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Here, we report the mechanical and water sorption properties of a green composite based on Typha latifolia fibres. The composite was prepared either completely binder-less or bonded with 10% (w/w) of a bio-based resin which was a mixture of an epoxidized linseed oil and a tall-oil based polyamide. The flexural modulus of elasticity, the flexural strength and the water absorption of hot pressed Typha panels were measured and the influence of pressing time and panel density on these properties was investigated. The cure kinetics of the biobased resin was analyzed by differential scanning calorimetry (DSC) in combination with the iso-conversional kinetic analysis method of Vyazovkin to derive the curing conditions required for achieving completely cured resin. For the binderless Typha panels the best technological properties were achieved for panels with high density. By adding 10% of the binder resin the flexural strength and especially the water absorption were improved significantly.
Powder coating of engineered wood panels such as medium density fibreboards (MDF) is gaining industrial interest due to ecological and economic advantages of powder coating technology. For transferring powder coating technology to temperature-sensitive substrates like MDF, a thorough understanding of the melting, flowing and curing behaviour of the used low-bake resins is required. In the present study, thermo-analysis in combination with iso-conversional kinetic data analysis as well as rheometry is applied to characterise the properties of an epoxy-based powder coating. Neat resin and cured powder coating films are examined in order to define an ideal production window within which the resin is preferably applied and processed to yield satisfactory surface performance on the one hand and without exposing the carrier MDF too high a temperature load on the other hand to prevent the panel from deteriorating in mechanical strength. In order to produce powder coated films of high surface gloss – a feature that has not yet successfully been realized on MDF with powder coatings – a new curing technology, in-mould surface finishing, has been applied.
Hardboards (HBs) (wet-process high-density fibreboards) were made in an industrial trial using a binder system consisting of cationic mimosa tannin and laccase or just cationic tannin without any thermosetting adhesive. The boards displayed superior mechanical strength compared to reference boards made with phenol–formaldehyde, easily exceeding the European standards for general-purpose HBs. The thickness swell of most of the boards was slightly greater than the standards would allow, so some optimisation is required in this area. The improved board properties appear to be mainly associated with ionic interactions involving quaternary amino groups in cationic tannin and negatively charged wood fibres rather than to cross-linking of fibres via laccase-assisted formation and coupling of radicals in tannin and fibre lignin.
Melamine–formaldehyde (MF) resins are widely used as adhesives and finishing materials in the wood industry. During resin cure, either methylene ether or methylene bridges are formed, leading to the formation of a three‐dimensional resin network. Not only the curing degree, but also the chemical species present in the cured resin determine the quality of the final product. Analytical methods allowing a detailed investigation of network formation are of great benefit to manufacturers. In the present work, resin cure of an MF precondensate is studied at different temperatures (100–200 °C) without considering the initial pH as a factor. Isoconversional kinetic analysis based on exothermal curing enthalpies enables calculation of the crosslinking degree at a given time/temperature regime. A semiquantitative determination of the chemical groups present is performed based on solid‐state nuclear magnetic resonance data. Fourier transform infrared spectroscopy has shown to be a fast and reliable analytical tool with high sensitivity toward functional groups and with great potential for at‐line process control.
The isothermal curing of melamine resin is investigated by in-line infrared spectroscopy at different temperatures. The infrared spectra are decomposed into time courses of characteristic spectral patterns using Multivariate Curve Resolution (MCR). It was found that depending on the applied curing temperature, melamine films with different spectral fingerprints and correspondingly different chemical network structures are formed. The network structures of fully cured resin films are specific for the applied curing temperatures used and cannot simply be compensated by changes in the curing time. For industrial curing processes, this means that cure temperature is the main system determining factor at constant M:F ratio. However, different MF resin networks can be specifically obtained from one and the same melamine resin by suitable selection of the curing time and temperatures profiles to design resin functionality. The spectral fingerprints after short curing time as well as after long curing time reflect the fundamental differences in the thermoset networks that can be obtained with industrial short-cycle and multi-daylight presses.
Here, we study resin cure and network formation of solid melamine formaldehyde pre-polymer over a large temperature range viadynamic temperature curing profiles. Real-time infrared spectroscopy is used to analyze the chemical changes during network formation and network hardening. By applying chemometrics (multivariate curve resolution,MCR), the essential chemical functionalities that constitute the network at a given stage of curing are mathematically extracted and tracked over time. The three spectral components identified by MCR were methylol-rich, ether linkages-rich and methylene linkages-rich resin entities. Based on dynamic changes of their characteristic spectral patterns in dependence of temperature, curing is divided into five phases: (I) stationary phase with free methylols as main chemical feature, (II) formation of flexible network cross-linked by ether linkages, (III) formation of rigid, ether-cross-linked network, (IV) further hardening via transformation of methylols and ethers into methylene-cross-linkages, and (V) network consolidation via transformation of ether into methylene bridges. The presented spectroscopic/chemometric approach can be used as methodological basis for the functionality design of MF-based surface films at the stage of laminate pressing, i.e., for tailoring the technological property profile of cured MF films using a causal understanding of the underlying chemistry based on molecular markers and spectroscopic fingerprints.
During curing of thermosetting resins the technologically relevant properties of binders and coatings develop. However, curing is difficult to monitor due to the multitude of chemical and physical processes taking place. Precise prediction of specific technological properties based on molecular properties is very difficult. In this study, the potential of principal component analysis (PCA) and principal component regression (PCR) in the analysis of Fourier transform infrared (FTIR) spectra is demonstrated using the example of melamine-formaldehyde (MF) resin curing in solid state. FTIR/PCA-based reaction trajectories are used to visualize the influence of temperature on isothermal cure. An FTIR/PCR model for predicting the hydrolysis resistance of cured MF resin from their spectral fingerprints is presented which illustrates the advantages of FTIR/PCR compared to the combination differential scanning calorimetry/isoconversional kinetic analysis. The presented methodology is transferable to the curing reactions of any thermosetting resin and can be applied to model other technologically relevant final properties as well.
