Dissertations / Theses: 'Poly (butylene succinate)'

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Lindström, Annika. "Poly (butylene succinate) and poly (butylene adipate) : quantitative determination of degradation products and application as PVC plasticizers." Licentiate thesis, KTH, Fibre and Polymer Technology, 2005. http://urn.kb.se/resolve?urn=urn:nbn:se:kth:diva-325.

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A solid phase extraction (SPE) method was developed for simultaneous extraction of dicarboxylic acids and diols formed during hydrolysis of poly(butylene succinate), PBS, and poly(butylene adipate), PBA. The developed SPE method and subsequent GC-MS analysis were used to extract, identify and quantify low molecular weight products migrating from linear and branched poly(butylene adipate) (PBA) and poly(butylene succinate) (PBS) during aging in aqueous media. The combination of SPE and GC-MS proved to be a sensitive tool, able to detect small differences in the degradation rate during early stages of hydrolysis before any significant differences were observed by weight loss and molecular weight measurements. The detected low molecular weight products included monomers i.e. adipic acid and 1,4-butanediol for the PBA polymers and succinic acid and 1,4-butanediol for PBS. Several dimers and trimers i.e. hydroxybutyl adipate, hydroxybutyl succinate, di(hydroxybutyl) adipate, di(hydroxybutyl) succinate and hydroxybutyl disuccinate were also detected. Best extraction efficiency for 1,4-butanediol and succinic acid was achieved with a hydroxylated polystyrene-divinylbenzene resin as solid phase. Linear range for the extracted analytes was 1-500 ng/ml for adipic acid and 2-500 ng/ml for 1,4-butanediol and succinic acid. Detection and quantification limits for all analytes were between 1-2 ng/ml (S/N=3) and 2-7 ng/ml (S/N=10) respectively. Relative standard deviations were between 3 % and 7 %. Comparison of measured weight loss and the amount of monomeric products showed that weight loss during early stages of hydrolysis was mainly caused by the release of water-soluble oligomers that on prolonged ageing were further hydrolyzed to monomeric species. Significant differences in degradation rate could be assigned to degree of branching, molecular weight, aging temperature and degradation medium.

Linear and branched PBA was mixed with PVC in solution cast films to study the effects of molecular weight and branching on plasticizer efficiency. Used as polymeric plasticizer, PBA formed a semi-miscible two-phase system with PVC where the amorphous part exhibited one single glass transition temperature and the degree of polyester crystallinity was dependent on molecular weight, degree of branching and blend composition. Plasticizing efficiency was favored by higher degree of branching and a 40 weight-percent polyester composition.

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Lindström, Annika. "Poly(butylene succinate) and poly(butylene adipate) - quantative determination of degradiation products and application as PVC plasticizers /." Stockholm, 2005. http://urn.kb.se/resolve?urn=urn:nbn:se:kth:diva-325.

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Jacquel, Nicolas. "Synthesis and properties of polyesters based on poly(butylene succinate), a renewable polymer." Thesis, Lyon, INSA, 2011. http://www.theses.fr/2011ISAL0127.

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Les polymères issus de la biomasse génèrent depuis quelques années un engouement certain puisqu’ils apparaissent comme de potentiels substituts aux polymères issus de l’industrie pétrolière. Parmi ces monomères récemment développés, l’acide succinique bio-sourcé a reçu une attention particulière notamment pour des applications dans le domaine des polyesters tels que le poly(butylène succinate). La présente thèse décrit la synthèse de ce polymère par estérification directe de l’acide succinique et du 1,4-butanediol dans un réacteur pilote de 7.5 L. Les principaux paramètres du procédé tels que l’excès de diol, la température de trans-estérification ainsi que la pureté de l’acide succinique ont été étudiés. Une attention particulière a été portée sur le choix du catalyseur (son type, la quantité utilisée …) afin d’observer son influence sur le procédé ainsi que sur la stabilité du polymère final. Puis différentes stratégies de modification du poly(butylene succinate) ont été testées pour améliorer à la fois sa mise en forme par extrusion gonflage et les propriétés des films obtenus. Dans ce but l’introduction d’agents de branchements, de silices nanométriques ainsi que des comonomères rigides a été étudiée
Polymers issued from biomass present a growing interest, since they seem to be a suitable alternative to conventional petrochemical polymers. Among the newly developed monomers, bio-based succinic acid received a particular attention for its application in the synthesis of aliphatic polyesters such as poly(butylene succinate). The present thesis reports the synthesis of this polymer via the direct esterification of succinic acid and 1,4-butanediol in a 7.5 L pilote scale reactor. Main process parameters such as the diol exces, the trans-esterification temperature as well as the purity of succinic acid have been studied. In addition a special attention was taken to highlight the influence of the catalyst (its type, quantity ...) on the synthesis and on the stability of the resulting polymer. Then several strategies of modification of poly(butylene succinate) have been studied to improve the processability of the polymer via film extrusion blowing and to enhance the properties of polymer films. To that end the introduction of branching agents, silica nanofillers as well as rigid comonomers have been studied

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Yhuel, Grégory. "Contribution à l’étude de polyesters aliphatiques renforcés par des fibres naturelles." Thesis, Reims, 2011. http://www.theses.fr/2011REIMS019/document.

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De par ses propriétés thermomécaniques proches des polyoléfines, le poly(butylene succinate)est l’un des polymères biosourcés les plus attractifs pour la substitution de matériaux pétro-sourcés pour des applications automobiles. L’incorporation de fibres de chanvre, via une étape d’extrusion,renforce la matrice et permet de tendre vers les propriétés cibles exigées par les cahiers des charges automobiles pour les applications visées dans cette étude. Afin d’améliorer les propriétés thermomécaniques de ce matériau, trois sujets ont été développés dans cette étude :1- Qualification de l’interface PBS / fibres de chanvre : via une nouvelle méthodologie basée sur l’analyse de la contribution effective des fibres sur la contrainte (CFC) durant une sollicitation mécanique, il est montré que les liaisons hydrogène formées entre le PBSet la fibre influent fortement sur les mécanismes de transfert de charge. Couplée au modèle de Bowyer et Bader, cette approche permet d’identifier les mécanismes d’endommagement de l’interface et de quantifier la contrainte interfaciale (τchanvre/PBS=25,2MPa).2 - Signification du ratio L/D d’une fibre naturelle : au cours des procédés de mises en oeuvre (extrusion et injection), la morphologie d’une fibre végétale évolue et apparait complexe due à la structure branchée engendrée par la fibrillation. A partir d’une nouvelleméthodologie d’analyse d’images spécifiquement développée, il est montré que la fibrillation contribue au renforcement de la matrice au même titre que le défibrage.3 -Synthèse de PBS-co-amides : afin de couvrir les contraintes thermomécaniques exigées,l’introduction de groupements amide dans le PBS est étudiée pour augmenter le point de fusion du polymère. Afin de contourner notamment la réaction parasite de cyclisation entre l’acide succinique et les amines, une stratégie de synthèses multi-étapes de monomères et de poly(ester-amide) est étudiée permettant d’obtenir un PEA de faible masse molaire dont le point de fusion atteint 172°C
With its thermomechanical properties closed to polyolefins, poly(butylene succinate) is one ofthe most interesting bio-based polymers for substitution of oil-based polymers for automotive applications. Addition of hemp fibers, through an extrusion process step, reinforces matrix and enables to fit with the targeted technical profile required by automotive specifications. In order to improve thermomechanical properties, three main topics have been investigated in this study:1 - PBS / hemp fibers interface qualification: through a new methodology based on the analysis of the effective fiber contribution on stress during mechanical solicitation, it was shown that hydrogen bonds between PBS and fibers play a major role in load transfer.Combined with the Bowyer and Bader model, this approach enables to highlight interface damages and to determine the interfacial shear strength (τhemp/PBS=25,2 MPa)2 - Meaning of natural fiber L/D ratio: during processes (extrusion and injection), vegetal fiber morphology changes and becomes complex due to the fibrillated structure. With anew developed image analysis tool, it was shown that fibrillation contributes to matrix einforcement as well as defibering.3 - Synthesis of PBS-co-amide: to reach the targeted thermomechanical performances,introduction of amide groups into PBS was studied to increase the melting point. In order to avoid the cyclic imide formation between succinic acid and amines, synthesis of monomers and poly(ester amide) were studied through a multistep strategy, enabling to get low molecular weight PEA with melting temperature around 172°C

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Llorens, Domenjó Elena. "Advanced electrospun scaffolds based on biodegradable polylactide and poly(butylene succinate) for controlled drug delivery and tissue engineering." Doctoral thesis, Universitat Politècnica de Catalunya, 2014. http://hdl.handle.net/10803/284662.

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Electrospinning is a manufacturing process that uses an electric field to produce fibers from a polymer solution. The accumulation of these fibers conform a three-dimensional fiber matrix or scaffold. Fibers can be prepared in a wide diameter range, namely from a micrometer to nanometer size. Furthermore, the fiber matrix or scaffold has a large surface per mass unit, a porous structure and mechanical properties influenced by the orientation of the fibers. The electrospinning technique is highly versatile and therefore a large number of polymers with different properties can be processed. However, a large number of variables can influence the characteristics of the resulting fibers, either because they are related to the polymer properties (e.g., solubility, molecular weight, etc.) or with the specific processing parameters (voltage, flow rate or distance tip-collector). Electrospun fiber matrices are attractive for biomedical applications as for example tissue engineering and drug delivery systems. In the last case, it is important the possibility to load the fibers with different drugs for their direct and localized administration into the human body. The goal of this Thesis is the study of different matrices constituted by electrospun micro- nanofibers and specifically four points have been considered. In the first one, polylactide electrospun scaffolds have been loaded with different molecules with antioxidant activity (i.e., vitamin B6 in pyridoxine and pyridoxal forms, p-coumaric acid and caffeic acid). The influence of these molecules on physical properties, morphology, in vitro release profiles and biocompatibility was determined. Furthermore, the application of these new materials for the inhibition of oxidative DNA damage caused by free radical initiators was demonstrated, and consequently, they appear appropriate candidates for purification of plasmidic or genomic DNA. In the second point, PLLA matrices loaded with two or three drugs were prepared in order to get a multifunctional activity. Thus, antioxidant, anti-inflammatory and antimicrobial molecules were considered in order to prevent chain oxidation processes in different biomolecules (proteins, DNA, etc.), avoid the subsequent local inflammation, and reduce the potential risk of microbial infection of wounds, respectively. These matrices are especially interesting due to the synergies and antagonisms that may occur during their simultaneous release. In the third point, the possibility of preparing biodegradable scaffolds from non electrospinable polymers has been considered. These polymers may have advantages like conductivity/electroactivity or bactericide activity. Hybrid scaffolds constituted by different ratios of polylactide as a biodegradable polymer and (poly(3-thiophene methyl acetate)) as electroactive polymer were evaluated. PLA nanofibers were also successfully loaded with polyhexamethylenebiguanide hydrochloride giving rise to 3D biodegradable scaffolds with a well proven antibacterial activity and a release that was highly dependent on the hydrophilicity of the medium. Finally electrospun scaffolds were obtained using a sacrificial polymer (e.g. poly(ethylene glycol) (PEG)) that could easily be subsequently removed by solubilization in aqueous media. Three approaches were evaluated: a) Preparation of scaffolds constituted by different ratios of PLA and PEG electrospun fibers, b) Preparation of scaffolds constituted by electrospun fibers with different PLA and PEG content; c) Preparation of scaffolds constituted by coaxial electrospun fibers with different core-shell polymer distributions. Cell colonization was in all cases favoured. The three procedures allowed preparing scaffolds with a differentiated drug release behavior.
La técnica de 'electrospinning' o electrohilado es un proceso de fabricación que utiliza un campo eléctrico para producir fibras a partir de disoluciones de polímeros. La acumulación de estas fibras conforma una matriz tri-dimensional o 'scaffold', y las fibras pueden ser preparadas en escala micro y nanométrica. Además, estas matrices o 'scaffold' se caracterizan por su gran superficie por unidad de masa, estructura porosa y propiedades mecánicas influenciadas por la orientación de las fibras. El 'electrospinning' es muy versátil y un gran número de polímeros con diferentes propiedades pueden ser procesados. Sin embargo, un gran número de variables pueden influir en las características de las fibras obtenidas, siendo variables propias del polímero (p.e., solubilidad, peso molecular, etc.) o relacionadas a los parámetros del proceso (voltaje, flujo, distancia colector-aguja). Estas matrices de fibras son atractivas para aplicaciones biomédicas como la ingeniería de tejidos y sistemas de liberación controlada de fármacos. En el último caso, es importante la carga de diferentes fármacos o drogas para su administración directa y localizada en el cuerpo humano. El objetivo de esta Tesis es el estudio de diferentes matrices constituidas por nano o microfibras electrohiladas. El desarrollo de este estudio se divide en cuatro bloques. En el primer bloque, matrices de fibras de poliláctico (PLA) fueron cargadas con diferentes moléculas con actividad antioxidante (vitamina B6 en sus formas de piridoxina y piridoxal, ácido p-cumárico y ácido cafeico). Se determinó la influencia de estas moléculas sobre las propiedades físicas, morfología, liberación in vitro y biocompatibilidad de dichas matrices. Además, se demostró la aplicación de estos nuevos materiales en la inhibición del daño oxidativo del ADN causado por iniciadores de radicales libres, y en consecuencia, estas matrices serían útiles para la purificación de ADN plasmídico o genómico. En el segundo bloque, las matrices de PLA fueron cargadas con dos o tres fármacos para obtener matrices multifuncionales en base a sus actividades. Con esta finalidad, moléculas con actividad antioxidante, anti-inflamatoria, y antimicrobiana fueron cargadas en las matrices para evitar los procesos de oxidación de diferentes biomoléculas (proteínas, ADN, etc.), evitar la inflamación local, y reducir el riesgo potencial de infección microbiana de las heridas, respectivamente. Estas matrices son especialmente interesantes debido a las sinergias y antagonismos que pueden ocurrir durante su liberación simultánea. En el tercer bloque, se prepararon matrices biodegradables a partir de polímeros no-electrohilables. Estos polímeros pueden presentar características particulares, como actividad bactericida, o actividad conductora/electroactividad. Matrices hibridas conformadas con diferentes ratios de PLA usado como polímero biodegradable y el poli(3-tiofeno metil acetato) como polímero electroactivo fueron preparadas y evaluadas. También se prepararon matrices de nanofibras de PLA cargadas con clorhidrato de polihexametilenbiguanida (PHMB) obteniéndose matrices biodegradables con actividad antibacteriana, y la liberación del PHMB fue altamente dependiente de la hidrófilicidad del medio. Finalmente, en el cuarto bloque, se prepararon matrices electrohiladas usando un polímero de sacrificio (polietilenglicol o PEG) que puede ser eliminado fácilmente por solubilización en medios acuosos. Tres preparaciones diferentes fueron evaluadas: a) Matrices constituidas por diferentes proporciones de PLA y PEG en las fibras, b) Matrices constituidas por fibras de PLA y fibras de PEG y, c) Matrices constituidas por fibras coaxiales con diferentes distribuciones de polímeros en el núcleo y la corteza de la fibra. La colonización celular en todas estas matrices fue mejorada. Estos tres procedimientos permitieron obtener matrices con diferentes comportamientos para la liberación de fármacos.

