一种窄分布聚合物GETPE自动分级制备方法研究

Study on automatic classification preparation method of a narrowly distributed polymer GETPE

采用半制备型凝胶渗透色谱(GPC)仪进行聚叠氮缩水甘油醚基含能热塑性弹性体(GETPE)窄分布聚合物自动分级制备方法的试验,确定了色谱制备最优条件:色谱柱为PLgelMIXED–D(300 mm×25 mm,10.0μm),流动相为四氢呋喃,流速为6.0 mL/min,自动进样器进样量为900μL,进样质量浓度为40 mg/mL,柱温为40℃,三通阀经过检测器和馏分收集器的体积流量比为1:5。严格控制制备色谱条件,采用馏分收集器进行多次收集、混批、合并,通过旋转蒸发的方式进行样品浓缩,获得质量为20 g,技术指标满足相对分子质量20 000±2 000、分子量分布<2.0的GETPE窄分布样品。该方法具有控制精准、自动化程度高的优点。

The test of automatic classification preparation method for the narrow distribution polymer of polyazido glycidyl ether-based energetic thermoplastic elastomer(GETPE)was carried out using the semi-preparative gel permeation chromatograph(GPC)instrument.The optimal conditions for chromatographic preparation were confirmed:the chromatographic column was PLgel MIXED-D(300 mm×25 mm,10.0μm),the mobile phase was tetrahydrofuran,the flow rate was 6.0 mL/min,the injection volume of the automatic sampler was 900μL,the sample mass concentration was 40 mg/mL,the column temperature was 4o C,and the volume flow ratio of the three-way valve passing through the detector and the fraction collector was l:5.The preparative chromatographic conditions were strictly controlled,and a fraction collector was used for multiple collecting,batch mixing and merging,and the sample was concentrated by rotary evaporation to obtain a narrowly distributed sample of GETPE with the mass of 20 g and technical specifications satisfying the relative molecular mass of 20000±2000 and the molecular weight distribution of<2.0.This method has the advantages of precise control and high degree of automation.