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Zinc(II) phthalocyanines immobilized in mesoporous silica Al-MCM-41 and their applications in photocatalytic degradation of pesticides

Silva, M.; Calvete, M. J. F.; Gonçalves, N. P. F.; Burrows, H. D.; Sarakha, M.; Fernandes, A.; Ribeiro, M. F.; Azenha, M. E; Pereira, M. M.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
ENG
Relevância na Pesquisa
99.40252%
In the present study the authors investigated a set of three new zinc(II) phthalocyanines (zinc(II) tetranitrophthalocyanine (ZnTNPc), zinc(II) tetra(phenyloxy)phthalocyanine (ZnTPhOPc) and the tetraiodide salt of zinc(II)tetra(N,N,N-trimethylaminoethyloxy) phthalocyaninate (ZnTTMAEOPcI)) immobilized into Al-MCM-41 prepared via ship-in-a-bottle methodology. The samples were fully characterized by diffuse reflectance-UV–vis spectroscopy (DRS-UV–vis), luminescence, thermogravimetric analysis (TG/DSC), N2 adsorption techniques and elemental analysis. A comparative study was made on the photocatalytic performance upon irradiation within the wavelength range 320–460 nm of these three systems in the degradation of pesticides fenamiphos and pentachlorophenol. ZnTNPc@Al-MCM-41 and ZnTTMAEOPcI@Al-MCM-41 were found to be the most active systems, with the best performance observed with the immobilized cationic phthalocyanine, ZnTTMAEOPcI@Al-MCM-41. This system showed high activity even after three photocatalytic cycles. LC–MS product characterization and mechanistic studies indicate that singlet oxygen (1O2), produced by excitation of these immobilized photosensitizers, is a key intermediate in the photocatalytic degradation of both pesticides.

Oligomerização de eteno catalisada pelo complexo Ni[MeCN]6[BF4]2 imobilizado nos suportes [AI]-MCM-41 e SiO2

Rodrigues, Larissa Ribeiro
Fonte: Universidade Federal do Rio Grande do Sul Publicador: Universidade Federal do Rio Grande do Sul
Tipo: Dissertação Formato: application/pdf
POR
Relevância na Pesquisa
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O presente trabalho trata do estudo da oligomerização de eteno catalisada pelo complexo Ni[MeCN]6[BF4]2 imobilizado por adsorção seletiva nos suportes inorgânicos [Al]-MCM41 e SiO2 associado ao agente alquilante AlEt3. O sistema suportado foi avaliado em suspensão empregando diclorometano como solvente, em um reator semicontínuo com alimentação a pressão constante de eteno. A caracterização por DRIFT e XPS do sistema suportado em [Al]-MCM-41 mostrou que a esfera de coordenação do níquel foi modificada. As análises de TEM e XRD demonstraram que a organização dos poros da [Al]-MCM-41foi mantida após a etapa de imobilização do complexo. A análise de TEM demonstrou ainda que o diâmetro dos poros é de 3 nm. A análise de adsorção de N2 demonstrou que a imobilização do complexo de níquel ocorreu dentro dos poros dos suportes [Al]-MCM-41 e SiO2.pois as áreas superficiais tiveram uma diminuição média de 25% após o processo de imobilização. Os resultados referentes aos testes catalíticos mostraram que esses novos sistemas são ativos na dimerização e trimerização de eteno, A concentração do agente alquilante (AlEt3) mostrou-se um parâmetro muito sensível em relação a produção seletiva de buteno-1...

