摘要
芳香族液晶聚酯(LCP)难溶于常用溶剂,给其组成分析带来了巨大的挑战。针对这一问题,提出了基于胺解和水解效应的间接分析方法,对LCP的氢氧化钠水溶液(NaOH/H_(2)O)水解产物和乙醇胺(META)胺解产物进行了核磁共振氢谱(^(1)H NMR)表征,对N,O-双(三甲基硅基)-乙酰胺(BSTFA)修饰的氢氧化钠/甲醇/二甲基亚砜(NaOH/CH_3OH/DMSO)水解产物进行了^(1)H NMR和气相色谱-质谱(GC-MS)表征。通过对比发现,以NaOH/CH_(3)OH/DMSO为溶剂水解LCP是可将LCP充分单体化的优选溶剂,而采用GC-MS对单体化后的产物进行表征是获得精确单体物质的量比的优选方法,结合两者为LCP组分分析提供了一种高效、准确的方法。此外,表征方式均表明LCP在聚合过程中发生了不期望但无法避免的副反应和反应物升华,进而导致了单体的损失。
Aromatic liquid crystalline polyester(LCP)was insoluble in common solvents,leading to a big challenge for their components analysis with widely used direct characterization methods.To address this issue,indirect analysis methods were proposed based on the aminolysis and hydrolysis effects,with the ^(1)H NMR characterization for the LCP-based aqueous sodium hydroxide(NaOH/H_(2) O)hydrolysis product and monoethanolamine(META)aminolysis product,as well as the gas chromatograpy-mass spectrum(GC-MS)characterization for sodium hydroxide/methanol/dimethyl sulfoxide(NaOH/CH_(3) OH/DMSO)hydrolysis product modified with N,O-bis(trimethylsilyl)-acetamide(BSTFA).Comparisons have demonstrated that the treatment with NaOH/CH_(3) OH/DMSO contributes to hydrolysis with the most extents for LCP molecules into monomeric components,while the GC-MS characterization for the derivatives of these products is the most privacy one for determining the molar ratio of each monomer,thus offering an efficient and accurate method for a components analysis of LCP.Additionally,these characterizations highlights that a certain loss of monomers took place,due to unpleasant but seemingly unavoidable adverse chemical reactions or the reactant sublimations during the polymerization process.
作者
肖中鹏
徐显骏
黄险波
孙华伟
姜苏俊
曹民
XIAO Zhongpeng;XU Xianjun;HUANG Xianbo;SUN Huawei;JIANG Sujun;CAO Min(National-certified Enterprise Technology Center,Kingfa Science and Technology Co.,Ltd.,Guangzhou 510663,China;Zhuhai Vanteque Specialty Engineering Plastics Co.,Ltd.,Zhuhai 519050,China)
出处
《塑料工业》
CAS
CSCD
北大核心
2023年第6期87-91,共5页
China Plastics Industry
基金
广东省重点领域研发计划项目(2020B010179001)
珠海市产学研合作项目(ZH22017001200004PWC)。
关键词
液晶聚酯
组成分析
水解
N
O-双(三甲基硅基)-乙酰胺修饰
气相色谱-质谱
Liquid Crystalline Polyesters
Components Analysis
Hydrolysis
N,O-bis(trimethylsilyl)-acetamide Modification
Gas Chromatograpy-mass Spectrum
