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  • Effects of ultrasonic vibration on the micro-molding processing of polylactide

     Sacristan, Matias; Planta, Xavier; Morell Bel, Mireia; Puiggali Bellalta, Jorge
    Ultrasonics sonochemistry
    Date of publication: 2014
    Journal article

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    A new ultrasonic micro-molding system was used to process polylactide (PLA) and fabricate reduced dimension specimens. Plasticization and molding of PLA were achieved by applying ultrasonic waves after feeding the polymer into a plasticizing chamber. Chemical and physical characteristics of processed PLA varied depending on the processing window (i.e. changes in ultrasonic wave amplitude between 14.2 and 48.1 µm and molding pressure between 0.5 in 6 bars). In terms of chemical effects, the application of ultrasound can lead to lower molecular weights (e.g. decreases of more than 45% in the weight average molecular weight), revealing partial degradation of the material. Also, the processed materials exhibited slightly higher thermal degradability than pure PLA because ultrasonic vibrations break molecular linkages and worsen the polymer structure. Finally, the processing conditions for the preparation of PLA specimens could be optimized without causing degradation and preserving structural characteristics and mechanical properties. Specifically, the use of an amplitude of 48.1 µm and a pressure of 3 bars gave samples with the same molecular weight as the raw material (i.e. 117,500 g/mol as opposed to 117,300 g/mol for Mw).

    A new ultrasonic micro-molding system was used to process polylactide (PLA) and fabricate reduced dimension specimens. Plasticization and molding of PLA were achieved by applying ultrasonic waves after feeding the polymer into a plasticizing chamber. Chemical and physical characteristics of processed PLA varied depending on the processing window (i.e. changes in ultrasonic wave amplitude between 14.2 and 48.1 μm and molding pressure between 0.5 in 6 bars). In terms of chemical effects, the application of ultrasound can lead to lower molecular weights (e.g. decreases of more than 45% in the weight average molecular weight), revealing partial degradation of the material. Also, the processed materials exhibited slightly higher thermal degradability than pure PLA because ultrasonic vibrations break molecular linkages and worsen the polymer structure. Finally, the processing conditions for the preparation of PLA specimens could be optimized without causing degradation and preserving structural characteristics and mechanical properties. Specifically, the use of an amplitude of 48.1 μm and a pressure of 3 bars gave samples with the same molecular weight as the raw material (i.e. 117,500 g/mol as opposed to 117,300 g/mol for Mw).

  • Poly(butylene azelate-co-butylene succinate) copolymers: Crystalline morphologies and degradation

     Diaz Andrade, Angelica Maria; Franco Garcia, Maria Lourdes; Estrany Coda, Francisco; Del Valle Mendoza, Luis Javier; Puiggali Bellalta, Jorge
    Polymer degradation and stability
    Date of publication: 2014-01
    Journal article

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    Random copolymers derived from 1,4-butanediol and two dicarboxylic units differing in the parity of the number of methylene groups and length of the polymethylene sequence (i.e. succinic and azelaic acids) were studied in terms of thermal properties, crystalline structure and morphology, crystallization kinetics and biodegradability. All samples were semicrystalline and their thermal properties varied in a wide temperature range. Copolymers crystallized according to the monoclinic a-form of polybutylene succinate and the orthorhombic structure postulated for polybutylene azelate depending on the predominant dicarboxylate unit. The behavior of the copolymer with an intermediate composition was complex due to strong dependence of the predominant crystalline form on crystallization and processing conditions. Interestingly, crystallization into the azelate structure was favored when samples were rapidly cooled from the melt, resulting in an unexpected increase in the degree of crystallinity. Spherulitic morphologies were clearly different (i.e. ringed spherulites and axialites) depending on the preferential crystalline structure. Enzymatic degradability of the two homopolyesters was highly different and could be enhanced by incorporation of comonomer units. Preferential enzymatic attack on amorphous regions highlighted the spherulitic morphologies of copolymers having well developed, distinctive ringed structures. © 2013 Elsevier Ltd. All rights reserved.

  • Mineralization of DNA into nanoparticles of hydroxyapatite

     Bertran Cànovas, Oscar; Del Valle Mendoza, Luis Javier; Revilla Lopez, Guillermo; Chaves Barboza, Gustavo Adolfo; Cardus Andreu, Lluis; Casas Becerra, M. Teresa; Casanovas Salas, Jordi; Turon, Pau; Puiggali Bellalta, Jorge; Aleman Llanso, Carlos Enrique
    Dalton transactions
    Date of publication: 2014-01-07
    Journal article

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    Encapsulation of DNA into hydroxyapatite (HAp) has been investigated using a rational approach that involves computer simulation and experimental techniques. The temporal evolution of the radial distribution functions derived from atomistic molecular dynamics simulations of Ca2+, PO 4 3- and OH--containing aqueous solutions in the presence and absence of B-DNA has been used to conclude that the backbone of the double helix acts as a template for HAp growth. More specifically, results reveal the formation of calcium phosphate clusters at the first stages of the simulations, which subsequently re-organize to nucleate HAp. This effect is produced in the absence and, especially, presence, of DNA indicating that the biomolecules do not inhibit but even promote mineral growth. Furthermore, computer simulations suggest that the diffusion of the OH- anions through the inorganic solution is the limiting step for the nucleation of the biomineral. Nanocapsules and crystalline nanorods of HAp containing DNA molecules inside have been prepared by mixing solutions containing Ca 2+ and PO4 3- ions with fish sperm DNA at high pH. The dimensions and morphology of such nanostructures have been examined by transmission electron microscopy, while the characterization of the biomineral has been focused on the identification of DNA inside HAp using infrared, X-ray photoelectron and UV-vis spectroscopies, as well as gel electrophoresis. The biominerals reported in this work are important for biomedical applications requiring the protection of DNA from aggressive environmental conditions. © 2014 The Royal Society of Chemistry.