Estudo da influência do ambiente química e textual do suporte sobre as propriedades catalíticas dos sistemas híbridos Ni(MeCN)6(BF4)2/SiO2, [Si,AL]-MCM-41 ou [Si]-MCM-41 na reação de oligomerização de eteno e propeno

Rodrigues, Larissa Ribeiro
Fonte: Universidade Federal do Rio Grande do Sul Publicador: Universidade Federal do Rio Grande do Sul
Tipo: Tese de Doutorado Formato: application/pdf
POR
Relevância na Pesquisa
70.06082%
Este trabalho trata do estudo das reações de oligomerização de eteno e propeno catalisada pelo complexo Ni(MeCN)6(BF4)2 imobilizado por adsorção seletiva nos suportes inorgânicos [Si]-MCM-41, [Al]-MCM-41 e SiO2 associados aos agentes alquilantes AlEt3 (oligomerização de eteno) e Al2Et3Cl3 (oligomerzação de propeno). Os sistemas suportados são avaliados em suspensão de diclorometano e clorobenzeno em um reator semicontínuo com alimentação à pressão constante de eteno ou propeno. A caracterização por a DRIFT e XPS dos sistemas suportados em [Si] - MCM-41 e [Si, Al] - MCM-41 demonstra a presença de espécies ativas diferentes e mostra que a esfera da coordenação de níquel é modificada pela natureza do suporte. As análises de TEM e XRD demonstram que a organização dos poros dos sistemas MCM-41 é mantida após a imobilização do complexo. A análise da adsorção do N2 demonstra que a imobilização do complexo ocorre dentro dos poros dos sistemas suportados em MCM-41 e SiO2. Os resultados que referem os testes catalíticos demonstram que estes novos sistemas são ativos na dimerização e na trimerização do eteno e do propeno. Os resultados que referem os testes catalíticos demonstram que estes novos sistemas são ativos na dimerização e na trimerização do eteno e do propeno. A concentração dos agentes de alquilação revela ser um parâmetro muito sensível em relação à produção seletiva de 1-buteno e à atividade das reações de oligomerização do propeno. São apresentados...

Production of biodiesel by esterification of palmitic acid over mesoporous aluminosilicate Al-MCM-41

Carmo, Alipio C.; de Souza, Luiz K. C.; da Costa, Carlos E. F.; Longo, Elson; Zamian, Jose R.; da Rocha Filho, Geraldo N.
Fonte: Elsevier B.V. Publicador: Elsevier B.V.
Tipo: Artigo de Revista Científica Formato: 461-468
ENG
Relevância na Pesquisa
68.97597%
Biodiesel has been obtained by esterification of palmitic acid with methanol, ethanol and isopropanol in the presence of Al-MCM-41 mesoporous molecular sieves with Si/Al ratios of 8.16 and 32. The catalytic acids were synthesized at room temperature and characterized by atomic absorption spectrometry (AAS), thermal analysis (TG/DTA), X-ray diffraction (XRD), nitrogen absorption (BET/BJH), infrared spectroscopy (IR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The reaction was carried out at 130 degrees C whilst stirring at 500 rpm, with an alcohol/acid molar ratio of 60 and 0.6 wt% catalyst for 2 h. The alcohol reactivity follows the order methanol > ethanol > isopropanol. The catalyst Al-MCM-41 with ratio Si/Al = 8 produced the largest conversion values for the alcohols studied. The data followed a rather satisfactory approximation to first-order kinetics. (C) 2008 Elsevier Ltd. All rights reserved.

Interaction of water vapour at 298K with Al-MCM-41 materials synthesised at room temperature

Russo, Patrícia; Ribeiro Carrott, Manuela; Padre-Eterno, A.; Carrott, Peter; Ravikovitch, P.I.; Neimark, A.V.
Fonte: Universidade de Évora Publicador: Universidade de Évora
Tipo: Artigo de Revista Científica Formato: 344592 bytes; application/pdf
ENG
Relevância na Pesquisa
99.28294%
The interaction of water vapour with Al-MCM-41, prepared by direct synthesis at ambient temperature and pressure, using tetraethoxysilane, aluminium sulfate, hexadecyltrimethylammonium bromide and ammonia, and its effect on the pore structure were studied in order to investigate the stability towards prolonged exposure to water vapour and the influence of the aluminium content. With this purpose two consecutive water adsorption isotherms were determined at 298 K on samples with Si/Al ratio between 15 and 100. The samples were characterised by X-ray diffraction and adsorption of nitrogen at 77 K and toluene at 298 K, prior to and after exposure to water vapour. Pore size distributions were calculated from nitrogen, toluene and water adsorption isotherms using, respectively, the NLDFT method, a recently developed hybrid MC-DBdB method and the DBdB macroscopic approximation. It was found that Al-MCM-41 samples are significantly stable and that the stability improves as the amount of aluminium increases. Upon prolonged exposure to water vapour, there is a small decrease in pore size (3-5%), pore volume (8-16%) and total surface area (3-7%). The structural changes are essentially a consequence of the surface hydroxylation that occurred and not a result of a partial collapse of the pore structure. Although the presence of some extraframework Al can contribute to the improvement of the stability by protecting the surface...

