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- ItemPressure- and Temperature-Dependent Crystallization Kinetics of Isotactic Polypropylene under Process Relevant Conditions(Basel : MDPI, 2021) Spoerer, Yvonne; Boldt, Regine; Androsch, René; Kuehnert, InesIn this study, a non-nucleated homopolymer (HP) and random copolymer (RACO), as well as a nucleated HP and heterophasic copolymer (HECO) were investigated regarding their crystallization kinetics. Using pvT-measurements and fast scanning chip calorimetry (FSC), the crystallization behavior was analyzed as a function of pressure, cooling rate and temperature. It is shown that pressure and cooling rate have an opposite influence on the crystallization temperature of the materials. Furthermore, the addition of nucleating agents to the material has a significant effect on the maximum cooling rate at which the formation of α-crystals is still possible. The non-nucleated HP and RACO materials show significant differences that can be related to the sterically hindering effect of the comonomer units of RACO on crystallization, while the nucleated materials HP and HECO show similar crystallization kinetics despite their different structures. The pressure-dependent shift factor of the crystallization temperature is independent of the material. The results contribute to the description of the relationship between the crystallization kinetics of the material and the process parameters influencing the injection-molding induced morphology. This is required to realize process control in injection molding in order to produce pre-defined morphologies and to design material properties.
- ItemThe Influence of Salt Anions on Heavy Metal Ion Adsorption on the Example of Nickel(Basel : MDPI, 2018) Mende, Mandy; Schwarz, Dana; Steinbach, Christine; Boldt, Regine; Schwarz, SimonaThe biodegradable polysaccharide chitosan possesses protonated and natural amino groups at medium pH values and has therefore been used as an adsorbing material for nickel salts in water treatment. Nickel is a problematic heavy metal ion which can cause various diseases and disorders in living organisms. Here, we show the influence of oxyanions (e.g., nitrate and sulfate) to the adsorption of nickel ions. Hence, simultaneously we are addressing the increasing global problem of nitrate and sulfate ion pollution in groundwater and surface water. A series of adsorption experiments was carried out in order to determine (i) the adsorption equilibrium, (ii) the adsorption capacity in dependence on the initial nickel ion concentration, and (iii) the influence of the anion presented in solution for the adsorption capacity. Surface morphology of chitosan flakes before and after the adsorption process has been studied with SEM-EDX analysis. The chitosan flakes exhibited promising adsorption capacities of 81.9 mg·g−1 and 21.2 mg·g−1 for nickel (sulfate) and nickel (nitrate), respectively. The calculated values of Gibbs free energy change ΔG0 confirm the higher adsorption of nickel ions in presence of sulfate ions. Hence, higher anion valence leads to a higher adsorption capacity.
- ItemThe Localization Behavior of Different CNTs in PC/SAN Blends Containing a Reactive Component(Basel : MDPI, 2021-3-1) GĂ¼ltner, MarĂ©n; Boldt, Regine; Formanek, Petr; Fischer, Dieter; Simon, Frank; Pötschke, PetraCo-continuous blend systems of polycarbonate (PC), poly(styrene-co-acrylonitrile) (SAN), commercial non-functionalized multi-walled carbon nanotubes (MWCNTs) or various types of commercial and laboratory functionalized single-walled carbon nanotubes (SWCNTs), and a reactive component (RC, N-phenylmaleimide styrene maleic anhydride copolymer) were melt compounded in one step in a microcompounder. The blend system is immiscible, while the RC is miscible with SAN and contains maleic anhydride groups that have the potential to reactively couple with functional groups on the surface of the nanotubes. The influence of the RC on the localization of MWCNTs and SWCNTs (0.5 wt.%) was investigated by transmission electron microscopy (TEM) and energy-filtered TEM. In PC/SAN blends without RC, MWCNTs are localized in the PC component. In contrast, in PC/SAN-RC, the MWCNTs localize in the SAN-RC component, depending on the RC concentration. By adjusting the MWCNT/RC ratio, the localization of the MWCNTs can be tuned. The SWCNTs behave differently compared to the MWCNTs in PC/SAN-RC blends and their localization occurs either only in the PC or in both blend components, depending on the type of the SWCNTs. CNT defect concentration and surface functionalities seem to be responsible for the localization differences.
- ItemSolubility and selectivity effects of the anion on the adsorption of different heavy metal ions onto chitosan(Basel : MDPI, 2020) WeiĂŸpflog, Janek; GĂ¼ndel, Alexander; Vehlow, David; Steinbach, Christine; MĂ¼ller, Martin; Boldt, Regine; Schwarz, Simona; Schwarz, DanaThe biopolymer chitosan is a very efficient adsorber material for the removal of heavy metal ions from aqueous solutions. Due to the solubility properties of chitosan it can be used as both a liquid adsorber and a solid flocculant for water treatment reaching outstanding adsorption capacities for a number of heavy metal ions. However, the type of anion corresponding to the investigated heavy metal ions has a strong influence on the adsorption capacity and sorption mechanism on chitosan. In this work, the adsorption capacity of the heavy metal ions manganese, iron, cobalt, nickel, copper, and zinc were investigated in dependence on their corresponding anions sulfate, chloride, and nitrate by batch experiments. The selectivity of the different heavy metal ions was analyzed by column experiments. © 2020 by the authors.