Natural wood colors occur within a wide range from almost white (e.g., white poplar), various yellowish, reddish, and brownish hues to almost black (e.g., ebony). The intrinsic color of wood is basically defined by its chemical composition. However, other factors such as specific anatomical formations or physical properties further affect the optical impression. Starting with the chemical composition of wood and anatomical basics, wood color and its modifications are discussed in this chapter. The classic method of coloring or re-coloring wood-based material surfaces is the application of a coating containing appropriate dyes or pigments. Different concepts for wood coating and coloration are presented. Another method used dyes for coloration of the wood structure. As alternative techniques, physical methods, for example, drying, steaming, ammoniation, bleaching, enzyme treatment, as well as treatment with electromagnetic irradiation (e.g., UV), are explained in this chapter.
Metalworking fluids (MWFs) are widely used to cool and lubricate metal workpieces during processing to reduce heat and friction. Extending a MWF’s service life is of importance from both economical and ecological points of view. Knowledge about the effects of processing conditions on the aging behavior and reliable analytical procedures are required to properly characterize the aging phenomena. While so far no quantitative estimations of ageing effects on MWFs have been described in the literature other than univariate ones based on single parameter measurements, in the present study we present a simple spectroscopy-based set-up for the simultaneous monitoring of three quality parameters of MWF and a mathematical model relating them to the most influential process factors relevant during use. For this purpose, the effects of MWF concentration, pH and nitrite concentration on the droplet size during aging were investigated by means of a response surface modelling approach. Systematically varied model MWF fluids were characterized using simultaneous measurements of absorption coefficients µa and effective scattering coefficients µ’s. Droplet size was determined via dynamic light scattering (DLS) measurements. Droplet size showed non-linear dependence on MWF concentration and pH, but the nitrite concentration had no significant effect. pH and MWF concentration showed a strong synergistic effect, which indicates that MWF aging is a rather complex process. The observed effects were similar for the DLS and the µ’s values, which shows the comparability of the methodologies. The correlations of the methods were R2c = 0.928 and R2P = 0.927, as calculated by a partial least squares regression (PLS-R) model. Furthermore, using µa, it was possible to generate a predictive PLS-R model for MWF concentration (R2c = 0.890, R2P = 0.924). Simultaneous determination of the pH based on the µ’s is possible with good accuracy (R²c = 0.803, R²P = 0.732). With prior knowledge of the MWF concentration using the µa-PLS-R model, the predictive capability of the µ’s-PLS-R model for pH was refined (10 wt%: R²c = 0.998, R²p = 0.997). This highlights the relevance of the combined measurement of µa and µ’s. Recognizing the synergistic nature of the effects of MWF concentration and pH on the droplet size is an important prerequisite for extending the service life of an MWF in the metalworking industry. The presented method can be applied as an in-process analytical tool that allows one to compensate for ageing effects during use of the MWF by taking appropriate corrective measures, such as pH correction or adjustment of concentration.
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.
Functionalised particles are highly requested in materials research, as they can be used as vital components in many advanced applications such as smart materials, functional coatings, drug carrier systems or adsorption materials. In this study, furan-functionalised melamine-formaldehyde (MF) particles were successfully prepared for the first time using an organic sol-gel process. Commercially available 2-Aminomethylfuran (AMF) and 2-Aminomethyl-5-methylfuran (AMMF) were used as modifying agents. In the isolated polymer particles, a melamine (M) to modifying agent ratio of M:AMF mol/mol 2.04:1 and M:AMMF ratio of mol/mol 1.25:1 was used. The obtained particles were isolated in various centrifugation and re-dispersion cycles and analysed using ATR-FT-IR, Raman and solid state 13C NMR spectroscopy, TGA, SEM and DSC measurements. Upon functionalisation the size of the MF particles increased (MF 1.59 µm, 27% CV (coefficient of variation); MF-AMF 2.56 µm, 25% CV; MF-AMMF 2.20 µm, 35% CV). DSC measurements showed that another type of exothermic residual reactivity besides condensation-based curing takes place with the furan-modified particles that is not related to the liberation of volatile compounds. The newly obtained particles are able to undergo Diels-Alder reactions with maleimide groups. The characteristic IR and Raman absorbance bands of the reaction products after the particles were reacted with 4,4′-Diphenylmethanebismaleimide reagent confirm the formation of a Diels-Alder adduct.
The data present in this article affords insides in the characterization of a newly described bi-functional furan-melamine monomer, which is used for the production of monodisperse, furan-functionalized melamine formaldehyde particles. In the related research article Urdl et al., 2019 data interpretations can be found. The furan functionalization of particles is necessary to perform reversible Diels-Alder reactions with maleimide (BMI) crosslinker to form thermoreversible network systems. To understand the reaction conditions of Diels Alder (DA) reaction with a Fu-Mel monomer and a maleimide crosslinker, model DA reaction were performed and evaluated using dynamic FT-IR measurements. During retro Diels-Alder (rDA) reactions of the monomer system, it was found out that some side reaction occurred at elevated temperatures. The data of evaluating the side reaction is described in one part of this manuscript. Additional high resolution SEM images of Fu Mel particles are shown and thermoreversible particle networks with BMI2 are shown. The data of different Fu-Mel particle networks with maleimide crosslinker are presented. Therefore, the used maleimide crosslinker with different spacer lengths were synthesized and the resulting networks were analyzed by ATR-FT-IR, SEM and DSC.
