由环己酮制备聚己内酯的反应研究+文献综述
毕业论文关键词: 环己酮；ε-己内酯；聚已内酯；苯甲醛；1,2-二氯乙烷，钛酸丁酯
Research on the Preparation of Polycaprolactone by Cyclohexanone
Abstract：The paper introduces the property and synthesis and applications of the PCL. We introduced the optimized conditions on the preparation of ε-caprolactone by oxidation of cyclohexanone, and discussed the direction of development of the PCL. With cyclohexanone as raw material, through the Baeyer-Villiger oxidation reaction to get ε-caprolactone for the preparation of polycaprolactone, then we used infrared spectrum for synthetic inspection. The results of the optimal reaction conditions for preparation of ε-caprolactone by cyclohexanone showed as follows: 50mL 1,2-dichloroethane,the molar ratio of formaldehyde/cyclohexanone is 2:1, the mass ratio of cyclohexanone/catalyst is 1:0.05. Reaction temperature 15 ℃, in the case of oxygen into the reactor through 12h.Cyclohexanone conversion rate of 93.21%.The optimal reaction conditions for preparation of PCL is that reaction temperature controled about 140 ℃, and butyl titanate as the initiator which reacting about 4h.
Keywords:cyclohexanone;ε-caprolactone;polycaprolactone;benzaldehyde;1,2-dichloroethane;Butyl titanate
目录
1 文献综述 1
1.1 选题背景 1
1.2 课题选择的意义 2
2 ε-己内酯的合成 2
2.1 环己酮氧化制备ε-己内酯 2
2.2 酞菁类仿生催化体系 4
3 聚己内酯的合成 5
3.1 聚己内酯的性能 5
3.2 ε-己内酯(CL）的聚合 6
3.2.1 活泼氢引发体系 6
3.2.2 阳离子型催化剂 6
3.2.3 阴离子型催化剂 6
4 实验部分 7
4.1 实验方案 7
4.1.1 研究方案 7
4.1.2 方案论证 7
4.2 主要试剂和实验仪器 7
4.2.1 主要试剂 7
4.2.2 实验仪器 8
4.3 ε-己内酯的合成 9
4.3.1 实验步骤 9
4.3.2 后处理方法 9
4.3.3 产物结构的鉴定 9
4.3.4 产物分析方法 10
4.3.5 标准曲线的绘制 10
4.3.6 ε-己内酯定量分析的数据处理 13
4.3.7 实验结果和讨论 13
4.3.8 小结 18
4.4 聚己内酯的合成 18
4.4.1 引发剂的选择 18
4.4.2 ε-己内酯的纯化 19
4.4.3 聚己内酯的聚合 19
4.4.4 所得聚己内酯的纯化 19
4.4.5 聚己内酯的红外表征 20
4.4.6 小结 21
5 总结 21
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