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The powder coating of veneered particle boards by the sequence electrostatic powder application -powder curing via hot pressing is studied in order to create high gloss surfaces. To obtain an appealingaspect, veneer Sheets were glued by heat and pressure on top of particle boards and the resulting surfaceswere used as carrier substrates for powder coat finishing. Prior to the powder coating, the veneeredparticle board surfaces were pre-treated by sanding to obtain good uniformity and the boards werestored in a climate chamber at controlled temperature and humidity conditions to adjust an appropriate electrical surface resistance. Characterization of surface texture was done by 3D microscopy. The surfaceelectrical resistance was measured for the six veneers before and after their application on the particleboard surface. A transparent powder top-coat was applied electrostatically onto the veneered particleboard surface. Curing of the powder was done using a heated press at 130◦C for 8 min and a smooth, glossy coating was obtained on the veneered surfaces. By applying different amounts of powder thecoating thickness could be varied and the optimum amount of powder was determined for each veneer type.
In the powder coating of veneered particle boards the highly reactive hybrid epoxy/polyester powder transparent Drylac 530 Series from TIGER Coatings GmbH & Co. KG, Wels, Austria was used. Curing is accelerated by a mixture of catalysts reaching curing times of 3 min at 150 °C or 5 min at 135 °C which allows for energy and time savings making Drylac Series 530 powder suitable for the coating of temperaturesensitive substrates such as MDF and wood.
Decorative laminates based on melamine formaldehyde (MF) resin impregnated papers are used at great extent for surface finishing of engineered wood that is used for furniture, kitchen, and working surfaces, flooring and exterior cladding. In all these applications, optically flawless appearance is a major issue. The work described here is focused on enhancing the cleanability and antifingerprint properties of smooth, matt surface-finished melamine-coated particleboards for furniture fronts, without at the same time changing or deteriorating other important surface parameters such as hardness, roughness or gloss. In order to adjust the surface polarity of a low pressure melamine film, novel interface-active macromolecular compounds were prepared and tested for their suitability as an antifingerprint additive. Two hydroxy-functional surfactants (polydimethysiloxane, PDMS-OH and perfluoroether, PF-OH) were oxidized under mild conditions to the corresponding aldehydes (PDMS-CHO and PF-CHO) using a pyridinium chlorochromate catalyst. With the most promising oxidized polymeric additive, PDMS-CHO, the contact angles against water, n-hexadecane, and squalene increased from 79.8°, 26.3° and 31.4° for the pure MF surface to 108.5°, 54.8°, and 59.3°, respectively, for the modified MF surfaces. While for the laminated MF surface based on the oxidized fluoroether the gloss values were much higher than required, for the surfaces based on oxidized polydimethylsiloxane the technological values as well as the lower gloss values were in agreement with the requirements and showed much improved surface cleanability, as was also confirmed by colorimetric measurements.
Here, we report the continuous peroxide-initiated grafting of vinyltrimethoxysilane (VTMS) onto a standard polyolefin by means of reactive extrusion to produce a functionalized liquid ethylene propylene copolymer (EPM). The effects of the process parameters governing the grafting reaction and their synergistic interactions are identified, quantified and used in a mathematical model of the extrusion process. As process variables the VTMS and peroxide concentrations and the extruder temperature setting were systematically studied for their influence on the grafting and the relative grafting degree using a face-centered central composite design (FCD). The grafting degree was quantified by 1H NMR spectroscopy. Response surface methodology (RSM) was used to calculate the most efficient grafting process in terms of chemical usage and graft yield. With the defined processing window, it was possible to make precise predictions about the grafting degree with at the same time highest possible relative degree of grafting.
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.
For optimization of production processes and product quality, often knowledge of the factors influencing the process outcome is compulsory. Thus, process analytical technology (PAT) that allows deeper insight into the process and results in a mathematical description of the process behavior as a simple function based on the most important process factors can help to achieve higher production efficiency and quality. The present study aims at characterizing a well-known industrial process, the transesterification reaction of rapeseed oil with methanol to produce fatty acid methyl esters (FAME) for usage as biodiesel in a continuous micro reactor set-up. To this end, a design of experiment approach is applied, where the effects of two process factors, the molar ratio and the total flow rate of the reactants, are investigated. The optimized process target response is the FAME mass fraction in the purified nonpolar phase of the product as a measure of reaction yield. The quantification is performed using attenuated total reflection infrared spectroscopy in combination with partial least squares regression. The data retrieved during the conduction of the DoE experimental plan were used for statistical analysis. A non-linear model indicating a synergistic interaction between the studied factors describes the reactor behavior with a high coefficient of determination (R²) of 0.9608. Thus, we applied a PAT approach to generate further insight into this established industrial process.
