Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / The mango is one of the most popular fruits in Brazil, and the best know type is Mangifera indica L. The production of this fruit is seasonal and its industrialization has grown in the last years as a means of diminishing loss in the harvest time. The mango processing generates a great amount of residues, around 40 to 60% of the entire amount of raw material. From the residues generated, 12 to 15% is made up of peel and 15 to 20% is seeds. The residues cannot be accumulated indefinitely where they were produced, and are normally discarded with no previous treatment, far from the processing unit. In this sense, the use of the mango seed as a source of cellulose is an alternative in order to diminish the loss and impact on the environment. In this study, the mango seed of the Ubá variety of mangifera indica L. was used as a source of cellulose. The mango seed, originating from a juice factory in the municipality of Araguari-MG, showed a content of cellulose of 55.00% ± 1.0, while the content of Klason lignin was 23.85% ± 0.3. The fibres of the mango seed were used in the production of methylcellulose and the samples were produced by means of heterogeneous methylation using dimethyl sulfate (DMS) and iodomethane as alkylating agents. The methylcelluloses produced were characterized as to their thermal properties by means of scanning exploratory calorimetry (DSC) and thermogravimetric analysis (TGA). The crystalline fraction of the polymers was determined by diffraction of X-rays (DRX), and the substitution degrees (GS) were determined by chemical means. The GS values, determined by chemical means were of 1.35 for MCD and 0.45 for MCI, showing a higher substitution in the synthesis using DMS as methylation agent. Aqueous solutions of methylcellulose, in the concentration of 0.2% m/m and 0.6% m/m (polymer mass/cement mass) were used as an additive in mortar and its effect was assessed, when newly prepared, by means of Consistency Index (CI) tests, density and water retention. After hardened, tests by means of the assessment of potential resistance in adherence and traction (Ra) were carried out. The methylcellulose samples obtained with DMS (MCD) and iodomethane (MCI) as methylate agents, used in the proportion of 0.6% w/w, showed better result; the increase was of 27.75% and 71.54% in the IC and an increase of 23.33% and 26.67% respectively in the Ra, showing that polymers can be used in the production of adhesive mortars. / A manga é uma das frutas mais populares no Brasil, sendo a espécie mais difundida a Mangifera indica L. A produção dessa fruta é sazonal e sua industrialização tem crescido nos últimos anos como forma de diminuir as perdas no período de safra. O processamento da manga gera uma grande quantidade de resíduos, em torno de 40 a 60% de toda a matéria prima. Dos resíduos gerados 12 a 15 % são constituídos de cascas e de 15 a 20% de sementes. Os resíduos não podem ser acumulados indefinidamente no local onde foram produzidos e geralmente são descartados sem um tratamento prévio, longe da unidade processadora. Nesse sentido a utilização do caroço de manga como fonte de celulose se torna uma alternativa para diminuir as perdas e o impacto ambiental. No presente trabalho, o caroço de manga, Mangifera indica L. variedade Ubá, foi utilizado como fonte de celulose. O caroço de manga, proveniente de uma fábrica de suco do município de Araguari-MG, apresentou um teor de celulose de 55,00 % ± 1,0, enquanto o teor de lignina Klason foi de 23,85 % ± 0,3. As fibras do caroço de manga foram utilizadas para produção de metilcelulose e as amostras foram produzidas através da metilação heterogênea, utilizando-se o dimetilsulfato (DMS) e o iodometano como agentes alquilantes. As metilceluloses produzidas foram caracterizadas quanto às propriedades térmicas por calorimetria exploratória de varredura (DSC) e análise termogravimétrica (TGA). A fração cristalina dos polímeros foi determinada por difração de raios-X (DRX), e os graus de substituição (GS) foram determinados por via química. Os valores de GS, determinados por via química, foram de 1,35 para a MCD e 0,45 para a MCI, demonstrando uma maior substituição na síntese utilizando DMS como agente metilante. Soluções aquosas de metilcelulose, na concentração de 0,2 % m/m e 0,6% m/m (massa de polímero/massa de cimento), foram empregadas como aditivo em argamassas e o seu efeito foi avaliado, no estado fresco, através de ensaios de Índice de Consistência (IC), densidade e retenção de água. No estado endurecido, através da resistência potencial de aderência à tração (Ra). As amostras de metilcelulose obtidas com DMS (MCD) e iodometano (MCI) como agentes metilantes, utilizadas na proporção de 0,6% m/m, apresentaram um melhor resultado, sendo que o aumento foi de 27,75 % e 71,54 % no (IC) e um aumento na Ra de 23,33 % e 26,67%, respectivamente, mostrando que os polímeros podem ser empregados na produção de argamassas adesivas. / Doutor em Química

