摘要
具有功能性端基的全氟聚醚具有优异的化学稳定性及较强的加工可塑性,被广泛用于航天航空、电子、化工等领域。在其制备及应用过程中,基于核磁共振技术的结构表征和解析至关重要。然而由于全氟聚醚及其活性化合物的结构复杂、分子量大且分布较宽,因此在核磁测试中存在制样难、主链骨架结构和端基难以分辨和归属等问题,进而影响对全氟聚醚的定性定量分析。针对Z型惰性及活性全氟聚醚的结构解析,系统考察了不同种类氘代试剂和含氟助溶剂的复配、样品浓度、测试条件等因素的影响,探索得到较优的核磁样品制备条件;进一步分析了Z型全氟聚醚混合物的氟谱,确定了全氟聚醚的主链结构和端基的归属;利用端基分析法计算得到分子量及聚合度、两组分全氟聚醚混合物组成。
Perfluoropolyether(PFPE)with functional end groups possesses excellent chemical stability and strong processing plasticity,thus being widely applied in high-end fields such as aerospace,electronics,chemical engineering.During production and application,it’s significant to characterize and analyze PFPE structure based on nuclear magnetic resonance technology(NMR).However,due to structure complexity,high molecular weight and wide distribution of PFPE,there have been difficulties in preparing samples for NMR test,distinguishing and attributing the main chain structure and end groups in NMR spectra,which further affects qualitative and quantitative analysis of PFPE.In view of the structural analysis of Z-type PFPE,this study investigated combination of kinds of deuterated solvents and fluorinated cosolvent,sample concentration and test conditions,obtaining a better method of NMR sample preparation.The attribution of main chain structure and end groups of PFPE were determined.Also,the molecular weight,the degree of polymerization,and the composition of twocomponent PFPE mixture were calculated by analyzing the end groups of PFPE.
作者
唐茹意
潘罕骞
郑侠俊
张广欣
汪星平
崔希利
邢华斌
TANG Ruyi;PAN Hanqian;ZHENG Xiajun;ZHANG Guangxin;WANG Xingping;CUI Xili;XING Huabin(College of Chemical and Biological Engineering,Zhejiang University,Hangzhou 310027,Zhejiang,China;Zhejiang Juhua Technology Center Co.,Ltd.,Quzhou 324000,Zhejiang,China;ZJU-Hangzhou Global Scientific and Technological Innovation Center,Hangzhou 311200,Zhejiang,China)
出处
《化工学报》
EI
CSCD
北大核心
2023年第1期479-486,共8页
CIESC Journal
基金
国家自然科学基金项目(22122811,21938011)
浙江省杰出青年科学基金项目(LR20B060001)
衢州市科学技术局项目(2021NC02)。
关键词
全氟聚醚
官能端基的活性全氟聚醚
结构解析
化学分析
聚合物
混合物
perfluoropolyether
reactive perfluoropolyether with functional end groups
structure elucidation
chemical analysis
polymers
mixtures