Dans ce travail, nous avons cherché à mettre en évidence l'influence de la méthode de préparation de films minces de polymère pour la biofonctionnalisation de surfaces planes. Dans un premier temps, un polymère réactif, le poly(méthacrylate de glycidyle) p(GMA) a été choisi et sa capacité de fixation vis-à-vis d'une biomolécule modèle l'albumine de sérum bovin a été étudiée. Deux stratégies principales de préparation du film polymère ont été utilisées : la technique du grafting onto et celle du grafting from avec deux voies de synthèse : la polymérisation radicalaire classique (PRC) avec l'amorceur en solution et la polymérisation initiée à partir de la surface avec un amorceur photochimique. Il a été montré que la méthode du « grafting from » permettait l'obtention de films d'épaisseur plus élevées que la technique du « grafting onto » avec une meilleure capacité de fixation de biomolécules de BSA. Ces films de p(GMA) se sont révélés relativement hydrophobes, ce qui nous incités à analyser l'influence de la balance hydrophobe/hydrophile des interfaces sur leurs propriétés, dans un second temps. Par la préparation de films copolymères poly(GMA-co-acrylamide) et poly(GMA-co-méthacrylate de glycérol) et la modification des films de poly(GMA) par de l'éthanolamine, l'influence de l'hydrophilie du film sur la capacité de fixation en molécules de BSA et l'activité de reconnaissance moléculaire de celles-ci ont été évaluées. Il a été démontré que par un choix judicieux de la méthode d'hydrophilisation du film polymère, il est possible de réduire considérablement l'adsorption non-spécifique de biomolécules d'où l'obtention de films polymères bioinertes. De plus, les résultats préliminaires ont montré qu'il est possible d'améliorer sensiblement la capacité de reconnaissance moléculaire entre la BSA et son anticorps l'anti-BSA / It is now well accepted that polymeric spacers permit to attach proteins to surfaces efficiently as they carry several binding sites. Moreover, direct attachment of proteins to surfaces might result in the decrease of bioactivity which is critical in the case of the development of biosensors. In this context, we modified gold substrates by polymer grafts via the so-called (i) grafting onto and (ii) grafting from strategies. In (i) preformed polymer chains were attached to the surface, whilst in (ii) surface-confined photopolymerization was performed on either acrylic monomer- or initiator-functionalized gold substrates. The polymer grafts were further biofunctionalized by covalent immobilization of an active protein (bovine serum albumin, BSA). Given the protein-polymer and polymer-gold covalent bonds, the gold/polymer/BSA hybrids permitted to design robust optical biosensors. The modified gold substrates were characterized in terms of chemical composition (X-ray photoelectron spectroscopy), hydrophobicity (contact angle measurements), and polymer coating thickness (surface plasmon resonance, SPR). SPR was also used to monitor in real time the interaction between the grafted antigen to the specific antibody (aBSA). Using unique reactive monomer, glycidyl methacrylate (GMA) in the present case, the implementation of these three methods is assumed to provide polymer films of similar chemical composition but varied interfacial chains conformation. In this respect, influence of polymer chains mobility on the performance of the immunosensing reaction was evaluated. In a further step, hydrophobic/hydrophilic balance of the polymer films was modulated through copolymerization of GMA with acrylamide, and with glycerol methacrylate. It was demonstrated that control over the surface chemical composition of the polymer grafts allows preparing bioinert films, i.e. resistant to non specific adsorption, with enhanced biospecific activity

Made available in DSpace on 2014-12-17T14:07:21Z (GMT). No. of bitstreams: 1 JeanneHCR.pdf: 2470228 bytes, checksum: 64b0abbe75bda944c8a21ce90a9f572b (MD5) Previous issue date: 2006-09-28 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Nowadays, composite resins are the direct restorative materials more important in dental clinical performance, due to their versatility and aesthetic excellence. Bis-GMA (2,2-bis[4(2-hydroxy-3-metacryloxypropoxy)phenil]propane) is the base monomer more frequently used in restorative composite resins. However, this monomer presents some disadvantages, such as high viscosity and two aromatic rings in its structure that can promote allergic reactions to the humans. In this work, the main purpose was to synthesize new monomers from glycidyl methacrylate to use in dental restorative materials. Structural characterization of the monomers was carried out through FTIR and NMR 1H, and eight composites were produced from the new monomers, by addition of silane-treated alumino silicate particles (inorganic filler) and a photocuring system (camphorquinone and ethyl 4-dimethylaminebenzoate). The composites were analyzed by environmental scanning electronic microscopy and the water sorption and solubility, compressive strength and elastic