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Preparation method of graphene

A graphene and graphite technology, applied in the field of graphene, can solve the problems of uncontrolled heating of reactants, failure of oxidation reaction, etc., and achieve the effects of strong temperature controllability and good batch consistency

Active Publication Date: 2015-07-22
GUANGDONG ZHUGUANG NEW ENERGY TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] However, when the oxidation method is used to prepare graphite oxide, the oxidants used are often concentrated sulfuric acid, potassium permanganate and other oxidants, which will release a large amount of heat during the feeding and mixing process, causing the temperature of the reactants to rise out of control, which in turn leads to the failure of the entire oxidation reaction. even serious accidents
[0005] In view of this, it is necessary to develop a new graphene preparation method to solve the problem of uncontrolled temperature rise of reactants in the feeding stage when preparing graphite oxide.

Method used

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  • Preparation method of graphene

Examples

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Embodiment 1

[0029] Embodiment 1, different from Comparative Example 1, this embodiment comprises the following steps:

[0030] Oxidation solution configuration: according to the quality relationship of potassium permanganate: concentrated sulfuric acid (concentration is 98%): sodium nitrate=5:60:1, first add concentrated sulfuric acid (concentration is 98%) and sodium nitrate to the temperature at 6 ℃ Stir in the reactor, then add potassium permanganate to it to obtain the oxidation solution, test and record the temperature T of the oxidation solution 0 .

[0031] Pre-reaction slurry configuration: according to the quality relationship of graphite:potassium permanganate=2:5, slowly add graphite powder to the above-mentioned oxidation solution to obtain the pre-reaction slurry, monitor and record the pre-reactant temperature T during the whole feeding process 1 The change.

[0032] Others are the same as those of Comparative Example 1 and will not be repeated here.

Embodiment 2

[0033] Embodiment 2, different from Embodiment 1, this embodiment includes the following steps:

[0034] Oxidation solution configuration: According to the mass relationship of potassium permanganate:concentrated sulfuric acid (98%):sodium nitrate=5:6:1, first add concentrated sulfuric acid (98%) and sodium nitrate at -10°C Stir in the reactor, then add potassium permanganate to it to obtain the oxidation solution, test and record the temperature T of the oxidation solution 0 .

[0035]Pre-reaction slurry configuration: when the temperature of the oxidation solution is at -10°C, according to the mass relationship of graphite: concentrated sulfuric acid (concentration: 98%) = 0.0005:1, slowly add graphite powder to the above oxidation solution to obtain a pre-reaction slurry , monitor and record the pre-reactant temperature T during the whole feeding process 1 The change.

[0036] Oxidation reaction: place the above-mentioned reactants in an environment of -10°C for 6 hours;...

Embodiment 3

[0039] Embodiment 3, different from Embodiment 1, this embodiment includes the following steps:

[0040] Oxidation solution configuration: according to the mass relationship of potassium permanganate: nitric acid: sodium sulfate = 1:2:1, first add nitric acid and sodium sulfate to a reactor with a temperature of 10°C and stir, then add potassium permanganate to it to obtain Oxidation solution, test and record the temperature T of the oxidation solution 0 .

[0041] Pre-reaction slurry configuration: when the temperature of the oxidation solution is at 10°C, according to the mass relationship of graphite: nitric acid = 2:1, slowly add graphite powder to the above oxidation solution to obtain a pre-reaction slurry, monitor and record the entire feeding process , pre-reactant temperature T 1 The change.

[0042] Oxidation reaction: place the above reactants in an environment of 10°C for 3 hours; then place them in an environment of 85°C for 30 minutes to complete the oxidation...

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Abstract

The invention belongs to the technical field of preparation of graphene and in particular relates to a preparation method of graphene. The preparation method of graphene comprises the following steps: firstly mixing oxidants uniformly in a process of preparing graphite oxide, then adding graphite powder, effectively separating the mixing heat from the reaction heat and enabling the temperature of the whole feeding stage to be controllable. Compared with the prior art, the graphene prepared through the method is relatively high in specific surface area and obviously high in batch stability.

Description

technical field [0001] The invention belongs to the technical field of graphene, in particular to a preparation method of graphene. Background technique [0002] In 2004, Andre K. Geim of the University of Manchester in the United Kingdom prepared graphene for the first time by mechanical exfoliation, which opened the prelude to the preparation and application of this material. The so-called graphene refers to a sheet-like body in which carbon atoms are arranged in a hexagonal ring, usually consisting of a single layer or multiple layers of graphite sheets, which can be infinitely extended in a two-dimensional space. Structural materials. It has outstanding advantages such as large specific surface area, excellent electrical and thermal conductivity, and low thermal expansion coefficient: specifically, high specific surface area (theoretical calculation value: 2630m 2 / g); high conductivity, carrier transport rate (200000cm 2 / V·s); high thermal conductivity (5000W / mK); h...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 杨玉洁
Owner GUANGDONG ZHUGUANG NEW ENERGY TECH
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