CN114433201A - Nox存储催化剂及其制备方法 - Google Patents
Nox存储催化剂及其制备方法 Download PDFInfo
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- CN114433201A CN114433201A CN202110511820.7A CN202110511820A CN114433201A CN 114433201 A CN114433201 A CN 114433201A CN 202110511820 A CN202110511820 A CN 202110511820A CN 114433201 A CN114433201 A CN 114433201A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title abstract description 16
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 81
- 239000010457 zeolite Substances 0.000 claims abstract description 77
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 76
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 35
- 150000003624 transition metals Chemical class 0.000 claims abstract description 35
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 29
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000003860 storage Methods 0.000 claims abstract description 19
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 16
- 239000012452 mother liquor Substances 0.000 claims abstract description 16
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 16
- 230000001939 inductive effect Effects 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 5
- 238000011068 loading method Methods 0.000 claims abstract description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 94
- UNYSKUBLZGJSLV-UHFFFAOYSA-L calcium;1,3,5,2,4,6$l^{2}-trioxadisilaluminane 2,4-dioxide;dihydroxide;hexahydrate Chemical compound O.O.O.O.O.O.[OH-].[OH-].[Ca+2].O=[Si]1O[Al]O[Si](=O)O1.O=[Si]1O[Al]O[Si](=O)O1 UNYSKUBLZGJSLV-UHFFFAOYSA-L 0.000 claims description 62
- 229910052676 chabazite Inorganic materials 0.000 claims description 62
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 229910052746 lanthanum Inorganic materials 0.000 claims description 8
- 229910052684 Cerium Inorganic materials 0.000 claims description 7
- RZCJYMOBWVJQGV-UHFFFAOYSA-N 2-naphthyloxyacetic acid Chemical compound C1=CC=CC2=CC(OCC(=O)O)=CC=C21 RZCJYMOBWVJQGV-UHFFFAOYSA-N 0.000 claims description 5
- 231100001143 noxa Toxicity 0.000 claims description 5
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 4
