含米氏酸型双马来酰亚胺的合成及结构表征

Synthesis and Structural Characterization of Meldrum’s Acid Containing Bismaleimide

首先以米氏酸、4-硝基苄氯为原料合成二硝基化合物(MADN),并将其还原为二元胺化合物(MADA),再用MADA与马来酸酐反应得到含米氏酸型双马酰亚胺(BMI-MAM)。采用核磁共振氢谱(^(1)H NMR)、核磁共振碳谱(^(13)C NMR)和红外光谱(FTIR)对MADN、MADA和BMI-MAM进行结构表征。采用差示扫描量热仪(DSC)和热重分析仪(TG)测试了BMI-MAM单体和聚合物P(BMI-MAM)的热稳定性,同时采用了FTIR对P(BMI-MAM)的结构进行了表征。结果表明,成功制备了MADN、MADA和BMI-MAM,且P(BMI-MAM)具有较好的热稳定性(T_(d,5)=425.0℃),较高的残炭率(CY_(800℃)=55.5%),因此拓宽了双马来酰亚胺在改性剂、碳材料等领域的应用。

The dinitro-compound(MADN)was synthesized from Meldrum's acid and 4-nitrobenzyl chloride,and further it was reduced to diamine compound(MADA).Then the Meldrum's acid containing bismaleimide(BMI-MAM)was obtained by the reaction of MADA and maleic anhydride.The structures of MADN,MADA and BMI-MAM were characterized by hydrogen magnetic resonance(^(1)H NMR),carbon magnetic resonance(^(13)C NMR)and Fourier transform infrared spectroscopy(FTIR).The thermal stability of BMI-MAM monomer and polymer[P(BMI-MAM)]was tested by differential scanning calorimeter(DSC)and thermogravimetric analyzer(TG),and the structure of P(BMI-Mam)was characterized by FTIR.The results show that MADN,MADA and BMI-MAM are successfully prepared,and P(BMI-MAM)has good thermal stability(T_(d,5)=425.0℃)and high char yield(CY_(800℃)=55.5%),broadening the application of bismaleimide in the fields of modifier and carbon materials.