Submitted by Emanuel Varela Cardoso (emanuel.varela@ufcg.edu.br) on 2018-06-13T19:56:21Z No. of bitstreams: 1 FRANCISCO PINTO FILHO – TESE (PPGEP) 2016.pdf: 2405186 bytes, checksum: d7b5b1d68600f138fc5134159b39d6fc (MD5) / Made available in DSpace on 2018-06-13T19:56:21Z (GMT). No. of bitstreams: 1 FRANCISCO PINTO FILHO – TESE (PPGEP) 2016.pdf: 2405186 bytes, checksum: d7b5b1d68600f138fc5134159b39d6fc (MD5) Previous issue date: 2016-08-29 / Capes / A busca por inovações tecnológicas nos últimos anos cada vez mais se intensifica. Neste contexto, dois importantes grupos, os lantanídeos e as hidantoínas se destacam com importantes contribuições em diversas áreas de pesquisas apresentando vasto campo de aplicações. Nesses termos, esta pesquisa teve como objetivo sintetizar e caracterizar nanocomplexos dos íons lantanídicos: Eu +3, Er+3 e Nd+3 com 5-(4-metilfenil)-3-fenil-2-tioxo-imidazolidin-4-ona (HPA) e um segundo ligante, 1,10-fenatrolina (Phen), almejando obter complexos com propriedades biológicas. Partindo da reação entre os cloretos dos respectivos lantanídeos com os ligantes orgânicos, sob refluxo de aproximadamente 8 horas e temperatura de 60°C, foram obtidos os complexos de európio, érbio e neodímio. Os nanocomplexos em pó foram caracterizados utilizando técnicas de análises espectroscópicas, térmicas e estrutural. Os complexos de íons lantanídicos apresentaram resultados da análise elementar conforme a estequiometria proposta (1:3:1). A coordenação dos ligantes com os íons lantanídicos ocorreu através dos átomos de oxi gênio e enxofre da estrutura do 5-(4-metilfenil)-3-fenil-2-tioxo-imidazolidin-4-ona (HPA) e dos átomos de nitrogênio (C=N) da 1,10’- fenantrolina, que podem ser observados nos espectros de infravermelho, através dos deslocamentos dessas bandas presentes nos ligantes livres e coordenados. Os espectros UV-Vis apresentaram discretos deslocamentos e mudanças nas intensidades das bandas de absorção dos complexos em relação ao ligante HPA. As curvas TG/DTG do ligante HPA apresentou 3 etapas de decomposição, enquanto, que os complexos apresentaram 4 etapas. O nanocomplexo de Eu+3 apresentou menor estabilidade térmica, o que possibilita o uso destes pós como fármacos. As curvas DSC dos nanocomplexos apresentaram uma série de eventos endotérmicos e exotérmicos correspondentes a processos de decomposição, desidratação, fusão e volatilização que corroboram com as curvas termogravimétricas. Todos os complexos lantanídicos obtidos apresentaram dimensões nanométricas, e o complexo de neodímio apresentou a estrutura mais cristalina. / The search for technological innovations in recent years increasingly intensifies. In this context, two major groups, the lanthanides and hydantoins stand out with important contributions in many areas of research showing wide field of applications. In these terms, this research aims to synthesize and characterize complex of lanthanide ions: Eu+3, Ho+3, Er+3 and Nd+3 with 5-(4-methyl-phenyl)-3-phenyl-2-thioxo-imidazolidin-4-one (HPA) and a second linker, 1,10-fenatrolina (Phen), aiming to obtain complexes with biological properties. From the reaction between the chlorides of lanthanides with the respective organic ligands under reflux for approximately 8 hours and 60°C, were obtained complexes of europium, holmium, erbium and neodymium. The powder complexes were characterized using spectroscopic techniques, thermal and structural analyzes. The complexes of lanthanide ions showed elemental analysis results according to the proposed stoichiometry (1:3:1). The coordination of the ligands with lanthanide ions occurred through oxygen and sulfur atoms in the structure of 5 - (4-methylphenyl) -3-phenyl-2-thioxo-imidazolidin-4-one (HPA) and nitrogen atoms (C = N) of 1,10'- phenanthroline, which can be observed in the infrared spectra, through the displacement of these bands present in free and coordinated ligands. UV-Vis spectra showed discrete displacements and changes in the intensities of the absorption bands of the complex compared to the HPA binder. The TG/ DTG curves HPA binder 3 had decomposition steps, while the complexes showed 4 and 5 steps. The complex synthesized Er+3 showed higher thermal stability. The DSC curves of the complexes showed a series of endothermic and exothermic events corresponding to decomposition processes, dehydration, fusion and volatilization, corroborating the thermogravimetric curves. All lanthanide complexes obtained showed nanometric dimensions, and neodymium complex presented the most crystalline structure.