The data presented in this article characterize the thermomechanical and microhardness properties of a novel melamine-formaldehyde resin (MF) intended for the use as a self-healing surface coating. The investigated MF resin is able to undergo reversible crosslinking via Diels Alder reactive groups. The microhardness data were obtained from nanoindentation measurements performed on solid resin film samples at different stages of the self-healing cycle. Thermomechanical analysis was performed under dynamic load conditions. The data provide supplemental material to the manuscript published by Urdl et al. 2020 (https://doi.org/10.1016/j.eurpolymj.2020.109601) on the self-healing performance of this resin, where a more thorough discussion on the preparation, the properties of this coating material and its application in impregnated paper-based decorative laminates can be found.
The self-healing effect of melamine-based surfaces, triggered by temperature, was investigated. The temperature triggered reversible healing chemistry, on which the self-healing effect is based, was the Diels-Alder (DA) reaction between furan and malemeide groups. Melamine-furan containing building blocks were connected by multi-functional maleimide crosslinker via a Diels-Alder (DA) reaction to giva a DA adduct. The DA adduct was then reacted with formaldehyde to form a network by conventional condensation reaction of melamine amino groups with formaldehyde. The obtained resin was characterised and used for the impregnation of paper. Impregnated papers and neat resin werde used to perform scratch-healing tests and mechanical analysis of the novel coating system.
Homogeneous and monodispersed furan functionalised melamine-formaldehyde particles were produced. As a precursor, 2-chloro-1,3,5-triazine-2,4-diamine (Mel) was selectively substituted with 2-aminomethyl furan (Fu) units in a convenient one step reaction. The pure reaction product Fu-Mel, which was used without further purification, was reacted with formaldehyde by conventional sol-gel condensation in aqueous medium to yield chemically homogenous, spherically shaped and monodispersed particles. The particles were analysed using ATR-FT-IR, Raman, 1H and 13C NMR spectroscopy, TGA, SEM and DSC measurements. The reactivity of the furan groups located at the particle surface was studied by performing a thermoreversible Diels-Alder cycloaddition reaction with bis-maleimide coupling agents. The formed networks showed thermoreversible behaviour, which was characterised by dynamic IR and DSC measurements.
Structural and functional thermosetting composite materials are exposed to different kinds of stress which can damage the polymer matrix, thus impairing the intended properties. Therefore, self-healing materials have attracted the attention of many research groups over the last decades in order to provide satisfactory material properties and outstanding product durability. The present article provides a critical overview of promising self-healing strategies for crosslinked thermoset polymers. It is organized in two parts: an overview about the different approaches to self-healing is given in the first part, whereas the second part focuses on the specific chemistries of the main strategies to achieve self-healing through crosslinking. It is attempted to provide a comprehensive discussion of different approaches which are described in the scientific literature. By comparison of the advantages and disadvantages, the authors wish to provide helpful insights on the assessment of the potential to transfer the extensive present knowledge about self-healing materials and methods to surface varnishing thermoset coatings.
We present the modification of ethylene-propylene rubber (EPM) with vinyltetra-methydisiloxane (VTMDS) via reactive extrusion to create a new silicone-based material with the potential for high-performance applications in the automotive, industrial and biomedical sectors. The radical-initiated modification is achieved with a peroxide catalyst starting the grafting reaction. The preparation process of the VTMDS-grafted EPM was systematically investigated using process analytical technology (in-line Raman spectroscopy) and the statistical design of experiments (DoE). By applying an orthogonal factorial array based on a face-centered central composite experimental design, the identification, quantification and mathematical modeling of the effects of the process factors on the grafting result were undertaken. Based on response surface models, process windows were defined that yield high grafting degrees and good grafting efficiency in terms of grafting agent utilization. To control the grafting process in terms of grafting degree and grafting efficiency, the chemical changes taking place during the modification procedure in the extruder were observed in real-time using a spectroscopic in-line Raman probe which was directly inserted into the extruder. Successful grafting of the EPM was validated in the final product by 1H-NMR and FTIR spectroscopy.
Thermoplastic polymers like ethylene-octene copolymer (EOC) may be grafted with silanes via reactive extrusion to enable subsequent crosslinking for advanced biomaterials manufacture. However, this reactive extrusion process is difficult to control and it is still challenging to reproducibly arrive at well-defined products. Moreover, high grafting degrees require a considerable excess of grafting reagent. A large proportion of the silane passes through the process without reacting and needs to be removed at great expense by subsequent purification. This results in unnecessarily high consumption of chemicals and a rather resource-inefficient process. It is thus desired to be able to define desired grafting degrees with optimum grafting efficiency by means of suitable process control. In this study, the continuous grafting of vinyltrimethoxysilane (VTMS) on ethylene-octene copolymer (EOC) via reactive extrusion was investigated. Successful grafting was verified and quantified by 1H-NMR spectroscopy. The effects of five process parameters and their synergistic interactions on grafting degree and grafting efficiency were determined using a face-centered experimental design (FCD). Response surface methodology (RSM) was applied to derive a causal process model and define process windows yielding arbitrary grafting degrees between <2 and >5% at a minimum waste of grafting agent. It was found that the reactive extrusion process was strongly influenced by several second-order interaction effects making this process difficult to control. Grafting efficiencies between 75 and 80% can be realized as long as grafting degrees <2% are admitted.
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.
This article provides a general overview of the most promising candidates of bio based materials and deals with the most important issues when it comes to their incorporation into PF resins. Due to their abundance on Earth, much knowledge of lignin-based materials has already been gained and uses of lignin in PF resins have been studied for many decades. Other natural polyphenols that are less frequently considered for impregnation are covered as well, as they do also possess some potential for PF substitution.
