磷酸二苯酯催化聚己内酯多元醇的合成毕业论文
2021-12-29 21:21:36
论文总字数:21253字
摘 要
聚酯多元醇是指在特定条件下,由多元酸与多元醇,经过酯化,脱水,聚合反应后,得到的一种高分子材料。根据反应条件,原材料,工艺方法的不同,所得的聚酯多元醇的性能也不相同。而这其中,脂肪族聚酯,以其优异的生物相容性,生物可降解性,以及其他理化性质,而脱颖而出,并逐渐成为了当下的研究热点之一。
本文采用有机化合物为催化剂,制备脂肪族聚酯,分别设计了四组不同的反应体系。第一组以己内酯为单体,戊二胺为引发剂,1,5,7-三叠氮双环 [4.4.0]癸-5-烯(TBD)为催化剂,比例分别为30:1:0.5、50:1:0.5和80:1:0.5。反应温度均为25℃,分别在反应1小时,2小时,12小时时取样,测得分子量分别为3240 g mol-1、4750 g mol-1和8310 g mol-1。PDI分别为1.10、1.13和1.17,转化率为95 %、90 %和91 %。第二组以己内酯为单体,2,2'-二硫二乙醇为引发剂,磷酸二苯酯(DPP)为催化剂,比例分别为30:1:0.5、50:1:0.5和100:1:0.5。反应温度均为50℃,分别在反应1小时,2小时,24小时时取样,测得分子量分别为2520 g mol-1、4540 g mol-1和9290 g mol-1。PDI分别为1.09、1.11和1.21,转化率为80 %、96 %和91 %。第三组以丙交酯为单体,戊二胺为引发剂,TBD为催化剂,比例分别为50:1:0.1、100:1:0.1和200:1:0.2。反应温度均为25℃,分别在反应2分钟,5分钟,10分钟时取样,测得分子量分别为6760 g mol-1、12260 g mol-1和23540 g mol-1。PDI分别为1.10、1.23和1.19,转化率为99 %、99 %和99 %。第四组以丙交酯为单体,2,2'-二硫二乙醇为引发剂,TBD为催化剂,比例分别为50:1:0.1、80:1:0.1和100:1:0.2。反应温度均为25℃,分别在反应5分钟,5分钟,10分钟时取样,测得分子量分别为6500 g mol-1、9070 g mol-1和12600 g mol-1。PDI分别为1.23、1.29和1.54,转化率为91 %、90 %和91 %。
关键词 聚己内酯 开环聚合 有机催化剂 磷酸二苯酯
ABSTRACT
Polyester polyol is a kind of polymer material which is produced by esterification, dehydration and polymerization of polyacid and polyol under specific conditions. The difference in the reaction conditions, raw materials and processing methods accounted for the varied properties. Among them, aliphatic polyester, with its excellent biocompatibility, biodegradability, and other physical and chemical properties is one of the current research hot spots.
In this paper, organic compounds are used as catalysts to prepare aliphatic polyesters, and four different reaction systems are designed. The first group uses caprolactone as the monomer, pentanediamine as the initiator, 1,5,7-triazide bicyclo [4.4.0] dec-5-ene (TBD) as the catalyst, and the ratios are 30: 1 : 0.5, 50: 1: 0.5 and 80: 1: 0.5. The reaction temperature was 25℃. Samples were taken at 1 hour, 2 hours, and 12 hours, and the measured molecular weights were 3240 g mol-1, 4750 g mol-1, and 8310 g mol-1. The PDI was 1.10, 1.13 and 1.17, and the conversion rates were 95%, 90% and 91%. The second group uses caprolactone as the monomer, 2,2'-dithiodiethanol as the initiator, and diphenyl phosphate (DPP) as the catalyst. The ratios are 30: 1: 0.5, 50: 1: 0.5 and 100 : 1: 0.5. The reaction temperature was 50℃. Samples were taken at 1 hour, 2 hours and 24 hours, and the measured molecular weights were 2520 g mol-1, 4540 g mol-1 and 9290 g mol-1. The PDI was 1.09, 1.11 and 1.21, and the conversion rates were 80%, 96% and 91%. The third group uses lactide as the monomer, pentanediamine as the initiator, and TBD as the catalyst. The ratios are 50: 1: 0.1, 100: 1: 0.1, and 200: 1: 0.2. The reaction temperature was 25 ℃, samples were taken at 2 minutes, 5 minutes and 10 minutes respectively, and the measured molecular weights were 6760 g mol-1, 12260 g mol-1 and 23540 g mol-1. The PDI was 1.10, 1.23 and 1.19, and the conversion rates were 99%, 99% and 99%. The fourth group uses lactide as the monomer, 2,2'-dithiodiethanol as the initiator, and TBD as the catalyst. The ratios are 50: 1: 0.1, 80: 1: 0.1, and 100: 1: 0.2. The reaction temperature was 25℃. Samples were taken at 5 minutes, 5 minutes, and 10 minutes respectively, and the measured molecular weights were 6500 g mol-1, 9070 g mol-1, and 12600 g mol-1. The PDI was 1.23, 1.29 and 1.54, and the conversion rates were 91%, 90% and 91%.
KEYWORDS Polycaprolactone;Ring opening polymerization;Organic catalyst;Diphenyl phosphate;
目录
摘 要 I
ABSTRACT III
第一章 绪 论 1
1.1 引言 1
1.2 脂肪族聚酯 1
1.2.1 聚己内酯 1
1.2.2 聚丙交酯 1
1.3 开环聚合的有机催化体系 2
1.3.1 碱催化体系 2
1.3.2 酸催化体系 4
1.3.3 酸碱共催化体系 4
1.3.4 双官能团催化体系 5
1.4 研究意义和目的 7
第二章 磷酸二苯酯催化聚己内酯多元醇的合成与表征 8
2.1 引言 8
2.2 实验方法 8
2.2.1 实验试剂与仪器 8
2.2.2 合成方法 8
2.3 结果与讨论 11
2.3.1 聚己内酯多元醇的合成 11
2.3.2 聚丙交酯多元醇的合成 12
2.3.3 表征与分析 13
第三章 结论与展望 19
3.1 结论 19
3.2 展望 19
参考文献 20
致谢 22
绪 论
引言
脂肪族聚酯具有十分优异的生物相容性以及生物可降解性。所以,近年来,脂肪族聚酯在生物医药,基因传递,高分子领域等诸多不同的方面都有着尤为突出的表现,得到了广泛的应用。因此,如何能够使得制备脂肪族聚酯的工艺流程更环保,效率更高,经济收益最大,是目前需要不断努力,深入研究的热点问题之一。
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