Sedimenten i området Kolkajen-Ropsten, Stockholm, innehåller höga halter av tjäroljor till följd avtidigare produktion i gasverket på området. Stockholms stad planerar att utföra byggnation i detnuvarande vattenområdet, vilket ökar risken för spridning av föroreningar. För att skydda arbetandeunder planerad byggnation och framtida boende måste föroreningssituationen åtgärdas. Tjäroljornainnehåller höga halter av polyaromatiska kolväten (PAH) och det är föroreningen av PAH-16 som styråtgärdsbehovet för området. En metod som använts med god framgång i flera projekt i Norden ochandra delar av världen är stabilisering och solidifiering, s/s, av sediment. Metoden går ut på att blandain utvalda bindemedel i sedimenten som då härdar. Därigenom minskar föroreningens mobilitet och degeotekniska egenskaperna förbättras. Om kravet på skjuvhållfasthet (>140 KPa), låg permeabilitet (10-8-10-9 m/s) samt minskad utlakning uppfylls kan de stabiliserade massorna utgöra grunden för planeradbyggnation.För att utvärdera möjligheterna av denna åtgärdsmetod analyserades en sats av prover från området föratt tillhandahålla information om platsspecifika parametrar. Analysen visade att sedimenten hade högvattenkvot och organiskt innehåll, dominerades av fina fraktioner samt en föroreningsgrad av PAH-16på 13000 mg/kg TS. Utifrån dessa parametrar och med stöd från en litteraturstudie valdes fyra receptpå bindemedel ut, med olika mängd bindemedel. De bindemedel som använts är: Bascement frånSkövde som är ett portland-flygaskecement, Monofill som består av 20 % cement och 80 % granuleratmasugnsslagg samt aktivt kol. De olika recepten blandades med sediment från området och lämnadesatt härda under 28 dygn. Efter härdningen utvärderades de stabiliserade massorna med avseende påminskad utlakning av PAH jämfört med obehandlat sediment, skjuvhållfasthet och permeabilitet.Analyser av de fyra blandningarna visade att kravet på skjuvhållfasthet och permeabilitet uppfylldesför samtliga tillsatser av bindemedel och överlag innebar större mängder tillsatt bindemedel högreskjuvhållfasthet och lägre permeabilitet. Resultaten från laktester indikerade att en större tillsats avaktivt kol minskade utlakningen av PAH.Tillsatsen av bindemedel som bedöms vara bäst lämpad för stabilisering av sedimenten från områdetvar en total mängd av cement och Monofill på 250 kg/m3 (30 % cement och 70 % Monofill) samt entillsats av aktivt kol på 5 % av TS.Inblandning i sedimenten enligt receptet ovan resulterade i en skjuvhållfasthet på 413 KPa samt enönskat låg permeabilitet. Utlakningen av PAH-16 reducerades med ~45 % jämfört med obehandlatsediment. / The sediments in the area Kolkajen-Ropsten, Stockholm, have shown high levels of tar oils due to thegasworks in the area. The city of Stockholm is planning construction in the area which increases therisk of contaminants spreading to the surrounding area. In order to protect workers during the plannedconstruction and future inhabitants, remediation has to be carried out. The tar oils have highconcentrations of polyaromatic hydrocarbons (PAH) and it is pollution of PAH-16 that dictates theneed for remediation.A remediation method that has been used in similar projects, with good results, is stabilization andsolidification (s/s) of the sediments. This is done by mixing binder materials with the sediments whichharden and it results in lowered mobility of the contaminants and improved geotechnical properties ofthe soil. If the shear strength is high enough (>140 KPa), the permeability is low enough (10-8-10-9m/s) and the leaching is reduced sufficiently, the stabilized sediments can be used as a foundation.To evaluate the possibility of this remediation method, a batch of sediment samples from the area wasanalyzed to obtain information about site specific parameters. The analysis showed that the sedimentshad high water content and were rich in organic matter. They were dominated by small particlefractions and had a PAH-16 concentration of 13000 mg/kg DM. With regard to these site specificparameters and a literature study, four different recipes with different amounts of binders wereselected and tested in a laboratory study. The used binders were: cement from Skövde which is aportland-fly ash cement, Monofill composed of 20 % cement and 80 % granulated furnace slag, andaddition of activated carbon.The sediments were mixed with binders according to the recipes and left to harden for 28 days.Following the 28 days of hardening, the