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Preparation method of graphene

A technology of graphene and graphene powder, which is applied in the direction of graphene, bulk chemical production, nano-carbon, etc., can solve the problems of large damage to graphene sheets, affecting the modification and application of polymer materials, and reducing the performance of graphene. Achieve good modification effect, lower oxygen content, and reduce dosage

Active Publication Date: 2018-11-13
中山市悦泰汽车零部件有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The existing redox method to prepare graphene oxide has great damage to the graphene sheet, resulting in a decrease in the performance of graphene, which further affects the modification application in polymer materials.

Method used

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Comparison scheme
Effect test

Embodiment 1

[0028] A kind of graphene preparation method of the present invention adopts the following steps:

[0029] Step 1, peel off 100kg of graphite powder by supercritical carbon dioxide method, add 500kg of water to the obtained graphite powder, and crush the obtained slurry through a homogenizer. The pressure of the homogenizer is 90MPa. , emulsified composite dispersion method for processing, after the dispersion is dried, the drying temperature is 150 ° C.

[0030] Step 2, add the dry product to 100kg of dilute hydrochloric acid for soaking at -10°C, and then add the compound of potassium dichromate and hydroperoxide after 4 hours, wherein 10kg of potassium dichromate and the mass of hydroperoxide 10kg, control the temperature at 10°C, add 400kg of deionized water after 2.5h of reaction, suction filter, wash, and finally dry to obtain graphene oxide powder, the drying temperature is 160°C.

[0031] Step 3, disperse the graphene oxide powder obtained in step 2 in 200kg of dichlo...

Embodiment 2

[0037] Present embodiment 2 a kind of graphene preparation method, adopts the following steps:

[0038] Step 1, 100kg of worm graphite is stripped by supercritical carbon dioxide, the graphite powder obtained is added to 500kg of water, and the obtained slurry is crushed by a homogenizer. The pressure of the homogenizer is 150MPa. The emulsified compound dispersion method is used for processing, and after the dispersion is completed, it is dried by air-flow spray drying, and the drying temperature is 230°C.

[0039] Step 2, add the dry product to 250kg of dilute hydrochloric acid for soaking at 15°C, and then add the compound mixture of potassium dichromate and hydroperoxide after 1 hour, wherein potassium dichromate is 90kg and the compound mixture of hydroperoxide The mass is 5kg, and the temperature is controlled at 85°C. After 6 hours of reaction, 400kg of deionized water is added, suction filtered, washed, and finally the graphene oxide powder is obtained by airflow spray...

Embodiment 3

[0045] Present embodiment 3 a kind of graphene preparation method, adopts the following steps:

[0046] Step 1, 100kg flake graphite is stripped by supercritical carbon dioxide, and the obtained graphite powder is added to 500kg water, and the obtained slurry is crushed by a homogenizer. The pressure of the homogenizer is 110MPa. The emulsified compound dispersion method is used for processing, and after the dispersion is completed, it is dried by air-flow spray drying, and the drying temperature is 170°C.

[0047] Step 2, add the dried product into 120kg of dilute hydrochloric acid for immersion at -1°C, then add the compound mixture of potassium dichromate and hydroperoxide after 2 hours, the quality of potassium dichromate 40kg and hydroperoxide is 9kg, control the temperature at 55°C, add 300kg of deionized water after 3.5h of reaction, filter with suction, wash, and finally obtain graphene oxide powder by airflow spray drying at a drying temperature of 170°C.

[0048] St...

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Abstract

The invention discloses a preparation method of graphene. The preparation method of the graphene comprises the following steps: 1, stripping graphite by a supercritical carbon dioxide stripping method, dispersing the obtained graphite powder into deionized water, crushing by a homogenizer, controlling the pressure to 90 to 150 MPa, and sequentially dispersing and drying; and 2, soaking and washingthe dry product in the step 1 with diluted hydrochloric acid, wherein the soaking temperature is -10 to 15 DEG C, the soaking time is 1 to 4 hours, and the mass ratio of the diluted hydrochloric acidto the graphite is (1-2.5):1, adding a compound of potassium dichromate and hydroperoxide, performing oxidation reaction at the reaction temperature of 10 to 85 DEG C for 2.5 to 6 hours, and sequentially performing water washing, suction filtration and drying after reaction to obtain graphene oxide powder. An aminated graphene sheet obtained by the preparation method of the graphene has small diameter and small layer number, is favorable for being dispersed in a base material when a macromolecular material is modified, avoids aggregation and can achieve a good modification effect under the condition of small adding amount.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, and in particular relates to a graphene preparation method. Background technique [0002] The existing redox method to prepare graphene oxide has great damage to the graphene sheet, resulting in a decrease in the performance of graphene, which further affects the modification application in polymer materials. Therefore, there is an urgent need for an efficient and mass-produced graphene preparation method. Contents of the invention [0003] 1. Technical problems to be solved [0004] The technical problem to be solved by the present invention is to provide a graphene preparation method to solve the technical problem. [0005] 2. Technical solution [0006] For solving described technical problem, the technical scheme that the present invention adopts is: a kind of preparation method of graphene, comprises the following steps: [0007] Step 1, the graphite is stripped by supercr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184C01B32/19
CPCC01B32/184C01B32/19Y02P20/54
Inventor 高维佳
Owner 中山市悦泰汽车零部件有限公司
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