无溶剂法混合催化剂催化多聚甲醛合成α-氰基丙烯酸酯

The α-cyanoacrylate synthesized by paraformaldehyde at solvent-free andmixed catalysts

无溶剂时将多聚甲醛和α-氰基乙酸正丁酯在混合催化剂(三乙醇胺、六氢吡啶)作用下进行反应,合成了医用黏合剂用α-氰基丙烯酸正丁酯单体。探讨了混合催化剂掺量、反应温度对上述合成反应的影响。研究结果表明:以n(α-氰基乙酸正丁酯)=1 mol为基准,以收率为考核指标,采用正交试验法优选出合成反应的最佳工艺条件是反应温度为85℃、n(三乙醇胺)=10.7 mmol和n(六氢吡啶)=4.0 mmol;红外光谱(FT-IR)法、核磁共振氢谱(1H-NMR)法的表征结果,证实了该单体的预期结构被成功合成;采用气相色谱(GC)法、万能试验机和黏度计对该单体的性能进行了检测,证实了该单体的收率为78.24%、纯度较高且性能有所改善。

A n-butyl a-cyanoacrylate monomer for medical adhesive was synthesized by reaction between paraformaldehyde and n-butyl or-cyanoacetate under action of mixed catalysts （such as triethanolamine, hexahydropyridine） at solvent-free. The inflUences of mixed catalyst contents and reaction temperatures on above synthetic reaction were discussed. The research results showed that the optimal process conditions of synthetic reaction were preferred by orthogonal experiment with 1 mol n-butyl α-cyanoacetate as a benchmark, yield as evaluation index, when reaction temperature was 85 ℃, triethanolamine and hexahydropyridine were 10.7, 4.0 mmol respectively. It was confirmed that the expectation structure of monomer was successfully synthesized by infrared spectroscopy （FT-IR） and nuclear magnetic resonance hydrogen spectrum （1H-NMR）. The properties of monomer were tested by gas chromatography （GC）, universal tester and viscosimeter, so it was confirmed that the monomer had the 78.24% yield, higher purity and somewhat improved properties.