  • Study on the crystallization of poly(butylene azelate-co-butylene succinate) copolymers

     Diaz Andrade, Angelica Maria; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    Thermochimica acta
    Date of publication: 2014-01-10
    Journal article

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    Poly(butylene azelate-co-butylene succinate) samples with different azelate/succinate ratios were synthesized and characterized. Calorimetric data indicate a semicrystalline character for all copolyesters studied and a melting point depression that could be interpreted on the basis of complete exclusion of comonomers from well organized lamellae. Crystallization first occurred through the succinate rich segments, which resulted in a peculiar behavior of copolymers having an intermediate composition. In this case, crystallization of azelate segments was paradoxically enhanced when samples were quenched. Equilibrium melting temperatures significantly decreased with increasing comonomer content compared to those of the corresponding homopolymers. Incorporation of comonomers had a distinct effect on the secondary nucleation constant depending on the composition as deduced from Lauritzen and Hoffman analysis. Thus, azelate units clearly increased the nucleation constant of copolymers rich on succinate units, whereas the incorporation of succinate units had a lower influence on the constant of copolyesters having high azelate content.

  • Structural transitions of nylon 47 and clay influence on its crystallization behavior

     Morales Gámez, Laura Teresa; Casas Becerra, M. Teresa; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    European polymer journal
    Date of publication: 2013-06
    Journal article

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    Basic diffraction data on nylon 47 pointed out a peculiar structure of hydrogen bonds along two directions. Nylon 47 showed reversible polymorphic transitions during heating/cooling processes that were analyzed by real time synchrotron WAXD experiments. Results indicated that nylon 47 had a first structural transition at low temperature, followed by a gradual Brill transition towards a pseudohexagonal packing. Nylon 47 crystallized from the melt giving rise to spherulites with different characteristics than those attained with conventional even-even nylons. Interestingly, spherulites crystallized at low supercooling underwent a reversible change in birefringence with temperature. This was due to the reversible structural changes caused by temperature variations and the flat on lamellar morphology. Intercalated and exfoliated nanocomposites based on nylon 47 were prepared by solution intercalation and melt mixing using Cloisites 25A and 30B. The influence of the final silicate layer morphology on the hot crystallization behavior was investigated. Crystallization rates of the neat polymer and its two nanocomposites were significantly different, mainly due to variations in the primary nucleation

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    Sensitive thermal transitions of nanoscale polymer samples using the bimetallic effect: Application to ultra-thin polythiophene  Open access

     Ahumada Heredero, Óscar; Perez Madrigal, Maria Del Mar; Ramírez García, Jorge; Curcó Cantarell, David; Esteves, Carina; Armelin Diggroc, Elaine; Luongo, Giovanni; Puiggali Bellalta, Jorge; Aleman Llanso, Carlos Enrique; Salvador Matar, Antonio
    Review of scientific instruments
    Date of publication: 2013-06-15
    Journal article

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    A sensitive nanocalorimetric technology based on microcantilever sensors is presented. The tech- nology, which combines very short response times with very small sample consumption, uses the bimetallic effect to detect thermal transitions. Specifically, abrupt variations in the Young¿s modu- lus and the thermal expansion coefficient produced by temperature changes have been employed to detect thermodynamic transitions. The technology has been used to determine the glass transition of poly(3-thiophene methyl acetate), a soluble semiconducting polymer with different nanotechno- logical applications. The glass transition temperature determined using microcantilevers coated with ultra-thin films of mass = 10 - 13 gis5.2 ¿ C higher than that obtained using a conventional differential scanning calorimeter for bulk powder samples of mass = 5 × 10 - 3 g. Atomistic molecular dynamics simulations on models that represent the bulk powder and the ultra-thin films have been carried out to provide understanding and rationalization of this feature. Simulations indicate that the film-air in- terface plays a crucial role in films with very small thickness, affecting both the organization of the molecular chains and the response of the molecules against the temperature.

    A sensitive nanocalorimetric technology based on microcantilever sensors is presented. The tech- nology, which combines very short response times with very small sample consumption, uses the bimetallic effect to detect thermal transitions. Specifically, abrupt variations in the Young’s modu- lus and the thermal expansion coefficient produced by temperature changes have been employed to detect thermodynamic transitions. The technology has been used to determine the glass transition of poly(3-thiophene methyl acetate), a soluble semiconducting polymer with different nanotechno- logical applications. The glass transition temperature determined using microcantilevers coated with ultra-thin films of mass = 10 − 13 gis5.2 ◦ C higher than that obtained using a conventional differential scanning calorimeter for bulk powder samples of mass = 5 × 10 − 3 g. Atomistic molecular dynamics simulations on models that represent the bulk powder and the ultra-thin films have been carried out to provide understanding and rationalization of this feature. Simulations indicate that the film-air in- terface plays a crucial role in films with very small thickness, affecting both the organization of the molecular chains and the response of the molecules against the temperature.

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    Modeling biominerals formed by apatites and DNA  Open access

     Revilla Lopez, Guillermo; Casanovas, Jordi; Bertran Cànovas, Oscar; Turon, Pau; Puiggali Bellalta, Jorge; Aleman Llanso, Carlos Enrique
    Biointerphases: an open access journal for the biomaterials interface community
    Date of publication: 2013-04-08
    Journal article

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    Different aspects of biominerals formed by apatite and DNA have been investigated using computer modeling tools. Firstly, the structure and stability of biominerals in which DNA molecules are embedded into hydroxyapatite and fluoroapatite nanopores have been examined by combining different molecular mechanics methods. After this, the early processes in the nucleation of hydroxyapatite at a DNA template have been investigated using molecular dynamics simulations. Results indicate that duplexes of DNA adopting a B double helix can be encapsulated inside nanopores of hydroxyapatite without undergoing significant distortions in the inter-strand hydrogen bonds and the intra-strand stacking. This ability of hydroxyapatite is practically independent of the DNA sequence, which has been attributed to the stabilizing role of the interactions between the calcium atoms of the mineral and the phosphate groups of the biomolecule. In contrast, the fluorine atoms of fluoroapatite induce pronounced structural distortions in the double helix when embedded in a pore of the same dimensions, resulting in the loss of its most relevant characteristics. On the other hand, molecular dynamics simulations have allowed us to observe the formation of calcium phosphate clusters at the surface of the B-DNA template. Electrostatic interactions between the phosphate groups of DNA and Ca 2+ have been found to essential for the formation of stable ion complexes, which were the starting point of calcium phosphate clusters by incorporating PO34 from the solution

  • Hybrid block copolymers constituted by peptides and synthetic polymers: An overview of synthetic approaches, supramolecular behavior and potential applications

     Morell Bel, Mireia; Puiggali Bellalta, Jorge
    Polymers (Basel)
    Date of publication: 2013-02-11
    Journal article

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    Hybrid block copolymers based on peptides and synthetic polymers, displaying different types of topologies, offer new possibilities to integrate the properties and functions of biomacromolecules and synthetic polymers in a single hybrid material. This review provides a current status report of the field concerning peptide-synthetic polymer hybrids. The first section is focused on the different synthetic approaches that have been used within the last three years for the preparation of peptide-polymer hybrids having different topologies. In the last two sections, the attractive properties, displayed in solution or in the solid state, together with the potential applications of this type of macromolecules or supramolecular systems are highlighted.

