A poliamida 6.6 é um dos mais importantes membros da família das poliamidas, principalmente pelas excelentes propriedades de engenharia, como desempenho mecânico e térmico. A sua área de aplicação é ampliada pela adição de cargas inorgânicas. Dentre estas cargas podemos destacar as fibras de vidro, talco, wollastonita e micro esferas de vidro, cargas estas industrialmente conhecidas. Por outro lado, partículas de vidro reciclado provenientes de descarte nunca foram estudadas como reforço de poliamida 6.6, em especial as partículas menores, que são rejeitadas na reciclagem pela indústria do vidro por apresentarem dificuldade de transporte para os fornos, podendo depositar-se nos refratários (fenômeno de arraste), aumentando sua taxa de corrosão, assim reduzindo a vida útil dos fornos. Além disso, essas partículas têm formato irregular. Desse modo, compósitos de poliamida 6.6 reforçados com porcentagens variadas de vidro reciclado e cargas usualmente empregadas pela indústria foram processados em laboratório, com o auxílio de uma extrusora dupla-rosca e as amostras avaliadas foram obtidas por injeção. As seguintes propriedades dos compósitos foram avaliadas: resistência à tração, alongamento na ruptura, módulo na tração, resistência ao impacto Charpy sem entalhe, estabilidade dimensional e microscopia eletrônica de varredura. Os resultados indicam que é possível utilizar-se partículas de vidro reciclado numa matriz de PA-6.6 uma vez que as propriedades do compósito final são compatíveis com aquelas proporcionadas pelas cargas comerciais usualmente empregadas. / Polyamide 6.6 is one of the most important members of the polyamide family, mainly for its excellent engineering properties such as good mechanical and thermal performances. Its application area is enlarged by the addition of inorganic fillers. Among these fillers, glass fibers, talc, wollastonite and glass microspheres could be highlighted, which are industrially known fillers. On the other hand, glass particles from glass cullet have never been studied as a polyamide reinforcement, specially the smaller particles, which are rejected by the glass industry because of the carry-over phenomenon, increasing the cost of the smoke washing, as well as the possibility of increasing refractory corrosion, therefore reducing the useful life of the furnaces. Furthermore, these particles present irregular shapes. In this research, polyamide 6.6 composites, reinforced with different percentages of recycled powder glass and other common fillers used by the industry, were processed in laboratory scale with the help of a double screw extruder. Specimens for testing were obtained by injection, and the following composite properties were evaluated: tensile strength, elongation at rupture, elastic modulus, notchless Charpy impact strength, and dimensional stability. The specimens were also observed in a scanning electron microscope. The results indicated that it is possible to use particles of recycled glass in a PA- 6.6 matrix, once the final composite properties are compatible to the ones of composites containing usual commercial fillers.

A poliamida 6.6 é um dos mais importantes membros da família das poliamidas, principalmente pelas excelentes propriedades de engenharia, como desempenho mecânico e térmico. A sua área de aplicação é ampliada pela adição de cargas inorgânicas. Dentre estas cargas podemos destacar as fibras de vidro, talco, wollastonita e micro esferas de vidro, cargas estas industrialmente conhecidas. Por outro lado, partículas de vidro reciclado provenientes de descarte nunca foram estudadas como reforço de poliamida 6.6, em especial as partículas menores, que são rejeitadas na reciclagem pela indústria do vidro por apresentarem dificuldade de transporte para os fornos, podendo depositar-se nos refratários (fenômeno de arraste), aumentando sua taxa de corrosão, assim reduzindo a vida útil dos fornos. Além disso, essas partículas têm formato irregular. Desse modo, compósitos de poliamida 6.6 reforçados com porcentagens variadas de vidro reciclado e cargas usualmente empregadas pela indústria foram processados em laboratório, com o auxílio de uma extrusora dupla-rosca e as amostras avaliadas foram obtidas por injeção. As seguintes propriedades dos compósitos foram avaliadas: resistência à tração, alongamento na ruptura, módulo na tração, resistência ao impacto Charpy sem entalhe, estabilidade dimensional e microscopia eletrônica de varredura. Os resultados indicam que é possível utilizar-se partículas de vidro reciclado numa matriz de PA-6.6 uma vez que as propriedades do compósito final são compatíveis com aquelas proporcionadas pelas cargas comerciais usualmente empregadas. / Polyamide 6.6 is one of the most important members of the polyamide family, mainly for its excellent engineering properties such as good mechanical and