modulus were determined. A commercial composite resin [Z100 (3M)] was used to comparison effect. The new composites presented general characteristics similar to the commercial ones; however, they didn t present the properties expected. This behavior was attributed to the lower degree of monomer reaction and to the granulometry and size distribution of the mineral filler in the polymeric matrix / Atualmente, as resinas compostas constituem-se no material restaurador direto mais utilizado nas interven??es da cl?nica odontol?gica, dada a sua versatilidade e excel?ncia est?tica. O mon?mero mais freq?entemente usado na matriz polim?rica dessas resinas ? o Bis-GMA (2,2-bis[4(2-hidr?xi-3-metacriloiloxipropoxi)fenil]propano). No entanto, esse mon?mero apresenta algumas desvantagens, tais como elevada viscosidade e a presen?a de dois an?is arom?ticos em sua estrutura que podem causar rea??es al?rgicas ao organismo humano. Dessa forma, o objetivo principal deste trabalho foi sintetizar, a partir do metacrilato de glicidila, novos mon?meros para serem utilizados como componentes de poss?veis materiais restauradores dentais. A estrutura qu?mica dos mon?meros obtidos foi caracterizada pelas t?cnicas espectrosc?picas FTIR e RMN 1H, e oito comp?sitos foram preparados a partir dos novos mon?meros e part?culas silanizadas de silicato de alum?nio (carga inorg?nica), utilizando um sistema fotoativador/iniciador composto por canforoquinona e 4-dimetil amina benzoato de etila. Os comp?sitos foram analisados por microscopia eletr?nica de varredura ambiental e avaliados quanto ? sor??o e solubilidade em ?gua, resist?ncia ? compress?o e m?dulo de elasticidade. Para efeito de compara??o, utilizou-se a resina composta comercial Z100 (3M). Os novos comp?sitos preparados apresentaram caracter?sticas gerais semelhantes ?s resinas comerciais, entretanto, n?o se comportaram como esperado em rela??o ?s propriedades estudadas, o que foi atribu?do ao menor grau de rea??o dos mon?meros e ? granulometria e distribui??o da carga mineral na matriz polim?rica

This thesis contains investigations in the area of polymers herein propellants binders are modified functionally to meet the requirements of future energetic propellants. Chapter 1 contains a broad introduction to the area of recent advances in solid propellants and the numerous applications of ‘Click Chemistry’. Chapters 2 details the materials, characterization tools and the experimental techniques employed for the studies. This is followed by Chapter 3, 4, and 5 which deals with functional modification of various propellants binders, their characterisation and evaluation in propellant formulations. Chapter 6 details with the thermal decomposition of diazides and its reaction with alkenes. The advent of modern rockets has opened a new era in the history of space exploration as well as defence applications. The driving force of the rocket emanates from the propellant – either solid or liquid. Composite solid propellants find an indispensable place, in today’s rockets and launch vehicles because of the inherent advantages such as high reliability, easy manufacturing, high thrust etc. The composite propellant consisting of inorganic oxidiser like ammonium perchlorate, (AP), ammonium nitrate (AN) etc), metallic fuel (aluminium powder, boron etc) and polymeric fuel binder (hydroxyl terminated polybutadiene-HTPB, polybutadiene-acrylic acid-acrylonitrile PBAN, glycidyl azide polymer (GAP), polyteramethylene oxide (PTMO) etc. is used in igniters, boosters, upper stage motors and special purpose motors in large launch vehicles. Large composite solid propellant grains or rocket motors in particular, demand adequate mechanical properties to enable them to withstand the stresses imposed during operation, handling, transportation and motor firing. They should also have a reasonably long ‘potlife’ to provide sufficient window for processing operations such as mixing and casting which makes the selection of binder with appropriate cure chemistry more challenging. In all composite solid propellants currently in use, polymers perform the role of a binder for the oxidiser, metallic fuel and other additives. It performs the dual role of imparting dimensional stability to the composite, provides structural integrity and good mechanical properties to the propellant besides acting as a fuel to impart the required energetics. Conventionally, the terminal hydroxyl groups in the binders like GAP, PTMO and HTPB are reacted with diisocyanates to form a polyurethane network, to impart the necessary mechanical properties to the propellant. A wide range of diisocyantes such as tolylene diisocyanate (TDI) and isophorone diisocyanate (IPDI) are used for curing of these binders. However, the incompatability of isocyanates with energetic oxidisers like ammonium dinitramide (ADN), hydrazinium nitroformate (HNF), short ‘potlife’ of the propellant slurry and undesirable side reactions with moisture are limiting factors which adversely affect the mechanical properties of curing binders through this route. The objective