Preparation method and application of a magnetic covalent organic framework solid-phase extraction agent

A covalent organic framework and magnetic technology, applied in chemical instruments and methods, inorganic chemistry, other chemical processes, etc., can solve the problems of unexplored universal applicability, low specific surface area, poor crystallinity of COFs, etc., to achieve excellent adsorption performance, Effect of high specific surface area and short adsorption path

Active Publication Date: 2019-11-08
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of the milling method is that a relatively large amount of COFs can be rapidly prepared, but the disadvantages are that the crystallinity of COFs is relatively poor, the specific surface area is low, and its general applicability to monomers remains to be explored.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 2.0g FeCl 3 ·6H 2 O and 5.2 g FeCl 2 4H 2 O and 0.85mL of concentrated hydrochloric acid were dissolved in 25mL of N 2 In the degassed deionized aqueous solution, the temperature of the water bath was raised to 80°C; under mechanical stirring, the above solution was added dropwise to 250mL1.5mol / L NaOH aqueous solution, as the reaction proceeded, black precipitates gradually appeared in the reaction solution, and the reaction After the end, use an external magnetic field to separate all the precipitates from the reaction medium, wash them repeatedly with deionized water, and dry them into powder.

[0039] 0.5mg of the above-mentioned magnetic nano-Fe 3 o 4 and 3ml of p-toluenesulfonic acid catalyst were placed in a 50mL zirconia grinding jar with a diameter of 5mm. Rotate at 300rpm, grind for 15 minutes at room temperature; then add 1,3,5-triformylphloroglucinol (Tp: 1mmol, 0.21mg) and melamine (MA: 1.5mmol, 0.190mg), and grind for 3 hours at room temperature ; F...

Embodiment 2

[0041] 2.0gFeCl 3 ·6H 2 O and 1.47gFeCl 2 4H 2 O and 0.85mL of concentrated hydrochloric acid were dissolved in 25mL of N 2 In the degassed deionized aqueous solution, the temperature of the water bath was raised to 60°C; under mechanical stirring, the above solution was added dropwise to 375mL 1mol / L NaOH aqueous solution, and as the reaction progressed, black precipitates gradually appeared in the reaction solution. , using an external magnetic field to separate all the precipitates from the reaction medium, wash them repeatedly with deionized water, and freeze-dry them into powder.

[0042] 0.337mg of the above-mentioned magnetic nano-Fe 3 o 4 and 2.77ml of p-toluenesulfonic acid catalyst were placed in a 50mL zirconia grinding jar with a diameter of 5mm. Rotate at 200rpm, grind at room temperature for 10 minutes; then add 1,3,5-triformylphloroglucinol (Tp: 1mmol, 0.21mg) and melamine (MA: 1mmol, 0.127mg), and grind at room temperature for 2h; finally Then add 5 drop...

Embodiment 3

[0044] 2.0gFeCl 3 ·6H 2 O and 5.88gFeCl 2 4H 2 O and 0.85mL of concentrated hydrochloric acid were dissolved in 25mL of N 2 In the degassed deionized aqueous solution, the temperature of the water bath was raised to 60°C; under mechanical stirring, the above solution was added dropwise to 200mL 2mol / L NaOH aqueous solution, and as the reaction progressed, black precipitates gradually appeared in the reaction solution. , using an external magnetic field to separate all the precipitates from the reaction medium, wash them repeatedly with deionized water, and freeze-dry them into powder.

[0045] 1.392mg of the above-mentioned magnetic nano-Fe 3 o 4 and 3.47ml of p-toluenesulfonic acid catalyst were placed in a 50mL zirconia grinding jar with a diameter of 5mm. Rotate at 500rpm, grind at room temperature for 20 minutes; then add 1,3,5-triformylphloroglucinol (Tp: 1mmol, 0.21mg) and melamine (MA: 2mmol, 0.254mg), and grind at room temperature for 4h; finally Then add 3 drop...

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Abstract

The invention belongs to the field of organic material synthesis, and particularly relates to preparation of a magnetic covalent organic framework material and application of the magnetic covalent organic framework material as a solid-phase extraction agent. The covalent organic framework material is prepared from the following components in parts by weight: FeCl3.6H2O, FeCl2.4H2O, concentrated hydrochloric acid, sodium hydroxide, p-toluenesulfonic acid, 1,3,5-triformylphloroglucinol and melamine, the preparation steps include: preparing a Fe3O4 magnetic nano-iron core, and encapsulating the generated magnetic nano-Fe3O4 into a network frame structure of TpMA-COFs by a mechanical method; the generated substance has strong adsorption capacity to hydrophobic organic pollutants in a water body, by adjustment of TpMA-COFs reaction conditions, an adsorbent can meet the needs of trace solid phase extraction in the water body is generated, and the adsorbent has high extraction rate of organicpollutants and is easy to separate.

Description

technical field [0001] The invention belongs to the field of organic material synthesis, and in particular relates to the preparation and application of a magnetic covalent organic framework solid-phase extraction agent. Background technique [0002] Covalent Organic Frameworks (COFs) are a class of crystalline organic porous materials, and are one of the hotspots in the field of functional materials. COFs are connected by covalent bonds (C-C, C=N, C-N, C-O, and B-O, etc.), and have the characteristics of high specific surface area, low density, good thermal stability, and high order. In view of the above advantages of COFs, COFs have shown good application prospects in engineering fields such as heterogeneous catalysis, but there are still few reports on the application of COFs materials as solid phase extraction agents for the separation and enrichment of organic pollutants. [0003] The synthesis of COFs materials has always been a difficult point, and research in this a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28C02F101/30
Inventor 赵晓丽吕宏洲王珺瑜汤智吴爱明
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI
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