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第 35 卷第 9 期 精 细 化 工 Vol.35, No.9
201 8 年 9 月 FINE CHEMICALS Sept. 2018

功能材料
HPLC 级二氧化硅微球的制备及其功能化

*
包建民，王惠柳，李优鑫
（天津大学 药物科学与技术学院，天津市现代药物传递及功能高效化重点实验室，天津化学化工协同创新
中心，天津 300072）

摘要：采用酸-碱催化的溶胶-凝胶法制备二氧化硅微球，系统探索了水用量、乙醇用量、旋蒸温度、搅拌速度和
致孔剂种类对二氧化硅微球形态和粒径分布的影响。将制得的二氧化硅微球经简单沉降筛分及功能化后，获得
了 C18 键合硅胶、亲水 C18 键合硅胶、氨丙基键合硅胶、乙二胺-N-丙基键合硅胶 4 种键合硅胶。结果表明：最
佳的二氧化硅微球制备条件为，n(H 2 O)∶n〔正硅酸乙酯（TEOS）〕=6∶4，V(EtOH)∶V(TEOS)=3∶5，旋蒸温
度为 57 ℃，搅拌速度为 2190 r/min，致孔剂为 N,N-二甲基甲酰胺（DMF）。所制二氧化硅微球球形度好、粒径
3
2
分布为 3~10 μm、比表面积为 464.11 m /g、孔体积为 1.14 m /g、平均孔径为 9.81 nm，且孔径分布窄、硅羟基含
量高达 0.5450 mmol/g。C18 键合硅胶和亲水 C18 键合硅胶的柱效分别为 53474/m 和 86984/m（以甲苯计），且
对分析物的分离良好。氨丙基键合硅胶和乙二胺-N-丙基键合硅胶的离子交换容量分别为 1.44 和 1.22 mmol/g，
对甲苯磺酸吸附量分别为 240.8 和 217.6 mg/g。
关键词：溶胶-凝胶法；二氧化硅微球；C18 键合硅胶；亲水 C18 键合硅胶；氨丙基键合硅胶；乙二胺-N-丙基
键合硅胶
中图分类号：TB34 文献标识码：A 文章编号：1003-5214 (2018) 09-1457-09

Preparation and Functionalization of HPLC Grade Silica Microspheres

*
BAO Jian-min, WANG Hui-liu, LI You-xin
（Collaborative Innovation Center of Tianjin Chemical Engineering, Tianjin Key Laboratory for Modern Drug Delivery
& High-Efficiency, School of Pharmaceutical Science and Technology, Tianjin University, Tianjin 300072, China）

Abstract: Porous silica microspheres were prepared via an acid-basic catalytic sol-gel method. The effects
of water amount, ethanol amount, rotary evaporation temperature, stirring speed and porogen species on the
morphology and particle size distribution of silica microspheres were investigated. After simple
sedimentation and sorting, the silica spheres were functionalized and four packings were obtained,
including C18 bonded silica gel, hydrophilic C18 bonded silica gel, aminopropyl bonded silica gel and
ethylenediamine-N-propyl bonded silica gel. Results showed that the optimal conditions for the preparation
of silica microspheres were as follows: n(H 2O)∶n〔tetraethyl orthosilicate(TEOS)〕=6∶4, V(EtOH)∶
V(TEOS)=3 ∶ 5, rotary evaporation temperature of 57 ℃ , stirring speed of 2190 r/min, and
N,N-dimethylformamide(DMF) as porogen. The obtained silica microspheres were mostly regular-ball and
had a narrow pore size distribution with an average pore size of 9.81 nm, the specific surface area was
2
3
464.11 m /g, and the pore volume was 1.14 m /g. The concentration of Si-OH groups was up to 0.5450
mmol/g. The column efficiency of C18 bonded silica gel and hydrophilic C18 bonded silica gel were
53474/m and 86984/m (toluene), respectively. Moreover, these two microspheres had good separation
effects for analytes. The ion exchange capacity of aminopropyl bonded silica gel and
ethylenediamine-N-propyl bonded silica gel were 1.44 and 1.22 mmol/g, respectively. Their absorption
capacity to p-toluenesulfonic acid was up to 240.8 and 217.6 mg/g.

收稿日期：2017-06-24; 定用日期：2017-11-13; DOI: 10.13550/j.jxhg.20170514
基金项目：国家自然科学基金（21375093，21605112）；天津市应用基础与前沿技术研究计划青年项目（15JCQNJC43200）
作者简介：包建民（1961—），男，教授，博士生导师，电话：022-27892820，E-mail：bao@tju.edu.cn。 联系人：李优鑫（1981—），
女，博士，副教授，电话：022-27892820，E-mail：lyx@tju.edu.cn。