    Hybrid block copolymers based on peptides and synthetic polymers, displaying different types of topologies, offer new possibilities to integrate the properties and functions of biomacromolecules and synthetic polymers in a single hybrid material. This review provides a current status report of the field concerning peptide-synthetic polymer hybrids. The first section is focused on the different synthetic approaches that have been used within the last three years for the preparation of peptide-polymer hybrids having different topologies. In the last two sections, the attractive properties, displayed in solution or in the solid state, together with the potential applications of this type of macromolecules or supramolecular systems are highlighted.

  • Influence of microstructure on the crystallization of segmented copolymers constituted by glycolide and trimethylene carbonate units

     Diaz Celorio, Elena; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    Express polymer letters
    Date of publication: 2013-02
    Journal article

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  • Study on the hydrolytic degradation of glycolide/trimethylene carbonate copolymers having different microstructure and composition

     Diaz Celorio, Elena; Franco Garcia, Maria Lourdes; Rodriguez Galan, Rafael Alfonso; Puiggali Bellalta, Jorge
    Polymer degradation and stability
    Date of publication: 2013-01
    Journal article

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    Hydrolytic degradation of a series of copolymers synthesized by ring opening polymerization of trimethylene carbonate and glycolide was studied by following the weight loss and changes in molecular weight, polydispersity index and mechanical properties. Analyses of H-1 NMR and FTIR spectra taken during exposure to a pH 7.4 phosphate buffered solution were also performed. Copolymers with different microstructures (i.e. random, triblock and segmented copolymers) were synthesized. Most segmented copolymers studied had identical trimethylene carbonate content but differed in the hard segment content. Composition was also varied to demonstrate the influence of the soft segment composition. Results were consistent with a model where degradation started in the amorphous phases and affected the glycolide units of the less compact soft segments and the regions within lamellar stacks. This degradation step led to a clear decrease of GGG triads (NMR data) and amorphous glycolide content (FTIR data), as well as an increase in Young's modulus. Degradation subsequently proceeded through the crystalline glycolide units belonging to lamellar stacks. The molecular weight of the degraded samples reached always an asymptotic value that corresponded to a solubility limit for fragments with high TMC content and for highly crystalline entities constituted by glycolide rich fragments. Results pointed to the importance of the hard segment content and the composition of the soft segment, which logically influenced the distribution between amorphous and crystalline phases.

  • Nanospheres and nanocapsules of amphiphilic copolymers constituted by methoxypolyethylene glycol cyanoacrylate and hexadecyl cyanoacrylate units

     Valente, Ilaria; Del Valle Mendoza, Luis Javier; Casas Becerra, M. Teresa; Franco Garcia, Maria Lourdes; Rodriguez Galan, Rafael Alfonso; Puiggali Bellalta, Jorge; Marchisio, D.
    Express polymer letters
    Date of publication: 2013-01
    Journal article

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  • New insights on the crystallization and melting of cyclic PCL chains on the basis of a modified Thomson-Gibbs equation

     Su, Hsuan-Han; Chen, Hsin-Lung; Diaz Andrade, Angelica Maria; Casas Becerra, M. Teresa; Puiggali Bellalta, Jorge; Hoskins, Jessica N; Grayson, Scott M.; Pérez, Ricardo A.; Müller, Alejandro J.
    Polymer
    Date of publication: 2013-01-24
    Journal article

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  • Bioactive nanomembranes of semiconductor polythiophene and thermoplastic polyurethane: Thermal, nanostructural and nanomechanical properties

     Perez Madrigal, Maria Del Mar; Giannotti, Marina I.; Oncins Marco, Gerard; Franco Garcia, Maria Lourdes; Armelin Diggroc, Elaine; Puiggali Bellalta, Jorge; Sanz Carrasco, Fausto; Del Valle Mendoza, Luis Javier; Aleman Llanso, Carlos Enrique
    Polymer Chemistry
    Date of publication: 2013-02-07
    Journal article

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  • Study on the hydrolytic degradation of the segmented GL-b-[GL-co-TMC-co-CL] -b-GL copolymer with application as monofilar surgical suture

     Marquez Lobato, Yolanda; Franco Garcia, Maria Lourdes; Turon, Pau; Rodriguez Galan, Rafael Alfonso; Puiggali Bellalta, Jorge
    Polymer degradation and stability
    Date of publication: 2013-12
    Journal article

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    The hydrolytic degradation of Monosyn¿, a segmented copolymer derived from glycolide, trimethylene carbonate and e-caprolactone, has been evaluated in buffered aqueous media at different pH and temperature. Degradation processes have been followed by considering mass loss and molecular weight profiles as well as the changes on 1H NMR and FTIR spectra, morphology and both calorimetric and mechanical properties during exposure to the selected media and temperature. In all cases, the mass and molecular weight evolutions fitted with first order kinetic processes which were indicative of a random chain scission mechanism. Rate constants were found to strongly depend on temperature and pH. A slight deviation towards a backbiting mechanism was only found in the acid medium at long exposure times when degradation progresses through crystalline domains and recombination of ester groups were probable. Amorphous and glycolide rich domains were more susceptible to the hydrolytic attack as revealed from mechanical assays and both spectroscopic and calorimetric data. Morphological changes occurring during degradation were highly dependent on pH and indeed different steps affecting the outer (longitudinal cracks) and inner (transversal cracks) parts of sutures could be distinguished. The high content on amorphous soft segments gave rise to well-defined circumferential cracks that affected the inner part of exposed sutures and were interpreted as a consequence of the hydrolytic attack to intralamellar regions. © 2013 Elsevier Ltd. All rights reserved.