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Xu, Jingwen. "Biobased nanocomposites for packaging applications — synthesis using melt extrusion of poly (lactic acid), poly (butylene succinate) and/or starch blended with natural nanofillers." Thesis, Kansas State University, 2015. http://hdl.handle.net/2097/20561.

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Master of Science
Department of Grain Science and Industry
Sajid Alavi
There is a renewed focus on biodegradable polymers in packaging applications due to environmental concerns associated with conventional plastics. Melt extrusion was used to synthesize nanocomposites from poly (lactic acid) (PLA) or poly (butylene succinate) (PBS) blended with natural nanofillers — chitin whiskers (CHW, 1-5%), nanocrystalline cellulose (NCC, 1-5%) or lignin-coated nanocrystalline cellulose (LNCC, 3%). Transmission electron microscopy and x-ray diffraction indicated that the natural nanofillers were uniformly dispersed in the polymer matrix. For PLA based nanocomposites, differential scanning calorimetry showed a decrease in change of heat capacity at glass transition (ΔCp) with increased nanofiller addition, indicating greater confinement of polymer chains. For PBS based nanocomposites, nanofillers acted as nucleating agents and promoted recrystallization of polymer as reflected in increase of degree of crystallinity (Xc) from 65.9-66.8 to 75.6%. By addition of NCC and CHW, tensile strength (TS) of PLA based films increased from 50.2 MPa to 70.9 MPa and 52.1 MPa, respectively, while TS of PBS increased from 23.2-24.9 MPa to 32.9 MPa and 43.6 MPa, respectively. Elongation at break (E%) of nanocomposite films ranged from 9.1 to 15.3, and in general decreased with addition of nanofillers. LNCC did not significantly improve mechanical properties of PBS and PLA films. Additionally, 3% NCC addition reduced oxygen transmission rate (OTR) of PLA from 209.9 to 180.8 cc/m[superscript]2/day, which further reduced to 109.3 cc/m[superscript]2/day by adding compatibilizer methylene diphenyl diisocyanate (MDI, 4%). Water vapor transmission rate (WVTR) of PLA also reduced from 44.4 to 28.6 g/m[superscript]2/day with 3% NCC and 4% MDI addition. Similarly OTR and WVTR of PBS decreased from 737.7 to 280 cc/m[superscript]2/day and 83.8 to 49.4 g/m[superscript]2/day, respectively with 3% NCC. Use of 4% MDI further reduced OTR and WVTR to 23.8 cc/m[superscript]2/day and 30.8 g/m[superscript]2/day, respectively. Use of starch can potentially reduce the costs of bio-based nanocomposites films. Up to 40% starch was incorporated during synthesis of PLA and NCC nanocomposites using solution mixing method. Addition of starch decreased TS from 35.8 MPa to 18.4 MPa and E% from 8.3% to 6.0%. Use of NCC (1%) and MDI (4%) improved the mechanical properties to a certain extent.

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Vandesteen, Marie. "Synthèse et modification d'un polyester biodégradable pour application agro-textile : le poly(butylène succinate)." Thesis, Lyon, INSA, 2015. http://www.theses.fr/2015ISAL0022.

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Au cours des dernières décennies, l’utilisation de polymères biodégradables a connu un regain d’intérêt pour des applications agricoles. Dans cette étude, nous nous concentrons sur le développement de textiles biodégradables destinés à la protection anti-insecte des cultures. Actuellement, ces textiles doivent être collectés par des entreprises après la saison agricole et entraîne un coût non négligeable pour l’utilisateur. Une alternative serait d’avoir des agro-textiles qui pourraient être collectés par l’utilisateur et minéralisés après quelques mois. Les polymères biodégradables pourraient répondre à ces objectifs. Dans cette étude, nous nous sommes concentrés sur le poly(butylene succinate) un polymère biodégradable et biosourcé. Le PBS a été synthétisé sur un pilote de polycondensation. Néanmoins, le PBS issu de cette synthèse présente de faibles propriétés rhéologiques. La structure du PBS a donc été modifiée par l’incorporation de branchements ou d’allongeurs de chaines. Les propriétés mécaniques ont également été optimisées via la synthèse de systèmes PBS/PLA transréagits et de PBS nanocomposites. Ces PBS modifiés ont été testés au filage. Finalement un fil de PBS avec 0,5% de silice sphérique a été produit à plus grande échelle et un textile a été fabriqué. Le vieillissement de ces fils PBS a été étudié et la conservation des propriétés mécaniques durant l’utilisation du fil en extérieur a été validée. Enfin, une dernière approche plus exploratoire a été testée. Elle consiste en la modification du PBS par des interactions supramoléculaires réversibles en température
In the last decade, biodegradable polymers have gained significant interest for agricultural applications. Here we focus on the development of biodegradable textiles for insect-proof nets. Currently these textiles must be collected by specialized companies after the growing season and generate disposal cost. An ideal agrotextile would be collected by the user at the end of the growing season, and undergo full mineralization within few months. These requirements can be achieved by using biodegradable polymers. In this study, poly(butylene succinate) (PBS), a biobased and biodegradable polymer was studied. PBS was synthesized by polycondensation on a pilot plant reactor. Because of low rheological properties of the synthesized polyester, the chemical structure of PBS was modified by several approaches like chain extension or branching. The mechanical properties were tuned with the synthesis of PBS/PLA transreacted systems and PBS nanocomposites. These modified PBS were tested upon fiber spinning. Finally a PBS yarn with 0,5% spherical silica was produced at higher scale and a textile was done. Ageing of the PBS yarns was also studied and the conservation of the mechanical properties during use of the textile was validated. Lastly a more exploratory approach was tested. It is synthesis of modified PBS by supramolecular interactions, which are reversible upon temperature

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Freyermouth, Floriane. "Etude et modification des propriétés du poly(butylène succinate), un polyester biosourcé et biodégradable." Thesis, Lyon, INSA, 2014. http://www.theses.fr/2014ISAL0009/document.

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Dans le contexte de développement durable actuel, les matériaux biosourcés et biodégradables commencent à prendre une place importante d’un point de vue économique et écologique. L’objectif de remplacer les polyoléfines utilisées actuellement dans des domaines clés tels que l’emballage et l’automobile est cependant difficile car les matériaux « verts » sont rarement aussi performants. Ils présentent en général des lacunes au niveau de leurs propriétés mécaniques et sont sensibles à des dégradations qui limitent leur durée de vie. Le poly(butylène succinate) est un polyester connu depuis longtemps mais qui regagne de l’intérêt grâce à son potentiel biosourcé et biodégradable ainsi que ses propriétés mécaniques proches de celles des polyoléfines. Néanmoins, sa rigidité est encore trop faible et sa sensibilité importante à l’hydrolyse limite son utilisation dans le temps, même dans des conditions standards de température et d’humidité. Des améliorations de la stabilité du PBS sont possibles et plusieurs solutions ont été envisagées. L’intérêt s’est porté sur la modification de la balance hydrophile/hydrophobe du PBS par l’ajout d’un comonomère ramifié très hydrophobe, le Pripol 1009 ou possédant un cycle aromatique, l’acide téréphtalique. L’addition de charges dans le matériau peut également s’avérer efficace pour neutraliser les fins de chaines acides catalysant la dégradation, en utilisant du carbonate de calcium, ou pour limiter la perméabilité du matériau, par incorporation de talc. Dans l’optique de moduler les propriétés mécaniques du PBS, la voie de modification la plus fructueuse est le mélange par incorporation de charges minérales, comme le carbonate de calcium ou le talc, ou le mélange avec d’autres polyesters possédant une rigidité plus importante, tels que le poly(acide lactique) ou le poly(butylène téréphtalate). Les mélanges doivent présenter une bonne compatibilité et être mis en œuvre à des températures convenables pour limiter la dégradation du PBS et conserver la ductilité du matériau final, comme c’est le cas des mélanges PBS/PLA. Des combinaisons ont également été envisagées entre les différentes solutions efficaces pour améliorer à la fois les propriétés mécaniques et la stabilité face à l’hydrolyse chimique
Within the frame of sustainable development, biobased and biodegradable polymers are going to play an important role according to economic and environmental perspectives. The polyolefins currently used in packaging and automotive industries will be replaced by biomaterials. The poly(butylene succinate), an “old” aliphatic polyester, has recently regained interest thanks to its biobased and biodegradable potential and mechanical properties similar to polyolefins. However, this polyester is very sensitive to degradation even at mild ambient conditions and, even though its flexibility is comparable to polyethylene or polypropylene, its modulus is too low. Some modifications of the chemical structure were considered to improve the long-term use of PBS. The synthesis of random copolymers using long-chain fatty acid Pripol 1009 or terephthalic acid allows to reduce significantly the hydrolysis rate and properties are maintained during a longer time. The incorporation of fillers like calcium carbonate and talc also enhance the PBS stability. The addition of calcium carbonate neutralizes carboxyl terminal group, which play an autocatalytic role in the hydrolytic degradation. High aspect ratio of talc increases the gas and liquid diffusion path, reducing permeability and providing better barrier properties to the material. In order to improve Young’s modulus, formulating blends with mineral fillers like calcium carbonate and talc, or with more rigid polyesters like polylactic acid or poly(butylene terephthalate) are efficient. The most interesting results are obtained by using calcium carbonate and polylactic acid, which allow the preservation of PBS’s flexibility. Processing parameters should be maximized to limit the degradation of PBS. Combinations of the most interesting solutions were investigated and lead to materials which fulfill the required specifications

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Bhatia, Amita, and abhatia78@yahoo com. "Experimental Study of Structure and Barrier Properties of Biodegradable Nanocomposites." RMIT University. Civil, Environmental and Chemical Engineering, 2008. http://adt.lib.rmit.edu.au/adt/public/adt-VIT20090304.143545.

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As nanocomposites provide considerable improvements in material properties, scientists and engineers are focussing on biodegradable nanocomposites having superior material properties as well as degradability. This thesis has investigated the properties of biodegradable nanocomposites of the aliphatic thermoplastic polyester, poly (lactide acid) (PLA) and the synthetic biodegradable polyester, poly (butylene succinate) (PBS). To enhance the properties of this blend, nanometer-sized clay particles, have been added to produce tertiary nanocomposite. High aspect ratio and surface area of clay provide significant improvement in structural, mechanical, thermal and barrier properties in comparison to the base polymer. In this study, a series of PLA/PBS/layered silicate nanocomposites were produced by using a simple twin-screw extruder. PLA/PBS/Cloisite 30BX nanocomposites were prepared containing 1, 3, 5, 7 and 10 wt% of C30BX clay, while PLA and PBS polymers compositions were fixed at a ratio of 80 to 20. This study also included the validation of a gas barrier model for these biodegradable nanocomposites. WAXD indicated an exfoliated structure for nanocomposites having 1 and 3 wt% of clay, while predominantly development of intercalated structures was noticed for nanocomposites higher than 5 wt% of clay. However, TEM images confirmed a mixed morphology of intercalated and exfoliated structure for nanocomposite having 1 wt% of clay, while some clusters or agglomerated tactoids were detected for nanocomposites having more than 3 wt% of clay contents. The percolation threshold region for these nanocomposites lied between 3-5 wt% of clay loadings. Liquid-like behaviour of PLA/PBS blends gradually changed to solid-like behaviour with the increase in concentration of clay. Shear viscosity for the nanocomposites decreased as shear rate increased, exhibiting shear thinning non-Newtonian behaviour. Tensile strength and Young's modulus initially increased for nanocomposites of up to 3 wt% of clay but then decreased with the introduction of more clay. At high clay content (more than 3 wt%), clay particles tend to aggregate which causes microcracks at the interface of clay-polymer by lowering the polymer-clay interaction. Percentage elongation at break did not show any improvement with the addition of clay. PLA/PBS blends were considered as immiscible with each other as two separate glass transition and melting temperatures were observed in modulated differential scanning calorimetry (MDSC) thermograms. MDSC showed that crystallinity of the nanocomposites was not much affected by the addition of clay and hence some compatibilizer is required. Thermogravimetric analysis showed that the nanocomposite containing 3 wt% of clay demonstrated highest thermal stability compared to other nanocomposites. Decrease in thermal stability was noticed above 3 wt% clay; however the initial degradation temperature of nanocomposites with 5, 7 and 10 wt% of clay was higher than that of PLA/PBS blend alone. Gas barrier property measurements were undertaken to investigate the transmission of oxygen gas and water vapours. Oxygen barrier properties showed significant improvement with these nanocomposites, while that for water vapour modest improvement was observed. By comparing the relative permeabilities obtained from the experiments and the model, it was concluded that PLA/PBS/clay nanocomposites validated the Bharadwaj model for up to 3 wt% of clay concentration.

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Ramoné, Audrey. "Evolutions moléculaires au cours de la dégradation biotique et abiotique de polymères bio-sourcés (PLA et PBS) et fossiles à l’aide de la viscoélasticité à l’état fondu." Thesis, Clermont-Ferrand 2, 2015. http://www.theses.fr/2015CLF22643/document.