Comparative study of Al-MCM materials prepared at room temperature with different aluminium sources and by some hydrothermal methods

Ribeiro Carrott, Manuela; Conceição, Filipe; Lopes, J.M.; Carrott, Peter; Bernardes, C.; Rocha, J.; Ribeiro, F. Ramôa
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica Formato: 95816 bytes; application/pdf
ENG
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A comparison of the pore structural properties and catalytic activity of MCM-41 containing aluminium, prepared at room temperature with different aluminium sources, is presented. In addition, they are compared with those of MCM-41 obtained by two conventional hydrothermal procedures and room temperature synthesised Al-MCM-48 grades. Al-MCM-41 samples were prepared by direct synthesis at room temperature with tetraethoxysilane (TEOS) and aluminium isopropoxide, aluminium sulfate or sodium aluminate, and by two hydrothermal routes using silica Ludox suspension and sodium aluminate (at 377K) or Cab-O-Sil silica and alumina (at 377K and 423K). The synthesis of MCM-48 grades was also carried out at room temperature with TEOS and aluminium sulfate or nitrate. The materials were characterised by X-ray diffraction, nitrogen adsorption at 77K and solid-state 27Al MAS NMR. The catalytic activity was evaluated in the reaction of double bond position isomerisation of 1-butene to 2-butenes at 373K. It is concluded that the room temperature synthesis method used resulted in the preparation in a short period of time of well structured MCM-41 materials that contained predominantly tetracoordinated aluminium and presented acidic catalytic activity similar to or better than those prepared by the two hydrothermal procedures. Aluminium sulfate is a good alternative to isoproxide in the room temperature synthesis as it resulted in samples with very uniform pore size...

Effect of hydrothermal treatment on the structure, stability and acidity of Al containing MCM-41 and MCM-48 synthesised at room temperature

Russo, Patrícia; Ribeiro Carrott, Manuela; Carrott, Peter
Fonte: Universidade de Évora Publicador: Universidade de Évora
Tipo: Artigo de Revista Científica Formato: 808650 bytes; application/pdf
ENG
Relevância na Pesquisa
59.858896%
The effect of hydrothermal treatment of the synthesis gel on the structure, hydrothermal and mechanical stabilities and acidity of MCM-41 and MCM-48 aluminosilicates synthesised at room temperature has been investigated by X-ray diffraction, nitrogen adsorption at 77K and DRIFTS with pyridine as probe molecule. The influence of the Al content and pore size on the structure of the resulting treated Al-MCM-41 materials has also been studied. For all samples improvement of the structural ordering and increase of the pore size, was observed, with pore wall thickness remaining practically unchanged. For Al-MCM-48 an improvement of the pore size uniformity occurs during the treatment. Only a small loss of pore size uniformity occurred for Al-MCM-41 prepared with hexadecyltrimethylammonium bromide, but with samples prepared with tetra and octadecyltrimethylammonium bromide the treatment generated a bimodal pore size distribution. The pore volume increased (17%) in the case of Al-MCM-48 but decreased (5.5–14%) for Al-MCM-41, suggesting a decrease in surface roughness resulting from increase of the degree of condensation of the pore walls. Both treated and untreated samples presented relatively strong Brønsted sites and increase of the Lewis acidity was found to occur upon treatment. Treated samples were found to be more resistant to refluxing in boiling water and mechanical compaction...