of the present study is to evolve an alternate approach of curing these binders is to make use of the 1,3 dipolar addition reactions between azide and alkyne groups which is a part of ‘Click chemistry’. This can be accomplished by the reaction of azide groups of GAP with triple bonds of alkynes and reactions of functionally modified HTPB/PTMO (azide/alkyne) to yield 1,2,3 -triazole based products. This offers an alternate route for processing of solid propellants wherein, the cured resins that have improved mechanical properties, better thermal stability and improved ballistic properties in view of the higher heat of decomposition resulting from the decomposition of the triazole groups. GAP is an azide containing energetic polymer. The azide groups can undergo reaction with alkynes to yield triazoles. In, Chapter 3 the synthesis and characterisation of various alkynyl compounds including bis propargyl succinate (BPS), bis propargyl adipate (BPA), bis propargyl sebacate (BPSc.) and bis propargyl oxy bisphenol A (BPB) for curing of GAP to yield triazoles networks are studied. The mechanism of the curing reaction of GAP with these alkynyl compounds was elucidated using a model compound viz. 2-azidoethoxyethane (AEE). The reaction mechanism has been analysed using Density Functional Theory (DFT) method. DFT based theoretical calculations implied marginal preference for 1, 5 addition over the 1, 4 addition for the uncatalysed cycloaddition reaction between azide and alkyne group. The detailed characterisation of these systems with respect to the cure kinetics, mechanical properties, dynamic mechanical behaviour and thermal decomposition characteristics were done and correlated to the structure of the network. The glass transition temperature (Tg), tensile strength and modulus of the system increased with crosslink density which in turn is, controlled by the azide to alkyne molar stoichiometry. Thermogravimetic analysis (TGA) showed better thermal stability for the GAP-triazole compared to GAP based urethanes. Though there have been a few reports on curing of GAP with alkynes, it is for the first time that a detailed characterisation of this system with respect to the cure kinetics, mechanical, dynamic mechanical, thermal decomposition mechanism of the polymer is being reported. To extent the concept of curing binders through 1,3 dipolar addition reaction, the binder HTPB as chemically transformed to propargyloxy carbonyl amine terminated polybutadiene (PrTPB) with azidoethoxy carbonyl amine terminated polybutadiene (AzTPB) and propargyloxy polybutadiene (PTPB). Similarly, PTMO was convnerted to propargyloxy polytetramethylene oxide (PTMP). Triazole-triazoline networks were derived by the reaction of the binders with alkyne/azide containing curing agents. The cure characteristics of these polymers (PrTPB with AzTPB, PTPB with GAP and PTMP with GAP) were studied by DSC. The detailed characterisations of the cured polymers for were done with respect to the, mechanical, dynamic mechanical behaviour and thermal decomposition characteristics were done. Propellant level studies were done using the triazoles derived from GAP, PrTPB-AzTPB, PTPB and PTMP as binder, in combination with ammonium perchlorate as oxidiser. The propellants were characterised with respect to rheological, mechanical, safety, as well as ballistic properties. From the studies, propellant formulations with improved energetics, safety characteristics, processability and mechanical properties as well defect free propellants could be developed using novel triazole crosslinked based binders. Chapter 6, is aimed at understanding the mechanism of thermal decomposition of diazido compounds in the first section. For this, synthesis and characterisation of a diazido ester 1,6 –bis (azidoacetoyloxy) hexane (HDBAA) was done. There have been no reports on the thermal decomposition mechanism of diazido compounds, where one azide group may influence the decomposition of the other. The thermal decomposition mechanism of the diazido ester were theoretically predicted by DFT method and corroborated by pyrolysis-GC-MS studies. In the second section of this chapter, the cure reaction of the diazido ester with the double bonds of HTPB has been investigated. The chapter 6B reports the mechanism of Cu (I) catalysed azide-alkene reaction validated using density functional theory (DFT) calculations in isomers of hexene (cis-3-hexene, trans-3-hexene and 2-methy pentene: model compound of HTPB) using HDBAA. This the first report on an isocyanate free curing of HTPB using an azide. Chapter 7 of the thesis summarizes the work carried out, the highlights and important findings of this work. The scope for future work such as development of high performance eco-friendly propellants based on triazoles in conjunction with chlorine-free oxidizer like ADN, synthesis of compatible plasticisers and suitable crosslinkers have been described. This work has given rise to one patent, three international publications and four papers in international conferences in the domain.