- KXHPPCXNWTUNSB-UHFFFAOYSA-M benzyl(trimethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC1=CC=CC=C1 KXHPPCXNWTUNSB-UHFFFAOYSA-M 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- GNUJKXOGRSTACR-UHFFFAOYSA-M 1-adamantyl(trimethyl)azanium;hydroxide Chemical compound [OH-].C1C(C2)CC3CC2CC1([N+](C)(C)C)C3 GNUJKXOGRSTACR-UHFFFAOYSA-M 0.000 claims description 3
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 3
- 235000019743 Choline chloride Nutrition 0.000 claims description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 3
- 229910052689 Holmium Inorganic materials 0.000 claims description 3
- 229910052765 Lutetium Inorganic materials 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 229910052772 Samarium Inorganic materials 0.000 claims description 3
- 229910052771 Terbium Inorganic materials 0.000 claims description 3
- 229910052775 Thulium Inorganic materials 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 3
- NDKBVBUGCNGSJJ-UHFFFAOYSA-M benzyltrimethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)CC1=CC=CC=C1 NDKBVBUGCNGSJJ-UHFFFAOYSA-M 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 3
- 229960003178 choline chloride Drugs 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 229910052701 rubidium Inorganic materials 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 238000006731 degradation reaction Methods 0.000 description 20
- 239000010949 copper Substances 0.000 description 18
- 230000015556 catabolic process Effects 0.000 description 16
- 238000005259 measurement Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 238000005342 ion exchange Methods 0.000 description 7
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 6
- 239000002243 precursor Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000010335 hydrothermal treatment Methods 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 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 4
- 238000003795 desorption Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000018537 nitric oxide storage Effects 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 229910052790 beryllium Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 150000002500 ions Chemical group 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
- 239000011148 porous material Substances 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 241000269350 Anura Species 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 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
