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以顺丁烯二酸酐和4,4’-二氨基二苯基甲烷(DDM)为原料,采用甲苯为溶剂、共沸蒸馏法,分别用一步法和两步法合成N,N’-4,4’-二苯甲烷双马来酰亚胺(BDM)。通过产物核磁氢谱、红外色谱、示差扫描量热(DSC)及产物收率的计算和双键含量、酸值、凝胶时间、凝胶温度等的测定,对BDM一步法、两步法合成工艺进行了研究并对两种方法中生成的副产物进行了分析。结果表明,一步法比两步法产品产率有很大提高,得到的残渣较少,主要是由DDM与BDM的加成反应生成的低聚物,重新利用价值较小;两步法副产物较多,如高温条件下BMA发生分子间脱水形成的线形低聚物,其可以水解成BMA重新利用。
Using maleic anhydride and 4,4’-diaminodiphenylmethane (DDM) as raw materials, using toluene as solvent and azeotropic distillation, N, N’-4, 4’-diphenylmethane bismaleimide (BDM). The BDM one-step and two-step synthesis methods were determined by NMR, IR, differential scanning calorimetry (DSC) and product yield calculation, double bond content, acid value, gel time and gel temperature. The process was studied and the by-products generated in the two methods were analyzed. The results showed that the product yield of the one-step method and the two-step method were greatly improved, and the residue obtained was less, mainly due to the oligomer formed by the addition reaction of DDM and BDM, with less re-use value. The two-step by-product More, such as under the high temperature BMA intermolecular dehydration linear oligomer formed, which can be hydrolyzed into BMA re-use.