Submitted by Raquel Vergara Gondran (raquelvergara38@yahoo.com.br) on 2016-05-02T20:14:03Z No. of bitstreams: 1 marcia selmo - efeito da adio de metilcelulose transglutaminase e spirulina nas caractersticas tecnolgicas e nutricionais de pes de farinha de arroz.pdf: 3042564 bytes, checksum: 26b28ff5e3467d517c6b957f1fb27f10 (MD5) / Approved for entry into archive by Gilmar Barros (gilmargomesdebarros@gmail.com) on 2016-05-03T20:21:37Z (GMT) No. of bitstreams: 1 marcia selmo - efeito da adio de metilcelulose transglutaminase e spirulina nas caractersticas tecnolgicas e nutricionais de pes de farinha de arroz.pdf: 3042564 bytes, checksum: 26b28ff5e3467d517c6b957f1fb27f10 (MD5) / Made available in DSpace on 2016-05-03T20:21:37Z (GMT). No. of bitstreams: 1 marcia selmo - efeito da adio de metilcelulose transglutaminase e spirulina nas caractersticas tecnolgicas e nutricionais de pes de farinha de arroz.pdf: 3042564 bytes, checksum: 26b28ff5e3467d517c6b957f1fb27f10 (MD5) Previous issue date: 2014 / A doença celíaca é uma enfermidade causada pela intolerância ao glúten, substância proteica presente no trigo e seus derivados. O controle desta doença é feito através da total restrição ao glúten, ou seja, os celíacos não podem consumir qualquer tipo de alimento que contenha farinha de trigo. A farinha de arroz é um bom substituto do trigo na elaboração de pães livres de glúten, no entanto, a farinha de arroz produz pães de pouco volume, pois não possui as mesmas características tecnológicas do glúten, principalmente para a elaboração de pães. Desta forma, vários aditivos têm sido usados para melhorar a qualidade dos pães feitos com farinha de arroz, dentre eles enzimas, gomas ou hidrocolóides, amidos modificados e outras fontes proteicas. Para aumentar o teor proteico e melhorar a qualidade nutricional dos pães, várias fontes proteicas podem ser usadas. A alga Spirulina platensis é muito estudada para uso na alimentação humana por apresentar um bom perfil nutricional, tornando-a ideal como suplemento alimentar, pois combina diversos constituintes como proteínas, vitaminas e minerais de maneira equilibrada. Assim, o objetivo deste trabalho foi avaliar o efeito da adição da metilcelulose, enzima transglutaminase e Spirulina na qualidade tecnológica e nutricional de pães de farinha de arroz. Para isso foi utilizado um delineamento central composto rotacional (DCCR) a fim de avaliar os efeitos tecnológicos da adição de metilcelulose, transglutaminase e Spirulina nos pães de farinha de arroz. As respostas do planejamento possibilitaram definir concentrações adequadas destes aditivos para a obtenção dos pães A, B e C com boas características tecnológicas, que foram avaliados pela composição proximal e sensorialmente por teste de preferência. A avaliação sensorial dos pães de farinha de arroz mostrou que a preferência dos consumidores independe da quantidade de Spirulina adicionada ao pão. A enzima transglutaminase teve maior eficiência na formação de ligações cruzadas na massa fermentada dos pães de farinha de arroz quando foi utilizada a concentração de 0,6% (em base à farinha de arroz), mas a proteína da Spirulina não aumentou a formação de “rede”. Através da microscopia eletrônica de varredura (MEV) das massas fermentadas dos pães foi verificado que a transglutaminase torna a microestrutura da massa mais compactada, enquanto que a proteína da Spirulina forma estruturas fibrosas na massa. A avaliação nutricional do pão de arroz com Spirulina através de ensaio biológico utilizando ratos Wistar mostrou que a adição de Spirulina (4% em base de farinha) não provocou aumento do valor proteico, mas o valor de coeficiente de eficiência alimentar (CEA) não diferiu da dieta controle com caseína. / Celiac disease is an illness caused by intolerance to gluten which is a protein substance found in wheat and its derivatives. The control of this disease is made by complete restriction to gluten, in other words, celiac people cannot eat any food containing wheat flour. Rice flour is a good substitute for wheat in the preparation of gluten free breads, however, the rice flour produces low volume breads once it does not have the same technological characteristics of gluten, especially for the preparation of breads. Thus, various additives have been used to improve the quality of rice flour breads, including enzymes, hydrocolloids or gums, modified starches and other protein sources. To increase the protein content and improve the nutritional quality for the breads, various protein sources may be used. The alga Spirulina platensis is widely studied for the use as food for human because it has a good nutritional profile so it becomes an ideal feed supplement, since it combines