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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
41

Use of ionic liquid for producing regenerated cellulose fibers

Jiang, Wei, master of science in textile and apparel technology 03 August 2012 (has links)
The objectives of the research are to establish the process of obtaining regenerated fibers and films from wood pulp and bagasse pulp with the ionic liquid 1-Butyl-3-methylimidazolium Chloride (BMIMCl) as a solvent; to study the impacts on tensile strength of different spinning parameters; to find the optimal spinning condition, and to obtain regenerated cellulose products with flame retardant properties. Solutions were obtained by dissolving cellulose (wood/bagasse) pulp into the BMIMCl. The solutions were extruded in a dry-jet and wet-spinning method using water as a coagulation bath. The obtained fibers were tested to evaluate the properties such as tensile strength, thermal property, thermal mechanical property, crystal order, and ionic liquid residue in obtained fiber. The orthogonal experiments were designed to find out the strongest affective variable and the optimal condition of the spinning process. The regenerated cellulose films with melamine resin or zinc oxide were obtained. Their flame retardant properties were tested. Cellulose fiber with melamine resin was also obtained. Thermo-gravimetric analyzer (TGA) was used to measure the thermal properties of obtained products, and to calculate their activation energies. Dynamic mechanical analysis (DMA) was used to determine the thermal mechanical properties of obtained fibers. Wide angle X-ray diffraction (WAXD) was used to measure the degree of crystallinity and degree of crystal orientation. The tensile strength was tested by a tensile machine. To evaluate the quantity of ionic liquid residue in the regenerated fibers, the instrumental methods of FT-IR and Mass Spectrometry were applied. Research results indicated increases in the degree of crystallinity and storage modulus under a higher fiber drawing speed. Both regenerated bagasse fibers and regenerated wood fibers had similar thermal properties. However, the regenerated bagasse fibers showed a higher degree of crystallinity and a higher tenacity than the regenerated wood fibers obtained under the same condition. The study also revealed water treatment would be helpful for eliminating the ionic residue in regenerated fibers. It was also found the concentration of cellulose in the BMIMCl solution affected the tensile strength of regenerated fiber mostly. Certain amount of melamine or zinc oxide nanoparticles contained in the cellulose matrix could improve the flame retardant property effectively. / text
42

Clay Mineralogy and Illite Crystallinity in the Late Devonian to Early Mississippian Woodford Shale in the Arbuckle Mountains, Oklahoma, USA

Whittington II, Richard Allen 14 April 2009 (has links)
Commonly the thermal maturity of the Late Devonian to Early Mississippian Woodford shale found on the flanks of the Arbuckle Mountains of Oklahoma is determined by vitrinite reflectance, values ranging from 0.3-1.5%. Using phyllosilicate minerals, specifically diagenetic mixed layer illite/smectite and diagenetic illite, an understanding of the extent and processes leading to the thermal maturation may be developed. Analysis by XRD of the clay mineralogy of the Woodford shale found kaolinite and mixed layer illite/smectite with <5% smectite and R≥3 stacking order. Modeling of the Woodford shale also suggests the percentage of smectite present in mixed layer illite/smectite to be <5% and commonly <2.5%. Deconvolution of the illite (001) peak supports the low smectite content and high illite crystallinity. The long range ordered illite, R≥3, and high illite crystallinity values are indicative of diagenesis to anchizone conditions suggesting a higher thermal maturity relative to previously measured values of vitrinite reflectance.
43

EVALUATION OF THE PHYSICOCHEMICAL PROPERTIES AND STABILITY OF SOLID LIPID NANOPARTICLES DESIGNED FOR THE DELIVERY OF DEXAMETHASONE TO TUMORS

