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Im IGF-Projekt Nr. 19617 N wurden stickstoff- und phosphorsubstituierte Alkoxysilane hergestellt und ihre flammhemmenden Eigenschaften für Textilien untersucht. Die Synthesen erfolgten nach unterschiedlichen Strategien wie der Klick-Chemie und der nukleophilen Substitution kommerziell erhältlicher Organophosphorverbindungen mit aminobasierten Trialkoxysilanen und/oder Cyanurchlorid. Diese neuartigen, halogen- und aldehydfreien Flammschutzmittel wurden auf Stoffe aus Baumwolle (BW), Polyethylenterephthalat (PET), Polyamid (PA), sowie Mischgeweben daraus mit der industriell etablierten Pad-Dry-Cure-Technik und mittels Sol-Gel-Verfahren aufgetragen. Die flammhemmenden Eigenschaften wurden mit den Prüfverfahren nach EN ISO 15025 (Schutzkleidung – Schutz gegen Hitze und Flammprüfverfahren für begrenzte Flammenausbreitung= bewertet. Eine gute Schwerentflammbarkeit der hybriden organisch-anorganischen Materialien wurde bei einer geringen Menge von 3-5 Gew.% auf Baumwollgeweben erreicht. Darüber hinaus konnten die Wasserlöslichkeit und die Waschbeständigkeit durch die an das Phosphoratom gebundenen funktionellen Gruppen und durch die Optimierung der Härtungstemperatur kontrolliert werden. Insgesamt zeigte das Forschungsprojekt, dass N-P-Silane sehr gute permanente Flammschutzmittel für Textilien sind.
In the IGF project No. 19617 N, nitrogen and phosphorous substituted alkoxysilanes were prepared and their ability to inhibit fire growth and spread for fabrics was explored. To this end, a series of flame retardants were synthesized using different strategies including click chemistry and nucleophilic substitution of commercial organophosphorus compounds with amino-based trialkoxysilanes and/or cyanuric chloride. The new halogen-free and aldehyde-free flame retardants were applied to different fabrics such as cotton (CO), polyethylene terephthalate (PET), polyamide (PA) and their blends using the well-known pad-dry-cure technique and sol-gel method. The flame-retarding efficiencies were evaluated by EN ISO 15025 test methods (protective clothing-protection against heat and flame method of test for limited flame spread). Good flame retardancy of the hybrid organic-inorganic materials was achieved with the addition of as small amount as 3-5 wt.% for cotton fabrics. Moreover, the water solubility and the washing resistance could be controlled through the functional groups attached to the phosphor atom or through the optimization of the curing temperature. Overall, the research project demonstrated that N-P-silanes are very good permanent flame retardants for textiles.
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.