High-performance liquid chromatography is one of the most important analytical tools for the identification and separation of substances. The efficiency of this method is largely determined by the stationary phase of the columns. Although monodisperse mesoporous silica microspheres (MPSM) represent a commonly used material as stationary phase their tailored preparation remains challenging. Here we report on the synthesis of four MPSMs via the hard template method. Silica nanoparticles (SNPs) which form the silica network of the final MPSMs were generated in situ from tetraethyl orthosilicate (TEOS) in the presence of (3-aminopropyl) triethoxysilane (APTES) functionalized p(GMA-co-EDMA) as hard template. Methanol, ethanol, 2-propanol, and 1-butanol were applied as solvents to control the size of the SNPs in the hybrid beads (HB). After calcination, MPSMs with different sizes, morphology and pore properties were obtained and characterized by scanning electron microscopy, nitrogen adsorption and desorption measurements, thermogravimetric analysis, solid state NMR and DRIFT IR spectroscopy. Interestingly, the 29Si NMR spectra of the HBs show T and Q group species which suggests that there is no covalent linkage between the SNPs and the template. The MPSMs were functionalized with trimethoxy (octadecyl) silane and used as stationary phases in reversed-phase chromatography to separate a mixture of eleven different amino acids. The separation characteristics of the MPSMs strongly depend on their morphology and pore properties which are controlled by the solvent during the preparation of the MPSMs. Overall, the separation behavior of the best phases is comparable with those of commercially available columns. The phases even achieve faster separation of the amino acids without loss of quality.
Mesoporous silica microspheres (MPSMs) find broad application as separation materials in high liquid chromatography (HPLC). A promising preparation strategy uses p(GMA-co-EDMA) as hard templates to control the pore properties and a narrow size distribution of the MPMs. Here six hard templates were prepared which differ in their porosity and surface functionalization. This was achieved by altering the ratio of GMA to EDMA and by adjusting the proportion of monomer and porogen in the polymerization process. The various amounts of GMA incorporated into the polymer network of P1-6 lead to different numbers of tetraethylene pentamine in the p(GMA-co-EDMA) template. This was established by a partial least squares regression (PLS-R) model, based on FTIR spectra of the templates. Deposition of silica nanoparticles (SNP) into the template under Stoeber conditions and subsequent removal of the polymer by calcination result in MPSM1-6. The size of the SNPs and their incorporation depends on the pore parameters of the template and degree of TEPA functionalization. Moreover, the incorporated SNPs construct the silica network and control the pore parameters of the MPSMs. Functionalization of the MPSMs with trimethoxy (octadecyl) silane allows their use as a stationary phase for the separation of biomolecules. The pore characteristics and the functionalization of the template determine the pore structure of the silica particles and, consequently, their separation properties.
The hard template method for the preparation of monodisperse mesoporous silica microspheres (MPSMs) has been established in recent years. In this process, in situ-generated silica nanoparticles (SNPs) enter the porous organic template and control the size and pore parameters of the final MPSMs. Here, the sizes of the deposited SNPs are determined by the hydrolysis and condensation rates of different alkoxysilanes in a base catalyzed sol–gel process. Thus, tetramethyl orthosilicate (TMOS), tetraethyl orthosilicate (TEOS), tetrapropyl orthosilicate (TPOS) and tetrabutyl orthosilicate (TBOS) were sol–gel processed in the presence of amino-functionalized poly (glycidyl methacrylate-co-ethylene glycol dimethacrylate) (p(GMA-co-EDMA)) templates. The size of the final MPSMs covers a broad range of 0.5–7.3 µm and a median pore size distribution from 4.0 to 24.9 nm. Moreover, the specific surface area can be adjusted between 271 and 637 m2 g−1. Also, the properties and morphology of the MPSMs differ according to the SNPs. Furthermore, the combination of different alkoxysilanes allows the individual design of the morphology and pore parameters of the silica particles. Selected MPSMs were packed into columns and successfully applied as stationary phases in high-performance liquid chromatography (HPLC) in the separation of various water-soluble vitamins.
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.