Howard, Melissa 01 January 2011 (has links)
Pre-clinical and clinical trials suggest that pre-treatment with dexamethasone (Dex) may facilitate enhanced uptake of subsequently administered chemotherapeutic agents. To reduce the side effects associated with systemic administration of Dex, solid lipid nanoparticles (SLNs) containing dexamethasone palmitate (Dex-P) were prepared as a means of achieving tumor-targeted drug delivery. These studies were aimed at evaluating the physicochemical properties and both the physiological and storage stability of the SLNs. SLNs were prepared using nanotemplate engineering technology. Stearyl alcohol (SA) was used as the lipid phase with Brij® 78 and Polysorbate 60 as surfactants and PEG6000 monostearate as a long-chain PEGylating agent. Both formulations exhibited a small particle size, ellipsoidal shape, and low polydispersity. 1H-NMR spectroscopy confirmed that SLNs have the expected solid core and PEGylated surface. Analysis of the bulk materials indicated that a number of complex interactions are present among the SLN components, including a eutectic between SA and Brij® 78. Dex-P could be incorporated in SLNs at 10-30% w/w SA with encapsulation efficiencies >85%. A preferential interaction with the SA-Brij® 78 eutectic was identified, indicating a possible interfacial localization. For comparison, SLNs were also prepared with ascorbyl palmitate (AP) and curcumin. Higher drug loads were achieved with both palmitate-containing prodrugs than curcumin, though all appeared to align differently within the SLNs. SLNs undergo a concentration-dependent particle size growth when incubated at physiological temperature. However, they appear to remain intact with over 85% of the added Dex-P retained at 24 h in conditions mimicking human plasma. In the presence of carboxylesterase, SLNs became turbid and showed a reduction in particle size as compared to controls. This instability was shown to be a result of the hydrolysis of PEG6000 monostearate and Polysorbate 60. To enhance storage stability, a lyophilization protocol designed to minimize changes in the physicochemical properties of SLNs was developed. During a 3 month period, lyophilized SLNs stored at 4°C demonstrated the greatest stability, showing a consistent particle size and an encapsulation efficiency >80%. Overall, these results indicate that Dex-P loaded SLNs possess the physicochemical properties and stability desirable for development as a tumor-targeted drug delivery system.
44

Cellulose fiber dissolution in sodium hydroxide solution at low temperature: dissolution kinetics and solubility improvement

Wang, Ying 31 July 2008 (has links)
Sodium hydroxide can cause cellulose to swell and can even dissolve cellulose in a narrow range of the phase diagram. It was found that for cellulose with low to moderate degree of polymerization, the maximal solubility occurs with 8~10% soda solution. In recent years, researchers found that sodium hydroxide with urea at cold temperature can dissolve cellulose better than sodium hydroxide alone. However, the lack of sufficient understanding of the NaOH and NaOH/urea dissolution process significantly constrains its applications. In order to fully understand the cellulose dissolution in alkali system, there are several aspects of problems that need to be addressed. Our focus in this study is in the interaction of cellulose with alkali solution at low temperatures, the improvement of its solubility, and the effect of hemicellulose and lignin.
45

Obtenção de óxido de nióbio nanoestruturado por método hidrotermal assistido por microondas e sua caracterização quanto à morfologia, cristalinidade e às propriedades ópticas