CATALYTIC AND ADSORPTION PROPERTIES OF Al- AND Ti-MCM-41 SYNTHESIZED AT ROOM TEMPERATURE

Silva, Tiago N.; Lopes, José Madeira; Ribeiro, Fernando Ramôa; Carrott, Manuela Ribeiro; Galacho, Cristina; Sousa, Maria José; Carrott, Peter
Fonte: Akadémiai Kiadó and Kluwer Academic Publishers Publicador: Akadémiai Kiadó and Kluwer Academic Publishers
Tipo: Artigo de Revista Científica
ENG
Relevância na Pesquisa
68.60926%
Aluminosilicate and titanosilicate MCM-41 were synthesized using a room temperature method. A preliminary catalytic evaluation was performed in the promotion of the 1-butene double bond isomerization, which was successful in probing differences in the acidity of the samples prepared.

Influence of the synthesis conditions on the pore structure and stability of MCM-41 materials containing aluminium or titanium

Ribeiro Carrott, M.M.L.; Galacho, C.; Conceição, F.L.; Carrott, P.J.M.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
ENG
Relevância na Pesquisa
58.850454%
A comparison of the pore structural properties of MCM-41 containing titanium, prepared at room temperature, with those of aluminosilicate grades is presented. The influence on the structural characteristics of using different metal sources, co-solvents and metal content is also considered. Additionally, the stability of Al-MCM-41 and Ti-MCM-41 samples, with Si/M=30, towards prolonged exposure to pure water vapour at 298K was investigated.

Al-containing MCM-41 type materials prepared by different synthesis methods: hydrothermal stability and catalytic properties

Lourenço, J. P.; Fernandes, A.; Henriques, C.; Ribeiro, M. F.
Fonte: Universidade do Algarve Publicador: Universidade do Algarve
Tipo: Artigo de Revista Científica
Publicado em //2006 ENG
Relevância na Pesquisa
69.284517%
Al-containing MCM-41 type materials were prepared by three different synthesis methods (aluminum grafting on the calcined MCM-41, pH adjustment during the crystallization period and crystallization in the presence of zeolite seeds). The samples were characterized by powder XRD, nitrogen adsorption, 27Al MAS NMR and FTIR with pyridine as probe molecule. All the samples exhibit a high hydrothermal stability at high temperature just with a minor structural degradation. N2 adsorption data obtained for the sample prepared from a gel containing zeolite seeds suggest a higher structural resistance to the hydrothermal treatment in comparison with the samples prepared by other methods. A different type of pyridine adsorbed, probably interacting simultaneously with a Brönsted and a Lewis acid site, is observed upon pyridine adsorption. This type of adsorption is stronger for the sample prepared in the presence of zeolite seeds and is not observed on Al-grafted MCM-41. 2 The catalytic activity towards the isomerization of α-pinene depends mainly on the number of Brönsted acid sites. The data obtained in this study strongly indicate that for this type of materials, the Lewis acid sites do not influence the selectivity for the isomerization products.

A Cu/Al-MCM-41 mesoporous molecular sieve: application in the abatement of no in exhaust gases

