Fabrication of a bi-hydroxyl-bi-DOPO compound with excellent quenching and charring capacities for lignin-based epoxy resin

Abstract

In this study, lignin-based epoxy resins (EP) were fabricated using lignin, phenol and glyoxal as crosslinking reagents. For improving the flame retardancy, a bi-DOPO compound with bi-hydroxyl structure was successfully synthesized, containing excellent quenching and charring capacities. Good pyrolysis behaviors of as-synthesized flame retardant resulted in significant quenching effect via structure decomposition to release PO and PO₂ free radicals for capturing reactive H and OH radicals produced from epoxy combustion. With addition of 0.18 wt% phosphorus, epoxy composite (10% LPG-ER-4) passed V-0 rating with high limited oxygen index (LOI) value of 35.2%. Cone calorimeter tests showed that heat release (including heat release rate (HRR) and total heat release (THR)) from combustion was reduced with assistance of flame retardant. Char residue analyses illustrated that bi-hydroxyl structure in DOPO-based flame retardant benefited the formation of char layer with higher compactness and integrity to serve as a protective shell of interior epoxy matrix. Furthermore, exterior pore size of char residue was narrowed or blocked to avoid the release of heat and volatiles generated from combustion. This study provided a feasible method to improve flame retardancy of lignin-based EP and proposed flame-retardant mechanism both in gaseous and solid phases.

Keywords: Bi-hydroxyl; DOPO; Lignin.