Romero, Ricardo Pavel Panta January 2017 (has links)
Neste trabalho foi estudada a produção, por síntese hidrotermal assistida por microondas, nanoestruturas de pentóxido de nióbio (Nb2O5) a partir do precursor pentacloreto de nióbio (NbCl5). A síntese foi realizada nas temperaturas de 150 e 200 °C durante 130 min, e o produto obtido foi tratado termicamente a temperaturas de 600, 800 e 1000 °C por 60 min com taxa de aquecimento de 10 °C/min. Os produtos obtidos foram caracterizados por análise termogravimétrica (ATG), para detectar a perda de massa com a temperatura; por difração de raios X (DRX), para análise da estrutura cristalina; por espectroscopia de infravermelho por transformada de Fourier (FTIR) e por espectroscopia Raman, para identificação das fases formadas; por microscopia eletrônica de varredura (MEV) e microscopia eletrônica de transmissão (MET), para verificação da morfologia do material; e por espectroscopia de refletância difusa (ERD), para identificar as propriedades ópticas do material. Além dessas, foram realizados cálculos do tamanho do cristalito pela equação de Scherrer. Os resultados indicaram a formação de nanoestruturas com diversas fases cristalinas de nióbio (TT, T, B, M e H-Nb2O5). O tamanho do cristalito variou em função da temperatura de tratamento térmico praticado: entre 35,85 e 38,80 nm para as amostras sintetizadas a 150 °C; e entre 34,84 e 40,93 nm para as amostras sintetizadas a 200 °C. Com a análise por refletância difusa foram obtidos os valores de band gaps para as amostras sintetizadas, e os resultados identificaram material semicondutor com uma variação de 3,13 a 3,90 eV. / In this work was studied the production by hydrothermal synthesis assist for microwave, niobium pentoxide nanocrystals (Nb2O5) obtained from the precursor pentachloride niobium (NbCl5). The synthesis was carried out at temperature of 150 and 200 °C for 130 min and the product obtained was calcined at temperatures 600, 800 and 1000 °C for 60 min and heating rate at 10 °C/min. The following characterizations were performed for analysis of the material, among them, thermal gravimetric analysis (ATG) for detecting the lost mass by temperature, X-ray diffraction (XRD) for analysis of the crystal structure, Fourier Transform Infrared spectroscopic (FTIR) and Raman spectroscopic was used for analyze the changes in superficial chemical connections, scanning electron microscopy (SEM) and transmission electronic microscopic (TEM) for morphology of material and diffuse reflectance spectroscopy (DRS) for identification the material optical properties. Moreover, calculate were realized of crystallite size by Scherrer’s equation. The results showed the formation of nanostrutured with various phases (TT, T, B, M e H-Nb2O5). The crystallite size varied in function of thermal treatment temperature from 35,85 to 38,80 nm for synthesizes samples in 150 °C and 34,84 to 40,93 nm for synthesizes samples in 200 °C. With the analysis by diffuse reflectance were obtained the band gap values for the synthesized samples and the results identify a semiconductor material with a variation from 3,13 to 3,90 eV.
46

Preparação e caracterização de compósitos de polipropileno pós-consumo reforçados com fibras de celulose

