芳香族液晶聚酯的组成分析  

Components Analysis of Aromatic Liquid Crystalline Polyester

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)

机构地区：[1]金发科技股份有限公司企业技术中心,广东广州510663 [2]珠海万通特种工程塑料有限公司,广东珠海519050

出　　处：《塑料工业》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)。

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.

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 

分 类 号：TQ324[化学工程—合成树脂塑料工业]