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Ionic liquid functionalized organic polymerized monolithic column and preparation method thereof

An ionic liquid, monolithic column technology, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., to achieve the effects of fast reaction speed, simple preparation, and fast mass transfer speed

Inactive Publication Date: 2016-07-20
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the growth of the polymer chain occurs at the end of the chain used for free radicals, there are few reactive sites; and as the polymerization reaction proceeds, the concentration of the reactants continues to decrease, the steric hindrance of the polymer continues to increase, and the reaction rate also decreases. The continuous decline has led to the preparation of ionic liquid functionalized monolithic columns using this technology is very time-consuming (generally requires thermal initiation for 15-24 hours)

Method used

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  • Ionic liquid functionalized organic polymerized monolithic column and preparation method thereof
  • Ionic liquid functionalized organic polymerized monolithic column and preparation method thereof
  • Ionic liquid functionalized organic polymerized monolithic column and preparation method thereof

Examples

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Embodiment 1

[0039] (1) Rinse the empty capillary column with 0.1 HCl solution for 15 minutes, then rinse with deionized water for 10 minutes, then rinse with 1mol / L NaOH solution for 3 hours, then rinse with deionized water for 15 minutes, then rinse with methanol for 15 minutes Minutes, blow dry with nitrogen at 50°C for later use;

[0040] (2) Inject a mixture of methanol and aminopropyltrimethoxysilane with a volume ratio of 1:1 into the empty capillary column treated in step (1), and react at 60°C for 12 hours to bond the amino group on the capillary wall. The silanized substance; washed with methanol for 15 minutes; blown dry with nitrogen at 70 ° C to obtain an aminosilanized capillary;

[0041] (3) Inject the mixture of acetonitrile and acetic anhydride with a volume ratio of 1:3 into the aminosilanized capillary in step (2), and react at room temperature for 1 hour to convert the bonded amino group on the inner wall of the capillary into acetamido; then use Rinse with acetonitril...

Embodiment 2

[0045] (1) Rinse the empty capillary column with 0.1 HCl solution for 15 minutes, then rinse with deionized water for 10 minutes, then rinse with 1mol / L NaOH solution for 3 hours, then rinse with deionized water for 15 minutes, then rinse with methanol for 15 minutes Minutes, blow dry with nitrogen at 50°C for later use;

[0046] (2) Inject a mixture of methanol and aminopropyltrimethoxysilane with a volume ratio of 1:1 into the empty capillary column treated in step (1), and react at 60°C for 12 hours to bond the amino group on the capillary wall. The silanized substance; washed with methanol for 15 minutes; blown dry with nitrogen at 70 ° C to obtain an aminosilanized capillary;

[0047] (3) Inject the mixture of acetonitrile and acetic anhydride with a volume ratio of 1:3 into the aminosilanized capillary in step (2), and react at room temperature for 1 hour to convert the bonded amino group on the inner wall of the capillary into acetamido; then use Rinse with acetonitril...

Embodiment 3

[0051] (1) Rinse the empty capillary column with 0.1 HCl solution for 15 minutes, then rinse with deionized water for 10 minutes, then rinse with 1mol / L NaOH solution for 3 hours, then rinse with deionized water for 15 minutes, then rinse with methanol for 15 minutes Minutes, blow dry with nitrogen at 50°C for later use;

[0052] (2) Inject a mixture of methanol and aminopropyltrimethoxysilane with a volume ratio of 1:1 into the empty capillary column treated in step (1), and react at 60°C for 12 hours to bond the amino group on the capillary wall. The silanized substance; washed with methanol for 15 minutes; blown dry with nitrogen at 70 ° C to obtain an aminosilanized capillary;

[0053] (3) Inject the mixture of acetonitrile and acetic anhydride with a volume ratio of 1:3 into the aminosilanized capillary in step (2), and react at room temperature for 1 hour to convert the bonded amino group on the inner wall of the capillary into acetamido; then use Rinse with acetonitril...

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Abstract

The invention discloses an ionic liquid functionalized organic polymerized monolithic column and a preparation method thereof. The monolithic column is synthesized by polymerizing a nucleophilic reagent, a protonizable reagent, an ionic liquid reagent containing nucleophilic group and a catalyst in one step, the nucleophilic reagent is a urea solution, the protonizable reagent is a formaldehyde solution, and room-temperature ionic liquid is N-acetyl-1-aminopropyl-3-methylimidazole bromide ionic liquid. Components are polymerized in a capillary tube in situ in one step based on polymerization. The imidazole bromide ionic liquid is connected into an upper urea formaldehyde resin matrix, and a quick preparation method of the ionic liquid functionalized monolithic column is provided. The monolithic column has different separation modes like hydrophilic interaction, hydrogen bond interaction, ion exchange / ion exclusion effect and pi-pi action on a same chromatographic column, is wide in separation object range and can meet requirements on efficient continuous separation of various compounds which are anionic, cationic, neutral and polar.

Description

Technical field: [0001] The invention belongs to the field of monolithic column material preparation, and in particular relates to an ionic liquid functionalized polymeric monolithic column and a preparation method thereof. Background technique: [0002] Ionic liquids are new functional materials composed of two asymmetric parts, organic cations and inorganic / organic anions. Monolithic columns using ionic liquids as functional groups have been used in capillary liquid chromatography (CLC) and capillary electrochromatography (CEC). ) is applied. After the introduction of ionic liquid groups on the monolithic stationary phase, the monolithic stationary phase has some characteristics of ionic liquids, making the stationary phase possess hydrophilic interaction (HI), anion exchange, cation repulsion, H-H interaction, π- Separation performance such as π interaction. [0003] At present, the preparation methods of ionic liquid-functionalized monolithic columns mainly include i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/22B01J20/285B01J20/30
CPCB01D15/22B01J20/285
Inventor 谢增鸿王家斌林旭聪
Owner FUZHOU UNIV
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