various constituents such as protein, vitamins and minerals in a balanced way. The objective of this study is to evaluate the effect of adding methylcellulose, Spirulina and transglutaminase enzyme on technological and nutritional quality of rice flour breads. The Rotational Central Composite Design (RCCD) method was used to assess the technological effects of adding methylcellulose, transglutaminase and Spirulina in rice flour breads. Responses from planning made it possible to define appropriate concentrations of these additives to obtain the A, B and C breads with good technological characteristics that were evaluated by proximate composition and sensory by means of preference test. The sensory evaluation of rice flour breads showed that consumers' preference is independent of the amount of Spirulina added to bread. The transglutaminase enzyme was more efficient at the crosslinking established in the sourdough of rice flour breads when the concentration of 0.6% (rice flour based) was used, but the Spirulina protein did not increase the network formation. By scanning electron microscopy (SEM) of the fermented dough of breads was found out that the mass microstructure becomes more compacted due to the transglutaminase enzyme while the Spirulina protein forms fibrous structures in the mass. The nutritional evaluation of the Spirulina based rice bread made through a biological test using rats showed that the addition of Spirulina (4% on flour basis) resulted in no increase for the protein value, but the amount of Food Efficiency Ratio (FER) did not differ from the control diet.

The aim of this doctoral thesis is to verify a possibilities of fibercement extrusion. A mixture for extrusion is typical for its high toughness and high fiber content, as the fiber content may be several times higher than when utilizing other production methods. The technology of a twin shaft kneader makes it possible to produce homogenous mixture for extrusion with low water/cement ratio. With use of auger moulder a mixture of high toughness is formed to final shape. The extreme shear and pressure stress is applied in the process. Therefore high requirements are posed on the equipment.

Combination of fine ground granulated slag with proper alkaline activator gives alkali-activated slag – a material with remarkable properties. Theoretical part of the thesis deals with summarizing basic informations about alkali-activated slag, its properties, production and utilization. It also follows research devoted to effects of curing of alkali activated slag and shrinkage-reducing admixtures on its properties. Objective of the experimental part is to determine the influence of curing conditions on the mechanical properties and microstructure of alkali-activated slag. These properties are also monitored in alkali-activated slag with carbon nanotubes and hydroxypropylmethylcellulose as an shrinkage-reducing admixtures.

Polymers with mucoadhesive properties are universally used in the development of mucoadhesive drug delivery system. Their physicochemical properties as well as the mechanisms related to their adhesive actions draw great attention for the modification of mucoadhesive properties. In this study, relationships between physicochemical properties of hydroxypropyl methylcellulose (HPMC) compacts and mucoadhesive performance were investigated. Different commercial grades of HPMC (K3, E3, E5, E50, K4M, E4M and K15M) were prepared into compacts, and their surface hydrophilicity and hydration behavior were characterized. The in vitro mucoadhesive performance was determined by the tension strength between the compacts and different regions of mucous membrane (buccal, sublingual, stomach, and intestine). Positive correlations were found between: (1) viscosity of HPMC compacts and contact angle values measured by different simulated body fluids; (2) viscosity of HPMC compacts and in vitro mucoadhesive force; (3) contact angle values and in vitro mucoadhesive force. The hydration behavior exhibited improvement with the increasing viscosity of HPMC compacts. Moreover, the polar lipid content of each mucosa was likely an important factor affecting the mucoadhesion phenomenon. Different ratios of ethyl cellulose (EC) was mixed with HPMC grade K15M to form combination compacts for the purpose of modifying the surface property. The mucoadhesive mechanism of both different grades of HPMC compacts and combination compacts were studied via the thermodynamic analysis of Lifshiz-van der Waals interaction and Lewis acid-base interaction. The total free energy of adhesion (〖∆G〗^TOT) provided a prediction of an overall tendency of mucoadhesion, however, the results were showing disagreement with the measured mucoadhesive force. In general, the involving of EC in the combination compacts did not give a boost to the whole mucoadhesive performance.

