Polyalcohol integral separation medium and preparation process thereof

A separation medium and polymer technology, applied in ion exchange column/bed methods, chemical instruments and methods, ion exchange, etc., can solve the problems of low separation column efficiency and uneven distribution of surface functional groups, and achieve low column pressure Effect

Inactive Publication Date: 2008-02-27
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This uneven internal structure leads to uneven distribution of functional groups on the surface, resulting in low separation column efficiency, which is only suitable for the separation and purification of biological samples, but is limited in analytical applications.

Method used

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  • Polyalcohol integral separation medium and preparation process thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1, preparation of monolithic column and weak cation exchange modification

[0021] Mix 1.2 mL glycidyl methacrylate (GMA), 0.8 mL ethylene glycol methacrylate (EDMA), 3 mL cyclohexanol, 0.4 mL dodecanol, 0.045 g azobisisobutyronitrile (AIBN) The solution was ultrasonically dissolved into a transparent homogeneous solution, and nitrogen gas was passed for 15 minutes. Then put the mixed solution into a dry stainless steel empty column tube, seal it and place it in a water bath at 55°C for 24 hours of reaction, then take it out and wash out the porogen and unreacted monomer with tetrahydrofuran.

[0022] A solution of ethylenediamine / tetrahydrofuran (1:1 by volume) was circulated through the chromatographic column at a flow rate of 0.1 mL / min at a constant temperature of 80° C. for 24 h. After the reaction is complete, wash the medium with dioxane / 20% sodium hydroxide (3:2, v / v), dioxane / water (3:2, v / v), methanol in sequence, and finally wash the medium with exce...

Embodiment 2

[0025] Example 2: Preparation of monolithic column and weak anion exchange modification

[0026] Dissolve 1.1mL of chloromethylstyrene and 0.6mL of divinylbenzene in a mixture of 3.5mL of cyclohexanol and 0.5mL of dodecanol, then add 0.045g of AIBN, ultrasonically dissolve into a homogeneous solution, and pass nitrogen gas for 15 minutes. Then put the mixed solution into a dry stainless steel empty column tube, seal it and place it in a 65°C water bath for 24 hours of reaction, then take it out and flush out the porogen and unreacted monomer with tetrahydrofuran.

[0027] A solution of ethylenediamine / tetrahydrofuran (1:1 by volume) was circulated through the chromatographic column at a flow rate of 0.1 mL / min at a constant temperature of 85° C. for 24 h. After the reaction is complete, wash the chromatographic column with excess methanol and water successively to obtain a weak anion exchange monolithic column.

[0028] The scanning electron microscope showed that the through...

Embodiment 3

[0029] Embodiment 3: Preparation of epoxy resin matrix monolithic separation column

[0030] First put 6.5ml of polyvinyl alcohol-200 in the test bottle, then add 0.52g of 4,4-diaminodicyclohexylmethane to dissolve, and finally add 2.5lg of bisphenol A diglycidyl ether, the resulting solution is clear transparent. Pour the above glue into a polytetrafluoroethylene tube, seal and react at 80°C for 2 hours, then raise the temperature to 160°C and react for 2h, then slowly cool down to room temperature, and take it out to prepare the wet epoxy resin monolithic medium. The monolithic medium was firstly washed with water, then repeatedly washed with acetone, and finally vacuum-dried at 60° C. for 24 hours to obtain an epoxy resin matrix monolithic separation column.

[0031] Scanning electron microscopy shows that the through hole diameter is about 3 μm. For a 100mm×4.6mm i.d. column, when the flow rate is 1mL / min, the pressure drop is 1.9Mpa; when the flow rate is 2mL / min, the p...

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Abstract

The invention discloses an integral separating dielectric of polymer and making method, which has regular three-dimensional frame structure constituted by polymer frame and through-out hole, wherein the nanometer grade middle-hole is formed on the surface of the polymer frame and/or in the polymer frame; the through-out hole is between 0. 1um and 10um and the middle hole is between 0nm and 50 nm; the frame size is 0. 2-2um. The invention has regular and sequent dielectric structure to be separated after doing chemical decoration for frame surface, which has huge applying potential in the macromolecular separating and purifying and solid phase extracting domain.

Description

technical field [0001] The invention relates to a polymer monolithic separation medium and a method for preparing the same. Background technique [0002] With the continuous advancement of science and technology, especially the rapid development of life science and pharmaceutical industry, a large number of complex biological samples and drugs urgently need to be separated and prepared, and separation science is facing great challenges. However, due to the limitation of column efficiency, it is difficult for the commonly used granular packing media to achieve efficient and rapid separation of separation objects. In addition, the granular packed column requires high packing technology, and a little carelessness may easily cause the column to collapse or stop flow. In order to adapt to the advancement of science and technology, it is urgent to develop a chromatographic packing medium that is both efficient and capable of rapid separation. [0003] Monolithic separation media...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J47/02B01J47/022
Inventor 杨更亮辛培勇尹俊发贾宏瑛
Owner INST OF CHEM CHINESE ACAD OF SCI
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