DOPO基阻燃剂的合成与耐热性能的实验研究

9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物简称DOPO,此种化合物及其衍生物在阻燃剂领域中因其低烟、低毒的特点而备受青睐。本文将DOPO、多聚甲醛、二乙醇胺反应合成出一种含氮含磷反应型DOPO类阻燃剂,对其结构进行了表征,并初步研究了这种物质在空气气氛中的耐热性能,结果表明,该产物在182．35℃开始分解,到700℃剩余7．22%。将其加入到聚氨酯中制备复合材料,在氮气气氛中进行热重测试,发现随着其用量加大,复合材料的初始分解温度先增高后降低,失重台阶的降解活化能也是先增加后降低,且都比纯粹聚氨酯的高,证明添加此种阻燃剂之后起到了一定的耐热效果,且当添加量为4%时综合性能最好；然后探讨了复合材料降解过程的机理。对4%添加量的复合材料在空气气氛中进行热重测试,发现其在227．2℃开始分解,主要有两大失重平台,分别失重26．01%和18．14%,在700℃时还剩余8．57%。

Synthesis of DOPO-based Flame Retardants and Experimental Study of Their Heat Resistance

9,10-Dihydro-9-oxa-10-phosphaphenanthrene 10-oxide（ DOPO） and its derivatives are highly at-tracted because of its smokeless and toxicityless properties in the flame retardant field. A reactive nitrogen-phos-phorus-contained DOPO-based flame retardant was synthesized with DOPO,paraformaldehyde and diethanolamine. The structure has been characterized,and the thermal properties were studied. The results showed that this product begins to decompose in 182. 35℃,it remaining 7. 22% at 700℃. When it was added to the polyurethane,the com-posite materials were produced,according to their TGA results in nitrogen,we found that the decomposition tempera-ture of the composite material is firstly increased and then decreased,the same as their weightlessness stepped deg-radation activation energy,and they are all higher than pure polyurethane,so it was proved that this composite play a certain flame-retardant effect after adding such flame retardants in polyurethane,when its content is 4%,the best overall performance were get. Then the mechanism of the degradation process of the composite material was ex-plored. At last,the TGA results in air atmosphere was get when the dosage of this kind of flame retardant was 4%, we found that it decomposed at 227. 2℃, there are two weight loss platform, the weight loss were 26. 01% and 18. 14% respectively,the remaining was 8. 57% at 700℃.