Spadetti, Carolini 29 September 2015 (has links)
Submitted by Morgana Andrade (morgana.andrade@ufes.br) on 2016-04-20T17:56:11Z No. of bitstreams: 2 license_rdf: 23148 bytes, checksum: 9da0b6dfac957114c6a7714714b86306 (MD5) DISSERTAÇÃO FINAL.pdf: 3035437 bytes, checksum: f52392fee9c0e0970b2d3b7152a93f87 (MD5) / Approved for entry into archive by Patricia Barros (patricia.barros@ufes.br) on 2016-05-11T16:21:17Z (GMT) No. of bitstreams: 2 license_rdf: 23148 bytes, checksum: 9da0b6dfac957114c6a7714714b86306 (MD5) DISSERTAÇÃO FINAL.pdf: 3035437 bytes, checksum: f52392fee9c0e0970b2d3b7152a93f87 (MD5) / Made available in DSpace on 2016-05-11T16:21:17Z (GMT). No. of bitstreams: 2 license_rdf: 23148 bytes, checksum: 9da0b6dfac957114c6a7714714b86306 (MD5) DISSERTAÇÃO FINAL.pdf: 3035437 bytes, checksum: f52392fee9c0e0970b2d3b7152a93f87 (MD5) / CAPES / Compósitos de polipropileno reforçados com fibras naturais são uma importante alternativa considerando-se aspectos como sustentabilidade, reciclabilidade, abundância e baixo custo, se comparadas às fibras sintéticas. Este trabalho foi realizado com o objetivo de incentivar o uso de materiais reciclados, tendo no resultado final um produto ainda mais ecológico e rentável, através da associação do polipropileno reciclado e das fibras naturais. Foram investigadas as propriedades térmicas, mecânicas e morfológicas de compósitos de polipropileno reciclado e virgem, reforçados com até 40% em massa de fibras de celulose tratadas pelo método alcalino, branqueadas (FB), sem branqueamento (FNB) e tratadas com o tensoativo catiônico brometo de hexadeciltrimetilamonio (CTAB), (FCTAB), com concentração de 0,01 mol/L. Para obtenção dos dados, foram utilizadas as técnicas de Análise Térmica Dinâmico-Mecânica (DMTA), Calorimetria Exploratória Diferencial (DSC), Microscopia Eletrônica de Varredura (MEV) e Ressonância Magnética Nuclear (RMN). Os resultados mostraram que, compósitos de polipropileno reciclado, com as fibras branqueadas e não-branqueadas, possuem módulo de armazenamento (E’), inferior, quando comparados aos compósitos preparados com o PP virgem, no entanto com valores bem próximos. Essa redução para os compósitos com FNB foi de 577 MPa, para os compósitos com FB de 567 MPa e para os compósitos com FCTAB, ocorreu um aumento de 256 MPa. Houve uma redução do grau de cristalinidade (χc), de todos os compósitos produzidos. Já sobre a temperatura de cristalização, a inserção de fibras acarretou na diminuição de em média 3°C nas amostras com matriz reciclada e um aumento de em média 8°C, para as amostras com matriz virgem. Ocorreu um pequeno aumento na temperatura de fusão cristalina (Tm), com a inserção de fibras para os compósitos com as duas matrizes e uma redução em torno de 6°C na temperatura de transição vítrea (Tg) para os compósitos com FCTAB, e em torno de 3°C para os com FNB e FB. / Polypropylene composites reinforced with natural fibers are an important alternative considering aspects such as sustainability, recyclability, abundance and low cost, compared to synthetic fibers. This work was carried out in order to encourage the use of recycled materials, and the end result is a product even greener and profitable, through the association of recycled polypropylene and natural fibers. Thermal, mechanical and morphological composite recycled and virgin polypropylene were investigated, reinforced with up to 40% by weight of pulp fibers treated by alkaline method, bleached (FB) without bleaching (FNB) and treated with cationic surfactant bromide hexadecyltrimethylammonium bromide (CTAB) (FCTAB) with concentration of 0.01 mol / L. To obtain the data, we used the techniques of Dynamic-Mechanical Thermal Analysis (DMTA), Differential Scanning Calorimetry (DSC), Scanning Electron Microscopy (SEM) and nuclear magnetic resonance (NMR). The results showed that recycled polypropylene composites with non-bleached and bleached fibers have a storage modulus (E '), lower compared to composites prepared with virgin PP, but with very close values. This reduction for composites FNB was 577 MPa for the composites FB 567 MPa and the composites FCTAB, an increase of 256 MPa. There was a reduction in the degree of crystallinity (χc) of the generated composite. Already on the crystallization temperature, the fiber insertion resulted in decreased an average of 3° C in samples with recycled mother and an increase of an average 8 ° C for the samples with virgin matrix. There was a small increase in the crystalline melting temperature (Tm), with the insertion of fibers for composites with two arrays and a decrease of about 6°C in glass transition temperature (Tg) for composites FCTAB, and around 3°C for at FNB and FB.
47

Mechanical performances of PEKK thermoplastic composites linked to their processing parameters / Performances mécaniques de composites thermoplastiques PEKK en relation avec leurs paramètres de mise en œuvre

