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

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 %。  

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

A novel phosphorus-containing flame-retardant, intermediate 4-hydroxy(6-oxido-6H-dibenzo c, e1, 2oxaphosphinin-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 ℃, while mol ratio of DOPO to 1, 4-phthaladehyde 1.1:1. 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 ℃, and the amount of residue(char yield) at 800 ℃ is 29.7%