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Pour limiter la production de déchets, la voie de polymères biodégradables est largement explorée. La biodégradation en compost est un phénomène complexe qui dépend de la température, de l’humidité, du soleil et du polymère lui-même. Dans un premier temps, les effets de ces différents paramètres sur la biodégradation de l’acide polylactique (PLA) sont étudiés à l’aide de la viscoélasticité à l’état fondu. Il en résulte que l’échantillon lui-même n’a que peu d’influence sur sa dégradation, mais les conditions de dégradation influencent d’avantage les phénomènes mis en jeu. Dans un deuxième temps, le PLA est associé au poly(butylène succinate) (PBS), un polymère plus favorable à la biodégradation afin d’améliorer la dégradation du PLA. Après s’être intéressée à la biodégradation de polymères « compostables », cette étude se tourne vers la biodégradation d’un polymère non-biodégradable : le polypropylène (PP). Afin d’initier un processus de bio assimilation, des charges sont ajoutées au PP pour dégrader préalablement le polymère et ainsi favoriser l’action des micro-organismes sur les chaines plus courtes. Les hydroxydes doubles lamellaires induisent bien une dégradation mais ce n’est pas assez pour permettre l’assimilation du polymère. Finalement, ce travail aborde la biodégradation de différents polymères dans le but de comprendre ce phénomène et d’améliorer la biodégradation des polymères étudiés
Nowadays, to minimize our waste production, many studies are focused on environmentally friendly polymers. Degradation in compost is a complex phenomenon with unclear mechanism depending on temperature, micro-organism population, humidity and polymer it-self. In a first hand, these different parameter effects on poly(lactic acid)(PLA) biodegradation are studied with melt viscoelasticity to assess the molecular evolution of the materials during biodegradation. In a second hand, PLA is mixed with a polymer more biodegradable, poly(butylene succinate), to improve PLA biodegradation. After the biodegradation of a compostable polymer, a non biodegradable polymer is studied: polypropylene(PP). To achieve the initiation of its bio-assimilation, fillers are added to promote its degradation and therefore improve its assimilation by micro-organisms. Layered double hydroxides induce degradation but not enough to observe polymer biodegradation

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Garin, Matthieu. "Synthèse et étude des propriétés physico-chimiques des poly(butylène succinate)s linéaire et branché." Thesis, Reims, 2012. http://www.theses.fr/2012REIMS014/document.

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Le poly(butylène succinate) (PBS) est un polyester aliphatique biodégradable dont les propriétés en font un bon candidat pour le remplacement des polyoléfines. De plus, ses deux monomères, l'acide succinique et le butane-1,4-diol, peuvent être issus de la biomasse via un procédé de fermentation de sucres. L'étude réalisée ici a été séparée en deux grandes parties : le PBS linéaire d'une part et le PBS branché d'autre part. La première partie montre que la cinétique de synthèse du PBS suit bien le modèle d'estérification établi par Flory. Par la suite, l'étude des propriétés physico-chimiques du PBS a permis de remonter à des paramètres comme la masse molaire critique d'enchevêtrement, le module du plateau caoutchoutique, l'énergie d'activation du PBS fondu ou encore les paramètres de l'équation Mark-Houwink-Sakurada. Une étude sur ses propriétés thermiques a permis de décrire l'évolution de son comportement en fonction de sa masse molaire. Enfin, le profil d'énergie potentielle de l'estérification entre l'acide succinique et le butane-1,4-diol a été tracé en utilisant un outil de chimie quantique. La seconde partie traite de l'étude de PBS branchés obtenus en employant des agents de branchement (polyols) pouvant être issus de la biomasse comme l'huile de ricin, le glycérol et le polyglycérol. La stratégie adoptée a été le couplage entre un oligomère PBS fonctionnalisé acide carboxylique et les agents de branchement. L'étude en présence d'huile de ricin a mis en avant les relations entre la structure, déterminée en SEC-Triple Détection, et les propriétés physico-chimiques du PBS branché. L'optimisation de la synthèse en présence de glycérol ou de polyglycérol a été abordée à partir de la méthode des plans d'expériences. Comparé à la méthode « un facteur à la fois », des résultats prometteurs et semblables à ce qui est rapporté dans la littérature ont été obtenus pour l'étude du PBS branché en présence de glycérol
Poly(butylene succinate) (PBS) is a biodegradable aliphatic polyester whose properties make it a promising polymer for the replacement of polyolefins. Moreover, its two monomers, succinic acid and 1,4-butanediol, can be produced via a fermentation process of sugars. This study has been separated into two great parts: linear PBS on the one hand and branched PBS on the other hand. In the first part, kinetics of the PBS synthesis showed a good agreement with the esterification model of Flory. We determined some fundamental parameters of PBS like critical molecular weight of entanglement, the rubbery plateau modulus, the energy of activation of melt PBS and parameters of the Mark-Houwink-Sakurada relationship. We have also realized a study on the influence of the molecular weight on the thermal properties of PBS. Finally, we constructed the potential energy profile of the esterification between succinic acid and 1,4-butanediol through a quantum chemistry study. The second part dealt with the study of branched PBS in the presence of biosourced polyols like castor oil, glycerol and polyglycerol. These syntheses were realized between an acid-functionalized PBS oligomer and the branching agents. We put forward the relationships between the structure, determined by SEC-Triple Detection, and the physicochemical properties of branched PBS in presence of castor oil. Syntheses of branched PBS in presence of glycerol or polyglycerol were optimized with design of experiments technique. Promising and similar results from the literature were obtained in the case of branched PBS in presence of glycerol compared to the method of “one parameter at a time”

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12

Ykhlef, Nazim. "Etude et optimisation de poly(butylène succinate) biosourcés pour l’injection moussage à l’azote par voie physique." Thesis, Ecole nationale supérieure Mines-Télécom Lille Douai, 2018. http://www.theses.fr/2018MTLD0004.

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Ce travail concerne le développement de polymères alvéolaires biosourcés adaptés à l’injection microcellulaire physique (Mucell®) ainsi que l’identification des leviers (procédé et/ou matériau) permettant de contrôler la structure cellulaire.Les paramètres directeurs du procédé ont été optimisés à l’aide d’un plan d’expérience de type Taguchi permettant d’atteindre un allégement de 15% tout en conservant un niveau de performance mécanique acceptable. Par ailleurs, des modifications structurales du PBS ont été menées dans le but de contrôler le processus de formation de la structure cellulaire (dissolution du gaz, nucléation, croissance cellulaire et stabilisation de la structure). La morphologie cellulaire a été améliorée en modifiant la conformation moléculaire des chaînes, en favorisant la nucléation hétérogène ou en modifiant les propriétés élongationnelles et la tension de surface du matériau. La formulation résultante a permis une diminution de plus de 80% de la taille des cellules et une densité cellulaire multipliée par 450.Enfin, une technique de mesure du comportement rhéologique du système monophasé polymère/gaz a été développée à l’aide d’une buse instrumentée en ligne permettant d’évaluer l’effet de la dissolution du gaz sur la viscosité du matériau en fonction des conditions expérimentales de l’étude
This work focused on the development of biobased polymer foams adapted to the microcellular injection molding (Mucell®) and the identification of the key parameters (process and/or material) controlling the cell structure.The process parameters were optimized using a Taguchi design of experiment which achieves 15% lightweighting while maintaining acceptable mechanical performances. In addition, structural modifications of PBS were carried out in order to control the foaming mechanism (gas dissolution, cell nucleation, cell growth and cell stabilization). Cell morphology has been improved by modifying the molecular conformation, promoting heterogeneous nucleation, or by adjusting the extensional viscosity and surface tension of the material. The resulting formulation exhibit a decrease of more than 80% in cell size and a cell density multiplied by 450.Finally, a measurement technique for the rheological behavior of the single phase polymer/gas mixture was developed using an instrumented on-line nozzle to evaluate the effect of gas dissolution on the viscosity under experimental conditions

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Mamzed, Saskia. "Valorisation de l'acide itaconique, un synthon dérivé de la biomasse, vers des monomères et polymères à motif pyrrolidone fonctionnalisée." Reims, 2010. http://theses.univ-reims.fr/sciences/2010REIMS021.pdf.

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L’acide itaconique (AI), produit par fermentation des hexoses, est un synthon renouvelable intéressant, présentant la double fonctionnalité acrylique et diacide. Notamment, il réagit avec les amines primaires pour donner des pyrrolidones fonctionnalisées en position 4 par un groupement carboxyle ou, partant du diester méthylique, par un groupement méthoxycarbonyle. L’objectif de cette thèse a consisté à synthétiser des monomères à motifs pyrrolidones pour les engager dans des polymérisations radicalaires ou des polycondensations. La 4-méthoxycarbonyl-1-vinylpyrrolidone (MCVP) a été synthétisée. Sa polymérisation et sa copolymérisation avec divers co-monomères, par voie radicalaire amorcée thermiquement ou photochimiquement, ont été étudiées. Les polymères obtenus sont solubles dans des solvants polaires, et leurs propriétés peuvent être modulées par aminolyse de la fonction carboxylique. Notamment des polymères amphiphiles ont été obtenus et peurs propriétés physico-chimiques mesurées. La condensation de l’AI avec des diamines a permis d’accéder à des diacide de type bis(pyrrolidones) avec des espaceurs variables, qui ont été engagées dans des polycondensations avec des diols ou des diamines. Divers polycondensats ont ainsi été étudiés et considérés comme compatibilisants susceptibles d’améliorer les propriétés d’alliages amidon plastifié (TPS)/ poly(butylène succincte) (PBS)
Itaconic acid, produced by fermentation from hexoses, is an interesting renewable building block presenting the double functionality of an acrylic-and a dicarbonic organic acid. Thus, itaconic acid reacts with primary amines in a Michael addition-cyclocondensation sequence to give pyrrolidones functionalized in the 4-position. The aim of this work is to synthesize monomers with pyrrolidone motifs, which will undergo radical polymerization reactions and polycondensation. The 4-methoxycarbonyle-1-vinylpyrroldione (MCVP) has been synthesized. Its radical polymerization and copolymerization with different comonomers, by thermal or photochemical initiation in solution has been studied. The obtained polymers are soluble in polar solvents and their properties could be modulated by aminolysis of the carboxylic function. By condensation of itaconic acid with diamines we obtained bis(pyrroldione)-type diacids with alkylidene spacers of variable size. Those have been used in polycondensation reactions with various diamines and diols. Diverse polycondensates have been studied as potential compatibilizer of plasticized starch (TPS) and poly-butylene succinate (PBS)

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Chiou, Hung-Wei, and 邱泓維. "Nonisothermal Crystallization Behaviors of Poly(butylene succinate-co-1,4-cyclohexanedimethylene succinate)s." Thesis, 2013. http://ndltd.ncl.edu.tw/handle/50112857432015918436.

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碩士
國立中山大學
材料與光電科學學系研究所
101
Poly(butylene succinate-co-1,4-cyclohexanedimethylene succinate) [PBCSu] were synthesized via a two-stage condensation reaction. PBCSu9505 and PBCSu9010 were characterized as having 5.6 and 12 mol% 1,4-cyclohexanedimethylene succinate (CS) units, respectively, by 1H NMR. Copolymers were characterized as random, based on 13C NMR spectra. A differential scanning calorimeter (DSC) and a polarized light microscope (PLM) were adapted to study the nonisothermal crystallization and melting behaviors of these copolymers. DSC data were analyzed via modified Avrami, Ozawa, and Mo models, respectively. Morphologies and growth of spherulites were monitored under PLM experiments at constant cooling rates. Isothermal growth rates obtained via nonisothermal method were analyzed using secondary nucleation theory. The regime transition temperature from II to III was found at 85.2 and 79.6 °C for PBCSu9505 and PBCSu9010, respectively. The results of PLM and DSC demonstrate that incorporation of minor CS units into PBSu inhibits the crystallization rate and crystallinity of the resulting copolyester. Small angle X-ray scattering (SAXS) and wide angle X-ray diffraction (WAXD) were used to analyze the lamellar and crystal structures of nonisothermally crystallized copolymers, respectively. Long period (L) and crystal thickness (lc) were found to decrease with increasing the cooling rate. However, the peak positions of WAXD patterns do not change with various cooling rates or the amount of CS units. It revealed that there was only one crystal form in this study and CS units were excluded from the crystal lamellae. Temperature-resolved FTIR was used to monitor the spectral variations during the nonisothermal crystallization process of PBSu and PBCSu copolymers. Different wavenumber regions (C-H and C=O stretching) were compared by second derivatives and two dimensional (2D) correlation analysis. The characteristic bands of crystalline and amorphous were identified in each region. In addition, C=O stretching region was also monitored to study the melting process. It was observed that the melting- recrystallization-remelting process occurred at boundary phase between the crystalline and amorphous regions. By 2D synchronous correlation analysis, it was found that the intensity change at 1723 cm-1, which is assigned to boundary phase, decreases with increasing the amount of CS units. It revealed that the crystallinity of boundary phase was restricted by the CS units excluded from the crystal lamellae. Thus, the thermal stability of boundary phase decreased with increasing the amount of CS units

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Peng, Jyun-siang, and 彭竣翔. "Copolymers and Blends of Poly(butylene succinate) and Poly(trimethylene succinate): Characterization, Crystallization, Melting, and Morphology." Thesis, 2007. http://ndltd.ncl.edu.tw/handle/j7vtd8.