Clay minerals play an increasingly important role as functional fillers and reinforcing materials for clay polymer nanocomposites (CPN) in advanced applications. Among the prerequisites necessary for polymer improvement by clay minerals are homogeneous and stable Distribution of the clay mineral throughout the CPN, good compatibility of the reinforcement with the Matrix component and suitable processability. Typically, clay minerals are surface-modified with organic interface active compounds like detergents or silanes to obtain favorable properties as filler. They are incorporated into the polymer matrix using manufacturing Equipment like extruders, batch reactors or other mixing machines. In order for the surface modification to survive the stresses and strains during incorporation, the modified clay minerals must display sufficient thermal and mechanical stability to retain the compatibilizing effect. In the present study, thermogravimetry was used in combination with isoconversional kinetic analysis to determine the thermal stability of a silane-modified clay mineral based on bentonite. These findings were compared with the stability of the same clay mineral that was only surfactant-modified. It was found that silane modification leads to significantly improved thermal stability, which depends strongly on the type of silane employed.
Recycling of poly(ethylene terephthalate) (PET) is of crucial importance, since worldwide amounts of PETwaste increase rapidly due to its widespread applications. Hence, several methods have been developed, like energetic, material, thermo-mechanical and chemical recycling of PET. Most frequently, PET-waste is incinerated for energy recovery, used as additive in concrete composites or glycolysed to yield mixtures of monomers and undefined oligomers. While energetic and thermo-mechanical recycling entail downcycling of the material, chemical recycling requires considerable amounts of chemicals and demanding processing steps entailing toxic and ecological issues. This review provides a thorough survey of PET-recycling including energetic, material, thermo-mechanical and chemical methods. It focuses on chemical methods describing important reaction parameters and yields of obtained reaction products. While most methods yield monomers, only a few yield undefined low molecular weight oligomers for impaired applications (dispersants or plasticizers). Further, the present work presents an alternative chemical recycling method of PET in comparison to existing chemical methods.
The intelligent recycling of plastics waste is a major concern. Because of the widespread use of polyethylene terephtalate, considerable amounts of PET waste are generated that are ideally re-introduced into the material cycle by generating second generation products without loss of materials performance. Chemical recycling methods are often expensive and entail environmentally hazardous by-products. Established mechanical methods generally provide materials of reduced quality, leading to products of lower quality. These drawbacks can be avoided by the development of new recycling methods that provide materials of high quality in every step of the production cycle. In the present work, oligomeric ethylene terephthalate with defined degrees of polymerization and defined molecular weight is produced by melt-mixing PET with different quantities of adipic acid as an alternative pathway of recycling PET with respect to conventional methods, offering ecofriendly and economical aspects. Additionally, block-copolyesters of defined block length are designed from the oligomeric products.
Ethylene terephthalate and ethylene naphthalate oligomers of defined degree of polymerization were synthesized via chemical recycling of the parent polymers. The oligomers were used as defined building blocks for the preparation of novel block-co-polyesters having tailored sequence compositions. The sequence lengths were systematically varied using Design of Experiments. The dispersive surface energy and the specific desorption energy of the co-polymers were determined by inverse gas chromatography. The study shows that polyethylene terephthalate-polyethylene naphthalate (PET-PEN) block-co-polyesters of defined sequence lengths can be prepared. Furthermore, the specific and dispersive surface energies of the obtained block-co-polyesters showed a linear dependence on the oligomer molecular weight and it was possible to regulate and control their interfacial properties. In contrast, with the corresponding random-block-co-polyesters no such dependence was found. The synthesized block-co-polyesters could be used as polymeric modifying agents for stabilizing PET-PEN polymer blends.
The interfacial compatibility between polymers and nanoclay fillers as well as the thermostability of both components are important characteristics for processing them into polymer composites. While the polymer component is often grafted using common polymerization reactions, the nanoclay component is usually surface modified by surfactant treatment to improve compatibility. In the present study, the polymer ethylene vinyl alcohol and a nanoclay filler based on natural bentonite are both surface modified by different silanes, 3-glycidoxypropyltrimethoxysilane and methacryloxymethyltrimethoxysilane and their interfacial properties are investigated by inverse gas chromatography. The silane-modified samples had improved interfacial properties as reflected by a significant increase in dispersive and specific surface energies. Lewis acidities were determined using chloroform and 1,4-dioxane as polar probes and showed a good match between polymer and nanofiller interfaces. Lewis acidity was generally lower after silane-modification. Silanization yielded increased thermal stability of the treated samples. Thus, silanization led to improved compatibility and enhanced thermal stability which facilitates further processing.