stabilized mixtures were evaluated with regard to: thereduction of leaching of PAH in comparison to the untreated sediments, shear strength, andpermeability.Analyses of the four mixtures showed that the desirable values of both shear strength and permeabilitywere achieved for all mixtures, and that a higher concentration of binders resulted in a higher shearstrength and lower permeability. The results from the leaching tests indicated that a higherconcentration of activated carbon resulted in a lowered leaching of PAH.The mixture of binders that was deemed to be most suitable for stabilizing the sediments from the areawas a total amount of cement and Monofill at 250 kg/m3 (30 % cement and 70 % Monofill) with anaddition of activated carbon at 5 % of DM (dry matter).Addition of this binder mixture to the sediments resulted in a shear strength of 413 KPa and a desiredlow permeability. The reduced leaching of PAH-16 was ~45 % compared to untreated sediments.

L’ingénierie protéique servant autrefois à comprendre les relations structures-fonctions des protéines connait un tournant majeur depuis plusieurs années. L’ingénierie protéique évolue pour créer des nouvelles fonctions protéiques : c’est la naissance de l’ingénierie protéique moderne. L’objectif de ma thèse a consisté à mettre en place et caractériser deux approches indépendantes d’ingénierie protéique dans le domaine du vaccin et du diagnostic. Le premier projet consistait à générer des ligands protéiques à partir d‘échafaudages moléculaires (des alternatifs aux anticorps) en couplant le ribosome display au NGS et en développant des outils d’analyses bio-informatiques. Des sélections contre des cibles protéiques d’origine bactérienne et virale ont conduit à l’identification de ligands Affibodies affins (µM au nM). Leur caractérisation a validé leur potentiel comme outil de recherche et de réactif diagnostique. Ces études ont permis de valider la plateforme de génération des ligands mise en place, en augmentant l’exploration de l’espace de diversité des interactions des ligands. Le second projet portait sur le développement d’une plateforme de présentation et de vectorisation à partir de particules d’encapsuline. Elles ont été génétiquement modifiées pour présenter de manière répétée à leur surface l’ectodomaine de la protéine de matrice M2 (M2e) du virus Influenza A H1N1 tout en encapsulant une protéine hétérologue : l’eGFP. Les nanoparticules modifiées sont correctement formées et encapsulent l’eGFP. Des souris immunisées par ces particules induisent une réponse anticorps spécifique contre l’épitope M2e et l’eGFP. L’utilisation de ces nanoparticules comme plateforme vaccinale de présentation et de vectorisation est prometteuse et ouvre la voie pour d’autres applications en biotechnologie / In the past, protein engineering used to understand function and structure relationship. But since few years, protein engineering was used to create new protein functions: modern protein engineering was born. The aim of my thesis was to set up and characterize two approaches of protein engineering in diagnostic and vaccine field. The first project was to generate artificial binder using protein scaffolds as an alternative to antibodies by coupling ribosome display (RD) to NGS and developing bio-informatics tools. Screening and selection against bacterial and viral targets have led to affibody binder’s identification with an affinity range from µM to nM. Their characterization has validated their potential as research tools and protein reagents for diagnostic assay. Coupling ribosome display to high throughput sequencing as means to directly identify selected binder coding sequences, enormously enhance binder discovery depth. The second project was to generate an innovative nanocarrier based on encapsulin nanoparticle, for customized peptide display and cargo protein vectorization. Encapsulin particles from T.maritima were genetically modified for simultaneous display of the matrix protein 2 ectodomain of the influenza H1N1 A virus and heterologous protein eGFP packaging. Genetically engineered encapsulin nanoparticles were well-formed and abled to efficiently load eGFP. Immunogenicity studies revealed antibody responses against both the surface epitope and the loaded cargo protein. Taken together, this display system is a versatile tool for rational vaccine design and paves the way for new applications in the research fields of vaccine, antimicrobial research and other biotechnological applications