Choupin, Tanguy 07 December 2017 (has links)
Les thermoplastiques hautes performances poly(éther-cétone-cétone) (PEKK) sont actuellement étudiés avec un grand intérêt dans l’industrie aéronautique comme matrice pour la fabrication de pièces de structure composites renforcées par des fibres de carbone. En effet, les composites thermoplastiques PEKK ont l’avantage d’être consolidables hors autoclave et ont des températures de mise en œuvre plus faibles que les composites PEEK.L’objectif de cette étude est de comprendre et prédire l’évolution des propriétés mécaniques des composites PEKK suivant le cycle thermique de mise en œuvre pour déterminer les paramètres de mise en œuvre optimaux pour la fabrication des pièces composites PEKK concernant les temps de mise en œuvre et les performances mécaniques finales.Une première partie traite de la modélisation des cinétiques de cristallisation des matrices PEKK ainsi que l’influence de la cristallinité et des morphologies cristallines sur les propriétés mécaniques des matrices PEKK. Une deuxième partie se concentre sur les modifications macromoléculaires des matrices PEKK pour des hautes températures de mise en œuvre sous air et sous azote et leurs impacts sur la cristallisation et les performances mécaniques des matrices PEKK. Enfin une dernière partie présente l’influence des fibres de carbones sur les morphologies cristallines et les cinétiques de cristallisation, la fabrication de composites PEKK unidirectionnels et tissés à ± 45° sous presse et sous autoclave et enfin l’impact de la cristallinité et des morphologies cristallines sur les performances mécaniques finales des composites PEKK. / Poly(ether-ketone-ketone) (PEKK) high performance thermoplastics are currently studied with a great interest by the aeronautic industry as matrix for carbon fiber reinforced structural parts. In fact, PEKK composites can be consolidated out of autoclave and they have lower processing temperatures than PEEK composites.The aim of the study was to investigate and predict the evolution of PEKK composite mechanical properties depending on the processing thermal cycle to determine the best processing parameters for PEKK composite part manufacturing regarding processing times and final mechanical performances.A first part investigates the crystallization kinetics modelling of PEKK matrices and the influence of crystallinity and crystalline morphologies on PEKK matrix mechanical properties. A second part focuses on the macromolecular modifications of PEKK matrices at high processing temperatures under air and nitrogen and their impact on PEKK matrices crystallization and mechanical properties. A last part presents the influence of carbon fibers on crystalline morphologies and crystallization kinetics, the manufacturing of unidirectional and ± 45° PEKK composites under press and autoclave and finally the impact of crystallinity and crystalline morphologies on PEKK composite mechanical properties.
48

Eletrofia??o e caracteriza??o de membranas biopolim?ricas a base de quitosana extra?das dos exoesqueletos de crust?ceos