thermal performances. Its application area is enlarged by the addition of inorganic fillers. Among these fillers, glass fibers, talc, wollastonite and glass microspheres could be highlighted, which are industrially known fillers. On the other hand, glass particles from glass cullet have never been studied as a polyamide reinforcement, specially the smaller particles, which are rejected by the glass industry because of the carry-over phenomenon, increasing the cost of the smoke washing, as well as the possibility of increasing refractory corrosion, therefore reducing the useful life of the furnaces. Furthermore, these particles present irregular shapes. In this research, polyamide 6.6 composites, reinforced with different percentages of recycled powder glass and other common fillers used by the industry, were processed in laboratory scale with the help of a double screw extruder. Specimens for testing were obtained by injection, and the following composite properties were evaluated: tensile strength, elongation at rupture, elastic modulus, notchless Charpy impact strength, and dimensional stability. The specimens were also observed in a scanning electron microscope. The results indicated that it is possible to use particles of recycled glass in a PA- 6.6 matrix, once the final composite properties are compatible to the ones of composites containing usual commercial fillers.

No description available.

Este trabalho tem por objetivo a comparação das propriedades da superfície da poliamida 6.6 tratada por plasma e por radiação ionizante, assim como determinar qual a melhor técnica e condição para ativação da superfície, visando a adesão da mesma e borracha poliacrílica utilizada na fabricação de retentores automotivos. O tratamento da poliamida 6.6 por plasma foi realizado utilizando um equipamento Electronic DIENER Plasma Surface- Technology LFG40, com gás nitrogênio à pressão de 1,40 kg/cm2. As amostras de poliamida 6.6 também foram tratadas por radiação ionizante, à pressão atmosférica e em vácuo, utilizando um acelerador industrial de elétrons, Dynamitron JOB 188, com dose de radiação de 5, 10, 20, 40, 50, 100, 200, 300, 400 e 500kGy com taxa de dose de 11,22 kGy/s para todas as doses e taxa de 11,22 kGy/s e 22,38 kGy/s para a dose de 20kGy. Após os processos de modificação da superfície da poliamida 6.6, parte das amostras não tratadas, tratadas por plasma e por radiação ionizante foram incorporadas à borracha poliacrílica, e outra parte foi destinada a caracterização da superfície utilizando as técnicas de MEV/EDS, FT-IR, PIXE/RBS, AFM e ângulo de contato. As amostras não tratadas e as amostras irradiadas não aderiram à borracha poliacrílica. As amostras tratadas por plasma aderiram à borracha poliacrílica com eficiência e apresentaram diferenças de rugosidade, nas análises de MEV e AFM, e aumento no ângulo de contato quando comparado com as amostras não tratadas. As amostras irradiadas não apresentaram diferenças significativas de propriedades nas análises utilizadas neste trabalho, quando comparadas com as amostras não tratadas. A radiação ionizante não foi eficiente na modificação da superfície da poliamida 6.6 para aderência à borracha poliacrílica. / This study aims to compare the surface properties of polyamide 6.6 plasma treatment and ionizing radiation, as well as determine the best technique and condition of the surface activation, adhesion of the same order and polyacrylic rubber used in manufacturing of automotive retainers. Treatment of polyamide 6.6 plasma was performed using an equipment \"Electronic Diener - Plasma - Surface-Technology LFG40\" with nitrogen gas at a pressure of 1.40 kg/cm2. Samples of polyamide 6.6 were also treated with ionizing radiation, atmospheric pressure and in vacuum, using an industrial electron accelerator, Dynamitron JOB 188 with radiation dose of 5, 10, 20, 40, 50, 100, 200, 300, 400 and 500kGy with a dose rate of 11.22 kGy/s for all doses and rate of 11.22 kGy/s and 22.38 kGy/s for a dose of 20kGy. After the processes of surface modification of polyamide 6.6, part of the untreated samples, treated by plasma and by ionizing radiation were incorporated into the polyacrylic rubber, and another part was designed to characterize the surface using the techniques of SEM / EDS, FT- IR, PIXE / RBS, AFM and contact angle. Untreated samples and the irradiated samples did not join the polyacrylic rubber. The samples treated by plasma joined the polyacrylic rubber efficiently and showed differences in roughness in SEM and AFM, and an increase in contact angle when compared with untreated samples. The irradiated samples showed no significant differences in the analysis of properties used in this study when compared with untreated samples. Ionizing radiation was not effective in surface modification of polyamide 6.6 for adherence with polyacrylic rubber.

