisition is strong at 60 DEG C
Power stirs 6h, obtains body of paste；（6）Body of paste is dried in 85 DEG C of baking ovens, crushed, 450 DEG C of calcining 6h, grindings, that is, is obtained
With loose porous SCR catalyst.
Fig. 1 is catalyst TEM image prepared by embodiment 1, it can be seen that outer hole is relatively abundanter, and distribution is compared
Uniformly.
Catalyst fines is prepared to embodiment 1 using micro- anti-fixed bed gas-solid phase reaction unit simulation tail gas and carries out difference
At a temperature of SCR conversion ratios test, test condition is:NO concentration 1000 ppm, O2：5%（Volume fraction）、NH3：1000 ppm、
H2O：8%（Volume fraction）, nitrogen be Balance Air, air speed is set as 150000h-1, test result is as shown in Fig. 2 the catalyst exists
150℃NOXHigh conversion rate is up to high conversion rate at 78%, 200 DEG C up to 98%, it is shown that excellent cryogenic property, the catalyst is 150
DEG C~450 DEG C of NOXHigh conversion rate is up to more than 75%.
Catalyst prepared by embodiment 1 is being subjected to presulfurization processing at 200 DEG C to fresh catalyst, the time is
24h, gas component composition is O28 vol %, SO2200ppm, N2Balance Air is tested, as a result as shown in figure 3, can by figure
See, compared with fresh exemplar prepared by embodiment 1, except 450-500 DEG C of NOXConversion ratio be declined slightly outer, other temperature sections
NOXActivity change is little, and this shows that the catalyst has preferable sulfur tolerance.
Comparative example 1
(1) by 900g copper nitrate and 100g cerous nitrates, it is dissolved in deionized water, stirring and dissolving, adds 3000gBeta40 molecules
Carrier is sieved, mixes 2h；(2) 100g carbamic acid ammonia is added, at 45 DEG C, stirring 3h obtains mixed liquor；（3）Mixed liquor passes through
105 DEG C of drying, 450 DEG C of calcining 5h, grindings obtain metal modified molecular screen powder.By comparative example 1 in NO concentration 1000
ppm、O2：5%（Volume fraction）、NH3：1000 ppm、H2O：5%（Volume fraction）, nitrogen be Balance Air, air speed is set as
150000h-1Tested, as a result as shown in Fig. 2 in 150 DEG C of NOXConversion ratio 62%, high conversion rate is up to 78% at 200 DEG C, temperature
Window is compared with Example 1, hence it is evident that to high-temperature mobile, this shows that the cryogenic property of catalyst in comparative example 1 does not have embodiment 1 to make
For the good of catalyst.
Embodiment 2
（1）By 1005g copper nitrate and 200g lanthanum nitrates, it is dissolved in 3000g deionized waters, stirring and dissolving, adds
3000gSapo34 molecular sieve carriers, mix 4h；(2) 118g aminoquinoxalines are added, at 60 DEG C, stirring 2h is mixed
Liquid；（3）Mixed liquor obtains metal modified molecular screen powder through 105 DEG C of drying, 450 DEG C of calcining 5h, grindings；（4）By 830g's
Zirconium acetate is dissolved in 2100g deionized water wiring solution-formings, adds 35g formamides, 825g mass fractions are 1.0%CMC and 150g third
Alcohol, 105 DEG C of strong stirring 3h；（5）Add 3000g（3）The metal-modified molecular sieve powder of middle acquisition, the strength at 105 DEG C
5h is stirred, obtains body of paste；（6）It will be dried in 105 DEG C of baking ovens of body of paste, be broken, 500 DEG C of calcining 5h, grindings, that is, being had
Loose porous SCR catalyst.
Embodiment 3
(1) by 1200g copper nitrate and 300g cerous nitrates, it is dissolved in 3500g deionized waters, stirring and dissolving, adds 3000gZSM5
Molecular sieve carrier, mix 4h；(2) 145g aminoquinoxalines are added, at 60 DEG C, stirring 1h obtains mixed liquor；（3）Mixed liquor
Metal modified molecular screen powder is obtained through 105 DEG C of drying, 450 DEG C of calcinings, grinding；（4）1005g cerous acetate is dissolved in
2900g deionized water wiring solution-formings, add 76g ammonium oxalate, 1000g mass fractions are 1.0%CMC and 160g absolute ethyl alcohols, and 85
DEG C strong stirring 2h；（5）Add 3000g（3）The metal-modified molecular sieve powder of middle acquisition, the strong stirring 3h at 105 DEG C,
Obtain body of paste；（6）Body of paste is dried in 120 DEG C of baking ovens, crushed, 450 DEG C of calcining 5h, grindings, that is, obtains having loose
Porous SCR catalyst.
