在150℃～230℃条件下,以氯化1-丁基-3-甲基咪唑离子液体与水组成的二元混合体系为介质进行尼龙6的解聚研究。固相残余物利用红外光谱和差示扫描量热仪进行分析。液相产物通过液相色谱-质谱联用仪和液相色谱进行定性与定量分析。建立了反应温度（A）、混合体系中离子液体的物质的量分数（B）以及反应时间（C）与ε-己内酰胺回收率（Y）之间的数学模型：Y（%）=43.76＋6.69A＋6.06B＋3.60C＋3.15AB＋3.48AC-17.06A2-16.56B2-14.18C2,并利用响应曲面法（RSM）确定了解聚的优化工艺条件,即反应温度175℃、离子液体的物质的量分数14.2%及反应时间7.3h,此时ε-己内酰胺的回收率为44.4%、尼龙6的降解率为88.4%。
Depolymerization of nylon6 to ε-caprolactam was carried out in the ionic liquids and water binary mixtures from 150 to 230 ℃.The products of depolymerization were analyzed by means of infrared spectroscopy,differential scanning calorimeter,liquid chromategraphy-mass spectrometry and high performance liquid chromatography.Response surface methodology（RSM）,based on three-variable-three-level Box-Behnken design（BBD）,was used to determine the effects of the main parameters on nylon 6 depolymerization.A express of Y（%）=43.76＋6.69A＋6.06B＋3.60C＋3.15AB＋3.48AC-17.06A2-16.56B2-14.18C2 was established to determine the yield of caprolactam at different reaction temperature（A）,the ILs＇ molar ratio（B）,and reaction time（C）.The optimal conditions for depolymerization was as follows： reaction temperature of 175 ℃,the molar ratio of IL 14.2%,and reaction time of 7.3 h.Under the condition,the yield of ε-caprolactam is 44.4% and the degradation rate of nylon 6 is 88.4%.
参考文献
| [1] | Ranu BC;Banerjee S;Das A .Catalysis by ionic liquids: cyclopropyl carbinyl rearrangements catalyzed by [pmim]Br under organic solvent free conditions[J].Tetrahedron letters: The International Journal for the Rapid Publication of Preliminary Communications in Organic Chemistry,2006(6):881-884. |
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