Emulsioner bildas då två vätskor som normalt sätt inte blandas med kraft vispas samman för att distribuera den ena vätskan i den andra. För att dessa vätskor inte efter avslutad vispning ska gå isär kan emulgeringsmedel tillsättas, till exempel polysackarider som hör till hydrokolloiderna. Hydrokolloider används inom livsmedelsindustrin för sin förmåga att påverka ett livsmedels reologiska egenskaper, så som viskositet och textur. Exempel på hydrokolloider som används inom den växtbaserade livsmedelsbranschen är derivat av cellulosa så som metylcellulosa. Metylcellulosan har egenskaper som löslighet i vatten samt termoreversibel gelatinering. Med detta menas att en lösning med metylcellulosa efter uppvärmning kommer att bilda en gel, men så fort temperaturen sjunker kommer viskositeten minska, och försvinna helt. Den huvudsakliga anledningen som ligger bakom intresset att utvärdera stabiliteten hos hydrokolloider är dagens allt större efterfrågan på växtbaserade proteinalternativ som efterliknar egenskaper hos de animaliska alternativen. Just stabiliteten av hydrokolloiderna är något som är svårt att utvärdera, men då kunskapen om konsistensgivare så som hydrokolloider blir allt större, ökar även möjligheten till bättre och fler modifierade proteinalternativ. Något som kan locka en större grupp konsumenter. Försöken som genomfördes gjordes med syftet att utvärdera egenskaperna hos metylcellulosa som konsistensgivare i en köttersättningsmix. En avgörande faktor vid beredningen är att kontrollera temperaturen. I försöken var den initiala temperaturer vid beredningen av emulsionerna innehållandes vatten, olja samt metylcellulosa antingen under 4°C eller över 4°C (10-15°C). Utöver detta  genomfördes även försök vid pH 5 samt pH 5,5. Metoder för att utvärdera stabiliteten hos emulsionerna utvecklades också. Data som erhölls bearbetades statistiskt och det visade sig att emulsioner tillverkade under 4°C hade en högre stabilitet än de som tillverkats vid temperaturer över 4°C. Skillnaden i stabilitet vid olika pH (pH 5,0 och pH 5,5) var däremot inte signifikant, men då försöken endast genomfördes med emulsioner med olja, vatten och metylcellulosa går det inte att med säkerhet säga att pH inte har någon signifikant effekt i en slutprodukt som även innehåller proteiner, stärkelse och kryddor. / Emulsions are formed when two liquids that does not combine naturally are mixed with force to distribute one liquid in the other. To prevent these liquids from separating when the mixing ends emulsifiers can be added, for example polysaccharides such as hydrocolloids. Hydrocolloids are used in the food industry for their ability to influence the rheological properties of a food, such as viscosity and texture. Examples of hydrocolloids used in the plant based food industry are cellulose derivates, such as methylcellulose. Methylcellulose has properties such as solubility in water and thermoreversible gelatinization. This means that the solution containing methylcellulose after heating will form a gel, but as soon as the temperature drops, the viscosity will decrease and vanish completely. The main reason to why a study of the stability in hydrocolloids is of interest is today's increasing demand for plant-based protein alternatives that largely have similar properties to the animal alternatives. The stability of hydrocolloids has previously been difficult to evaluate, but as knowledge about sensory enhancers such as hydrocolloids grows, so does the possibility of producing better and more reconstructed protein alternatives. Thus attracting a larger consumer group. The experiments that was carried out aimed at the evaluation of properties of methylcellulose as a sensory enhancer in a meat substitute mix. A critical point in the preparation is to control the temperature. The initial temperature during preparation of the emulsions containing water, oil and methylcellulose was either below 4°C or above 4°C (10-15°C). In addition, experiments were also performed at pH 5 and pH 5.5. Methods to measure the stability of the emulsions were also developed. The data obtained were processed statistically and the results indicated that emulsions prepared below 4°C had a higher stability than those prepared at temperatures above 4°C. Difference in stability due to pH, on the other hand, was not significant, but since the experiments were carried out with emulsions only containing oil, water and methylcellulose it is not possible to say with certainty that pH has no significant effect in a product containing more components such as protein, starch and spices.

