Embora a soja em grão seja pouco consumida pela população brasileira, seus derivados protéicos são utilizados como ingredientes em diversos alimentos e a tendência é um aumento significativo do seu uso com a aprovação pela FDA e pela ANVISA da alegação funcional referente ao consumo de proteína de soja. Em paralelo, um número crescente de pesquisas sobre as isoflavonas, fitoestrógenos presentes em quantidades significativas na soja, vem demonstrando diversos efeitos benéficos destes compostos, entre os quais a sua ação antioxidante, anticarcinogênica e hipocolesterolêmica. O objetivo foi estudar as interações entre isoflavonas e proteínas da soja, seu efeito na biodisponibilidade in vitro e in vivo e o status antioxidante das isoflavonas. Os resultados sugerem que a presença da proteína reduz a quantidade e leva a um retardo no tempo de absorção das isoflavonas em relação à administração na forma livre. O efeito sobre a capacidade antioxidante do plasma e sobre a atividade e expressão gênica das enzimas CAT, GPx e SOD divergiu para a suplementação de isoflavonas ou proteínas separadamente ou em associação. / Although soybeans are not commonly consumed by the Brazilian population, soybean products are used as ingredients by the food industry and there is an increased trend in their consumption due to the approval of FDA and ANVISA on the claim regarding the health benefits of soy proteins. Therefore, many studies involving isoflavones, the phytoestrogens found in significant quantities in soybeans, have demonstrated several health benefits of these compounds, such as antioxidant capacity, and anticarcinogenic and hypocholesterolemic effects. The objective of the present study was to evaluate the interaction between isoflavones and soy proteins as well as the effect of this interaction on the in vitro and in vivo bioavailability of isoflavones and on the antioxidant status. The results indicated that the association with protein decreased the rate and proportion of absorption of isoflavones when compared to the free form. The effect of isoflavones on the plasma antioxidant capacity and on the enzymatic activity and gene expression levels of CAT, GPx and SOD was different when isoflavones were combined with soy protein compared to isoflavones alone.

<p>Detection of pathogens, toxins, hazardous chemicals, and allergens in the food industry with reliable, sensitive, efficient, and rapid results has increased the demand to develop innovative diagnostic tools. Surface-enhanced Raman spectroscopy (SERS) sensors have demonstrated to detect a wide variety of analytes using nanomaterials like metal nanoparticles. Concerns of synthetic materials that can affect the environment with disposal of sensors have opened the possibility of fabricating SERS sensors with biodegradable materials. Fabrication of electrospun nanofibers from natural polymeric materials such as soy protein isolate can be used as a SERS platform. In the first part of this research, the characteristics of SPI solutions blended with NaOH and polyethylene oxide (PEO) such as PEO Mw, zeta potential and viscosity as well operating parameters such as voltage (15, 20, and 27 kV) were studied to evaluate the best solutions for a nanofibrous SERS platform. Characteristics of electrospun nanofibers, such as surface wettability, fiber diameters, and morphology using SEM, helped determine the most feasible fibers for decoration with noble metal nanoparticles. Fibers fabricated with 12 wt% SPI + 5 wt% PEO (0.1 MDa) + 1 wt% NaOH solution showed the smallest fiber diameter and highest water contact angle measurements. Glutaraldehyde (GLA) was added as a crosslinker to partly increase nanofibers hydrophobicity. These nanofibers were decorated with Au-nanostars and Au@Ag-NPs suspended in 90% butanol and in water. Partly hydrophobic nanofibers decorated with Au-nanostars and Au@Ag-NPs in butanol showed the most feasible results for a SERS platform due to smallest fiber diameter and higher water contact angle. In the second part of this research, decorated SPI nanofibers were evaluated to study its feasibility as a SERS platform for detecting bisphenol A (BPA), a toxic chemical present in food packaging materials. However, SERS spectra were difficult to obtain due to CCD overflow (excessive number of photons) at all laser powers on SPI nanofiber mats. Optimizing other Raman spectroscopy parameters such as the exposure time and the number of averages could enhance the SERS measurements. The fabricated SPI nanofibers in this research showed that hydrophilic and partly hydrophobic nanofibers mats could be used for decoration with metal nanoparticles by suspending the nanoparticles in a hydrophobic solvent. Hydrophilic nanofiber mats with nanoparticles in a hydrophobic solvent open a new strategy for developing another type of SERS platform.</p>