Submitted by Renata Lopes (renatasil82@gmail.com) on 2016-01-15T12:14:11Z No. of bitstreams: 1 liviasalgado.pdf: 1200969 bytes, checksum: 244d1e72c0eb8f8d2b1211681283ab46 (MD5) / Approved for entry into archive by Adriana Oliveira (adriana.oliveira@ufjf.edu.br) on 2016-01-25T17:38:49Z (GMT) No. of bitstreams: 1 liviasalgado.pdf: 1200969 bytes, checksum: 244d1e72c0eb8f8d2b1211681283ab46 (MD5) / Made available in DSpace on 2016-01-25T17:38:49Z (GMT). No. of bitstreams: 1 liviasalgado.pdf: 1200969 bytes, checksum: 244d1e72c0eb8f8d2b1211681283ab46 (MD5) Previous issue date: 2015-04-27 / FAPEMIG - Fundação de Amparo à Pesquisa do Estado de Minas Gerais / Avaliou-se a rugosidade das superfícies de duas resinas compostas, antes e após a sua imersão em solução aquosa com diferentes pH e solução enzimática. Para a confecção dos 60 corpos de prova, 30 para cada resina composta, utilizou-se uma matriz de acrílico com 5mm de diâmetro e 2mm de espessura, sobre uma tira de poliéster posicionada em uma placa de vidro estéril que foram preenchidas com as resinas compostas Filtek Z350 (3M ESPE) e Empress Direct (Ivoclar-Vivadent), em um único incremento e sobre esta foi colocada outra tira de poliéster e procedeu a fotopolimerização por 40s. Os corpos de prova foram divididos 06 grupos (n=10) de acordo com a solução empregada: água deionizada (Grupos ZA e EA); hidróxido de sódio com pH 13.2 (Grupos ZNa e ENa) e solução enzimática de colesterol esterase (Grupos ZE e EE). Para dar acabamento utilizou-se uma sequência decrescente de granulação de lixas d’água: 600, 1000, 1200, 1500 e 2000 e para o polimento, suspensões de alumina (Arotec, São Paulo, SP, Brasi): 1μm, 0,3μm e 0,05μm. Após o polimento foram armazenados em estufa a 37°C durante 7 dias e realizadas 3 medições de cada superfície no rugosímetro e realizada a média e foram imersos individualmente nas soluções por 30 dias e mantidos em estufa a 37°C, a cada 7 dias as soluções eram trocadas. Após 30 dias foram realizadas mais 3 medições da rugosidade das superfícies e realizada a média. Foi realizada ANOVA e o teste de Tukey. A partir dos resultados obtidos conclui-se que as resinas compostas testadas apresentaram degradação hidrolítica apenas na solução aquosa por um período de imersão de 30 dias. / The roughness of the surfaces was evaluated two composites before and after their immersion in aqueous solutions with different pH and the enzyme solution. For producing the 60 test specimens, 30 for each composite was used an acrylic matrix with 5mm in diameter and 2mm thick on a polyester strip placed on a sterile glass plate were filled with the resins Filtek Z350 (3M ESPE) and Empress Direct (Ivoclar Vivadent-) in a single increment and this was placed on another strip of polyester and proceeded to light curing for 40 seconds. The specimens were divided 06 groups (n = 10) according to the used solution: deionized water (ZA Groups and EA); sodium hydroxide at pH 13.2 (ZNA Groups ENA) and enzyme solution of cholesterol esterase (ZE and EE groups). To finish used a descending sequence of sanding granulation water: 600, 1000, 1200, 1500 and 2000 and for polishing alumina suspensions (Arotec, São Paulo, SP, Brasi): 1μm, and 0,3μm 0,05μm. After polishing were stored at 37 ° C for 7 days and 3 measurements carried out on each surface roughness and the carried medium and were immersed in individual solutions and kept for 30 days at 37 ° C every 7 days the solutions were exchanged. After 30 days there were over 3 measurements of surface roughness and made average. ANOVA and Tukey test was performed. From the results obtained it is concluded that the composites tested showed hydrolytic degradation in aqueous solution only for a period of 30 days immersion.

