In this study, 20/80 (weight %) Poly(ethylene terephthalate) (PET) /High Density Polyethylene (HDPE) Microfibrillar Reinforced Composites (MFC) were prepared by using high density polyethylene (HDPE) as the matrix material, poly(ethylene terephthalate) (PET) as the reinforcing component. Ethylene n-butyl acrylate-glycidyl methacrylate (E-nBA-GMA) and ethylene methyl acrylate (E-MA) as the compatibilizers in 1, 5, and 10 wt. %. The objective of this study is to produce MFCs based on PET and HDPE via extrusion-drawing-injection method and to characterize as extruded, as drawn and injection molded materials in terms of morphologies, and mechanical and thermal properties. In addition, the effect of compatibilizer type and content on properties of PET-HDPE composites was studied. For comparison purposes, conventional PET-HDPE composites with and without compatibilizer were prepared. Also, the effect of screw speed and drawing speed on the morphologies and mechanical and thermal properties were investigated. The effect of low and high injection temperature molding on morphologies were also observed. SEM analyses showed that, extruded blends became oriented after drawing. The fibrillar structure was preserved after injection molding. High injection molding temperature destroyed the structure of PET microfibers. In addition, it was also observed that the adhesion between HDPE and PET improved with the addition of the compatibilizers. Tensile strength and tensile modulus values of PET/HDPE MFCs increased with increasing drawing speed. Increasing the screw speed resulted in a slight decrease in tensile strength values. Addition of the compatibilizers to the system decreased tensile strength and tensile modulus values. Results of impact tests designated that the impact strength of the materials with and without MFC structure increased with the increasing amounts of E-nBAGMA. DSC analyses pointed out that, melting temperatures of HDPE and PET phase did not change significantly with increasing drawing speed or with the addition of the compatibilizer. As the drawing speed increased from 2.7 m/min to 6.2 m/min, degree of crystallinity of the drawn samples of the PET phase increased.

The objectives of this study are to synthesize sub-micron sized zinc borate and to use them with other flame retardant additives in poly(ethylene terephthalate) (PET) based composites. The study can be divided into two parts. In the first part, it was aimed to synthesize sub-micron sized zinc borate (2ZnO.3B2O3.3.5H2O) with the reaction of zinc oxide and boric acid. For this purpose, low molecular weight additives or surfactants were used in the syntheses to prevent the agglomeration and to decrease particle size. Effect of type of surfactant and its concentration / effect of using nano-sized zinc oxide as reactant on the synthesis, properties and morphology of 2ZnO.3B2O3.3.5H2O were investigated. Synthesized zinc borates were characterized by X-Ray diffraction (XRD), Scanning Electron Microscope (SEM) and Thermogravimetric Analysis (TGA). The results were compared with a commercial zinc borate, Firebrake (FB). Characterization results showed that at least in one dimension sub-micron size was obtained and synthesized zinc borates did not lose their hydration water until the process temperature of the composites. In the second part of the study, PET based composites, which mainly included synthesized sub-micron sized zinc borates were prepared by using a co-rotating twin screw extruder and injection molding machine. Synergist materials such as boron phosphate (BP) and triphenyl phosphate (TPP) were also used in the composite preparation. The composites were characterized in terms of flammability and mechanical properties. Flammability of composites was determined by using a Limiting Oxygen Index (LOI) test. Mechanical properties such as tensile strength, elastic modulus, elongation at break and impact strength were also studied. According to LOI and impact tests, the composites containing 3 wt. % BP and 2 wt. % zinc borate which was modified with poly(styrene-co-maleic anhydride), 2PSMA05/3BP and 2PSMA1/3BP have higher LOI and impact values when compared to neat PET.

Visco-elastic behaviour at the nano-level of a commonly used polymer (PET) is characterised using atomic force microscopy (AFM) at a range of temperatures. The modulus, indentation creep and relaxation time of the PET film (thickness = 100 m) is highly sensitive to temperature over an experimental temperature range of 22¿175 ¿C. The analysis showed a 40-fold increase in the amount of indentation creep on raising the temperature from 22 ¿C to 100 ¿C, with the most rapid rise occurring above the glass-to-rubber transition temperature (Tg = 77.1 ¿C). At higher temperatures, close to the crystallisation temperature (Tc = 134.7 ¿C), the indentation creep reduced to levels similar to those at temperatures below Tg. The calculated relaxation time showed a similar temperature dependence, rising from 0.6 s below Tg to 1.2 s between Tg and Tc and falling back to 0.6 s above Tc. Whereas, the recorded modulus of the thick polymer film decreases above Tg, subsequently increasing near Tc. These visco-elastic parameters are obtained via mechanical modelling of the creep curves and are correlated to the thermal phase changes that occur in PET, as revealed by differential scanning calorimetry (DSC).

