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Doctoral Thesis
DOI
https://doi.org/10.11606/T.3.2022.tde-05092022-101237
Document
Author
Full name
Kleber Bitencourt Vaccioli
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Paulo, 2022
Supervisor
Committee
Valera, Ticiane Sanches (President)
Silva, Leonardo Gondim de Andrade e
Calvão, Patrícia Schmid
Drumond, Walker Soares
Esper, Fábio José
Title in Portuguese
Efeito da adição de sílica, óxido de grafeno e agentes organossulfurados na vulcanização e nas propriedades de compostos baseados em borracha natural.
Keywords in Portuguese
Borracha
Grafeno
Materiais compósitos
Polímeros (Materiais)
Sílica
Abstract in Portuguese
Neste trabalho foram obtidos compostos vulcanizados de borracha natural (NR) com adição de dois tipos de carga, sílica amorfa comercial e partículas de óxido de grafeno (GO) obtidas a partir da grafita, e dois tipos de agentes organossulfurados, o tetrassulfeto de bis(trietoxisililpropil) (TESPT) e o 4,4- ditiodimorfolina (DTDM). A borracha natural foi obtida por meio da coagulação do látex de NR originário da Malásia. As cargas foram adicionadas à borracha natural por dois métodos: a) inseridas em dispersão aquosa diretamente no látex, antes da etapa de coagulação; b) inseridas na borracha natural seca por mistura mecânica. Assim, o trabalho foi dividido em duas etapas: na primeira, avaliou-se a síntese e caracterização do óxido de grafeno. Na segunda estudou-se a vulcanização e as propriedades mecânicas de compósitos de NR. Nesse estudo, foi investigado, inicialmente, o efeito dos agentes organossulfurantes, individualmente, no composto de NR. A seguir, foi investigado o efeito das cargas sobre os compostos de NR. Por fim avaliou-se o efeito da presença simultânea das cargas e dos agentes nos compostos. As partículas de GO foram caracterizadas por FTIR, AFM-IR, MEV, DRX e espectroscopia Raman. Os resultados indicaram a presença de grupos oxigenados nas partículas de GO, as quais apresentaram folhas nano e micrométricas, com espessuras nanométricas. Os parâmetros de vulcanização do composto de NR e dos compósitos foram obtidos por reometria de disco oscilatório (ODR). As propriedades físicas e químicas foram obtidas por DSC, TGA e FTIR. A morfologia e a composição química dos compósitos foram analisadas por MEV e EDS e as propriedades mecânicas determinadas por ensaios de resistência à tração, resistência ao rasgo e dureza. Os resultados indicaram que a adição de DTDM aumenta a taxa de vulcanização, os valores de resistência à tração, de módulo e de resistência ao rasgo, quando comparados aos valores obtidos para o composto de NR. Estes efeitos foram mais pronunciados com a adição simultânea de sílica e DTDM. Por outro lado, a adição de TESPT não afetou significativamente a vulcanização e as propriedades do composto de NR, mesmo em presença das cargas.
Title in English
Effect of the addition of silica, graphene oxide, and organosulfur agents on the vulcanization and properties of natural rubberbased compounds.
Keywords in English
Composite
DTDM
Graphene oxide
Natural rubber
Silica
TESTP
Abstract in English
In this work, vulcanized compounds of natural rubber (NR) were obtained with the addition of two types of fillers, commercial amorphous silica, and graphene oxide(GO) obtained from graphite, and two types of organosulfur agents, bis(triethoxysilylpropyl) (TESPT) and 4,4-dithiodimorpholine (DTDM). Natural rubber was obtained by coagulating NR latex. The fillers were added to the natural rubber by two methods: a) in an aqueous dispersion directly into the latex, before the coagulation step; b) into dry natural rubber by mechanical mixing. The work was divided in two stages: firstly, the synthesis and characterization of graphene oxide were evaluated. Secondly, the vulcanization and properties of NR composites were studied. In this stage, the effect of the organosulfur agents, individually, on the NR compound, was initially investigated. Next, the effect of the fillers on NR compounds was investigated. Finally, the effect of the simultaneous presence of fillers and agents in the compounds was evaluated. The GO particles were characterized by FTIR, AFM-IR, SEM, XRD, and Raman spectroscopy. The results indicated the presence of oxygenated groups in the GO particles that presented nano and micrometric sheets, with nanometric thicknesses. The vulcanization parameters of the NR compounds and composites were obtained by oscillating disk rheometry (ODR). Physical and chemical properties were obtained by DSC, TGA and FTIR. The morphology and chemical composition of the composites were analyzed by SEM and EDS and the mechanical properties determined by tensile and tear strength, and hardness tests. The results indicated that the addition of DTDM increases the vulcanization rate, the values of tensile strength, modulus, and tear strength, when compared to the values obtained for the NR compound. These effects were more pronounced with the simultaneous addition of silica and DTDM. On the other hand, the addition of TESPT did not significantly affect the vulcanization and properties of NR compound, even in the presence of fillers.
 
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Publishing Date
2022-09-06
 
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