Gegenstand dieser Arbeit ist die Herstellung funktioneller Polymerpartikel und deren Nutzung für biomedizinische Applikationen. Die Anwendungsgebiete der resultierenden Hybridmaterialien reichen vom Einsatz als Kontrastmittel in bildgebenden Verfahren der medizinischen Diagnostik über die Verwendung als Antimikrobium bis hin zum Einsatz als „Werkzeug“ zur Zellisolierung und aktivierung. Dazu wurden kompakte Latexpartikel und sensitive, poröse Mikrogelpartikel mittels emulgatorfreier Heterophasenpolymerisation synthetisiert. Als funktionelles Monomer wurde Glycidylmethacrylat verwendet, über dessen reaktive Epoxygruppen anschließend weitere Moleküle angebunden werden können. Die Funktionalisierung der Polymerpartikel erfolgte einerseits mit anorganischen Nanopartikeln (dotierte Lanthanfluorid-Nanopartikel, Gold- und Silbernanopartikel) und andererseits mit Biomolekülen wie Nukleotiden und Antikörpern. Einige Verwendungsgebiete, wie die Stimulierung von Memory-T-Zellen mit Antikörper-Polymer-Konjugaten oder der Einsatz der Silberkomposite aufgrund ihrer antimikrobiellen Wirkung, wurden näher untersucht. / The aim of this work was the synthesis of functional polymeric particles and their use for biomedical purposes. The application areas of the resulting hybrid materials range from contrast agents in medical diagnostics and usage due to antimicrobial properties to “tools” for cell isolation and activation. Compact core-shell particles and porous microgel particles were prepared by surfactant-free heterophase polymerization in water. All particles contain glycidyl methacrylate whose epoxy groups are capable to bind other molecules covalently. On the one hand, polymeric particles were functionalized with inorganic nanoparticles (doped lanthanum fluoride nanoparticles, gold and silver nanopariticles) and on the other hand with biomolecules such as nucleotides and antibodies. Selected application fields like the stimulation of memory T-cells with polymer-antibody-conjugates or the use of the silver composites due to their antimicrobial activity were investigated in detail.

No description available.

Background: The light-cured resin-based pit and fissure sealants success and longevity are enhanced by sufficient curing. Multiple emission peak Light Emitting Diode Light Curing Units offer a wider range of wavelengths and different levels of irradiances to ensure sufficient curing.The irradiance is considered a main curing factor that can affect the material properties. Purpose: The aim of this study was to assess the effect of different settings of a multiwave LED LCU on the degree of conversion and microhardness of a pit and fissure sealant comparing the irradiance of 1000 mW/cm2 to 1400 mW/cm2 and 3200 mW/cm2 irradiances of the LCU using manufacturer’s guidelines for curing times at 2, 4 and, 6 mm distances. Methods: A multiwave LED light curing unit was evaluated on three different irradiance levels 1000 mW/cm2 (S), 1400 mW/cm2 (H), and 3200 mW/cm2 (X). A total of 90 samples made from the fissure sealant were fabricated and divided into eighteen groups (n=5/group). Samples were cured following manufacturer’s guidelines of curing times for each curing mode at 2, 4, or 6 mm distance between the light tip and top of samples. The DC was measured using (ATR-FTIR) spectroscopy. The KHN test was performed on five different locations of each specimen using a hardness tester (Leco LM247AT, MI, USA, software; Confident V 2.5.2). Results: The top DC for H-8 was significantly higher than S-10 at 2 and 4mm, H-20 DC was significantly lower than S-30 at only 2mm. The bottom DC for H-8 was significantly higher than S-10 at 2mm only, H-20 DC was significantly lower than S-30 at 4 and 6mm only. H-8 KHN at top surface was significantly lower than S-10 at 2mm only, H-20 was significantly lower than S-30 at 2 and 6mm only. H-8 KHN at bottom surface was significantly lower than S-10 at 4 and 6mm but significantly higher at 2mm. H-20 was significantly lower than S-30 at 2mm but significantly higher at 4 and 6mm. The top DC for X-3 was significantly lower than S-10 at all curing distances with no significant difference at all curing distances between X-9 and S-30. The bottom DC for X-3 was significantly higher than S-10 at all curing distances with no significant difference between X-9 and S-30. X-3 KHN at top surface was significantly lower than S-10s at all curing distances. X-9 was significantly lower than S-30 at 6mm only. X-3 KHN at bottom surface was significantly lower than S-10 at 2 and 4mm only with no significant difference at all curing distances between X-9 and S-30. Conclusions: Using a multiwave LED LCU to polymerize Delton Opaque resin-based fissure sealants will result in an optimal DC and KHN values for any irradiance level if the curing distance is kept at 4 mm or less and with at least two cycles of the shortest curing time recommended by the manufacturer. Using a multiwave LED LCU with 1000, 1400 or 3200 mW/cm2 irradiance levels with shortest curing times recommended resulted in unsatisfactory DC and KHN levels. LED LCU with high and extra high irradiance levels (1400 and 3200 mW/cm2) can result in high DC and KHN levels when used adequately. Xtra Power mode (3200 mW/cm2) used on shortest curing time (3 seconds) resulted in significantly lower mechanical properties and for that reason it is not recommended to be used.