Os isolados protéicos de soja são utilizados como ingredientes em diversos alimentos e sua utilização vêm aumentando juntamente com o aumento das pesquisas sobre os metabólitos secundários da soja, as isoflavonas. Alguns efeitos benéficos vem sendo associados às isoflavonas, entre estes a sua ação antioxidante, a redução ao risco de câncer, doenças cardiovasculares e osteoporose. O objetivo deste estudo foi o de otimizar as condições de extração das isoflavonas e de suas formas conjugadas a partir da farinha desengordurada de soja, visando o preparo de isolado protéico de soja. Os resultados mostraram que a obtenção de isolados protéicos de soja com teor aumentado de isoflavonas depende da utilização de condições brandas de centrifugação para a separação do precipitado isoelétrico, assim como da utilização de água acidificada na sua lavagem. A presença de isoflavonas no isolado resulta de três fatores, o primeiro referindo-se à associação entre isoflavonas e proteínas através de interações hidrofóbicas, eletrostáticas, e pontes de hidrogênio; o segundo à menor solubilidade das isoflavonas presentes na farinha desengordurada de soja no pH isoelétrico; e o último ao processo de carreamento (físico) das isoflavonas pelas proteínas insolubilizadas. / Soy protein isolates are used as ingredients in several food products and their use is increasing together with the increase of the researches on the secondary metabolites of soy, the isoflavones. Some beneficial effects have been associated to the isoflavones, among these their antioxidant action, prevention of cancer, cardiovascular diseases and osteoporosis. The objective of this study was to optimize the extraction conditions of the isoflavones from the defatted soy flour, seeking the preparation of soy protein isolates. The results showed that the obtention of soy protein isolates with increased content of isoflavones depends on the use of mild conditions of centrifugation for the separation of the isoelectric precipitate, as well as on the use of water acidified in the washing step. The presence of isoflavones in the isolates resulted from three factors, the first refers to the association between isoflavones and proteins through hydrophobic; and electrostatic interactions, and hydrogen bonding; the second to the decreased solubility of the isoflavones extracted from the defatted soy flour in the isoelectric pH; and the last to the carrying process (physical) of isoflavones by the precipitating proteins.

The application of current soy protein films are limited due to their low mechanical strength and high moisture sensitivity compared to synthetic materials. This research studied several methods to improve the mechanical properties [tensile strength (TS), elongation at break (EAB), Young’s modulus of elasticity (YM)] of solvent cast soy protein isolate (SPI) films. Drying times were significantly reduced through the use of a heated casting surface. Neutral (pH 7) SPI films were prepared but were found to have lower TS, EAB and YM than control films prepared under alkaline conditions. Cellulose was extracted from soybean wastes and transmission electron microscopy (TEM) verified the existence of nano-sized fibres. Composite SPI films were prepared using either extracted cellulose fibres or titanium dioxide (TiO2) nanoparticles and their mechanical and barrier properties (water vapour, and oxygen permeability) were evaluated under different relative humidity (RH) conditions. In general, TS and YM decreased and EAB increased with increasing RH. Films with 5% (w/w) added cellulose exhibited significant (p-value < 0.05) improvements in TS and YM but decreased EAB. TiO2 composites possessed similar TS, YM, and EAB values to control films. Barrier properties were comparable across all samples, and decreased with increasing RH. Samples were characterized using Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and atomic force microscopy (AFM). Preliminary work investigating synthesis of filler materials using cross-linked sodium alginate particles increased the TS and YM of SPI films to a similar extent as extracted cellulose. A method for electrospinning cellulose using ionic liquids was developed, but requires further process optimization to be used for fibre/filler synthesis. / OMAFRA; Hannam Soy Utilization Fund