- ItemBlending In Situ Polyurethane-Urea with Different Kinds of Rubber: Performance and Compatibility Aspects(Basel : MDPI, 2018-11-02) Tahir, Muhammad; Heinrich, Gert; Mahmood, Nasir; Boldt, Regine; WieĂŸner, Sven; Stöckelhuber, Klaus WernerSpecific physical and reactive compatibilization strategies are applied to enhance the interfacial adhesion and mechanical properties of heterogeneous polymer blends. Another pertinent challenge is the need of energy-intensive blending methods to blend high-tech polymers such as the blending of a pre-made hard polyurethane (-urea) with rubbers. We developed and investigated a reactive blending method to prepare the outstanding blends based on polyurethane-urea and rubbers at a low blending temperature and without any interfacial compatibilizing agent. In this study, the polyurethane-urea (PUU) was synthesized via the methylene diphenyl diisocyanate end-capped prepolymer and m-phenylene diamine based precursor route during blending at 100 °C with polar (carboxylated nitrile rubber (XNBR) and chloroprene rubber (CR)) and non-polar (natural rubber (NR), styrene butadiene rubber (sSBR), and ethylene propylene butadiene rubber (EPDM)) rubbers. We found that the in situ PUU reinforces the tensile response at low strain region and the dynamic-mechanical response up to 150 °C in the case of all used rubbers. Scanning electron microscopy reveals a stronger rubber/PUU interface, which promotes an effective stress transfer between the blend phases. Furthermore, energy filtered transmission electron microscopy (EFTEM) based elemental carbon map identifies an interphase region along the interface between the nitrile rubber and in situ PUU phases of this exemplary blend type.
- ItemEffect of Molar Mass on Critical Specific Work of Flow for Shear-Induced Crystal Nucleation in Poly (l-Lactic Acid)(Basel : MDPI, 2021) Du, Mengxue; Jariyavidyanont, Katalee; KĂ¼hnert, Ines; Boldt, Regine; Androsch, RenĂ©The concept of specific work of flow has been applied for the analysis of critical shearing conditions for the formation of crystal nuclei in poly (l-lactic acid) (PLLA). Systematic variation in both time and rate of shearing the melt in a parallel-plate rheometer revealed that these parameters are interconvertible regarding the shear-induced formation of crystal nuclei; that is, low shear rate can be compensated for by increasing the shear time and vice versa. This result supports the view that critical shearing conditions can be expressed by a single quantity, providing additional options for tailoring polymer processing routes when enhanced nuclei formation is desired/unwanted. Analysis of PLLA of different mass-average molar masses of 70, 90, 120, and 576 kDa confirmed improved shear-induced crystal nucleation for materials of higher molar mass, with critical specific works of flow, above which shear-induced nuclei formation occurs, of 550, 60, 25, and 5 kPa, respectively.
- ItemCorrelation between Processing Parameters, Morphology, and Properties of Injection-Molded Polylactid Acid (PLA) Specimens at Different Length Scales(Basel : MDPI, 2023) Meinig, Laura; Boldt, Regine; Spoerer, Yvonne; Kuehnert, Ines; Stommel, MarkusPolylactic acid (PLA) is one of the most promising bioplastic representatives that finds application in many different areas, e.g., as single-use products in the packaging industry, in the form of mulch film for agriculture, or in medical devices. For the development of new areas, especially in terms of long-term applications and the production of recyclable products, the material properties controlled by processing must be known. The state of the art is investigations at the global scale (integral values) without consideration of local structure inhomogeneities and their influence on the material properties. In this work, morphological, thermal, and mechanical properties of injection-molded PLA tensile bars are investigated at different length scales (global and local) as a function of processing parameters. In addition to the processing parameters, such as melt temperature, mold temperature, and cooling time in the mold, the influence of the D-isomer content on the crystallization behavior and the resulting material properties are investigated. The material was found to form crystalline structures only when cooled in a mold tempered above Tg. In addition, PLA with a lower content of D-isomer was found to have a higher degree of crystallinity. Since the mechanical properties obtained by tensile tests could not be correlated with the degree of crystallinity, detailed analysis were performed showing a characteristic inhomogeneous morphology within the tensile bars. By means of micromechanical investigations on samples with different microstructure ranges, the relationship between local morphology and failure behavior could be explained.
- ItemBarrier properties of GnP-PA-extruded films(Basel : MDPI, 2020) Boldt, Regine; Leuteritz, Andreas; Schob, Daniela; Ziegenhorn, Matthias; Wagenknecht, UdoIt is generally known that significant improvements in the properties of nanocomposites can be achieved with graphene types currently commercially available. However, so far this is only possible on a laboratory scale. Thus, the aim of this study was to transfer results from laboratory scale experiments to industrial processes. Therefore, nanocomposites based on polyamide (PA) and graphene nanoplatelets (GnP) were prepared in order to produce membranes with improved gas barrier properties, which are characterized by reduced permeation rates of helium. First, nanocomposites were prepared with different amounts of commercial availably graphene nanoplatelets using a semi-industrial-scale compounder. Subsequently, films were produced by compression molding at different temperatures, as well as by flat film extrusion. The extruded films were annealed at different temperatures and durations. In order to investigate the effect of thermal treatment on barrier properties in correlation to thermal, structural, and morphological properties, the films were characterized by differential scanning calorimetry (DSC), wide angle X-ray scattering (WAXS), optical microscopy (OM), transmission electron microscopy (TEM), melt rheology measurements, and permeation measurements. In addition to structural characterization, mechanical properties were investigated. The results demonstrate that the permeation rate is strongly influenced by the processing conditions and the filler content. If the filler content is increased, the permeation rate is reduced. The annealing process can further enhance this effect.