Impregnated paper-based decorative laminates prepared from lignin-substituted phenolic resins
(2020)
High Pressure Laminates (HPL) panels consist of stacks of self-gluing paper sheets soaked with phenol-formaldehyde (PF) resins. An important requirement for such PFs is that they must rapidly penetrate and saturate the paper pores. Partially substituting phenol with bio-based phenolic chemicals like lignin changes the physico-chemical properties of the resin and affects its ability to penetrate the paper. In this study, PF formulations containing different proportions of lignosulfonate and kraft lignin were used to prepare paper-based laminates. The penetration of a Kraft paper sheet was characterized by a recently introduced, new device measuring the conductivity between both sides of the paper sheet after a drop of resin was placed on the surface and allowed to penetrate the sheet. The main target value measured was the time required for a specific resin to completely penetrate the defined paper sample (“penetration time”). This penetration time generally depends on the molecular weight distribution, the flow behavior and the polarity of the resin which in turn are dependent on the manufacturing conditions of the resin. In the present study, the influences of the three process factors: (1) type of lignin material used for substitution, (2) lignin modification by phenolation and (3) degree of phenol substitution on the penetration times of various lignin-phenolic hybrid impregnation resins were studied using a complete twolevel three-factorial experimental design. Thin laminates made with the resins diluted in methanol were mechanically tested in terms of tensile and flexural strains, and their cross-sections were studied by light microscopy.
Here, the effects of substituting portions of fossil-based phenol in phenol formaldehyde resin by renewable lignin from two different sources are investigated using a factorial screening experimental design. Among the resins consumed by the wood-based industry, phenolics are one of the most important types used for impregnation, coating or gluing purposes. They are prepared by condensing phenol with formaldehyde (PF). One major use of PF is as matrix polymer for decorative laminates in exterior cladding and wet-room applications. Important requirements for such PFs are favorable flow properties (low viscosity), rapid curing behavior (high reactivity) and sufficient self-adhesion capacity (high residual curing potential). Partially substituting phenol in PF with bio-based phenolic co-reagents like lignin modifies the physicochemical properties of the resulting resin. In this study, phenol-formaldehyde formulations were synthesized where either 30% or 50% (in weight) of the phenol monomer were substituted by either sodium lignosulfonate or Kraft lignin. The effect of modifying the lignin material by phenolation before incorporation into the resin synthesis was also investigated. The resins so obtained were characterized by Fourier Transform Infra-Red (FTIR) spectroscopy, Size Exclusion Chromatography (SEC), Differential Scanning Calorimetry (DSC), rheology, and measurements of contact angle and surface tension using the Wilhelmy plate method and drop shape analysis.
Impact of phenolic resin preparation on its properties and its penetration behavior in Kraft paper
(2018)
The core of decorative laminates is generally made of stacked Kraft paper sheets impregnated with a phenolic resin. As the impregnation process in industry is relatively fast, new methods need to be developed to characterize it for different paper-resin systems. Several phenolic resins were synthesized with the same Phenol:Formaldehyde ratio of 1:1.8 and characterized by Fourier Transform Infrared Spectrometry (FTIR) as well as Size-Exclusion Chromatography (SEC). In addition, their viscosities and surface tensions when diluted in methanol to 45% of solid content were measured. The capacity of each resin to penetrate a Kraft paper sheet was characterized using a new method, which measures the conductivities induced by the liquid resin crossing the paper substrate. With this method, crossing times could be measured with a good accuracy. Surprisingly, the results showed that the penetration time of the resin samples is not correlated to the viscosity values, but rather to the surface tension characteristics and the chemical characteristics of paper. Furthermore, some resins had a higher swelling effect on the fibers that delayed the crossing of the liquid through the paper.
High quality decorative laminate panels typically consist of two major types of components: the surface layers comprising décor and overlay papers that are impregnated with melamine-based resins, and the core which is made of stacks of kraft papers impregnated with phenolic (PF) resin. The PF-impregnated layers impart superior hydrolytic stability, mechanical strength and fire-resistance to the composite. The manufacturing involves the complex interplay between resin, paper and impregnation/drying processes. Changes in the input variables cause significant alterations in the process characteristics and adaptations of the used materials and specific process conditions may, in turn, be required. This review summarizes the main variables influencing both processability and technological properties of phenolic resin impregnated papers and laminates produced therefrom. It is aimed at presenting the main influences from the involved components (resin and paper), how these may be controlled during the respective process steps (resin preparation and paper production), how they influence the impregnation and lamination conditions, how they affect specific aspects of paper and laminate performance, and how they interact with each other
(synergies).
Properties data of phenolic resins synthetized for the impregnation of saturating Kraft paper
(2018)
The quality of decorative laminates boards depends on the impregnation process of Kraft papers with a phenolic resin,which constitute the raw materials for the manufacture of the cores of such boards.In the laminates industries,the properties of resins are adapted via their syntheses,usually by mixing phenol and formaldehyde in a batch,where additives,temperature and stirring parameters can be controlled. Therefore, many possibilities of preparation and phenolic resins exist, that leads to different combinations of physico chemical properties. In this article, the properties data of eight phenolic resins synthetized with different parameters of pH and reaction times at 60 °C and 90 °C are presented: the losses of pH after synthesis and the dynamic viscosities measured after synthesis and one the solid content is adjusted to 45%w/w in methanol. Data aquired by Differential Scanning Calorimetry (DSC) of the resins and Inverse Gas Chromatography (IGC) of cured solids are given as well.