Este trabalho tem por objetivo a comparação das propriedades da superfície da poliamida 6.6 tratada por plasma e por radiação ionizante, assim como determinar qual a melhor técnica e condição para ativação da superfície, visando a adesão da mesma e borracha poliacrílica utilizada na fabricação de retentores automotivos. O tratamento da poliamida 6.6 por plasma foi realizado utilizando um equipamento Electronic DIENER Plasma Surface- Technology LFG40, com gás nitrogênio à pressão de 1,40 kg/cm2. As amostras de poliamida 6.6 também foram tratadas por radiação ionizante, à pressão atmosférica e em vácuo, utilizando um acelerador industrial de elétrons, Dynamitron JOB 188, com dose de radiação de 5, 10, 20, 40, 50, 100, 200, 300, 400 e 500kGy com taxa de dose de 11,22 kGy/s para todas as doses e taxa de 11,22 kGy/s e 22,38 kGy/s para a dose de 20kGy. Após os processos de modificação da superfície da poliamida 6.6, parte das amostras não tratadas, tratadas por plasma e por radiação ionizante foram incorporadas à borracha poliacrílica, e outra parte foi destinada a caracterização da superfície utilizando as técnicas de MEV/EDS, FT-IR, PIXE/RBS, AFM e ângulo de contato. As amostras não tratadas e as amostras irradiadas não aderiram à borracha poliacrílica. As amostras tratadas por plasma aderiram à borracha poliacrílica com eficiência e apresentaram diferenças de rugosidade, nas análises de MEV e AFM, e aumento no ângulo de contato quando comparado com as amostras não tratadas. As amostras irradiadas não apresentaram diferenças significativas de propriedades nas análises utilizadas neste trabalho, quando comparadas com as amostras não tratadas. A radiação ionizante não foi eficiente na modificação da superfície da poliamida 6.6 para aderência à borracha poliacrílica. / This study aims to compare the surface properties of polyamide 6.6 plasma treatment and ionizing radiation, as well as determine the best technique and condition of the surface activation, adhesion of the same order and polyacrylic rubber used in manufacturing of automotive retainers. Treatment of polyamide 6.6 plasma was performed using an equipment \"Electronic Diener - Plasma - Surface-Technology LFG40\" with nitrogen gas at a pressure of 1.40 kg/cm2. Samples of polyamide 6.6 were also treated with ionizing radiation, atmospheric pressure and in vacuum, using an industrial electron accelerator, Dynamitron JOB 188 with radiation dose of 5, 10, 20, 40, 50, 100, 200, 300, 400 and 500kGy with a dose rate of 11.22 kGy/s for all doses and rate of 11.22 kGy/s and 22.38 kGy/s for a dose of 20kGy. After the processes of surface modification of polyamide 6.6, part of the untreated samples, treated by plasma and by ionizing radiation were incorporated into the polyacrylic rubber, and another part was designed to characterize the surface using the techniques of SEM / EDS, FT- IR, PIXE / RBS, AFM and contact angle. Untreated samples and the irradiated samples did not join the polyacrylic rubber. The samples treated by plasma joined the polyacrylic rubber efficiently and showed differences in roughness in SEM and AFM, and an increase in contact angle when compared with untreated samples. The irradiated samples showed no significant differences in the analysis of properties used in this study when compared with untreated samples. Ionizing radiation was not effective in surface modification of polyamide 6.6 for adherence with polyacrylic rubber.

