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Method for preparing nano Fe3O4/SiO2 composite aerogel granule by supercritical process

A composite aerogel, supercritical technology, applied in chemical instruments and methods, colloidal chemistry, colloidal chemistry, etc., can solve problems such as uneven distribution of nanoparticles that are easy to fall off

Active Publication Date: 2009-07-22
江苏安珈新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is in order to prepare nano-Fe in the past 3 o 4 / SiO 2 Composite airgel particles in the application process of SiO 2 Easy Shedding and Fe 3 o 4 The problem of uneven distribution of nanoparticles provides a supercritical method for preparing nano-Fe 3 o 4 / SiO 2 A method for composite airgel particles, the method has simple process, easy control of the preparation process, uniform nanoparticles and strong magnetic properties

Method used

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  • Method for preparing nano Fe3O4/SiO2 composite aerogel granule by supercritical process
  • Method for preparing nano Fe3O4/SiO2 composite aerogel granule by supercritical process
  • Method for preparing nano Fe3O4/SiO2 composite aerogel granule by supercritical process

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Effect test

Embodiment 1

[0034] Prepare FeCl according to the condition that the total iron concentration is 0.5mol / L 2 4H 2 O and FeCl 3 ·6H 2 Mixed aqueous solution of O, where Fe 2+ with Fe 3+ The molar ratio is 8:1, stir to dissolve, then add 20mL 1mol / L NaOH ethanol solution, stir rapidly, wash the mixed colloid with absolute ethanol 3 times, ultrasonically break, the ultrasonic frequency is 20KHz, and the ultrasonic time is 10min, so that the colloid is uniform Dispersion in ethanol, where Fe(OH) 2 with Fe(OH) 3 The molar ratio is 8:1. Add 50mL of absolute ethanol, 2mL of 1mol / L HCl solution and 5.4mL of twice distilled water to 11.2mL tetraethyl orthosilicate, heat and stir for 6.5h, control the temperature at 85°C, and completely hydrolyze tetraethyl orthosilicate to form Si(OH) 4 . Fe(OH) 2 with Fe(OH) 3 The mixed colloids are quickly added to the Si(OH) 4 , stirring continuously, adding 1:2 KOH ethanol solution to adjust the pH value to 8.9, and keeping the temperature in a const...

Embodiment 2

[0039] Prepare FeSO under the condition that the total iron concentration is 0.1mol / L 4 ·6H 2 O and Fe(NO 3 ) 3 9H 2 Mixed aqueous solution of O, where Fe 2+ with Fe 3+ The molar ratio is 1:1, stir quickly to dissolve, then add 60mL0.1mol / L ammonia water ethanol solution, stir quickly, wash the mixed colloid with absolute ethanol 5 times, ultrasonically break, the ultrasonic dispersion frequency is 60KHz, and the ultrasonic time is 6min , so that the colloid is uniformly dispersed in ethanol, where Fe(OH) 2 with Fe(OH) 3 The molar ratio is 1:1. in Na 2 SiO 4Add 1 mL of 1.5 mol / L HCl solution and 7 mL of distilled water into the ethanol solution, heat and stir for 1 h, and control the temperature at 70 °C to make Na 2 SiO 4 Complete hydrolysis to Si(OH) 4 . Fe(OH) 2 with Fe(OH) 3 The mixed colloids are quickly added to the Si(OH) 4 , stirring continuously, adding 1:50 NaOH ethanol solution to adjust the pH value to 7.8, keeping the temperature in a constant temp...

Embodiment 3

[0043] Prepare FeCl according to the condition that the total iron concentration is 0.1mol / L 2 4H 2 O and FeCl 3 ·6H 2 Mixed ethanol solution of O, where Fe 2+ with Fe 3+ The molar ratio is 1:4, stir quickly to dissolve, then add 10mL1.2mol / L NaOH ethanol solution, stir quickly, wash the mixed colloid with absolute ethanol 3 times, ultrasonically break, ultrasonic dispersion frequency is 100KHz, ultrasonic time is 4min, Make the colloid evenly dispersed in ethanol, where Fe(OH) 2 with Fe(OH) 3 The molar ratio is 1:4. Add 0.6 mL of 1 mol / L HCl solution and 5.4 mL of distilled water into the ethanol solution of tetraethyl orthosilicate, heat and stir for 1 hour, and control the temperature at 60°C to completely hydrolyze tetraethyl orthosilicate to generate Si(OH) 4 . Fe(OH) 2 with Fe(OH) 3 The mixed colloids are quickly added to the Si(OH) 4 , stirring continuously, adding 1:20 ammonia water ethanol solution to adjust the pH value to 8.6, and keeping the temperature ...

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Abstract

The invention relates to a method for preparing a nanometer Fe3O4 / SiO2 composite aerogel particle by a supercritical method. The method is characterized in that: firstly, by utilizing a sol-gel method, precursors-Fe(OH)2 and Fe(OH)3 of a Fe3O4 crystal are prepared, and the precursors are added in a precursor of SiO2 aerogel, subjected to ultrasound for a few minutes, stirred at a high speed and added with certain amount of alkali solution to be gelled so as to obtain a composite wet gel system; by utilizing a supercritical drying method, a nanometer magnetic Fe3O4 / SiO2 composite aerogel material is prepared by drying, and a nanometer magnetic Fe3O4 / SiO2 composite aerogel material with stable dispersion, no obvious agglomeration and even distribution is further prepared; and finally, the composite aerogel material is ball-milled to obtain the nanometer magnetic Fe3O4 / SiO2 composite aerogel particle. The preparation method has the advantages of simple and practical process and easy control of the preparation process, and the prepared nanometer magnetic Fe3O4 / SiO2 composite material is stable in quality.

Description

technical field [0001] The invention relates to the preparation of nano-Fe 3 o 4 / SiO 2 A method for composite airgel particles, especially a supercritical method for preparing nano-Fe 3 o 4 / SiO 2 Method for Composite Airgel Particles. Background technique [0002] Nano Fe 3 o 4 It has excellent performance in magnetism, catalysis, biology and so on. Nano Fe 3 o 4 Nano Fe 3 o 4 It has been widely used in the fields of pigment, magnetic fluid, magnetic microsphere, magnetic recording, catalysis, electronics, finance, communication, paint, ink, medicine, developer, photosensitive material and microwave absorbing material. [0003] SiO 2 Airgel is a new type of porous material with controllable structure, which has a large specific surface area (up to 1000g / m 2 ), high porosity (up to 90%), low density (minimum 0.02g / cm 3 ), low refractive index, strong adsorption, typical fractal structure and many unique properties, which have been widely used in many research...

Claims

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Application Information

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IPC IPC(8): B01J13/00
Inventor 沈晓冬伊希斌崔升
Owner 江苏安珈新材料科技有限公司
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