Orientador: Fernanda Paula Collares / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-06T15:44:35Z (GMT). No. of bitstreams: 1 UclesSantos_JoseRicardo_M.pdf: 2719947 bytes, checksum: c27f8219ba712b28246c216abd73b478 (MD5) Previous issue date: 2006 / Resumo: O pão de queijo, um produto tipicamente brasileiro, é considerado um produto de panificação que não contém glúten, pois em sua formulação não é utilizada farinha de trigo e sim fécula nativa de mandioca ou fécula de mandioca fermentada naturalmente e/ou modificada. Devido ao seu alto teor de carboidratos, possui grande aceitabilidade e pode ser utilizado por pessoas portadoras de doença celíaca. O alto consumo deste produto no Brasil e a procura crescente dos consumidores por produtos alimentícios não somente nutritivos e saborosos, mas que também tragam benefício à saúde, estimula o estudo da incorporação de ingredientes nutricionais e funcionais à massa de pão de queijo que não afetem suas propriedades reológicas, físicas e sensoriais. O objetivo deste trabalho, portanto, foi avaliar o efeito da incorporação de componentes nutricionais e funcionais, como o isolado protéico de soja e a polidextrose, na qualidade da massa e do pão de queijo assado, com e sem adição de fécula de mandioca pré-gelatinizada, visando determinar quais dos teores adicionados de cada um destes ingredientes conferem as melhores características físicas e sensoriais ao pão de queijo. Para atingir este objetivo, o trabalho foi dividido em três etapas: (i) avaliação do teor adequado de fécula de mandioca e polvilho azedo adicionado à formulação de pão de queijo, através da determinação de suas propriedades físicas, reológicas e sensoriais; (ii) análise do efeito combinado dos ingredientes nutricionais e funcionais incorporados à massa de pão de queijo com diferentes teores de fécula de mandioca e polvilho azedo, com e sem a etapa de escaldamento, nas suas propriedades reológicas, físicas e sensoriais, utilizando a metodologia de superfície de resposta; (iii) caracterização física, química, reológica e sensorial das formulações de pão de queijo, com e sem a adição de fécula de mandioca pré-gelatinizada, escolhidas no item anterior. Na primeira etapa do trabalho, massas elaboradas com teores de 70% e 100% de fécula de mandioca apresentaram maiores consistências em U.F. em relação às massas elaboradas com altos teores de polvilho azedo, durante o processo de mistura similado no farinógrafo Brabender. Os pães de queijo elaborados com altos teores de polvilho azedo apresentam coeficientes de expansão de até 80,00%, sendo que os pães elaborados com fécula de mandioca apresentaram valor máximo de expansão de 66,67%. Devido a este poder de expansão apresentado pelos pães de queijo elaborados com polvilho azedo, a força de compressão (textura dos pães) obtida foi de 7,85% a 28,40% menor à reportada para pães de queijo elaborados com fécula de mandioca. Sensorialmente, os pães de queijo elaborados com altos teores de fécula de mandioca apresentaram as maiores médias em relação aos atributos de aceitação geral, textura, cor e sabor em comparação com os pães de queijo com altos teores de polvilho azedo, que segundo os provadores lembra o biscoito de polvilho. Na segunda etapa do trabalho, foi possível a determinação de um modelo matemático para o volume específico dos pães de queijo elaborados com adição de fécula de mandioca pré-gelatinizada, e para o ângulo de tonalidade do miolo (h) de pães de queijo elaborados sem adição de fécula de mandioca prégelatinizada, explicando a interação que existe entre as variáveis (fécula de mandioca, polvilho azedo, isolado protéico de soja e polidextrose). O modelo matemático do volume mostra que a utilização de teores entre 79,76% e 100% de polvilho azedo, 5,50% de isolado protéico de soja e teores abaixo de 1,03% de polidextrose confere grandes volumes ao pão de queijo, assim como teores de 0,00% de polvilho azedo, 5,50% de isolado protéico de soja e teores de polidextrose acima de 5,07%. Para