The extraction and quantitative analysis of low molar mass compounds in polymers is an analytical challenge. It is also important from a practical point of view because the low molar mass compounds in time will migrate from the polymers into the surrounding environment. It is especially important to gain knowledge about the migrating compounds in applications such as medical implants, packaging materials and car interiors. The main aim of this thesis was to develop headspace solid phase microextraction (HS-SPME) methods to meet this challenge. In addition, the work aimed to show the applicability of the methods developed in quality control of polymers, degradation studies and assessment of polymer durability. Factors influencing the extraction of low molar mass compounds from polyamide 6.6 were studied. Particular attention was paid to the matrix effects and to the establishment of headspace equilibrium of 2-cyclopentyl-cyclopentanone in solid polyamide. Hydrogen bonding and adsorption of analyte to the polar matrix was observed and found to cause exceedingly slow establishment of equilibrium. The adsorption could be eliminated by the addition of water, which replaced 2-cyclopentyl-cyclopentanone at the adsorption sites of the polyamide and made it possible to measure the 2-cyclopentyl-cyclopentanone content in polyamide 6.6 using multiple headspace solid-phase microextraction (MHS-SPME). A correlation between the emitted amount of 2-cyclopentyl-cyclopentanone and the amount 2-cyclopentyl-cyclopentanone in the material was found. The correlation was valid also under non-equilibrium conditions, which allows rapid assessment of the 2-cyclopentyl-cyclopentanone content in polyamide 6.6 using headspace sampling. 20 different low molar mass compounds were identified in virgin and recycled polyamide 6.6. The compounds could be classified into four groups: cyclic imides, pyridines, chain fragments and cyclopentanones. The structures of the degradation products imply that the thermo-oxidative degradation starts at the N-vicinal methyl group. Larger amounts of degradation products at lower degree of degradation were formed in recycled than in virgin polyamide 6.6. Thus, processing increases the susceptibility of polyamide 6.6 to thermal oxidation. The total amount of cyclopentanones was reduced upon processing and oxidation. Cyclopentanones are thus not thermo-oxidation products of polyamide 6.6. N-pentyl-succinimide showed the most significant increase due to oxidation and processing. The formation of N-pentyl-succinimide was in correlation with the simultaneous changes in tensile strength. The largest increase in N-pentyl-succinimide coincided with the largest drop in tensile strength.

<p>The extraction and quantitative analysis of low molar mass compounds in polymers is an analytical challenge. It is also important from a practical point of view because the low molar mass compounds in time will migrate from the polymers into the surrounding environment. It is especially important to gain knowledge about the migrating compounds in applications such as medical implants, packaging materials and car interiors. The main aim of this thesis was to develop headspace solid phase microextraction (HS-SPME) methods to meet this challenge. In addition, the work aimed to show the applicability of the methods developed in quality control of polymers, degradation studies and assessment of polymer durability. </p><p>Factors influencing the extraction of low molar mass compounds from polyamide 6.6 were studied. Particular attention was paid to the matrix effects and to the establishment of headspace equilibrium of 2-cyclopentyl-cyclopentanone in solid polyamide. Hydrogen bonding and adsorption of analyte to the polar matrix was observed and found to cause exceedingly slow establishment of equilibrium. The adsorption could be eliminated by the addition of water, which replaced 2-cyclopentyl-cyclopentanone at the adsorption sites of the polyamide and made it possible to measure the 2-cyclopentyl-cyclopentanone content in polyamide 6.6 using multiple headspace solid-phase microextraction (MHS-SPME). </p><p>A correlation between the emitted amount of 2-cyclopentyl-cyclopentanone and the amount 2-cyclopentyl-cyclopentanone in the material was found. The correlation was valid also under non-equilibrium conditions, which allows rapid assessment of the 2-cyclopentyl-cyclopentanone content in polyamide 6.6 using headspace sampling. </p><p>20 different low molar