Dicationic liquid chromatographic stationary phase and preparation method and application thereof

A liquid stationary phase and double cation technology, applied in the field of ionic liquid chromatography stationary phase materials, to achieve good thermal stability, improved wetting ability, and good reproducibility

Active Publication Date: 2020-02-04
DALIAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are few domestic researches on the stationary phase of dicationic liquid gas c

Method used

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  • Dicationic liquid chromatographic stationary phase and preparation method and application thereof
  • Dicationic liquid chromatographic stationary phase and preparation method and application thereof
  • Dicationic liquid chromatographic stationary phase and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] R in the synthesized dicationic liquid stationary phase in this embodiment is C 1 , whose structural formula is:

[0058]

[0059] The preparation method is as follows:

[0060] Synthesis of Dication Liquid Iodine Salt (MM(mim) 2 -(NTf 2 ) 2 ), adding 2:1 methylimidazole (8.21g) and 1,3-bis(iodomethyl)tetramethyldisiloxane (18.35g) in the reaction flask, adding 50mL of anhydrous acetonitrile solvent, reflux at 80°C, and react under nitrogen atmosphere for 72h. The solvent was distilled off under reduced pressure, and the unreacted substance was extracted with three equal parts of ethyl acetate, and dried to obtain a light yellow viscous compound, which is the dicationic liquid iodine salt. Synthesis of Dicationic Liquid Ditrifluoromethanesulfonylimide Salt (MM(mim) 2 -(NTf 2 ) 2 ), 0.01 mol of iodide salt was dissolved in 20 mL of deionized water, and 5.742 g of two molar equivalents of lithium bistrifluoromethanesulfonimide dissolved in 10 mL of deionized wa...

Embodiment 2

[0062] R in the synthesized dicationic liquid stationary phase in this embodiment is C 4 , whose structural formula is:

[0063]

[0064] The preparation method is as follows:

[0065] Synthesis of Dication Liquid Iodine Salt (MM(bim) 2 -I 2 ), adding butylimidazole (12.42g) and 1,3-bis(iodomethyl)tetramethyldisiloxane (18.35g) with a molar ratio of 2:1 in the reaction flask, adding 50mL of anhydrous acetonitrile for solvent, reflux at 80°C, and react under nitrogen atmosphere for 72h. The solvent was distilled off under reduced pressure, and the unreacted substance was extracted with three equal parts of ethyl acetate, and dried to obtain a light yellow viscous compound, which is the dicationic liquid iodine salt. Synthesis of Dicationic Liquid Bistrifluoromethanesulfonylimide Salt (MM(bim) 2 -(NTf 2 ) 2 ), 0.01 mol of iodide salt was dissolved in 20 mL of deionized water, and 5.742 g of two molar equivalents of lithium bistrifluoromethanesulfonimide dissolved in 10...

Embodiment 3

[0067] R in the dicationic liquid stationary phase synthesized in this embodiment is benzyl, and its structural formula is:

[0068]

[0069] The preparation method is as follows:

[0070] Synthesis of Dication Liquid Iodine Salt (MM(benzim) 2 -I 2 ), adding 2:1 benzyl imidazole (15.82g) and 1,3-bis(iodomethyl)tetramethyldisiloxane (18.35g) in the reaction flask, adding 50mL of anhydrous acetonitrile solvent, reflux at 80°C, and react under nitrogen atmosphere for 72h. The solvent was distilled off under reduced pressure, and the unreacted substance was extracted with three equal parts of ethyl acetate, and dried to obtain a light yellow viscous compound, which is the dicationic liquid iodine salt. Synthesis of Dicationic Liquid Ditrifluoromethanesulfonylimide Salt (MM(benzim) 2 -(NTf 2 ) 2 ), 0.01 mol of iodide salt was dissolved in 30 mL of methanol, and 5.742 g of two molar equivalents of lithium bistrifluoromethanesulfonylimide dissolved in 10 mL of deionized wate...

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Abstract

The invention provides a novel dicationic liquid chromatographic stationary phase and a preparation method and application thereof. Specifically, a silane coupling agent serves as a bridging group tosynthesize the dicationic liquid gas chromatographic stationary phase. The invention further provides the preparation method of the gas chromatographic stationary phase, and the preparation method includes the steps that firstly, the chlorosilane coupling agent is exchanged into iodosilane coupling, then a quaternary ammonium salt reaction is conducted for synthesizing dicationic liquid iodate, and then through an anion exchange reaction, dicationic liquid with anions being tetrafluoroboric acid, hexafluorophosphoric acid, trifluoromethanesulfonic acid and bistrifluoromethanesulfonimide sol. to serve as the gas chromatographic stationary phase. The dicationic liquid stationary phase has the good film formation property and thermal stability, shows good retention and separation selectivityto alkanes, alcohols, fatty acid methyl esters and polycyclic aromatic hydrocarbons, and shows good application prospects by serving as the gas chromatographic stationary phase.

Description

technical field [0001] The invention belongs to the field of ionic liquid chromatographic stationary phase materials, and in particular relates to a method for synthesizing dicationic liquids with silicon-oxysilane as the main chain and the application thereof as chromatographic stationary phases. Background technique [0002] Gas chromatography is an important modern separation and analysis technology, which plays a vital role in many aspects, including petrochemical, medical and health, environmental monitoring, biochemistry, food testing and other fields. Among them, the stationary phase is an important part of chromatographic separation, and its development and research has always been a hot spot in the field of chromatography. Ionic liquids are a class of organic substances that are completely composed of anions and cations and remain liquid at room temperature. Ionic liquids have physical and chemical properties such as low vapor pressure, low melting point, high ther...

Claims

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Application Information

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IPC IPC(8): C07F7/18C07F9/54C07C303/40C07C311/48B01J20/292B01D15/20
CPCG01N30/48C07F7/1892C07F9/5414C07C303/40C07C311/48B01J20/292B01D15/20
Inventor 魏立纲马浩邵国林安庆大康致强郝一博
Owner DALIAN POLYTECHNIC UNIVERSITY
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