Preparation method of industrial aminated graphene

A technology of aminated graphene and graphene powder, applied in graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problem that surface groups cannot be fully utilized, the amount of various groups on the surface cannot be determined, and graphene sheets cannot be fully utilized. 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: 2018-08-07
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] Such as figure 1 The method for preparing industrial aminated graphene according to the present invention adopts the following steps:

[0036] Step 1. Strip 100kg of graphite powder by supercritical carbon dioxide method, add 500kg of water to the obtained graphite powder, and crush the resulting slurry through a homogenizer. The pressure of the homogenizer is 80MPa. After the crushing is completed, ultrasonic and shearing , The emulsified compound dispersion method is used for processing. After the dispersion is completed, it is dried. The drying temperature is 150℃. Add the dried product to 100kg dilute hydrochloric acid for soaking at -10℃, and then add potassium permanganate and hydrogen peroxide compound after 4h. The mass of potassium permanganate is 10kg, the mass of hydrogen peroxide is 10kg, the temperature is controlled at 10℃, 400kg of deionized water is added after 2h reaction, suction filtration, washing, and finally drying to obtain graphene oxide powder, the...

Embodiment 2

[0044] The method for preparing industrial aminated graphene in Example 2 adopts the following steps:

[0045] Step 1. Exfoliate 100kg of vermicular graphite with supercritical carbon dioxide, add 500kg of water to the obtained graphite powder, and crush the resulting slurry through a homogenizer. The pressure of the homogenizer is 150MPa. After the crushing is completed, ultrasonic, shear, The emulsified compound dispersion method is used for processing. After the dispersion is completed, air-flow spray drying is used for drying. The drying temperature is 230 ℃, and the dried product is added to 300 kg of dilute sulfuric acid for soaking at 20 ℃. After 0.5h, potassium perchlorate and benzene peroxide are added. The compound mixture of formyl, in which potassium perchlorate is 100kg, the mass of benzoyl peroxide is 1kg, the temperature is controlled at 90℃, 400kg of deionized water is added after 6 hours of reaction, filtered, washed, and finally obtained by airflow spray drying ...

Embodiment 3

[0051] The method for preparing industrial aminated graphene in Example 3 adopts the following steps:

[0052] Step 1. Strip 100kg of flake graphite through supercritical carbon dioxide, add 500kg of water to the obtained graphite powder, and crush the resulting slurry through a homogenizer. The pressure of the homogenizer is 110MPa. After the crushing is completed, ultrasonic, shear, The emulsified compound dispersion method is used for processing. After the dispersion is completed, it is dried by airflow spray drying. The drying temperature is 170 ℃, and the dried product is added to 120 kg of dilute nitric acid for soaking at -1 ℃. After 1.5 hours, potassium dichromate and potassium dichromate are added. The compound mixture of hydrogen peroxide, 40kg potassium dichromate, 9kg hydrogen peroxide, control the temperature at 55℃, add 300kg deionized water after 3 hours of reaction, suction filter, wash, and finally obtain graphene oxide powder by airflow spray drying , Drying tem...

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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 kind of sp 2 The hybrid orbitals are arranged into a hexagonal flat film with a honeycomb lattice, and its thickness is the thickness of a carbon atom layer (0.35nm), which is the thinnest material found so far. Graphene has unique physical and chemical properties and is the hardest substance known at present. Its Young's modulus exceeds 1000 GPa and has good toughness; thermal conductivity is 3000W / mK; charge transfer 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 give it some new characteristics. The functional groups include the base surface of graphene oxide. The hydroxy and epoxy groups as well as the carboxyl and hydroxy gr...

Claims

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Application Information

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Patent Type & Authority Applications(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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