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碩士
國立中山大學
材料科學研究所
95
A small amount of poly(trimethylene succinate) (PTSu) were copolymerized or blended with poly(butylenes succinate) (PBSu) in this study. The range of intrinsic viscosity for PBSu and PBSu-enriched copolymers are between 1.62 and 0.97 dL/g; number-average molecular weights are in the range of 2.5x104 and 11.9x104 g/mol with polydispersity indices ranging from 1.52 to 3.94. Copolymer composition is calculated from 1H and 13C NMR spectra, and the distribution of BS and TS units in these copolymers are supported to be random from the evidence of a single glass transition temperature (Tg) and a randomness value close to 1.0. Tg of PBSu is -40.8 °C. The Tg values of copolymers and blends increased with TS contents. The melting temperature (Tm) and the exothermic heat of crystallization of blends were not strongly affected by blending with PTSu. The values of Avrami exponent (n) for PBSu, copolymers and blends ranging from 2.3 to 3.1 indicate that heterogeneous nucleation with three-dimensional growth and homogeneous nucleation with two-dimensional growth might happen during the crystallization process. Multiple melting behavior was observed for PBSu, PBSu- enriched copolyesters and blends. Their peak temperatures are denoted as Tm1, Tm2 and Tm3 in order of increasing temperature. Tm1 corresponds to the melting temperature of the so-called annealing peak which might be resulted from the competition between continuous melting and re-crystallization. In contrast the peak at Tm2 is attributed to the melting of the primary crystals formed during isothermal crystallization. The peak at Tm3 may arise from the melting of re-crystallized primary crystals. Equilibrium melting temperatures were determined by the Hoffman-Weeks linear extrapolations which yield of 127.4 °C for PBS, 125.7 °C for PBTSA95/05, 120.6 °C for PBTSu90/10, 128.6 °C for PBSu/PTSu 98/02, 127.0 °C for PBSu/PTSu 95/05 and 125.5 °C for PBSu/PTSu 90/10. The thickness coefficient ( ) is located between 0.77 and 0.80. Three characteristics temperatures of thermal degradation, defined as temperature of thermal degradation at begining (Tstart), weight losses of 2% (Tloss2%) and maximum degradation rate (Tmax), were employed to characterize the thermal stability of polyesters and blends. The Tloss2% and Tstart values of PBTSu90/10 are higher than the values of the others because of its unusually high molecular weight. Wide-angle x-ray diffraction patterns were obtained after complete isothermal crystallization. Diffraction peaks are in the same positions, and these peaks become sharper and increase in intensity as the crystallization temperature increases. This indicates that during the heating process, only one crystal form appears and both of the crystallite size and perfect degree increase. The isothermal growth rate of PBSu spherulite increases from 0.01 μm/sec at 103 °C to 3.33 μm/sec at 75 °C. When the TS units increase, the spherulitic growth rates of PBTSu95/05 and PBTSu90/10 copolyesters decline dramatically. One of the reasons is that the incorporation of TS units into PBSu significantly inhibits the crystallization behavior of PBSu. Growth rates data were treated with Lauritzen-Hoffman secondary nucleation theory to find the regime transition. Using the Williams-Landel-Ferry (WLF) values, regime II to III transition is found at 95.1 °C for PBSu, 84.4 °C PBTSu95/05, and 77.1 °C for PBTSu 90/10. All melt-crystallized specimens formed two dimensional axial-like spherulites with negative birefringence. Extinction bands were observed when PBSu, PBSu- enriched copolymers and blends specimens were crystallized at large undercooling.

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Lu, Hsin-ying, and 呂信穎. "Characterization, Crystallization, Melting and Morphology of Poly(ethylene succinate), Poly(butylene succinate), their Blends and Copolyesters." Thesis, 2007. http://ndltd.ncl.edu.tw/handle/2pvtd6.

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碩士
國立中山大學
材料科學研究所
95
Minor amounts of monomers or homopolymer of poly(butylene succinate) (PBS) were copolymerized or blended with monomers or homopolymer of poly(ethylene succinate) (PES). PEBSA 95/05 represents a copolymer synthesized from a feed ratio of 95 mol% ethylene glycol and 5 mol% 1,4-butanediol with 100 mol% succinic acid. Copolymers PEBSA 90/10 and 50/50 were also synthesized. Blends of PES and PBS were prepared in solution with ratios of PES/PBS: 98/02, 95/05 and 90/10. Molecular weights of homopolymers and copolymers were measured using capillary viscometer and gel permeation chromatography. The results indicate that polyesters used in this study have high molecular weights. The chemical composition and the sequence distribution of co-monomers in copolyesters were determined using 1H NMR and 13C NMR. The distribution of ES and BS units in these copolyesters was found to be random from the evidence of a single Tg and a randomness value close to 1.0 for a random copolymer. Thermal properties of polyesters and blends were characterized using differential scanning calorimeter (DSC), temperature-modulated DSC (TMDSC) and thermogravimeter. For copolymers, melting point of PES significantly decreases from 100.9 to 94.5 to 89.8 oC with an increasing in BS units from 0 to 5 to 10 mol%. Blends keep the intrinsic melting points of PES and PBS homopolymers. There is no significant difference or no trend about the thermal stability of these polyesters and blends. Wide-angle X-ray diffractograms (WAXD) were obtained for specimens after complete isothermal crystallization. Diffraction peaks indicate that the crystal structure of PES is dominated in PES-enriched copolymers. However, PEBSA 50/50 displays weak diffraction peaks of the characteristic peaks of PBS homopolymer. Isothermal crystallization of copolyesters and blends were performed using DSC. Their crystallization kinetics and melting behavior after complete crystallization were analyzed. The n1 values of the Avrami exponent for copolyesters increased from 2.54 to 2.84 as the isothermal temperature (Tc) increased. The Hoffman-Weeks linear plots yielded an equilibrium melting temperature of 111.1 and 107.0 oC, respectively, for PEBSA 95/05 and 90/10. Homopolymer PES has an equilibrium melting temperature of 112.7 oC. For blends, the n1 value has a minimum at Tc of 40 oC then it increases with an increase in Tc or in PBS. At the same Tc, n1 increases slightly and the rate constant (k1) decreases when the ratio of PBS in blends increases. All of these blends gave an equilibrium melting temperature of 113.1 oC. Multiple melting behavior involves melting-recrystallization-remelting and various lamellar crystals. As Tc or BS unit in copolymer increases, the contribution of recrystallization slowly declines. Acetophenone was used a diluent for PES homopolymer. Five concentrations were used to estimate the melting point depression, and the heat of fusion of PES was obtained to have a value of 163.3 J/g according to Flory equation. Spherulitic growth rates of copolymers were measured at Tc between 30 and 80 oC using polarized light microscope (PLM). Maximum growth rates occurred at Tc around 50 oC. It is found that the growth rate of copolymer decreases significantly after randomly incorporating BS units into PES. Non-isothermal method at a cooling rate of 2, 4 or 6 oC/min was used to calculate the isothermal growth rates of copolymers. These continuous data fit very well with the data points measured isothermally. Growth rates data are separately analyzed using the Hoffman-Lauritzen equation. A regime II-III transition is found at 59.4 and 52.4 oC, respectively, for copolyesters PEBSA 95/05 and PEBSA 90/10. The results of DSC and PLM indicate that blend PES/PBS 98/02 not only retains the melting point and the crystallinity of PES homopolymer, but also increases the nucleation rate of this blend. The effect of blending 2 mol% PBS with PES on the biodegradability of PES is deserved to be investigated furthermore.

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Huang, Kai-lun, and 黃凱倫. "Crystallization Kinetics and Foaming of Crosslinked Poly(butylene succinate)." Thesis, 2005. http://ndltd.ncl.edu.tw/handle/93305451243415458116.

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碩士
義守大學
生物技術與化學工程研究所碩士班
93
In this work, we attempted to study crystallization kinetics of cross- linked poly(butylene succinate) (PBSU). PBSU can be effectively cross- linkked by adding a peroxide, t-butyl perbenzoate (BPB), into the polymer matrix. It was found that crystallization rate decreased with increasing BPB concentration. In isothermal crystallization, the n values in Avrami equation were close to 3 and the k values decreased with increasing BPB concentration. PBSU exhibited two endotherms in DSC thermograms upon melting. The high melting endotherm corresponded to melting of the crystallites re-crystallized from melting of those crystallites in the lower endotherm. In addition, both chemical and physical foaming of crosslinked PBSU were also studied. The foam pieces from chemical foaming had higher density and the cells were mostly closed. Foam pieces of very low density and very fine cellular structure could be obtained by high pressure CO2 foaming (physical foaming). The cells were mostly open, with a open-cell ratio higher than 90%. Unlike chemical foaming, the processing window became narrower as the crosslinking level had been increased in a CO2 foaming process.

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Chen, Chi-He, and 陳紀何. "Synthesis and characterization of biodegradable poly(butylene succinate) copolyesters." Thesis, 2010. http://ndltd.ncl.edu.tw/handle/03660685227360017385.

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博士
國立中山大學
材料與光電科學學系研究所
98
Three series copolyesters [poly(butylene succinate-co-propylene succinate) (PBPSu), poly(butylene succinate-co-2-methyl-1,3-propylene succinate) (PBMPSu) and poly(ethylene succinate-co-butylene succinate) (PEBSu)] and their homopolyesters [poly(butylene succinate) (PBSu), poly(ethylene succinate) (PESu), poly(propylene succinate) (PPSu) and poly(2-methyl-1,3-propylene succinate) (PMPSu)] were synthesized by a two-step reaction (esterification and polycondensation) with titanium tetraisopropoxide as the catalyst. Molecular weights of all synthesized polyesters were determined by intrinsic viscosity and gel permeation chromatography (GPC) measurements. The values of intrinsic viscosity (0.97 ~ 1.62 dL/g) and relative molecular weight (2.4x10000 ~ 11.9x10000 g/mol) indicate that these polyesters can be made into films without complications. Compositions and sequence distributions of copolyesters were determined by analyzing the spectra of 1H NMR and 13C NMR. The randomness values of these copolyesters are closed to 1.0 that represents random sequence distribution of the comonomers. Thermal properties and stabilities were characterized using differential scanning calorimeter (DSC) and thermogravimetric analyzer (TGA), respectively. All copolyesters exhibited a single glass transition temperature (Tg). For PBPSu copolyesters, incorporating propylene succinate units to PBSu not only narrows the window between Tg and melting temperature (Tm), but also retards the cold crystallization ability, thereby lowering the crystallinity to a considerable extent. This phenomenon also occurred in PBMPSu and PEBSu copolyesters when the 2-methyl-1,3-propylene succinate (MPS) and butylene succinate (BS) units were incorporated into PBSu and PESu, respectively. Tstart is the temperature of first detectable deviation from the derivative curve of weight loss. Tstarts of all synthesized polyesters around 240 οC, higher than the temperature of polycondensation reaction (220 οC), demonstrates that there is no necessity of using a thermal stabilizer during the synthesis of these polyesters. Additionally, the thermal stability does not vary significantly with compositions in the same series polyester. Wide-angle X-ray diffractograms (WAXDs) at room temperature were obtained from polyesters crystallized isothermally at a temperature around 5-20 οC below their melting temperatures. WAXD patterns of two series polyesters elucidated that the incorporation of PS or MPS units into PBSu markedly inhibits the crystallization behavior of PBSu. The phenomenon also occurred in PEBSu copolyesters when BS units were incorporated into PESu. Results of WAXD and DSC measurements showed that PMPSu is a amorphous polyester. The retarding effect on crystallization by methyl substituents on the polymer chain is efficient.

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Yeh, Ling-ling, and 葉玲伶. "Crystal Structure and Spherulite Growth of Crosslinked Poly(butylene succinate)." Thesis, 2005. http://ndltd.ncl.edu.tw/handle/17139013352196659027.

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碩士
義守大學
生物技術與化學工程研究所碩士班
93
Poly(butylene succinate) (PBSU) specimens with different crosslinking levels was prepared by adding different amounts of t-butyl perbenzoate (BPB). The morphology evolution was then studied using tools such Fourier transform infred (FTIR) spectroscopy, optical microscopy, calorimetry and X-ray diffraction. Several IR absorption peaks which changed as crystallization proceeded had been identified. In optical microscope observations, it was found that the growth rate of PBSU spherulites decreased with increasing BPB concentration. Several types of spherulite structure had been identified: at low temperatures, spherulites with a typical Maltese cross were observed; at higher temperatures, their appearance became feather-like; finally, spherultes with irregular texture were observed for highly crosslinked PBSU. Heat of fusion for PBSU, and hence crystallinity, decreased with increasing BPB concentration. Although crystallinity and morphology changed as PBSU was crosslinked, from the X-ray analysis, it was found that crystal structure remained unchanged.

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Moussa, Hassan. "Life Cycle Assessment of a Hybrid Poly Butylene Succinate Composite." Thesis, 2014. http://hdl.handle.net/10012/8204.

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Poly butylene succinate (PBS) is a biodegradable plastic polymer that has physical and mechanical properties similar to common petroleum plastics like polypropylene (PP) and polyethylene (PE). PBS may be produced from petroleum or bio-based feedstocks, or by a hybrid combination of petroleum and bio-based resources. Producers are reducing content of petroleum components used for the production of PBS, and by doing so are seeking potential environmental performance improvements. In this study, ???hybrid??? PBS refers to the production of PBS polymer from bio-based succinic acid (SAC) sourced from sorghum and petroleum-based 1, 4-butanediol (BDO). Given its biodegradability, PBS is commercially used for compostable bags and agricultural mulching film applications. A recent study in Ontario identified composite materials made with PBS blended with natural fibres like switchgrass (SG) as promising for applications in automotive products. Such novel composite materials are touted as potential bio-based alternatives to conventional petroleum-based plastics. Of the few studies that have considered the environmental performance of PBS materials, none have assessed the potential environmental impacts of a hybrid PBS composite. Therefore, this study undertook a life cycle assessment (LCA) of SG reinforced hybrid PBS composite (hybrid composite). LCA is an environmental management technique that is used to assess environmental aspects (inputs and outputs) and potential environmental impacts of a product or service throughout its life cycle. The analysis considered a cradle-to-gate system boundary and evaluated eleven environmental performance indicators. The environmental performance of the hybrid composite was compared to a conventional glass fibre (GF) reinforced polypropylene (PP) composite (baseline composite), a material that is widely used in automotive components. Results showed that the production of the hybrid composite in comparison to the baseline composite decreased potential impact for most of the assessed indicators: cumulative energy demand by 40%, waste heat by 23%, global warming potential by 35%, smog by 2%, carcinogens by 54%, non-carcinogens by 172%, respiratory effects by 22% and ecotoxicity by 45%. Increases in the values of impact indicators were apparent for ozone depletion, acidification, and eutrophication by 43%, 16%, and 322%, respectively. Analysis revealed that dominant influences on results were not related directly to the bio-based make-up. Rather, the biggest influence on the environmental performance of composite production were the sources of heat used in petroleum-based materials, the energy mix in electricity for bio-based materials, the type of reinforcing fibre and the co-product treatment methodology used. The study helps fill a gap in knowledge regarding bio-based chemicals and hybrid biodegradable plastic composites, and points to opportunities for future research on feedstocks for industrial composite materials. The importance of this study is that it helps to identify the environmental strengths and weaknesses associated with the production of the hybrid composite specifically, and bio-based materials more generally. It points to alternative material substitution options for use in the automotive industry. In this study, life cycle assessment exemplifies multidisciplinary methodologies, which seek to traverse the boundaries between the social and natural sciences and disciplines to support more sustainable policy decisions for a bio-economy. The systematic nature and the widely applicable consequences of this LCA study have the potential to contribute to industrial and business management, and reach the public policy arena in an effort to drive environmental and social change.