O ensaio de fluência e recuperação sob tensão múltipla (MSCR) é resultado do aperfeiçoamento do ensaio de fluência repetida e recuperação (RCRT) pela Administração Rodoviária Federal dos Estados Unidos (FHWA) e tem por objetivo avaliar o percentual de recuperação, a compliância não-recuperável e a dependência dos ligantes asfálticos, especialmente os modificados, quanto ao nível de tensão. O MSCR foi utilizado neste estudo para caracterizar o comportamento fluência-recuperação de diversos ligantes asfálticos modificados virgens e envelhecidos a curto prazo. Foi empregado o procedimento da norma ASTM D7405, que prescreve os tempos de fluência e recuperação de 1 e 9 s, e avaliada a influência do aumento dos tempos de fluência e recuperação de 1 e 9 s para 2 e 18 s nas propriedades dos ligantes asfálticos envelhecidos a curto prazo. Além dos resultados destes ensaios, foram utilizados os valores de penetração, ponto de amolecimento, viscosidade rotacional, penetração retida, incremento do ponto de amolecimento, incremento de viscosidade e perda de massa para verificar quais ligantes asfálticos apresentam melhor comportamento à luz das propriedades e parâmetros considerados. Foram preparados doze materiais modificados e de classificação PG 76-XX tendo como base um CAP 50/70 de classificação PG 64-XX: CAP+PPA, CAP+Elvaloy+PPA, CAP+borracha, CAP+borracha+PPA, CAP+SBS, CAP+SBS+PPA, CAP+EVA, CAP+EVA+PPA, CAP+PE, CAP+PE+PPA, CAP+SBR e CAP+SBR+PPA. O CAP+Elvaloy+PPA apresenta, em um contexto geral, o melhor desempenho nas propriedades e parâmetros analisados em virtude dos bons resultados do percentual de recuperação e da compliância não-recuperável e das menores sensibilidades à tensão. O CAP+PE apresenta o pior desempenho geral dentre os materiais estudados, na medida em que os resultados do percentual de recuperação e da compliância não-recuperável deste ligante asfáltico são ruins e as sensibilidades ao aumento nos tempos de fluência e recuperação de 1 e 9 s para 2 e 18 s são elevadas. Ao ordenar os ligantes asfálticos do melhor para o pior à luz das propriedades e parâmetros considerados, o resultado é: CAP+Elvaloy+PPA, CAP+EVA, CAP+EVA+PPA, CAP+PPA, CAP+borracha+PPA, CAP+SBR+PPA, CAP+SBS+PPA, CAP+SBS, CAP+PE+PPA, CAP+borracha, CAP+SBR, CAP 50/70 e CAP+PE. / The multiple stress creep and recovery (MSCR) test is the result of a refinement of the repeated creep and recovery test (RCRT). This refinement was performed by the United States Federal Highway Administration (FHWA) with the aim of evaluating the percent recovery, the non-recoverable compliance and the stress dependency of asphalt binders, especially the modified ones. The MSCR test was applied in this study in order to characterize the creep-recovery behavior of unaged and short-term aged modified asphalt binders. The test procedure prescribed in ASTM D7405 specification was adopted and, to evaluate the influence of a greater creep-recovery time in the behavior of asphalt binders, the creep and recovery times of 2 and 18 s were also adopted in additional tests. The results of these tests, as well as the penetration, softening point, rotational viscosity, retained penetration, softening point increase, viscosity increase and mass loss data and mixing and compaction temperatures, were used with the objectives of ranking the asphalt binders and checking the ones with the best results in the parameters and properties considered. By using a PG 64-XX base asphalt-binder of 50/70 penetration grade, the following PG 76-XX odified asphalt binders were prepared: AC+PPA, AC+Elvaloy+PPA, AC+crumb rubber, AC+crumb rubber+PPA, AC+SBS, AC+SBS+PPA, AC+EVA, AC+EVA+PPA, AC+PE, AC+PE+PPA, AC+SBR and AC+SBR+PPA. In general, AC+Elvaloy+PPA has the best results in the parameters and properties considered in this study, especially due to the good results in the percent recovery and non-recoverable compliance and the lower stress sensitivity. In general, AC+PE has the worst results among the asphalt binders considered in this work, due to the facts that the percent recovery and non-recoverable compliance results are not good and the sensitivities to the creep-recovery times are high. By taking the results of this study and ranking the asphalt binders from the best to the worst, the following sequence is obtained: AC+Elvaloy+PPA, AC+EVA, AC+EVA+PPA, AC+PPA, AC+crumb rubber+PPA, AC+SBR+PPA, AC+SBS+PPA, AC+SBS, AC+PE+PPA, AC+crumb rubber, AC+SBR, neat AC and AC+PE.

