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Preparation method of graphene oxide/silicon dioxide hybrid aerogel

A silica and graphene technology, applied in the field of aerogels, can solve the problems of inability to resist, poor gel network structure strength, etc., and achieve the effects of good adsorption, strong solvent adsorption, and guaranteeing strength and stability.

Active Publication Date: 2016-01-06
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, although freeze-drying can remove the solvent in the gel network, the gel network itself has poor structural strength and cannot resist the volume expansion of the solvent crystallization during the freezing process. In the end, only powdered airgel can be obtained instead of a block. Aerogels, which limit their applications

Method used

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  • Preparation method of graphene oxide/silicon dioxide hybrid aerogel

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Embodiment 1

[0041] A preparation method of graphene oxide / silica hybrid airgel, the steps are as follows: A, preparation of silica microspheres: 0.05mol ethyl orthosilicate is added to 9ml of distilled water, then slowly drop Add the 0.5mol / L oxalic acid solution into the tetraethyl orthosilicate aqueous solution, wherein the molar ratio of oxalic acid and tetraethyl orthosilicate is 1:50; stir for 5 hours at 25°C; then add the ammonia solution with a concentration of 1mol / L , adjusting the pH value of the reaction system to pH = 7, stirring for 10 min to obtain a dispersion containing silica microspheres;

[0042] B. Preparation of hybrid hydrogel: Dilute the dispersion of silica microspheres with water 10 times to obtain a diluted dispersion of silica microspheres; then dilute the dispersion of silica microspheres with a concentration of 0.8mg / ml Mix equal volumes of the graphene oxide dispersion, stir for 15 minutes at a stirring speed of 50 r / min, and then ultrasonicate for 15 minutes...

Embodiment 2

[0046] A preparation method of graphene oxide / silica hybrid airgel, the steps are as follows: A, preparation of silica microspheres: 0.05mol ethyl orthosilicate is added to 9ml of distilled water, then slowly drop Add the 0.5mol / L oxalic acid solution into the tetraethyl orthosilicate aqueous solution, wherein the molar ratio of oxalic acid and tetraethyl orthosilicate is 1:50; stir for 5 hours at 25°C; then add the ammonia solution with a concentration of 1mol / L , adjusting the pH value of the reaction system to pH = 7, stirring for 10 min to obtain a dispersion containing silica microspheres;

[0047] B. Preparation of hybrid hydrogel: Dilute the dispersion of silica microspheres with water 20 times to obtain a diluted dispersion of silica microspheres; then dilute the dispersion of silica microspheres with a concentration of 0.8mg / ml Mix equal volumes of the graphene oxide dispersion, stir for 15 minutes at a stirring speed of 50 r / min, and then ultrasonicate for 15 minutes...

Embodiment 3

[0057] A preparation method of graphene oxide / silica hybrid airgel, the steps are as follows: A, preparation of silica microspheres: 0.1mol ethyl orthosilicate is added to 18ml of distilled water, then slowly drop Add oxalic acid solution with a concentration of 0.6mol / L to an aqueous tetraethyl orthosilicate solution, where the molar ratio of oxalic acid and ethyl orthosilicate is 1:100; stir for 6 hours at 30°C; then add ammonia with a concentration of 0.5mol / L aqueous solution, adjust the pH value of the reaction system to pH = 6.5, and stir for 45 minutes to obtain a dispersion containing silica microspheres;

[0058] B. Preparation of hybrid hydrogel: Dilute the dispersion of silica microspheres with water 5 times to obtain a diluted dispersion of silica microspheres; then dilute the dispersion of silica microspheres with oxidized The graphene dispersion was mixed in equal volumes, stirred for 10 minutes, the stirring speed was 100r / min, and then ultrasonicated for 10 min...

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Abstract

A preparation method of graphene oxide / silicon dioxide hybrid aerogel comprises the following steps: A, adding 0.05-0.1 mol of a precursor into 9-18 ml of distilled water and dropwise adding a hydrolyst with its concentration of 0.2-0.6 mol / L into the precursor aqueous solution, wherein molar ratio of the hydrolyst to the precursor is 1:20-1:100; stirring at 20-30 DEG C for 5-8 h; adjusting pH value to 6-7 and stirring for 5-45 min so as to obtain a dispersion containing silicon dioxide microspheres; B, adding water to dilute the silicon dioxide microsphere dispersion by 5-50 times, carrying out iso-volume mixing on the diluted silicon dioxide microsphere dispersion and a graphene oxide dispersion with its concentration being 0.6-2 mg / ml, stirring for 10-30 min, carrying out ultrasonic treatment for 10-30 min so as to obtain graphene oxide / silicon dioxide hybrid aerogel; and C, freezing the hybrid aerogel under liquid nitrogen for 5-10 min, freeze-drying and dewatering to obtain the graphene oxide / silicon dioxide hybrid aerogel. The method is environmentally friendly, and the technology is simple. The prepared hybrid aerogel has advantages of complete gel network structure, high porosity, good adsorptivity, high strength, low density and the like.

Description

technical field [0001] The invention relates to a preparation method of graphene oxide / silicon dioxide hybrid airgel, which belongs to the technical field of airgel. Background technique [0002] Airgel refers to a lightweight nano-solid material that aggregates micro-nano particles to form a nano-porous network structure, and is filled with a gaseous dispersion medium in the network pores. It has extremely low density, high specific surface area, extremely high porosity and ultra-high porosity. volumetric characteristics. Therefore, airgel materials have received extensive attention in energy materials, optical materials, magnetic materials, catalyst materials, and heat and sound insulation materials. The most common airgel is silicon dioxide (SiO 2 ) airgel. SiO 2 Airgel is a porous, lightweight, amorphous nano-solid material with a continuous three-dimensional space network structure formed by interconnected nano-scale particles. Typical SiO 2 Airgel has a high speci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/16
Inventor 王勇肖燕君杨静晖张楠黄婷
Owner SOUTHWEST JIAOTONG UNIV
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