聚硅氧烷酯类液晶(PMMS)气相色谱固定液的研究——Ⅰ.侧链为苯甲酸联苯酚酯型的PMMS

Synthesesand Properties of Poly-(methylsiloxane) Type Liquid Crystals (PMMS) as Gas Chromatographic Stationary Phase Ⅰ. PMMSs with Side Chain of Biphenyl Benzoate Type

设计并合成了聚甲基硅氧烷酯(PMMS),其侧键为4-n-烷氧基联苯酚苯甲酸酯型的计8个,具类似结构侧键的计5个。合成的中间伴和产物分别由MS、NMR、IR和EAR等分析方法得到证实。并用IR谱图说明了硅氢加成反应的进行。相变温度的测定结果,表明这些PMMS大多具有较宽的液晶相温度范围(大于100℃)。毛细管气相色谱的测定表明,PMMS-AOBPAIOB既有SE-52的高柱效和热稳定性,又有BBBT的优异分离性能。PMMS-A_m~*OBPAIOB的填充柱有优异的分离选择性,可以有效地分离喳啉、异喳啉和2-甲基喳啉。表明了作为固定液,PMMS兼有硅油和液晶的特点。

8 PMMSs with side chain of 4-n-alkoxybiphenyl-4'-yl-benzoate and 5 with similar side chain were designed and synthesized. The intermediates and final PMMSs were identified by using NMR, IR, MS, EAR and so on. Most of them have a wide mesogenic temperature range (more than 100℃). PMMSs have shown high efficiency and thermal stability (similar to SE-52) as well as selectivity (similar to BBBT) in capillary column of GC. In packed column of GC, PMMS-Am ~*OBPA1OB shows a good result of the separation of Quinoline, Isoquinoline and 2-Methylquinoline. PMMS is useful as GC stationary phase with the characteristic of the siloxane and the liquid crystal.