新型含磷阻燃剂DOPO-ITA的合成与表征

Synthesis and characterization of 10-( 2, 5-dicarbonylpropyl) 9,10-dihydro-9-oxa-10- phospha-phenanthrene-10-oxide

以9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)、衣康酸(ITA)为原料,二甲苯作溶剂合成出了新型含磷阻燃剂DOPO-ITA,并通过红外光谱、1 H核磁谱、质谱等对该化合物结构进行了鉴定。同时考察了反应温度、反应时间、溶剂种类和气氛等对收率的影响。结果表明,当n(DOPO):n(ITA)=1:1;反应温度160℃;反应时间18 h;工业氮气保护条件下DOPO-ITA的收率为91%。

A novel phosphorous-containing flame retardants 10-（2,5-dicarbonylpropyl）9,10-dihydro-9-oxa-10-phospha- phenanthrene - 10- oxide （DOPO-ITA） was synthesized using 9,10-dihydro-9-oxa- 10-phospha-phenanthrene- 10-oxide （DOPO） and itaconic acid（ITA） as starting materials. The structures of the obtained compound was identified by IR, IHNMR and MS. Factors that influenced the product yield such as the reaction temperature, the reaction time, solvent and inlet gas were discussed. The reaction conditions were determined as follows： mol ratio of DOPO： ITA is 1：1; the reaction temperature is 160℃; the reaction time is 18 h .In the condition, the yield of DOPO-ITA is 91% with a nitrogen inlet.