Powder coatings provide several advantages over traditional coatings: environmental friendliness, freedom of design, robustness and resistance of surfaces, possibility to seamlessly all-around coating, fast production process, cost-effectiveness. In the last years these benefits of the powder coating technology have been adopted from metal to heat-sensitive natural fibre/ wood based substrates (especially medium density fibre boards- MDF) used for interior furniture applications. Powder coated MDF furniture parts are gaining market share already in the classic furniture applications kitchen, bathroom, living and offices. The acceptance of this product is increasing as reflected by excellent growth rates and an increasing customer base. Current efforts of the powder coating industry to develop new powders with higher reactivity (i.e. lower curing temperatures and shorter curing times; e.g. 120°C/5min) will enable the powder coating of other heat-sensitive substrates like natural fibre composites, wood plastic composites, light weight panels and different plastics in the future. The coating could be applied and cured by the conventional powder coating process (electrostatic application, and melting and curing in an IR-oven) or by a new powder coating procedure based on the in-mould-coating (IMC) technique which is already established in the plastic industry. Extra value could be added in the future by the functional powder toner printing of powder coated substrates using the electrophotographic printing technology, meeting the future demand of both individualization of the furniture part surface by applying functional 3D textures and patterns and individually created coloured images and enabling shorter delivery times for these individualized parts. The paper describes the distinctiveness of powder coating on natural fibre/ wood based substrates, the requirements of the substrate and the coating powder.
Despite the significant potential offered by the powder coating process for finishing wood-based materials, until now it has been used almost exclusively for coating Medium Density Fiber Board (MDF). A research project aims to develop processes and substrate materials that will allow lightweight boards to be powder coated.
The powder coating of wood products as an emerging environmentally sustainable coating technology holds promise in terms of novel product quality features for engineered wood like medium-density fiberboards (MDFs). However, one major limitation currently impeding widespread application of powder coating technology is the availability of MDF panels that are suitable for this process. Typically, special-grade MDF panels are required that are more costly than standard-grade MDF panels to provide reliable coating quality, which makes powder coating economically unattractive for many users. Methods are needed that allow extending the range of available MDF grades. In the present study, three surface pretreatment approaches for MDFs were studied to increase the processability of standard-grade MDF in the powder coating process: atmospheric plasma pretreatment, infrared irradiation, and moisture equilibration in a climate chamber prior to electrostatic powder application. While atmospheric plasma treatment had no beneficial effect on the use of standard-grade MDF panels, both infrared preheating and preconditioning of the panels under controlled temperature–humidity conditions demonstrated that the range of MDF panels suitable for powder coating can be significantly extended by appropriate selection of the pretreatment procedure.
Processing
(2014)
In this chapter, some relevant aspects and illustrative examples of online monitoring tools as the basis for process control in the manufacturing and processing of thermosetting resins are briefly discussed. In principle, any chemical or physical information made accessible by sensors can be used for online monitoring of resin formation, resin location in the mold, and resin cure. For instance, changes in the flow properties of the reaction mixture are often routinely recorded in dependence of the reaction time during resin synthesis as a measure for the degree of conversion of raw materials into macromolecules or oligomers by applying rheometry in an in-process environment. Typically, a small sample of the reaction mixture is by-passed, subjected to rheological measurement, and re-introduced into the bulk reactor. In a similar way, pH measurements, turbidimetric measurements, or other analyses are performed. Although rheometry may not always be suitable for following resin cure (especially in cases where there is a very rapid increase in viscosity after initiation of the cure), [1] naturally, the method can in principle also be used in the subsequent processing of the thermosets, for instance in the curing of wood glue applied to wood specimen [2]. Similarly, pH changes during thermoset curing can be followed. Hence, an encyclopedic and comprehensive approach to present process control methods would systematically proceed according to the involved physical measurement principle. However, since only a very Brief sketch of means for monitoring thermoset processing can be given here, only a small, personally biased selection of important methods and application examples is addressed in the following sections. These examples hopefully illustrate some of the general strategies and solutions to problems that are typically encountered when processing thermosets.
Cyanate esters
(2014)
Cyanate ester resins are an important class of thermosetting compounds that have experienced an ever-increasing interest as matrix systems for advanced polymer composite materials, which among other applications, are especially suitable for highly demanding functions in the aerospace or microelectronics industries. Other names for cyanate ester resins are cyanate resins, cyanic esters, or triazine resins. The various types of cyanate ester monomers share the aOCN functional group that trimerizes in the course of resin formation to yield a highly branched heterocyclic polymeric network based on the substituted triazine core structure. The basic reaction sequence leading to the typical cyanate ester polymer molecule is depicted in Figure 11.1. The curing reaction may take place with or without catalyst.