o ângulo de tonalidade (h), o modelo matemático determinou que a utilização dos valores extremos, teores mínimo e máximo, de polvilho azedo (0,00% e 100,00%) com teores de 0,00% a 9,00% de isolado protéico de soja e teores médios de polidextrose (2,21%) na formulação de pão de queijo, conferiu altos ângulos de tonalidade do miolo. Os parâmetros de textura, luminosidade e saturação da cor da crosta e do miolo dos pães de queijo, com e sem a adição de fécula de mandioca prégelatinizada, não apresentaram diferença significativa (p=0,05), sendo que a elaboração de pães de queijo utilizando concentrações na faixa estudada não produz alterações na qualidade do produto. Na última etapa do trabalho, duas formulações de pão de queijo, selecionadas na 2a etapa considerando os escores sensoriais de aparência geral, textura, aroma e sabor, foram caracterizadas física, química, reológica e sensorialmente, sendo que as duas formulações apresentaram diferença significativa (p=0,05) no perfil reológico da massa, no volume, textura e cor dos pães de queijo assados, mas sensorialmente foram igualmente aceitas pelos consumidores, quanto à aparência geral, cor do miolo, textura, aroma e sabor / Abstract: ¿Pao de queijo¿ (cheese bread), a typically Brazilian product, is considered a gluten-free bakery product, as its formulation does not contain wheat flour but native cassava starch, naturally fermented and/or modified. Due to its high content of carbohydrates, it has great acceptance and can be consumed by individuals who suffer from celiac disease. The high consumption of this product in Brazil and the growing demand, by consumers, of food products that are not only nutritious and tasty, but also bring health benefits, stimulates the study of the incorporation of nutritional and functional ingredients to cheese bread doughs, which do not affect its rheological, physical and sensorial properties. The objective of this study, therefore, was to evaluate the effect of the incorporation of the nutritional and functional components, such as soy protein isolate and the polydextrose, on the quality of cheese bread dough and of baked cheese bread, with or without the addition of pre-gelatinized cassava starch, with the objective of determining the contents of each of these ingredients that confer the best physical and sensorial characteristics to cheese bread. In order to achieve this objective, the study was divided in three phases: (i) evaluation of the appropriate content of cassava starch and sour cassava starch added to the formulation, by determining physical, rheological and sensorial properties; (ii) analysis of the combined effect of functional and nutritional ingredients incorporated to the cheese bread dough with different contents of cassava starch and sour cassava starch, with and without the scalding process, on rheological, physical and sensorial properties, using the response surface methodology; (iii) physical, chemical and rheological characterization of the cheese bread formulations, with or without the addition of pre-gelatinized cassava starch, chosen in the previous stage/step. In the first phase of the study, doughs elaborated with 70% and 100% of cassava starch presented greater consistency profiles when compared to high contents of sour cassava starch, during the mixing process simulated in the Brabender farinograph. The cheese breads elaborated with high contents of sour cassava starch presented expansion coefficients of up to 80.00%, while the cheese breads elaborated with cassava starch presented a maximum value of expansion of 66.67%. Due to this power of expansion presented by the cheese breads elaborated with sour cassava starch, the force of compression (texture of breads) obtained was 7.85% to 28.40% lower than that of those reported for cheese breads elaborated with cassava starch. Sensorially, the cheese breads produced with high contents of cassava starch presented the highest scores with respect to the attributes general acceptance, texture, color and flavor, in comparison to the cheese breads with high contents of sour cassava starch, which according to the panelists resembled the sour cassava starch biscuits (¿biscoito de polvilho¿). In the second phase of the study, it was possible to determine a mathematical model for the specific volume of cheese breads elaborated with the addition of pre-gelatinized cassava