汽车尾气净化Pd/CZ/Al_2O_3催化剂浸渍工艺研究
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摘要
以Pt、Rh、Pd贵金属为主的三效催化剂是控制汽油车尾气污染的重要方法。单钯(Pd)催化剂由于具有相对低廉的价格、丰富的资源和良好的低温催化活性,成为汽车尾气三效催化剂的研究热点之一。本论文针对Pd/CZ/Al_2O_3模型催化剂,对制备单钯催化剂的的浸渍工艺和参数进行了研究和优化,为汽油车尾气单钯催化剂的研发提供理论支持。
本论文采用浸渍法,考察了Pd前驱液浓度、浸渍次数,浸渍次序和焙烧次序对催化剂的催化活性和动态储放氧性能的影响;结合XRD、BET、TPR和贵金属分散度等表征手段,分析了贵金属形貌,贵金属与载体作用对催化剂的三效催化性能、动态储放氧性能的影响。
研究表明:前驱液浓度和浸渍次数与催化剂的催化活性不是单调递增或递减的关系,存在最优的前驱液浓度和浸渍次数有利于提高催化剂的催化性能和储放氧性能。分散度表征结果表明最优的前驱液浓度和浸渍次数提高了Pd的分散度,增加了催化剂的表面活性位,增强了Pd的抗烧结能力。
浸渍次序和焙烧次序结果表明Pd与CZ作用对CO转化有利,Pd与Al_2O_3作用对HC和NO转化有利,TPR结果显示Pd的浸渍次序影响了新鲜催化剂中Pd与载体的作用方式,高温老化后Pd在载体上的分布趋于一致。
Comparing with Pt and Rh, Pd is more abundant in resource, cheaper and better at light-off performance among the three kinds of rare-mental active components of TWC catalyst, and the Pd-only catalyst is playing more and more important role in the automotive emission control materals.This paper investigated the impregnation technics of Pd/CZ/Al_2O_3 catalyst, optimized the technics parameters and provided data for the further study of Pd-only catalyst.
The paper prepared the Pd/CZ/Al_2O_3 catalyst by impregnation method. The effect of Pd precursor concentration, the number of single-dipping, Pd addition order and calcining sequence on the three-way catalytic activity and dynamic oxygen storage capacity of the catalysts were studied and analysed combining with XRD, BET, TPR and noble metals dispersion.
The results of Pd precursor concentration and the number of single-dipping show that: There is not a monotony increase or decrease by degrees of Pd precursor concentration or the single-dipping number versus the three-way catalytic activity, but they have optimized values. Noble metal dispersion shows that Pd dispersion is elevated at that value, the active sites is increased and the agglomeration of Pd particle is prevented.
The results of Pd addition order and calcining sequence indicate that: Pd/CZ interaction has an advantage over the conversion of CO while Pd/Al_2O_3 interaction has an advantage over the conversion of HC and NO. TPR result shows that the interaction mode between Pd and carrier is affected by Pd addition order and calcined sequence before aging and the distribution of Pd over the catalysts keeps consistent after aged.
本论文采用浸渍法,考察了Pd前驱液浓度、浸渍次数,浸渍次序和焙烧次序对催化剂的催化活性和动态储放氧性能的影响;结合XRD、BET、TPR和贵金属分散度等表征手段,分析了贵金属形貌,贵金属与载体作用对催化剂的三效催化性能、动态储放氧性能的影响。
研究表明:前驱液浓度和浸渍次数与催化剂的催化活性不是单调递增或递减的关系,存在最优的前驱液浓度和浸渍次数有利于提高催化剂的催化性能和储放氧性能。分散度表征结果表明最优的前驱液浓度和浸渍次数提高了Pd的分散度,增加了催化剂的表面活性位,增强了Pd的抗烧结能力。
浸渍次序和焙烧次序结果表明Pd与CZ作用对CO转化有利,Pd与Al_2O_3作用对HC和NO转化有利,TPR结果显示Pd的浸渍次序影响了新鲜催化剂中Pd与载体的作用方式,高温老化后Pd在载体上的分布趋于一致。
Comparing with Pt and Rh, Pd is more abundant in resource, cheaper and better at light-off performance among the three kinds of rare-mental active components of TWC catalyst, and the Pd-only catalyst is playing more and more important role in the automotive emission control materals.This paper investigated the impregnation technics of Pd/CZ/Al_2O_3 catalyst, optimized the technics parameters and provided data for the further study of Pd-only catalyst.
