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The chemical synthesis of polysiloxanes from monomeric starting materials involves a series of hydrolysis, condensation and modification reactions with complex monomeric and oligomeric reaction mixtures. Real-time monitoring and precise process control of the synthesis process is of great importance to ensure reproducible intermediates and products and can readily be performed by optical spectroscopy. In chemical reactions involving rapid and simultaneous functional group transformations and complex reaction mixtures, however, the spectroscopic signals are often ambiguous due to overlapping bands, shifting peaks and changing baselines. The univariate analysis of individual absorbance signals is hence often only of limited use. In contrast, batch modelling based on the multivariate analysis of the time course of principal components (PCs) derived from the reaction spectra provides a more efficient tool for real time monitoring. In batch modelling, not only single absorbance bands are used but information over a broad range of wavelengths is extracted from the evolving spectral fingerprints and used for analysis. Thereby, process control can be based on numerous chemical and morphological changes taking place during synthesis. “Bad” (or abnormal) batches can quickly be distinguished from “normal” ones by comparing the respective reaction trajectories in real time. In this work, FTIR spectroscopy was combined with multivariate data analysis for the in-line process characterization and batch modelling of polysiloxane formation. The synthesis was conducted under different starting conditions using various reactant concentrations. The complex spectral information was evaluated using chemometrics (principal component analysis, PCA). Specific spectral features at different stages of the reaction were assigned to the corresponding reaction steps. Reaction trajectories were derived based on batch modelling using a wide range of wavelengths. Subsequently, complexity was reduced again to the most relevant absorbance signals in order to derive a concept for a low-cost process spectroscopic set-up which could be used for real-time process monitoring and reaction control.
Allyls
(2014)
This chapter addresses the importance and usage of the commercially low volume thermoset plastics group known as allyls. The three significant sub-elements of this group are poly(diallylphthalates), poly(diallylisophthalates), and poly(allyldiglycol carbonate). Chemistry, processing, and properties are also described. Allyl polymers are synthesized by radical polymerizations of allyl monomers that usually do not produce high-molecular-mass macromolecules. Therefore, only a few specific monomers can produce thermosetting materials. Diallyldiglycolcarbonate (CR-39) and diallylphthalates are the most significant examples that have considerably improved our everyday life.
Allyls
(2022)
This chapter addresses the importance and usage of the commercially low-volume thermoset plastics group known as allyls. The three significant subelements of this group are poly(diallylphthalates), poly(diallylisophthalates), and poly(allyldiglycol carbonate). Chemistry, processing, and properties are also described. Allyl polymers are synthesized by radical polymerizations of allyl monomers that usually do not produce high-molecular-mass macromolecules. Therefore only a few specific monomers can produce thermosetting materials. Diallyldiglycolcarbonate (CR-39) and diallylphthalates are the most significant examples that have considerably improved our everyday life.
Porous silica materials are often used for drug delivery. However, systems for simultaneous delivery of multiple drugs are scarce. Here we show that anisotropic and amphiphilic dumbbell core–shell silica microparticles with chemically selective environments can entrap and release two drugs simultaneously. The dumbbells consist of a large dense lobe and a smaller hollow hemisphere. Electron microscopy images show that the shells of both parts have mesoporous channels. In a simple etching process, the properly adjusted stirring speed and the application of ammonium fluoride as etching agent determine the shape and the surface anisotropy of the particles. The surface of the dense lobe and the small hemisphere differ in their zeta potentials consistent with differences in dye and drug entrapment. Confocal Raman microscopy and spectroscopy show that the two polyphenols curcumin (Cur) and quercetin (QT) accumulate in different compartments of the particles. The overall drug entrapment efficiency of Cur plus QT is high for the amphiphilic particles but differs widely between Cur and QT compared to controls of core–shell silica microspheres and uniformly charged dumbbell microparticles. Furthermore, Cur and QT loaded microparticles show different cancer cell inhibitory activities. The highest activity is detected for the dual drug loaded amphiphilic microparticles in comparison to the controls. In the long term, amphiphilic particles may open up new strategies for drug delivery.
