摘要
以季戊四醇、三氯氧磷为原料,采用无溶剂法首先合成了季戊四醇二磷酸酯二磷酰氯(PDD),n(季戊四醇)n∶(三氯氧磷)=1 5∶,收率为84%;然后以PDD和对苯二酚为原料,乙腈为溶剂,三乙胺为缚酸剂,在氮气氛围下合成了低聚阻燃剂聚季戊四醇磷酸酯,n(PDD)∶n(对苯二酚)=1∶1,收率为79%。采用红外光谱、磷谱、热重分析和差示扫描量热法对聚合物的结构和热行为分别进行了表征和研究。结果表明,该聚合物具有较高的玻璃态转变温度(Tg=231℃),聚合物质量损失5%时的温度为301℃。当聚合物被加热到600℃时,其炭残留物的质量分数为46.4%。
Pentaerythritol diphosphonate dichloride （PDD） was synthesized in yield 84% from pentaerythritol and phosphorous oxychloride （5equiv.） first in the absence of organic solvent, and then an oligomer polymeric pentaerythrityl phosphate was synthesized in yield 79% from PDD and hydroquinone （lequiv.） using acetonitrile as solvent and triethylamine as acid acceptor under N2 atmosphere. The structure and thermal behaviors of the polymer were characterized and studied by IR, ^31p NMR, TGA and DSC respectively. The results indicated that the polymer had high glass transition temperature （Tg=231℃）, the polymer had 5% weight-loss at 301℃. When it was heated to 600℃, the char residue was 46.4%.
出处
《精细化工中间体》
CAS
2006年第3期43-45,48,共4页
Fine Chemical Intermediates
关键词
阻燃剂
聚季戊四醇磷酸酯
合成
玻璃态转变温度
炭残留物
flame retardant
polymeric pentaerythrityl phosphate
synthesis
glass transition temperature
char residue
