反相高效液相色谱表征无定型聚芳醚酮(砜)成环解聚产物

Characterization of Cyclo-depolymerization Products of Amorphous Polyether Ketone (Sulfones) by Reversed Phase High Performance Liquid Chromatography

建立了一种反相高效液相色谱表征无定型聚芳醚酮(砜)成环解聚产物的新方法。采用岛津VP-ODSC18反相色谱柱(150mm×4.6mm;5μm,i.d.),以四氢呋喃/水为流动相,流速1.0mL/min,梯度淋洗方式;254nm紫外检测,由此方法可将全部同系物组分有效地分离并可准确给出产物中各环状低聚体组分的百分含量。分析结果表明,酚酞聚醚酮、酚酞聚醚砜、双酚A聚砜经成环解聚反应高产率得到环状聚合体,最高成环率达97.57%。通过与激光质谱的比较证实了HPLC方法更适合于对成环解聚产物体系的表征。

A gradient elution method for the characterization of cyclo-depolymerization products of amorphous polyether ketone（sulfone） by reversed phase high performance liquid chromatography was proposed. On a SHIMADZU CIS ODS column（ 150 mm ×4.6 mm, 5 μm i. d. ）, using tetrahydrofuran（THF）/H2O as mobile phase with a flow rate of 1.0 mL/min and detection wavelength of 254 nm, all cyclic components were separated effectively and contents of cyclic oligomers were gained accurately. Results show that polyether ketone-C （ PEK-C）, polyether sulfones-C （ PES-C ）, bisphenol A polysulfone （PBS） convert in good yield to a family of macrocycles through cyclo-depolymerization, the highest yield gets to 97.57% . The comparison with MALDI- TOF-MS proves that HPLC is more suitable for characterization of cyclo-depolymerization product.