Chiral covalent organic framework materials have many excellent properties, which have received much attention in the field of separation. Synthesized the covalent organic framework COF‐TpBD (NH2)2 modified, respectively, by L‐valine trifluoroacetyl derivative, L‐hydroxyproline, and (1S)‐(+)‐10‐camphorsulfonyl chloride, three capillary columns of chiral covalent organic framework materials were obtained for gas chromatography. Those columns are able to separate some chiral compounds, positional isomers, n‐alkanes, n‐alcohols, aromatic hydrocarbon mixture, and Grob's reagents. They are complementary to other chiral capillary columns and are possible for potential applications.

Four chiral hexagonal ordered mesoporous silica were synthesized by self‐assembly and templated by surface active agents prepared from d‐phenylalanine, l‐phenylglycine, l‐proline, and l‐isoleucine, with tetraethoxylsilane as the silica source and N‐trimethoxysilylpropyl‐N,N,N‐trimethylammonium chloride as the structure promoter under the induction of templates. The four generated mesoporous silica materials were used to prepare chromatographic columns to separate chiral compounds and positional isomers of benzene series with a good separation effect and a complementary effect on species separation. The experiment suggests that the four chromatographic columns have a wide range of applications and potential practical value, providing a possible direction to explore new chiral stationary phases.

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