  • Formulation of anticorrosive paints employing conducting polymers  Open access

     Martí Barroso, Mireia
    Defense's date: 2013-07-08
    Universitat Politècnica de Catalunya
    Theses

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    The intention and purpose of the present thesis is to prepare a series of protective coatings using some conducting polymers (CPs) as corrosion inhibitors. The use of organic paints is the most common method for corrosion prevention. Anticorrosive coatings form a class of high-performance systems with a very wide range of applications and being classified in two broad groups: heavy-duty coatings, for high performance, and light-duty coatings, for medium performance. The first class being required for highly aggressive medium, like oil platforms, bridges, chemical industry plants, containers, shipping, and others; the late being employed mainly for outside industrial environments, urban environments, houses, offices, and others. This thesis consists of an overview and a compendium of the following work stages and results: 1. Preparation of nanostructured CPs for corrosion inhibition: Study of the ability of poly(N-methylpyrrole) to form nanostructures and the performance of such nanostructures when act as anticorrosive additive of organic coatings. 2. Partial replacement of metallic zinc dust usually employed in heavy duty protective coatings, by a small concentration of CPs: Study of the use of a small amount of polyaniline emeraldine salt as a partial substitute of metallic zinc dust in marine epoxy primers in order to maintain corrosion inhibition. 3. Evaluation of an environmentally friendly anticorrosive pigment for alkyd priming: Study of the substitution of a high concentration of zinc phosphate, commonly employed in light-duty coatings, by a very low concentration of polyaniline emeraldine base (undoped form), polyaniline emeraldine salt (doped form) and an eco-friendly polythiophene derivative (partially oxidized) in an alkyd coatings and the study of their protective performance using accelerated corrosion assays. 4. Preparation of a novel epoxy coating, based on DMSO as green solvent and free of zinc anticorrosive pigment, and its application on carbon steel protection: Formulation and evaluation of a novel anticorrosive epoxy coating based on DMSO solvent and free of zinc, using polyaniline emeraldine base and poly[2,2’-(3-methylacetate)thiophene] as anticorrosive pigments. All the results derived from the present thesis have been accepted or have been sent for publication in international journals and also reported in some international congresses, as we point below: 1. M. Martí, G. Fabregat, F. Estrany, C. Alemán, E. Armelin, “Nanostructured conducting polymer for dopamine detection”, J.Mater. Chem., 2010, 20, 10652-10660. 2. E. Armelin, M. Martí, F. Liesa, J.I. Iribarren, C. Alemán, “Partial replacement of metallic zinc dust in heavy duty protective coatings by conducting polymer”, Prog. Org. Coat., 2010, 69, 26-30. 3. M. Martí, G. Fabregat, D.S. Azambuja, C. Alemán, E. Armelin, “Evaluation of an environmentally friendly anticorrosive pigment for alkyd primer”, Prog. Org. Coat., 2012, 73, 321–329. 4. M. Martí, L. Molina, C. Alemán, E. Armelin, “Replacement of toxic solvents and anticorrosive pigments used in solvent-borne epoxy coatings by safer functional organic compounds”, submitted for publication in Journal of Hazardous Materials, 2013. 5. M. Martí, E. Armelin, J. Iribarren, C. Alemán. Soluble polythiophenes as anticorrosive additives for marine epoxy paints”, submitted for publication in Materials and Corrosion, 2013. 6. G. Fabregat, M. Martí, F. Estrany, C. Alemán, E. Armelin, “Nanostructured Poly(N-Methylpyrrole) and Its Application in Dopamine Detection”, E-MRS 2010 Spring Meeting. 2010, Strasbourg, France. 7. E. Armelin, M. Martí, F. Estrany, C. Alemán, “Environmentally friendly anticorrosive additive to replace zinc and its compounds in alkyd and epoxy primers”, 12th Mediterranean Congress of Chemical Engineering: shaping the future of chemical engineering. 2011, Barcelona, Spain

    El propósito de la presente tesis es preparar una serie de recubrimientos protectores empleando polímeros conductores (CPs) como inhibidores de la corrosión. El uso de pinturas orgánicas es el método más empleado para la prevención de la corrosión. Los recubrimientos anticorrosivos forman una clase de sistemas de alto rendimiento con una amplia variedad de aplicaciones y pueden ser clasificados en dos grandes grupos: recubrimientos de altas prestaciones y recubrimientos de suaves prestaciones. El primero de ellos es el que se emplea en estructuras expuestas a ambientes muy agresivos, tales como: plataformas petrolíferas, puentes, plantas industriales químicas, contenedores, barcos, entre otros; y el último es el que se suele emplear en el exterior de ambientes industriales, ambientes urbanos, casas, oficinas, entre otros. La presente tesis consiste en un compendio de las siguientes etapas del trabajo y resultados: 1. Preparación de CPs nanoestructurados para inhibición de la corrosión: Estudio de la habilidad del Poli(N-metilpirrol) para formar estructuras nanoestructuradas y la actuación de éstas como aditivo anticorrosivo en recubrimientos orgánicos. 2. Sustitución parcial del zinc metálico en polvo habitualmente empleado en pinturas de altas prestaciones, por una pequeña cantidad de CP: Estudio del uso de pequeñas concentraciones de polianilina sal emeraldina (PAni-EB), como sustituto parcial del zinc metálico en polvo, en pinturas de imprimación epoxi marinas, con el objetivo de mantener la inhibición a la corrosión. 3. Evaluación de pigmentos anticorrosivos amigables con el medio ambiente para pinturas de imprimación alquídicas: Estudio de la sustitución de una elevada concentración de fosfato de zinc, generalmente empleado en recubrimientos de suaves prestaciones, por una concentración muy baja de PAni-EB (forma no-dopada), PAni-ES (forma dopada) y un derivado del politiofeno (parcialmente dopado) en un recubrimiento alquídico, y el estudio de sus capacidades protectoras empleando ensayos de corrosión acelerados. 4. Preparación de una nueva pintura epoxi, basada en DMSO como disolvente ecológico y libre de pigmento anticorrosivo de zinc, y su aplicación para la protección de acero al carbono: Formulación y evaluación de una nueva pintura epoxi basada en DMSO como solvente y empleando PAni-EB y poli[2, 2’-(3-metilacetato)tiofeno] como nuevos pigmentos anticorrosivos. Todos los resultados obtenidos en la presente tesis han sido aceptados o han sido enviados para publicación en revistas internacionales; además, algunos resultados han sido divulgados recientemente en congresos internacionales, tal y como se describe abajo: 1. M. Martí, G. Fabregat, F. Estrany, C. Alemán, E. Armelin, “Nanostructured conducting polymer for dopamine detection”, J. Mater. Chem., 2010, 20, 10652-10660. 2. E. Armelin, M. Martí, F. Liesa, J.I. Iribarren, C. Alemán, “Partial replacement of metallic zinc dust in heavy duty protective coatings by conducting polymer”, Prog. Org. Coat., 2010, 69, 26-30. 3. M. Martí, G. Fabregat, D.S. Azambuja, C. Alemán, E. Armelin, “Evaluation of an environmentally friendly anticorrosive pigment for alkyd primer”, Prog. Org. Coat., 2012, 73, 321–329. 4. M. Martí, L. Molina, C. Alemán, E. Armelin, “Replacement of toxic solvents and anticorrosive pigments used in solvent-borne epoxy coatings by safer functional organic compounds”, enviado para publicación en Journal of Hazardous Materials, 2013. 5. M. Martí, E. Armelin, J. Iribarren, C. Alemán. Soluble polythiophenes as anticorrosive additives for marine epoxy paints”, enviado para publicación en Materials and Corrosion, 2013. 6. G. Fabregat, M. Martí, F. Estrany, C. Alemán, E. Armelin, E-MRS 2010 Spring Meeting. 2010, Strasbourg, France. 7. E. Armelin, M. Martí, F. Estrany, C. Alemán, 12th Mediterranean Congress of Chemical Engineering: shaping the future of chemical engineering. 2011, Barcelona, Spain.