Embodiment 4
(1) by 1350g copper nitrate and 250g manganese nitrates, it is dissolved in deionized water, stirring and dissolving, adds 3000gSSZ13 molecules
Carrier is sieved, mixes 3h；(2) 160g aminoquinoxalines are added, at 45 DEG C, stirring 2h obtains mixed liquor；（3）Mixed liquor passes through
115 DEG C of drying, 500 DEG C of calcinings, grinding obtain metal modified molecular screen powder；（4）950g chromium acetate is dissolved in 2800g
Ionized water wiring solution-forming, add 56g aminoquinoxalines, 920g mass fractions are 1%CMC and 120g absolute ethyl alcohols, 60 DEG C of strengths
Stir 3h；（5）Add 3000g（3）The metal-modified molecular sieve powder of middle acquisition, strong stirring 4h, obtains cream at 85 DEG C
Shape body；（6）Body of paste is dried in 105 DEG C of baking ovens, crushed, 520 DEG C of calcining 4h, grindings, that is, obtains that there is loose porous SCR
Catalyst.
Embodiment 5
(1) by 1000g copper nitrate and 130g Titanium Nitrates, it is dissolved in deionized water, stirring and dissolving, adds 3000gBeta25 points
Son sieve carrier, mixes 4h；(2) 138g aminoquinoxalines are added, at 50 DEG C, stirring 2h obtains mixed liquor；（3）Mixed liquor passes through
105 DEG C of drying, 500 DEG C of calcinings, grinding obtain metal modified molecular screen powder；（4）1200g manganese acetate is dissolved in 3200g
Deionized water wiring solution-forming, add 56g ammonium carbonates, 1350g mass fractions are 1%CMC and 215g absolute ethyl alcohols, 70 DEG C of strengths
5h is stirred, obtains body of paste；（5）Add 3000g（3）The metal-modified molecular sieve powder of middle acquisition, is strongly stirred at 115 DEG C
3h is mixed, obtains body of paste；（6）Body of paste is dried in 115 DEG C of baking ovens, crushed, 500 DEG C of calcining 5h, grindings, that is, is had
Loose porous SCR catalyst.
Embodiment 6
(1) by 1350g copper nitrate and 300g chromic nitrates, it is dissolved in deionized water, stirring and dissolving, adds 3000gZSM5 molecules
Carrier is sieved, mixes 4h；(2) 165g aminoquinoxalines are added, at 60 DEG C, stirring 2h obtains mixed liquor；（3）Mixed liquor passes through
105 DEG C of drying, 500 DEG C of calcinings, grinding obtain metal modified molecular screen powder；（4）1430g cobalt acetate is dissolved in 3000g
Deionized water wiring solution-forming, adds 72g ammonium hydrogen carbonate, 1150g mass fractions are 1.0%CMC and 200g absolute ethyl alcohols, 85 DEG C
Strong stirring 2h；（5）Add 3000g（3）The metal-modified molecular sieve powder of middle acquisition, strong stirring 3h, is obtained at 115 DEG C
To body of paste；（6）Body of paste is dried in 115 DEG C of baking ovens, crushed, 520 DEG C of calcining 4h, grindings, that is, obtains having loose more
Hole SCR catalyst.
Embodiment 7
(1) by 900g copper nitrate and 180g lanthanum nitrates, it is dissolved in 3200g deionized waters, stirring and dissolving, adds
3000gSapo34 molecular sieve carriers, mix 3h；(2) 110g aminoquinoxalines are added, at 60 DEG C, stirring 3h is mixed
Liquid；（3）Mixed liquor obtains metal modified molecular screen powder through 115 DEG C of drying, 500 DEG C of calcinings, grinding；（4）By 800g second
Sour cerium is dissolved in 2500g deionized water wiring solution-formings, adds 60g urea, 900g mass fractions are the anhydrous second of 1.0%CMC and 160g
Alcohol, 120 DEG C of strong stirring 2h；（5）Add 3000g（3）The metal-modified molecular sieve powder of middle acquisition, the strength at 115 DEG C
3h is stirred, obtains body of paste；（6）Body of paste is dried in 115 DEG C of baking ovens, crushed, 480 DEG C of calcining 5h, grindings, that is, is had
There is loose porous SCR catalyst.
