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High-strength and high-elasticity graphene aerogel free of slag falling and preparation method thereof

A graphene airgel, high-strength technology, applied in graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of large environmental pollution, environmental protection, and graphene airgel slag drop, and achieve excellent return Elastic performance, ultra-high thermal insulation ability, and the effect of improving mechanical strength

Active Publication Date: 2022-01-04
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent application CN108525649A uses polyethyleneimine as the cross-linking agent of the graphene oxide precursor, uses sodium alginate as the reinforcing material, and the sodium alginate cross-links under the action of calcium ions to form graphite oxide with an interpenetrating network structure Graphene airgel, prepared a high-strength graphene airgel material, but without reduction reaction and high-temperature thermal annealing, the overlap between graphene sheets is relatively weak
Chinese patent application CN111100291A reports a method for preparing polybenzoxazine-enhanced three-dimensional graphene foam. Polybenzoxazine polymers are introduced into the three-dimensional graphene system, which can not only play the role of cross-linked graphene sheets, but also It can disperse and transfer stress, and then realize the construction of high-strength three-dimensional graphene structure. However, benzoxazine monomer, which is a raw material that pollutes the environment and is harmful to the body, is used in the preparation process, and it must be used later. A large amount of organic solvents are used for cleaning, which is not environmentally friendly
[0004] In short, the preparation technology of highly elastic graphene airgel has been greatly developed, but the strength of the prepared material still needs to be further improved, and the more serious Yes, there is no report trying to solve the problem of graphene airgel slag drop. Using a simple and easy method to prepare high-strength and high-elastic graphene aerogel without slag drop is of great significance for promoting its engineering application

Method used

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  • High-strength and high-elasticity graphene aerogel free of slag falling and preparation method thereof
  • High-strength and high-elasticity graphene aerogel free of slag falling and preparation method thereof
  • High-strength and high-elasticity graphene aerogel free of slag falling and preparation method thereof

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preparation example Construction

[0032] The present invention provides a method of preparing a high-strength high-elastic graphene gas gel without removing slag, the method comprising the steps of:

[0033] (1) Uniformly mix the oxidation graphene solution, dimethylsiloxane oligomer, and the alkaline catalyst, and then reacted with pre-hydrolysis and pre-woven, to obtain a predetermined graphene precursor; in the present invention, The oxidation graphene solution is an oxide in grapiene aqueous solution; in the present invention, the dimethylsiloxane is inexhate after mixing the oxide in graphene solution, dimethylsiloxane oligomer, and the alkaline catalyst. The polymer is prehydrolyzed under the action of the alkaline catalyst, resulting in a prehyd hydrolyzed dimethylsiloxane oligomer, and the resulting prehyd monomethylsiloxane oligomer is said to the oxide oxide layer The pre-structure (i.e., pre-spoken) is performed at the edge of the upper and lower sides and the oxide oxide to obtain a predetermined oxide...

Embodiment 1

[0051] 1 Single-layer oxide solution of 50 ml of concentration of 20 mg / ml, 0.3 g of dimethylsiloxane oligomer PDMSSSSSSSSSSSSSSELGARD 184 A gum and 0.01 g of concentrated ammonia water (ammonia in concentrated ammonia is 28%), Uniform mixing was mixed with magnetic stirring, pre-hydrolysis and pre-woven reaction for 2 h were stirred at room temperature, resulting in a preparation of the oxide oxide precursor.

[0052] 2 Add 0.5 g of the alkyl glycosidin, 4G reductant disulfuritol, and 0.03 g of dimethylsiloxane crosslinker PDMS Sylgard184B glue, stirring and mixing Sol gel and crosslinking reaction at a high temperature of 120 ° C for 24 h, resulting in a modified graphene wet gel.

[0053] 3 The above-described modified graphene wet gel is placed in a refrigerator having a temperature of -40 ° C to freeze overnight, then placed in a cryogenic dryer, and the inside of the freeze dryer is controlled below 20 Pa, and the temperature is controlled at 25. After 48 h, lyophilized fo...

Embodiment 2

[0055] 1 Single layer oxide solution of 50 ml of concentration of 20 mg / ml, 0.1 g of dimethylsiloxane oligomers PDMSSSSSSSSSSSYLGARD 184 A glue and 0.001 g of concentrated ammonia water (the mass fraction of ammonia contained in concentrated ammonia is 28%), It was mixed with mixing with magnetic stirring, pre-hydrolysis and pre-woven reaction 12 h were prepared at room temperature, resulting in a prehydrolysis and prefluential precursor.

[0056] 2 Add 0.5 g of the alkyl glycosidin, 4G reducing agent disulfurol and 0.01 g of dimethylsiloxane crosslinker PDMS Sylgard184B, and stir well Sol gel and crosslinking reaction at a high temperature of 120 ° C for 24 h, resulting in a modified graphene wet gel.

[0057] 3 The above-described modified graphene wet gel is placed in a refrigerator having a temperature of -40 ° C to freeze overnight, then placed in a cryogenic dryer, and the inside of the freeze dryer is controlled below 20 Pa, and the temperature is controlled at 25. After ...

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Abstract

The invention relates to a high-strength and high-elasticity graphene aerogel free of slag falling and a preparation method thereof. The method comprises the following steps of: well mixing a graphene oxide solution, a dimethyl siloxane oligomer and a basic catalyst, and carrying out pre-hydrolysis and pre-organization reaction to obtain a pre-lapped graphene oxide precursor; adding a foaming agent, a reducing agent and a dimethyl siloxane cross-linking agent into the pre-lapped graphene oxide precursor, stirring well, and then carrying out high-temperature reaction to obtain modified graphene wet gel; and freezing, freeze-drying and thermally annealing the modified graphene wet gel in sequence to obtain the high-strength and high-elasticity graphene aerogel free of slag falling. The graphene aerogel disclosed by the invention has a structure in which a polydimethylsiloxane network and a graphene skeleton network structure penetrate through each other, and the polydimethylsiloxane network plays a role in enhancing lap joint of graphene lamellas, especially edges, so that the problem that the graphene aerogel is easy to slag and low in strength is effectively solved.

Description

Technical field [0001] The present invention belongs to the field of graphene gel technology, and the method of preparation of graphene gas gels, and more particularly to a high-strength high-elastic graphene gas gel and preparation method thereof without removing slag. Background technique [0002] High-elastic graphene gel is a graphene sheet having a certain elasticity as a construction primitive, through various physical or chemical three-dimensional mutual attachment, forming a porous graphene three-dimensional macro Assembly. Elastic graphene gas gel has many excellent characteristics such as ultra high porosity, large specific surface area, ultra-low density, ultra-low-density, excellent conductivity, ultra-low thermal conductivity, etc. Mechanical properties, this elastic material having a larger reversible variable function has broad demand in various engineering applications including insulation, adsorption, sensor, causing strong concern. However, due to the insufficie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184
CPCC01B32/184C01B2204/24C01B2204/26
Inventor 张晚林刘圆圆张恩爽雷朝帅王鹏李文静赵英民张昊
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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