New hybrid sol–gel coatings based on tetraethoxysilane (TEOS) and phytic acid (PA) were designed and applied to cotton; the flame-retardant properties of the treated fabrics were thoroughly investigated by means of flame-spread and forced-combustion tests. The first goal was to identify the TEOS:PA weight ratio that allowed the achievement of the best flame-retardant properties, with the lowest final dry add-on on the fabrics. Therefore, different TEOS:PA sols were prepared and applied to cotton, and the resulting coated fabrics were thoroughly investigated. In particular, solid-state NMR spectroscopy was exploited for assessing the condensation degree during the sol–gel process, even for evaluating the occurrence of possible reactions between phytic acid and the cellulosic substrate or the alkoxy precursor. It was found that a total dry add-on of 16 wt. % together with 70:30 TEOS:PA weight ratio provided cotton with self-extinction, as clearly indicated by flame-spread tests. This formulation was further investigated in forced-combustion tests: a significant reduction of heat release rate (HRR), of the peak of HRR, and of total heat release (THR) was found, together with a remarkable increase of the residues after the test. Unfortunately, the treated fabrics were not resistant to washing cycles, as they significantly lost their flame-retardant properties, consequently to the partial removal of the deposited hybrid coatings.
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