Calixarene bonded silica gel immobile phase preparing process

A technology of calixarene and stationary phase, which is applied in the field of preparation of calixarene bonded silica gel stationary phase, which can solve the problems of complex preparation process, narrow application range of bonding reaction, and few types of calixarene bonded phases.

Inactive Publication Date: 2003-10-29
WUHAN UNIV
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  • Application Information

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Problems solved by technology

Since then, although there have been related reports, there are very few types of calixarene bonded phase

Method used

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Embodiment Construction

[0014] The present invention prepares the synthetic method of calixarene silica gel bonded silica gel stationary phase as follows: one, activated silica gel

[0015] Weigh a certain amount of silica gel in a round bottom flask, add 3molmL -1 The ratio of hydrochloric acid, silica gel weight (g) and hydrochloric acid volume (mL) is 1:10-1:15. After soaking for 10 hours, reflux for 24 hours, filter while hot with a G-4 sand core funnel, wash the solid repeatedly with distilled water until neutral, and wash twice with acetone, first bake it under infrared light until the silica gel is dispersed, and then put it in the oven Bake at 160°C for 6 hours, take it out and cool it to room temperature in a desiccator, quickly transfer it to a drying gun, heat it in a water bath, dry it in vacuum for at least 16 hours, and take it out before use. 2. Preparation of precursor silica gel

[0016] Add freshly distilled anhydrous toluene (anhydrous toluene is prepared by refluxing metal sodiu...

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Abstract

A process for preparing the chromatographic bonded immobile phase includes preparing gamma-epoxypropoxypropyl silica gel as precursor, reaction of sodium hydride calixarene in anhyrous toluene at 70-80 deg.C to obtain calixarene phenol sodium salt, carrying it on said precursor under the action of quaternary ammonium salt, and reaction in nitrogen or argon gas at 110-120 deg.c. Its advantages aresimple process, low cost and high acid stability.

Description

technical field [0001] The invention relates to a preparation method of a calixarene bonded silica gel stationary phase. Background technique [0002] Chromatography is the fastest growing and most widely used separation and analysis technology in modern analytical chemistry, and is developing into an efficient and energy-saving separation engineering technology, which is playing an increasingly important role in many fields such as chemistry, biology and biotechnology, medicine, and life sciences. more important role. The basic requirement of chromatographic analysis is to achieve the separation of the components of the mixture, and the essence of the separation is based on the difference in the interaction between the analyzed solute and the mobile phase and stationary phase. Among them, the development of highly selective stationary phase is the core field of chromatography system. Among the many chromatographic stationary phases, silica gel and modified silica gel were...

Claims

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Application Information

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IPC IPC(8): G01N30/40G01N30/50
Inventor 达世禄冯钰锜李来生刘敏
Owner WUHAN UNIV
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