The paper prepared the Pd/CZ/Al_2O_3 catalyst by impregnation method. The effect of Pd precursor concentration, the number of single-dipping, Pd addition order and calcining sequence on the three-way catalytic activity and dynamic oxygen storage capacity of the catalysts were studied and analysed combining with XRD, BET, TPR and noble metals dispersion.
The results of Pd precursor concentration and the number of single-dipping show that: There is not a monotony increase or decrease by degrees of Pd precursor concentration or the single-dipping number versus the three-way catalytic activity, but they have optimized values. Noble metal dispersion shows that Pd dispersion is elevated at that value, the active sites is increased and the agglomeration of Pd particle is prevented.
The results of Pd addition order and calcining sequence indicate that: Pd/CZ interaction has an advantage over the conversion of CO while Pd/Al_2O_3 interaction has an advantage over the conversion of HC and NO. TPR result shows that the interaction mode between Pd and carrier is affected by Pd addition order and calcined sequence before aging and the distribution of Pd over the catalysts keeps consistent after aged.
引文
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[39] Mart′?nez-Arias.A, Fernández-Garc?a.M, Ballesteros.V, et al. Characterization of High Surface Area Zr-Ce (1:1) Mixed Oxide Prepared by a Microemulsion Method . Langmuir, 1999, 15: 4796~4811.
[40]冯长根,胡玉才,王丽琼,铈锆氧化物固溶体对全钯三效固溶体性能的影响,应用化学,2003,20(2):159~162
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[2]黄振中,中国大气污染防治技术综述,世界科技研究与发展,26(2):30~35
[3]彭宝成,叶舜华,汽车尾气对动物的生物学效应研究,上海环境科学,1995,14(2):14~19
[4]吕源明,叶舜华,柴油机废气生物学效应的研究进展,中华预防医学杂志,1995,29(5):305~306
[5]时宗波,邵龙义,T.P.Jones等,城市大气可吸入颗粒物对质粒DNA的氧化性损伤,科学通报,2004,49(7):673~678
[6]许生,刘洋,朱丽娟,机动车废气对人体健康危害的分析,北方环境,2004,29(4):38~39
[7]李延红,袁东,阚海东等,大气颗粒物污染与人群死亡率变化流行病学研究进展,环境与职业医学,2003,20(1):47~49
[8]叶舜华,吕源明,祁萍萍,柴油机尾气颗粒提取物不同组分的致突变性,环境医学,1995,14(8):35~44
[9]贺克斌,傅立新,郝吉明等,我国汽车排气污染净化研究,环境科学进展,1996,4(3):62~69
[10]王建昕,傅立新,黎维彬,汽车排气污染治理及催化转化器,北京:化学工业出版社,2000,153~247
[11]王务林,赵航,王继先,汽车催化转化器系统概论,北京:人民交通出版社,1999,1~62
[12]杜志良,申江华,朱自航,车用乙醇汽油实验研究,汽车科技,2003,1:6~9
[13]李正西,对车用乙醇汽油的一些探讨,科技与经济,2001,14(4):11~13
[14]钱叶剑,谈建,左承基等,车用乙醇汽油对电喷汽油机性能影响的实验研究,内燃机学报,2006,24(4):320~325
[15]阎存仙,何凤英,车用三效催化转化器发展概况,环境污染与防治,2002,24(6):346~349
[16]朱振忠,田群,陈宏德,汽车尾气三效催化剂,中国环保产业,2002,37(7):34~36
[17] Gandhi. H.S, Graham. G.W, andMcCabe. R.W, Automotive exhaust catalysis, Journal of Catalysis, 2003, 216: 433~442
[18] Hu.Z, Wan .C.Z, Lui.Y.K, et al. Design of a novel Pd three-way catalyst: integration of catalytic functions in three dimensions, Catalysis Today 1996, 30 :83~89
[19] Fernández-García.M, Iglesias-Juez.A, Martínez-Arias.A. Role of the state of the metal component on the light-off performance of Pd-based three-way catalysts, Journal of Catalysis, 2004, 221: 594~600
[20] Ka?par.J, Fornasiero.P , Graziani.M,Use of CeO2-based oxides in the three-way catalysis, Catalysis Today, 1999, 50: 285~298
[21] Trovarelli A, Catalysis by Ceria and Related Materials, London: Imperial College Press, 2002, 73
[22] Mart?nez-Arias.A, Fernández-Garc?a.M. Iglesias-Juez.A, New Pd/CexZr1?xO2/Al2O3 three-way catalysts prepared by microemulsion Part 1. Characterization and catalytic behavior for CO oxidation Applied Catalysis B: Environmental 2001, 31:39~50
