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多功能橡胶助剂PDM的低温溶剂法合成工艺研究 |
Low-temperature Solvent Synthesis Process of Multifunctional Rubber Auxiliaries PDM |
Received:January 12, 2021 Revised:February 01, 2021 |
DOI:10.12137/j.issn.2095-5448.2021.05.0241 |
中文关键词: 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 |
英文关键词: N,N′-m-phenylene dimaleimide synthesis process orthogonal experiment amidation reaction dehydration and ring-closure |
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中文摘要: |
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 1.5 h;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3 h时,PDM的收率和熔点较高,且反应易于控制。 |
英文摘要: |
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:dehydration and ring-closure reaction temperature 40 ℃,maleic anhydride/m-phenylenediamine substance ratio 2.2,amidation reaction temperature 25 ℃,amidation reaction time 1.5 h.When the mass ratio of DMF/m-phenylenediamine was 8,the mass 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. |
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