  • NUEVOS POLIMEROS DERIVADOS DE LACTIDA: ESTRUCTURA, APLICACIONES BIOMEDICAS Y

     Puiggali Bellalta, Jorge
    Participation in a competitive project

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  • Electrospun nanofibers of a degradable poly(ester amide). Scaffolds loaded with antimicrobial agents

     Del Valle Mendoza, Luis Javier; Roa Ardilla, Manuel; Diaz Andrade, Angelica Maria; Casas Becerra, M. Teresa; Puiggali Bellalta, Jorge; Rodriguez Galan, Rafael Alfonso
    Journal of polymer research
    Date of publication: 2012-01
    Journal article

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  • Biodegradable polyesters reinforced with triclosan loaded polylactide micro/nanofibers: Properties, release and biocompatibility

     Del Valle Mendoza, Luis Javier; Diaz Andrade, Angelica Maria; Royo, M.; Rodriguez Galan, Rafael Alfonso; Puiggali Bellalta, Jorge
    Express polymer letters
    Date of publication: 2012
    Journal article

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  • New Sulfonated Polystyrene and Styrene¿Ethylene/Butylene¿Styrene Block Copolymers for Applications in Electrodialysis

     Müller, Franciélli; Ferreira, Carlos Arthur; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge; Aleman Llanso, Carlos Enrique; Armelin Diggroc, Elaine
    Journal of physical chemistry B
    Date of publication: 2012-09
    Journal article

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  • Thermal degradation studies on homopolymers and copolymers based on trimethylene carbonate and glycolide units

     Diaz Celorio, Elena; Franco Garcia, Maria Lourdes; Marquez, Yolanda; Rodriguez Galan, Rafael Alfonso; Puiggali Bellalta, Jorge
    Thermochimica acta
    Date of publication: 2012-01-20
    Journal article

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    The non-isothermal degradation kinetics of poly(trimethylene carbonate) (PTMC) and polyglycolide (PGL) was investigated by thermogravimetric (TG and DTG) analysis in the temperature range between 50 and 550 °C at different heating rates (0.5–40 °C/min). Both homopolymers showed a complex multi-step degradation process. Kinetic analysis was successfully performed for the main degradation steps using the isoconversional Kissinger–Akahira–Sunose and Friedman methods. Activation energies of these steps were practically independent of the degree of conversion. The true kinetic triplets (E, A, f(α)) were determined by the Coats–Redfern method. The results clearly indicated that the two homopolymers mainly degraded by quite different mechanisms, i.e. A3 and F1, which may be associated with different depolymerization processes (e.g. decarboxylation or unzipping). Degradation of copolymers of trimethylene carbonate and glycolide with different chemical microstructures (i.e. random, blocky and segmented) and of blends with different percentages of both homopolymers was also studied. Interestingly, a deceleration and an acceleration for the decomposition of trimethylene carbonate and glycolide segments were observed, respectively. Specifically, the two-step degradation process of the blend with 50 wt% of each homopolymer was analyzed by the above methodologies. Kinetic data indicated that the main degradation process involved a different mechanism from that previously determined for PTMC and PGL, and that the activation energy was intermediate (i.e. EPTMC < EBlend < EPGL).

  • Synthesis of glycolide/trimethylene carbonate copolymers: influence of microstructure on properties

     Diaz Celorio, Elena; Franco Garcia, Maria Lourdes; Rodriguez Galan, Rafael Alfonso; Puiggali Bellalta, Jorge
    European polymer journal
    Date of publication: 2012-01
    Journal article

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    Copolymers of glycolide and trimethylene carbonate with different compositions and microstructures (i.e. random, blocky and segmented) were synthesized by two-step ring opening polymerization. NMR analyses revealed that transesterification reactions took place during the first step, which corresponded to the synthesis of soft segments, and mainly when the trimethylene carbonate content of the reaction medium was high. The transesterification percentage did not significantly change with the addition of hard blocks in the second reaction step. Infrared spectroscopy was a complementary, highly effective tool to evaluate the hard segment length, crystallinity and glycolide percentage incorporated into the crystalline phase for all studied samples. Calorimetric analyses showed dependency of properties on the length of the polyglycolide hard segment and also good miscibility between glycolide and trimethylene carbonate rich phases. Crystalline morphologies attained with segmented and random copolymers were significantly different, although in all cases a positive birefringence was detected. Thermogravimetric analyses indicated that all studied copolymers had a similar degradation behavior, which was intermediate between those observed in the corresponding homopolymers. Samples with a significant glycolide unit content showed a stabilizing effect for the degradation of poly(trimethylene carbonate) blocks.