Monodisperse polystyrene spheres are functional materials with interesting properties, such as high cohesion strength, strong adsorptivity, and surface reactivity. They have shown a high application value in biomedicine, information engineering, chromatographic fillers, supercapacitor electrode materials, and other fields. To fully understand and tailor particle synthesis, the methods for characterization of their complex 3D morphological features need to be further explored. Here we present a chemical imaging study based on three-dimensional confocal Raman microscopy (3D-CRM), scanning electron microscopy (SEM), focused ion beam (FIB), diffuse reflectance infrared Fourier transform (DRIFT), and nuclear magnetic resonance (NMR) spectroscopy for individual porous swollen polystyrene/poly (glycidyl methacrylate-co-ethylene di-methacrylate) particles. Polystyrene particles were synthesized with different co-existing chemical entities, which could be identified and assigned to distinct regions of the same particle. The porosity was studied by a combination of SEM and FIB. Images of milled particles indicated a comparable porosity on the surface and in the bulk. The combination of standard analytical techniques such as DRIFT and NMR spectroscopies yielded new insights into the inner structure and chemical composition of these particles. This knowledge supports the further development of particle synthesis and the design of new strategies to prepare particles with complex hierarchical architectures.
Comments on “Solubility parameter of chitin and chitosan”, Carbohydrate Polymers 36 (1998) 121–127
(2017)
Results on the solubility parameters of chitin and chitosan presented in the paper DOI: 10.1016/S0144-8617(98)00020-4 were recalculated and data evaluation was redone. A number of misprints, erroneous calculations and data evaluations were found with respect to Hansen as well as total solubility parameters as derived according to group contribution methods by Hoftyzer-Van Krevelen and Hoy’s system. Revised numerical data are presented.
Comparative analysis of the chemical and rheological curing kinetics of formaldehyde-based wood adhesives is crucial for assessing their respective performance. Differential scanning calorimetry (DSC) and rheometry are the conventional techniques used for monitoring the curing processes leading to crosslinking polymerization of the adhesives. However, the direct comparison of these techniques is inappropriate due to the intrinsic differences in their underlying procedures. To address this challenge, the two adhesive samples were sequentially cured, firstly with rheometry and followed by DSC. The observed higher curing degree in the subsequent DSC procedure underpins the incomplete curing of the samples during initial rheometry. Furthermore, the comparative assessment of the activation energies, molar ratios, and active groups of the two adhesives highlights the importance of the pre-exponential factor in addition to the activation energies, as it attributes to the probability of active groups coinciding at the appropriate spatial arrangement.
Cross-linked thermoplastics
(2022)
Cross-linked thermoplastics represent an important class of materials for numerous applications such as heat-shrinkable tubing, rotational molded parts, and polyolefin foams. By cross-linking olefins, their mechanical performance can be significantly enhanced. This chapter covers the three main methods for the cross-linking of thermoplastics: radiation cross-linking, chemical cross-linking with organic peroxides, and cross-linking using silane-grafting agents. It also considers the major effects of the cross-linking procedure on the performance of the thermoplastic materials discussed.
Crosslinked thermoplastics
(2014)
Cross-linked thermoplastics represent an important class of materials for numerous applications such as heat-shrinkable tubing, rotational molded parts, and polyolefin foams. By cross-linking olefins, their mechanical performance can be significantly enhanced. This chapter covers the three main methods for the cross-linking of thermoplastics: radiation cross-linking, chemical cross-linking with organic peroxides, and cross-linking using silane-grafting agents. It also considers the major effects of the cross-linking procedure on the performance of the thermoplastic materials discussed.
We report on the cure characterization, based on inline monitoring of the dielectric parameters, of a commercially available epoxy phenol resin molding compound with a high glass transition temperature (>195 °C), which is suitable for the direct packaging of electronic components. The resin was cured under isothermal temperatures close to general process conditions (165–185 °C). The material conversion was determined by measuring the ion viscosity. The change of the ion viscosity as a function of time and temperature was used to characterize the cross-linking behavior, following two separate approaches (model based and isoconversional). The determined kinetic parameters are in good agreement with those reported in the literature for EMCs and lead to accurate cure predictions under process-near conditions. Furthermore, the kinetic models based on dielectric analysis (DEA) were compared with standard offline differential scanning calorimetry (DSC) models, which were based on dynamic measurements. Many of the determined kinetic parameters had similar values for the different approaches. Major deviations were found for the parameters linked to the end of the reaction where vitrification phenomena occur under process-related conditions. The glass transition temperature of the inline molded parts was determined via thermomechanical analysis (TMA) to confirm the vitrification effect. The similarities and differences between the resulting kinetics models of the two different measurement techniques are presented and it is shown how dielectric analysis can be of high relevance for the characterization of the curing reaction under conditions close to series production.