Two novel types of phosphate derivatives of phosphaphenanthrene with a high phosphorus content were prepared by phosphorylation reaction between either 2-(6-oxido-6H-dibenz<c,e><1,2>oxaphosphorin-6-yl)-methanol (ODOPM) or 2-(6-oxido-6H-dibenz<c,e><1,2>oxaphosphorin-6-yl)-1,4-benzenediol (ODOPB) and dialkyl phosphoryl chloride. The structures of all compounds were characterised by 1H NMR, 13C NMR, 31P NMR, Fourier transform infrared spectroscopy, and high-resolution mass spectrometry. The thermal stability of representative compounds was determined by thermal gravimetric analysis and differential scanning calorimetry. The results showed that the compounds have excellent resistance to oxidation, high thermal stability with an onset decomposition temperature above 200°C, and a high char yield over 25 %, owing to the high P content. The representative compound was added to conventional electrolytes of lithium-ion batteries as flame retardant additive, and the self-extinguishing time and ionic conductivity were measured. The result showed that the compounds have effective flame retardant properties.
通过 2-(6-氧代-6H-二苯并<;c,e><1,2>oxaphosphorin-6-yl)-methanol (ODOPM) 或 2-(6-oxido-6H-dibenz<c,e><1,2>oxaphosphorin-6-yl)-1,4-benzenediol (ODOPB) 与二烷基磷酰氯之间的磷化反应制备了高磷含量的磷菲衍生物。所有化合物的结构均通过 1H NMR、13C NMR、31P NMR、傅立叶变换红外光谱和高分辨率质谱进行了表征。通过热重分析和差示扫描量热法测定了代表性化合物的热稳定性。结果表明,这些化合物具有优异的抗氧化性、较高的热稳定性(起始分解温度高于 200°C)以及较高的炭化率(由于 P 含量较高),炭化率超过 25%。将代表性化合物作为阻燃添加剂添加到锂离子电池的常规电解液中,并测量了其自熄时间和离子电导率。结果表明,该化合物具有有效的阻燃特性。