有机硅改性席夫碱聚氨酯型液晶固定相的制备、表征及色谱性能

Synthesis,Characterization and Chromatographic Performance of Schiff-base Type Silicone Polyurethane Liquid Crystal Polymer

以对苯二胺、3-氯丙醇和4-羟基苯甲醛为原料,合成对苯二（对苯丙氧基醇）亚胺液晶基元,再与对苯二异氰酸酯和1,3-双（3-氨基丙基）四甲基二硅氧烷反应,合成席夫碱型硅氧烷聚氨酯液晶聚合物。通过红外光谱法、X射线衍射、热分析、偏光显微镜等技术手段对其结构和性能进行了表征。结果表明,该物质为席夫碱有机硅聚氨酯液晶聚合物,属于近晶相液晶,液晶区间为103-150℃,热分解温度为300℃。用席夫碱型硅氧烷聚氨酯液晶固定相制备填充色谱柱,考察固定液的相对极性及其对取代苯位置异构体的色谱分离性能。合成的席夫碱型硅氧烷聚氨酯液晶聚合物的液晶温度范围为103-146℃,属于强极性固定液（Px=79）,各组分色谱峰的分离度为0.96-3.33。

Abstract A new kind of small molecule Schiff base liquid crystal unit, p-phenylene （p-styrene acrylic oxo alcohol） imine was synthesized using hydroxybenzaldehyde, 3-chloropropanol, p-phenylenediamine as raw meterials. Schiff base type silicone polyurethane liquid crystal polymer was synthesized by the liquid crystal unit, 1,4-phenylene diisocyanate and 1, 3-bis （ 3-aminopropyl ）-1, 1, 3, 3-tetramethyldisiloxane. The construction of liquid crystal unit and the silicone liquid crystalline polymer were characterized by Fourier transform infrared spectrometry. The crystal structures of the liquid crystal unit and the Schiff base type silicone polyurethane liquid crystal polymer liquid crystal were identified by X-ray diffraction. The liquid crystal phase and phase transition temperature of the Schiff base type silicone polyurethane liquid crystal polymer were investigated by differential scanning calorimetry. The phase change process and optical properties of the liquid crystal material were observed by polarizing optical microscope. The chromatography column was made using Schiff base type silicone polyurethane liquid crystal polymer as stationary phase. The relative polarity of stationary liquid and the chromatographic separation performance for substituted benzene isomers were determined. Liquid crystal temperature ranges of the liquid crystal polymer are 103 ~ 146 ~C. It belongs to strongly polar stationary liquid （Px = 79）, the separation degree of the chromatographic peaks are O. 96 -3.33.