Mass-customization is a megatrend that also affects the wood industry. To obtain individually designed laminates in batch size one efficient printing and processing technologies are required. Digital printing was envisaged as it does not depend on highly costly printing cylinders (as used in rotogravure printing) and allows rapid exchange of the printing designs. In the present work, two wellestablished digital printing approaches, the multi-pass and the single-pass technique, were investigated and evaluated for their applicability in decorating engineered wood and low-pressure melamine films. Three different possibilities of implementing digital printing in the decorative laminates manufacturing process were studied: (1) digital printing on coated chipboard and subsequently applying a lacquered top-coat or melamine overlay (designated as “direct printing”, since the LPM was the printing substrate), (2) digital printing on decorative paper which was subsequently impregnated before hot pressing (designated as “indirect printing, variant A”) and (3) digital printing on decorative paper with subsequent interlamination of the paper between impregnated under- and overlay paper layers during the pressing process (designated as “indirect printing, variant B”). Due to various advantages of the resulting cured melamine resin surfaces including a much better technological performance and flexibility in surface texture design, it was decided to industrially further pursue only the indirect digital printing process comprising interlamination and the direct printing process with a melamine overlay-finishing. Basis for the successful trials on production and laboratory scales were the identification of applicable inks (in terms of compatibility with melamine resin) and of appropriate printing paper quality (in terms of impregnation and imprinting ability). After selection and fine tuning of suitable materials, the next challenge to overcome was the initially insufficient bond strength between impregnated overlay and the ink layers which led to unsatisfactory quality of the print appearance and delamination effects. However, the optimization of the pressing program and the development of a modified impregnation procedure for the underlay and overlay papers allowed the successful implementation of digital printing in the production line of our industrial partner FunderMax.
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.
Rapid and robust quality monitoring of the composition of meat pastes is of fundamental importance in processing meat and sausage products. Here, an in-line near-infrared spectroscopy/micro-electro-mechanical-system-(MEMS)-based approach, combined with multivariate data analysis, was used for measuring the constituents fat, protein, water, and salt in meat pastes within a typical range of meat paste recipes. The meat pastes were spectroscopically characterized in-line with a novel process analyzer prototype. By integrating salt content in the calibration set, robust predictive PLSR models of high accuracy (R2 > 0.81) were obtained that take interfering matrix effects of the minor and NIR-inactive meat paste recipe component “salt” into account as well. The nonlinear blending behavior of salt concentration on the spectral features of meat pastes is discussed based on a designed mixture experiment with four systematically varied components.
Monodisperse porous poly(glycidyl methacrylate-co-ethylene glycol dimethacrylate) particles are widely applied in different fields, as their pore properties can be influenced and functionalization of the epoxy group is versatile. However, the adjustment of parameters which control morphology and pore properties such as pore volume, pore size and specific surface area is scarcely available. In this work, the effects of the process factors monomer:porogen ratio, GMA:EDMA ratio and composition of the porogen mixture on the response variables pore volume, pore size and specific surface area are investigated using a face centered central composite design. Non-linear effects of the process factors and second order interaction effects between them were identified. Despite the complex interplay of the process factors, targeted control of the pore properties was possible. For each response a response surface model was derived with high predictive power (all R2 predicted > 0.85). All models were tested by four external validation experiments and their validity and predictive power was demonstrated.
Hybrid organic/inorganic nanocomposites combine the distinct properties of the organic polymer and the inorganic filler, resulting in overall improved system properties. Monodisperse porous hybrid beads consisting of tetraethylene pentamine functionalized poly(glycidyl methacrylateco-ethylene glycol dimethacrylate) particles and silica nanoparticles (SNPs) were synthesized under Stoeber sol-gel process conditions. A wide range of hybrid organic/silica nanocomposite materials with different material properties was generated. The effects of n(H2O)/n(TEOS) and c(NH3 ) on the hybrid bead properties particle size, SiO2 content, median pore size, specific surface area, pore volume and size of the SNPs were studied. Quantitative models with a high robustness and predictive power were established using a statistical and systematic approach based on response surface methodology. It was shown that the material properties depend in a complex way on the process factor settings and exhibit non-linear behaviors as well as partly synergistic interactions between the process factors. Thus, the silica content, median pore size, specific surface area, pore volume and size of the SNPs are non-linearly dependent on the water-to-precursor ratio. This is attributed to the effect of the water-to-precursor ratio on the hydrolysis and condensation rates of TEOS. A possible mechanism of SNP incorporation into the porous polymer network is discussed.
Sol-gel-controlled size and morphology of mesoporous silica microspheres using hard templates
(2023)
Mesoporous silica microspheres (MPSMs) represent a promising material as a stationary phase for HPLC separations. The use of hard templates provides a preparation strategy for producing such monodisperse silica microspheres. Here, 15 MPSMs were systematically synthesized by varying the sol–gel reaction parameters of water-to-precursor ratio and ammonia concentration in the presence of a porous p(GMA-co-EDMA) polymeric hard template. Changing the sol–gel process factors resulted in a wide range of MPSMs with varying particle sizes from smaller than one to several micrometers. The application of response surface methodology allowed to derive quantitative predictive models based on the process factor effects on particle size, pore size, pore volume, and specific surface area of the MPSMs. A narrow size distribution of the silica particles was maintained over the entire experimental space. Two larger-scale batches of MPSMs were prepared, and the particles were functionalized with trimethoxy(octadecyl) silane for the application as stationary phase in reversed-phases liquid chromatography. The separation of proteins and amino acids was successfully accomplished, and the effect of the pore properties of the silica particles on separation was demonstrated.
