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Flame-retardant finishing of cotton fabrics using DOPO functionalized alkoxy- and amido alkoxysilane
(2023)
In the present study, DOPO-based alkoxysilane (DOPO-ETES) and amido alkoxysilane (DOPO-AmdPTES) were synthesized by one-step and without by-products as halogen-free flame retardants. The flame retardants were applied on cotton fabric utilizing sol–gel method and pad-dry-cure finishing process. The flame retardancy, the thermal stability and the combustion ehaviour of treated cotton were evaluated by surface and bottom edge ignition flame test (according to EN ISO 15025), thermogravimetric analysis (TGA) and micro-scale combustion calorimeter (MCC). Unlike CO/DOPO-ETES sample, cotton treated with DOPO-AmdPTES nanosols exhibits self-extinguishing ehaviour with high char residue, an improvement of the LOI value and a significant reduction of the PHRR, HRC and THR compared to pristine cotton. Cotton finished with DOPO-AmdPTES reveals a semi-durability after ten laundering cycles keeping the flame-retardant properties unchanged. According to the results obtained from TGA-FTIR, Py-GC/MS and XPS, the major activity of flame retardant occurs in the condensed phase via catalytic induced char formation as physical barrier along with the activity in the gas phase derived mainly from the dilution effect. The early degradation of CO/DOPO-AmdPTES compared to CO/DOPO-ETES, triggered by the cleavage of the weak bond between P and C=O, as the DFT study indicated, provides the beneficial effect of this flame retardant on the fire resistance of cellulose.
Polyester fibers are widely employed in a multitude of sectors and applications from the technical textiles to everyday life thanks to their durability, strength, and flexibility. Despite these advantages, polyester lacks in dyeability, adhesion of coating, hydrophilicity, and it is characterized by a low wettability respect to natural fibers. On this regard, beyond the harmful hydrophobic textile finishings of polyester fabrics containing fluorine-compounds, and in order to avoid pre-treatments, such as laser irradiation to improve their surface properties, research is moving towards the development of fluorine-free and safer coatings. In this work, the (3-glycidyloxypropyl)trimethoxysilane (GPTMS) and various long alkyl-chain alkoxysilanes were employed for the fabrication in the presence of a catalyst of a water-based superhydrophobic finishing for polyester fabrics with a simple sol-gel, non-fluorinated, sustainable approach and the dip-pad-dry-cure method. The finished polyester fabrics surface properties were investigated by static and dynamic water repellency tests. Additionally, the resistance to common water-based liquids, abrasion resistance, moisture adsorption, and air permeability measurements were performed. Scanning electron microscopy was employed to examine the micro- and nano-morphology of the functionalized polyester fabrics surfaces. The obtained superhydrophobic finishings displayed high water-based stain resistance as well as good hydrophobicity after different cycles of abrasion.
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.
The properties of polyelectrolyte multilayers are ruled by the process parameters employed during self-assembly. This is the first study in which a design of experiment approach was used to validate and control the production of ultrathin polyelectrolyte multilayer coatings by identifying the ranges of critical process parameters (polyelectrolyte concentration, ionic strength and pH) within which coatings with reproducible properties (thickness, refractive index and hydrophilicity) are created. Mathematical models describing the combined impact of key process parameters on coatings properties were developed demonstrating that only ionic strength and pH affect the coatings thickness, but not polyelectrolyte concentration. While the electrolyte concentration had a linear effect, the pH contribution was described by a quadratic polynomial. A significant contribution of this study is the development of a new approach to estimate the thickness of polyelectrolyte multilayer nanofilms by quantitative rhodamine B staining, which might be useful in all cases when ellipsometry is not feasible due to the shape complexity or small size of the coated substrate. The novel approach proposed here overcomes the limitations of known methods as it offers a low spatial sampling size and the ability to analyse a wide area without restrictions on the chemical composition and shape of the substrate.
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.
The present study investigated the possibilities and limitations of using a low-cost NIR spectrometer for the verification of the presence of the declared active pharmaceutical ingredients (APIs) in tablet formulations, especially for medicine screening studies in low-resource settings. Spectra from 950 to 1650 nm were recorded for 170 pharmaceutical products representing 41 different APIs, API combinations or placebos. Most of the products, including 20 falsified medicines, had been collected in medicine quality studies in African countries. After exploratory principal component analysis, models were built using data-driven soft independent modelling of class analogy (DD-SIMCA), a one-class classifier algorithm, for tablet products of penicillin V, sulfamethoxazole/trimethoprim, ciprofloxacin, furosemide, metronidazole, metformin, hydrochlorothiazide, and doxycycline. Spectra of amoxicillin and amoxicillin/clavulanic acid tablets were combined into a single model. Models were tested using Procrustes cross-validation and by projection of spectra of tablets containing the same or different APIs. Tablets containing no or different APIs could be identified with 100 % specificity in all models. A separation of the spectra of amoxicillin and amoxicillin/clavulanic acid tablets was achieved by partial least squares discriminant analysis. 15 out of 19 external validation products (79 %) representing different brands of the same APIs were correctly identified as members of the target class; three of the four rejected samples showed an API mass percentage of the total tablet weight that was out of the range covered in the respective calibration set. Therefore, in future investigations larger and more representative spectral libraries are required for model building. Falsified medicines containing no API, incorrect APIs, or grossly incorrect amounts of the declared APIs could be readily identified. Variation between different NIR-S-G1 spectroscopic devices led to a loss of accuracy if spectra recorded with different devices were pooled. Therefore, piecewise direct standardization was applied for calibration transfer. The investigated method is a promising tool for medicine screening studies in low-resource settings.