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 150000003840 hydrochlorides Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000012430 stability testing Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- 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
- B01J29/7049—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing rare earth elements, titanium, zirconium, hafnium, zinc, cadmium, mercury, gallium, indium, thallium, tin or lead
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- B01J29/00—Catalysts comprising molecular sieves
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- 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
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
- B01J29/76—Iron group metals or copper
- B01J29/763—CHA-type, e.g. Chabazite, LZ-218
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- 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
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- 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
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- B01D53/9413—Processes characterised by a specific catalyst
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- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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- 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
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- B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
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Abstract
本发明涉及一种NOX存储催化剂及其制备方法。NOX存储催化剂包括CHA沸石、CHA沸石中的离子交换的过渡金属、以及与过渡金属不同并且负载在CHA沸石上的稀土金属。用于制备NOX存储催化剂的方法包括制备合成母液,合成母液包含作为二氧化硅和氧化铝源的沸石原料、结构诱导材料、复合材料和溶剂,使合成母液反应以制备CHA沸石,和在制备的CHA沸石上负载过渡金属和不同于过渡金属的稀土金属。
Description
相关申请的引证
本申请要求2020年11月4日在韩国知识产权局提交的韩国专利申请号10-2020-0146181的权益,该申请通过引证合并于此。
技术领域
本公开涉及一种NOX存储催化剂(storage catalyst,吸藏催化剂,储存催化剂)及其制备方法。
背景技术
随着废气法规变得越来越严格,催化剂在初始启动时的性能变得越来越重要。然而,由于三效催化剂需要花费一些时间才能被活化,因此在启动之后,大部分废气在活化之前被排出。
为了对此进行补偿,已经开发了吸附型或吸留型催化剂。这些催化剂在车辆的初始启动时吸收或吸留废气组分,从而在三效催化剂被加热的同时抑制废气的排放。
例如,NOX存储催化剂在初始启动时吸留NOX,然后在高温下的还原气氛下,存储的NOX被废气中的还原剂组分除去。
然而,由于应用高效发动机技术来应对燃料效率和加强的法规,从而逐渐降低废气温度,因此减少从冷启动阶段(cold start section,冷启动部分)(即初始启动时的低温部分)排放的NOX存在限制。
发明内容