In der vorliegenden Studie werden typische, kommerziell erhältliche und mit unterschiedlichen Lacksystemen beschichtete MDF für den Küchenbereich hinsichtlich ihres Emissionsverhaltens und deren Oberflächeneigenschaften verglichen: wasserlack-, lösungsmittellack- und pulverlackbasierte Oberflächen. Es zeigt sich, dass eine Pulverlackierung insgesamt zu höherwertigen Produkten führt, sowohl in Bezug auf Kratzbeständigkeit, Haftung und Beständigkeit gegen feuchte Hitze als auch insbesondere in Bezug auf VOC-Emissionen. Die Wasserlackoberflächen schnitten hinsichtlich ihres Emissionsverhaltens deutlich besser ab als die lösemittelbasierten Beschichtungssysteme und zeigten in Bezug auf die Oberflächeneigenschaften mit einer Ausnahme vergleichbare Kennwerte.
Melamine-formaldehyde resins are widely used for decorative paper impregnation. Resin properties relevant for impregnation are mainly determined already at the stage of resin synthesis by the applied reaction conditions. Thus, understanding the relationship between reaction conditions and technological properties is important. Response surface methodology based on orthogonal parameter level variations is the most suitable tool to identify and quantify factor effects and deduce causal correlation patterns. Here, two major process factors of MF resin synthesis were systematically varied using such a statistical experimental design. To arrive at resins having a broad range of technological properties, initial pH and M:F ratio were varied in a wide range (pH: 7.9–12.1; M:F ratio: 1:1.5–1:4.5). The impregnation behavior of the resins was modeled using viscosity, penetration rate and residual curing capacity as technological responses. Based on the response surface models, nonlinear and synergistic action of process factors was quantified and a suitable process window for preparing resins with favorable impregnation performance was defined. It was found that low M:F ratios (~1:2–1:2.5) and comparatively high starting pHs (~pH 11) yield impregnation resins with rapid impregnation behavior and good residual curing capacity.
Melamine-formaldehyde (MF) resins are widely used as surface finishes for engineered wood-based panels in decorative laminates. Since no additional glue is applied in lamination, the overall residual curing capacity of MF resins is of great technological importance. Residual curing capacity is measured by differential scanning calorimetry (DSC) as the exothermic curing enthalpy integral of the liquid resin. After resin synthesis is completed, the resulting pre-polymer has a defined chemical structure with a corresponding residual curing capacity. Predicting the residual curing capacity of a resin batch already at an early stage during synthesis would enable corrective measures to be taken by making adjustments while synthesis is still in progress. Thereby, discarding faulty batches could be avoided. Here, by using a batch modelling approach, it is demonstrated how quantitative predictions of MF residual curing capacity can be derived from inline Fourier Transform infrared (FTIR) spectra recorded during resin synthesis using partial least squares regression. Not only is there a strong correlation (R2 = 0.89) between the infrared spectra measured at the end of MF resin synthesis and the residual curing capacity. The inline reaction spectra obtained already at the point of complete dissolution of melamine upon methylolation during the initial stage of resin synthesis are also well suited for predicting final curing performance of the resin. Based on these IR spectra, a valid regression model (R2 = 0.85) can be established using information obtained at a very early stage of MF resin synthesis.
Comparative analysis of the R&D efficiency of 14 leading pharmaceutical companies for the years 1999–2018 shows that there is a close positive correlation between R&D spending and the two investigated R&D output parameters, approved NMEs and the cumulative impact factor of their publications. In other words, higher R&D investments (input) were associated with higher R&D output. Second, our analyses indicate that there are "economies of scale" (size) in pharmaceutical R&D.
Block-copolyesters of polyethylene terephthalate (PET) and polyethylene naphthalate (PEN) were synthesized via reactive extrusion. The influence of processing parameters on the material properties on a molecular scale like degree of trans-esterification, block length, and degree of randomness were investigated. The varied process factors were extrusion temperature and rotational speed. The effects of process parameter variation were investigated by 1H-NMR-spectroscopy. The experimental results show a clear dependence of the molecular properties on the processing conditions. By using statistical experimental design (DoE), it was possible to prepare defined copolyesters from PET and PEN without addition of further chemicals. With a degree of randomness between 0.05 and 0.5, the presence of an actual copolyester was confirmed when appropriate extrusion conditions were applied. The reactive extrusion process was confirmed to be suitable to produce defined block-copolyesters in a predictable and reproducible way. It was possible to produce designed sequence lengths, which could be adjusted within a range of 11–136 repeating units in the case of PET and, in the case of PEN, of 2.5–26. The produced materials can be used as barrier materials or barrier coatings to protect substrates against molecular oxygen and water vapour, e.g., in organic photovoltaic applications or food packaging. The described method is a one-pot alternative method to the previously described chemical recycling pathway.
Soft thermoplastic polysiloxane-urea-elastomers (PSUs) were prepared for the application as a biomaterial to replace the human natural lens after cataract surgery. PSUs were synthesized from amino-terminated polydimethylsiloxanes (PDMS), 4,4′-Methylenebis(cyclohexylisocyanate) (H12MDI) and 1,3–Bis(3-aminopropyl)-1,1,3,3–tetramethyldisiloxane (APTMDS) by a two-step polyaddition route. Such a material has to be highly transparent and must exhibit a low Young’s Modulus and excellent dimensional stability. Polydimethylsiloxanes in the range of 3000–33,000 g·mol−1 were therefore prepared by ring-chain-equilibration of octamethylcyclotetrasiloxane (D4) and APTMDS in order to study the influence of the soft segment molecular weight on the mechanical properties and the transparency of the PSU-elastomers. 2,4,6,8-Tetramethyl-2,4,6,8-tetraphenylcyclotetrasiloxane (D4Me,Ph) was co-polymerized with D4 in order to adjust the refractive index of the polydimethyl-methyl-phenyl-siloxane-copolymers to a value equivalent to a young human natural lens. Very elastic PSUs with Elongation at Break values higher than 700% were prepared. PSU-elastomers, synthesized from PDMS of molecular weights up to 18,000 g·mol−1, showed transmittance values of over 90% within the visible spectrum range. The soft segment refractive index was increased through the incorporation of 14 mol % of methyl-phenyl-siloxane from 1.4011 to 1.4346 (37 °C). Young’s Moduli of PSU-elastomers were around 1 MPa and lower at PDMS molecular weights up to 15,000 g·mol−1. 10-cycle hysteresis measurements were applied to evaluate the mechanical stability of the PSUs at repeated stress. Hysteresis values at 100% strain decreased from 32 to 2% (10th cycle) with increasing PDMS molecular weight. Furthermore, hysteresis at 5% strain was only detected in PSU-elastomers with low PDMS molecular weights. Finally, preliminary results of in vitro cytotoxicity tests on a PSU-elastomer showed no toxic effects on HaCaT-cells.