Batista,M. S.; Melo,R. A. A.; Wallau,M.; Urquieta-González,E. A.
Fonte: Brazilian Society of Chemical Engineering Publicador: Brazilian Society of Chemical Engineering
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/09/2005 EN
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Propane oxidation and reduction of NO to N2 with propane under oxidative conditions on a Cu-Al-MCM-41 mesoporous molecular sieve and Cu-ZSM-5 zeolites were studied. Both types of catalysts were prepared by ion exchange in aqueous solutions of copper acetate and characterised by X-ray diffraction (XRD), nitrogen sorption measurement, diffuse reflectance ultra-violet spectroscopy (DRS-UV), diffuse reflectance infra-red Fourier transform spectroscopy (DRIFTS) of the adsorption of CO on Cu+ and temperature-programmed reduction with hydrogen (H2-TPR). The NO reduction was performed between 200 and 500 ºC using a GHSV = 42,000 h-1. H2-TPR data showed that in the prepared Cu-Al-MCM-41 all the Cu atoms are on the surface of the mesopores as highly dispersed CuO, which results in a decrease in specific surface area and in mesopore volume. H2-TPR together with DRIFTS data provided evidence that in Cu/ZSM-5 catalysts, Cu atoms are found as two different Cu2+ cations: Cualpha2+ and Cubeta2+, which are located on charge compensation sites, and their thermo-redox properties were different from those of Cu atoms in Cu-Al-MCM-41. The specific activity of the Cu2+ exchangeable cations in Cu-ZSM-5, irrespective of their nature, was much greater than that of the Cu2+ in Cu-Al-MCM-41...

MCM-41 ordered mesoporous molecular sieves synthesis and characterization

Melo,Rogério A.A.; Giotto,Marcus V.; Rocha,João; Urquieta-González,Ernesto A.
Fonte: ABM, ABC, ABPol Publicador: ABM, ABC, ABPol
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/07/1999 EN
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69.12432%
The aim of this work was to study the hydrothermal synthesis of Si and SiAlMCM-41 performed under both autogenic pressure and refluxing conditions. XRD data showed that the MCM-41 phase may be formed by both processes and that the synthesized material in the presence of Al and/or under reflux presents the hexagonally arrangement of less ordered mesopores. However, as verified by XRD and physisorption data, the order was improved with higher synthesis times. 29Si and 1H - 29Si C/P MAS NMR spectra showed that a great part of the Si atoms exists as silanol groups which originate resonance peaks at -110, -100 and -91 ppm. The presence of Al atoms may generate Si(3Si, Al) and Si(2Si, 2Al) environments which might be contributing to resonance peaks at -100 and -91 ppm. The 27Al MAS NMR spectrum of the as synthesized AlSiMCM-41 showed a resonance peak of tetrahedral framework aluminum close to 53 ppm and two others, one close to 14 ppm attributed to Al(H2O)6+3 species and the other a weak signal close to 32 ppm attributed to pentacoordinated Al. 27Al MAS NMR spectra of the calcined sample showed a peak at 0 ppm corresponding to an hexacoordinated extra-framework aluminum formed during calcination.

CuO nanoparticles encapsulated inside Al-MCM-41 mesoporous materials via direct synthetic route

Huo, Chengli; Ouyang, Jing; Yang, Huaming
Fonte: Nature Publishing Group Publicador: Nature Publishing Group
Tipo: Artigo de Revista Científica
Publicado em 14/01/2014 EN
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Highly ordered aluminum-containing mesoporous silica (Al-MCM-41) was prepared using attapulgite clay mineral as a Si and Al source. Mesoporous complexes embedded with CuO nanoparticles were subsequently prepared using various copper sources and different copper loadings in a direct synthetic route. The resulting CuO/Al-MCM-41 composite possessed p6mm hexagonally symmetry, well-developed mesoporosity, and relatively high BET surface area. In comparison to pure silica, these mesoporous materials embedded with CuO nanoparticles exhibited smaller pore diameter, thicker pore wall, and enhanced thermal stability. Long-range order in the aforementioned samples was observed for copper weight percentages as high as 30%. Furthermore, a significant blue shift of the absorption edge for the samples was observed when compared with that of bulk CuO. H2-TPR measurements showed that the direct-synthesized CuO/Al-MCM-41 exhibited remarkable redox properties compared to the post-synthesized samples, and most of the CuO nanoparticles were encapsulated within the mesoporous structures. The possible interaction between CuO and Al-MCM-41 was also investigated.