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21

Wang, Tzu-Ya, and 王姿雅. "A Study of Crosslinked Poly(butylene succinate)/Layered Silicate Nanocomposites." Thesis, 2006. http://ndltd.ncl.edu.tw/handle/86360919309924974748.

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碩士
國立中興大學
化學工程學系所
94
Abstracts In this research, two types of nanocomposites were prepared and characterized.For the first type, poly(butylene succinate) (PBS)-clay nanocomposites (PBSMC) were prepared by dispersing organically modified montmorillonite (MMT) into polymer solution. On the other hand, PBSMC were simultaneously crosslinked using dicumyl peroxide (DCP).As a result,the crosslinked PBS-clay (PBSDMC) nanocomposites were obtained. Montmorillonite modified with hexadecylpyridium chloride were used for these two nanocomposites at various concentration (1wt%, 3wt%, 5wt% and 10wt%). Wide angle X-ray diffraction (WAXD) studies revealed these two types of nanocomposites with different basal spacing comparing to neat MMT. Transmission electron microscopy (TEM) showed ordered intercalation and partial exfoliation structures in these nanocomposites with 5wt% loading level. According to WAXD and TEM analysis, we proved that PBSMC and PBSDMC successfully obtained via solution intercalation method. The dynamic mechanical analysis (DMA) showed that glass transition temperature (Tg), storage modulus(E’) and loss modulus(E”) can be enhanced by the addition of the modified MMT. In particular, the PBSDMC sample with 10wt% loading level of MMT demonstrated 10.5℃ enhancement in Tg. This was attributed to the crosslinked structure and PBS-MMT entanglement. To further study how did MMT dispersion in PBS influence the crystallization, nonisothermal crystallization kinetics were investigated by using differential scanning calorimeter (DSC) to study crystallization characteristics of PBSMC and PBSDMC. For a given cooling rate, crystallization temperature (Tc) and crystallinity decreased with increasing MMT concentration in PBS. In addition, Oxygen permeability rate of nanocomposites decreased with increasing MMT content. It is important to note that enzymetic hydrolysis of PBSMC and PBSDMC were improved by blending with MMT.

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22

Wu, Chen-zhe, and 吳臣哲. "Biodegradable poly(butylene succinate) and its copolyesters with minor amounts of propylene succinate/montmorillonite nanocomposites." Thesis, 2015. http://ndltd.ncl.edu.tw/handle/fthz49.

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碩士
國立中山大學
材料與光電科學學系研究所
103
In this study, biodegradable nanocomposites were prepared. In order to improve the compatibility between polymer and montmorillonite (MMT), the surface of MMT was organo-modified by disodium cocoamphdipropionate (K2). Then, poly(butylene succinate) (PBSu) and its copolyesters with minor amount of propylene succinate (PBPSu90/10, PBPSu80/20) were blended with 1, 3, or 5 wt% of MMT-K2, respectively, by the melt intercalation. The physical properties of these biodegradable nanocomposites were characterized before studying their crystallization and melting behaviors. The Fourier Transform Infrared spectrum and wide-angle X-ray diffraction (WAXD) pattern show that MMT was successfully modified with K2, and the interlayer distance of MMT was increased from 1.62 to 3.94 nm. The WAXD patterns of nanocomposites yield that the interlayer distance of MMT-K2 was higher than 5.94 nm. The micrographs of transmission electron microscope indicate that these nanocomposites were intercalated, not exfoliated. The results of thermogravimetric analysis revealed that the thermal stability of the resultant nanocomposites was reduced after the addition of MMT-K2. Dynamic mechanical properties of the fabricated 3wt% or 5 wt% nanocomposites of these aliphatic copolyesters showed significant enhancements in the storage modulus compared with the neat matrix, even higher than that of PBSu. The effect of MMT-K2 on the isothermal crystallization behavior of PBSu, PBPSu90/10, and PBPSu80/20 was investigated using a differential scanning calori- meter (DSC) and polarized light microscopy (PLM). The Avrami equation successfully describes the isothermal crystallization kinetics of these nanocomposites and the value of Avrami exponent was between 2.42 and 3.35. The crystallization rate of neat BP80 was faster than BP80/MMT nanocomposites. This may be ascribed to the incompatibility of BP80 with MMT. On the contrast, the crystallization rate of BP90 or B100 nanocomposites was enhanced as the amount of MMT-K2 increased. The molecular weight of neat polymer before and after the melt intercalation indicated that the reduced molecular weight resulted in the increase of the growth rate of spherulites. Besides, it was found that the incorporation of MMT-K2 has little effect on the crystalline structure as well as the melting behavior of B100, BP90, or BP80.

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23

Liu, Wei-Chen, and 柳偉偵. "A Study on Natural Fiber Reinforced Poly(butylene succinate) (PBS) Biocomposites." Thesis, 2011. http://ndltd.ncl.edu.tw/handle/27875131828321420394.

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碩士
朝陽科技大學
應用化學系碩士班
99
In this study, poly(butylene succinate) (PBS) was reinforced by pineapple leaves fiber and recycled chopsticks fiber (the weight ratio is 7:3), and twin-screw mixer was used to mix the substrate and reinforcement materials. Subsequently, the test specimens of such natural fiber reinforced poly(butylene succinate) green biocomposites were prepared by injection molding machine. Firstly, the fibers were chemically treated by alkaline solution and silane coupling agent (Triethoxy-vinylsilan) to remove the pectin, hemicellulose and other impurities on the surface of the fibers. It’s expected that the compatibility between substrate (PBS) and reinforcement materials (pineapple leaf fibers and recycled chopsticks fiber) will be enhanced after the surface treatment. Subsequently, the PBS and reinforcement materials were mixed to form the natural plant fiber reinforced green biocomposites, and the morphology, mechanical and thermal properties of these biocomposite were investigated. The results reveal that the composite containing 30wt% of chemically modified natural plant fiber exhibited the best properties. SEM analysis shows that the compatibility between the substrate and the reinforcing materials was improved after chemical modification. As adding the fibers, the tensile, flexural and impact strengths of PBS can be improved by 121.7, 66.1 and 14.9%, respectively. TGA and DSC results show that the thermal stability of PBS can be improved, and heat deflection temperature can be increased about 33.6% by the addition of natural fibers. Furthermore, this type of reinforced PBS would be more environmentally friendly than the artificial additive-reinforced one. It can also effectively reduce and re-use the wastes of pineapple leaves fiber and recycled chopsticks fiber, as well as lower the costs of the materials.

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24

Jian, Da-jyun, and 簡大鈞. "A study of various organically modified clay/ poly (butylene succinate) nanocomposites." Thesis, 2008. http://ndltd.ncl.edu.tw/handle/46366748192042505693.

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碩士
朝陽科技大學
應用化學系碩士班
96
In this study, three kinds of organic intercalating agents were used for the modification of pristine montmorillonite.{i.e., cetyltrimethylammonium bromide (CTAB), decamethonium bromide (DEB), and cetylpyridinium chloride (CPC)} The influence of organically modified montmorillonite (OM) on PBS in aspects of mechanical properties, thermal properties and biodegradability were investigated OM were synthesized by replacing Na+ ions in two different layered silicates with quatemary ammonium cations by ion exchange, and subsequently, PBS/OM nanocomposites were prepared by a solution process. The results of wide-angle x-ray diffraction (WAXD) analyses and transmission electron microscopy (TEM) showed that silicate layers of the clay were intercalated, stacked, and randomly distributed in the PBS/OM nanocomposites. Dynamic mechanical analyzer (DMA) of the PBS/OM nanocomposite revealed that the storage modulus (E''), loss modulus (E") and glass transition temperature (Tg) increased with the inorganic concentration up to (5wt%). Enzymatic hydrolysis of PBS and PBS/OM was investigated by using Lipase PS. The hydrolysis rate took place preferentially in the amorphous part of the PBS sample and supported the conclusion that the crystallinity of a sample plays a major role in hydrolytic degradation.

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25

Guo, Ming-Tai, and 郭明泰. "Physical Properties of Biodegradable Poly(butylene succinate)/Proplyene-Ethylene Copolymer Polyblends." Thesis, 2008. http://ndltd.ncl.edu.tw/handle/6vzmvb.

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碩士
萬能科技大學
工程科技研究所
95
PBS/PER polyblends were perpared with from melt method in the BRABENDER by 190℃ 5 minutes and blending PBS with PER ratios of 100/0, 90/10, 80/20, 70/30, 60/40, 50/50, 40/60, 30/70, 20/80, 10/90, 0/100. Miscibility, crystallization behavior, and mechanical properties of PBS/PER polyblends were investigated by differential scanning calorimetry (DSC), scanning electron microscopy (SEM), and tensile tests (DMA and MTS) in this work. The PBS/PER polyblends in the differential scanning calorimetry (DSC), scanning electron microscopy (SEM) exhibited PBS/PER polyblends phase behavior. The PBS/PER polyblends indicating the PBS/PER (70/30)only presented one glass-transition and melt-transition，indicating the blending of PBS and PER at the component of 70/30(wt/wt) present good compatibility than other polymer blends. Futhermore, melt-coling scanning of melt-transition enthalpy higher than initial scanning. Because of PBS/PER polyblends presented spinodal decomposition (SD). As shown in DMA. Notably, the width of tan δ peak of PBS/PER (70/30) blend is narrower than other polymer blends, indicating that the blend has good distribution in the mixed macromolecular chains. That is, the blending of PBS and PER at the component of 70/30(wt/wt) present good compatibility.

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26

Praphulla, Praphulla, and Praphulla Praphulla. "Studies on Reactive Blends of Poly (hydroxybutyrate-co-valerate) and Poly (butylene succinate) Bioplastics." Thesis, 2012. http://hdl.handle.net/10214/4869.

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Various commodity plastics used today are based on fossil fuels. Most of these plastics are non-biodegradable and will persist in the environment over a long time. The bioplastics from renewable resources have the potential to support a greener economy. The two of such renewably resourced bioplastics are poly (hydroxyl butyrate-co-valerate), PHBV and poly (butylene succinate), PBS. We have used petro-based PBS in our study, but renewable resource based PBS is expected to be available on a commercial scale in a very near future. These two bioplastics are both biodegradable. These two bioplastics are both biodegradable. In our study we have used PBS from petroleum resource but PHBV is a brittle bioplastic with a high modulus value and a low elongation at break while PBS is a low modulus bioplastic with a high elongation at break. Complementary properties can be obtained by blending PHBV and PBS. The direct melt blends showed poor mechanical properties due to limited interaction between PHBV and PBS phases. This research focuses on increasing the interaction between PHBV and PBS blends by using compatibilizers. The compatibilizers used in this thesis were dicumyl peroxide, DCP and trimethylolpropane triacrylate, TMPTA. Use of an in situ compatibilization method was done for the melt mixing of PHBV and PBS yielding blends with improved characteristics. The investigations were performed at three different ratios of PHBV and PBS blends. The increase in the compatibility between the two phases was demonstrated through various thermal, thermo-mechanical, rheological and morphological means. The increase in elongation at break was used as a primary marker for compatibilization. The optimization of DCP and TMPTA was carried out, which showed the enhanced interaction between PHBV and PBS phases, with the successful stress transfer from PHBV phase to the PBS phase resulting in increase in elongation at break. Inward shifts in tan delta peak on addition of DCP and TMPTA to the blends also showed increase in compatibility between the two phases. The interfacial adhesion between a brittle and ductile polymer, PHBV and PBS respectively was increased by using DCP and TMPTA. This opened gateways to various novel applications of PHBV and PBS blends via in situ reactive extrusion process.
The Ontario Ministry of Agriculture, Food, and Rural Affairs (OMAFRA) for their financial support via New directions research program (SR9235). We would also like to thank Canadian Foundation for Innovation (CFI) and Ontario Ministry of Agriculture, Food, and Rural Affairs (OMAFRA) for their equipment supports.

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27

Kassos, Nikolaos, Adrian L. Kelly, Timothy D. Gough, and A. A. Gill. "Synergistic toughening and compatibilisation effect of Poly(butylene succinate) in PLA/poly-caprolactone blends." 2018. http://hdl.handle.net/10454/16750.

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Yes
Binary and ternary blends of a polylactic acid matrix with polycaprolactone (PCL) and polybutylene succinate (PBS) were produced by twin screw extrusion, containing up to 30 wt% loading. Mechanical, thermal and rheological characterisation techniques were used to quantify properties of the different blend formulations and miscibility was investigated using scanning electron microscopy. PCL is known to act as an impact modifier in PLA but to cause a corresponding reduction in strength. Results showed that addition of both PBS and PCL seperatly caused a reduction in melt viscosity, elastic modulus and tensile strength, but an increase in impact strength and strain at break. Analysis of morphology suggested that immiscibility was evident, particularly at higher PCL and PBS loadings. Results indicated that incorporation of a small loading of PBS had a synergistic effect on the PLA-PCL blend properties. Miscibility was improved and enhanced mechanical properties were observed for a ternary blend containing 5 wt% of both PBS and PCL compared to blends containing 10% of each polymer alone.
Financial support of Floreon- Transforming Packaging Ltd through the PhD sponsorship and materials provision.

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28

Kai-NingChuang and 莊凱甯. "Spherulitic Morphology and Phase Behavior of Poly(butylene succinate) Interacting with Poly(ethylene adipate)." Thesis, 2015. http://ndltd.ncl.edu.tw/handle/55450338412443612927.

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29

Chung, Shao Hua, and 鍾少華. "Effect of adding cellulose nanowhiskers on the physical properties of poly(butylene succinate-co-butylene adipate)." Thesis, 2014. http://ndltd.ncl.edu.tw/handle/64144545629430520882.

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30

HSU, CHIAO-YING, and 許巧穎. "Investigations on Crystallization Behaviors of Multi-component Composite Comprising Poly(butylene succinate)." Thesis, 2019. http://ndltd.ncl.edu.tw/handle/3eb3rk.

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31

Wang, Chun-Chieh, and 王俊傑. "Non-isothermal Crystallization Kinetics and Melting Behaviors of Poly(butylene succinate) and Poly(trimethylenesuccinate) blends." Thesis, 2008. http://ndltd.ncl.edu.tw/handle/72355726306432489944.