Andrade, S?nia Maria Bel?sio de 13 April 2012 (has links)
Made available in DSpace on 2014-12-17T14:57:53Z (GMT). No. of bitstreams: 1 SaniaMBA_TESE.pdf: 2511848 bytes, checksum: 97413b8278096d3ff64cc7f5138841e7 (MD5) Previous issue date: 2012-04-13 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Chitin and chitosan are nontoxic, biodegradable and biocompatible polymers produced by renewable natural sources with applications in diverse areas such as: agriculture, textile, pharmaceutical, cosmetics and biomaterials, such as gels, films and other polymeric membranes. Both have attracted greater interest of scientists and researchers as functional polymeric materials. In this context, the objective of this study was to take advantage of the waste of shrimp (Litopenaeus vannamei and Aristeus antennatus) and crabs (Ucides cordatus) from fairs, beach huts and restaurant in Natal/RN for the extraction of chitin and chitosan for the production of membranes by electrospinning process. The extraction was made through demineralization, deproteinization, deodorization and deacetylation. Morphological analyzes (SEM and XRD), Thermal analysis (TG and DTG), Spectroscopy in the Region of the Infrared with Transformed of Fourier (FTIR) analysis Calorimetry Differential Scanning (DSC) and mechanical tests for traction were performed. In (XRD) the semicrystalline structure of chitosan can be verified while the chitin had higher crystallinity. In the thermal analysis showed a dehydration process followed by decomposition, with similar behavior of carbonized material. Chitosan showed temperature of maximum degradation lower than chitin. In the analysis by Differential Scanning Calorimetry (DSC) the curves were coherent to the thermal events of the chitosan membranes. The results obtained with (DD) for chitosan extracted from Litopenaeus vannamei and Aristeus antennatus shrimp were (80.36 and 71.00%) and Ucides cordatus crabs was 74.65%. It can be observed that, with 70:30 solutions (v/v) (TFA/DCM), 60 and 90% CH3COOH, occurred better facilitate the formation of membranes, while 100:00 (v/v) (TFA/DCM) had formation of agglomerates. In relation to the monofilaments diameters of the chitosan membranes, it was noted that the capillary-collector distance of 10 cm and tensions of 25 and 30 kV contributed to the reduction of the diameters of membranes. It was found that the Young s modulus decreases with increasing concentration of chitosan in the membranes. 90% CH3COOH contributed to the increase in the deformation resulting in more flexible material. The membranes with 5% chitosan 70:30 (v/v) (TFA/DCM) had higher tensile strength / Quitina e quitosana s?o pol?meros at?xicos, biodegrad?veis e biocompat?veis produzidos por fontes naturais renov?veis com aplica??es em diversas ?reas como: agricultura, t?xtil, farmac?utica, cosm?ticos e biomateriais, tais como g?is, filmes, membranas polim?ricas entre outros. Ambas t?m despertando grande interesse de cientistas e pesquisadores como materiais polim?ricos funcionais. Nesse contexto, o objetivo do presente trabalho foi aproveitar os res?duos de camar?es (Litopenaeus vannamei e Aristeus antennatus) e de caranguejos (Ucides cordatus) proveniente de feiras, barracas de praia e restaurantes em Natal/RN para extra??o de quitina, quitosana e produ??o de membranas pelo processo de eletrofia??o. A extra??o foi realizada a partir das etapas de desmineraliza??o, desproteiniza??o, desodoriza??o e desacetila??o. An?lises morfol?gicas (MEV e DRX), an?lises das propriedades t?rmicas (TG e DTG), an?lise por Espectroscopia na Regi?o do Infravermelho com Transformada de Fourier (FTIR), an?lise de Calorimetria Explorat?ria Diferencial (DSC) e ensaios mec?nicos por tra??o foram realizados. Na an?lise de DRX pode-se verificar a estrutura semicristalina da quitosana enquanto a quitina teve alta cristalinidade. As an?lises t?rmicas demonstraram um processo de desidrata??o seguido da decomposi??o com comportamento similar de material carbonizado. A quitosana apresentou temperaturas de m?xima degrada??o mais baixas do que a quitina. Na an?lise por Calorimetria Explorat?ria Diferencial (DSC) as curvas foram coerentes aos eventos t?rmicos das membranas de quitosana. Os resultados obtidos com (GD) para quitosana extra?da de camar?es Litopenaeus vannamei e Aristeus antennatus foram (80,36 e 71,00%) e caranguejos Ucides cordatus foi 74,65%. Pode-se perceber que, com solu??es 70:30 (v/v) (TFA/DCM), 60 e 90% CH3COOH, ocorreu melhor facilita??o na forma??o das membranas, enquanto em 100:00 (v/v) (TFA/DCM) houve forma??o de aglomerados. Em rela??o aos di?metros dos nanofilamentos das membranas de quitosana, percebeu-se que a dist?ncia capilar-coletor de 10 cm e tens?es de 25 e 30 kV contribu?ram para a redu??o dos di?metros das membranas. Quanto ao m?dulo de Young diminui com o aumento da concentra??o da quitosana nas membranas. 90% CH3COOH contribuiu para o aumento da deforma??o, sendo um material mais flex?vel. As membranas com 5% quitosana 70:30 (v/v) (TFA/DCM) apresentaram maior valor de resist?ncia ? tra??o
49

Obtenção de óxido de nióbio nanoestruturado por método hidrotermal assistido por microondas e sua caracterização quanto à morfologia, cristalinidade e às propriedades ópticas