starch, and for the shade angle (h) of cheese breads elaborated without the addition of pre-gelatinized cassava starch, explaining the interaction between the variables (cassava starch, sour cassava starch, soy protein isolate and polydextrose). The mathematical model showed that the use of contents between 79.76% and 100% of sour cassava starch, 5.50 % of soy protein isolate and contents below 1.03% of polydextrose confers great volumes to cheese bread, as well as contents of 0.00% of sour cassava starch, 5.50% of soy protein isolate and contents of polydextrose above 5.07%. For the shade angle (h), the mathematical model determined that the use of extreme values, minimum and maximum contents, of sour cassava starch (0.00% and 100.0%) with contents of 0.00% to 9.00% of soy protein isolate and intermediate contents of polydextrose (2.21%) in the formulation of cheese bread conferred high shade angles to the crumb. The parameters of texture, luminescence (L*) and color saturation (C*) of the crust and crumb of the cheese breads, with and without the addition of pregelatinized cassava starch, did not present significant difference (p=0.05), indicating that the elaboration of cheese breads using the concentrations in the range studied for the different variables does not produce alterations in the quality of the product. In the last phase of the study, two formulations of cheese bread, selected in the second phase considering the sensorial scores of general appearance, aroma and flavor, were characterized physically, sensorially, rheologically and chemically. These two formulations presented significant differences (p=0.05) in the rheological profile of the dough, specific volume, texture and color of the baked cheese breads, but were equally accepted by consumers, as to general appearance, color of the cr8umb, texture, aroma and flavor / Mestrado / Mestre em Tecnologia de Alimentos

Os isolados protéicos de soja são utilizados como ingredientes em diversos alimentos e sua utilização vêm aumentando juntamente com o aumento das pesquisas sobre os metabólitos secundários da soja, as isoflavonas. Alguns efeitos benéficos vem sendo associados às isoflavonas, entre estes a sua ação antioxidante, a redução ao risco de câncer, doenças cardiovasculares e osteoporose. O objetivo deste estudo foi o de otimizar as condições de extração das isoflavonas e de suas formas conjugadas a partir da farinha desengordurada de soja, visando o preparo de isolado protéico de soja. Os resultados mostraram que a obtenção de isolados protéicos de soja com teor aumentado de isoflavonas depende da utilização de condições brandas de centrifugação para a separação do precipitado isoelétrico, assim como da utilização de água acidificada na sua lavagem. A presença de isoflavonas no isolado resulta de três fatores, o primeiro referindo-se à associação entre isoflavonas e proteínas através de interações hidrofóbicas, eletrostáticas, e pontes de hidrogênio; o segundo à menor solubilidade das isoflavonas presentes na farinha desengordurada de soja no pH isoelétrico; e o último ao processo de carreamento (físico) das isoflavonas pelas proteínas insolubilizadas. / Soy protein isolates are used as ingredients in several food products and their use is increasing together with the increase of the researches on the secondary metabolites of soy, the isoflavones. Some beneficial effects have been associated to the isoflavones, among these their antioxidant action, prevention of cancer, cardiovascular diseases and osteoporosis. The objective of this study was to optimize the extraction conditions of the isoflavones from the defatted soy flour, seeking the preparation of soy protein isolates. The results showed that the obtention of soy protein isolates with increased content of isoflavones depends on the use of mild conditions of centrifugation for the separation of the isoelectric precipitate, as well as on the use of water acidified in the washing step. The presence of isoflavones in the isolates resulted from three factors, the first refers to the association between isoflavones and proteins through hydrophobic; and electrostatic interactions, and hydrogen bonding; the second to the decreased solubility of the isoflavones extracted from the defatted soy flour in the isoelectric pH; and the last to the carrying process (physical) of isoflavones by the precipitating proteins.

