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Preparation of surface roughened magnetic nano-microspheres and composite materials thereof

A magnetic nanometer and nanometer microsphere technology, applied in the field of nanomaterials, can solve the problems of composite material performance influence, poor interface compatibility, etc.

Active Publication Date: 2016-12-14
UNIV OF ELECTRONIC SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the surface of magnetic nanomaterials prepared by solvothermal method is relatively dense and smooth, and the interfacial compatibility is poor when composited with the polymer matrix, which has a significant impact on the properties of the obtained composite materials.

Method used

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  • Preparation of surface roughened magnetic nano-microspheres and composite materials thereof
  • Preparation of surface roughened magnetic nano-microspheres and composite materials thereof
  • Preparation of surface roughened magnetic nano-microspheres and composite materials thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Step 1. Weigh 6.75g FeCl 3 ·6H 2 O was dissolved in 200mL of ethylene glycol, 1.0g of biphenol type bisphthalonitrile resin (BPh) was dissolved in 3mL of NMP and added to the ethylene glycol solution, then 5.0g of polyethylene glycol 2000 was added, After stirring for 30 minutes, slowly add 18 g of crystalline sodium acetate, and react for 1 hour at normal temperature and pressure;

[0026] Step 2. Transfer the above reaction solution to a polytetrafluoro autoclave, the filling amount of the precursor solution is 80%, and react at 200°C for 15 hours;

[0027] Step 3. Wash the nanospheres prepared in step 2 with deionized water and ethanol for 2-3 times, then transfer them to 100mL NMP, and react at 80°C for 30h;

[0028] Step 4, the suspension obtained in Step 3 is subjected to solid-liquid separation, and then the solid component is washed 3-4 times with deionized water, and finally dried in a freeze dryer;

[0029] Step 5. Add 0.1 g of the microspheres obtained in ...

Embodiment 2

[0033] Step 1. Weigh 11.2g FeCl 3 ·6H 2 O was dissolved in 200mL ethylene glycol, 3.5g trifunctional phthalonitrile resin (TPh) was dissolved in 5mL NMP and added to the ethylene glycol solution, then 5.6g polyethylene glycol 2000 was added, and stirred for 30min Slowly add 31.2g of crystalline sodium acetate, and react for 1h at normal temperature and pressure;

[0034] Step 2. Transfer the above reaction solution to a polytetrafluoro autoclave, the filling amount of the precursor solution is 80%, and react at 200°C for 15 hours;

[0035] Step 3. Wash the nanospheres prepared in Step 2 with deionized water and ethanol for 2-3 times, then transfer them to 100 mL of NMP, and react at 80° C. for 30 h;

[0036] Step 4, the suspension obtained in Step 3 is subjected to solid-liquid separation, and then the solid component is washed 3-4 times with deionized water, and finally dried in a freeze dryer;

[0037]Step 5. Add 0.06g of microspheres obtained in step 4 into 6mL NMP, and ...

Embodiment 3

[0041] Step 1. Weigh 7.3g FeCl 3 ·6H 2 O was dissolved in 160mL of ethylene glycol, 2.0g of phthalonitrile resin (2PEN-Ph) containing bisphenol A ether nitrile chain segment was dissolved in 3mL of NMP and added to the ethylene glycol solution, and then 5.4g of poly Ethylene glycol 2000, after stirring for 30 minutes, slowly add 24.48 g of crystalline sodium acetate, and react for 1 hour at normal temperature and pressure;

[0042] Step 2. Transfer the above reaction solution to a polytetrafluoro autoclave, the filling amount of the precursor solution is 80%, and react at 200° C. for 12 hours;

[0043] Step 3. Wash the nanospheres prepared in Step 2 with deionized water and ethanol for 2-3 times, then transfer them to 100 mL of NMP, and react at 80° C. for 30 h;

[0044] Step 4, the suspension obtained in Step 3 is subjected to solid-liquid separation, and then the solid component is washed 3-4 times with deionized water, and finally dried in a freeze dryer;

[0045] Step 5...

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Abstract

The invention relates to a preparation technology of surface roughened (microporous) magnetic nano-microspheres and composite materials thereof and belongs to the field of nanometer materials. The technology comprises the following steps: taking a series of phthalonitrile of different structures as organic monomers, taking FeCl3.6H2O as an iron source, taking ethylene glycol as a solvent and a reducing agent, performing redox self-assembling according to a one-step solvothermal method, thereby obtaining iron phthalocyanine / Fe3O4 magnetic nano-microspheres; performing surface etching on the microspheres to obtain surface roughened and porous nano-microspheres, uniformly dispersing the nano-microspheres into an aromatic nitrile polymer, thereby obtaining a polymer-based nanometer composite material which is high in thermal stability and excellent in interfacial compatibility and has excellent magnetic properties. According to the invention, the surface roughened and porous iron phthalocyanine / Fe3O4 magnetic nano-microspheres are prepared according to a simple method, and have potential application values in aspects such as catalyst carriers, adsorbing materials and the like. In addition, due to the roughened surface, the interfacial compatibility between a matrix and a filler is effectively improved, and the nano-microspheres can be widely applied to the field of materials such as magnetic composite materials, capacitors, semiconductor film devices and the like.

Description

technical field [0001] The invention relates to a technology for preparing surface roughened (microporous) magnetic nano microspheres and composite materials thereof. The technology includes the preparation of magnetic nano-microspheres under specific conditions, the roughening of the surface of the microspheres and the preparation of composite materials with high interfacial compatibility, and belongs to the field of nano-materials. The surface of the obtained magnetic nano microspheres is rough and porous, and the specific surface area and pore volume are large. The obtained composite material has the characteristics of high temperature resistance, good interfacial compatibility, magnetic functionalization and the like. Background technique [0002] Magnetic nano-hybrid materials are organic functional materials with certain magnetic properties and special structures formed by combining inorganic magnetic nanoparticles and organic matter through appropriate methods. As a...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01D53/02
CPCB01D53/02B01J20/06B01J20/223B01J20/28007B01J20/28009B01J20/28059B01J2220/46B01J2220/4806B01J2220/4812
Inventor 徐明珍李逵潘海尤勇刘孝波
Owner UNIV OF ELECTRONIC SCI & TECH OF CHINA
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