超支化聚缩水甘油氟封端研究.pdf

超支化聚缩水甘油的氟封端研究
摘要
本文利用对外部羟基保护的方法成功将线形氟碳链和超支化聚
缩水甘油的内部羟基反应合成了内部以线形氟碳链为臂的内部亲
油外部亲水的氟改性超支化聚缩水甘油并通过核磁共振 NMR
红外光谱 IR 液相色谱质谱联用 LC-MS ,凝胶渗透色
谱(GPC),元素分析 EA 等表征手段对其分子量支化度等分
子结构信息和氟含量羟基转化率进行了表征得到其支化度为
内部羟基反应率为 30 左右主要是线性单元 L14 参与反应
利用差热分析 DSC 乌氏粘度仪等测试方法对其结晶性能
热性能特征粘度进行了初步研究发现该聚合物在测试范围内
为无定型态具有较低的玻璃化转变温度改性后聚合物玻璃化转
变温度提高改性后的聚合物特征粘度也有很大的提高
另外本文研究比较了两种合成方法中的羟基转化率 1 将第三
章的产物和全氟醋酸酐反应 2 将超支化聚缩水甘油和全氟醋酸酐
直接反应用 IR NMR 对两种合成方法得到的产物进行表征分
析比较羟基转化率通过红外测试看到前一种合成方法使更多的
羟基参加了反应通过核磁测试对羟基含量进行计算发现前一种
合成方法羟基反应率达 而后一种合成方法的羟基反应率为

该聚合物在其在添加剂润滑剂和涂料方面有广阔的应用前
景其内部亲油外部亲水结构独特同时聚缩水甘油和氟碳聚
合物都具有良好的生物相容性相信在生物医药方面将会有潜在
的应用另外利用超支化聚合物内外部官能团的性质差别进
行分步接枝的合成方法能够在超支化聚合物改性研究中得到广
泛应用
关键词超支化缩水甘油氟保护法羟基转化率
By protecting the outer hydroxyl groups, linear perfluroalkyls
were essfully grafted into the inner hydroxyl groups in
hyperbranched polyglycidol. The resulting polymers were
characterized by 13C- NMR, IR, LC-MS, EA, GPC, DSC, and Ubbelohde
eter. The important parameters about structure were obtained. The
Degree of branching (DB) is . The conversion of inner hydroxyl groups
is 30 , and the hydroxyl groups took reaction are mainly linear units (L14).
XRD and DSC results suggest the sample is amorphous within the
experiment range. The differences between the spin-spin relaxation times
indicate that terminal segments of star are more flexible than the core.
Crystallinity, thermal property and viscosity were investigated by
DSC and Ubbelohde eter. In the range of testing temperature, the
polymers are amorphism, and have very low Tg. Tg of modified
hyperbranched polyglycidol is higher than Tg of hyperbranched
polyglycidol. And viscosity has the same trend.
Moreover, pared hydroxyl groups’percent conversion
between synthesis method based on inner grafted hyperbranched
polyglycidol and the one based on hyperbranched polyglycidol. Through
IR, we see that the first method have higher conversion. Through NMR, we
computed the conversion which is 4