A kind of method utilizing supercritical fluid to prepare and disperse graphene

A supercritical fluid, dispersed graphite technology, applied in graphene, bulk chemical production, nano-carbon and other directions, can solve the problems of weakening some properties of materials, requiring organic solvents, and taking a long time to achieve easy large-scale production, improve Safety, the effect of mature equipment

Active Publication Date: 2018-03-20
陕西霸天虎信息科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in these modification methods, organic chemical reactions are involved, which have disadvantages such as time-consuming, low efficiency, and the need for organic solvents.
At the same time, studies have shown that the introduction of a third component such as a compatibilizer can also effectively weaken the agglomeration of graphene in the matrix, but the third component may weaken some of the properties of the material.
[0005] It can be seen that there is still a lack of an efficient, green and environmentally friendly method for improving the dispersion of graphene nanomaterials in polymer matrices in the prior art.

Method used

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  • A kind of method utilizing supercritical fluid to prepare and disperse graphene

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Effect test

Embodiment 1

[0027] A method utilizing supercritical fluid to prepare and disperse graphene, the steps are as follows:

[0028] A. First, add 16kg of graphite powder, 8kg of sodium nitrate and 15L of intercalation agent into the reaction kettle f, and then add 400l of sulfuric acid solution, stir and mix under ice-water bath; then gradually add 72kg of potassium permanganate within 1 hour Add to the reaction system, keep the temperature below 10°C and stir for 1 hour; remove the ice bath, heat the system at 30°C for 2 hours, then gradually add 1600l of water into the reaction system under strong stirring conditions , followed by adding hydrogen peroxide (3%) aqueous solution until disappearance of bubbling; then washing with distilled water to neutrality to obtain a uniform colloidal graphite oxide solution, and drying in a vacuum oven at 60°C for 72h to obtain graphite oxide; Put the dry graphite oxide into the quartz tube, pump out the air in the quartz tube, then slowly introduce argon ...

Embodiment 2

[0033] A method utilizing supercritical fluid to prepare and disperse graphene, the steps are as follows:

[0034] A. Put it in a mixed solution composed of concentrated sulfuric acid, hydrogen peroxide and dimethylformamide, and stir it at 50°C for 2 hours. Treat at medium temperature and high temperature of 800°C for 20s to obtain expanded graphite product for later use;

[0035]B. After mixing 85g of expanded graphite, 0.5g of sodium dodecylbenzenesulfonate and 200g of polylactic acid-glycolic acid copolymer to obtain a mixture, the internal mixer is heated to 80°C, and then added to the mixture, and Pump in supercritical carbon dioxide to a pressure of 15 MPa, then banbury with the mixer at a stirring speed of 260rpm for 27min, then raise the temperature to 150°C, and banbury at a stirring speed of 150rpm for 30min;

[0036] C. After banburying, release the pressure to normal pressure, and the pressure release time is 100min, so that the graphene can be uniformly disperse...

Embodiment 3

[0038] A method utilizing supercritical fluid to prepare and disperse graphene, the steps are as follows:

[0039] A. First, add 16kg flake graphite, 8kg sodium nitrate and 15L methylacetamide to the reaction kettle, and then add 400l sulfuric acid solution, stir and mix under ice-water bath; then gradually add 80L concentrated nitric acid to the reaction vessel within 1 hour In the system, keep the temperature below 10°C and stir for 1 hour; remove the ice bath, heat the system at 30°C for 2 hours, then gradually add 1600l of water into the reaction system under strong stirring conditions, and then add Hydrogen peroxide (3%) aqueous solution, bubble until disappearance; Then wash with distilled water to neutrality, obtain uniform colloidal graphite oxide solution, and place in the vacuum oven of 60 ℃ and dry 72h, obtain graphite oxide; Graphite oxide is put into the quartz tube, the air in the quartz tube is pumped out, and then the argon gas is slowly introduced, and the arg...

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Abstract

The invention relates to the technical field of production of graphene and particularly relates to a method for preparation and dispersion of graphene through a supercritical fluid. The method comprises dispersing expanded graphite in a polymer, carrying out melting internal mixing and stretching in an internal mixer, simultaneously, applying a supercritical fluid to materials so that the supercritical fluid permeates into layers of the expanded graphite, wherein in internal mixing, graphene is obtained by in-situ stripping of graphite under polymer shearing, stretching and dispersion and is uniformly dispersed in the polymer, and carrying out slow pressure release to obtain a graphene dispersoid. The method is free of fast pressure release, safely strips and prepares graphene through a supercritical gas flow and uniformly disperses graphene. The product can be well dispersed in plastic and rubber.

Description

technical field [0001] The invention relates to the technical field of production and preparation of graphene, in particular to a method for preparing and dispersing graphene using a supercritical fluid. Background technique [0002] In 2004, two scientists from the University of Manchester in the United Kingdom discovered graphene using the method of micromechanical exfoliation, and won the Nobel Prize in Physics in 2010. Graphene is a flat plate structure with a single atom thickness and sp2 bonded carbon atoms. In theory, it has a perfect hexagonal network structure and exhibits excellent electronic stability, thermal conductivity, optical properties, and mechanical properties. Since the discovery of graphene, due to its excellent performance and huge market application prospects, it has triggered a research boom in the fields of physics and material science. Graphene is currently the thinnest and hardest nanomaterial. It also has properties that many ordinary materials ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19C08L23/06C08L67/04C08K7/24C08K3/04C08K7/00C08L67/02C08L39/06
CPCC01P2004/03C08K3/04C08K7/00C08K7/24C08L67/02C08L23/06C08L67/04C08L39/06Y02P20/54
Inventor 陈庆曾军堂陈兵
Owner 陕西霸天虎信息科技有限公司
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