本公开涉及一种NOX存储催化剂及其制备方法。具体地,实施方式涉及NOX存储催化剂,其具有改善的从冷启动阶段排出的NOX的存储性能,该冷启动阶段是初始启动时的低温阶段。
本公开的实施方式可以提供一种具有优异的从冷启动阶段排出的NOX的存储性能的NOX存储催化剂,该冷启动阶段是初始启动期间的低温阶段。
本公开的其他实施方式提供了一种用于制备NOX存储催化剂的方法。
根据本公开的实施方式,用于存储NOX的催化剂包括CHA沸石、与CHA沸石进行离子交换的过渡金属、以及与过渡金属不同并且负载在CHA沸石上的稀土金属。
CHA沸石可以是硅铝酸盐沸石。
CHA沸石可具有约1至约50的Si/Al摩尔比。
过渡金属可以包括Cu、Fe、Co、Ti、Zn、Ag、Mn或其组合。
稀土金属可包括La、Ce、Nd、Pr、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu或其组合。
基于催化剂的总重量,催化剂可包含约1wt%至约10wt%的过渡金属。
基于催化剂的总重量,催化剂可包含约1wt%至约30wt%的稀土金属。
基于催化剂的总重量,催化剂可包含约1.5wt%至约3wt%的Cu和约3wt%至约16wt%的La。
基于催化剂的总重量,催化剂可包含约1.5wt%至约3wt%的Cu和约6wt%至约16wt%的Ce。
催化剂可以进一步包括在CHA沸石中进行离子交换的Be、Mg、Ca、Sr、Ba、Ra、Li、Na、K、Rb、Cs、Pr或其组合。
根据本公开的实施方式,一种用于制备NOX存储催化剂的方法包括制备合成母液,所述合成母液包含作为二氧化硅和氧化铝源(source of silica and alumina)的沸石原料、结构诱导材料(structure-inducing material)、复合材料(complexing material,络合材料)和溶剂,使合成母液反应以制备CHA沸石,并在制备的CHA沸石上负载过渡金属和不同于过渡金属的稀土金属。
沸石原料可包括Y型沸石或超稳定Y型沸石(USY沸石)。
沸石原料可具有约5至约100的SiO2/Al2O3摩尔比。
结构诱导材料可包括苄基三甲基氢氧化铵、苄基三甲基氯化铵、三甲基金刚烷基氢氧化铵(AdaOH)、氯化胆碱或其组合。
基于1摩尔份(part by mole)的沸石原料,合成母液可包含约0.1摩尔份至约0.4摩尔份的结构诱导材料和约0.1摩尔份至约0.4摩尔份的复合材料。
本公开的NOX存储催化剂具有改善的从冷启动阶段排出的NOX的存储性能,该冷启动阶段是初始启动时的低温阶段。
附图说明
图1是显示根据本公开的实施方式的用于制备NOX存储催化剂的方法的工艺流程图。
图2和图3是显示在实施例1和实施例2中制备的NOX存储催化剂的降解之前/之后的NOX吸附结果的图。
图4和图5是显示实施例1中制备的NOX存储催化剂的降解之前/之后的NO TPD(程序升温脱附)测量结果的图。
图6和图7是显示实施例2中制备的NOX存储催化剂的降解之前/之后的NO TPD(程序升温脱附)测量结果的图。
具体实施方式
在下文的详细描述中,将在下文中更全面地描述本公开,其中,参照附图描述了本公开的一些而非全部实施方式。本公开可以许多不同的形式来体现,并且不应被解释为限于这里阐述的实施方式。除非另有定义,否则本说明书中使用的所有术语(包括技术术语和科学术语)可以本领域普通技术人员通常理解的含义来使用。此外,除非明确定义相反的情况,否则在通用字典中定义的术语不会被理想地或过度地解释。
另外,除非明确描述相反的情况,否则词语“包含(comprise)”和诸如“包含(comprises)”或“包含(comprising)”的变体将被理解为暗示包括所述要素,但不排除任何其他要素。
此外,单数包括复数,除非另有说明。
根据本公开的实施方式的NOX存储催化剂包括CHA沸石、CHA沸石中的离子交换的过渡金属(transition metal ion-exchanged in the CHA zeolite)、以及与过渡金属不同并且负载在CHA沸石上的稀土金属。
CHA(菱沸石(chabazite))沸石是具有通过三维多孔结构连接的八元环孔(约3.8埃)的小孔沸石。CHA沸石的笼形结构通过连接带有4个环的双6环构建单元获得。
CHA沸石可以是铝硅酸盐沸石、硼硅酸盐、镓硅酸盐、SAPO、ALPO、MeAPSO或MeAPO,并且例如,CHA沸石的晶体结构可以是铝硅酸盐沸石。
CHA沸石可具有约1至约50、例如约4至约40、或约5至约30的Si/Al摩尔比。
在CHA沸石中,过渡金属和不同于过渡金属的稀土金属负载在其上。
过渡金属可以包括Cu、Fe、Co、Ti、Zn、Ag、Mn或其组合,例如Cu。
基于催化剂的总重量,催化剂可包含约1wt%至约10wt%、例如约1wt%至约5wt%、或约1.5wt%至约3wt%的过渡金属。
稀土金属可包括La、Ce、Nd、Pr、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu或其组合,例如La或Ce。
基于催化剂的总重量,催化剂可包含约1wt%至约30wt%、例如约3wt%至约30wt%、或约3wt%至约16wt%的稀土金属。
具体地,当稀土金属为La时,基于催化剂的总重量,催化剂可包括约3wt%至约16wt%的稀土金属,并且当稀土金属为Ce时,基于催化剂的总重量,催化剂可包括约6wt%至约16wt%的稀土金属。