Submitted by isabela.moljf@hotmail.com (isabela.moljf@hotmail.com) on 2017-07-24T11:39:19Z No. of bitstreams: 1 flaviaherediaesilva.pdf: 2351726 bytes, checksum: 548858280f72c798bbde46f0f2b9ef00 (MD5) / Approved for entry into archive by Adriana Oliveira (adriana.oliveira@ufjf.edu.br) on 2017-08-08T18:43:46Z (GMT) No. of bitstreams: 1 flaviaherediaesilva.pdf: 2351726 bytes, checksum: 548858280f72c798bbde46f0f2b9ef00 (MD5) / Made available in DSpace on 2017-08-08T18:43:46Z (GMT). No. of bitstreams: 1 flaviaherediaesilva.pdf: 2351726 bytes, checksum: 548858280f72c798bbde46f0f2b9ef00 (MD5) Previous issue date: 2017-03-23 / Neste trabalho foram sintetizados dois novos polímeros de coordenação {[Zn(SIP)(H2O)4]K}n (Zn-SIP), {[Ag(INH)2]SIP}n (Ag-SIP) e um complexo metálico [Zn(INH)2(H2O)2][1,5-NDS]∙H2O (Zn-NDS). Para a síntese destes compostos foi empregada à metodologia de ligantes mistos. Os ligantes utilizados foram o sal de sódio do ácido 5-sulfo-1,3-benzenodicarboxílico (SIP), ácido 1,5-naftalenodisulfônico (1,5-NDS) e a piridina-4-carboidrazida (INH). A caracterização química dos compostos obtidos foi realizada através das técnicas de análise elementar de C, H e N, espectroscopia vibracional na região do infravermelho e espectroscopia Raman. A caracterização estrutural foi realizada através da técnica de difração de raios X por monocristal, revelando Zn-SIP e Zn-NDS pertencem ao sistema cristalino monoclínico e grupo espacial P21/n enquanto o Ag-SIP pertence ao sistema cristalino monoclínico e grupo espacial P21/c. A resolução estrutural do polímero Ag-SIP revelou a ocorrência de desordem posicional em dois átomos de oxigênio do grupo sulfonato do SIP, sendo que a ocupação dos mesmos é de 68:32. Para os polímeros de coordenação realizou-se também descrição topológica, que revelou que o Zn-SIP é composto por uma rede 3D, binodal (4,6)-conectada que pode ser descrita com o símbolo de ponto (44∙610∙8) (44∙62). Esta rede apresenta uma subrede bidimensional, uninodal 4-conectada que pode ser descrita com o símbolo de ponto (44∙62), sendo classificada como uma rede plana tetragonal do tipo sql/Shubnichov. A descrição topológica do Ag-SIP revelou que o mesmo apresenta uma rede 2D, uninodal 4-conectada e pode ser descrita com um símbolo de ponto (44∙62), classificada como uma rede plana tetragonal do tipo sql. / In this work two new coordination polymers were synthesized, {[Zn(SIP)(H2O)4]K}n (Zn-SIP), {[Ag(INH)2]SIP}n (Ag-SIP) and a metal complex [Zn(INH)2)(H2O)4][1,5-NDS]∙H2O (Zn-NDS). For the synthesis of these compounds to the methodology of mixed binders was used. Binders used were sodium salt of 5-sulpho-1,3-benzenedicarboxylic acid (SIP), 1,5-naphthalenedisulfonic acid (1,5-NDS) and pyridine-4-carbohydrazide (INH). The chemical characterization of the elements obtained through the elementary analysis techniques of C, H and N, infrared spectroscopy and Raman spectroscopy. The structural characterization was performed using the X-ray diffraction by single crystal. The Zn-SIP and Zn-NDS belong to the monoclinic crystal system and the space group P21/n and the Ag-SIP belongs to the monoclinic crystal system and space group P21/c. A structural solution of the Ag-SIP polymer revealed an occurrence of positional disorder in two oxygen atoms of the SIP sulfonate group, with occupancy of 68:32. For the coordination polymers, a topological description was also performed, which revealed that Zn-SIP is composed of a 3D, binodal (4,6)-connected network that can be described with the point symbol (44∙610∙8)(44∙62). This network is presented in a two-dimensional, uninodal 4-connected subnet that can be described with the symbol of the point (44∙62), being classified as a flat square network of type sql/Shubnichov. The topological description of Ag-SIP reveals that this compound is composed of a 2D, uninodal 4-connected network and can be described with a point symbol (44∙62), classified as a flat tetragonal network of sql type.