Indiana University-Purdue University Indianapolis (IUPUI) / Reduction of the polymerization shrinkage stress inherent of dimethacrylate-based resin composites has been a work in progress since the phenomenon was first described by Dr. Rafael L. Bowen in 1967. Contemporary efforts to modify the composites or the curing protocols for polymerization have proven a challenging task with controversial results. Influenced by existing mathematical models relating exposure, curing time and depth of cure of resin composites, a novel method for the reduction of polymerization shrinkage stress is proposed. By polymerizing through a single aperture mask, a dental light curing unit is transformed from a planar light source to a point light source, and a fully cured, three-dimensional “bullet” shaped curing front is predicted for the cured resin below. So long as the edges of the bullet do not touch the cavity walls or floor, the shrinkage stress of the bullet is not transferred. Follow-up with an unmasked curing unit then fully polymerizes the restoration. By reducing the volume of uncured composite in contact with the cavity walls and floor, shrinkage stress of the restoration is also reduced. The objective of the present study was to demonstrate this curing phenomenon with a model resin composite using masks with aperture diameters of 0.5, 0.4, and 0.25 mm and curing times of 10, 20, 30, and 40 seconds. The resulting curing front was evaluated quantitatively and qualitatively. From this, mathematical models of the curing front were derived. Selected combinations of aperture mask and curing time were then investigated to evaluate the influence of this phenomenon on the degree of conversion, Knoop hardness, and polymerization shrinkage stress of the same model resin composite. Group differences were analyzed using a one-way ANOVA at 5% significance.

Nesta Dissertação, foram sintetizadas microesferas poliméricas com propriedades magnéticas à base de metacrilato de glicidila e divinilbenzeno pela técnica de polimerização em suspensão. O material utilizado para conferir as propriedades magnéticas ao copolímero foi magnetita sintetizada no laboratório. Foram estudados os efeitos da modificação da magnetita com ácido oleico, da velocidade de agitação, do teor de agente reticulante, do teor de material magnético adicionado e do teor de agente de suspensão sobre as características das partículas poliméricas obtidas. As microesferas foram caracterizadas quanto ao seu aspecto morfológico, à estabilidade térmica, à incorporação de material magnético e quanto às suas propriedades magnéticas. A quantidade de partículas de ferro incorporadas foi afetada pela velocidade de agitação durante a síntese, pelo teor de material magnético adicionado, pela fase de dispersão do material magnético e pelo teor de monômeros no copolímero. A estabilidade térmica dos copolímeros foi afetada, principalmente, pelo teor de material magnético incorporado e pelo teor de monômeros, levando em consideração resinas com a mesma quantidade de material magnético adicionado. A magnetização de saturação para as microesferas foi afetada pelo teor de material magnético incorporado. A modificação da superfície da magnetita com ácido oleico foi considerada importante para a incorporação do material magnético na matriz do copolímero.Partículas poliméricas magnéticas com comportamento superparamagnéticos foram obtidas com morfologia esférica e magnetização de saturação de 7,11 (emu/g), utilizando razão molar de monômeros de 50/50 %, 1 % de PVA, 20 % de magnetita modificada com ácido oleico adicionada à fase orgânica e velocidade de agitação mecânica de 500 rpm / In this dissertation, polymeric microspheres with magnetic properties based on glycidyl methacrylate and divinylbenzene were synthesized by suspension polymerization technique. In order to obtain magnetic properties, magnetite particles modified by oleic acid were synthesized in laboratory. The effects of stirring rate, concentration of crosslink, the concentration of magnetite added and the concentration of stabilizer on the particles properties were studied. The magnetic microspheres were characterized according their morphology, thermal stability, incorporation of magnetite and their magnetic properties. The incorporate of iron particles content was mainly affected by stirring rate during