mass compounds were identified in virgin and recycled polyamide 6.6. The compounds could be classified into four groups: cyclic imides, pyridines, chain fragments and cyclopentanones. The structures of the degradation products imply that the thermo-oxidative degradation starts at the N-vicinal methyl group. Larger amounts of degradation products at lower degree of degradation were formed in recycled than in virgin polyamide 6.6. Thus, processing increases the susceptibility of polyamide 6.6 to thermal oxidation. The total amount of cyclopentanones was reduced upon processing and oxidation. Cyclopentanones are thus not thermo-oxidation products of polyamide 6.6. N-pentyl-succinimide showed the most significant increase due to oxidation and processing. The formation of N-pentyl-succinimide was in correlation with the simultaneous changes in tensile strength. The largest increase in N-pentyl-succinimide coincided with the largest drop in tensile strength.</p>

Orientadores: Chang Tien Kiang, Elias Hage Junior / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Quimica / Made available in DSpace on 2018-07-20T05:26:20Z (GMT). No. of bitstreams: 1 Cardoso_Giselia_M.pdf: 2679256 bytes, checksum: 20c2cfedadeeb83bd8a03e60f9c2c1a4 (MD5) Previous issue date: 1994 / Resumo: Misturas poliméricas binárias de poliamida 6,6 com aditivo macromolecular ¿ poliamida 6 modificada, policarbonato e poli(metacrilato de metila) ¿ em quantidades de 1 a 10% em massa, foram preparados por fusão e moldadas por injeção através do Mini Max Molder de fabricação da Custom Scientific Instruments. Os produtos obtidos foram caracterizados por microscopia ótica (MO), calorimetria diferencial de varredura (DSC) e análise dinâmico-mecânica (DMA). A análise em microscopia ótica foi realizada de forma qualitativa na observação da influência da natureza química e da quantidade de aditivo macromolecular na modificação da microestrutura da poliamida 6,6. as análises de DSC foram realizadas de duas maneiras: varredura de temperatura, na verificação de existência de miscibilidade nas e determinação. Pela equação de Nishi ¿ Wang, do parâmetro de interação de Flory ('X IND. 12¿); e isotérmica, na avaliação do efeito da presença dos aditivos macromoleculares na velocidade de cristalização da poliamida 6,6. A existência de separação de fase no estado sólido das misturas foi verificada através da análise do comportamento dinâmico-mecânico. O estudo conclui que a adição de pequena quantidade de macromoléculas retarda o aparecimento e reduz a taxa de crescimento dos esferulitos na poliamida 6,6 / Abstract: Binary polymeric blends of polyamide 6,6 with macromolecular additive ¿ modified polyamide 6, polycarbonate and poly(methyl methacrylate) ¿ in amounts varying from 1% to 10% in mass, were prepared by melting and injection ¿ molded a Mini Max Molder ¿ Custom Scientific Instruments. The obtained products were characterized by optical microscopy (OM), differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA). The optical microscopy analysis was performed as a qualitative observation of the influence of chemical nature and quantity of macromolecular additive in the modification of microstructure of polyamide 6,6. the DSC analysis were done in two ways: temperature scanning, where it was verified the miscibility of mixtures and the Flory¿s interaction parameter 'X IND. 12¿ was determined by Nishi ¿ Wang equation; and isothermally, where the presence of macromolecular additives in the rate of crystallization of polyamide 6,6 was evaluated. DMA of rod samples were performed to evaluate the presence of phase separation in the solid state. It is concluded that blending small amounts of macromolecular additives can delay and reduce the spherulitic crystallization growth in the polyamide 6,6 / Mestrado / Ciencia e Tecnologia de Materiais / Mestre em Engenharia Química

NR 20140805

