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采用凝胶渗透色谱法(GPC),通过对二次催化溶胶-凝胶法制备硅胶微球原料硅酸乙酯40(TES40)、中间产物聚硅酸乙酯(PES)分子量的在线测定,实现了对反应过程的监控。采用Shodex KF-802凝胶色谱柱,以四氢呋喃为流动相,流速0.5mL/min,柱温40℃,采用示差折光检测器检测。校正曲线为lg Mw=-0.377VR+5.69,其中lg Mw为重均分子量对数,VR为淋洗液体积,线性相关系数r=0.9995,相对标准偏差(RSD)小于0.4%。结果表明:TES40分子量分布对PES分子量分布以及PES分子量分布对制得硅胶微球粒径都有较大影响。通过对TES40及PES分子量的控制可实现硅胶微球制备的重现。本方法高效、准确,样品处理简单,可用于二次催化溶胶-凝胶法制备硅胶微球过程的监控,有利于确保硅胶微球制备的重现性。
Gel permeation chromatography (GPC) was used to determine the molecular weight of silica gel microspheres (TES40) and the intermediate product polysilicate ethyl ester (PES) by the second catalytic sol-gel method. The monitoring of the reaction process. A Shodex KF-802 gel column was used with tetrahydrofuran as the mobile phase at a flow rate of 0.5 mL / min and a column temperature of 40 ° C., using a differential refractive index detector. The calibration curve is lg Mw = -0.377VR + 5.69, where lg Mw is the logarithm of weight average molecular weight, VR is the eluent volume, the linear correlation coefficient is r = 0.9995 and the relative standard deviation (RSD) is less than 0.4%. The results showed that the molecular weight distribution of TES40 had a great effect on the molecular weight distribution of PES and the molecular weight distribution of PES. Reproduction of silica gel microspheres can be achieved by controlling the molecular weight of TES40 and PES. The method is efficient and accurate, and the sample processing is simple. The method can be used for monitoring the preparation of the silica gel microspheres by the second catalytic sol-gel method, and is favorable for ensuring the reproducibility of the preparation of the silica microspheres.