Conversão térmica e termocatalítica à baixa temperatura do óleo de girassol para obtenção de bio-óleo

Araújo, Aruzza Mabel de Morais
Fonte: Universidade Federal do Rio Grande do Norte; BR; UFRN; Programa de Pós-Graduação em Ciência e Engenharia do Petróleo; Pesquisa e Desenvolvimento em Ciência e Engenharia de Petróleo Publicador: Universidade Federal do Rio Grande do Norte; BR; UFRN; Programa de Pós-Graduação em Ciência e Engenharia do Petróleo; Pesquisa e Desenvolvimento em Ciência e Engenharia de Petróleo
Tipo: Dissertação Formato: application/pdf
POR
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The use of biofuels remotes to the eighteenth century, when Rudolf Diesel made the first trials using peanut oil as fuel in a compression ignition engine. Based on these trials, there was the need for some chemical change to vegetable oil. Among these chemical transformations, we can mention the cracking and transesterification. This work aims at conducting a study using the thermocatalytic and thermal cracking of sunflower oil, using the Al-MCM-41 catalyst. The material type mesoporous Al-MCM-41 was synthesized and characterized by Hydrothermical methods of X-ray diffraction, scanning electron microscopy, nitrogen adsorption, absorption spectroscopy in the infrared and thermal gravimetric analysis (TG / DTG).The study was conducted on the thermogravimetric behavior of sunflower oil on the mesoporous catalyst cited. Activation energy, conversion, and oil degradation as a function of temperature were estimated based on the integral curves of thermogravimetric analysis and the kinetic method of Vyazovkin. The mesoporous material Al-MCM-41 showed one-dimensional hexagonal formation. The study of the kinetic behavior of sunflower oil with the catalyst showed a lower activation energy against the activation energy of pure sunflower oil. Two liquid fractions of sunflower oil were obtained...

Degradacao termica e catalitica da borra oleosa de Petroleo com materiais nanoestruturados al-mcm-41 e AL-SBA-15

Paulino, Ana Adalgisa Dias
Fonte: Universidade Federal do Rio Grande do Norte; BR; UFRN; Programa de Pós-Graduação em Ciência e Engenharia do Petróleo; Pesquisa e Desenvolvimento em Ciência e Engenharia de Petróleo Publicador: Universidade Federal do Rio Grande do Norte; BR; UFRN; Programa de Pós-Graduação em Ciência e Engenharia do Petróleo; Pesquisa e Desenvolvimento em Ciência e Engenharia de Petróleo
Tipo: Tese de Doutorado Formato: application/pdf
POR
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Aiming to reduce and reuse waste oil from oily sludge generated in large volumes by the oil industry, types of nanostructured materials Al-MCM-41 and Al-SBA-15, with ratios of Si / Al = 50, were synthesized , and calcined solids used as catalysts in the degradation of oily sludge thermocatalytic oil from oilfield Canto do Amaro, in the state of Rio Grande do Norte. Samples of nanostructured materials were characterized by thermogravimetric analysis (TG / DTG), X-ray diffraction (XRD), scanning electron microscopy (SEM), absorption spectroscopy in the infrared Fourier transform (FT-IR) and adsorption nitrogen (BET). The characterization showed that the synthesized materials resulted in a catalyst nanostructure, and ordered pore diameter and surface area according to existing literature. The oily sludge sample was characterized by determining the API gravity and sulfur content and SARA analysis (saturates, aromatics, resins and asphaltenes). The results showed a material equivalent to the average oil with API gravity of 26.1, a low sulfur content and considerable amount of resins and asphaltenes, presented above in the literature. The thermal and catalytic degradation of the oily sludge oil was performed from room temperature to 870 ° C in the ratios of heating of 5...