  • Conformational Exploration of Two Peptides and Their Hybrid Polymer Conjugates: Potentialities As Self-Aggregating Materials

     Haspel, Nurit; Laurent, Adele D.; Zanuy Gomara, David; Nussinov, Ruth; Aleman Llanso, Carlos Enrique; Puiggali Bellalta, Jorge; Revilla Lopez, Guillermo
    Journal of physical chemistry B
    Date of publication: 2012-12-06
    Journal article

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  • Thermal degradation studies of poly(trimethylene carbonate)blends with either polylactide or polycaprolactone

     Marquez Lobato, Yolanda; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    Thermochimica acta
    Date of publication: 2012-10-04
    Journal article

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    The thermal stability and degradation kinetics of poly(trimethylene carbonate) (PTMC) blends with different ratios of polylactide (PLA) and alternatively polycaprolactone (PCL) were investigated by thermogravimetric analysis under a nitrogen atmosphere. These studies were extended to the single components (i.e. PCL and PLA). In all cases, the derivative thermogravimetric curves indicated a complex decomposition process with at least two degradation steps. The kinetic parameters of the main step, including activation energy, reaction model and pre-exponential factor, were evaluated by the Kissinger, isoconversional (Friedman and KAS) and Coats¿Redfern methods. Data of the main decomposition process were obtained by mathematical deconvolution of experimental DTG curves acquired at heating rates ranging from 2 to 40 °C/min. It was demonstrated that degradation of blends did not correspond to a mere superposition of the characteristic decomposition processes of the two involved polymers. Furthermore, PCL and PLA influenced the decomposition of the less thermally stable PTMC component in a different way. Thus, PLA modified the degradation of PTMC, and specifically led to thermal stabilization and a new decomposition process characterized by a higher activation energy. On the other hand, PCL favored the degradation of PTMC by enhancing a typical minor decomposition process that occurred in the single component at a lower temperature. The main decomposition step of PTMC, PLA, PCL and the studied blends always followed an Avrami model but with significant differences in their exponents (i.e. from 2 to 7

  • Influence Of Composition And Microstructure On Properties Of New Trimethylene Carbonate/Glycolide Copolymers With Biomedical Applications

     Díaz Celorio, Elena
    Defense's date: 2012-07-23
    Department of Chemical Engineering, Universitat Politècnica de Catalunya
    Theses

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  • Study of Nanocomposites Prepared from Polyamides and Biodegradable Polyesters and Poly(ester amide)s  Open access

     Morales Gámez, Laura Teresa
    Defense's date: 2012-01-23
    Department of Chemical Engineering, Universitat Politècnica de Catalunya
    Theses

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    Polymer clay nanocomposites of polyamides and biodegradable polymers with three kinds of organomodified clays were prepared by different techniques (in situ polymerization, solution casting, and melt mixing). The polymers used in this research were nylons 56, 65 and 47 and the biodegradable polymers: poly (glycolic acid-alt-6-hydrohexanoic acid) and poly(glycolic acid-alt-6-aminohexanoic acid). The development of biodegradable nanocomposites with improved or modified material properties is an interesting topic since these new materials are expected to replace already existing biodegradable and non-biodegradable commodity plastics in some specific applications.This project aims to study the influence of clay particles incorporated in a polymer matrix on the crystallization processes, the study of the in situ polymerization kinetics of mixtures of clays and monomers of biodegradable polymers, as well as the influence of nanoparticles on the thermal behavior and morphologic parameters. Even-odd, and odd-even polyamides were chosen to study the Brill transition and to prepare nanocomposites with organomodified clays. These polyamides have a peculiar structure where hydrogen bonds are established along two different directions. X-ray diffraction as well as SAXS-WAXD synchrotron experiments were employed to study the structural changes induced by temperature, during heating and cooling. Different organomodified clays were used to prepare nanocomposites, which final structure was found to be dependent on the preparation method. Nanocomposites derived from biodegradable polymers were characterized by means of X-ray diffraction and transmission electron microscopy. Morphological studies showed that the extent of clay dispersion depended on the clay type and on the preparation technique. Hence, exfoliated and intercalated nanocomposites could be obtained. The final nanocomposite structure was found to have a great influence on both cold and hot crystallization processes. Hence, the crystallization rate increased and decreased with respect to the neat polymer when intercalated and exfoliated structures were respectively obtained. The kinetics of the polymerization process was also studied by means of FTIR and SAXS-WAXD. The results indicate that the presence of the organomodified clay had a remarkable effect on the kinetic parameters.

  • Copolymerization of potassium chloroacetate and potassium N-chloroacetyl-6-aminohexanoate

     Murase Fernandez, Sara Keiko; Franco Garcia, Maria Lourdes; Rodriguez Galan, Rafael Alfonso; Puiggali Bellalta, Jorge
    Journal of applied polymer science
    Date of publication: 2012-11-15
    Journal article

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  • Biodegradable free-standing nanomembranes of conducting polymer:polyester blends as bioactive platforms for tissue engineering

     Armelin Diggroc, Elaine; Gomes, Alex Linardi; Perez Madrigal, Maria Del Mar; Puiggali Bellalta, Jorge; Franco Garcia, Maria Lourdes; Del Valle Mendoza, Luis Javier; Rodriguez Galan, Rafael Alfonso; Campos, J.S.D.C.; Ferrer Anglada, Nuria; Aleman Llanso, Carlos Enrique
    Journal of materials chemistry B
    Date of publication: 2012-01-14
    Journal article

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    Aliphatic polyester and Poly(ester amide) Clay nanocomposites by In-situ Polymerization  Open access

     Morales Gámez, Laura Teresa; Rodriguez Galan, Rafael Alfonso; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    Date of publication: 2011
    Book chapter

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  • Nonisothermal crystallization behavior of a biodegradable segmented copolymer constituted by glycolide and trimethylene carbonate units

     Díaz Celorio, Elena; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    Journal of applied polymer science
    Date of publication: 2011-02-05
    Journal article

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    Biodegradable Poly(Ester Amide)s: Synthesis and Applications  Open access