Polyurethane thermosets have a wide range of applications. In this study, alternative raw materials were used to enhance sustainability. In two newly developed biobased polyurethanes (PUs), the cross-linker content was varied, which caused phase separation and therefore affected the turbidity. To investigate this phenomenon, UV–Vis–NIR spectroscopy was utilized. Spectra were recorded from 200 to 2500 nm in transmittance mode, and multivariate data analysis was applied to the three UV, Vis, and NIR sections separately. For the two different PU classes, each with five different cross-linker contents, classification by principal component analysis combined with linear or quadratic discriminant analysis was possible with an accuracy between 93% and nearly 100%. The best separation was achieved in the NIR range. Partial least-squares regression models were determined to predict the cross-linker content. As mentioned, the model for the NIR range is the most suitable, with the highest R2 (validation) of 0.99 for PU1 and 0.98 for PU2. The corresponding root-mean-square error of prediction values of the external validation was the lowest, with 0.82% (PU1) and 1.25% (PU2). Therefore, UV–Vis–NIR absorbance spectroscopy, especially NIR, is a suitable tool for monitoring the appropriate material composition of turbid PU thermosets in line.
Thin, flat textile roofing offers negligible heat insulation. In warm areas, such roofing membranes are therefore equipped with metallized surfaces to reflect solar heat radiation, thus reducing the warming inside a textile building. Heat reflection effects achieved by metallic coatings are always accompanied by shading effects as the metals are non-transparent for visible light (VIS). Transparent conductive oxides (TCOs) are transparent for VIS and are able to reflect heat radiation in the infrared. TCOs are, e.g., widely used in the display industry. To achieve the perfect coatings needed for electronic devices, these are commonly applied using costly vacuum processes at high temperatures. Vacuum processes, on account of the high costs involved and high processing temperatures, are obstructive for an application involving textiles. Accepting that heat-reflecting textile membranes demand less perfect coatings, a wet chemical approach has been followed here when producing transparent heat-reflecting coatings. Commercially available TCOs were employed as colloidal dispersions or nanopowders to prepare sol-gel-based coating systems. Such coatings were applied to textile membranes as used for architectural textiles using simple coating techniques and at moderate curing temperatures not exceeding 130 °C. The coatings achieved about 90% transmission in the VIS spectrum and reduced near-infrared transmission (at about 2.5 µm) to nearly zero while reflecting up to 25% of that radiation. Up to 35% reflection has been realized in the far infrared, and emissivity values down to ε = 0.5777 have been measured.
Ecuador, traditionally an agricultural based economy, has a great potential for valorizing their industrial residues. This study, presents a techno-economic analysis for applying a novel biomass oxidation method to produce formic and acetic acids from coffee husk residues in Machala, Ecuador. The analysis determined that the time of return of investment was lower than 5 years, making this project economically feasible, when producing approx. 1000 tons of formic acid per year, which is enough for supplying the Ecuadorian market. This production, would reduce imports costs and develop the chemical industry in the country.
Gegenstand dieser Arbeit ist die Darstellung und Charakterisierung einheitlicher, mesoporöser Silica-Partikel (MPSM) im Mikrometerbereich mit maßgeschneiderten Partikel- und Porendesign für die Hochleistungsflüssigkeitschromatographie. Die Synthese umfasst die Einlagerung von Silica-Nanopartikeln (SNP) in poröse organische Template, welche anschließend bei 600°C zersetzt werden. Die Impfsuspensionspolymerisation von Polystyrol-Partikeln, unter Verwendung von Glycidylmethacrylat, Ethylenglycoldimethacrylat und Porogenen, ermöglicht die Herstellung hochgradig einheitlicher, poröser p(GMA-co-EDMA)-Template. Der Einfluss wesentlicher Faktoren, einschließlich des Monomer-Porogen-Verhältnisses, des Monomerverhältnisses und der Porogenzusammensetzung, werden systematisch untersucht sowie ihre Auswirkungen auf die Porengröße, das Porenvolumen und die spezifische Oberfläche erläutert. Die Anbindung aminofunktionalisierter Substanzen erfolgt durch die Ringöffnung der Epoxidgruppe. Im anschließenden basischen Sol-Gel-Prozess werden die Silica-Nanopartikel aufgrund der Ladungsunterschiede in die funktionalisierten p(GMA-co-EDMA)-Template eingebaut. Die Partikelgröße der SNP beeinflusst wesentlich die Poreneigenschaften der MPSM und hängt von drei Faktoren ab: (i) der Wachstumsgeschwindigkeit in der kontinuierlichen Phase, die durch die Einstellungen des Sol-Gel-Prozesses gesteuert wird, (ii) der Diffusionsrate, die durch elektrostatische Anziehung reguliert wird und vom Grad der Funktionalisierung abhängt und (iii) der Porosität des Polymer-Templats. Die gezielte Anpassung der Poreneigenschaften durch die Prozesseinstellungen erlaubt die präzise Herstellung von MPSM, die auf spezifische Trennherausforderungen zugeschnitten werden und somit die Qualität der HPLC verbessern. Die vorgestellte Synthesestrategie ermöglicht, aufgrund des stufenweisen molekularen Aufbaus, eine bessere Adaption der stationären Phase an spezifische Trennherausforderungen.