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Benzyl nitrogen bridged calix[2]arene[2]triazine bonded silica stationary phase, its preparation method and its purpose

A technology of bonded silica gel and benzyl nitrogen bridge, which is applied in the field of benzyl nitrogen bridged calix[2]arene[2]triazine bonded silica gel stationary phase and its preparation, achieves simple and convenient preparation method, low preparation cost, High bonding effect

Inactive Publication Date: 2012-06-13
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The introduction of aromatic heterocycles and bridging heteroatoms provides new chemical structures and properties for this new type of calixarene. There are no related reports about heteroatom calixarene bonded silica gel stationary phases at home and abroad.

Method used

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  • Benzyl nitrogen bridged calix[2]arene[2]triazine bonded silica stationary phase, its preparation method and its purpose
  • Benzyl nitrogen bridged calix[2]arene[2]triazine bonded silica stationary phase, its preparation method and its purpose
  • Benzyl nitrogen bridged calix[2]arene[2]triazine bonded silica stationary phase, its preparation method and its purpose

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preparation example Construction

[0032] Two, the preparation method of benzyl bridged calix [2] arene [2] triazine bonded silica gel stationary phase of the present invention, comprises the following steps,

[0033] 1. Activated silica gel:

[0034] Weigh a certain amount of porous silica gel and immerse it in hydrochloric acid aqueous solution (the volume ratio of hydrochloric acid and water is 1:3), the ratio of silica gel weight (g) to hydrochloric acid volume (ml) is 1:15-1:20. Soak for 12 hours, reflux for 24 hours under magnetic stirring to remove metal ions, then filter with a G5 sand core funnel, rinse repeatedly with double distilled water until neutral, finally wash twice with acetone, and dry at 160°C for 10 hours to remove Remove the surface solvent and water to obtain activated silica gel with evenly distributed hydroxyl groups on the surface, and store it in a desiccator for later use.

[0035] 2. Preparation of aminopropyl silica gel:

[0036] with N 2 Introductory tube, condenser tube, CaCl...

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Abstract

The invention discloses a benzyl nitrogen bridged calix [2] arene [2] triazine bonded silica stationary phase, its preparation method and its purpose. The preparation method comprises the following steps: a continuous solid-liquid reaction is used, 3-aminopropyltriethoxysilane silica and tetraazacalix[2]arene[2]triazineN2 is subjected to the reflux reaction under the temperature of 130 DEG C, tetraazacalix[2]arene[2]triazine bonded silica is prepared, then active hydrogen atoms are provided on the benzyl-substituted tetraazacalix[2]arene[2]triazine, and the benzyl nitrogen bridged calix[2]arene[2]triazine bonded silica stationary phase is prepared. The synthesized calixarene bonded stationary phase has the advantages of simple method, high bonding amount, stable bonding layer, low preparation cost, wide application field of preparation method and the like. possesses a traditional ODS reversed phase mode, and can provide a plurality of action sites of hydrogen bond action, Pi-Pi actionand the like, and provides separation possibility for substances which are difficult to separate.

Description

technical field [0001] The invention relates to a separation material, in particular to a benzyl nitrogen-bridged calix[2]arene[2]triazine bonded silica gel stationary phase, a preparation method and application thereof. Background technique [0002] High performance liquid chromatography plays a pivotal role in modern separation analysis. It is widely used in various fields such as chemistry, medicine, life science and environmental science, and has become an indispensable research method. Separation systems are becoming more and more complex, especially the analysis of actual samples puts forward higher requirements for chromatographic techniques, especially chromatographic stationary phases. At present, there are many kinds of commercially available silica gel and modified silica gel, among which octadecyl bonded silica gel (ODS) as the representative reversed-phase chromatographic stationary phase can no longer meet the requirements of separation and analysis. Therefor...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01J20/30
Inventor 赵文杰张书胜汤超常红王彩娟胡锴吴养洁
Owner ZHENGZHOU UNIV
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