the synthesis, by the content of magnetic material added, by the dispersion phase of magnetic material and by the monomers content in the copolymer. The thermal stability of copolymers was mainly affected by the content of magnetic material incorporated and by the monomers content, taking in account the resins with the same content of magnetic material added. The saturation magnetization for the microspheres was effected by the content of magnetic material incorporated. The modification with oleic acid was considered important to the incorporation of the magnetic material in the copolymer matrix.Magnetic polymeric particles with superparamagnetic behavior have been obtained with spherical morphology and saturation magnetization of 7.11 (emu/g). It was used monomers molar ratio of 50/50 %, 1% PVA, 20 % magnetite particles modified by oleic acid dispersion on organic phase and stirring rate of 500 rpm during the synthesis

Nesta Dissertação, foram sintetizadas microesferas poliméricas com propriedades magnéticas à base de metacrilato de glicidila e divinilbenzeno pela técnica de polimerização em suspensão. O material utilizado para conferir as propriedades magnéticas ao copolímero foi magnetita sintetizada no laboratório. Foram estudados os efeitos da modificação da magnetita com ácido oleico, da velocidade de agitação, do teor de agente reticulante, do teor de material magnético adicionado e do teor de agente de suspensão sobre as características das partículas poliméricas obtidas. As microesferas foram caracterizadas quanto ao seu aspecto morfológico, à estabilidade térmica, à incorporação de material magnético e quanto às suas propriedades magnéticas. A quantidade de partículas de ferro incorporadas foi afetada pela velocidade de agitação durante a síntese, pelo teor de material magnético adicionado, pela fase de dispersão do material magnético e pelo teor de monômeros no copolímero. A estabilidade térmica dos copolímeros foi afetada, principalmente, pelo teor de material magnético incorporado e pelo teor de monômeros, levando em consideração resinas com a mesma quantidade de material magnético adicionado. A magnetização de saturação para as microesferas foi afetada pelo teor de material magnético incorporado. A modificação da superfície da magnetita com ácido oleico foi considerada importante para a incorporação do material magnético na matriz do copolímero.Partículas poliméricas magnéticas com comportamento superparamagnéticos foram obtidas com morfologia esférica e magnetização de saturação de 7,11 (emu/g), utilizando razão molar de monômeros de 50/50 %, 1 % de PVA, 20 % de magnetita modificada com ácido oleico adicionada à fase orgânica e velocidade de agitação mecânica de 500 rpm / In this dissertation, polymeric microspheres with magnetic properties based on glycidyl methacrylate and divinylbenzene were synthesized by suspension polymerization technique. In order to obtain magnetic properties, magnetite particles modified by oleic acid were synthesized in laboratory. The effects of stirring rate, concentration of crosslink, the concentration of magnetite added and the concentration of stabilizer on the particles properties were studied. The magnetic microspheres were characterized according their morphology, thermal stability, incorporation of magnetite and their magnetic properties. The incorporate of iron particles content was mainly affected by stirring rate during the synthesis, by the content of magnetic material added, by the dispersion phase of magnetic material and by the monomers content in the copolymer. The thermal stability of copolymers was mainly affected by the content of magnetic material incorporated and by the monomers content, taking in account the resins with the same content of magnetic material added. The saturation magnetization for the microspheres was effected by the content of magnetic material incorporated. The modification with oleic acid was considered important to the incorporation of the magnetic material in the copolymer matrix.Magnetic polymeric particles with superparamagnetic behavior have been obtained with spherical morphology and saturation magnetization of 7.11 (emu/g). It was used monomers molar ratio of 50/50 %, 1% PVA, 20 % magnetite particles modified by oleic acid dispersion on organic phase and stirring rate of 500 rpm during the synthesis