Under det här kandidatexamensarbetet har protein-nanofibers påverkan på material undersökts genom att jämföra fibrillerade filmer med ofibrillerade. Sojaproteinisolat fibrillerades under förhållandena pH 2 och 85 ◦C under minst ett dygn och de syntetiserade nanofibrerna analyserades med Thioflavin T (ThT) fluorescens och atomkraftsmikroskopi (AFM). Spektra från analysmetoden ThT fluorescens indikerade på förekomsten av β-flak och analyserna med AFM visade på att fibrerna hade en morfologi som är karakteristisk för protein-nanofibrer. Resultaten antyder att de parametrar som påverkar morfologin hos fibrerna är fibrilleringstid och typ av protein. De gjutna filmerna från fibrillära respektive ofibrillära proteiner var sammanhängande bortsett från vissa sprickor. Värdena på E-modulen från AFM visade att det fibrillerade materialet var mer heterogent än det ofibrillerade. Filmer med sammanhängande yta erhölls vid tillsats av det mjukgörande additivet glycerol. Slutligen, material av både fibrillär och ofibrillär form kan framställas, däremot krävs vidare forskning för att optimera materialens egenskaper. / During this bachelor thesis project, the impact of protein nanofibers on materials has been analysed by comparing films made from fibrillar and non-fibrillar protein. Fibrillation of soy protein isolate was performed during at least 24 hours at pH 2 and a temperature of 85 ◦C. Analysis of the nanofibers was made with Thioflavin T (ThT) fluorescence and atomic force microscopy (AFM). The spectra from ThT Fluorescens indicated the presence of β-sheets and AFM confirmed that the fibrils had a morphology that is characteristic of protein nanofibers. The results indicated that heating time and protein type were the parameters which had the largest impact on the morphology of the fibrils. The synthesised films from both fibrillar and non-fibrillar protein were coherent with exception of some cracks. The elastic modulus from AFM indicated that the fibrillar film was more heterogeneous compared to the non-fibrillar film. To attain coherent films, the plasticising agent glycerol was added. To summarise, both fibrillar as well as non-fibrillar materials were successfully synthesised, however, further research is necessary to optimise the properties of the material.

<p dir="ltr">Pea protein is one of the most used plant proteins in food products, acting as an alternative to conventional animal protein sources due to its abundant, nutritious, and ease in supply chain characteristics. The objective of this study was to investigate the impact of homogenization and UHT processing parameters on the properties of protein emulsion. Protein emulsions (8% w/w pea protein isolate and 1% w/w sunflower oil) were freshly prepared prior to processing, and the untreated sample was considered as the control (NT). The pilot-scale aseptic processing system (APS) used in this study consisted of two coil-in-shell heaters and two coolers. Samples flowed through each section of the APS system following this order: balance tank, pre-heater, final heater, hold tube, pre-cooler, and final cooler. The homogenizer was located either after the pre-cooler (AC) or the pre-heater (AH) with a controlled temperature of 165F. A third setup was utilized by bypassing the homogenizer in the UHT system. An additional 8-hour continuous run was conducted to mimic a commercial manufacturing operation by recirculating the protein emulsion in the UHT system, and fouling detections were made using a non-intrusive sensor (NICS). 5% w/w soy protein, 1% w/w sunflower oil oil-in-water emulsion was also used for fouling tests. Protein concentration, pH and zeta potential, Cryo-SEM microscopic image, particle size distribution, flocculation index (FI), coalescence index (CI), viscosity and color data were collected and analyzed. The protein concentration had a 23.20 ± 4.00 %, 28.35 ± 5.02 %, 27.98 ± 5.05% and 21.38 ± 5.75% reduction for AC, AH, UHT and NT samples, respectively, when compared with the initial concentration in the formula. AC, AH, UHT and NT samples had pH values of 7.24 ± 0.01, 7.27 ± 0.01, 7.28 ± 0.02, 7.41 ± 0.01, and zeta potential values of -42.91 ± 0.89, -47.30 ± 0.91, -46.91 ± 1.40 and -50.11 ± 1.47 mV. AC sample had a smaller and NT sample had a bigger, respectively, mean weighted size D 4,3 value than AH and UHT samples, which