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Aromatic hydrocarbon linked silica gel solid phase and its preparation and use

A technology for bonding silica gel and calixarene, which is applied in chemical instruments and methods, other chemical processes, instruments, etc., can solve the problems of unprovided synthetic routes and technologies, improve the symmetry of chromatographic peaks, reduce silanol effects, and manufacture simple effect

Inactive Publication Date: 2005-06-08
WUHAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its stationary phases are all synthesized by patented methods, no specific synthetic routes and technologies are provided

Method used

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  • Aromatic hydrocarbon linked silica gel solid phase and its preparation and use
  • Aromatic hydrocarbon linked silica gel solid phase and its preparation and use
  • Aromatic hydrocarbon linked silica gel solid phase and its preparation and use

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preparation example Construction

[0020] 2. Preparation of halopropyl bonded silica gel

[0021]Add freshly distilled anhydrous toluene (anhydrous toluene is prepared by refluxing metal sodium to remove water) into a 250ml three-necked flask, quickly add activated silica gel, and then pipette a certain amount of coupling agent (halopropyl triethyl ( M)oxysilane). Under the protection of dry nitrogen (nitrogen was pre-dried by concentrated sulfuric acid and calcium chloride), magnetic stirring (slow speed). The mass of silica gel (g): coupling agent (mmoL): anhydrous toluene (mL) is generally: 10:50:500, add 3 drops of freshly distilled triethylamine dropwise, heat the oil bath to 110-120°C rapidly, and Under the condition of reaction for 24 hours (a drying tube with anhydrous calcium chloride is installed on the upper end of the condensation tube), suction filtration is carried out with a G-4 sand core funnel while it is hot, and the solid is washed with toluene, acetone, methanol, water, and acetone in seque...

Embodiment

[0035] Embodiment: Using chloropropyltriethoxysilane as coupling agent and tetrabutylammonium bromide as phase transfer catalyst, p-tert-butyl calix[8]arene as raw material, Kromasil 5 μm spherical silica gel as substrate, preparation of calix Aromatic silica gel bonded stationary phase. Prepare p-tert-butylcalix[8]arene bonded stationary phase according to one to four steps. Characterized by infrared spectroscopy, thermal analysis and elemental analysis, the stationary phase was successfully synthesized.

[0036] Using chloropropyl silica gel and KBr pellets as references, the computer carried out background subtraction to obtain the FTIR spectrum of the p-tert-butylcalix[8]arene bonded stationary phase. Spectrum display: ν2961.5cm -1 ;ν2929.7cm -1 ;ν2847.0cm -1 Stretching vibration absorption peak of saturated C-H; ν1599.1cm -1 ;ν1577.7cm -1 ;ν1487.6cm -1 Benzene ring skeleton vibration absorption peak; ν1477.9cm -1 ;ν1384.3cm -1 CH 2 、CH 3 Bending vibration peak;...

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Abstract

The present invention relates to a calixarene bonded silica gel stationary phase, the structural formula of which is ∴. The present invention also provides a preparation method of the above-mentioned calixarene bonded silica gel stationary phase. In the presence of a phase transfer catalyst quaternary ammonium salt, calixarene phenol sodium salt The desired calixarene silica gel bonded stationary phase is prepared by solid phase condensation reaction with halopropyl bonded silica gel at 110-120°C in nitrogen or argon. The calixarene silica gel bonded stationary phase prepared by the method has stable performance and is suitable for high performance liquid chromatography, microcolumn liquid chromatography and electrochromatographic separation and analysis.

Description

technical field [0001] The invention relates to a calixarene bonded silica gel stationary phase, a preparation method and application thereof. Background technique [0002] Chromatography plays a pivotal role in modern separation and analysis, and is widely used in chemistry, biology, medicine, life science and environmental science, and has become an indispensable research method. The separation system is becoming more and more complex, especially the separation and analysis of actual samples puts forward higher requirements for chromatographic technology, especially chromatographic stationary phase. At present, there are many types of commercially available silica gel and modified silica gel, but the octadecyl bond The reversed-phase chromatographic stationary phase represented by synthetic silica gel (ODS) can no longer meet the requirements of separation and analysis. Therefore, the research and development of high-selectivity chromatographic stationary phase is one of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/08B01J20/26
Inventor 达世禄冯钰锜刘敏李来生
Owner WUHAN UNIV
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