La fonctionnalisation d'emballages biodégradables avec des antioxydants naturels est l'une des techniques prometteuses pour améliorer la conservation des aliments, diminuer la quantité de conservateurs chimiques utilises, protéger la dégradation aromatique des produits et ainsi conserver une meilleure qualité globale. Le contrôle du relargage de ces composés actifs de l'emballage vers l'aliment permet d'étendre l'efficacité de la fonctionnalisation en libérant progressivement les antioxydants à la surface de l'aliment. L'objectif global de ce travail était de fonctionnaliser le polymère HPMC afin de produire un film d'emballage coloré à activité antioxydante et d'évaluer son aptitude à servir d'emballage actif. Tout d'abord, des films d'HPMC contenant différents colorants synthétiques comme le bleu, le vert, le jaune, le rouge et le blanc ont été testés afin de déterminer la couleur la plus adaptée pour le contrôle de la photo-oxydation de produits gras. Ensuite, la couleur rouge synthétique, montrant un maximum de contrôle contre la photo-oxydation, a été remplacée par des composés actifs naturels de même couleur. Ces composés provenaient soit d'un mélange d'extraits de betterave et de carottes pourpres, d'un mélange de bétalaïnes soit d'un mélange d'anthocyanes. Le mode d'incorporation de ces composés actifs dans la matrice d'HPMC, leurs effets sur les propriétés thermiques, mécaniques, barrière et structurales des films ont été étudiés. Les résultats ont montré que l'intégration de ces différents composés actifs naturels a permis d'améliorer les propriétés des films. Les composés actifs utilisés ont la capacité de contrôler le photo-vieillissement de la matrice polymérique et que l'HPMC est un bon candidat pour incorporer ces molécules et permettre le contrôle de la dégradation de produits alimentaires riches en lipides / Biodegradable packaging functionalized with natural antioxidants is one of the promising techniques to enhance foods shelf-life, lower use of preservatives in food formations, higher protection of flavours and higher food qualities. Controlled release of these bioactive compounds from packaging to food surface provides longer food stability by continuously librating antioxidants at food surface. The overall objective of the present work was to functionalize the HPMC polymer as colored antioxidant packaging and investigate its suitability as active packaging for unsaturated lipids. Firstly, HPMC films containing different synthetic colours like blue, green, yellow, red and white were tested to chose a suitable color having control against photo-oxidation. Secondly, red synthetic color (showing maximum control against pho-oxidation) was replaced by natural active red compounds including "natural red color" (beetroot extract + purple carrot extract), betalains and anthocyanins to produce bioactive food packaging. Mode of incorporation of these active compounds in HPMC matrix and also their potential effects on thermal, mechanical, barrier and structural properties of films were investigated. Controlled release kinetics, antioxidant capacity and light stability of bioactive compounds in HPMC films were also investigated. The overall results showed that successful incorporation of different natural active compounds have capability to improve film properties. The active compounds under discussion have ability to control photo ageing of polymer matrix and HPMC has the capability for being a suitable carrier for antioxidant active packaging for some food products