This study was conducted to investigate the effects of component concentrations and addition order of the components, on the final properties of ternary nanocomposites composed of poly(ethylene terephthalate), organoclay, and an ethylene/methyl acrylate/glycidyl methacrylate (E-MA-GMA) terpolymer acting as an impact modifier for PET. In this context, first, the optimum amount of the impact modifier was determined by melt compounding binary PET-terpolymer blends in a corotating twin-screw extruder. The amount of the impact modifier (5 wt. %) resulting in the highest Young&rsquo / s modulus and reasonable elongation at break was selected owing to its balanced mechanical properties. Thereafter, by using 5 wt. % terpolymer content, the effects of organically modified clay concentration and addition order of the components on ternary nanocomposites were systematically investigated. Mechanical testing revealed that different addition orders of the materials significantly affected mechanical properties. Among the investigated addition orders, the best sequence of component addition (PI-C) was the one in which poly(ethylene terephthalate) was first compounded with E-MA-GMA. Later, this mixture was compounded with the organoclay in the subsequent run. Young&#039 / s modulus of not extruded pure PET increased by 67% in samples with 5 wt. % E-MA-GMA plus 5 wt. % clay loading. The highest percent elongation at break was obtained as 300%, for the addition order of PI-C, with 1 wt. % clay content, which is nearly 50 fold higher than that obtained for pure PET. In X-ray diffraction analysis, extensive layer separation associated with delamination of the original clay structure occurred in PI-C and CI-P sequences with both 1 and 3 wt. % clay contents. X-ray diffraction patterns showed that, at these conditions exfoliated structures resulted as indicated by the disappearence of any peaks due to the diffraction within the consecutive clay layers.

Polymeric composites are any of the combinations or compositions that comprise two or more materials as separate phases, at least one of which is a polymer. By mixing a polymer with another material, such as glass, carbon, or another polymer, it is often possible to improve the desired properties of the polymer. In this study, ternary composites were prepared by using recycled poly(ethylene terephthalate), PET as the matrix material, short glass fiber (SGF) as the reinforcing filler and thermoplastic elastomer as the impact modifier. Bottle grade recycled PET was mixed in a twin screw extruder with a thermoplastic elastomer which is a terpolymer of ethylene/methyl acrylate/glycidyl methacrylate (E-MA-GMA), and E type short glass fiber is fed to the extruder from a side feeder. During this study, recycled PET was mixed with from 10 to 50 wt. % elastomer, and SGF was added to the system in the range from 10 to 40 % by weight. Processing parameters were kept constant during extrusion. The composites were then compression molded for characterization experiments. The produced composites were characterized in terms of their mechanical and thermal properties and morphologies. Melt behavior and fiber length distribution of the composites were also determined for selected composites. In ternary systems with 10 % elastomer, highest tensile strength values were observed. High tensile and flexural moduli values were obtained for the composites containing 20 % elastomer. Results of impact tests designated that impact strength increased significantly after 30 % elastomer content. Thermal analyses of the composites were done by using a DSC (Differential Scanning Calorimeter). Degree of crystallinity of ternary system decreased with increasing elastomer content, but melting points of the composites were not affected significantly. SEM micrographs showed that the adhesion between the matrix and fiber increased considerably with elastomer addition.

Thesis (Ph. D.)--Ohio State University, 2007. / Title from first page of PDF file. Includes bibliographical references (p. 208-232).

