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Preparation method and application thereof of chromatography packed column of rodlike nano mesoporous molecular sieve material

A nano-mesoporous and molecular sieve technology, applied in the field of chromatographic columns, can solve the problems of chromatographic column filling difficulties, increased pressure, increased back pressure, etc., and achieve the effects of uniform, accurate and controllable structure, efficient separation, and simple preparation methods

Inactive Publication Date: 2013-04-24
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, with the increasing development of separation science, the requirements for higher column efficiency and faster separation speed are limited by the particle size of spherical stationary phase
When the particle size of the spherical stationary phase decreases, the back pressure increases accordingly, which brings great difficulties to the filling of the chromatographic column, especially the packed capillary electrochromatographic column. In addition, during the operation, the pressure to maintain normal operation is also corresponding increased

Method used

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  • Preparation method and application thereof of chromatography packed column of rodlike nano mesoporous molecular sieve material
  • Preparation method and application thereof of chromatography packed column of rodlike nano mesoporous molecular sieve material

Examples

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Effect test

Embodiment 1

[0040] Preparation of packed column: 50mg SBA-15 rod filler, add 100μL water, 500uμL methanol, 50uL [3-(2-aminoethyl)aminopropyl]trimethoxysilane, stir the suspension with nitrogen gas for 6h and let it stand overnight. Discard the supernatant, wash with water until neutral; re-suspend with 200 μL of methanol; fill it into a 75 μm capillary column by pressure packing method to prepare a capillary electrochromatography packed column.

Embodiment 2

[0042]Preparation of packed column: Add 50mg SBA-15 rod filler, add 50μL water, 500uμL methanol, 50uL 3-aminopropyltrimethoxysilane, pass nitrogen gas into the suspension and stir the suspension for 7h, then let it stand overnight, discard the supernatant, wash with water until Neutral; re-suspended with 200 μL of methanol; electropacked into a 75 μm capillary column to prepare a packed column for capillary electrochromatography. figure 1 Four organic acids were separated for the bond and the [3-(2-aminoethyl)aminopropyl]trimethoxysilane SBF-15 packing.

Embodiment 3

[0044] Preparation of packed column: 50mg SBA-15 rod filler, add 200μL water, 200μL methanol, 10uL [3-(2-aminoethyl)aminopropyl]trimethoxysilane, stir the suspension for 7h with nitrogen gas and let stand overnight , discard the supernatant, wash with water until neutral; re-suspend with 200 μL of methanol; fill it into a 75 μm capillary column by pressure packing method to prepare a capillary electrochromatography packed column. figure 2 Separation of three organic acids for 3-aminopropyltrimethoxysilane SBF-15 packing.

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Abstract

The invention relates to a preparation method and application thereof of a chromatography packed column of a rodlike nano mesoporous molecular sieve material. The preparation method comprise the concrete steps of: suspending a modified rodlike nano chromatography packing by using a 200 mu L solvent, wherein the suspension solvent is selected from one of water, acetone, methyl alcohol and acetonitrile; preparing a packed high performance liquid chromatography column by adopting a pressure packing method; and preparing a capillary electrochromatography column by adopting a pressure or electric packing method. The invention has the advantages of simple preparation method, uniform, accurate and controllable mesoporous material and benefit to the high-efficiency separation of a sample; and a real nanoscale packing separation operation can be realized on the basis of the surface characteristics of the nano material and a spatial structure formed in the column.

Description

【Technical field】 [0001] The invention relates to the technical field of chromatographic columns, in particular to a preparation method and application of a rod-shaped nanometer mesoporous molecular sieve material chromatographic packed column. 【Background technique】 [0002] In 1992, Mobil Corporation of the United States first successfully used alkyl quaternary ammonium salt cationic surfactants as templates to synthesize a new type of M41S series silica (aluminum)-based ordered mesoporous molecular sieves. This type of molecular sieve has a large specific surface area and uniform The pore diameter distribution of mesoporous molecular sieves can be adjusted in the range of 1.5-10nm, and has broad application prospects in catalysis, separation and adsorption. In recent years, people have successfully prepared silicon-based molecular sieves such as M41S, SBA, HMS, MSU and Al with different surfactants and according to different assembly routes. 2 o 3 , WO 3 , ZrO 2 and o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/56
Inventor 张维冰张凌怡杜一平
Owner EAST CHINA UNIV OF SCI & TECH
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