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Silicon oxynitride chromatographic stationary phase material and preparation and application thereof

A chromatographic stationary phase and silicon oxynitride technology, which is applied to the silicon oxynitride chromatographic stationary phase material and its preparation and application fields, can solve the problems of many types of surface forces, unpredictable chromatographic behavior, complex separation mechanism, etc. The effect of structure and surface area, low industrial production cost and high reaction efficiency

Active Publication Date: 2012-05-16
DALIAN 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

(2) A certain amount of silanol groups still remain on the surface of silica gel modified by alkylation, and it is easy to produce irreversible adsorption on strong polar substances such as N-containing basic compounds, resulting in the separation of polar analytes in reversed-phase mode. Severe tailing of chromatographic peaks and even dead adsorption of chromatographic peaks
Due to the Lewis acid and base interaction sites and anion exchange, cation exchange and ligand exchange centers on the surface of metal oxides, various types of forces on the surface and complex forces often coexist in the separation process. The separation mechanism Complicated, when adjusting common chromatographic conditions such as mobile phase, pH value, buffer salt, etc., the chromatographic behavior of its surface is more difficult to predict than that of silica gel matrix

Method used

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  • Silicon oxynitride chromatographic stationary phase material and preparation and application thereof
  • Silicon oxynitride chromatographic stationary phase material and preparation and application thereof
  • Silicon oxynitride chromatographic stationary phase material and preparation and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0033] The non-porous spherical silica chromatographic stationary phase material with a particle size of 1.5 microns is subjected to nitriding treatment in a high-temperature furnace with pure and dry ammonia gas. The flow rate of ammonia gas during high-temperature nitriding treatment is 0.001L / min. The nitriding temperature is 600° C., and the nitriding time is 0.1 hour. The obtained silicon oxynitride material was degassed in vacuum at 60° C. for 0.1 hour, and then washed and filtered with water and methanol in sequence. Elemental analysis showed a nitrogen content of 0.3% for the silica oxynitride chromatography stationary phase material.

Embodiment 2

[0035] The porous spherical silica chromatographic stationary phase material with a particle size of 5 microns is subjected to nitriding treatment in a high-temperature furnace with pure and dry ammonia gas, and the flow rate of ammonia gas during high-temperature nitriding treatment is 0.2L / min. The nitriding temperature is 850° C., and the nitriding time is 20 hours. The obtained silicon oxynitride material was degassed in vacuum at 200° C. for 20 hours, and then washed and filtered with water and methanol in sequence. Elemental analysis showed that the nitrogen content of the silica oxynitride chromatography stationary phase material was 8.0%.

Embodiment 3

[0037] The porous spherical silica chromatographic stationary phase material with a particle size of 1.5 microns is subjected to nitriding treatment in a high-temperature furnace with pure dry ammonia gas. The flow rate of ammonia gas during high-temperature nitriding treatment is 200L / min, and the nitriding temperature The temperature is 1200°C, and the nitriding time is 100 hours. The prepared silicon oxynitride material is degassed in vacuum at 100° C. for 0.1-20 hours, and then washed and filtered with water and methanol in sequence. Elemental analysis showed that the nitrogen content of the silica oxynitride chromatography stationary phase material was 36.6%.

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Abstract

The invention provides a silicon oxynitride chromatographic stationary phase material and a preparation method thereof. The silicon oxynitride chromatographic stationary phase material containing silicon-ammonia groups and imido group on a surface is prepared by undergoing a nitridation reaction on ammonia gas and silanol of a silicon oxide material serving as a raw material at a high temperature. The nitrogen content of the prepared silicon oxynitride material can be controlled by controlling the flow rate, nitridation speed and nitridation time of ammonia gas. The silicon oxynitride material prepared with the method can well keep the shape, pore canal structure and specific surface area of the silicon oxide raw material. The silicon oxynitride material prepared with the method has high chemical stability, can exist stably in a mobile phase of which the pH is 1-13 without losing, and has a wide application prospect when taken as a chromatographic stationary phase material and a solid phase extracting material. The preparation method is easy to operate, has low production cost, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method and application of silicon nitride oxide chromatographic stationary phase material. Specifically, the silicon amino group is used to replace the silicon hydroxyl group in the silicon oxide material, and the preparation method of the silicon nitrogen oxide chromatographic stationary phase material and its application in the fields of separation analysis, solid phase extraction and the like are provided. Background technique [0002] With the rapid development of life sciences, environmental sciences, pharmaceuticals, and synthetic chemistry centered on human health and bioengineering, high performance liquid chromatography (HPLC), as an efficient, fast, and mild separation and analysis technology, has attracted much attention. , is currently one of the most widely used analytical separation methods. As the core of HPLC technology, chromatographic column packing is very important for chromatographic separati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/283B01J20/30B01D15/08
Inventor 梁鑫淼万慧慧薛兴亚
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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