O envelhecimento dos ligantes asfálticos possui uma grande influência sobre as propriedades mecânicas das misturas asfálticas. As especificações atuais limitam determinados índices ou parâmetros de envelhecimento, visando contornar o endurecimento excessivo do ligante asfáltico, porém, não levam em conta o efeito da radiação ultravioleta (UV). O objetivo deste trabalho é avaliar o efeito dos envelhecimentos termo-oxidativo e foto-oxidativo sobre as propriedades reológicas de um CAP puro e 11 ligantes asfálticos modificados, incluindo polímeros elastoméricos e plastoméricos, borracha moída de pneus e ácido polifosfórico, incluindo também combinações destes aditivos. Os ligantes asfálticos, com classificação por grau de desempenho PG 76-XX, preparados com base em um CAP 50-70 com classificação PG 64-22, foram previamente envelhecidos a curto prazo na estufa RTFO e posteriormente submetidos ao envelhecimento foto-oxidativo em uma estufa UV sob dois níveis de radiação, 0,68 W/m² e 1,00 W/m², por um período de 240 h. Para efeitos de comparação dos resultados, as mesmas amostras foram submetidas ao envelhecimento termo-oxidativo na estufa PAV. As amostras virgens e envelhecidas a curto prazo foram caracterizadas por meio de ensaios empíricos. Os resíduos obtidos nos envelhecimentos foram submetidos a ensaios no reômetro de cisalhamento dinâmico (DSR). Propriedades reológicas dos ligantes asfálticos foram analisadas por meio de curvas-mestre e do ensaio de fadiga LAS. Algumas amostras foram caracterizadas quimicamente por meio de espectroscopia no infravermelho (FTIR), cromatografia por permeação em gel (GPC) e do fracionamento SARA. Para a maioria das amostras os procedimentos PAV e UV a 0,68 W/m² apresentam certa equivalência, em termos da capacidade de alterar as propriedades reológicas analisadas. O ligante asfáltico que mostrou ser menos sensível ao envelhecimento PAV foi o CAP+SBR, o que demonstrou ser menos sensível ao envelhecimento UV a 0,68 W/m² foi o CAP+EVA, e o que demonstrou menor sensibilidade ao envelhecimento UV a 1,00 W/m² foi o CAP+SBS. O CAP+SBS+PPA foi a amostra que apresentou maior sensibilidade ao envelhecimento PAV e UV a 1,00 W/m². / Aging of the asphalt binders has a great influence on the mechanical properties of asphalt mixtures. The current specifications establish limits for some indexes or aging parameters in an attempt to avoid the excessive hardening of the asphalt binder; however, they do not take into account the effects of ultraviolet (UV) irradiation. The objective of this study is to analyze the impact of thermo-oxidative and UV aging methods on the rheological properties of a base asphalt cement (AC) and 11 formulations prepared with additives, i. e., elastomeric and plastomeric polymers, ground tire rubber and polyphosphoric acid. Combinations these additives were also included in the study. The modified asphalt binders are graded as PG-76 XX in the Superpave specification, whereas the 50-70 base AC is graded as PG 64-22 in the same specification. The materials were first aged in the rolling thin-film oven (RTFO), and then submitted to photo-oxidative aging in an UV oven at two irradiation levels (0.68 W/m² and 1.00 W/m²) for 240 h. For comparison purposes, these formulations were also subjected to thermo-oxidative aging in the pressurized aging vessel (PAV). The unaged and short-term aged samples were characterized by means of empirical tests. The residues obtained in the RTFOT, PAV e UV aging methods were tested in the dynamic shear rheometer (DSR). The rheological properties of asphalt binders were analyzed by means of master curves and the linear amplitude sweep (LAS) fatigue test. Some samples were chemically characterized by the Fourier transform infrared spectroscopy (FTIR), the gel permeation chromatography (GPC) and the SARA fractionation techniques. The PAV and the UV procedures at 0.68 W/m² show some similarities for many formulations in terms of the ability to change their rheological properties. The AC+SBR was found to be less sensitive to PAV aging than the other studied binders, whereas the AC+EVA was the less sensitive material to UV aging at 0.68 W/m² and the AC+SBS showed the lowest sensitivity to UV aging at 1.00 W/m². The AC+SBS+PPA was the most sensitive formulation to PAV and UV aging at 1.00 W/m².