     Rodriguez Galan, Rafael Alfonso; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    Date of publication: 2011
    Book chapter

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  • Handbook of Biodegradable Polymers

     Rodriguez Galan, Rafael Alfonso; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    Date of publication: 2011
    Book chapter

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  • New biodegradable poly(ester amide)s: study of polymerization, crystallization and degradation processes

     Botines Mas, Maria Emma
    Defense's date: 2011-09-30
    Department of Chemical Engineering, Universitat Politècnica de Catalunya
    Theses

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  • Single crystals morphology of biodegradable double crystalline PLLA-b-PCL diblock copolymers

     Casas Becerra, M. Teresa; Puiggali Bellalta, Jorge; Raquez, Jean-Marie; Dubois, Philippe; Cordova, Miguel E.; Mueller, Alejandro J.
    Polymer
    Date of publication: 2011-10-13
    Journal article

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  • Thermal stability studies on clay nanocomposites prepared from a degradable poly(ester amide) constituted by glycolic acid and 6-aminohexanoic acid

     Morales Gámez, Laura Teresa; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    Thermochimica acta
    Date of publication: 2011-01
    Journal article

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    An intercalated nanocomposite of the organically modified montmorillonite Cloisite C25A and a degradable poly(ester amide) based on glycolic acid and 6-aminohexanoic acid units (poly(glc-alt-amh)) was prepared using a twin-screw co-rotating extruder. The non-isothermal degradation kinetics was investigated by thermogravimetric analysis (TG and DTG) in the temperature range of 50–600 ◦C at five heating rates (2, 5, 10, 20 and 40 ◦C/min) and compared with the neat polymer. Significant differences were found since the nanocomposite showed three degradation steps instead of the two decomposition processes detected in the pristine sample. The onset mass loss temperature decreased in the nanocomposite due to the presence of the organo-modifier compound, but the presence of the silicate layers significantly decreased the degradation rate at the last stages of decomposition. Kinetic analysis was performed using the Kissinger method and the isoconversional (Kissinger–Akahira–Sunose and Friedman) methods. The true kinetic triplets (E, A, f(˛)) were determined for the first two steps of degradation through the Coats–Redfern and the Invariant Kinetic Parameters methods. The results clearly indicated that the presence of the organo-modified clay modified the mechanisms of degradation.

  • Electrospinning of polylactide and polycaprolactone mixtures for preparation of materials with tunable drug release properties

     Del Valle Mendoza, Luis Javier; Camps, Roger; Diaz Andrade, Angelica Maria; Franco Garcia, Maria Lourdes; Rodriguez Galan, Rafael Alfonso; Puiggali Bellalta, Jorge
    Journal of polymer research
    Date of publication: 2011-11
    Journal article

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    Nanocomposites of new biodegradable poliesters and polyesteramides  Open access

     Puiggali Bellalta, Jorge; Morales Gámez, Laura Teresa; Franco Garcia, Maria Lourdes; Casas Becerra, M. Teresa; Del Valle Mendoza, Luis Javier; Rodriguez Galan, Rafael Alfonso
    Plastics research online
    Date of publication: 2011-03-16
    Journal article

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    Polymers are easily prepared by bulk polycondensation based on metal-halide salt formation, while crystallization is strongly influenced by incorporation and distribution of silicate nanoparticles.

  • Poly(ester amide) nanocomposites by in situ polymerization: Kinetic studies on polycondensation and crystallization

     Morales Gámez, Laura Teresa; Jones, Ignacio; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    Express polymer letters
    Date of publication: 2011
    Journal article

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  • Crystallization studies on a clay nanocomposite prepared from a degradable poly(ester amide) constituted by glycolic acid and 6-aminahexanoic acid

     Morales Gámez, Laura Teresa; Franco Garcia, Maria Lourdes; Casas Becerra, M. Teresa; Puiggali Bellalta, Jorge
    Polymer engineering and science
    Date of publication: 2011-08
    Journal article

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  • Preparation and release study of ibuprofen-loaded porous matrices of a biodegradable poly(ester amide) derived from L -alanine units

     Del Valle Mendoza, Luis Javier; Roca, Diana; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge; Rodriguez Galan, Rafael Alfonso
    Journal of applied polymer science
    Date of publication: 2011-11
    Journal article

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    Scaffolds of a biodegradable poly(ester amide)constituted of L-alanine, sebacic acid, and 1,12-dodecanediol units (abbreviated as PADAS) were prepared by the compression-molding/particulate-leaching method. The influence of the type, size, and percentage of salt on the scaffold porosity and morphology was evaluated. The thermal behavior and crystallinity were also studied for samples obtained under different processing conditions. PADAS scaffolds were not cytotoxic because they showed good cell viability and supported cell growth at a similar ratio to that observed for the biocompatible materials used as a reference. The use of PADAS scaffolds as a drug-delivery system was also evaluated by the employment of ibuprofen, a drug with well known anti-inflammatory effects. Different drug-loading methods were considered, and their influence on the release in a so¨rensen’s medium was evaluated as well as the influence of the scaffold morphology. A sustained release of ibuprofen could be attained without the production of a negative effect on the cell viability. The release kinetics of samples loaded before melt processing was well described by the combined Higuchi/first-order model. This allowed the estimation of the diffusion coefficients, which ranged between 3x10‾14 and 5x10‾13 m2/ s. Samples loaded by immersion in ibuprofen solutions showed a rapid release that could be delayed by the addition of polycaprolactone to the immersion medium (i.e., the release rate decreased from 0.027 to 0.015 h‾1).

