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Preparation of silica microspheres with a broad pore size distribution and their use as the support for a coated cellulose derivative chiral stationary phase
Author(s) -
Huang Mingxian,
Ma Hongyan,
Niu Mengna,
Hu Fei,
Wang Shige,
Li Lulu,
Lv Chunguang
Publication year - 2018
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201701215
Subject(s) - tetraethyl orthosilicate , materials science , chemical engineering , cellulose , porosimetry , silicon dioxide , silica gel , thermogravimetric analysis , porosity , nanotechnology , composite material , porous medium , engineering
Abstract A templating strategy using crosslinked and functionalized polymeric beads to synthesize silica microspheres with a broad pore size distribution has been developed. The polymer/silica hybrid microspheres were prepared by utilizing the combination of a templating weak cation exchange resin, a structure‐directing agent N ‐trimethoxysilylpropyl‐ N , N , N ‐trimethylammonium chloride, and a silica precursor tetraethyl orthosilicate. The silica microspheres were then obtained after calcinating the hybrid microspheres. The as‐prepared materials were characterized by scanning electron microscopy, mercury intrusion porosimeter, and thermal gravimetric analysis. The results showed that the starting templating beads were about 5 μm in diameter and the formed silica microspheres were less than 3 μm with a pore size range of 10–150 nm, some pores were even extended to beyond 250 nm. It was demonstrated that cellulose tris(3,5‐dimethylphenylcarbamate) was readily coated onto the surface of the as‐synthesized silica microspheres without any additional surface pretreatment. The coated silica microspheres were uniformly dispersed even with high loading of the chiral stationary phase, which exhibited high resolution chiral separations in high‐performance liquid chromatography.