[23] Mart?nez-Arias.A, Fernández-Garc?a.M, Iglesias-Juez.A . New Pd/CexZr1?xO2/Al2O3 three-way catalysts prepared by microemulsion Part 2. In situ analysis of CO oxidation and NO reduction under stoichiometric CO+NO+O2, J.Applied Catalysis B: Environmental 2001, 31:51~60
[24] Alessandro Trovarelli, Eliana Rocchini, et al, Some recent developments in the characterization of ceria-based catalysts, Journal of Alloys and Compounds, 2001, 12(4): 584~591
[25]郑育英,邓淑华,三效催化剂中助剂的研究进展,三峡大学学报,2004,26(1):93~94
[26] Byong K.Cho, Chemical modification of catalyst support for enhancement of transient catalytic activity: nitric oxide reduction by carbon monoxide over rhodium, Journal of catalysis, 1991, 131(1): 74~87
[27] Kobayashi.T, Yamada.T, Kayano.K, Effect of basic metal additives on NOx reduction property of Pd-based three-way catalyst. Applied Catalysis B: Environmental 2001, 30: 287~292
[28] Norman Macleod, James Isaac, Richard M. Lambert , A comparison of sodium-modified Rh/-Al2O3 and Pd/-Al2O3 catalysts operated under simulated TWC conditions. Applied Catalysis B: Environmental. 2001, 33: 335~343
[29]Pérez-Alonso.F.J,LópezGranados.M, Ojeda.M,Chemical Structures of Coprecipitated Fe-Ce Mixed Oxides, Chem. Mater, 2005, 17: 2329~2339
[30] Pérez-Alonso.F.J,Melián-Cabrera .I, López Granados.M, Synergy of FexCe1?xO2 mixed oxides for N2O decomposition, Journal of Catalysis, 2006, 239: 340~346
[31]范煜,王立秋,张守臣,萤石结构铜-铈-氧催化剂组成与催化活性,大连理工大学学报,2001,41(4):421~425
[32] Williams, L.Jimmie. Monolith structures,materials, properties and uses. Catalysis Today, 2001, 69(1～4): 3~9
[33] Miller.W.S, Zhuang.L, Bottema.J. Recent development in aluminium alloys for the automotive industry. Materials Science and Engineering, 2000, 1: 37~49
[34] Padakis.VG, Pliangos.CA, Yentekakis.I.V,et al. Development of high performance, Pd-based, three way catalysts. Catalysis Today, 1996, 29: 71~75
[35] Fernández-García.M, Iglesias-Juez.A, Martínez-Arias.A. Role of the state of the metal component on the light-off performance of Pd-based three-way catalysts. Journal of Catalysis, 2004, 221:594~600
[36]黄莺,金属载体的活性氧化铝涂层工艺研究:[硕士学位论文],天津大学,2005
[37] Tanak.S, Mizukami.F, Niwa.S. Preparation of highly dispersed silica supported palladium catalysts by a complexing agent-assisted sol–gel method and their characteristics. Applied Catalysis A:General, 2002, 229(1~2): 165~174
[38] Do Heui Kima, Seong Ihl Wooa, O-Bong Yang. Effect of pH in a sol–gel synthesis on the pHysicochemical properties of Pd–alumina three-way catalyst. Applied Catalysis B: Environmental 2000, 26: 285~289
[39] Mart′?nez-Arias.A, Fernández-Garc?a.M, Ballesteros.V, et al. Characterization of High Surface Area Zr-Ce (1:1) Mixed Oxide Prepared by a Microemulsion Method . Langmuir, 1999, 15: 4796~4811.
[40]冯长根,胡玉才,王丽琼,铈锆氧化物固溶体对全钯三效固溶体性能的影响,应用化学,2003,20(2):159~162
[41]储伟,催化剂工程,成都:四川大学出版社,2006,57~57
[42] Schwarz.J.A. The adsorpotion/impregnation of catalytic precursors on pure and composite oxides. Catalysis Today, 1992, 15: 395~405.
[43] Schwarz.J.A, Ugbor.C.T, Zhang.R. The adsorpotion/impregnation of Pd(Ⅱ) cations on alumina, silica and their composite oxides. Journal of Catalysis, 1992, 138: 38~54.
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