Aerogéis de hidroxipropil metilcelulose (HPMC) com diferentes graus de substituição por grupos metila (DS) e hidroxipropila (MS) foram preparados por liofilização utilizando diferentes ácidos como agentes de reticulação, a saber: ácido cítrico, ácido oxálico e ácido tereftálico. Nanocristais de celulose bacteriana (BCN) neutros e negativamente carregados foram utilizados como carga de reforço nas concentrações de 5% (m/m) e 15% (m/m) em relação à massa da matriz. Os resultados indicaram que HPMCs com menores valores de DS e maiores valores de MS resultam em aerogéis com maior eficiência na reticulação. Além disso, agentes de reticulação insolúveis em água minimizaram a capacidade de reticulação, enquanto agentes de reticulação com uma maior quantidade de grupos funcionais ácidos aumentaram a probabilidade e a eficiência da reação de reticulação das cadeias de HPMC. Os aerogéis apresentaram alta estabilidade em água, solventes orgânicos e meio ácido, além de apresentar resiliência quanto à deformação em meio aquoso. Os aerogéis apresentaram porosidade de ~98%, densidade média variando de 0,021 à 0,026 (± 0,002) g.cm-3, módulo de Young variando de 101 à 150 (± 19) kPa e capacidade média de absorção de água de 18 g de água/g de aerogel. A adição de carga de reforço resultou em um aumento de até 13% na densidade aparente do aerogel e um aumento médio de 20% no módulo de Young dos materiais. A morfologia dos poros dos aerogéis sintetizados é irregular, com ampla faixa de distribuição de tamanho de poros, podendo variar cerca de 5 µm a 500 µm. Nos aerogéis reforçados, as BCNs encontram-se preferencialmente no interior das paredes dos aerogéis, onde o reforço mecânico é mais eficiente. Isotermas de adsorção de 17α-etinilestradiol (EE) foram realizadas, resultando em capacidades de remoção de até 90%, com possibilidade de reciclo. As isotermas indicam que a matriz HPMC J5MS possui maior afinidade para adsorção de EE e que a adição de BCNs aumenta a afinidade das moléculas pelo substrato. As isotermas foram melhor ajustadas com o modelo de Freundlich, indicando que a adição de 5% de BCNs aumenta a capacidade de adsorção do aerogel, enquanto a adição de 15% de BCNs provoca uma diminuição nesta propriedade. / Aerogels of Hydroxypropyl methylcellulose (HPMC), with different degrees of substitution for methyl groups (MS) and hydroxypropyl groups (DS) were prepared by freeze-drying. The HPMCs were combined with three organic acids as crosslinking agents: citric acid, oxalic acid and terephthalic acid. Bacterial cellulose nanocrystals (BCN) neutral and negatively charged were used as reinforcement particles from 5% to 15% m/m in relation to the polymer mass. The results indicated that HPMC with lower DS and higher MS levels result in aerogels with higher crosslink efficiency. Besides that, crosslinking agents that are water insoluble minimized the crosslinking capacity, while crosslinking agents with more functional acid groups presented higher probability and efficiency in the crosslinking reaction. The aerogels presented high stability in water, organic solvents and acid media, and presented mechanical resilience in aqueous media. The resulting aerogels presented porosity of ~98%, average density of 0.021 to 0.026 (± 0.002) g.cm-3, Young modulus of 101 to 150 (± 19) kPa and an average capacity of water absorption of 18 g of water/g of aerogel. The addition of reinforcement particles resulted in an increase in density up to 13% and an average increase in the Young modulus of 20%. The morphology of the aerogels was irregular, with a wide pore size distribution, varying between de 5 µm a 500 µm. In the reinforced aerogels, the BCNs were found preferably inside the aerogels walls, were the mechanical reinforcement is more efficient. Adsorption isotherms of 17 ethinyl estradiol (EE) revealed removal capacity up to 90% and possibility of adsorbent recycling. The isotherms indicated that the HPMC J5MS has higher affinity for EE molecules and that the use of BCNs increases aerogels affinity. The isotherms were well fitted with the Freundlich model, indicating that the addition of 5% BCN increases the adsorption capacity of the aerogels, while the addition of 15 % BCN results in a decrease in this property.