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碩士
高雄醫學大學
醫藥暨應用化學研究所碩士在職專班
96
Biodegradable aliphatic polyesters were synthesized by Showa Highpolymer company, trademarked “BIONOLLE”. BIONOLLE is a white crystalline thermoplastic such as poly(butylene succinate), poly(ethylene succinate) and polybutylene succinate adipate copolymer. The mechanical properties of BIONOLLE were similar to that of polyethylene. Avrami and Ozawa equations were used to analyze the experiment data in this study. Because the melting point of PBS is high and the mechanical properties are worse. In addition, the PTS is uncrystallized. Therefore, PBS and PTS were mixed to improve their properties. PBS containing 5wt% PTS can be able to reduce the crystallization performance, and make the polymer strength to enhance. Furthermore, the brittle fracture situation of PBS is also improved simultaneously. The thermostability of PBS/PTS (90/10) is similar to that of PBS/PTS (95/05). With PTS percentage increasing under the same condition, the thermal degradation temperature was decrease. Increasing the PTS percentage is helpful to the thermal degradation of PBS.

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32

HSU, KAI-HUNG, and 許凱閎. "Eco-Friendly Fully Bio-based Poly (Butylene Succinate-co-Propylene Succinate) Copolyesters:Effect in Glycerol as Cross-linking Agent." Thesis, 2019. http://ndltd.ncl.edu.tw/handle/xp74c3.

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碩士
國立臺北科技大學
分子科學與工程系有機高分子碩士班
107
In this study, Poly(butylene succinate-co-propylene succinate) (PBSPS) was polymerized and composed of succinic acid (SA), 1,4-butanediol (1,4-BDO), 1,3-propanediol (1,3-PDO), and glycerol (GC). All the used monomers could be derived from plant extraction and renewable. Poly(butylene succinate) (PBS) has a higher crystallinity of 71.5% and at a melting point (Tm) of 110 °C, while the poly(propylene succinate) (PPS) has a relatively low crystallinity with a Tm of 45 °C. The synthesized PBSPS copolyester at a BS/PS ratio of 7/3 has a low Tm at 80 °C and crystallization temperature (Tc) at a value of 20 °C. The amount of PS segment was increased from 30 to 50 mole%, the Tm and Tc of the obtained copolyesters were decreased, which caused by the occurrence of isodimorphism in the different composition of BS/PS ratio. The featured crystalline lattice of (021) and (110) of PBS were gradually disappeared at a 2θ of 21.5° and 22.5° with the increase of PS content more than 50 mole% to form PPS crystalline lattice in a 2θ of 22.3°. The PBSPS copolyesters have excellent thermal stability, having a higher Td above 300 ℃. The Young's modulus was decreased with the increase of the PS segment due to the decrease of crystallinity. In WAXD analysis, the amount of glycerol has an influence on the regularity of the chain movement, resulting in a decrease of crystallinity. The chain movement could be restricted by glycerol content with partially cross-linking to enhance the thermal and mechanical property. From the point of view of DSC and WAXD analysis, the crystallinity could be decreased with varying content of glycerol due to the irregularity of the molecular chain. The PBSPS copolyesters could be exhibited in elastic property in a glycerol content of 0.001 mole% and have transformed to the rigid property with the glycerol content more than 0.01 mole%. The chain conformation has examined in irregular architecture at the glycerol ratio of 0.02–0.03 mole% due to a more cross-linking point. The molecular chain tended to flexible in a glycerol content between 0.001 and 0.01 mole%. Finally, the fully bio-based PBSPS copolyesters have been copolymerized successfully and could be controlled the thermal and mechanical behavior with adjusting the glycerol composition. Based on the above, this study successfully prepared fully-biobased/low melting temperature thermolplastic, and modified the properties of copolyesters with a small amount of glycerin in different ranges.

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33

Wang, Tian-Yow, and 王天佑. "A study of the biodegradability of organically modified montmorillonate / poly-butylene succinate nanocomposites." Thesis, 2009. http://ndltd.ncl.edu.tw/handle/01363388868039206942.

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碩士
朝陽科技大學
應用化學系碩士班
97
In this study, the montmorillonite(MMT) was modified by cetyltrimethylammonium bromide (CTAB). The interlayer structural changes and the effects of modified MMT on the properties of poly-n-butyl succinate (Poly (butylenes succinate), PBS) were investigated. First of all, the modified MMT was obtained by cation exchange of sodium ions (Na+) in the interlayer of MMT and then PBS / MMT nanocomposites was prepared by solvent intercatation method. The wide-angle X-ray diffraction analyzer (WAXD) was used to analyze the interlayer distance of organic montmorillonite nanocomposites. Composting method was used to analyze the biodegradibility, and compared with the enzyme decomposition method. It is found that particle size and crystallinity will affect the decomposition rate of PBS. As the MMT content increased, the relatively smaller particles, will accelerate the hydrolysis reaction, and there by enhane the rate of biological decomposition.

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34

Hsu, Hui-Shun, and 許惠舜. "Copolymers and Blends of Poly(butylene succinate): Characterization, Crystallization, Melting Behavior, and Morphology." Thesis, 2009. http://ndltd.ncl.edu.tw/handle/gmreb7.

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碩士
國立中山大學
材料與光電科學學系研究所
97
The topics of this study are as follows: (a) Poly(butylene succinate) (PBSu) rich random copolymers containing ~20% and ~50% trimethylene succinate (TS), PBTSu 80/20 and PBTSu 50/50 that were synthesized from 1,4-butanediol, 1,3-propanediol and succinic acid: The influence of minor TS units on the thermal properties and crystallization rate of PBSu was investigated. (b) Random copolymer of ~90% PBSu and ~10% poly(1,4-cyclohexanedimethylene succinate), PBCHDMSu 90/10, that was synthesized from 1,4-butanediol, 1,4-cyclohexanedimethanol and succinic acid: The influence of cyclohexene unit on the thermal properties and crystallization rate of PBSu was investigated. (c) Blends of PBSu and poly(trimethylene succinate) (PTSu) or poly(ethylene succinate) (PESu): The weight ratio PBSu and PTSu (or PESu ) were 1:1. The crystallization and morphology of blends (PBSu/PTSu 50/50 and PBSu/PESu 50/50) were investigated and compared with PBTSu 50 and PBESu 50/50. The chemical composition and the sequence distribution of co-monomers in copolyesters were determined using NMR. Thermal properties of polyesters and blends were characterized using differential scanning calorimeter (DSC) and temperature-modulated DSC (TMDSC). The crystallization kinetics and equilibrium melting temperature were analyzed with Avrami equation and Hoffman-Weeks linear extrapolation. The thermal stability of polyesters was analyzed by thermogravimeter (TGA) and polarized light microscope (PLM) under nitrogen. Wide-angle X-ray diffractograms (WAXD) were obtained for specimens after complete isothermal crystallization. The growth rates, regime transition temperature, morphology and phase separation were studied using polarized light microscope (PLM) with isothermal method or nonisothermal method. The morphology of specimens after chemical etching were investigated using atomic force microscope (AFM) and scanning electron microscope (SEM). The distribution of butylene succinate (BS) and TS units in PBTSu 80/20 was found to be random from the evidence of a single Tg and a randomness value close to 1.0 for a random copolymer. With the increasing of minor amounts of comonomers, the sequence length of butylene succinate decreases, and the crystallization rate and the degree of crystallinity drop. DSC heating curves of isothermal crystallized PBTSu 80/20 and PBCHDMSu 90/10 showed triple melting peaks. Multiple melting behaviors indicate that the upper melting peaks are associated with the primary and the recrystallized crystals, or the crystals with different lamellar thickness. As the Tc increases, the contribution of recrystallization slowly decreases and finally disappears. Hoffman-Weeks linear plots gave an equilibrium melting temperature of 113.5

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35

Tsai, Gang-Shian, and 蔡岡憲. "Microstructure and Characterization of Poly(butylene succinate-co-adipate)/Layered double hydroxides Nanocomposites." Thesis, 2015. http://ndltd.ncl.edu.tw/handle/31061086754517402750.

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碩士
國立中興大學
材料科學與工程學系所
103
Semicrystalline poly(butylene succinate-co-adipate) (PBSA), a copolymer of butylene adipic acid and butylene succinic acid, can be synthesized using various molar ratio of butylene adipic acid and butylene succinic acid to obtain the designed properties of materials. Biodegradable PBSA is degraded by microorganisms to form the water and carbon dioxide. In order to enhance the physical properties of PBSA, the inorganic Mg-Al layered double hydroxides (LDH) was added into the PBSA polymer matrix. In this study, the organically modified Mg-Al LDH (SOLDH) were synthesized using the mixture of sorbitol and oleate through one-step coprecipitation. The interlayer spacing of SOLDH determined by X-ray diffraction was increased from 0.84 nm for LDH to 4.1 nm for SOLDH. The FT-IR spectrum of SOLDH contains four more absorption bands at 1005 cm-1, 1558 cm-1, 2831 cm-1 and 2922 cm-1 compared to that of LDH. The stacking of sheet-like morphology of SOLDH observed using scanning electron microscopy revealed a high aspect ratio. The PBSA/SOLDH nanocomposites were prepared by solution-casting. It was found that structure of PBSA/SOLDH nanocomposites were exfoliated and the incorporation of SOLDH into PBSA did not change the crystal arrangement of the PBSA crystal. The thermal properties of nanocomposites observed by Thermogravimetric analysis show the decrease the temperature at 10 % weight loss about 28~50℃ through catalytic action. Crystallization behavior was performed on differential scanning calorimetry (DSC) and polerized optical microscopy (POM). Results of isothermal crystallization of PBSA/SOLDH nanocomposites showed that the addition of high ratio of SOLDH into PBSA 3：1 induced more steric hindrance of the diffusion of PBSA polymer chain, reducing the transportation ability of polymer chains during crystallization, thus decreasing the crystallization rate and increasing chain folding surface energy. The long period of PBSA/SOLDH was studies by small-angle X-ray scattering (SAXS). The addition of low ratio of SOLDH into PBSA 3：1 can enhance the crystalline lamellar arrangement, but the addition of high ratio of SOLDH will hinder crystal plate layer arrangement. While the addition of SOLDH into PBSA 1：1, the crystalline lamellar arrangement of PBSA 1：1 is improved. Then the addition of SOLDH into PBSA 1：3, the crystal and amorphous plate layer arrangement is hindered. Degradation tests using Lipase from Pseudomonas fluorescens as the enzyme enzymatic degradation solution. Was observed by measuring the percentage of weight loss. The loading of SOLDH limited the motion of Lipase from Pseudomonas fluorescens and reduce the accessible attack spots for PBSA depolymerase.

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36

Lu, Shih-fu, and 盧世福. "Nonisothermal Crystallization and Thermal Degradation Behaviors of Poly(butylene succinate) and its Copolyesters with Minor Amounts of Propylene Succinate." Thesis, 2010. http://ndltd.ncl.edu.tw/handle/18196361621408894247.

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博士
國立中山大學
材料與光電科學學系研究所
98
Poly(butylene succinate) (PBSu) and two poly(butylene succinate-co-propylene succinate)s (PBPSu 95/5 and PBPSu 90/10) were synthesized via the direct polycondensation reaction. The copolyesters were characterized as having 7.0 and 11.5 mol% propylene succinate (PS) units, respectively, by 1H NMR. Copolyesters were characterized as random, based on 13C NMR spectra. They were fully investigated during nonisothermal crystallization and thermal degradation through various approaches in this study. A differential scanning calorimeter (DSC) and a polarized light microscope (PLM) adopted to study the nonisothermal crystallization of these polyesters at a cooling rate of 1, 2, 3, 5, 6 and 10 ºC/min. Morphologies and the isothermal growth rates of spherulites under PLM experiments were monitored and obtained by curve-fitting, respectively. These continuous rate data were analyzed with the Lauritzen-Hoffman equation. A transition of regime II → III was found at 95.6, 84.4, and 77.3 ºC for PBSu, PBPSu 95/5, and PBPSu 90/10, respectively. DSC exothermic curves show that all of the nonisothermal crystallization occurred in regime III. DSC data were analyzed using modified Avrami, Ozawa, Mo, Friedman and Vyazovkin equations. Ozawa equation does not accurately describe the nonisothermal crystallization kinetics of this polyester because part of the crystallization is secondary crystallization. All the results of PLM and DSC measurements indicate that incorporation of minor PS units into PBSu markedly inhibits the crystallization of the resulting polymer. The melting behavior of nonisothermally crystallized samples presents a continuous melting–recrystallization–remelting process. Additionally, three absorption bands during the nonisothermal crystallization were identified for PBSu and two PBPSu copolyesters, namely, 916, 955, 1045 cm-1 in the attenuated total reflectance FTIR spectra. Thermogravimetric analysis (TGA)-FTIR was heated at 5 ºC/min under N2 to monitor the degradation products of these three polyesters. FTIR spectra revealed that the major products were anhydrides, which were obtained following two cyclic intramolecular degradation mechanisms by breaking the weak O-CH2 bonds around a succinate group. Thermal stability at heating rates of 1, 3, 5, and 10 ºC/min under N2 was investigated using TGA. The model-free methods of Friedman and Ozawa equations are useful for studying the activation energy of degradation in each period of mass loss. The results reveal that the random incorporation of minor PS units into PBSu did not markedly affect their thermal resistance. Two model-fitting mechanisms were used to determine the loss mass function f(α), the activation energy and the associated mechanism. The mechanism of autocatalysis nth-order, with f(α)=αm(1-α)n, fitted the experimental data much more closely than did the nth-order mechanism given by f(α)=(1-α)n. The obtained activation energy was used to estimate the failure temperature (Tf). The values of Tf for a mass loss of 5% and an endurance time of 60,000 hr are 160.7, 155.5, and 159.3 ºC for PBSu and two the copolyesters, respectively.

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37

Hung, Ming-Chun, and 洪銘駿. "Characterization and Degradation behavior of Poly(butylene succinate -co-adipate)/ Modified-flax fiber composites." Thesis, 2015. http://ndltd.ncl.edu.tw/handle/43831000624460853476.

