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Covalent organic frame magnetic composite microspheres of core-shell structure and preparation method of microspheres

A technology of magnetic composite microspheres and covalent organic frameworks, which can be used in the preparation of microspheres, the magnetism of inorganic materials, magnetic materials, etc., can solve the problems of high specific surface area, limited wide application, etc. Shell thickness controllable effect

Active Publication Date: 2016-11-16
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Most of the currently studied COFs microspheres are prepared by the direct solvothermal method, and the obtained COFs microspheres cannot meet the following conditions: regular shape, uniform size, controllable size, good solution dispersion, high specific surface area and highly ordered pores. , which limits its wide application in industry

Method used

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  • Covalent organic frame magnetic composite microspheres of core-shell structure and preparation method of microspheres
  • Covalent organic frame magnetic composite microspheres of core-shell structure and preparation method of microspheres
  • Covalent organic frame magnetic composite microspheres of core-shell structure and preparation method of microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1: Core-shell Fe with a shell thickness of around 100 nm 3 o 4 Preparation of @COF Composite Microspheres

[0050] 1. Citrate stabilized Fe 3 o 4 Preparation of Magnetic Particles

[0051] Dissolve 1.3 g of ferric chloride hexahydrate, 3.8 g of acetate and 0.4 g of citrate in 70 mL of ethylene glycol, stir mechanically at 160 °C for 1 h, and then place in a stainless steel high-pressure tank with a Teflon liner In the reaction kettle, place the reaction kettle in an oven at 200°C for 16 hours, take it out, and cool it to room temperature with water; separate the product with a magnet, and wash it with absolute ethanol and deionized water to remove unreacted raw materials, and finally ferric ferric oxide The magnetic particles are dispersed in absolute ethanol for later use;

[0052] 2. Core-shell Fe 3 o 4 Preparation of @Polyimine Composite Microspheres

[0053] 16mg Fe 3 o 4 Add magnetic particles, 16mg benzidine and 11mL anhydrous THF into the reacto...

Embodiment 2

[0056] Example 2: Core-shell Fe with a shell thickness of around 50 nm 3 o 4 Preparation of @COF Composite Microspheres

[0057] 1. Citrate stabilized Fe 3 o 4 The preparation of magnetic particles is the same as described in Example 1-1;

[0058] 2. Core-shell Fe 3 o 4 The preparation of @Polyimine composite microspheres is the same as described in Example 1-2. The difference is Fe 3 o 4 The dosages of magnetic particles, benzidine and trihydroxy-tritylaldehyde are: 10mg, 8mg, 6mg respectively;

[0059] 3. Core-shell Fe 3 o 4 The preparation of @COF composite microspheres was the same as described in Examples 1-3.

Embodiment 3

[0060] Example 3: Core-shell Fe with a shell thickness of around 20 nm 3 o 4 Preparation of @COF Composite Microspheres

[0061] 1. Citrate stabilized Fe 3 o 4 The preparation of magnetic particles is the same as described in Example 1-1;

[0062] 2. Core-shell Fe 3 o 4 The preparation of @Polyimine composite microspheres is the same as described in Example 1-2. The difference is Fe 3 o 4 The dosages of magnetic particles, benzidine and trihydroxy-tritylaldehyde are: 10mg, 4mg, 3mg respectively;

[0063] 3. Core-shell Fe 3 o 4 The preparation of @COF composite microspheres was the same as described in Examples 1-3.

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Abstract

The invention belongs to the technical field of functional materials and particularly relates to covalent organic frame magnetic composite microspheres of core-shell structure and a preparation method of microspheres. Cores of the core-shell type composite microspheres are ferroferric oxide magnetic particles, and shells are covalent organic frames of ordered porous structures. The preparation method includes the steps that the ferroferric oxide magnetic particles are prepared through the solvothermal method; core-shell type magnetic composite microspheres are obtained through aldimine condensation reaction; under the solvothermal condition, the core-shell type magnetic composite microspheres in a formless and disordered channel state are induced to be converted into highly crystallized covalent organic frames with ordered channels, and the covalent organic frame magnetic composite microspheres with the excellent porous property are obtained. The composite microspheres have the advantages of being uniform in size, high in dispersity, high in mangnetic responsiveness, high and ordered in porosity and the like. The preparation method is simple, the process is controllable, and the size and the appearance of the composite microspheres are kept unchanged. The composite microspheres and the preparation method have wide application prospects in the fields of catalysis, drug loading, molecular sensing, energy storage and the like.

Description

technical field [0001] The invention belongs to the technical field of functional materials, and specifically relates to a covalent organic framework magnetic composite microsphere with a core-shell structure and a preparation method thereof. Background technique [0002] Since Yaghi's group synthesized Covalent Organic Frameworks (COFs) for the first time in 2005, it has aroused extensive research interests of researchers in many fields such as chemistry, materials, energy, and environment. COFs is an organic porous material with a crystalline structure. Compared with traditional porous materials, it has the characteristics of highly ordered porosity, adjustable structure (pore size, specific surface area, etc.), easy functionalization, and thermal stability. Gas adsorption separation, photoelectricity, catalysis and sensing have a very wide range of application potential. [0003] Although the design and synthesis of COFs materials have continued for nearly a decade, ther...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/08C08G12/40C08K3/22H01F1/36B01J13/14
CPCB01J13/14C08G12/08C08G12/40C08K3/22C08K2003/2275H01F1/344H01F1/36
Inventor 郭佳谭晶孔维夫
Owner FUDAN UNIV
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