新型含磷阻燃剂DOPO-PPO的合成及其阻燃性能

Synthesis and Flame Retardant Properties of A Novel Phosphorous-containing Flame Retardant DOPO-PPO

以苯基磷酰二氯,对羟基苯甲醛及9,10-二氢-9-氧杂-10-磷杂菲(DOPO)为原料,合成了一种新型含磷阻燃剂——二[4-(次甲基-羟基-磷杂菲)苯氧基]苯基氧化磷(DOPO-PPO),其结构经1H NMR和IR表征。通过TGA和DTG研究了DOPO-PPO的热稳定性,热降解行为及成炭性能。结果表明:DOPO-PPO的起始热分解温度为210℃,在700℃时残炭为30.4%。以环氧树脂为基材,DOPO-PPO为阻燃剂,二氨基二苯硫砜为固化剂,制备了阻燃环氧树脂(3)。通过极限氧指数(LOI)和垂直燃烧(UL-94)测试了3的阻燃性能。结果表明:当DOPOPPO的添加量为12.0%(质量百分数,即312)时,阻燃级别为V-0级,LOI为34.0%。

A novel phosphorus-containing flame retardant,bis[4-( methylene-hydroxy-DOPO) phenoxy]phenyl phosphine oxide( DOPO-PPO),was synthesized from phenylphosphonic dichloride,p-hydroxybenzaldehyde and 6H-dibenz[c,e][1,2]oxaphosphorin 6-oxide( DOPO). The structure was characterized by1 H NMR and IR. The thermal stability,thermal degradation behavior and charring property of DOPO-PPO were investigated by TGA and DTG. The results showed that the initial thermal decomposition temperature of DOPO-PPO was 210 ℃ and the char yield was 30. 4% at 700 ℃. A flame retardant epoxy resin(3) was prepared,using epoxy resin as base material,DOPO-PPO as flame retardant and 4,4'-diaminodiphenylsulfone as curing agent. The flame retardant properties of 3 were investigated by limiting oxygen index(LOI) and vertical burning(UL-94) test. The results showed that the LOI of 312(dosage of DOPO-PPO was 12. 0 wt%) was 34. 0% with flammability rating V-0.