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碩士
國立中興大學
材料科學與工程學系所
103
To increase environmental consciousness, the use of biodegradable polymer has proved to be a solution to reduce the production and pollution of oil-based plastics. Poly (butylene succinate-co- adipate) (PBSA) containg good biodegration ability and processing properties. has been wildly study in recent years. However, this biopolymer needs to be reinforced to a better mechanical properties in applications. To keep the bio-based characteristics of composites, it is interesting to use natural fibers to replace the synthetic fibers in fiber-reinforced polymer composites. Flax fibers were considered as an environmentally friendly filler in fiber-reinforced polymer composites. This study described the measurement and comparison of several important properties of Flax/PBSA composites, such as morphology, mechanical performance, crystalline properties and enzymes degradation behavior. Two different flax fibers, 100 and 10 μm in diameter, were used to melt blend with PBSA. The influence of PEG treatment on Flax fibers has been investigated. The tensile modulus and storage modulus of composites were enhanced with increasing fibers content.The tensile strength and breaking elongation of composites were increase by decreasing fiber’s diameters.SEM images of composites showed that the vacancy between fiber and matrix in PEG-treated Flax/ PBSA composites were smaller than Flax/PBSA composites. The impact strength of PEG-treated Flax/ PBSA composites was higher than Flax/PBSA composites. The result of non-isothermal crystallization showed that the crystallization temperature of composites were higher than neat PBSA. The glass-transition temperature of composites were increased with increasing fiber content. It indicated that the Flax fibers can inhibit mobility of PBSA polymer chains. Degradation test use Lipase from Pseudomonas fluorescens as enzyme enzymatic degradation solution. It can be observed that the percentage of weight loss for the composites with 0.5 wt % flax fiber enhance the disintegration rate than that of the neat PBSA. On the other hand, the percentage of weight loss for the composites with 2 wt % PEG-treated fiber reduce the disintegration rate than that of the neat PBSA. This result indicated that the Flax fiber and PEG treatment can affect the biodegradation of PBSA.

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38

Liao, Hsi-Ling, and 廖希翎. "Study on the Toughening of Polylactic acid by Thermoplastic polyurethane and Poly(butylene succinate)." Thesis, 2010. http://ndltd.ncl.edu.tw/handle/15292544638816930260.

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碩士
逢甲大學
紡織工程所
98
This study focused on miscibility, phase morphology, and mechanical properties of a series of Polylactic acid/ Thermoplastic polyurethane/ Poly(butylene succinate) blends. Thermal behavior was analyzed by thermal gravimetric analyzer (TGA), differential scanning calorimeter (DSC) and dynamic mechanical analyzer (DMA). Mechanical properties were investigated by universal material testing machine. Blend morphology was observed by scanning electron microscopy. TGA showed that the initial degradation temperature decreased when TPU or PBS were added to PLA. And DSC results showed that the TPU and PBS could accelerate the crystallization rate of PLA. DMA results showed that the blends were immiscible. Otherwise, the compatibility of PLA and PBS was better than PLA and TPU, so the phase separation also could be observed in the liquid nitrogen fracture surface by SEM. With regard to mechanical properties, the elongation at break significantly increased when TPU and PBS were added to PLA, and the elongation at break exceeded 190% in the three component blends, indicating the brittle property of the material was transformed into ductile. The tensile fracture surface of blends was also observed by SEM.

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39

Gao, Guei-De, and 高貴德. "Biodegradable poly(butylene succinate) and its copolyesters with minor amounts of 2-methyl-1,3-propylene succinate/layered double hydroxide nanocomposites." Thesis, 2013. http://ndltd.ncl.edu.tw/handle/83969592261376947217.

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碩士
國立中山大學
材料與光電科學學系研究所
101
In this study, magnesium/aluminum layered double hydroxide (MgAl LDH) with a molar ratio of Mg/Al = 2 was synthesized by the co-precipitation method. In order to improve the compatibility between polymer and LDH, the surface of LDH was organo-modified by sodium dodecyl sulfate (SDS). Poly(butylene succinate) (B100) and its copolyesters with minor amounts of 2-methyl-1,3-propylene succinate (BM90 and BM80) were blended with 1, 3, or 5 wt% of SDS modified LDH, respectively, by the melt intercalation at 120, 100, and 90 °C and at a rotor speed of 50 rpm for 3 min. The physical properties of these biodegradable nanocomposites were characterized before studying their crystallization and melting behaviors. X-ray diffraction patterns and transmission electron micrographs indicated that the LDHs were intercalated and exfoliated, island-type exfoliated, and island-type exfoliated into the B100, BM90, and BM80 matrix, respectively, when the content of LDHs was 3 wt%. TGA results revealed that the thermal stability of the resultant nanocomposites was reduced after the addition of LDH. DSC heating thermograms of the amorphous nanocomposites (at a heating rate of 10 °C/min under nitrogen atmosphere) indicated that the cold crystallization ability and the degree of crystallinity of these nanocomposites decreased as the amount of LDH increased. Dynamic mechanical properties of the fabricated 3 wt% nanocomposites (at a heating rate of 2 °C/min) showed significant enhancements in the storage modulus compared with the neat matrix and 1 or 5 wt% nanocomposites. The effect of LDH-SDS on the isothermal crystallization behavior of B100, BM90, and BM80 was investigated using a differential scanning calorimeter (DSC) and polarized light microscopy (PLM). The Avrami equation successfully describes the isothermal crystallization kinetics of these nanocomposites and the value of Avrami exponent was between 2.32 and 3.15. The rate constant was significantly reduced when the amount of LDH was 3 wt%. Besides, it was found that the incorporation of LDH-SDS has little effect on the crystalline structure as well as the melting behavior of B100, BM90, and BM80. PLM micrographs revealed that smaller and less perfect crystals were formed in the nanocomposites because of the steric hindrance of the matrix diffusion, i.e. reducing the transportation ability of polymer chains during the crystallization. Finally, the overall results suggest that LDH-SDS at nanometer level acted as non-nucleating agent and decelerated the overall crystallization process of B100, BM90, and BM80.

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40

Lin, Sheng-Hsiang, and 林聖翔. "Preparation and characterization of organically modified layered zinc phenylphosphonate/ poly(butylene succinate-co-terephthalate) nanocomposites." Thesis, 2018. http://ndltd.ncl.edu.tw/handle/5sys6p.

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碩士
國立中興大學
材料科學與工程學系所
106
Poly(butylene succinate-co-terephthalate) (PBST), a semicrystalline copolymer and biodegradable, can be synthesized using terephthalic acid and butylene succinic acid. Biodegradable PBST can be degraded by microorganisms to form carbon dioxide and water. For the purpose of enhancing the physical properties of PBST, the inorganic layered zinc phenylphosphonate (PPZn) was added into the PBST polymer matrix. In this work, the organically-modified layered zinc phenylphosphonate prepared using coprecipitation method were sucessfully synthesized to intercalate diaminohexane and dodecanediamine into the interlayer spacing of PPZn (designated as C6-PPZn and C12-PPZn). The interlayer spacing of PPZn determined by wide-angle X-ray diffraction (WAXD) was increased from 14.34 Å for PPZn to 22.31 and 16.07 Å for C6-PPZn and C12-PPZn, respectively. The FT-IR spectra of modified-PPZn contain absorption bands at 2830-3000 and 1650-1550 cm-1 for the C-H stretching vibration and NH2 deformation of diaminohexane and dodecanediamine. Compare to that PPZn, the additional absorption peaks are attributed to diaminohexane and dodecanediamine in corporation into PPZn. The PBST-g-AA/modified-PPZn nanocomposites were prepared by solvent intercalation method. The structure and morphology of the PBST-g-AA/modified-PPZn nanocomposites were characterized using WAXD and transmission electron microscopy (TEM). Both WAXD and TEM results demonstrate that most of the partial-delamination modified-PPZn was randomly dispersed in the PBST matrix and the incorporation of modified-PPZn into PBST did not change the crystalline structure of the nanocomposites. Crystallization behavior was performed using the differential scanning calorimetry (DSC). The n value of nanocomposite is close to 2, suggesting that the PBST spherulite grows with a 2-dimensional structure. Degradation tests using Lipase from Pseudomonas fluorescens as the enzyme enzymatic degradation solution. The weight loss of PBST increase with an increase in the content of modified-PPZn. The C6-PPZn nanocomposites has a faster degradation rate. This result is probably due to the lower degree of crystallinity for C6-PPZn nanocomposites. The PBST and its nanocomposites with porous morphology were successfully fabricated by combining pseudo steady state unidirectional freezing and freeze-drying techniques. The weight loss of PBST increase with an increase in the content of modified-PPZn.

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41

Yang, Tsun-Wu, and 楊村梧. "Biodegradable Polycarbonate Blends with Polylactide and Poly(butylene succinate-co-L-lactate):Morphology and Properties." Thesis, 2015. http://ndltd.ncl.edu.tw/handle/02141351659809095824.

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碩士
東海大學
化學工程與材料工程學系
103
The PC/PLA composites have bad compatibility. In order to improve compatibility of composites and keep composites biodegrade. This research has two parts. First part, use barbender and twin screw to make PLA/PBSL copolymer. Twin screw part: we used Dicumyl peroxide (DCP) to make grafted copolymer. When the content of DCP was from 0.05 to 0.2 phr., the rheological properties increase with increasing the DCP content. Barbender part: we used epoxy (high and low molecular weight) and isocyanate (linear and aromatic) to make block copolymer.Epoxy1010 has the higher storage modulus than other additive in DMA, and Epoxy1010 has good compatibility. Second part, use barbender and twin screw to make PC/PLA/PBSL composites. Barbender part: use the copolymer which made from part1 to be compatibilizer to blend with PC. BCP1010 has smallest dimension change, and has almost no defect. Finally, adjust PC/PLA/BCP to find the best composition. Composites have mixed with modifier made from twin screw mechanical properties become batter. We can confirm composites with fewer defects by using SEM. I have done other analysis in this research.

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42

Kuo, Dong-Lin, and 郭東霖. "Preparation and characterization of organically modified layered zinc phenylphosphonate/ Poly(butylene succinate - co - adipate) nanocomposites." Thesis, 2016. http://ndltd.ncl.edu.tw/handle/20654927967827418473.

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碩士
國立中興大學
材料科學與工程學系所
104
Poly(butylene succinate-co-adipate) (PBSA), a semicrystalline copolymer of butylene adipic acid and butylene succinic acid, can be synthesized using butylene adipic acid and butylene succinic acid. Biodegradable PBSA is degraded by microorganisms to form carbon dioxide and water. For the purpose of enhancing the physical properties of PBSA, the inorganic layered zinc phenylphosphonate (PPZn) was added into the PBSA polymer matrix. In this work, the organically-modified layered zinc phenylphosphonate prepared using coprecipitation method were sucessfully synthesized to intercalate dodecylamine, hexadecylamine and octadecylamine into the interlayer spacing of PPZn (designated as C12-PPZn、C16-PPZn and C18-PPZn). The interlayer spacing of PPZn determined by wide-angle X-ray diffraction (WAXD) was increased from 1.43 nm for PPZn to 2.28, 2.75 and 3.04 nm for C12-PPZn, C16-PPZn and C18-PPZn, respectively. The FT-IR spectrum of modified-PPZn contains absorption bands at 2830-3000 and 1650-1550 cm-1 for the C-H stretching vibration and NH2 deformation of dodecylamine, hexadecylamine and octadecylamine. Compare to that PPZn, the additional absorption peaks attributed to dodecylamine, hexadecylamine and octadecylamine in corporation into PPZn. The paracrystalline distortion patameter of C12-PPZn, C16-PPZn and C18-PPZn are 1.96, 2.15 and 2.36 using the Hosemann equation. The PBSA/modified-PPZn nanocomposites were prepared by melt-mixing. The structure and morphology of the PBSA/modified-PPZn nanocomposites were characterized using WAXD and transmission electron microscopy (TEM). Both WAXD and TEM results demonstrate that most of the partial-delamination modified -PPZn was randomly dispersed in the PBSA matrix and the incorporation of modified-PPZn into PBSA did not change the crystal arrangement of the PBSA crystalline structrue. Crystallization behavior was performed on differential scanning calorimetry (DSC) and polerized optical microscopy (POM). The n value of the neat PBSA is close to 3, indicating that the neat PBSA spherulite grows with a 3-dimensional structure. The n value of nanocomposite with the incorporation of PPZn is close to 3, suggesting that the PBSA spherulite still grows with a 3-dimensional structure. Upon addition of modified -PPZn into PBSA result in increasing chain folding surface energy due to the limit of molecular chain arrangement of PBSA. The long period of PBSA/modified-PPZn was studies by small-angle X-ray scattering (SAXS). The addition of modified-PPZn into PBSA will hinder crystal plate layer arrangement. Then the addition of modified-PPZn into PBSA the long period and crystal plate layer arrangement decreases owing to modified-PPZn hinder molecular chain arrangement of PBSA. Degradation tests using Lipase from Pseudomonas fluorescens as the enzyme enzymatic degradation solution. The weight loss of PBSA increase with an increase in the content of modified-PPZn. The weight loss percentage of the C18-PPZn nanocomposites approached about 99.2 % after 3 days of degradation. This result is probably due to the lowest degree of crystallinity for C18-PPZn.

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43

Shi, Zhe-Wei, and 石哲維. "Ternary Blends of Polycarbonate, Polylactide, and Poly(butylene succinate-co-L-lactate):Morphology and Properties." Thesis, 2014. http://ndltd.ncl.edu.tw/handle/84032611069066702832.

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碩士
東海大學
化學工程與材料工程學系
102
The research is mainly for ternary blends of PC / PLA / PBSL. Discussion is divided into two parts; the first part is added among PC, PLA, and PBSL to achieve the properties of biodegradable materials. The experiments for the first part, separated the two systems, one of that is PC possession 70% of the ternary blends, and the other one is PC possession 50% of the ternary blends. For PC possession 70% of the ternary blends, the continuous phase is PC; with the increase of PBSL and PLA decrease, the tensile test results show that has batter ductility than before, and thermal distortion temperature gradually drops. For PC possession 50% of the ternary blends, the continuous phase transformed into PLA and PBSL, with the increase of PBSL and PLA decrease, the tensile test results show that has batter ductility than before, and thermal distortion temperature gradually increase, but adding to much PBSL, the tensile test results would be worse, and thermal distortion temperature would drops. From different proportions of composite plastics, when increase of PBSL and PLA decrease we can discover reduced surface defects, and compatibility becomes better by the picture of SEM. The second part is added ternary blends MDI modifier or DCP, using the PLA and PBSL crosslinking copolymer to increase the compatibility of the ternary blends system. The ternary blends which added modifier, can see that fewer defects and the dispersed phase have become smaller and more evenly dispersed from SEM picture. The mechanical properties of the blends have a tendency to enhance. That can proof the blends, which added modifier compatibility further improved.

