Preparation method of industrial aminated graphene

A technology of aminated graphene and graphene powder, applied in the fields of graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problem that the surface groups cannot be fully utilized, the amount of various groups on the surface cannot be determined, and the graphene sheet The problem of large damage to the layer is achieved, and the effect of reducing oxygen content, high nitrogen content and high interfacial bonding force is achieved.

Active Publication Date: 2019-01-29
CHANGZHOU HIGHBERY NEW NANO MATERIALS TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the above-mentioned problems existing in the prior art, the present invention aims to provide a preparation method for industrialized production of aminated graphene, which solves the problem that the large amount of oxidizing agent used in the preparation process of graphene oxide currently causes high oxygen content in graphene oxide, and the surface cannot be determined. The amount of various groups, surface groups cannot be fully utilized, and the traditional oxidation-reduction method damages the graphene sheet to a great extent, resulting in a decrease in the performance of graphene itself, so that the modification effect cannot be achieved.

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  • Preparation method of industrial aminated graphene

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Embodiment 1

[0035] like figure 1 The method for preparing industrial aminated graphene of the present invention shown, adopts the following steps:

[0036] Step 1, 100kg of graphite powder is peeled off by supercritical carbon dioxide method, the obtained graphite powder is added to 500kg of water, and the obtained slurry is crushed by a homogenizer. The pressure of the homogenizer is 80MPa. , emulsified compound dispersion method, and dry after the dispersion. The drying temperature is 150°C. Add the dried product to 100kg of dilute hydrochloric acid for soaking at -10°C, and then add potassium permanganate and hydrogen peroxide for 4 hours. 10kg of potassium permanganate and 10kg of hydrogen peroxide were used to control the temperature at 10°C. After 2 hours of reaction, 400kg of deionized water was added, suction filtered, washed, and finally dried to obtain graphene oxide powder at a drying temperature of 160°C.

[0037] Step 2, disperse the graphene oxide powder obtained in step 1 ...

Embodiment 2

[0044] The method for preparing industrial aminated graphene of present embodiment 2 adopts the following steps:

[0045] 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 treatment. After the dispersion is completed, it is dried by air-flow spray drying. The drying temperature is 230 ° C. At 20 ° C, the dried product is added to 300 kg of dilute sulfuric acid for soaking. The compound mixture of formyl, in which potassium perchlorate is 100kg, and the mass of benzoyl peroxide is 1kg, the temperature is controlled at 90°C, after 6 hours of reaction, 400kg of deionized water is added, suction filtered, washed, and finally obtained by airflow spray drying Graphene oxide powder, drying temperature is 230°C.

[0046] Step 2, disperse the graphene oxid...

Embodiment 3

[0051] The method for preparing industrial aminated graphene of present embodiment 3 adopts the following steps:

[0052] 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 treatment. After the dispersion is completed, it is dried by air-flow spray drying. The drying temperature is 170 ° C, and the dried product is added to 120 kg of dilute nitric acid for soaking at -1 ° C. The compound mixture of hydrogen peroxide, potassium dichromate 40kg, the mass of hydrogen peroxide is 9kg, the temperature is controlled at 55°C, after 3 hours of reaction, 300kg of deionized water is added, suction filtered, washed, and finally the graphene oxide powder is obtained by airflow spray drying , The drying temperature is 170°C.

[0053] Step 2, disperse the graphen...

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Abstract

The invention discloses a preparation method of industrial aminated graphene. The preparation method of the industrial aminated graphene belongs to the technical field of graphene preparation, and comprises the steps of firstly stripping graphite through a mechanical stripping method, oxidizing through adjusting the matching ratio of a main oxidizing agent and an auxiliary oxidizing agent, then activating hydroxyl and carboxyl on the surface of graphene oxide through a chlorinating agent, and finally selecting appropriate diamine for carrying out amination reaction. According to the preparation method of the industrial aminated graphene provided by the invention, through adopting a stripping manner at first, the dosage of the oxidizing agents can be reduced, an ideal effect is achieved atthe same time, and the problem of poor modification effect caused by high oxygen content and severe destructiveness on a graphene slice layer due to large dosage of the oxidizing agents is solved.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, and more specifically relates to a method for preparing industrial aminated graphene. Background technique [0002] Graphene is a carbon atom with sp 2 The hybrid orbital line forms a hexagonal planar film with a honeycomb lattice, and its thickness is the thickness of a carbon atomic layer (0.35nm), which is the thinnest material found so far. Graphene has unique physical and chemical properties. It is the material with the highest hardness known so far. Its Young's modulus exceeds 1000GPa, and it also has good toughness; thermal conductivity is 3000W / mK; charge migration speed is 2×105cm 2 / Vs; Specific surface area up to 2600m 2 / g. [0003] Graphene oxide (GO) is a functionalized graphene that introduces functional groups on the graphene sheet to make it have some new properties. The functional groups include the basal surface of graphene oxide. The hydroxyl group and epoxy g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19C01B32/194C01B32/198C08L77/02C08K9/04C08K9/02C08K9/00C08K7/00
CPCC01B32/19C01B32/194C01B32/198C01B2204/04C01B2204/32C08K7/00C08K9/00C08K9/02C08K9/04C08L2201/02C08L77/02Y02P20/54
Inventor 蒋炎曹建鹏黄荣庆周良艳
Owner CHANGZHOU HIGHBERY NEW NANO MATERIALS TECH CO LTD
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