could also be seen in Cryo-SEM images where only AC images contained more visually observable smaller particles. FI and CI for AC, AH and UHT indicated the formation of flocs but no irreversible aggregations were found. Shear-thinning AC, AH, UHT and NT samples had viscosity decreases from 4.00 to 3.56, 3.88 to 3.75, 4.02 to 3.79 and 10.42 to 9.56 mPa*s in 1 1/s to 100 1/s shear rate range. NT sample had a very noticeable color difference from the other three treated samples. Overall, AC samples had similar or better emulsion stability in all aspects than AH and UHT samples, suggesting that AC processing could potentially be used in the protein beverage industry for manufacturing products with improved shelf stability. Severe foulants buildups were neither observed nor detected by a non-intrusive continuous sensor (NICS) in the UHT system within 8 hours of process for both pea protein and soy protein emulsion, indicating that this UHT-homogenization processing can potentially be adapted to current industrial practices for higher-quality protein beverages.</p>

Formaldehyde-based adhesives have been reported to be detrimental to health. Petrochemical-based adhesives are non-renewable, limited and costly. Therefore, the improvement of environmental-friendly adhesive from natural agricultural products has awakened noteworthy attention. A novel adhesive for wood application was successfully prepared with enhanced shear strength and water resistance. The Fourier transmform infrared spectra showed the surface functionalities of the functionalized carbon nanotubes (FCNTs) and soy protein isolate nanocomposite adhesive. The attachment of carboxylic functional group on the surface of the carbon nanotubes (CNTs) after purification contributed to the effective dispersion of the CNTs in the nanocomposite adhesive. Hence, enhanced properties of FCNTs were successfully transferred into the SPI/CNTs nanocomposite adhesive. These unique functionalities on FCNTs however, improved the mechanical properties of the adhesive. The shear strength and water resistance of SPI/FCNTs was higher than that of the SPI/CNTs. SEM images showed the homogenous dispersion of CNTs in the SPI/CNTs nanocomposite adhesive. The carbon nanotubes were distributed uniformly in the soy protein adhesive with no noticeable clusters at relatively reduced fractions of CNTs as shown in the SEM images, which resulted into better adhesion on wood surface. Mechanical (shear) mixing and ultrasonication with 30 minutes of shear mixing both showed an improved dispersion of CNTs in the soy protein matrix. However, ultrasonication method of dispersion showed higher tensile shear strength and water resistance than in mechanical (shear) mixing method. Thermogravimetric analysis of the samples also showed that the CNTs incorporated increases the thermal stability of the nanocomposite adhesive at higher loading fraction. Incorporation of CNTs into soy protein isolate adhesive improved both the shear strength and water resistance of the adhesive prepared at a relatively reduced concentration of 0.3%.The result showed that tensile shear strength of SPI/FCNTs adhesive was 0.8 MPa and 7.25MPa at dry and wet state respectively, while SPI/CNTs adhesive had 6.91 MPa and 5.48MPa at dry and wet state respectively. There was over 100% increase in shear strength both at dry and wet state compared to the pure SPI adhesive. The 19% decrease in value of the new adhesive developed compared to the minimum value of ≥10MPa of European standard for interior wood application may be attributed to the presence of metallic particles remaining after purification of CNTs. The presence of metallic particles will prevent the proper penetration of the adhesive into the wood substrate. The type of wood used in this study as well as the processing parameters could also result into lower value compared to the value of European standard. Therefore, optimization of the processing parameter as well as the conversion of carboxylic acid group on the surface of the CNTs into acyl chloride group may be employed in future investigation. However, the preparation of new nanocomposite adhesive from soy protein isolate will replace the formaldehyde and petrochemical adhesive in the market and be of useful application in the wood industry. / Civil and Chemical Engineering / M. Tech. (Chemical Engineering)

