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Method for preparing polyvinyl imidazole type silica gel filler

A technology of polyvinylimidazole and vinylimidazole, which is applied in the field of preparation of high-performance liquid chromatography fillers, can solve problems such as single separation mechanism, impossibility of chromatographic application, difficult separation of samples, etc., and achieve stable chromatographic performance and superior chromatographic performance , synthetic reproducible effect

Inactive Publication Date: 2012-12-12
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, the traditional high performance liquid chromatography packing is specific, and the separation mechanism is relatively simple. It is difficult to separate complex samples in the same chromatographic mode, and it is impossible to realize the chromatographic application of the same chromatographic column in multiple modes.

Method used

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  • Method for preparing polyvinyl imidazole type silica gel filler
  • Method for preparing polyvinyl imidazole type silica gel filler
  • Method for preparing polyvinyl imidazole type silica gel filler

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: Preparation of poly-N-vinylimidazole grafted silica gel

[0033] Include the following steps A and B in turn:

[0034] A. Synthesis of brominated silica gel

[0035] Add 5.0g of aminopropyl silica gel to the reaction vessel, add 50ml of toluene, stir evenly, add 0.8ml of 2-bromoisobutyryl bromide and 0.6ml of triethylamine, and react at room temperature for 24h. Then, vacuum filter, wash with 200ml methanol, 300ml water, 200ml methanol successively, and then vacuum dry at 65°C for 12h to obtain brominated silica gel.

[0036] B. Synthesis of poly-N-vinylimidazole-grafted silica gel

[0037] Add 4.0g of brominated silica gel to the reaction vessel, add 20ml of N,N'-dimethylformamide as the reaction solvent, stir it evenly, add 20ml of N , N'-dimethylformamide solution, and then add 2ml of N-vinylimidazole, under the protection of high-purity nitrogen, heat and react at 45°C for 36h. Then cool to room temperature, filter with suction, wash with 200ml met...

Embodiment 2

[0038] Embodiment 2: Preparation of poly-N-vinylimidazole grafted silica gel

[0039] Include the following steps A and B in turn:

[0040] A. Synthesis of brominated silica gel

[0041] Add 5.0g of aminopropyl silica gel to the reaction vessel, add 60ml of toluene, stir evenly, add 1.2ml of 2-bromoisobutyryl bromide and 0.5ml of triethylamine, and react at room temperature for 12h. Then, vacuum filter, wash with 300ml methanol, 400ml water, 200ml methanol successively, and then vacuum dry at 65°C for 8h to obtain brominated silica gel.

[0042] B. Synthesis of poly-N-vinylimidazole-grafted silica gel

[0043] Add 4.0g of brominated silica gel to the reaction vessel, add 20ml of N,N'-dimethylformamide as the reaction solvent, stir it evenly, add 20ml of N , N'-dimethylformamide solution, and then added 4ml of N-vinylimidazole, protected by high-purity nitrogen, and heated at 80°C for 24h. Then cool to room temperature, filter with suction, wash with 300ml methanol, 400ml w...

Embodiment 3

[0044] Embodiment 3: Preparation of poly-N-vinylimidazole grafted silica gel

[0045] Include the following steps A and B in turn:

[0046] A. Synthesis of brominated silica gel

[0047] Add 5.0g of aminopropyl silica gel to the reaction vessel, add 50ml of toluene, stir evenly, add 0.7ml of 2-bromoisobutyryl bromide and 0.6ml of triethylamine, and react at room temperature for 36h. Then, vacuum filter, wash with 200ml methanol, 400ml water, 200ml methanol successively, and then vacuum dry at 65°C for 8h to obtain brominated silica gel.

[0048] B. Synthesis of poly-N-vinylimidazole-grafted silica gel

[0049] Add 4.0g of brominated silica gel to the reaction vessel, add 20ml of N,N'-dimethylformamide as the reaction solvent, stir it evenly, add 20ml of N with 160mg of cuprous bromide and 200mg of 2,2'-bipyridyl , N'-dimethylformamide solution, and then added 4ml of N-vinylimidazole, protected by argon, and heated at 130°C for 24h. Then cool to room temperature, filter wit...

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Abstract

The invention discloses a method for preparing a high-efficiency liquid-phase chromatogram filler, in particular to a method for preparing a polyvinyl imidazole type silica gel filler by an atom transfer free radical polymerization technique. The method comprises the following steps of: bromizing full porous spherical silica gel modified by an aminopropyl silanization reagent to prepare bromized silica gel; and performing atom transfer free radical polymerization on the bromized silica gel and N-vinylimidazole to generate polyN-vinylimidazole grafted silica gel. The filler has the advantages of uniform thickness of a polymerized layer, controllability, multiple action mechanism, capacity of separating many kinds of substances under the same chromatographic mode, separation under inverse phase, normal phase and ion chromatography modes, high selectivity and stability, symmetrical peak shape, high column efficiency, large column capacity, good application potential and the like.

Description

technical field [0001] The invention belongs to a preparation method of high-performance liquid chromatography filler, in particular to a method for preparing poly-N-vinylimidazole grafted silica gel as high-performance liquid chromatography filler by adopting atom transfer radical polymerization technology. The chromatographic material is used for separation and analysis in different chromatographic separation modes, and the filler is used as reversed phase, normal phase and ion chromatographic filler for chromatographic separation. Background technique [0002] The silica-based high-performance liquid chromatography packing prepared by the traditional bonding method has defects such as low surface coverage of stationary phase molecules, residual silanol effect, low surface carbon content, and low column capacity. In order to improve the coverage of the stationary phase on the surface of the silica gel matrix and reduce the residual silanol effect, people pay attention to t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30
CPCC08F2438/01
Inventor 蒋生祥孙敏刘霞邱洪灯
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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