Aerogéis de hidroxipropil metilcelulose (HPMC) com diferentes graus de substituição por grupos metila (DS) e hidroxipropila (MS) foram preparados por liofilização utilizando diferentes ácidos como agentes de reticulação, a saber: ácido cítrico, ácido oxálico e ácido tereftálico. Nanocristais de celulose bacteriana (BCN) neutros e negativamente carregados foram utilizados como carga de reforço nas concentrações de 5% (m/m) e 15% (m/m) em relação à massa da matriz. Os resultados indicaram que HPMCs com menores valores de DS e maiores valores de MS resultam em aerogéis com maior eficiência na reticulação. Além disso, agentes de reticulação insolúveis em água minimizaram a capacidade de reticulação, enquanto agentes de reticulação com uma maior quantidade de grupos funcionais ácidos aumentaram a probabilidade e a eficiência da reação de reticulação das cadeias de HPMC. Os aerogéis apresentaram alta estabilidade em água, solventes orgânicos e meio ácido, além de apresentar resiliência quanto à deformação em meio aquoso. Os aerogéis apresentaram porosidade de ~98%, densidade média variando de 0,021 à 0,026 (± 0,002) g.cm-3, módulo de Young variando de 101 à 150 (± 19) kPa e capacidade média de absorção de água de 18 g de água/g de aerogel. A adição de carga de reforço resultou em um aumento de até 13% na densidade aparente do aerogel e um aumento médio de 20% no módulo de Young dos materiais. A morfologia dos poros dos aerogéis sintetizados é irregular, com ampla faixa de distribuição de tamanho de poros, podendo variar cerca de 5 µm a 500 µm. Nos aerogéis reforçados, as BCNs encontram-se preferencialmente no interior das paredes dos aerogéis, onde o reforço mecânico é mais eficiente. Isotermas de adsorção de 17α-etinilestradiol (EE) foram realizadas, resultando em capacidades de remoção de até 90%, com possibilidade de reciclo. As isotermas indicam que a matriz HPMC J5MS possui maior afinidade para adsorção de EE e que a adição de BCNs aumenta a afinidade das moléculas pelo substrato. As isotermas foram melhor ajustadas com o modelo de Freundlich, indicando que a adição de 5% de BCNs aumenta a capacidade de adsorção do aerogel, enquanto a adição de 15% de BCNs provoca uma diminuição nesta propriedade. / Aerogels of Hydroxypropyl methylcellulose (HPMC), with different degrees of substitution for methyl groups (MS) and hydroxypropyl groups (DS) were prepared by freeze-drying. The HPMCs were combined with three organic acids as crosslinking agents: citric acid, oxalic acid and terephthalic acid. Bacterial cellulose nanocrystals (BCN) neutral and negatively charged were used as reinforcement particles from 5% to 15% m/m in relation to the polymer mass. The results indicated that HPMC with lower DS and higher MS levels result in aerogels with higher crosslink efficiency. Besides that, crosslinking agents that are water insoluble minimized the crosslinking capacity, while crosslinking agents with more functional acid groups presented higher probability and efficiency in the crosslinking reaction. The aerogels presented high stability in water, organic solvents and acid media, and presented mechanical resilience in aqueous media. The resulting aerogels presented porosity of ~98%, average density of 0.021 to 0.026 (± 0.002) g.cm-3, Young modulus of 101 to 150 (± 19) kPa and an average capacity of water absorption of 18 g of water/g of aerogel. The addition of reinforcement particles resulted in an increase in density up to 13% and an average increase in the Young modulus of 20%. The morphology of the aerogels was irregular, with a wide pore size distribution, varying between de 5 µm a 500 µm. In the reinforced aerogels, the BCNs were found preferably inside the aerogels walls, were the mechanical reinforcement is more efficient. Adsorption isotherms of 17 ethinyl estradiol (EE) revealed removal capacity up to 90% and possibility of adsorbent recycling. The isotherms indicated that the HPMC J5MS has higher affinity for EE molecules and that the use of BCNs increases aerogels affinity. The isotherms were well fitted with the Freundlich model, indicating that the addition of 5% BCN increases the adsorption capacity of the aerogels, while the addition of 15 % BCN results in a decrease in this property.

