摘要
研究以顺丁烯二酸酐和间苯二胺为原料,N,N′-二甲基甲酰胺(DMF)为溶剂,乙酸酐为脱水剂合成N,N′-间苯双马来酰亚胺(PDM)的工艺。结果表明:正交试验得出PDM合成的最优方案为脱水闭环反应温度40℃,顺丁烯二酸酐/间苯二胺物质的量比2.2,酰胺化反应温度25℃,酰胺化反应时间1.5h;DMF/间苯二胺质量比为8、乙酸酐/间苯二胺的物质的量比为2.4、脱水闭环反应为3h时,PDM的收率和熔点较高,且反应易于控制。
The synthesis process of N,N′-m-phenylene dimaleimide(PDM)using maleic anhydride and m-phenylenediamine as raw materials,N,N′-dimethylformamide(DMF)as solvent,and acetic anhydride as dehydrating agent.The results showed that,the optimal scheme of PDM synthesis obtained by orthogonal experiment was as follows:dehydration and ring-closure reaction temperature 40℃,maleic anhydride/m-phenylenediamine molar ratio 2.2,amidation reaction temperature 25℃,and amidation reaction time1.5 h.When the mass ratio of DMF/m-phenylenediamine was 8,the molar ratio of acetic anhydride/m-phenylenediamine was 2.4,and the dehydration and ring-closure reaction time was 3 h,the yield and melting point of PDM was higher and the reaction was easy to control.
作者
郑记栓
张振飞
张永旺
郑瑞谦
ZHENG Jishuan;ZHANG Zhenfei;ZHANG Yongwang;ZHENG Ruiqian(Puyang Hongtianwei Pharmaceutical Co.,Ltd,Puyang 457000,China;Puyang Zhongyuan Petrifaction Industry Co.,Ltd,Puyang 457000,China;Henan Yuanbo New Material Co.,Ltd,Puyang 457163,China;Beijing Zhongke Sanqing Environmental Technology Co.,Ltd,Beijing 100094,China)
出处
《橡胶科技》
2021年第5期241-243,共3页
Rubber Science and Technology
关键词
N
N′-间苯双马来酰亚胺
合成工艺
正交试验
酰胺化
脱水闭环
N,N′-m-phenylene dimaleimide
synthesis process
orthogonal experiment
amidation reaction
dehydration and ring-closure
