Preparation method of benzimidazole ionic liquid functional silica gel liquid chromatogram filler

A technology of benzimidazole and ionic liquid, which is applied in the field of preparation of high-performance liquid chromatography fillers, can solve problems that have not been reported, and achieve the effects of adjustable hydrophilicity and hydrophobicity, stable chromatographic performance, and good separation performance

Inactive Publication Date: 2012-07-11
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the existing research has focused on imidazolium-based ionic liquid functionalized packing, and there is no report on benzimidazolium-based ionic liquid functionalized silica gel chromatography packing.

Method used

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  • Preparation method of benzimidazole ionic liquid functional silica gel liquid chromatogram filler
  • Preparation method of benzimidazole ionic liquid functional silica gel liquid chromatogram filler
  • Preparation method of benzimidazole ionic liquid functional silica gel liquid chromatogram filler

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Preparation of benzimidazole ionic liquid functionalized silica gel chromatography filler

[0034] Include the following steps A and B in turn:

[0035] A. Synthesis of Chloropropyl Silica Gel

[0036] Add 5.0g of silica gel into the reaction vessel, add 50ml of toluene, stir evenly, add 5.0ml of 3-chloropropyltrimethoxysilane, stir and reflux for 24 hours. After the reaction was completed, it was vacuum filtered, washed with 200ml of toluene, 200ml of ethanol, 100ml of water, and 200ml of methanol in sequence, and then vacuum-dried at 65°C for 12 hours to obtain chloropropyl silica gel.

[0037] B. Synthesis of benzimidazole ionic liquid functionalized silica gel

[0038] Add 3.0g of chloropropyl silica gel into the reaction vessel, add 30ml of N,N'-dimethylformamide, stir evenly, add 3.0g of benzimidazole, and let the reaction proceed at 130°C for 96 hours. Then, suction-filtered, washed with 200ml of ethanol, 200ml of water, and 200ml of methanol in seq...

Embodiment 2

[0039] Example 2: Preparation of benzimidazole ionic liquid functionalized silica gel chromatography filler

[0040] Include the following steps A and B in turn:

[0041] A. Synthesis of Chloropropyl Silica Gel

[0042] Add 5.0 g of silica gel into the reaction vessel, add 50 ml of toluene, stir evenly, add 5.0 ml of 3-chloropropyltrimethoxysilane, stir and reflux for 24 hours. Then, vacuum filter, wash with 200ml toluene, 200ml ethanol, 100ml water, 200ml methanol successively, and then vacuum dry at 65°C for 12 hours to obtain chloropropyl silica gel.

[0043] B. Synthesis of benzimidazole ionic liquid functionalized silica gel

[0044] Add 5.0g of chloropropyl silica gel into the reaction vessel, add 50ml of N,N'-dimethylformamide, stir mechanically, then add 2.5g of N-methylbenzimidazole, and let the reaction proceed at 120°C for 24 hours. Then, filter with suction, wash with 300ml of ethanol, 300ml of water, and 300ml of methanol successively, and then vacuum-dry at 65...

Embodiment 3

[0045] Example 3: Benzimidazole ionic liquid functionalized silica gel packing column reversed-phase chromatographic separation

[0046] The benzimidazole ionic liquid functionalized silica gel chromatographic filler of Example 1 is packed into a column, the column length is 150 mm, and the column inner diameter is 4.6 mm. Using methanol-water (80:20, v / v) as mobile phase, flow rate 1ml / min, UV detection wavelength 254nm, separation of condensed ring compounds (benzene, naphthalene, fluorene, anthracene, fluoranthene, chrysene, 3,4-benzene and pyrene); with methanol-water (50:50, v / v) as mobile phase, flow rate 1.0ml / min, ultraviolet detection wavelength 230nm, separation of phthalic acid diester compounds (dimethyl phthalate, Diallyl phthalate, dibutyl phthalate, dicyclohexyl phthalate); with methanol-water (60:40, v / v) as mobile phase, flow rate 1.0ml / min, Ultraviolet detection wavelength 254nm, separation of phenolic compounds (phenol, p-chlorophenol, methyl p-hydroxybenzo...

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Abstract

The invention discloses a preparation method of a benzimidazole ionic liquid functional silica gel liquid chromatogram filler. By the aid of the two-step chemical reaction, the preparation method comprises the following steps: carrying out silanization reaction on the surface of the full porous spherical silica gel by using a chloropropyl silane reagent to obtain chloropropyl silica gel; and carrying out amination reaction on the chloropropyl silica gel by using benzimidazole (or N-alkylbenzimidazole) to generate benzimidazole ionic liquid functional silica gel, thereby obtaining the liquid chromatogram filler. The liquid chromatogram filler is a multimode filler, has a reverse-phase chromatographic separation mode and an anion exchange chromatographic separation mode for respectively separating phenols, phenyl amines, fused ring compounds and inorganic and organic anions, and has favorable selectivity and stability.

Description

technical field [0001] The invention belongs to a preparation method of high-performance liquid chromatography filler, in particular to a method for preparing benzimidazole ionic liquid functionalized fully porous spherical silica gel as a high-performance liquid chromatography filler by using a benzimidazole-based functional monomer. In high performance liquid chromatography, silica gel functionalized with benzimidazole ionic liquids can be used as reversed-phase and ion chromatography fillers for chromatographic separation, and various mechanisms of action are involved in the separation process. Background technique [0002] Ionic liquids are usually composed of a relatively large organic cation (such as imidazole, pyridine, quaternary ammonium cation, etc.) and a relatively small inorganic anion (such as Cl - , Br - , BF 4 - etc.), the boiling point of the ionic compounds is mostly below 100°C. Because of its low boiling point, low vapor pressure, good thermal stabili...

Claims

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Application Information

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IPC IPC(8): B01J20/292B01J20/286B01J20/30
Inventor 蒋生祥孙敏冯娟娟刘霞
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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