ABSTRACTMelamine−formaldehyde resin (MF)/polyvinyl alcohol (PVA) composite fibers with different phase structures and properties were prepared through reaction induced phase separation by wet spinning. Raman spectroscopy, rotary viscometer, and miscibility index were used to characterize the MF resins with different reaction degrees (RD). The phase structures of composite spinning dopes and composite fibers were observed by optical microscope (OM) and scanning electron microscope (SEM). Mechanical properties, flame retardant properties, and thermal stability of the composite fibers were also tested. Results show that the composite fibers made from MF resins with different RD have different phase structures and properties; when the miscibility index (MI) of MF resin is 1.60, the obtained MF/PVA composite fiber shows a sea‐island phase structure, which endues the fiber with the best comprehensive properties: the breaking strength, breaking elongation, rupture work and limiting oxygen index (LOI) are 4.29 cN/dtex, 13.55%, 8.46 × 10−5 J/dtex and 43.1%, respectively. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016, 133, 42918.
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