Submitted by TAYANE WESTERMANN LOPES CASTILHO null (tayanewest@uol.com.br) on 2018-01-26T16:12:01Z No. of bitstreams: 1 Dissertação Tayane Westermann Lopes Castilho.pdf: 4997047 bytes, checksum: c0457ac97bc5e87fd929dbe70703dd0d (MD5) / Approved for entry into archive by Maria Marlene Zaniboni null (zaniboni@bauru.unesp.br) on 2018-01-26T18:07:08Z (GMT) No. of bitstreams: 1 castilho_twl_me_bauru.pdf: 4997047 bytes, checksum: c0457ac97bc5e87fd929dbe70703dd0d (MD5) / Made available in DSpace on 2018-01-26T18:07:08Z (GMT). No. of bitstreams: 1 castilho_twl_me_bauru.pdf: 4997047 bytes, checksum: c0457ac97bc5e87fd929dbe70703dd0d (MD5) Previous issue date: 2017-12-18 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Este trabalho avaliou a influência da inclusão de fibras recicladas extraídas de garrafas constituídas de politereftalato de etileno (PET) na resistência ao cisalhamento de solos arenoso e argiloso. Por meio de ensaios de compressão simples das amostras dos solos e misturas desses com diferentes teores e comprimentos de fibras, obteve-se que a combinação de 1,5% de fibras, em relação à massa de solo seco, com comprimento de 20 mm levou a um aumento de 92,8% na resistência não confinada para a amostra de solo arenoso, e de 10,5% para a de solo argiloso. Ensaios de cisalhamento direto foram realizados com essa dosagem, em duas diferentes condições de compactação, e revelam o ganho de 66,4% no intercepto de coesão para o solo arenoso com grau de compactação de 100%, e de 55,5% com grau de compactação de 95%, em relação ao solo sem fibra. Enquanto os ângulos de atrito interno praticamente não se alteraram. A mesma dosagem para o solo argiloso promoveu reduções de coesão de 7,6% e 5,4%, respectivamente, para os graus de compactação de 100% e de 95% e aumentos relativos de 2,9% e 7,3% no ângulo de atrito interno. Esses resultados aplicados em dois casos hipotéticos, capacidade de carga de fundações em sapatas e estabilidade de taludes de aterros, demonstram o efeito da inclusão de fibras na melhoria da estimativa da capacidade de carga para ambos os solos e o aumento do fator de segurança para o solo arenoso. O trabalho oferece uma alternativa tecnicamente viável para a melhoria dos solos e que prioriza o reuso de garrafas PET, colaborando para preservação ambiental, mas não só, pois a atividade promove ainda benefícios sociais e econômicos. / This study presents an analysis of the influence of the inclusion of polyethylene terephthalate (PET) fibers, extracted from waste plastic bottles, in the shear strength of sandy and clayey soils. Simple compression tests were performed with soil samples and mixtures of these with different fiber contents and lengths. The combination of 1,5% of fibers in relation to the dry soil mass with a length of 20 mm led to a 92.8% increase in the unconfined resistance for the sandy soil sample and 10.5% for the clayey soil sample. Direct shear tests were carried out with this dosage, with two different compaction conditions, showing the gain of 66.4% in the cohesion intercept for sandy soil with 100% compaction degree, and 55.5% with the degree of 95%, in relation to the soil without fiber. While the angles of internal friction remained almost constant. The same dosage for clayey soil promoted cohesion reductions of 7.6% and 5.4%, respectively, for compaction degrees of 100% and 95% and relative increases of 2.9% and 7.3% in the angle of internal friction. These results, applied in two hypothetical cases, load capacity of an isolated footing foundation and slope stability of landfills, demonstrate the effect of the inclusion of fibers in improving the estimation of the load capacity for both soils and the increase of the safety factor for the sandy soil. The study offers a technically feasible alternative for the improvement of soils, and that prioritizes the reuse of PET bottles, collaborating for environmental preservation, but not only, since the activity also promotes social and economic benefits.

Nesse trabalho foi analisada a viabilidade da utilização de poli(tereftalato de etileno) reciclado, PET, como agente de contenção de areia, utilizando o PET virgem e o poli(óxido de metileno), POM, para comparação. As amostras recebidas foram caracterizadas utilizando ressonância magnética nuclear de carbono-13 (13C-NMR), calorimetria diferencial de varredura (DSC), análise termogravimétrica (TG), microscopia eletrônica de varredura (SEM) e cromatografia de exclusão por tamanho (SEC). Também foram realizados ensaios mecânicos para avaliação da permeabilidade de um pacote de grãos, segundo as normas API RP 61 e API RP 58. Dessa forma, uma quantidade pré-definida dos polímeros granulados foi confinada separadamente em células cilíndricas metálicas, juntamente com substâncias normalmente utilizadas no tratamento de formações portadoras de hidrocarbonetos (como HCl a 15%, Dietileno-triamino-penta-acetato de potássio a 10 % e mistura de solventes, tais como xileno 45 %, óleo diesel 45 % e butilglicol 10 %) e também a petróleo e água do mar. As amostras foram submetidas a temperatura e pressão constantes, além de agitação por