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Preparation method for polymer-grafted silica gel chromatographic fixed phase

A technology of silica gel chromatography and stationary phase, applied in the field of materials, can solve the problems of difficult control of the reaction process, long reaction cycle, cumbersome steps, etc., and achieve the effect of simple steps, short preparation cycle and strong universality

Inactive Publication Date: 2015-06-10
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polymer grafting density obtained by this preparation method is high, but the reaction process is difficult to control, which may cause pore blockage, and usually requires more than two steps of reaction, the steps are cumbersome, and the reaction cycle is long

Method used

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  • Preparation method for polymer-grafted silica gel chromatographic fixed phase
  • Preparation method for polymer-grafted silica gel chromatographic fixed phase
  • Preparation method for polymer-grafted silica gel chromatographic fixed phase

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Disperse 2g of amino silica gel in 10mL of anhydrous toluene, add 1g of chain transfer agent DIAzTC, 20mg of initiator azobisisobutyronitrile, and 4g of monomer styrene, mix well and ultrasonicate for 5min, N 2 Heating under reflux for 20 hours under protection and mechanical stirring, after the reaction is complete, cool the product, filter it with suction, wash it with toluene, methanol and acetone in sequence, and dry it in vacuum.

Embodiment 2

[0029] Disperse 2g of amino silica gel in 10mL of anhydrous toluene, add 1g of chain transfer agent DIAzTC, 20mg of initiator azobisisobutyronitrile, and 4g of monomeric methacrylic acid, mix well and ultrasonicate for 5min, N 2 Heating under reflux for 20 hours under protection and mechanical stirring, after the reaction is complete, cool the product, filter it with suction, wash it with toluene, methanol and acetone in sequence, and dry it in vacuum.

Embodiment 3

[0031] Disperse 2g of amino silica gel in 10mL of anhydrous toluene, add 1g of chain transfer agent DIAzTC, 20mg of initiator azobisisobutyronitrile, and 2g of monomer styrene, mix well and ultrasonicate for 5min, N 2 Heating under reflux for 20 hours under protection and mechanical stirring, after the reaction is complete, cool the product, filter it with suction, wash it with toluene, methanol and acetone in sequence, and dry it in vacuum.

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Abstract

The invention provides a preparation method for a polymer-grafted silica gel chromatographic fixed phase. The preparation method comprises the steps of grafting an azotized azido chain transfer agent on the surface of silica gel by taking an amino on amino silica gel as an anchor; bonding a polymer onto the surface of the silica gel by utilizing reversible addition-fragmentation chain transfer reaction produced between the vinyl on a vinyl monomer and the azido chain transfer agent with one step. The preparation method is simple in steps, and short in preparation period, the prepared fixed phase is high in grafting density, strong in universality, wide in application range, and beneficial to developing more polymer-grafted silica gel fixed phases with different function groups.

Description

technical field [0001] The invention belongs to the field of materials, and relates to a preparation method of a polymer-grafted silica gel chromatographic stationary phase. Background technique [0002] In recent years, polymer-grafted silica gel has been widely used in high performance liquid chromatography stationary phase, and achieved good separation effect. However, due to the heterogeneous pore structure and higher mass transfer resistance, the polymer-grafted silica-based stationary phase has lower column efficiency than the traditional silica-based stationary phase. The non-uniform pore structure is often caused by the uncontrollable polymerization reaction. The emergence of controllable radical-initiated polymerization provides a solution to this problem. [0003] Atom transfer radical polymerization (ATRP), reversible addition-fragmentation chain transfer (RAFT), nitroxide-mediated polymerization (AMRP), ring-opening polymerization (ROP) and other controllable r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30
Inventor 冯钰锜张铮
Owner WUHAN UNIV