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Preparation and application of polyethyleneimine modified reversed-phase/strong anion exchange mixed-mode polymer

A mixture and cross-linking agent technology, applied in the direction of anion exchanger materials, anion exchange, inorganic anion exchangers, etc., can solve the problems of poor retention capacity of polar substances, low exchange capacity, complicated preparation, etc., and achieve uniform particle size , simple preparation process and high yield

Active Publication Date: 2020-09-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commercial mixed-mode materials include silica-based and polymer-based materials, usually with low exchange capacity, poor retention of polar substances, complicated preparation, and expensive

Method used

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  • Preparation and application of polyethyleneimine modified reversed-phase/strong anion exchange mixed-mode polymer
  • Preparation and application of polyethyleneimine modified reversed-phase/strong anion exchange mixed-mode polymer
  • Preparation and application of polyethyleneimine modified reversed-phase/strong anion exchange mixed-mode polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Dissolve 90mg of azobisisobutyronitrile in 1.69g of 1-dodecanol, 4.55mL of toluene, 4.55mL of divinylbenzene, and 1.6mL of diethylaminoethyl methacrylate, sonicate for 10min, pass Nitrogen deoxygenated for 10 minutes to prepare solution A;

[0029] (2) 80mg nano-SiO 2 Disperse in 10mL of water and ultrasonically disperse for 10min to prepare solution B. Take 4mL of solution A and add it to 10mL of solution B, homogenize it with a homogenizer at 6000rpm for 1min, seal it, and put it in a water bath at 70°C for polymerization for 16h to obtain PDEAEMA-SiO 2 Complex.

[0030] (3) PDEAEMA-SiO 2 Disperse and soak in 10% hydrofluoric acid for 12 hours to obtain PDEAEMA microspheres.

[0031] (4) Disperse 2.0g of PDEAEMA microspheres in 20mL of methanol, stir magnetically, add 2mL of BDDE, and react at 80°C for 3h. After the reaction, filter and wash with ethanol to obtain PDEAEMA-BDDE polymer microspheres with epoxy end groups.

[0032] (5) Disperse 2.0 g of PDEAEMA-B...

Embodiment 2

[0035] 2.0 g of PDEAEMA-BDDE microspheres with epoxy end groups were dispersed in 20 mL of 5% PEI (M w =10000) solution, the solvent was methanol and water (1:1), magnetically stirred, and reacted at 80°C for 1h. After the reaction, filter and wash with deionized water to neutrality, the product obtained is PDEAEMA-PEI with amino end groups 10000,5% ; 2.0 g of PDEAEMA-PEI with amino end groups 10000,5% Disperse in 20mL of methanol, add 5mL of phenyl glycidyl ether, stir with magnetic force, and react at 80°C for 4h. After the reaction, filter and wash with deionized water until neutral, then vacuum dry at 50°C for 24h to obtain PDEAEMA-QPEI 10000,5% MAX adsorbent. Other steps are with embodiment (1).

Embodiment 3

[0037] 2.0 g of PDEAEMA-BDDE microspheres with epoxy end groups were dispersed in 20 mL of 5% PEI (M w =70000) solution, the solvent was methanol and water (1:1), magnetically stirred, and reacted at 80°C for 1h. After the reaction, filter and wash with deionized water to neutrality, the product obtained is PDEAEMA-PEI with amino end groups 70000,5% ; 2.0 g of PDEAEMA-PEI with amino end groups 70000,5% Disperse in 20mL of methanol, add 5mL of phenyl glycidyl ether, stir with magnetic force, and react at 80°C for 4h. After the reaction, filter, wash with deionized water until neutral, and dry in vacuum at 50°C for 24h to obtain PDEAEMA-QPEI 70000,5% MAX adsorbent, other steps are with embodiment (1).

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Abstract

The invention provides a method for preparing a novel polyethyleneimine modified reversed-phase / strong anion exchange mixed mode adsorbent, and application of the adsorbent. The preparation method comprises the following steps: preparing a polymer with an amino functional group by adopting a Pickering emulsion polymerization method; and grafting hyperbranched polyethyleneimine to the surface of the polymer through an epoxy-amine reaction, and converting an amino group into a quaternary amino group through the epoxy-amine reaction to obtain the reversed-phase / strong anion exchange (MAX) mixed mode adsorbent with the ultrahigh capacity. According to the preparation method, the branch structure and high functional group density of polyethyleneimine are fully utilized, the preparation method is simple, and the ion exchange capacity and extraction efficiency of the material are greatly improved. The preparation method provided by the invention is simple, efficient, short in preparation period and high in yield. When used as a solid-phase extraction filler, the novel polyethyleneimine modified reversed-phase / strong anion exchange mixed mode adsorbent can be used for separating and purifying alkaline, neutral and acidic organic pollutants in a complex matrix.

Description

technical field [0001] The invention belongs to the field of environmental monitoring and new materials, and specifically relates to the preparation and preparation of a polyethyleneimine-modified reversed-phase / strong anion-exchange mixed-mode adsorbent with ultra-high selectivity for enrichment and purification of acidic, neutral and alkaline substances. application. Background technique [0002] Environmental samples, biological samples, and food samples are characterized by complex components and low levels of target analytes (ng / mL–μg / mL), and almost all samples need to be purified and concentrated before instrumental analysis. At present, commonly used solid-phase extraction packings include florisil, activated carbon, alumina, silica gel, silica gel-modified C18, ethylene and divinylbenzene polymers, etc., and these materials are retained by reversed phase or normal phase. Action, retention The mode of action is single, the selectivity is poor, and the retention of p...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J41/12B01D15/36B01D15/08
CPCB01D15/08B01D15/361B01J20/26B01J20/28019B01J41/12
Inventor 黄超囡李云陈吉平
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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