CIESC Journal ›› 2024, Vol. 75 ›› Issue (4): 1718-1723.DOI: 10.11949/0438-1157.20231411

• Material science and engineering, nanotechnology • Previous Articles     Next Articles

Fluorine spectrum analysis and structural characterization of Y-type perfluoropolyether carboxylic acid

Wenhui ZHANG1(), Ruyi TANG1, Xili CUI1,2(), Huabin XING1,2   

  1. 1.College of Chemical and Biological Engineering, Zhejiang University, Hangzhou 310027, Zhejiang, China
    2.ZJU-Hangzhou Global Scientific and Technological Innovation Center, Hangzhou 311200, Zhejiang, China
  • Received:2023-12-13 Revised:2024-03-26 Online:2024-06-06 Published:2024-04-25
  • Contact: Xili CUI

羧酸端基Y型全氟聚醚的氟谱解析及结构表征

张文惠1(), 唐茹意1, 崔希利1,2(), 邢华斌1,2   

  1. 1.浙江大学化学工程与工业生物工程学院,浙江 杭州 310027
    2.浙江大学杭州国际科创中心,浙江 杭州 311200
  • 通讯作者: 崔希利
  • 作者简介:张文惠(2000—),女,博士研究生,zhang_wenhui@zju.edu.cn
  • 基金资助:
    浙江省尖兵领雁研发攻关计划项目(2023C01187);国家自然科学基金项目(22122811)

Abstract:

Perfluoropolyether and their derivatives (PFPEs) are a class of fluoropolymers with high added value. Their specific physicochemical properties make them have a good commercial prospect. At present, domestic related products are heavily dependent on imports, and there is a lack of research on PFPEs, especially on Y-type PFPEs, so it is urgent to strengthen the development and research in related fields. Nuclear magnetic resonance fluorine spectroscopy (19F NMR) is an important technique for the structure analysis of perfluorinated polyether compounds. However, due to technical blockade and difficulties in preparation, the analysis of 19F NMR spectroscopy of Y-type PFPE carboxylic acid (PFPE-CA) is still not perfect. In this study, appropriate sample preparation conditions were used to obtain a clear 19F NMR spectrum of Y-type PFPE-CA, and chemical shifts of F atoms in different chemical environments in the main chain and end group were assigned. The composition of the active mixture and the number average molecular weight of the sample can be calculated by integrating the spectral peaks. This analysis method is accurate and fast, and provides a research basis for the breakthrough of production and separation technology of Y-type PFPEs.

Key words: perfluoropolyether carboxylic acid, Y-type, structural analysis, polymers, electronic materials

摘要:

全氟聚醚及其衍生物(PFPEs)是一类高附加值的含氟聚合物,特异的理化性质使其具有较好的商业前景。目前国内相关产品严重依赖进口,对PFPEs的研究比较缺乏,尤其对Y型PFPEs的研究非常少,亟需加强对相关领域的开发和研究。核磁共振氟谱(19F NMR)是解析PFPEs结构的重要技术,但由于技术封锁、制备困难等原因,有关Y型PFPE羧酸(PFPE-CA)的19F NMR谱图解析尚不完善。本研究采用合适的制样条件,得到了清晰的Y型PFPE-CA的19F NMR谱图,并对主链和端基中不同化学环境的F原子化学位移进行归属。对谱峰进行积分可计算活性混合物的组成以及样品的数均分子量。该分析方法准确、快捷,可为Y型PFPEs的生产及分离技术的突破提供研究基础。

关键词: 全氟聚醚羧酸, Y型, 结构解析, 聚合物, 电子材料

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