Le manque de granulats de qualité dans certaines régions françaises tend à devenir un problème majeur pour les entreprises de travaux publics. En effet, avec une consommation annuelle de 200 millions de tonnes de granulats, la route se doit de faire face en imaginant de nouvelles solutions comme la valorisation de certains matériaux.La craie, située entre roche et sol, possède une place particulière dans le monde des travaux publics. En effet, si son usage est relativement bien maîtrisé en vue de la réalisation de remblais ou de couches de forme, il en est tout autrement des couches d’assise de chaussées.Ce type de matériau est usuellement rejeté de la conception des assises de chaussées car il ne s’insère pas dans les guides normatifs utilisés par les professionnels de la route. Les performances mécaniques et la grande sensibilité à l’eau de ce matériau ne lui permettent pas d’entrer dans les spécifications requises par les normes. Cependant, il est tout à fait envisageable que la craie trouve sa place de manière totale ou partielle en assise de chaussée.Ce matériau que l’on trouve en abondance dans certaines régions françaises pauvres en granulats "haut de gamme" (Nord-Pas de Calais, Champagne-Ardenne…), pourrait ainsi palier un certain manque, participer à la préservation de ressources naturelles et économiser frais et pollution générés par un approvisionnement lointain.Ces travaux menés en partenariat entre le Laboratoire de Génie Civil de l’Ecole Centrale de Lille et le Laboratoire Routier Eurovia de Loos ont donc pour but de proposer des pistes d’amélioration des performances mécaniques de la craie en vue de sa valorisation en assise de chaussée routière / The lack of high quality aggregates in some French regions seems to become a main issue for road work firms. With an annual consumption of 200 millions tonnes of aggregates, road professionals must square up finding new solutions like the valorisation of some forgotten materials. Between rock and soil, chalk has a particular position in road work. While its use is relatively well managed for the realisation of fills and subgrade courses, the same certainly cannot be said for base courses. This kind of material is usually rejected for the design of road base courses because it is not approved within the current standards used by road professionals. Indeed, the low mechanical performances and the high water sensibility of chalk do not allow this material to be used. However, it seems possible to find some pre-treatments to harden chalk for a use in road base courses.This material is found profusely in some French regions otherwise limited in upscale aggregates (Nord-Pas de Calais, Champagne-Ardenne…). Therefore, valorising chalk may overcome the lack of aggregates, contribute to the preservation of natural resources, save up money and avoid pollution due to distant supplying.The study presented here is conducted in partnership between the Ecole Centrale de Lille Civil Engineering Laboratory and the Eurovia Roadworks Laboratory of Loos. We provide several trails aimed at improving the mechanical properties of chalk for its use in road base courses

La présente étude vise à valoriser des résidus agroindustriels comme matériaux pour l’habitat et la construction. Dans ce contexte, les travaux de recherche s’articulent autour de deux axes majeurs : le développement d’un liant alternatif et l’élaboration de matériaux composites à partir de ce liant alternatif et des matériaux végétaux. Deux liants composés utilisant des cendres de bagasse, nommés cendres de bagasse-chaux et ciment-cendres de bagasse ont été étudiés. A partir de ces liants composés, deux types de matériaux composites incluant des matériaux végétaux ont été élaborés : un composite incorporant des granulats de bagasse et de coco et un autre renforcé par des pulpes d’eucalyptus. Les propriétés physiques, chimiques, mécaniques et hydriques de ces matériaux ont été déterminées. Les résultats obtenus montrent que la calcination des cendres de bagasse à 600°C et la sélection des particules de taille inférieure à un diamètre seuil compris