In this work, two kinds of rare earth hypophosphites (REHP), lanthanum hypophosphite (LaHP) and cerium hypophosphite (CeHP), were synthesized and characterized. Subsequently, LaHP and CeHP were added into polylactide to improve its flame retardant properties. Thermal gravimetric analysis was employed to investigate the thermal decomposition behavior of REHP and flame retardant polylactide composites (FR-PLA). The fire performance evaluated by microscale combustion calorimetry and cone calorimeter clearly demonstrated that the addition of LaHP and CeHP resulted in significant reduction of the heat release rate, low total heat release, and compact intumescent char layer. Thermogravimetric analysis− infrared spectrometry testing indicated that the addition of REHP significantly decreased the yields of pyrolysis products. Furthermore, the crystallization behaviors of FR-PLA composites were investigated by differential scanning calorimetry. The char residue of FR-PLA composites after cone calorimeter testing were also be investigated by scanning electron microscope, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy.
■ INTRODUCTIONIn recent years, the increasing awareness of petroleum source and the environmental problems caused by persistent plastic wastes has impelled people to develop new ecofriendly and renewable materials to replace petroleum-based plastics. 1−3 Among these materials, polylactide (PLA) has received considerable attention because of its biodegradable, abundant renewable source, transparency and excellent mechanical properties. PLA holds tremendous promise in many fields, such as biomedical, household, engineering, packing industries, and so on. 4−8 However, like many other plastics, PLA presents poor flammability (typical limiting oxygen index (LOI) of 19.5 vol %, easily dripping in burning) in fire testing, which restricts its further development in some important fields. Therefore, it is meaningful to investigate flame-retarded PLA.It is well-known that intumescent flame retardant (IFR) shows good performance in some polymers as a halogen-free additive due to the advantage of little smoke production and low toxicity. 9 Reti et al. 10 studied the efficiency of different intumescent formulations to flame retard PLA, and the quantity of the additives has been optimized. Feng and Zhan et al. have researched different intumescent flame retardant systems for preparation of FR-PLA composites that showed good performance in the testing. 10−12 Other flame retardant additives, such as expanded graphite, 13 aluminum hydroxide, 14 and silica gel 15 have also been reported.Recently, aluminum hypophosphite (AHP) has been used as a flame retardant that has achieved effective flame retardance in polymer materials. Yang et al. found aluminum hypophosphite showed perfect flame retardancy in PET and PBT composites; 16,17 20 wt % of AHP could make glass-fiber/PBT composite reach an UL-94 V0 rating with a LOI value of 29 vol %, and 10 wt % of AHP could make glass-fiber/PET comp...