  • Isothermal crystallization study on a biodegradable segmented copolymer constituted by glycolide and trimethylene carbonate units

     Diaz Celorio, Elena; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    Journal of applied polymer science
    Date of publication: 2010-04-05
    Journal article

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    The isothermal crystallization behavior of a segmented copolymer constituted by hard blocks of polyglycolide and soft segments derived from the copolymerization of glycolide and trimethylene carbonate was investigated. This polymer has applied relevance because it is one of the most widely used for bioabsorbable surgical sutures. Calorimetric, optical microscopy, and infrared techniques were combined to understand the thermal properties and the different factors that influence the crystallization process. Basically, only the hard blocks crystallized, although certain processing conditions allowed performing an additional crystallization associated with small lamellar domains of the soft segment. Crystallization from both the melt and the glass state rendered positive spherulites with a fibrillar texture. The observed unusual sign of birefringence was a consequence of the close packing structure of polyglycolide, which was also corroborated by electron diffraction patterns. Crystallization was characterized by an athermal nucleation, which allowed accurate estimation of the secondary nucleation parameter by using the calorimetric data only. Significant differences in the Avrami exponent (from 2.32 to 1.45) were found between the cold and hot isothermal crystallizations. The stronger geometric constraints observed in the crystallization from the glass state were also corroborated by FTIR analyses

  • Conducting poly(3,4-ethylenedioxythiophene)-montmorillonite exfoliated nanocomposites

     Aradilla Zapata, David; Estrany Coda, Francisco; Azambuja, Denise S.; Casas Becerra, M. Teresa; Puiggali Bellalta, Jorge; Ferreira, Carlos Arthur; Aleman Llanso, Carlos Enrique
    European polymer journal
    Date of publication: 2010-03
    Journal article

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  • Brill transition and melt crystallization of nylon 56: An odd¿even polyamide with two hydrogen-bonding directions

     Morales Gámez, Laura Teresa; Soto, David X.; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    Polymer
    Date of publication: 2010-11-12
    Journal article

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    Brill transition and crystallization behaviour of nylon 56, a representative polymer of odd–even polyamides, were investigated by simultaneous WAXD and SAXS synchrotron radiation. Nylon 56 crystallized from solution into a peculiar structure where hydrogen bonds were established along the two directions. Nylon 56 experimented on heating a Brill transition that lead to a pseudohexagonal packing and lately to a monoclinic unit cell where neighbouring molecular segments were shifted along the chain axis direction. In disagreement with conventional polyamides, the Brill transition of nylon 56 was not reversible since on cooling the pseudohexagonal arrangement was mainly attained. Optical microscopy studies performed under both isothermal and non-isothermal conditions demonstrated that nylon 56 spherulites had different optical properties than even–even nylons having conventional sheet structures. The birefringence sign changed in the sequence positive–negative–positive when crystallization temperature was decreased.

  • Crystallization Behavior of Clay Nanocomposites Prepared from a Degradable Alternating Copolyester Constituted by Glycolic Acid and 6-Hydroxyhexanoic Acid

     Morales Gámez, Laura Teresa; Franco Garcia, Maria Lourdes; Casas Becerra, M. Teresa; Puiggali Bellalta, Jorge
    Journal of polymer science. Part B, polymer physics
    Date of publication: 2010-01
    Journal article

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    Degradable Poly(ester amide)s for biomedical aplications  Open access

     Rodriguez Galan, Rafael Alfonso; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    Polymers (Basel)
    Date of publication: 2010-12-27
    Journal article

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    Poly(ester amide)s are an emerging group of biodegradable polymers that may cover both commodity and speciality applications. These polymers have ester and amide groups on their chemical structure which are of a degradable character and provide good thermal and mechanical properties. In this sense, the strong hydrogen‑bonding interactions between amide groups may counter some typical weaknesses of aliphatic polyesters like for example poly(e-caprolactone). Poly(ester amide)s can be prepared from different monomers and following different synthetic methodologies which lead to polymers with random, blocky and ordered microstructures. Properties like hydrophilic/hydrophobic ratio and biodegradability can easily be tuned. During the last decade a great effort has been made to get functionalized poly(ester amide)s by incorporation of a-amino acids with hydroxyl, carboxyl and amine pendant groups and also by incorporation of carbon-carbon double bonds in both the polymer main chain and the side groups. Specific applications of these materials in the biomedical field are just being developed and are reviewed in this work (e.g., controlled drug delivery systems, hydrogels, tissue engineering and other uses like adhesives and smart materials) together with the main families of functionalized poly(ester amide)s that have been developed to date.

  • Study on the brill transition and melt crystallization of nylon 65: A polymer able to adopt a structure with two hydrogen-bonding directions

     Morales Gámez, Laura Teresa; Ricart López, Albert; Franco Garcia, Maria Lourdes; Puiggali Bellalta, Jorge
    European polymer journal
    Date of publication: 2010-11
    Journal article

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  • Influence of degradation on the crystallization behaviour of a biodegradable segmented copolymer constituted by glycolide and trimethylene carbonate units

     Franco Garcia, Maria Lourdes; Rodriguez Galan, Rafael Alfonso; Puiggali Bellalta, Jorge
    Polymer degradation and stability
    Date of publication: 2010-12
    Journal article

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    The influence of degradation on non-isothermal crystallization from the melt of a segmented copolymer constituted of glycolide and trimethylene carbonate units and used as a bioabsorbable surgical suture was studied by optical microscopy, differential scanning calorimetry and time-resolved X-ray diffraction. Fibrillar positive spherulites were obtained with slightly degraded samples but new axialitic morphologies were detected when samples had a molecular weight, Mw, lower than 29,000 g/mol and the crystallization started at a high temperature. Crystal growth kinetics of samples degraded under different conditions was evaluated over a wide temperature range by a non-isothermal method. Two crystallization regimes (I and II) were determined for the more degraded samples (i.e., those able to crystallize according to axialitic and spherulitic morphologies), whereas only regime II was found for samples of higher molecular weights. Primary nucleation density decreased with the extent of degradation provided no morphological changes occurred, and so did the regularity of lamellar stacking, as shown by synchrotron measurements, although the morphological parameters remained practically constant.

  • MATERIALES BASADOS EN UNIDADES DE TRIMETILENCARBONATO. NANOCOMPUESTOS DE POLIESTERES Y POLIESTERAMIDAS CON APLICACIONES COMMODITIES

     Casas Becerra, M. Teresa; Franco Garcia, Maria Lourdes; Rodriguez Galan, Rafael Alfonso; Del Valle Mendoza, Luis Javier; Urpi Garriga, Lourdes; Puiggali Bellalta, Jorge
    Participation in a competitive project

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  • Crystalline structure of sequential poly(ester amide)s derived from glycolic acid, 1,6-Hexanediamine, and even aliphtic dicarboxylic acids

     Casas Becerra, M. Teresa; Puiggali Bellalta, Jorge
    Journal of polymer science. Part B, polymer physics
    Date of publication: 2009-01
    Journal article

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