Romero, Ricardo Pavel Panta January 2017 (has links)
Neste trabalho foi estudada a produção, por síntese hidrotermal assistida por microondas, nanoestruturas de pentóxido de nióbio (Nb2O5) a partir do precursor pentacloreto de nióbio (NbCl5). A síntese foi realizada nas temperaturas de 150 e 200 °C durante 130 min, e o produto obtido foi tratado termicamente a temperaturas de 600, 800 e 1000 °C por 60 min com taxa de aquecimento de 10 °C/min. Os produtos obtidos foram caracterizados por análise termogravimétrica (ATG), para detectar a perda de massa com a temperatura; por difração de raios X (DRX), para análise da estrutura cristalina; por espectroscopia de infravermelho por transformada de Fourier (FTIR) e por espectroscopia Raman, para identificação das fases formadas; por microscopia eletrônica de varredura (MEV) e microscopia eletrônica de transmissão (MET), para verificação da morfologia do material; e por espectroscopia de refletância difusa (ERD), para identificar as propriedades ópticas do material. Além dessas, foram realizados cálculos do tamanho do cristalito pela equação de Scherrer. Os resultados indicaram a formação de nanoestruturas com diversas fases cristalinas de nióbio (TT, T, B, M e H-Nb2O5). O tamanho do cristalito variou em função da temperatura de tratamento térmico praticado: entre 35,85 e 38,80 nm para as amostras sintetizadas a 150 °C; e entre 34,84 e 40,93 nm para as amostras sintetizadas a 200 °C. Com a análise por refletância difusa foram obtidos os valores de band gaps para as amostras sintetizadas, e os resultados identificaram material semicondutor com uma variação de 3,13 a 3,90 eV. / In this work was studied the production by hydrothermal synthesis assist for microwave, niobium pentoxide nanocrystals (Nb2O5) obtained from the precursor pentachloride niobium (NbCl5). The synthesis was carried out at temperature of 150 and 200 °C for 130 min and the product obtained was calcined at temperatures 600, 800 and 1000 °C for 60 min and heating rate at 10 °C/min. The following characterizations were performed for analysis of the material, among them, thermal gravimetric analysis (ATG) for detecting the lost mass by temperature, X-ray diffraction (XRD) for analysis of the crystal structure, Fourier Transform Infrared spectroscopic (FTIR) and Raman spectroscopic was used for analyze the changes in superficial chemical connections, scanning electron microscopy (SEM) and transmission electronic microscopic (TEM) for morphology of material and diffuse reflectance spectroscopy (DRS) for identification the material optical properties. Moreover, calculate were realized of crystallite size by Scherrer’s equation. The results showed the formation of nanostrutured with various phases (TT, T, B, M e H-Nb2O5). The crystallite size varied in function of thermal treatment temperature from 35,85 to 38,80 nm for synthesizes samples in 150 °C and 34,84 to 40,93 nm for synthesizes samples in 200 °C. With the analysis by diffuse reflectance were obtained the band gap values for the synthesized samples and the results identify a semiconductor material with a variation from 3,13 to 3,90 eV.
50

Amido e farinha de cañihua (Chenopodium pallidicaule): extração, caracterização e desenvolvimento de filmes biodegradáveis / Cañihua starch and flour (Chenopodium pallidicaule): extraction, characterization and development of biodegradable films

