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Paula Celeste Da Novel Microporous Silicates and Mesoporous MCM Silva Ferreira Materials Derivatised with Inorganic and Organometallic Complexes

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Paula Celeste Da Novel Microporous Silicates and Mesoporous MCM Silva Ferreira Materials Derivatised with Inorganic and Organometallic Complexes Universidade de Aveiro Departamento de Quimica 0 @ 2000 qso 5a"s Paula Celeste da Novel microporous silicates and mesoporous MCM Silva Ferreira materials derivatised with inorganic and organometallic complexes Dissertação apresentada à Universidade de Aveiro para cumprimento dos requisitos necessários a obtenção do grau de Doutor em Quirnica, realizada sob orientação científica do Doutor João Carlos Matias Celestino Gomes da Rocha, Professor CatedrBtico do Departamento de Quirnica da Universidade de Aveiro. o Júri Presidente: Doutor Casimiro Adrião Pio Professor Catedrático da Universidade de Aveiro Vogais: Doutor Carlos José Rodrigues Crispim Romão Professor Catedrático do Instituto de Tecnologia Química e Biológica da Universidade Nova de Lisboa Doutor João Carlos Matias Celestino Gomes da Rocha Professor Catedrático da Universidade de Aveiro Doutora Maria Filipa Gomes Ribeiro Professora Associada do Departamento de Engenharia Química do Instituto Superior Técnico, da Universidade Técnica de Lisboa Doutora Ana Maria Vieira Silva Viana Cavaleiro Professora Associada da Universidade de Aveiro Doutora Isabel Maria de Sousa Gonçalves Professora Auxiliar da Universidade de Aveiro Doutor Michael William Anderson Full Professor, Department of Chemistry, Institute of Science and Technology, University of Manchester acknowledgements I would like to express my sincere gratitude to my supervisor Prof. Dr. João Rocha for giving me the opportunity to work with him and for sharing with me some of his knowledge. I also acknowledge his continuous help, specially, in the solid state NMR experiments and in the correction of this thesis. I would like to thank Prof. Dr. Isabel Gonçalves for her indispensable help, advice and guidance in the derivatisation of mesoporous MCM rnaterials with organometallic and inorganic complexes. I would like to acknowledge the fundamental contributions to this thesis of Dr. Artur Ferreira in the Rietveld refinement; Dr. Martyn Pillinger in the derivatisation of the mesoporous MCM materials and for carring out the EXAFS experiments, Ana Santos and Dr. Fritz Kuhn for the catalytic results; Prof Dr. Luís Carlos for the emission spectrum; Prof. Dr. Michael Anderson and Dr. Jonathan Agger; Dr. Alan Thursfield and Anabela Valente for the adsorption measurements. In particular, I would like to thank Dr. Paula Brandáo, Dr. Zhi Lin, and José Paulo Rainho for being always so ready to help me. I also thank Luísa Paula Valente, Dr. Anthony Baggaley and Duarte Marques. I wish to express my appreciation to Prof. Dr. Teixeira Dias, Prof. Dr. Vitor Félix, Prof. Dr. Cruz Pinto for helping me to solve some problems of my research. Thanks to Maria Rosário Sousa, Maria da Conceição Costa, Augusto Lopes, Ana Paula Esculcas and Gilberto Vasco for their continuous technical support. I wish to thank the Chemistry Department of the University of Aveiro and the Inorganic Group for providing the experimental conditions for this work. I thank Praxis XXI programrne for financia1 support (Ph.D. grant Praxis XXI/BD/3863/96). I cannot finish before deeply thanking my Farnily and Friends for their strong encouragement, love, patience and ...everything!!! ... Thanks for being with me always and making rny life so enjoyable!!! Thank you! "üeep down, I donY believe it takes any speclal talent for a person to lifi himself ofíthe ground and hover in the air. We a11 have it h us - every man, woman, and child - and with enough hard work and concentration, every human being is capable of duplicating the feats..." Paul Auster, 1994 Mr. Verügo resumo Os materiais microporosos e mesoporosos são potenciais catalisadores heterogéneos. Os zeólitos e outros materiais microporosos do tipo zeolítico tradicionais, têm átomos tetracoordenados no esqueleto. Nos últimos anos, um vasto número de titanossilicatos contendo Ti(IV) hexacoordenado e Si(IV) tetracoordenado, com estruturas tridimensionais, têm sido alvo de grande interesse. Um dos objectivos desta tese foi preparar silicatos microporosos, contendo átomos metálicos com número de coordenação superior a quatro, e possuindo quer novas estruturas quer propriedades físicas e químicas interessantes. Neste contexto, foi preparado um novo ítriossilicato de sódio, AV-1, análogo do raro mineral montregianite, Na4K2Y2Si16O38·10H2O. Este material é o primeiro sólido microporoso que contem quantidades estequiométricas de sódio (e ítrio) no esqueleto. Foi, também, sintetizado um silicato de cério, AV-5, análogo estrutural do mineral montregianite com potencial aplicação em optoelectrónica. Nesta tese é, ainda, descrita a síntese e