4-[(6-氧-6H-二苯并(c,e)(1,2)氧磷杂己烷-6-取代)羟甲基]苯甲醛的合成与表征  

Synthesis and Characterization of 4-[Hydroxy( 6-Oxido-6H-dibenzo[c,e][1,2]oxaphosphinin-6-yl) methyl]benzaldehyde

作　　者：毛飞飞[1] 刘访琴 周玲[1] 孙一峰[2] 刘治国[1] 

机构地区：[1]西华大学理学院,四川成都610039 [2]中国广州分析测试中心,广东广州510070

出　　处：《西华大学学报（自然科学版）》2015年第6期73-76,共4页Journal of Xihua University:Natural Science Edition

基　　金：西华大学创新基金(Ycjj2015164);西华大学创新基金(Ycjj2014042)

摘　　要：以对苯二甲醛和9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)为原料合成新型含醇羟基和醛基的有机磷阻燃剂中间体4-[(6-氧-6H-二苯并(c,e)(1,2)氧磷杂己烷-6-取代)羟甲基]苯甲醛(DOPO-HO-BD)。探讨原料比和反应温度对反应结果的影响,结果表明,DOPO与对苯二甲醛摩尔比为1.1∶1、反应温度30℃时与二氧六环中反应7 h,DOPO-HO-BD收率为89.3%。采用傅里叶红外光谱(FT-IR)、核磁共振和质谱表征了DOPO-HO-BD的结构,热失重分析结果证明,DOPO-HO-BD初始分解温度为211℃(质量损失率1%),800℃时残炭率高达29.7%。A novel phosphorus- containing flame- retardant,intermediate 4-[hydroxy（ 6- oxido- 6H- dibenzo[c,e][1,2]oxaphosphinin- 6- yl]methyl） benzaldehyde（ DOPO- HO- BD）,was successfully synthesized by the reaction of 1,4- phthalaldehyde with 9,10- dihydro- 9- oxa- 10- phosphaphenan- threne- 10- oxide（ DOPO） in dioxane solution. The experimental results indicate that the yield of DOPO- HO- BD is 89. 3% under 7 h of reaction at 30 ° C,while mol ratio of DOPO to 1,4- phthaladehyde1. 1∶ 1. The structure of DOPO- HO- BD was characterized with Fourier transform infrared spectrometry（ FT- IR）,nuclear magnetic resonance spectrometry（ NMR） and mass spectrometry（ MS）. Thermogravimetric（ TG） analysis results show that the initial decomposition temperature at 1% mass loss of DOPO- HO- BD is 211 °C,and the amount of residue（ char yield） at 800 °C is 29. 7%

关 键 词：含磷阻燃剂 对苯二甲醛 中间体 

分 类 号：TQ016.1[化学工程] TQ265.1