Síntese, caracterização e aplicação de MCM-41 funcionalizado com diisopropilamina no processo de adsorção do dióxido de carbono

Barbosa, Marcela Nascimento
Fonte: Universidade Federal do Rio Grande do Norte; BR; UFRN; Programa de Pós-Graduação em Química; Físico-Química; Química Publicador: Universidade Federal do Rio Grande do Norte; BR; UFRN; Programa de Pós-Graduação em Química; Físico-Química; Química
Tipo: Dissertação Formato: application/pdf
POR
Relevância na Pesquisa
59.925%
Emissions of CO2 in the atmosphere have increased successively by various mechanisms caused by human action, especially as fossil fuel combustion and industrial chemical processes. This leads to the increase in average temperature in the atmosphere, which we call global warming. The search for new technologies to minimize environmental impacts arising from this phenomenon has been investigated. The capture of CO2 is one of the alternatives that can help reduce emis ions of greenhouse gases. The CO2 can be captured through the process of selective adsorption using adsorbents for this purpose. Were synthesized by hydrothermal method, materials of the type MCM-41 and Al-MCM-41 in the molar ratio Si / Al equal to 50. The synthesis of gels were prepared from a source of silicon, sodium, water and aluminum in the case of Al-MCM-41. The period of synthesis of the materials was 5 days in autoclave at 100°C. After that time materials were filtered, washed and dried in greenhouse at 100 º C for 4 hours and then calcined at 450 º C. Then the calcined material was functionalized with the Di-isopropylamine (DIPA) by the method of wet impregnation. We used 0.5 g of material mesopores to 3.5 mL of DIPA. The materials were functionalized in a closed container for 24 hours...

Síntese e caracterização de materiais nanoporosos para pirólise catalítica de óleos pesados

Costa, Maria José Fonseca
Fonte: Universidade Federal do Rio Grande do Norte; BR; UFRN; Programa de Pós-Graduação em Química; Físico-Química; Química Publicador: Universidade Federal do Rio Grande do Norte; BR; UFRN; Programa de Pós-Graduação em Química; Físico-Química; Química
Tipo: Dissertação Formato: application/pdf
POR
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The present work reports the study of nanoporous structures, aiming at their use in research directed to the current demand of the petroleum industry to value heavy oil. Initially, two ways were chosen for the synthesis of porous structures from the molecular sieves of type Si-MCM-41. In the first way, the structure MCM-41 is precursory for heteroatom substitutes of silicon, generating catalyst of the type Al-MCM-41 from two different methods of incorporation of the metal. This variation of the incorporation method of Aluminum in the structure of Si-MCM-41 was carried out through the conventional procedure, where the aluminum source was incorporated to the gel of synthesis, and the procedure post-synthesis, where the Aluminum source was incorporated in catalyst after the synthesis of Si-MCM-41. In the second way, the MCM-41 acts as a support for growth of nanocrystals of zeolite embedded in their mesoporous, resulting in hybrid MCM-41/ZSM-5 catalyst. A comparative analysis was carried through characterizations by XRD, FTIR, measures of acidity through n-butylamine adsorption for TGA, SEM-XRF and N2 adsorption. Also crystalline aluminosilicate with zeolitic structure MFI of type ZSM-5 was synthesized without using organic templates. Methodologies to the preparation of these materials are related by literature using conventionally reactants that supply oxides of necessary silicon and aluminum...

Síntese, caracterização e aplicação do MCM-41 e A1-MCM-41 na pirólise do resíduo atmosférico de petróleo

Castro, Kesia Kelly Vieira de
Fonte: Universidade Federal do Rio Grande do Norte; BR; UFRN; Programa de Pós-Graduação em Química; Físico-Química; Química Publicador: Universidade Federal do Rio Grande do Norte; BR; UFRN; Programa de Pós-Graduação em Química; Físico-Química; Química
Tipo: Dissertação Formato: application/pdf
POR
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90.1435%
In present work, mesoporous materials of the M41S family were synthesized, which were discovered in the early 90s by researchers from Mobil Oil Corporation, thus allowing new perspectives in the field of catalysis. One of the most important members of this family is the MCM-41, which has a hexagonal array of mesopores with pore diameters ranging from 2 to 10 nm and a high surface area, enabling it to become very promising for the use as a catalyst in the refining of oil in the catalytic cracking process, since the mesopores facilitate the access of large hydrocarbon molecules, thereby increasing the production of light products, that are in high demand in the market. The addition of aluminum in the structure of MCM-41 increases the acidity of the material, making it more beneficial for application in the petrochemical industry. The mesoporous materials MCM-41 and Al-MCM-41 (ratio Si / Al = 50) were synthesized through the hydrothermal method, starting with silica gel, NaOH and distilled water. CTMABr was used as template, for structural guiding. In Al-MCM-41 the same reactants were used, with the adding of pseudoboehmite (as a source of aluminum) in the synthesis gel. The syntheses were carried out over a period of four days with a daily adjustment of pH. The optimum conditions of calcination for the removal of the organic template (CTMABr) were discovered through TG / DTG and also through analysis by XRD...

