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Thesis--University of Florida. / Description based on print version record. Typescript. Vita. Includes bibliographical references (leaves 90-93).

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Thesis (Ph. D.)--Institute of Paper Chemistry, 1973. / Includes bibliographical references (p. 137-142).

Orientador: Heloise de Oliveira Pastore / Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Química / Made available in DSpace on 2018-08-24T05:33:50Z (GMT). No. of bitstreams: 1 Vieira_RomuloBatista_M.pdf: 2977230 bytes, checksum: 57a4048c4901f10fbcf41751f5c96040 (MD5) Previous issue date: 2013 / Resumo: A síntese dos silicatos lamelares bem como as modificações com polietilenimina (PEI) foram confirmadas através de difração de raios-X (DRX), espectroscopia no infravermelho (FT-IR), ressonância magnética nuclear (RMN) de C e Si. Modificações do tipo não covalentes (intercalação) e covalentes (reação de sililação) nos silicatos lamelares foram realizadas com PEI de forma sintetizar um novo tipo de adsorvente que tenha boas propriedades para a adsorção de CO2. Diversas metodologias para a modificação de PEI foram propostas e todas conseguiram ligar covalente ou não-covalentemente a PEI nas lamelas da magadiita. Verificou-se uma relação entre a concentração de íons hexadeciltrimetilamônio (CTA) presentes e a eficiência no grau de funcionalização de grupos cloropropil na magadiita. Quando realizou-se troca iônica com a PEI protonada, os melhores de resultados foram obtidos em pH 9, sugerindo que as aminas terciárias presentes na PEI foram protonada primeiramente. Através da dessorção à temperatura programada de CO2 (TPD-CO2) para os materiais estudados: magadiita impregnada com PEI (MAG-PEIx) e magadiita trocada com CTA na razão molar de 25 % (25CTA-MAG-PEIx); foi possível identificar a presença de dos sítios de adsorção presentes na PEI: camada exposta de PEI e PEI bulk, além de mostrar que o modelo de adsorção segue o modelo de subsuperfície. Os resultados de TPD-CO2 tiveram suas curvas de dessorção ajustadas ao modelo cinético de Avrami, apresentando uma boa correlação e mostrando que há interações diferentes entre o adsorvente (aminas primárias, secundárias e grupos Si-OH) e o CO2. Os melhores resultados de adsorção mostraram uma capacidade de 6,11 mmol g, na temperatura de adsorção de 75 °C, durante 3 h. / Abstract: The syntheses of layered silicates as well as changes in PEI were confirmed by X-ray diffraction (XRD), infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR) C and Si. Non-covalent modifications of the type (intercalation) and covalent (silylation reaction) in the layer silicates were performed with polyethylenimine (PEI) in order to synthesize a new type of adsorbent that has good properties for the adsorption of CO2. Several methodologies for modification of PEI have been proposed and succeeded to bind covalent or non-covalent into the interlayer space of magadiite. There was a relationship between the concentration of hexadecyltrimethylammonium ions (CTA) present and the efficiency in the degree of functionalization of the magadiite chloropropyl groups. When the ion exchange was carried out with the protonated PEI, the best results were obtained at pH 9, suggesting that the tertiary amines are protonated first. CO2-TPD for the materials studied: magadiite impregnated with PEI (MAG-PEIx) and magadiite exchanged with CTA at molar ratio 25% (25CTA-MAG-PEIx) was possible to identify the presence of different adsorption sites present in PEI: exposed layer of PEI and PEI bulk, and show that the adsorption model follows the subsurface model. The results of the desorption curves was fitted by Avrami kinetic model, showing a good correlation and revealing different interactions between the adsorbent (primary, secondary and Si-OH groups) and CO2. The best results showed adsorption capacity of 6.11 mmol g, at 75 ° C for 3h. / Mestrado / Quimica Inorganica / Mestre em Química

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第22162号 / 工博第4666号 / 新制||工||1728(附属図書館) / 京都大学大学院工学研究科化学工学専攻 / (主査)教授 宮原 稔, 教授 山本 量一, 教授 松坂 修二 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DGAM

To extend the time of service of asphalt roads modified montmorillonite nanoparticles were incorporated into bitumen with the aim of creating a gas barrier inside the bitumen which slows down the diffusion of oxygen through the bitumen. For this purpose [montmorillonite/alkyl-quat-primer] adducts ([MMT/PEI(nkD)xQyR]) were fabricated in which single-montmorillonite platelets were coated by a ultrathin polymer film by reacting montmorillonite particles with poly(ethylenimine) based polycations. The alkyl-quat-primer polymers were synthesised by adding ammonium groups and alkyl chains to hyperbranched poly(ethylenimine)s in a solvent-free reaction. Adducts with fully intercalated polymers were obtained when the polymers were reacted with an aqueous solution of [MMT/CTAB] or by mixing the polymers with montmorillonite and CTAB in an aqueous solution. The polymers replaced the CTAB in an intermediate formed [MMT/CTAB] adduct and adhered strongly to the montmorillonite due to a cooperative electrostatic interaction between the positively charged ammonium moieties of the macromolecules and the negatively charged montmorillonite surface. [MMT/alkyl-quat-primer] and [MMT/CTAB] adducts were incorporated via a single screw extruder into polymer- and non-polymer-modified bitumina to create bitumen-nanocomposites. Composites prepared under optimised conditions exhibited an adduct network inside the bitumen at adduct concentrations larger 5 wt.% and when non-polymer modified bitumina were modified. The aspect ratio of the incorporated montmorillonite platelets depended strongly on the adduct composition and the used bitumen, and was with [MMT/PEI(10kD)10Q80R10] adducts were very high (~ 300 - 1000) but with [MMT/PEI(10kD)10Q60R14] and [MMT/CTAB] adducts considerably lower (~ 30 - 90).

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