Des solutions d'isolat de protéine de lactosérum (WPI) et d'isolat de protéine de soja (SPI) ont été chauffées à différentes concentrations en protéines conduisant à la formation d'agrégats fractals polydisperses de taille moyenne variable. Lastructure des solutions a été analysée par diffusion de la lumière en fonction de la concentration en protéine. La compressibilité osmotique et la longueur de corrélation dynamique diminuent quand la concentration augmente deviennent indépendantes de la taille initiale des agrégats pour les suspensions denses. Pour une taille d'agrégat donnée, la viscosité augmente initialement exponentiellement avec la concentration croissante puis diverge. Plus lesagrégats sont grands, plus l’augmentation de la viscosité apparaît à des concentrations faibles. La dépendance avec la concentration de la viscosité des solutions d'agrégats fractals est beaucoup plus forte que celle de microgels. Le comportement de mélanges de différents types d’agrégats (fractals/fractals ; fractals/microgels et WPI/SPI) a étéétudié principalement par rhéologie.Le recouvrement de fluorescence après photoblanchiment (FRAP) a été utilisé pour étudier la diffusion de chaînes de dextran marquées par des fluorophores dans des solutions d’agrégats et des gels de WPI. Une diffusion brownienne estobservée dans des suspensions d’agrégats et des gels faibles formés juste au-delà de Cg avec un coefficient de diffusion (D) qui diminue avec l'augmentation de la concentration mais, avec une dépendance plus faible que celle de la viscosité (). A des concentrations plus élevées, des gels densément réticulés sont formés, ce qui induit une forte diminution de la mobilité des chaînes de dextran. Pour ces systèmes, la recouvrance de la fluorescence est logarithmique avec le temps,suggérant une distribution exponentielle des coefficients de diffusion. La diffusion des chaînes de dextran a également été étudiée en fonction de la concentration en protéines pour les suspensions de trois types d'agrégats de WPI (petits et grands fractals et microgels). / Polydisperse fractal aggregates of varying average sizes were formed when solutions of whey protein isolate and soy protein isolate were heated at different protein concentrations and at neutral pH. The structure of these fractals aggregates solutions was analyzed by light scattering as a function of protein concentration. In dense suspension, the osmotic compressibility and the correlation length decreases with increasing concentration and become independent of the initial aggregate size. In this concentration regime, the aggregates are strongly interpenetrated and can be visualized as a set of "blobs". For a fixed aggregate size, the viscosity initially increases exponentially with increasing concentration and then diverges at the gel point. Larger fractal aggregates show a more important increase of the viscosity with increasing concentration than smaller aggregates, because they are less dense. The increase of the viscosity was much stronger for large fractal aggregates than for homogeneous microgels (microgels were formed by heating the WPI solution in present of CaCl2) of the same size.Dynamic light scattering, rheology and FRAP measurements were performed to investigate mixtures of different type of aggregates of WPI (fractals/fractals, fractals/microgels) and fractals of mixtures of WPI and SPI. Flow measurements were used to characterise the rheological properties of the aggregate suspension whereas Fluorescence recovery after Photobleaching (FRAP) was used to determine the self diffusion of fluorophore-labelled dextrans chains in mixtures over a wide range of concentrations. The results were compared to the concentration dependence of zero shear viscosity, gel stiffness, osmotic compressibility and correlation length. Brownian diffusion of the dextran chains was observed in aggregate suspensions and weak gels formed just above the gel point with a diffusion coefficient that decreased with increasing concentration, but the dependence was weaker than that of the viscosity. At higher concentrations, densely crosslinked gels were formed, which induced a sharp decrease in the mobility of the dextran chains. For these systems, the recovery of fluorescence was logarithmic over time, suggesting an exponential distribution of diffusion coefficients.