De senaste decennierna har visat på en stor ökning av den textila konsumtionen som följd av efterfrågan, samtidigt som den textila återvinningen idag är nästintill obefintlig. Detta leder till att mycket av det textila materialet deponeras istället för att återvinnas, vilket innebär ett stort slöseri av redan befintlig råvara som skulle kunna användas till att skapa nytt textilt material. Genom att undersöka olika återvinningsmetoder och -processer skulle denna råvara kunna användas på nytt. Examensarbetet är en del av forskningsprojektet ”Från spill till guld” som leds av forskningsinstitutet Swerea IVF. Forskningsprojektets utgångspunkt är att minimera produktionsspill och att höja dess värde inom bland annat textilindustrin. Examensarbetet syftar till att undersöka termomekanisk återvinning av plagg gjorda av polyamid 6.6 (PA6.6) och elastan, smältspinna filament samt formspruta provstavar från denna nya polymerblandning utan att separera fibrerna. Andra syftet är att även hitta en lösning för produkterna som undersöks i detta examensarbete kan återvinnas i sin helhet, så att ingen demontering av produkterna ska behövas. Fyra olika plagg undersöktes i examensarbetet bestående av materialblandningen PA6.6 och elastan. Analyser av de fyra olika plaggen genomfördes för att fastställa materialen. Hela plagg tillverkade i de olika materialen klipptes eller maldes ned och smältes sedan om genom kompoundering, därefter tillverkades granulat. Materialen testades i spinnbarhet genom smältspinningsförsök, sedan smältspanns eller formsprutades materialen. Resultaten från smältspinningsförsöken analyserades i ljusmikroskop för att avgöra om elastanen är termoplastiskt eller inte då detta är en avgörande faktor vid smältspinning. Olika tester gjordes på materialen för att undersöka deras eventuella kemiska nedbrytning som resultat av kompoundering. Resultatet visade att smältspinning och formsprutning inte är möjligt från denna polymerblandning. Ett antagande kan göras att återvinningen inte fungerade på grund av PA6.6:s höga smälttemperatur, då elastanen antagligen bryts ned vid denna höga temperatur, vilket förstör materialet. Slutsatsen blir då att smältspinning och formsprutning inte är möjligt utifrån denna polymerblandning, men återvinning till plastdetaljer kan produceras vid kompounderingsstadiet och återanvändas i annan industri än textilindustrin. Potential finns för återvinning av plagg till plagg om ändringar görs under processens gång och om elastanen identifieras som termoplastisk eller inte. / The latest decades have shown a large increase in textile consumption as a result of demand, at the same time the textile recycling today is almost non-existent. This means that much of the textiles are used for landfill rather than being recycled, which generates a large waste of raw material that could be used to create new textiles. By exploring various recycling methods and processes this raw material could be used again. This thesis is part of a research project, “From Waste To Gold”, which is led by the research institute Swerea IVF. The research projects foundation is to minimize production waste and to increase its value in areas such as textile industries. This thesis’ foundation is to examine the mechanical recycling of garments made by polyamide 6.6 (PA6.6) and spandex, melt spin filaments and produce injection moulded samples from this new polymer blend, without separating the fibres. The other foundation is to find a solution for the products that are examined in this thesis so they could be recycled as a unit, no disassembly of the products would be necessary Four different garments was examined in this thesis, the materials were a combination of PA6.6 and spandex. Different analyses were made on the four different garments. Whole garments from the different materials were cut or milled and then re melted through compounding, after compounding granulates was made. The materials spin ability was tested through melt spinning trials, then the materials were either melt spun or injection moulded. The results from the spinning trials was analysed in a light microscope to examine if the spandex were thermoplastic or not, as this is a crucial factor when melt spinning. Various tests were conducted to analyse their chemical degradation after the compounding. The results from the melt spinning and injection moulding showed that it was not possible to recycle this polymer combination this way. An assumption can be made that the recycling methods did not work because of the high melt temperature of PA6.6, the spandex assumes to decompose at this high temperature and therefore destroys the material. The conclusion is that melt spinning and injection moulding is not possible to conduct with this polymer combination, but recycling to plastic details could be done at the compound stage and then be used in some other industry, not in the textile industry. There are potential for garment-to-garment recycling if changes are made during the recycling processes and if the spandex could be identified as a thermoplastic or a non-thermoplastic.