Santiago Ramírez-López 27 April 2016 (has links)
O desenvolvimento de materiais biodegradáveis, a partir de biopolímeros, para embalagens ou coberturas tem grande interesse para a indústria de alimentos. Na elaboração desses materiais, os amidos e as proteínas são muito usados por serem abundantes na natureza, de baixo custo e apresentam propriedades de formar filmes. A cañihua (Chenopodium pallidicaule), grão alto-andino pouco explorado industrialmente, tem altos conteúdos de carboidratos (~58 %) e proteínas (~18 %), e apresenta potencial para ser utilizado como matéria-prima na extração de amido comercial. Diante desse contexto, o objetivo desse trabalho foi extrair e caracterizar o amido de duas variedades de cañihua, Cupi (CC) e Illpa (CI), e selecionar uma dessas variedades para o desenvolvimento de filmes a base de amido ou de farinha. Além disso, a variedade selecionada foi usada para obter um material rico em amido e proteínas, denominado de farinha, que também foi usado para a produção de filmes biodegradáveis. Os grãos de cañihua das variedades Illpa e Cupi são muito similares na forma e tamanho dos grãos, porém os conteúdos de lipídios e cinzas são maiores para CC e o teor de fibras, para a CI. A extração do amido foi feita com solução de hidróxido de sódio (0,25 % m/v) e suas características estruturais, físico-químicas e funcionais foram determinadas. O rendimento desse processo foi de aproximadamente 33 %, e o amido da variedade CC apresentou maiores teores de lipídeos. Os amidos de ambas as variedades, observados em microscópio de varredura eletrônica, apresentaram superfícies granulares lisas e com formatos esféricos de pequeno tamanho (D[3,2] ~ 0,96 &micro;m). A distribuição de tamanho de partícula, o índice de cristalinidade, os espectros de FTIR, poder de inchamento, propriedades óticas e térmicas foram semelhantes, porém o teor de amilose foi maior para a variedade CC. Maiores valores de solubilidade e viscosidade (propriedades de pasta) foram observados para o amido da variedade Cupi e pode estar associado ao maior conteúdo de amilose. O amido da cañihua Cupi foi selecionado para a produção de filmes, por apresentar maiores teores de amilose e de lipídeos. Na obtenção da farinha de CC, usando soluções de NaOH e HCl (0,2 N), o rendimento foi estimado em 56 % (g/100 g de grãos). O teor de proteínas na farinha foi de 79 % (g/100 g sólidos) em relação ao grão. O alto conteúdo de proteínas favoreceu a formação de aglomerados que foram observados nas micrografias da farinha de CC, que apresentou diferenças nas propriedades óticas, de pasta e de solubilidade em relação ao amido da mesma variedade. Os filmes de amido ou farinha foram obtidos pelo método casting com adição de glicerol como plastificante (15 g/100 g de macromoléculas). A caracterização da microestrutura permitiu observar as diferenças físicas entre os filmes de amido ou farinha de cañihua Cupi, assim como as características estruturais foram úteis para explicar o comportamento das outras propriedades. Em umidades relativas altas, os filmes de amido ou farinha CC apresentam o mesmo comportamento de sorção de umidade e permeabilidade ao vapor de água, no entanto, em contato direito com a água (solubilidade e ângulo de contato), esses materiais apresentaram comportamento diferentes, sendo que os filmes de amido são mais resistentes. As diferenças nas propriedades mecânicas dos filmes de amido e farinha foram significativas (p&gt;0,05). O coeficiente de permeabilidade ao oxigênio foi menor para os filmes de amido do que para a farinha de CC. / The development of biodegradable materials based on biopolymers, films or coatings, have great interest for the food industry. For the production of these materials, starches and proteins are widely used because they are abundant in nature, have low cost and have films-forming property. Cañihua (Chenopodium pallidicaule), high Andean region grain underexplored industrially, has high carbohydrate content (~ 58 %) and proteins (~ 18 %) contents, and has the potential to be used as raw material in commercial starch extraction. In this context, the objectives of this study were to extract and characterize starch from two varieties cañihua, Cupi (CC) and Illpa (CI) and select a variety to develop starch films. Furthermore, the selected variety was used to obtain a rich starch and protein material, known as flour, which was also used to produce biodegradable films. Cañihua grains Illpa and Cupi varieties are very similar in shape and size, but the content of fat and ash are higher for CC and fiber content for the CI. The extraction of starch was performed with sodium hydroxide solution (0.25 % w/v) and their structural, physicochemical and functional characteristics were determined. The yield of this process was approximately 33 %, and CC variety starch showed higher levels of lipids. Starches from both varieties observed in scanning electron microscope, showed smooth granular surfaces and spherical shapes of small size (D3,2 ~ 0.96 &micro;M). The particle size distribution, crystallinity index, FTIR spectra, swelling power, thermal and optical properties were similar, but the amylose content was higher for CC variety. Higher values of solubility and viscosity of pasting properties were observed for CC variety starch and may be associated with higher amylose contents. Cañihua Cupi starch was selected to produce films, due to the higher amylose and lipid content. CC flour was also extracted with NaOH solution and adjusting the pH to 5.0 with HCl (0.2 N) in the protein precipitation step, the yield of this extraction process was estimated at 56 %. The protein content of the flour was 79 % compared to this fraction in the grain. The high protein content favors the agglomerates formation which was observed in the CC flour micrographs that showed differences in solubility, optical and pasting properties. The starch or flour films were obtained by casting method with addition of glycerol (15 g/100 g of macromolecules), as plasticizer. The characterization of the microstructure allowed observation of physical differences between starch or flour films of cañihua Cupi, and also structural characteristics were useful to explain the behavior of the other properties. When submitted to high relative humidity, films exhibited the same moisture sorption capacity behavior and water vapor permeability, however in films were in direct contact to water (solubility analysis and contact angle), the behavior of starch and flour films were different, being the structures of the starch films most resistant. Differences in mechanical properties of starch and flour films were significant (p&gt;0.05). The oxygen permeability coefficient was lower for cañihua Cupi starch films than cañihua Cupi flour films.

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