同时,催化剂可通过水热处理降解。水热处理可以进行约12小时,同时使包含约10%的水的空气以约100ml/min流入在约650℃至约850℃下加热的催化剂层中。
另一方面,除了过渡金属和稀土金属以外,催化剂可进一步与碱土金属或碱金属进行离子交换,具体地,催化剂可进一步与Be、Mg、Ca、Sr、Ba、Ra、Li、Na、K、Rb、Cs、Pr或其组合进行离子交换。
一种用于制备NOX存储催化剂的方法包括制备合成母液,所述合成母液包含作为二氧化硅和氧化铝源的沸石原料、结构诱导材料、复合材料和溶剂,使合成母液反应以制备CHA沸石,以及在制备的CHA沸石上负载过渡金属和不同于过渡金属的稀土金属。
图1是示出用于制备NOX存储催化剂的方法的工艺流程图。在下文中,参考图1描述用于制备NOX存储催化剂的方法。
首先,制备包括沸石原料、结构诱导材料、复合材料和溶剂的合成母液(S1)。
沸石原料可包括Y型沸石或超稳定Y型沸石(USY沸石)。
沸石原料可具有约5至约100的SiO2/Al2O3摩尔比,并且例如,沸石原料可以是具有约30的SiO2/Al2O3摩尔比的沸石USY。
结构诱导材料可包括苄基三甲基氢氧化铵、苄基三甲基氯化铵、三甲基金刚烷基氢氧化铵(AdaOH)、氯化胆碱或其组合。另外,也可以包括用于制备CHA的通用结构诱导材料。
复合材料可以是包括氢氧化钠的碱性氢氧化物溶液。
基于1摩尔份的沸石原料,合成母液可包含约0.1摩尔份至约0.4摩尔份的结构诱导材料和约0.1摩尔份至约0.4摩尔份的复合材料。根据添加到合成母液中的复合材料的量,存在于合成的CHA沸石骨架中的铝的量可以变化,从而水热特性可以变化。因此,在本公开中制备的CHA沸石可具有约1至约50的Si/Al摩尔比。
随后,使合成母液反应以制备CHA沸石(S2)。
具体地,使合成母液在约120℃至约140℃下反应约2天至约6天,同时以约0rpm至约60rpm旋转,然后通过离心分离、洗涤并在约500℃至约600℃下煅烧约6小时至约12小时以制备CHA沸石。
另一方面,CHA沸石可以是Na形式的CHA沸石(Na-formed CHA zeolite),并且任选地,可以通过将Na形式的CHA沸石与阳离子进行离子交换来进一步包括制备NH4-形式的CHA沸石(NH4-formed CHA zeolite)。具体地,将Na形式的CHA沸石浸入1.5M硝酸铵水溶液中,然后在约60℃至约80℃下搅拌大于或等于约3小时,这可以重复三次以将其离子交换成NH4 +的形式,然后洗涤并干燥以获得NH4形式的CHA沸石。
随后,将过渡金属和与过渡金属不同的稀土金属负载在制备的CHA沸石上(S3)。
具体地,将过渡金属和稀土金属负载在CHA沸石上可包括用稀土金属前体溶液浸渍CHA沸石,以及将所得物煅烧(firing,烧制,烘烤)以制备其上负载有稀土金属的CHA沸石,然后在包含过渡金属前体的溶液中对其上负载有稀土金属的CHA沸石进行离子交换以负载过渡金属。
过渡金属和稀土金属的前体可以包括硝酸盐、盐酸盐、乙酸盐或硫酸盐。例如,当过渡金属是Cu时,前体可以是硝酸铜(II)(Cu(NO3)2)或乙酸铜(乙酸Cu),当稀土金属是La时,前体可以是硝酸镧,并且当稀土金属是Ce时,前体可以是硝酸铈。
溶剂可包括蒸馏水、去离子水、乙醇、甲醇、乙二醇、丙二醇、异丙醇或其组合。
取决于过渡金属的类型和交换的离子的量,离子交换可以在约25℃至约80℃下进行约1小时至约24小时。
另一方面,可以对制备的NOX存储催化剂进行水热处理以进行水热稳定性测试。水热处理可以进行约12小时,同时使包含约10%的水的空气以约100ml/min流入在约650℃至约850℃下加热的催化剂层中。
在下文中,给出了本发明的具体实例。然而,以下描述的实例仅用于说明性目的,并且本发明的范围不限于此。
[制备实施例1:CHA沸石的制备]
(制备实施例1)
用表1所示的组成制备合成母液。
将合成母液混合并放入高压釜中,然后反应4天,同时在140℃下以40rpm旋转,通过离心分离,洗涤并在550℃下煅烧12小时,以获得CHA沸石(CHA-1,Si/Al=12.1)。
(表1)
1)SDA:苄基三甲基氯化铵(BTMACl)
[制备实施例2:NOX存储催化剂的制备]
(比较例1)
将根据制备实施例1的CHA沸石(CHA-1)添加到1.0M的硝酸铜水溶液中以在25℃下离子交换24小时,然后洗涤、干燥、煅烧以制备与铜进行离子交换的CHA沸石。
(实施例1)
将制备实施例1的CHA沸石(CHA-1)浸入硝酸镧水溶液中,然后在100℃下干燥12小时,在550℃下煅烧2小时以制备La(x)/CHA(x是负载的La的wt%),其中La分别以5wt%、10wt%、15wt%、20wt%和30wt%负载。
将La(x)/CHA添加到1.0M硝酸铜水溶液中以在25℃下离子交换24小时,然后洗涤、干燥并在550℃下煅烧2小时以制备与铜进行离子交换的Cu/La(x)/CHA沸石(Cu:2wt%至2.5wt%)。
(实施例2)
将制备实施例1的CHA沸石(CHA-1)浸入硝酸铈水溶液中,在100℃下干燥12小时,在550℃下煅烧2小时以制备Ce(x)/CHA(x是负载的Ce的wt%),其中Ce分别以5wt%、10wt%、15wt%、20wt%和30wt%负载。
将制备的Ce(x)/CHA添加到1.0M硝酸铜水溶液中以在25℃下离子交换24小时,然后洗涤、干燥并在550℃下煅烧2小时以制备与铜进行离子交换的Cu/Ce(x)/CHA沸石(Cu:1.9wt%至3.0wt%)。
