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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  • 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 nanopar

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

Examples

Experimental program
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Example Embodiment

[0033] Example 1

[0034] Prepare FeCl under the condition that the total iron concentration is 0.5mol / L 2 ·4H 2 O and FeCl 3 ·6H 2 A 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 quickly, wash the mixed colloid with absolute ethanol 3 times, ultrasonically break, the ultrasonic frequency is 20KHz, the ultrasonic time is 10min, to make the colloid uniform Dispersed 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 double distilled water to 11.2mL of tetraethylorthosilicate, heat and stir for 6.5h, and control the temperature at 85℃ to completely hydrolyze the tetraethylorthosilicate. Si(OH) 4 . Fe(OH) 2 With Fe(OH) 3 The mixed colloid is quickly added to Si(OH) 4 In the process, keep stirring, add 1:2 KOH ethanol solution to adjust the pH value to 8.9, keep the temperature in a constant temperature box...

Example Embodiment

[0038] Example 2

[0039] Prepare FeSO under the condition of total iron concentration of 0.1mol / L 4 ·6H 2 O and Fe(NO 3 ) 3 ·9H 2 A mixed aqueous solution of O, where Fe 2+ With Fe 3+ The molar ratio is 1:1, stir quickly to dissolve, then add 60mL 0.1mol / L ammonia ethanol solution, stir quickly, wash the mixed colloid with absolute ethanol 5 times, ultrasonically break, ultrasonic dispersion frequency is 60KHz, ultrasonic time is 6min , Make the colloid evenly 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 to the ethanol solution, heat and stir for 1 h, control the temperature at 70 ℃, and make Na 2 SiO 4 Completely hydrolyze to form Si(OH) 4 . Fe(OH) 2 With Fe(OH) 3 The mixed colloid is quickly added to Si(OH) 4 In the process, keep stirring, add 1:50 NaOH ethanol solution to adjust the pH value of 7.8, and keep the temperature at 60°C for 5 hours, the mixed solution will form...

Example Embodiment

[0042] Example 3

[0043] Prepare FeCl under the condition that the total iron concentration is 0.1mol / L 2 ·4H 2 O and FeCl 3 ·6H 2 O mixed ethanol solution, of which 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, Disperse the colloid evenly in ethanol, where Fe(OH) 2 With Fe(OH) 3 The molar ratio is 1:4. Add 0.6mL of 1mol / L HCl solution and 5.4mL of distilled water to the ethanol solution of tetraethylorthosilicate, heat and stir for 1h, and control the temperature at 60℃ to completely hydrolyze the tetraethylorthosilicate to produce Si(OH) 4 . Fe(OH) 2 With Fe(OH) 3 The mixed colloid is quickly added to Si(OH) 4 In the process, keep stirring, add 1:20 ammonia ethanol solution to adjust the pH value of 8.6, keep the temperature in a constant temperature box at ...

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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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