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Citation: WU Haibo, XUE Xingya, LI Kuiyong, ZHOU Yongzheng. Preparation of macroporous silica and its application on polysaccharide derivative based chiral stationary phase[J]. Chinese Journal of Chromatography, ;2018, 36(10): 972-978. doi: 10.3724/SP.J.1123.2018.05007 shu

Preparation of macroporous silica and its application on polysaccharide derivative based chiral stationary phase

1.
Zhejiang Acchrom Technologies Co. Ltd., Wenling 317503, China;
2.
Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China

Received Date: 12 May 2018

In order to prepare 100-nm macroporous silica, spherical silica (5 μm in particle size, 10 nm in pore diameter) was treated by hydrothermal or baking methods. During hydrothermal treatment, 22 g/L NaF was added, which efficiently promoted the enlargement of pore diameters. By this method, the average pore diameter of silica reached 100 nm after heating for 48 h at 160℃ in an autoclave, but showed a poor size distribution. In the baking method, pore diameter enlargement was controlled by modifying the baking temperature, time, and the amount of double salt LiCl-NaCl added. The addition of 1.125 g LiCl·H₂O and 0.75 g NaCl per 10 g silica and baking at 500℃ for 3-5 h yielded silica with 100-nm pore diameters. This method was more efficient, easier, and better in the product pore diameter distribution than hydrothermal treatment. The obtained silica was very similar to commercial Fuji-1000 gel. The macroporous silicas obtained from the hydrothermal and baking treatments were both modified with aminopropyl silane and coated by cellulose tri(3,5-dimethylphenyl carbamate) to prepare chiral stationary phases (CSPs). The CSP based on the baking-treated silica exhibited much better selectivity and resolution for enantiomers.
- hydrothermal,
- baking,
- pore diameter enlargement,
- polysaccharide derivative,
- chiral stationary phases,
- chiral separation
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