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44

HappyMandala, Yahya, and 曼達拉. "Mechanism of Lamellar Assembly in Janus-faced Spherulites of Poly(butylene succinate) Blended With Water-Soluble Poly(ethylene oxide)." Thesis, 2015. http://ndltd.ncl.edu.tw/handle/42898369113621581830.

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碩士
國立成功大學
化學工程學系
103
Morphology of semicrystalline poly(butylene succinate) (PBSu) revealed Janus-faced spherulites with fine banded spherulites. The spherulitic morphology of neat PBSu showed banded spherulites with minor fibrous part at low crystallization temperature of 70 oC. On the other hand, morphology of neat PEO naturally exhibited fibrous pattern or coarse-grained morphology. In brief, the PBSu/PEO blend presented complex crystallization behaviours depending on the blend composition. The band-spacing of neat PBSu became larger with the increasing of PEO content on the blend, the optimum ring-band formation revealed at PBSu/PEO 70/30. Top cover confinement also had influenced on spherulite morphology in the blend. PEO domains were found to nucleate and grow continuously in the blend 70/30 melted at Tmax 150 oC and after melted at 160 and 170 oC those small PEO segregations were increased and growth continuously after crystallized at room temperature for 30 minutes, while in Tmax 190 and 200 oC PEO spherulite disappeared because homogeneous phase segregation (well distributed). From AFM observation, the AFM images of PBSu/PEO blend before and after etching, were found an amount of PEO crystallized on the top of PBSu making the surface of PBSu spherulites mostly covered by plat-like lamellae of PEO. Thermal behaviour observation, two melting endotherm peaks were observed by DSC for all blend system. Blending PBSu with PEO did not generate any new endotherm peak of the blend. By WAXD, PBSu/PEO blend did not show any new crystal peak, from DSC and WAXD indicated that both of PBSu and PEO were crystallized in their own crystal lattices. From the FTIR result, the usage of 190 oC melting temperature did not give any significant effect on PEO degradation. The mechanism of Janus-faced spherulites of PBSu/PEO blend composed a ring-band and fibrous pattern. The fibrous lamellae packed by wider lamellae in flat-on orientation. The growth rate of fibrous lamellae had possibility to grow in all directions. From top view by AFM and SEM images, proved that the lamellae in the nuclei part composed by “tied” or sheaf-like lamellae bundled compactly. The sheaf-like or tied lamellae were discerned to grow radially as a periodic ridge consist of edge-on orientation while the valley composed by narrow flat-on lamellae, such phenomenon occured periodically. It led to the formation of the ring-banded pattern. The areas without sheaf-like lamellae was covered by plated lamellae that tent to grow as fibrous continuously. The ring-banded and fibrous pattern were parallel with each other, suggesting identical growth rates for these two regions. The growth rates of both regions were quite similar. From top view the lamellar arrangement in the fibrous pattern as flat-on orientation growth with small branches on the side part and growth continuously along radial direction and packed of long and wide lamellae. From lateral view of fibrous region, the lamellae orientation composed by flat-on lamellae, resulting in the formation of a fibrous pattern. On the other hand, with the same view , the center part was stood as the main ridge consisting of edge-on lamellae and bending to form flat-on lamellae on the valley composed by narrow lamellae in flat-on orientation. From top view, it was shown that the valley (darker region) packed by flat-on lamellae and ridge region packed with small edge-on lamellae resulting the formation of ring-banded pattern.

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45

Lu, Jin-Shan, and 呂金山. "Nonisothermal Crystallization and Thermal Degradation Behaviors of Poly(butylene succinate) and its Copolyesters with Minor Amounts of 2-methyl-1,3-Propylene Succinate." Thesis, 2012. http://ndltd.ncl.edu.tw/handle/75057954889313142244.

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博士
國立中山大學
材料與光電科學學系研究所
100
Poly(butylene succinate) (PBSu), poly(2-methyl-1,3-propylene succinate) (PMPSu), and their two novel poly(butylene succinate-co-2-methyl-1,3-propylene succinate)s (PBMPSu 95/05 and PBMPSu 90/10) were synthesized by a two-stage esterification reaction. PBMPSu 95/05 and PBMPSu 90/10 were characterized as having 6.5 and 10.8 mol% 2-methyl-1,3-propylene succinate (MPS) units, respectively, by 1H NMR. These copolymers were characterized to be random from the 13C NMR spectra. In this study, the nonisothermal crystallization and thermal degradation behaviors of the polyesters were investigated via different approaches. A differential scanning calorimeter (DSC) and a polarized light microscope (PLM) were employed to investigate the nonisothermal crystallization of these copolyesters and neat PBSu. Morphology and the isothermal growth rates of spherulites under PLM experiments at three cooling rates of 1, 2.5 and 5 °C/min were monitored and obtained by curve-fitting. These continuous rate data were analyzed with the Lauritzen-Hoffman equation. A transition of regime II → III was found at 96.2, 83.5, and 77.9 °C for PBSu, PBMPSu 95/05, and PBMPSu 90/10, respectively. DSC exothermic curves at five cooling rates of 1, 2.5, 5, 10 and 20 °C/min show that almost all of the nonisothermal crystallization occurred in regime III. DSC data were analyzed using modified Avrami, Tobin, Ozawa, Mo, Friedman and Vyazovkin equations. All the results of PLM and DSC measurements reveal that incorporation of minor MPS units into PBSu markedly inhibits the crystallization of the resulting polymer. The nonisothermal crystallization behavior of these polyesters was also investigated using a Fourier-transform infrared spectrometer (FTIR) with an attenuated total reflection (ATR). The absorbance peaks of crystals for the α form (918, 955, and 1045 cm-1) of PBSu and PBMPSu copolyesters were observed by ATR-FTIR under nonisothermal crystallization. When these semicrystalline polyesters started to be solidified from the melt state, these characteristic absorption bands for PBSu and its copolyesters crystals have been detected. In this study, the thermal degradation mechanisms of PBSu, PMPSu, PBMPSu 95/05, and PBMPSu 90/10 were investigated using a thermogravimetric analyzer combined Fourier-transform infrared spectrometer (TGA-FTIR) and a pyrolysis-gas chromatography–mass spectrometry (Py-GC-MS). The volatile products evolved from the thermal degradation of these two copolyesters were identified to be anhydride, ether, ester, alcohol, alkene, aldehyde, and CO2. FTIR spectra displayed that the main degradation products for these four polymers were anhydrides. Moreover, PBSu-rich PBMPSu copolymers exhibited the same thermal degradation mechanism as that of PBSu at lower thermal degradation temperatures (< 403 ºC) and as that of PMPSu at higher thermal degradation temperatures (> 403 ºC) by the TGA-FTIR analysis. The results of the TGA-FTIR analysis clearly demonstrates that the influence of MPS units on the thermal degradation process is gradually increased as the temperature increases for PBMPSu copolymers. The degradation mechanism of PBMPSu at lower thermal degradation temperatures and PBSu mainly follows the β-hydrogen bond scission mechanism and the back-biting process from the polymer chains. Moreover, the degradation mechanism of PBMPSu at higher thermal degradation temperatures and PMPSu occurred mainly through the β-hydrogen bond scission and secondarily through α-hydrogen bond scission. Finally, the thermal stability and degradation kinetics of these polyesters were investigated using a TGA at heating rates of 1, 3, 5, and 10 ºC/min under dynamic nitrogen. The activation energies of thermal degradation in elective conversions were estimated using the Friedman and Ozawa methods. The results clearly demonstrated that the thermal stabilities of these PBMPSu copolyesters were slightly reduced with the incorporation of minor MPS units into PBSu. Two model-fitting methods of nth-order and autocatalysis nth-order reaction mechanisms were adopted to determine the mass loss function f(α), the activation energy and the associated degradation parameters. The results revealed that the mechanism of autocatalysis nth-order fitted the experimental data much more closely than did the nth-order mechanism for PBSu, PMPSu and PBMPSu copolymers.

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46

Ojijo, Vincent Omondi. "Development of environmentally-friendly polymeric materials based on polylactide and poly[(butylene succinate)-co-adipate] blends." 2013. http://encore.tut.ac.za/iii/cpro/DigitalItemViewPage.external?sp=1000972.

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D. Tech. Polymer Technology.
Objectives of this work were to develop PLA/PBSA-based hybrid materials with better barrier properties, thermal stability, impact strength and at the same time, have relatively good strength and modulus. The specific objectives were: 1) To optimise PLA/PBSA blend composition for the desired blend properties. This entailed understanding of the role of specific interfacial area obtained from the morphologies of the blends in controlling the properties of the same and relate qualitatively, the phase morphologies to the properties of the PLA/PBSA blends. 2) To study the effect of annealing on the properties of PLA/PBSA blends. 3) To study the effect of organic modifiers on clay surfaces and the interlayer d-spacing of the clay on the morphology and properties of PLA/PBSA-clay composites 4) To study clay dispersion at various loadings and how it affects the crystallization of PLA and PBSA components in the blend.5) To study clay loading effect on the thermal and mechanical properties of the PLA/PBSA-clay composites. 6) To optimise the processing parameters, vis-a-vis: reaction time, coupling agent content, PLA/PBSA composition and processing sequence during in-situ reactive compatibilization of PLA/PBSA blends. 7) To improve the thermal stability and barrier properties through reactive processing of PLA/PBSA, in the presence of organoclays and a coupling agent. 8) To study the rheological properties of the blends prepared, as a function of clay content in the physically and reactively compatibilized PLA/PBSA blends.

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47

Ya-LingTseng and 曾雅羚. "Spherulites Sectored into Complex Ringed/Dendritic Faces in Poly(butylene succinate) Crystallized with an Isomeric Polymer." Thesis, 2019. http://ndltd.ncl.edu.tw/handle/z7y4a7.

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48

Lin, Chin-Sheng, and 林錦昇. "Preparation and properties of biodegradable poly(butylene succinate)/Jeffamine® polyetheramine modified multi-walled carbon nanotube nanocomposites." Thesis, 2010. http://ndltd.ncl.edu.tw/handle/88136801543634315794.

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碩士
國立中興大學
化學工程學系所
98
In this study, poly(butylene succinate)/multi-walled carbon nanotubes (PBS/MWNTs) hybrids were prepared by a melt-blending method. In order to enhance the compatibility between PBS and MWNTs, the surfaces of MWNTs were chemically modified. MWNTs were first pre-treated using acid solution (HNO3) to obtain functionalized carboxylic groups. Subsequently, Jeffamine® polyetheramine (M2005 (EO/PO = 6/29) and M2070 (EO/PO = 33/10)) were respectively grafted onto MWNTs with the assistance of a dehydrating agent, N,N’-dicyclohexyl-carbodiimide (DCC). As a result, organically modified MWNTs (MWNT-2005D and MWNT-2070D) were obtained. It was found that MWNT-2005D could be well dispersed in organic solvents such as acetone, THF, and chloroform. In addition, MWNT-2070D could be well dispersed in water. Moreover, the PBS/MWNTs nanocomposites were further prepared through the melt-blending method. Mechanical properties, thermal behavior, and conductivity of resultant PBS/MWNTs composites were investigated. The results show that excellent dispersion of nanotubes in the PBS matrices was achieved. Moreover, an improvement in thermal properties was also observed. With the addition of 3.0 wt % of MWNT-2070D, Td of the nanocomposite was 10.1 oC higher than that of the pristine PBS sample. Apart from that, the increments of E’ and E” of the nanocomposite at 25 oC were 113 and 116 %, respectively. In the aspect of conductivity, the surface resistivity decreased from 2.35×1014 Ω/cm2 for neat PBS to 5.88×103 Ω/cm2 for the nanocomposites with 3.0 wt % of MWNT-2070D. Such PBS/MWNT-2070D nanocomposites are highly efficient for anti-static purpose, even electrostatic discharge and EMI shielding, which can be applied in electronic materials.

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49

Li, Kan-Rung, and 李侃融. "Characteristics of Biodegradable Poly(lactic acid) / Poly(butylenes succinate) Blends." Thesis, 2010. http://ndltd.ncl.edu.tw/handle/36793164916684276295.

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碩士
萬能科技大學
材料科技研究所
98
The poly(lactic acid)/poly(butylenes succinate) blends(PLA/PBS) were here in prepared by a method of melting blend, and had PBS content from 10 to 90wt%. The PLA/PBS characteristics for the phase transition regions, compatibility and morphology were investigated by DSC, DMA and SEM; and the effects of the characteristics on the tensile property were determined by the tensile strength. The various PLA/PBS blends present three regions of phase transition, including the glass transition region of PBS at -31~-37℃, the glass transition region of PLA at 52~-58℃ and the melting region of crystal at 108~110℃. The morphologies of PLA/PBS were a dispersive two-phase structure involved the sphere, layer and random dispersive morphology. The random dispersive morphology for the PLA/PBS had the random dispersive morphology, which presented a high ultimate elongation at 460% according to the analysis of tensile strength. Because a serious interface occurred at the dispersive phase of PLA sphere resulted from the process of nucleation and growth, it exhibited the low compatibility and tensile strength. Furthermore, as the PBS content was increased the Tan δ value and tensile strength were increased, indicating that the toughness of PLA was improved by the PBS blended with PLA.

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50

Liu, Chien-ting, and 劉建廷. "A study of poly(butylenes succinate) composites reinforced by the fiber recycling from disposable chopsticks." Thesis, 2010. http://ndltd.ncl.edu.tw/handle/01673423951189143058.

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碩士
朝陽科技大學
應用化學系碩士班
98
This study adopts the compounding method using a Bradender to blend Poly(butylene succinate) and fibers (recycling from chopsticks) to obtain the natural fiber-reinforced green PBS composites. First of all, the bamboo chopsticks were treated with alkali to remove the surface pectin, hemicellulose and other impurities, and then treated by coupling agent to change its nature chemically. Subsequently, PBS was blended with different proportions of these chemically-treated fibers and non-treated fibers, to form the plant fiber-reinforced composites. The materials were then investigated for their mechanical and heat properties. In general, the addition of plant fibers to obtain the natural fiber-reinforced green PBS composites is not only to lower the costs of the materials, but also reduce the consumption of petrochemical plastics that would cause pollution. Moreover, it is also capable of enhancing agricultural development and cutting down agricultural wastes that would damage the environment.

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