This article contains data on the synthesis and mechanical characterization of polysiloxane-based urea-elastomers (PSUs) and is related to the research article entitled “Influence of PDMS molecular weight on transparency and mechanical properties of soft polysiloxane-urea-elastomers for intraocular lens application” (Riehle et al., 2018) [1]. These elastomers were prepared by a two-step polyaddition using the aliphatic diisocyanate 4,4′-Methylenbis(cyclohexylisocyanate) (H12MDI), a siloxane-based chain extender 1,3-Bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane (APTMDS) and amino-terminated polydimethylsiloxanes (PDMS) or polydimethyl-methyl-phenyl-siloxane-copolymers (PDMS-Me,Ph), respectively. (More details about the synthesis procedure and the reaction scheme can be found in the related research article (Riehle et al., 2018) [1]).
Amino-terminated polydimethylsiloxanes with varying molecular weights and PDMS-Me,Ph-copolymers were prepared prior by a base-catalyzed ring-chain equilibration of a cyclic siloxane and the endblocker APTMDS. This DiB article contains a procedure for the synthesis of the base catalyst tetramethylammonium-3-aminopropyl-dimethylsilanolate and a generic synthesis procedure for the preparation of a PDMS having a targeted number average molecular weight of 3000 g mol−1. Molecular weights and the amount of methyl-phenyl-siloxane within the polysiloxane-copolymers were determined by 1H NMR and 29Si NMR spectroscopy. The corresponding NMR spectra and data are described in this article.
Additionally, this DiB article contains processed data on in line and off line FTIR-ATR spectroscopy, which was used to follow the reaction progress of the polyaddition by showing the conversion of the diisocyanate. All relevant IR band assignments of a polydimethylsiloxane-urea spectrum are described in this article.
Finally, data on the tensile properties and the mechanical hysteresis-behaviour at 100% elongation of PDMS-based polyurea-elastomers are shown in dependence to the PDMS molecular weight.
The effect of hard segment content and diisocyanate structure on the transparency and mechanical properties of soft poly(dimethylsiloxane) (PDMS)-based urea elastomers (PSUs) was investigated. A series of PSU elastomers were synthesized from an aminopropyl-terminated PDMS (M¯n: 16,300 g·mol−1), which was prepared by ring chain equilibration of the monomers octamethylcyclotetrasiloxane (D4) and 1,3-bis(3-aminopropyl)-tetramethyldisiloxane (APTMDS). The hard segments (HSs) comprised diisocyanates of different symmetry, i.e., 4,4′-methylenebis(cyclohexyl isocyanate) (H12MDI), 4,4′-methylenebis(phenyl isocyanate) (MDI), isophorone diisocyanate (IPDI), and trans-1,4-cyclohexane diisocyanate (CHDI). The HS contents of the PSU elastomers based on H12MDI and IPDI were systematically varied between 5% and 20% by increasing the ratio of the diisocyanate and the chain extender APTMDS. PSU copolymers of very low urea HS contents (1.0–1.6%) were prepared without the chain extender. All PSU elastomers and copolymers exhibited good elastomeric properties and displayed elongation at break values between 600% and 1100%. The PSUs with HS contents below 10% were transparent and became increasingly translucent at HS contents of 15% and higher. The Young’s modulus (YM) and ultimate tensile strength values of the elastomers increased linearly with increasing HS content. The YM values differed significantly among the PSU copolymers depending on the symmetry of the diisocyanate. The softest elastomer was that based on the asymmetric IPDI. The elastomers synthesized from H12MDI and MDI both exhibited an intermediate YM, while the stiffest elastomer, i.e., that comprising the symmetric CHDI, had a YM three-times higher than that prepared with IPDI. The PSUs were subjected to load–unload cycles at 100% and 300% strain to study the influence of HS morphology on 10-cycle hysteresis behavior. At 100% strain, the first-cycle hysteresis values of the IPDI- and H12MDI-based elastomers first decreased to a minimum of approximately 9–10% at an HS content of 10% and increased again to 22–28% at an HS content of 20%. A similar, though less pronounced, trend was observed at 300% strain. First-cycle hysteresis among the PSU copolymers at 100% strain was lowest in the case of CHDI and highest in the IPDI-based elastomer. However, this effect was reversed at 300% strain, with CHDI displaying the highest hysteresis in the first cycle. In vitro cytotoxicity tests performed using HaCaT cells did not show any adverse effects, revealing their potential suitability for biomedical applications.