Claims (5)
1. the preparation method with loose porous SCR catalyst, it is characterised in that comprise the following steps that：(1) by 12.5~15.6
One or more in the mantoquita and 1.6~3.7 parts of metal promoters of part, are dissolved in deionized water, stirring and dissolving, and addition 34~
47.6 parts of molecular sieve carriers, mix 2~4h；(2) 1.5~1.9 parts of aminoquinoxalines are added, at 45~60 DEG C, stirring 1~
3h obtains mixed liquor；（3）Mixed liquor drying, high-temperature calcination, grinding obtain metal modified molecular screen powder；（4）By 10.8
~16.2 parts of transition metal acetates are dissolved in deionized water wiring solution-forming, add 0.5~0.9 part of activity increase agent, 12.5~15.6
Especially layer switching imported agent and 1.5~2.6 parts of surface dispersants, 45~105 DEG C of 2~5h of strong stirring；（5）Addition 33.3~
43.2 part（3）Obtained metal-modified molecular sieve powder, 3~6h of strong stirring, obtains body of paste at 60~115 DEG C；
（6）Body of paste is dried in 85~120 DEG C of baking ovens, crushed, 450~520 DEG C of calcining 4h~6h, grindings, that is, obtains having soft
The porous double-decker SCR catalyst of property.
2. according to the preparation method with loose porous SCR catalyst described in claim 1, it is characterised in that the metal
Auxiliary agent is the one or more in La, Ti, Cr, Mn and Ce.
3. according to the preparation method with loose porous SCR catalyst described in claim 1, it is characterised in that transition metal
Acetate is the one or several kinds in Co, Zr, Cr, Mn and Ce metal.
4. according to the preparation method with loose porous SCR catalyst described in claim 1, it is characterised in that the chemokine
Agent is one or several kinds in ammonium formate, aminoquinoxaline, ammonium oxalate, formamide, ammonium carbonate, ammonium hydrogen carbonate and urea, described
Outer layer switching imported agent is CMC（Mass fraction 1%）.
5. according to the preparation method with loose porous SCR catalyst described in claim 1, it is characterised in that the surface
Dispersant is ethanol, one kind in propyl alcohol or combination.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110227538A (en) * | 2019-06-11 | 2019-09-13 | 一汽解放汽车有限公司 | The preparation method of the high activity DPF coating of NOx and PM is removed simultaneously |
| CN112023908A (en) * | 2020-08-04 | 2020-12-04 | 华北电力大学 | Nitrogen oxide removing catalyst and preparation method thereof |
| US20220023849A1 (en) * | 2018-12-06 | 2022-01-27 | Basf Se | Aqueous suspension comprising a zeolitic material and a zirconium chelate complex |
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| CN105289711A (en) * | 2015-11-06 | 2016-02-03 | 中国第一汽车股份有限公司 | Composite Fe-based molecular sieve based catalyst and preparing method thereof |
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| CN105289711A (en) * | 2015-11-06 | 2016-02-03 | 中国第一汽车股份有限公司 | Composite Fe-based molecular sieve based catalyst and preparing method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20220023849A1 (en) * | 2018-12-06 | 2022-01-27 | Basf Se | Aqueous suspension comprising a zeolitic material and a zirconium chelate complex |
| US11786887B2 (en) * | 2018-12-06 | 2023-10-17 | Basf Se | Aqueous suspension comprising a zeolitic material and a zirconium chelate complex |
| CN110227538A (en) * | 2019-06-11 | 2019-09-13 | 一汽解放汽车有限公司 | The preparation method of the high activity DPF coating of NOx and PM is removed simultaneously |
| CN112023908A (en) * | 2020-08-04 | 2020-12-04 | 华北电力大学 | Nitrogen oxide removing catalyst and preparation method thereof |
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