Tetraazacalix [2] arene [2] triazine bonded silica gel stationary phase and preparation method and application thereof

A technology of bonded silica gel and tetraaza, which is applied to the stationary phase of tetraazacalix[2]arene[2]triazine bonded silica gel. Requirements and other issues, to achieve the effect of low preparation cost, stable bonding layer, and simple method

Inactive Publication Date: 2011-06-22
ZHENGZHOU UNIV
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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

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  • Tetraazacalix [2] arene [2] triazine bonded silica gel stationary phase and preparation method and application thereof
  • Tetraazacalix [2] arene [2] triazine bonded silica gel stationary phase and preparation method and application thereof
  • Tetraazacalix [2] arene [2] triazine bonded silica gel stationary phase and preparation method and application thereof

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Embodiment Construction

[0019] The structural formula of the tetraazacalix [2] arene [2] triazine bonded silica gel stationary phase of the present invention is as follows figure 1 shown.

[0020] Its specific preparation method is:

[0021] 1. Activation of silica gel: Weigh a certain amount of porous silica gel and immerse in HCl / H 2 In O(1:3, v / v), 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.

[0022] 2. Preparation of precursor silica gel: 2 Add a certain amount of 3-aminopropyltriethoxysilane into the introduction tube, condensation tu...

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Abstract

The invention discloses a tetraazacalix [2] arene [2] triazine bonded silica gel stationary phase with high bonding quantity and stable bonding layers. A preparation method for the stationary phase comprises that: 3-aminopropyltriethoxysilane silica gel and tetraazacalix [2] arene [2] triazine undergo reflux reaction in N2 at the temperature of 130 DEG C in the presence of anhydrous potassium carbonate to form the tetraazacalix [2] arene [2] triazine bonded silica gel stationary phase. The calixarene bonded stationary phase synthesized by adopting the method has high bonding quantity and stable bonding layers; and the preparation method is simple and convenient, has low preparation cost and wide application range. The stationary phase not only has the reversed phase chromatography performance of the traditional ozone depleting substance (ODS), but also can provide multiple acting sites of complexing, hydrogen bonding effect, phi-phi effect, spatial matching and the like, so the stationary phase can replace the ODS to a certain degree, and provides separation possibility for difficultly separated substances at the same time.

Description

technical field [0001] The invention relates to a separation material, in particular to a tetraazacalix[2]arene[2]triazine bonded silica gel stationary phase with a high bonding amount and a stable bonding layer; the present invention also relates to a preparation method of the stationary phase and apply. 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 sta...

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Application Information

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IPC IPC(8): B01J20/283B01J20/30B01D15/08
Inventor 张书胜赵文杰梁松于阿娟胡锴赵晓兰吴养洁
Owner ZHENGZHOU UNIV
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