Fundação de Amparo a Pesquisa do Estado de Minas Gerais / In this work, methylcellulose (MC) was produced from sugarcane bagasse cellulose by heterogeneous route in alkaline medium, according to two methodologies: i) reaction with DMS, successive exchange of reagents and a step of mercerization and ii) reaction with iodomethane in two steps of mercerization. The synthesized methylcelluloses and a commercial methylcellulose sample, used as standard, have been evaluated as admixtures for adhesive mortars in civil construction by 2 methods, being added as a suspension in water (method 1) and in the powder form, dispersed in the mortar during its preparation (method 2). One of the main points of innovation of this study was to apply the polymers as a powder during mortar preparation, so that it approaches the commercial adhesive mortars, which consist of mixtures pre-dosed powder. In this study, methylcellulose produced using DMS (MCD), iodomethane (MCI) and commercial methylcellulose (MCC) were characterized according to their degree of substitution (DS) by chemical route, by Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD), Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA) and viscosity measurements. The modifications observed in the FTIR spectra showed the efficiency of methylation processes using DMS and iodomethane. The samples showed differences in water solubility, MCI was more soluble, and related to the crystallinity, the MCD presented more crystalline pattern and MCI more amorphous. The MCD was more thermally stable. The adhesion of mortars prepared by method 1 was close to the values obtained for reference mortar, particularly only to the MCD sample that increased by about 28% compared to reference. For the mortars produced by method 2, the direct addition of polymers effectively changed the properties of mortars, especially in relation to the adhesion, that increased by approximately 23% to mortar containing MCI, about 70% for MCD and 20% for MCC. It is observed that MCD samples perform best in all tests, this may be related to the higher DS for this sample, which favors the gel formation and the water retention, making the mortar more viscous and \"sticky\", altering the interactions between mortar and substrate and increasing the adhesion. / Neste trabalho, a metilcelulose (MC) foi produzida a partir da celulose extraída do bagaço de cana-de-açúcar pela rota heterogênea em meio alcalino. Foram empregadas duas metodologias de síntese: i) reação com sulfato de dimetila (DMS), troca sucessiva de reagentes e uma etapa de mercerização e ii) reação com iodometano e duas etapas de mercerização. As amostras de MC produzidas e uma amostra de MC comercial, utilizada como padrão, foram avaliadas como aditivos para argamassas colantes na construção civil por 2 métodos, sendo adicionadas às argamassas como uma suspensão em água (método 1) e na forma de pó, disperso diretamente na argamassa durante sua preparação (método 2). Um dos principais pontos de inovação deste trabalho foi a aplicação dos polímeros na forma de pó durante a preparação das argamassas, forma essa que se aproxima das argamassas colantes comerciais que consistem em misturas pré-dosadas em pó. Neste estudo, as amostras de metilcelulose produzidas usando DMS (MCD), iodometano (MCI) e a amostra de metilcelulose comercial (MCC) foram caracterizadas quanto ao seu Grau de Substituição (GS) por via química, pelas técnicas de Espectroscopia de Infravermelho com Transformada de Fourier (FTIR), Difratometria de Raios-X (DRX), Calorimetria Exploratória Diferencial (DSC), Análise Termogravimétrica (TGA), Microscopia Eletrônica de Varredura (MEV) e por medidas de viscosidade. As modificações observadas nos espectros de FTIR mostraram a eficiência dos processos de metilação usando DMS e iodometano. As amostras apresentaram diferenças quanto à solubilidade em água, sendo a amostra MCI mais solúvel, e quanto à cristalinidade, a MCD apresentou um padrão mais cristalino e a MCI mais amorfo. A amostra MCD apresentou a maior estabilidade térmica. A adesão das argamassas preparadas pelo método 1, foi próxima dos valores da argamassa de referência, com destaque apenas para a MCD que apresentou aumento de cerca de 28%. Para as argamassas produzidas pelo método 2, a adição direta dos polímeros modificou efetivamente as propriedades das argamassas, principalmente em relação à aderência, que aumentou cerca de 23% para a argamassa com MCI, 70% para MCD e 20% para MCC. A amostra MCD apresentou o melhor desempenho em todos os ensaios, fato que pode estar relacionado ao seu maior GS, que favorece a formação de gel e a retenção de água pela argamassa, tornando-a mais viscosa e pegajosa , alterando as interações da argamassa com o substrato e consequentemente, aumentando a aderência. / Doutor em Química