entre 45 et 63µm augmentent sa réactivité. Le liant composé cendres de bagasse-chaux est susceptible de développer une résistance à la compression de l’ordre de 39MPa à 28 jours, une valeur supérieure à celle des liants composés matériaux pouzzolaniques-chaux étudiés dans la littérature. Grace à sa faible alcalinité, ce liant composé préserve mieux les matériaux végétaux vis à vis de leur minéralisation et leur fragilisation comparativement au liant à base de ciment. L’incorporation de pulpes cellulosiques dans le liant composé cendres de bagasse-chaux permet d’obtenir des matériaux composites ayant des propriétés à la flexion comparables à celles d’un composite ciment-pulpes cellulosiques. / The present study aims to add value to agroindustrial residues as housing and building materials. In this context, the research works revolve around two main lines: the development of an alternative binder using agroindustrial residues and the production of composite materials from this alternative binder and plant resources. Two composed binder using bagasse ash, named bagasse ash lime and cement-bagasse ash, were optimised and produced. Using these composed binder, two kinds of composite materials including plant resources were produced: one composite developed with vegetable aggregates and another one reinforced with eucalyptus pulps. The physical, chemical, mechanical and hydric properties of these materials were investigated. The results show that the bagasse ash recalcination at 600 °C and the selection of the particles under a diameter limit (between 45 and 63 µm) improve its reactivity. Blended with slaked lime, the composed binder obtained with these parameters is likely to develop a compressive strength higher than 39 MPa at 28 days; this value is higher than the compressive strength of pouzzolanic material and lime based binder studied in the literature. In addition, due to the lower alkalinity of the interstitial solution of this composed binder, related to the lime consumption by the pouzzolanic material, it better protects vegetable materials from mineralization than the binders based on Portland cement. The incorporation of the cellulosic pulps in the composed binder lime-bagasse ash produces composite materials with a similar flexural behaviour as a composite made with cement and cellulosic pulp.

This thesis is focused at possibilities of preparation and characterization of XRD-amorphous delaminated and dehydroxylated talc phase – meta-talc, which can have its potential application and a starter material for a preparation of magnesium-silicate analogues of geopolymers. Changes in structure and morphology of talc ore were observed during this work. For the purposes of this research, two various talc ores – chloritic and dolomitic were examined. Whole process of meta-talc preparation was examined with whole scale of instrumental techniques such as X-ray diffraction, simultaneous thermogravimetric a differential thermal analysis, infrared spectroscopy, scanning electron microscopy or laser analysis of particle size. Meta-talc can be obtained via mechanochemical activation of talc ore with subsequent calcination. Mechanochemical treatment lead to destruction of original crystal structure and breaking of original bonds, i.e. the product of this treatment was almost amorphous and delaminated. Most of hydroxyl groups were converted to molecules of water which remained adsorbed or coordinated in ore structure. These molecules were removed during calcination step.

In modern point of view of waste management is desirable to effectively process the grates possible amount of wastes. Sediments from cleaning of mined lime stones contains a lot of clay components, but there is also indispensable share of soft calcite. This composition makes these sediments a promising material for preparation of hydraulic binders. Production of common hydraulic binders, especially Portland cement, is very energy-intensive plus loads environment with considerable amount of combustion gases, therefore it is necessary to explore possibilities of alternative low - energy binders production and usage.