caracterização estrutural de um silicato de cálcio hidratado, AV-2, análogo do raro mineral rhodesite (K2Ca4Na2Si16O38.12H2O). Na continuação do trabalho desenvolvido em Aveiro na síntese de novos titanossilicatos surgiu o interesse de preparar novos zirconossilicatos microporosos por síntese hidrotérmica. Foram preparados dois novos materiais análogos dos minerais petarasite Na5Zr 2Si3O18(Cl,OH)·2H2O (AV-3) e kostylevite, K2Si3O9·H2O (AV-8). Foram, também, obtidos análogos sintéticos dos minerais parakeldyshite e wadeite, por calcinação a alta temperatura de AV-3 e de umbite sintética. A heterogeneização de complexos organometálicos na superfície de materiais mesoporosos do tipo M41S permite ix associar a grande actividade catalítica e a presença de sítios activos localizados típicos dos complexos organometálicos, com a robustez e fácil separação, características dos materiais mesoporosos siliciosos. Nesta dissertação relata-se a derivatização dos materiais MCM-41 e MCM-48 através da 5 5 reacção de [SiMe2{(h -C5H4)2}]Fe e [SiMe2{(h -C5H4)2}]TiCl2 com os grupos silanol das superfícies mesoporosas. Os materiais MCMs derivatizados com ansa-titanoceno foram testados na epoxidação de cicloocteno a 323 K na presença de hidrogenoperóxido de t-butilo. Estudou-se a heterogeneização dos sais de complexos com ligação metal-metal [Mo 2(MeCN)10][BF4]4, [Mo 2(m-O2CMe)2(MeCN)6][BF4]2 e [Mo2(m- O2CMe)2(dppa)2(MeCN)2][BF4]2 via imobilização nos canais do MCM-41. A imobilização dos catalisadores homogéneos na superfície do MCM-41 envolve a saída dos ligandos nitrilo lábeis, preferencialmente em posição axial, através da reacção com os grupos Si-OH da sílica. Verificou-se que a ligação Mo-Mo se mantém intacta nos produtos finais. É provável que estes materiais sejam eficientes catalisadores heterogéneos em reacções de polimerização. As técnicas de caracterização utilizadas nesta tese foram a difracção de raios-X de pós, a microscopia electrónica de varrimento, a espectroscopia de ressonância magnética nuclear do estado sólido (núcleos 13C, 23Na e 29Si), as espectroscopias de Raman e infravermelho com transformadas de Fourier, as análises termogravimétricas e as análises de adsorção de água e azoto. x abstract Microporous and mesoporous materials have great potential to be used as inorganic heterogeneous catalysts. Traditional zeolites and microporous zeolite-type materials contain four-coordinated framework atoms. A large number of titanosilicates containing six-coordinated Ti(IV) atoms and four- coordinated Si(IV) atoms, with three-dimensional structures, are extensively described in the literature. One of the aims of this thesis was to prepare new microporous framework oxide materials, containing metal atoms in different coordinations, which may possess novel structures and display interesting physical and chemical properties. In this context, a sodium yttrium silicate analogue of the rare mineral montregianite, Na4K2Y2Si16O38·10H2O (AV-1), was prepared. This material is the first microporous solid containing stoichiometric amounts of framework sodium (and yttrium) cations. A cerium silicate (AV-5) structural analogue of montregianite with potential for applications in optoelectronics was also prepared. In addition, the synthesis and structural characterisation of a calcium silicate hydrate analogue of the rare mineral rhodesite, K2Ca4Na2Si16O38.12H2O, (AV-2) is reported. As a natural extension of the work carried out on microporous titanosilicates, microporous zirconosilicates were prepared via hydrothermal synthesis. Two new synthetic analogues of the minerals petarasite (AV-3), Na5Zr2Si3O18(Cl,OH)·2H2O, and kostylevite (AV-8), K2Si3O9·H2O, were obtained. The preparation of analogues of parakeldyshite and Zr/Ti-wadeite was achieved by calcination at high temperature of AV-3 and synthetic Zr/Ti-umbite. The heterogenisation of homogeneous catalysts on the surfaces of mesoporous materials of the M41S type attempts to xi bring together the advantages of high activity and single-site active centres of homogeneous catalysts, and the robustness and easy separation of mesoporous siliceous material. The derivatisation of MCM-41 and 5 MCM-48 materials by covalent reaction of [SiMe 2{(h -C5H4)2}]Fe 5 and [SiMe2{(h -C5H4)2}]TiCl2 with pendant silanol groups is reported. Ti-modified mesoporous silicas were screened as catalysts for the epoxidation of cyclooctene at 323 K with t- butylhydroperoxide. Potential polymerisation catalysts were prepared by grafting of dimolybdenum complexes [Mo 2(MeCN)10][BF4]4, [Mo 2(m-O2CMe)2(MeCN)6][BF4]2 and [Mo 2(m- O2CMe)2(dppa)2(MeCN)2][BF4]2 onto the surface of purely siliceous MCM-41. The mechanism of surface attachment involves the displacement of labile acetonitrile ligands, most likely in the axially coordinated position, from the complexes by reaction with isolated nucleophilic silanol groups at the silica surface. The characterisation techniques used in this work were powder
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