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Itaconic acid bonded silica gel based hydrophilic chromatography stationary phase and preparation method thereof

A stationary phase and bonding technology, applied in chemical instruments and methods, other chemical processes, ion exchange, etc., to achieve good separation performance, good separation, and a wide range of applications

Inactive Publication Date: 2018-11-13
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the literature on the preparation of polymer-grafted silica stationary phases by surface radical chain reaction in DES has not been reported

Method used

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  • Itaconic acid bonded silica gel based hydrophilic chromatography stationary phase and preparation method thereof
  • Itaconic acid bonded silica gel based hydrophilic chromatography stationary phase and preparation method thereof
  • Itaconic acid bonded silica gel based hydrophilic chromatography stationary phase and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In a 100ml three-necked flask, add 3g of silica gel and 30ml of DES, ultrasonically disperse for 10 minutes, then add 6mmol of 3-mercaptopropyltriethoxysilane (1.43g), heat and stir at 60°C for 24 hours, and react After completion, the product was cooled to room temperature, washed with ethanol, distilled water: ethanol (1:1), ethanol in sequence, and finally dried in a vacuum oven at 65°C for 24 hours to obtain mercaptopropyl silica gel. Put the prepared mercaptopropyl silica gel in a three-necked flask, add 30ml of DES, then add 2g of itaconic acid and 0.02g of AIBN, ultrasonically disperse for 10 minutes, heat and stir the mixture at 60°C under nitrogen for 15 hours, Cool to room temperature, then wash with the above washing method in sequence, and dry in a vacuum oven at 65°C for 24 hours. Finally, itaconic acid chromatographic stationary phase is obtained.

[0033] Elemental analysis results: mercaptopropyl modified silica: N: 0%, C: 2.82%, H: 0.76%; polyitaconic ...

Embodiment 2

[0037] In a 100ml three-necked flask, add 3g of silica gel and 30ml of DES, ultrasonically disperse for 10 minutes, then add 6mmol of 3-mercaptopropyltriethoxysilane (1.43g), heat and stir at 65°C for 22 hours, and react After completion, the product was cooled to room temperature, washed with ethanol, distilled water: ethanol (1:1), ethanol in sequence, and finally dried in a vacuum oven at 65°C for 24 hours to obtain mercaptopropyl silica gel. Put the prepared mercaptopropyl silica gel in a three-necked flask, add 30ml of DES, then add 2g of itaconic acid and 0.02g of AIBN, ultrasonically disperse for 10 minutes, heat and stir the mixture at 60°C under nitrogen for 15 hours, Cool to room temperature, then wash with the above washing method in sequence, and dry in a vacuum oven at 65°C for 24 hours. Finally, itaconic acid chromatographic stationary phase is obtained.

[0038] Elemental analysis: N: 0%, C: 6.23%, H: 1.52%. Infrared spectrum; 1723cm -1 Carbonyl characteristi...

Embodiment 3

[0042] In a 100ml three-necked flask, add 3g of silica gel and 30ml of DES, ultrasonically disperse for 10 minutes, then add 6mmol of 3-mercaptopropyltrimethoxysilane (1.43g), heat and stir at 70°C for 20 hours, the reaction is complete Finally, the product was cooled to room temperature, washed with ethanol, distilled water: ethanol (1:1), ethanol in sequence, and finally dried in a vacuum oven at 65°C for 24 hours to obtain mercaptopropyl silica gel. Put the prepared mercaptopropyl silica gel in a three-necked flask, add 30ml of DES, then add 2g of itaconic acid and 0.02g of AIBN, ultrasonically disperse for 10 minutes, heat and stir the mixture at 60°C under nitrogen for 15 hours, Cool to room temperature, then wash with the above washing method in sequence, and dry in a vacuum oven at 65°C for 24 hours. Finally, itaconic acid chromatographic stationary phase is obtained.

[0043] Elemental analysis: N: 0% C: 5.43% H: 1.718%. Infrared spectrum: 1729cm -1 Carbonyl charact...

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Abstract

The invention discloses an itaconic acid bonded silica gel based hydrophilic chromatography stationary phase and a preparation method of the itaconic acid bonded silica gel based hydrophilic chromatography stationary phase. The invention provides the high performance liquid chromatography stationary phase and the preparation method of the high performance liquid chromatography stationary phase, the stationary phase is a reversed phase liquid chromatography stationary phase taking itaconic acid as a bonded phase; a mercaptopropyl silica gel and the itaconic acid are polymerized through the radical chain transfer reaction, a polymer monomer comprises two carboxyl, then the hydrophilic performance of the stationary phase is stronger, and the stationary phase is better separated; the preparation process of the stationary phase is simple and reliable, the raw materials are easy to get, the preparation method is favorable for implementing quantity production; the provided stationary phase isa universal hydrophilic chromatography stationary phase, has an excellent performance of separating most of polar compounds, and has an excellent market application prospect.

Description

(1) Technical field [0001] The invention relates to a hydrophilic chromatographic stationary phase and a preparation method thereof, in particular to a novel hydrophilic high-performance liquid chromatographic stationary phase whose bonded phase is itaconic acid and a preparation method thereof. (2) Background technology [0002] High performance liquid chromatography (HPLC) plays an important role in the field of separation and analysis. As the core of HPLC, stationary phase is of great significance to the development of HPLC. In previous studies, the solvents used to synthesize stationary phases were mainly volatile toxic substances, such as toluene, chloroform, and methanol. At present, our group has successfully applied deep eutectic solvent (DES) to the preparation of chromatographic stationary phase. However, the literature on the preparation of polymer-grafted silica stationary phases by surface radical chain reaction in DES has not been reported yet. [0003] Stat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/287B01J20/30B01D15/08
CPCB01D15/08B01J20/287B01J20/30B01J2220/54
Inventor 胡永兴李祖光
Owner ZHEJIANG UNIV OF TECH
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