rotação, na temperatura de 70 C e na pressão de 24,1 MPa. Os ensaios duraram de 24 a 96 horas para os produtos químicos mais agressivos e 172 dias para a água do mar e o petróleo. Para os testes mais longos, foram coletadas amostras periodicamente, a fim de se verificar as condições de cada polímero, utilizando as técnicas anteriormente citadas, com exceção de 13C-NMR. A permeabilidade foi analisada ao final do período de exposição previsto. Os resultados obtidos foram comparados com os observados para os polímeros não-expostos, sendo constatada a degradação do POM quando em contato com HCl a 15 %, mas sem observar variações significativas que indicassem a degradação apreciável de qualquer dos tipos de PET nas condições testadas, sendo concluído que a utilização do PET reciclado como agente de contenção de areia é viável. / This work analyses the viability of applying recycled poly(ethylene terephthalate), PET, as sand control agent, using virgin PET and poly(methylene oxide), POM, for comparison means. The polymer samples were characterized by carbon-13 magnetic nuclear resonance (13C-NMR), differential scanning calorimetry (DSC), thermal gravimetric analysis (TG), scanning electronic microscopy (SEM) and size exclusion chromatography (SEC). Also, mechanical experiments were performed, in order to determine the grain pack permeability, according to API RP 61 and API RP 58. In this way, a predefined amount of polymer grains were separately confined into cylindrical metallic cells, with substances commonly used to treat hydrocarbon formations (15 % HCl, 10 % potassium diethylene triamine pentaacetate and a solvent mixture, like xylene 45 %, diesel oil 45 % and EGMBE 10 %) and sea water and petroleum, likewise. The samples were submitted to a temperature of 70oC, a pressure of 24,1 MPa, which were maintained constant. Cell rotational agitation did not varied in the experiments. The exposure time was 24 and 96 hours, for the aggressive chemical products, and 172 days for sea water and oil. During the latter period, samples were periodically collected to test the polymer conditions, using all the above techniques, but the 13C-NMR. The pack permeability was analyzed only by the end of each established exposition period. The test results were compared to those obtained to non-exposed polymers and they have shown that POM was degraded by 15 % HCl. On the other hand, PET samples did not present significant changes under test conditions. Therefore, it has being concluded that the use of recycled PET as sand control agent is viable.

[pt] A presente pesquisa tem como objetivo avaliar o comportamento de misturas asfálticas do tipo CBUQ (Concreto Betuminoso Usinado a Quente) adicionadas com garrafas PET (Polietileno Tereftalato) trituradas em diferentes granulometrias e teores. O filer convencional (pó de pedra) utilizado em misturas asfálticas foi substituído pelo pó proveniente da moagem das garrafas PET, já que o seu elevado ponto de fusão permite a utilização como agregado na mistura. Portanto, foi utilizado o material triturado nos diâmetros 10 mm e 2 mm, nos teores de 0,5 porcento e 1,0 porcento adicionadas ao CBUQ e, também, a substituição de 2,5 porcento do pó de pedra por pó de PET, juntamente com a adição de 0,5 porcento de PET triturado no diâmetro de 10 mm. A partir dos ensaios de caracterização dos agregados (granulometria, durabilidade, densidade, massa específica e abrasão Los Angeles) e do ligante asfáltico CAP 30/45 (densidade específica, penetração, ponto de amolecimento, ductilidade, solubilidade em tricloroetileno e envelhecimento em estufa de filme rotativo), foram feitas as dosagens das misturas asfálticas, pelo método Marshall, e a confecção de corpos de prova, o que possibilitou a realização dos ensaios mecânicos de estabilidade e fluência Marshall, resistência à tração, módulo de resiliência e de vida de fadiga. A inserção de PET triturado às misturas de CBUQ foi satisfatória, sendo os resultados dependentes dos teores e das granulometrias das partículas de PET utilizados. Observa-se que o incremento nos parâmetros de resistência e na vida útil das misturas estudadas foi mais efetivo para o CBUQ com 0,5 porcento de PET triturado em 10 mm e com a substituição de 2,5 porcento do filer por pó de PET, na sua composição granulométrica. Portanto, o uso de resíduos de garrafas PET para o melhoramento de misturas asfálticas pode minimizar os problemas atuais disposição do resíduo, contribuir com a redução do consumo de recursos naturais e dar um uso nobre para este material. / [en] This research aims to evaluate the behavior of HMA mixtures (hot mix asphalt concrete) added with PET (Polyethylene Terephthalate) bottles pounded into different particle sizes and concentrations in the mixture. The usual filler (stone dust) was replaced by the powder from the milling of PET bottles, since its high melting point allows the use as an aggregate in the mix. Thus, it was used the material in diameters of 10 mm and 2 mm, in concentrations of 0.5 percent and 1.0 percent added in the HMA and, also, the replacement of 2.5 percent of the stone powder for the PET