Estudo cinético da degradação térmica e catalítica de petróleo pesado usando Al-MCM-41

Oliveira, Aline Araújo Alves de
Fonte: Universidade Federal do Rio Grande do Norte; BR; UFRN; Programa de Pós-Graduação em Química; Físico-Química; Química Publicador: Universidade Federal do Rio Grande do Norte; BR; UFRN; Programa de Pós-Graduação em Química; Físico-Química; Química
Tipo: Tese de Doutorado Formato: application/pdf
POR
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The mesoporous nanostructured materials have been studied for application in the oil industry, in particular Al-MCM-41, due to the surface area around 800 to 1.000 m2 g-1 and, pore diameters ranging from 2 to 10 nm, suitable for catalysis to large molecules such as heavy oil. The MCM-41 has been synthesized by hydrothermal method, on which aluminum was added, in the ratio Si/Al equal to 50, to increase the generation of active acid sites in the nanotubes. The catalyst was characterized by X-ray diffraction (XRD), surface area by the BET method and, the average pore volume BJH method using the N2 adsorption, absorption spectroscopy in the infrared Fourier Transform (FT-IR) and determination of surface acidity with application of a probe molecule - n-butylamine. The catalyst showed well-defined structural properties and consistent with the literature. The overall objective was to test the Al-MCM-41 as catalyst and thermogravimetric perform tests, using two samples of heavy oil with API º equal to 14.0 and 18.5. Assays were performed using a temperature range of 30-900 ° C and heating ratios (β) ranging from 5, 10 and 20 °C min-1.The aim was to verify the thermogravimetric profiles of these oils when subjected to the action of the catalyst Al- MCM-41. Therefore...

VAPOR-PHASE CATALYTIC CONVERSION OF ETHANOL INTO 1,3-BUTADIENE ON Cr-Ba/MCM-41 CATALYSTS

La-Salvia,N.; Lovón-Quintana,J. J.; Valença,G. P.
Fonte: Brazilian Society of Chemical Engineering Publicador: Brazilian Society of Chemical Engineering
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/06/2015 EN
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AbstractAl-MCM-41, 16%Ba/Al-MCM-41 and 1.4%Cr-16%Ba/Al-MCM-41 were used as catalysts in the vapor-phase catalytic conversion of ethanol. Physical-chemical properties of the catalysts and the effect of barium and chromium on the Al-MCM-41 activity and 1,3-butadiene yield were studied. The catalysts were characterized by X-ray diffraction (XRD), N2 physisorption (BET method), CO2chemisorption and Fourier transform infrared spectroscopy (FT-IR). When ethanol was completely converted on Al-MCM-41 and 16%Ba/Al-MCM-41, the reaction products showed a high selectivity for ethylene (90-98%). However, on the 1.4%Cr-16%Ba/Al-MCM-41 catalyst, a greater number of reaction products were obtained such as ethylene, acetaldehyde, diethyl ether and 1,3-butadiene. The maximum 1,3-butadiene yield obtained from ethanol reaction was 25% at 723 K and W/FEtOH = 15 g h mol-1. The latter result was obtained in a single step and without addition of reaction promoters (e.g., acetaldehyde, crotonaldehyde, hydrogen) in the feed stream to the reactor.