Film formation of self synthesized Polymer EPM–g–VTMDS (ethylene–propylene rubber, EPM, grafted with vinyltetramethyldisiloxane, VTMDS) was studied regarding bonding to adhesion promoter vinyltrimethoxysilane (VTMS) on oxidized 18/10 chromium/nickel–steel (V2A) stainless steel surfaces. Polymer films of different mixed solutions including commercial siloxane and silicone, dimethyl, vinyl group terminated crosslinker (HANSA SFA 42100, CAS# 68083-19-2, 0.35 mmol Vinyl/g) and platinum, 1,3-diethenyl-1,1,3,3-tetramethyldisiloxane complex Karstedt's catalyst (ALPA–KAT 1, CAS# 68478-92-2) were spin coated on V2A stainless steel surfaces with adsorbed VTMS thin layers in order to analyze film formation of EPM–g–VTMDS at early stages. Surface topography and chemical bonding of the high performance polymers on different oxidized V2A surfaces were investigated with X–ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), scanning electron microscopy (SEM) and surface enhanced Raman spectroscopy (SERS). AFM and SEM as well as XPS results indicated that the formation of the polymer film proceeds via growth of polymer islands. Chemical signatures of the essential polymer contributions, linker and polymer backbones, could be identified using XPS core level peak shape analysis and also SERS. The appearance of signals which are related to Si–O–Si can be seen as a clear indication of lateral crosslinking and silica network formation in the films on the V2A surface.
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.
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.
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.
Determination of the gel point of formaldehyde-based wood adhesives by using a multiwave technique
(2023)
Determining the instant of gelation of formaldehyde-based wood adhesives as an assessment parameter for their curing rate is important for optimizing the curing behavior. Due to the stoichiometrically imbalanced networks of formaldehyde-based adhesives, the crossover point of storage G′ and loss modulus G″ cannot unconditionally be assumed as the gel point in oscillatory time sweeps as the material response is frequency-dependent. This study aims to determine the gel point of selected adhesives by the isothermal multiwave oscillatory shear test. A thorough comparison between the gel and the crossover point of G′ and G″ is performed. Rheokinetic analysis showed no significant difference between the activation energies calculated at the gel point determined by a multiwave test and the crossover point obtained by the time sweep test. Hence, for resins with similar curing reactions, a reliable determination of gel point by applying a multiwave test is needed for a comparison of their reactivity.
A systematic study using a central composite design of experiments (DoE) was performed on the oxygen plasma surface modifications of two different polymers—Pellethane 2363-55DE, which is a polyurethane, and vinyltrimethoxysilane-grafted ethylene-propylene (EPR-g-VTMS), a cross-linked ethylene-propylene rubber. The impacts of four parameters—gas pressure, generator power, treatment duration, and process temperature—were assessed, with static contact angles and calculated surface free energies (SFEs) as the main responses in the DoE. The plasma effects on the surface roughness and chemistry were determined using scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Through the sufficiently accurate DoE model evaluation, oxygen gas pressure was established as the most impactful factor, with the surface energy and polarity rising with falling oxygen pressure. Both polymers, though different in composition, exhibited similar modification trends in surface energy rise in the studied system. The SEM images showed a rougher surface topography after low pressure plasma treatments. XPS and subsequent multivariate data analysis of the spectra established that higher oxidized species were formed with plasma treatments at low oxygen pressures of 0.2 mbar.
Silicones
(2014)
Silicones are found in a variety of applications with requirements that range from long life at elevated temperatures to fluidity at low temperatures. This chapter first considers silicone elastomers and their application in room temperature vulcanizing (RTV) and heat curing systems (HTV). Also, new technologies for UV curing are introduced. Coverage of RTVs includes both one-component and two-component systems and the different cure chemistries of each, and is followed by a separate discussion of silicone laminates. Due to the high importance of silicone fluids, they are also discussed. Fluids include polishes, release agents, surfactants, and dielectric fluids.
Silicones
(2022)
Silicones are found in a variety of applications with requirements that range from long life at elevated temperatures to fluidity at low temperatures. This chapter first considers silicone elastomers and their application in room temperature vulcanizing (RTV) and heat curing systems (HTV). Also, new technologies for UV curing are introduced. Coverage of RTVs includes both one-component and two-component systems and the different cure chemistries of each and is followed by a separate discussion of silicone laminates. Due to the high importance of silicone fluids, they are also discussed. Fluids include polishes, release agents, surfactants, and dielectric fluids.
Three different polyols (soluble starch, sucrose, and glycerol) were tested for their potential in the chemical modification of melamine formaldehyde (MF) resins for paper impregnation. MF impregnated papers are widely used as finishing materials for engineered wood. These polyols were selected because the presence of multiple hydroxy groups in the molecules was suspected to facilitate cocondensation with the main MF framework. This should lead to good resin performance. Moreover, they are readily produced from natural feedstock. They are available in large quantities and may serve as economically feasible, environmentally harmless alternative co-monomers suitable to substitute a portion of fossil-based starting material. In the presented work, a number of model resins were synthesized and tested for covalent incorporation of the natural polyol into the MF Framework. Spectroscopic evidence of chemical incorporation of glycerol was found by applying by 1H, 13C, 1H/13C HSQC, 1H/13C HMBC, and 1H DOSY methods. It was furthermore found that covalent incorporation of glycerol in the network took place when glycerol was added at different stages during synthesis. Further, all resins were used to prepare decorative laminates and the performance of the novel resins as surface finishing was evaluated using standard technological tests. The technological performance of the various modified thermosetting resins was assessed by determining flow viscosity, molar mass distribution, the storage stability, and in a second step laminating impregnated paper to particle boards and testing the resulting surfaces according to standardized quality tests. In most cases, the average board surface properties were of acceptable quality. Our findings demonstrate the possibility to replace several percent of the petrol-based product melamine by compounds obtained from renewable resources.