[实验实施例:NOX存储催化剂的性能评估]
通过将含有约10%的水的空气以100ml/min流入加热到至高达750℃的催化剂层中,将根据实施例1和2的催化剂进行水热处理(降解)12小时,然后,评估降解之前和之后的其NO吸附性能。
在NO吸附性能评价中,将0.2g的每种催化剂在空气流动下在500℃下预处理1小时,500ppm的NO被吸附,同时流过在50℃下加热的每个催化剂层1小时,然后,通过在50℃下使N2流动1小时来进行吹扫。随后,测量在N2流下脱附的NOX的浓度,同时以10℃/min将温度升至高达600℃。
图2和图3是显示在实施例1和2中制备的NOX存储催化剂的降解之前/之后的NOx吸附结果的图。图2是显示降解前的NOX存储催化剂的图,且图3是显示降解后的NOX存储催化剂的图。
参考图2和图3,在降解之前,当负载La和Ce时,无论它们的含量如何,NOX存储量均增加,但是在降解之后,当负载3wt%至16wt%的La和6wt%至16wt%的Ce时,NOX存储量增加。
图4和图5是显示实施例1中制备的NOX存储催化剂的降解之前/之后的NO TPD(程序升温脱附)测量结果的图。图4是显示降解前的NO TPD测量结果的图,且图5是显示降解之后的NO TPD测量结果的图。
参考图4和图5,当负载La时,降解之前/之后的NOX存储性能得到改善,并且在降解前,Cu/La(20)/CHA表现出最大的NO存储量,而在降解后,Cu/La(10)/CHA表现出最大的NO存储量。
图6和图7是显示实施例2中制备的NOX存储催化剂的降解之前/之后的NO TPD(程序升温脱附)测量结果的图。图6是显示降解前的NO TPD测量结果的图,且图7是显示降解之后的NO TPD测量结果的图。
参考图6和图7,当负载Ce时,降解之前/之后的NOX存储性能得到改善,并且Cu/Ce(10)/CHA表现出最大的NO存储量。
尽管已经结合当前被认为是实际的示例性实施方式描述了本发明,但是应当理解,本发明不限于所公开的实施方式。相反,其旨在覆盖所附权利要求的精神和范围内所包括的各种修改和等效布置。
Claims (18)
1.一种NOX存储催化剂,包括
菱沸石;
所述菱沸石中的离子交换的过渡金属;以及
稀土金属,所述稀土金属不同于所述过渡金属并且负载在所述菱沸石上。
2.根据权利要求1所述的NOX存储催化剂,其中,所述菱沸石为铝硅酸盐沸石。
3.根据权利要求1所述的NOX存储催化剂,其中,所述菱沸石具有1至50的Si/Al摩尔比。
4.根据权利要求1所述的NOX存储催化剂,其中,所述过渡金属包括选自由Cu、Fe、Co、Ti、Zn、Ag、Mn以及它们的组合组成的组的元素。
5.根据权利要求1所述的NOX存储催化剂,其中,所述稀土金属包括选自由La、Ce、Nd、Pr、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu以及它们的组合组成的组的元素。
6.根据权利要求1所述的NOX存储催化剂,其中,基于所述催化剂的总重量,所述催化剂包括1wt%至10wt%的所述过渡金属。
7.根据权利要求1所述的NOX存储催化剂,其中,基于所述催化剂的总重量,所述催化剂包括1wt%至30wt%的所述稀土金属。
8.根据权利要求7所述的NOX存储催化剂,其中,基于所述催化剂的总重量,所述催化剂包括1wt%至10wt%的所述过渡金属。
9.根据权利要求1所述的NOX存储催化剂,其中,基于所述催化剂的总重量,所述催化剂包括1.5wt%至3wt%的Cu和3wt%至16wt%的La。
10.根据权利要求1所述的NOX存储催化剂,其中,基于所述催化剂的总重量,所述催化剂包括1.5wt%至3wt%的Cu和6wt%至16wt%的Ce。
11.根据权利要求1所述的NOX存储催化剂,其中,所述催化剂进一步包括在所述菱沸石中进行离子交换的选自由下述组成的组的元素:Be、Mg、Ca、Sr、Ba、Ra、Li、Na、K、Rb、Cs、Pr或它们的组合。
12.一种用于制备NOX存储催化剂的方法,包括
制备合成母液,所述合成母液包含作为二氧化硅和氧化铝源的沸石原料、结构诱导材料、复合材料和溶剂;
使所述合成母液反应以制备菱沸石;以及
在制备的所述菱沸石上负载过渡金属和不同于所述过渡金属的稀土金属。
13.根据权利要求12所述的方法,其中,所述沸石原料包括Y型沸石。
14.根据权利要求12所述的方法,其中,所述沸石原料包括超稳定Y型沸石。
15.根据权利要求12所述的方法,其中,所述沸石原料具有5至100的SiO2/Al2O3摩尔比。
16.根据权利要求12所述的方法,其中,所述结构诱导材料包括苄基三甲基氢氧化铵、苄基三甲基氯化铵、三甲基金刚烷基氢氧化铵、氯化胆碱或它们的组合。
17.根据权利要求12所述的方法,其中,基于1摩尔份的所述二氧化硅和氧化铝源,所述合成母液包含0.1摩尔份至0.4摩尔份的所述结构诱导材料和0.1摩尔份至0.4摩尔份的所述复合材料。
18.根据权利要求12所述的方法,其中,进行所述方法产生NOX存储催化剂,所述NOX存储催化剂包括菱沸石、所述菱沸石中的离子交换的过渡金属、以及负载在所述菱沸石上的所述稀土金属。
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