powder with addition of 0.5 percent triturated with diameter of 10 mm. From the characterization tests of aggregates (particle sizes, durability, density, Los Angeles abrasion) and asphalt (specific density, penetration, softening point, ductility, solubility in trichloroethylene, RTFOT – rolling thin film oven test), it was made the calculations of the dosage by the Marshall method, production of specimens, which enabled the realization of mechanical tests of Marshall Stability and Flow, Tensile Strength, Resilient Modulus and Fatigue. The insertion of triturated PET was satisfactory, being dependent on the results of the percentages and particle sizes of the PET used. It was observed that the increase in the strength parameters and the useful life of the mixtures studied is more effective for the HMA with 0.5 percent PET of 10 mm diameter and the substitution of 2.5 percent of the filler for PET powder in its granulometric compositions. Therefore, the use of PET bottle waste to the improvement of asphalt mixtures can minimize the current problems of waste disposal, contribute to reduce the consumption of natural resources and make a noble use for this material.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / O Tereftalato de Polietileno PET é um termoplástico polar,com elevada estabilidade dimensional e temperatura de fusão, alta impermeabilidade a gases e resistência química a ácidos e solventes, empregado na fabricação de garrafas no Brasil. A biodegradação tem sido descrita como uma possível metodologia para reduzir o acúmulo de plásticos. Neste trabalho foi avaliado o desempenho das linhagens de Bacillus subtilis e Phanerochaete chrysosporium isoladamente na biodegradação do tereftalato de polietileno. Neste sentido, foram preparadas partículas do polímero sendo submetidas aos tratamentos com luz ultra violeta (6 e 36 horas) e temperaturas (35C e 50C) em seguida, foram colocadas nos meios caldo nutriente (B.subtilis) e Sabouraud (P. chrysosporium), incubados por 30 e 60 dias, incubados a 35C e 28C, respectivamente. Com a degradação das partículas observou-se que o pH passou de 5 para >8, com formação de biofilmes e indução da produção de enzimas (amilase, protease, esterase e polifenoloxidases). A formação do biofilme foi evidenciada por microscopia eletrônica de varredura. Os produtos metabólicos formados no meio de cultura foram avaliados pelo teste de toxicidade utilizando Artemia salina. A microscopia eletrônica demonstrou que B. subtilis colonizou completamente a superfície das partículas do PET, tanto nas condições controle (sem tratamento), como tratados. Os melhores resultados foram observados com o tratamento à temperatura de 50C, onde ocorreu alteração na superfície do polímero, perda da massa polimérica, permitindo maior colonização de ambos os microrganismos. As enzimas hidrolíticas foram produzidas pelos microrganismos em todos os tratamentos, em especial, à temperatura de 50C. Contudo, observou-se que B. subtilis não produziu polifenoloxidases. Os subprodutos da degradação do PET nas condições estudadas apresentaram alta toxicidade para Artemia salina no caso do P. chrysosporium e baixa toxicidade para B. subtilis. Os resultados obtidos sugerem o tratamento o prévio com a temperatura de 50C como importante para o processo de biorremediação / In recent years, the consumption of the poly ethylene terephtalate plastic - PET is used in the manufacture of bottles, comes increasing in Brazil. PET is a polar thermoplastic, with raised dimensional stability and temperature of fusion, high impermeability the acid gases and chemical resistance to solvents. The biodegradation has been described as a possible methodology to reduce the accumulation of plastics. In this work it was carried through the evaluation by Bacillus subtilis and Phanerochaete chrysosporium performance on the biodegradation of the polyethylene terephtalate. In this direction, particles of polymer were submitted to the treatments: exposition to ultra violet light (6 and 36 hours) and temperatures (35C and 50C), followed incubation with the microorganisms during 30 and 60 days. The polymer degradation process was accompanied by determination of pH, biofilm formation and the cells viability, enzymes detection (amylase, protease, esterase, and polyphenoloxidase), as well as the scanning electron microscopy of biofilm and toxicity tests. The results obtained observed the biofilm formation by Bacillus subtilis on polyethylene terephtalate surface particles. The treatment using the temperature of 50C demonstrated a higher alteration in the surface of the polymer, supported the colonization of the microorganisms followed of the hydrolytic enzymes production. It was observed that Bacillus subtilis does not produced polyphenoloxidase. The results indicated the temperature (50.C), induces the esterase production and it is related to degradation process. The P. chrysosporium produced esterases and polyphenoloxidase, whose enzymes had demonstrated to be involved with the polyethylene terephtalate degradation process, and were formed products with higher toxicities to Artemia salina