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Method for preparing high-intrinsic-degree graphene by electrolysis

A graphene and electrolyte technology, applied in the field of electrolytic preparation of high intrinsic degree graphene, achieves the effects of low cost, easy availability of raw materials, and convenience for industrialization

Inactive Publication Date: 2019-10-25
SINOSTEEL NANJING NEW MATERIALS RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there is no report on the method of preparing graphene with high intrinsic degree by using ammonia water to regulate the pH value of the sulfate solution to alkaline conditions in the electrolysis process.

Method used

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  • Method for preparing high-intrinsic-degree graphene by electrolysis
  • Method for preparing high-intrinsic-degree graphene by electrolysis
  • Method for preparing high-intrinsic-degree graphene by electrolysis

Examples

Experimental program
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Effect test

Embodiment 1

[0045] A kind of preparation method of high intrinsic degree graphene is characterized in that, the method comprises the following steps:

[0046] (1) Preparation of reactants: graphite foil is pressed into graphite flakes, and the thickness of the pressed sheet is 3mm, as the positive electrode reactant A during electrolysis; the platinum electrode is selected as the negative electrode of electrolysis; ammonium sulfate is selected to be made into 1mol / L Ammonium sulfate solution B; in B solution according to 2% volume ratio, promptly every 100mL B solution adds the ammoniacal liquor of the 30% mass fraction of 2mL to control the pH value of B solution to be 9, and mixed solution uniform velocity stirs 15 minutes, and in Ultrasonic at room temperature (25°C) with a power of 50W for 5 minutes to obtain alkaline electrolyte solution C;

[0047] (2) Reaction stripping: place the electrolyte device in a constant temperature environment at 0°C; use reactant A as the positive electr...

Embodiment 2

[0052] The preparation method of high graphene oxide is mainly characterized in that it is different from step (2) in embodiment 1, step (2) in this embodiment does not add ammoniacal liquor to adjust the pH of the solution, and the specific method comprises the following steps:

[0053] (1) Preparation of reactants: graphite foil is pressed into graphite flakes, and the thickness of the pressed sheet is 3mm, as the positive electrode reactant A during electrolysis; the platinum electrode is selected as the negative electrode of electrolysis; ammonium sulfate is selected to be made into 1mol / L Ammonium sulfate solution B;

[0054] (2) Reaction stripping: place the electrolyte device in a constant temperature environment at 0°C; use reactant A as the positive electrode, platinum electrode as the negative electrode, and solution B as the electrolyte, and maintain it stably for 2 hours under a DC voltage of 3V; then increase the voltage and Keep it stable at 10V, and continue to ...

Embodiment 3

[0058] A kind of preparation method of high intrinsic degree graphene is characterized in that, the method comprises the following steps:

[0059] (1) Preparation of reactants: Scale graphite is pressed into graphite flakes, and the thickness of the pressed sheets is 4mm, as the positive electrode reactant A during electrolysis; the platinum electrode is selected as the negative electrode of electrolysis; ammonium bisulfate is selected as the electrolyte, and it is made into 0.6mol / L ammonium bisulfate solution B; according to the volume ratio of 3% in the B solution, that is, every 100mL of the B solution is added with 3mL of 30% mass fraction of ammonia water, the pH value of the B solution is adjusted to be 10, and the mixed solution is uniformly Stir for 15 minutes, and sonicate for 5 minutes at room temperature (25°C) at a power of 40W to obtain alkaline electrolyte solution C;

[0060] (2) Reaction stripping: place the electrolyte device in a constant temperature environ...

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Abstract

The invention belongs to the technical field of inorganic material preparation, and particularly relates to a preparation method of high-intrinsic-degree grapheme. The preparation method comprises thefollowing steps that a graphite material is prepared into a positive electrode; sulfate is prepared into an electrolyte, firstly the electrode is pretreated under the condition of an applied voltage,then the pH of a solution is adjusted to be alkaline by adding ammonia water, and electrolytic stripping of the graphite positive electrode is performed at a certain temperature; and an electrolyzedproduct is subjected to solid-liquid separation and drying to obtain the high-intrinsic-degree grapheme. Lower oxidation activity of a solvent to the graphite material can be ensured by controlling the pH value of the electrolyte, the reduction of the oxidation degree of the product grapheme is facilitated, and the improvement of the quality of the grapheme is further facilitated. The grapheme isprepared form conventional chemical raw materials, the raw materials are low in cost and easy to obtain, and industrialization is convenient.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic materials, in particular to a method for electrolytically preparing graphene with high intrinsic degree. Background technique [0002] The large-scale preparation of graphene with high intrinsic degree at low cost is a key technical problem that must be solved to give full play to the excellent electrical and thermal conductivity of graphene and promote the application of graphene in the fields of electrothermal, sensing and energy storage. The most important technical route to prepare graphene with high intrinsic degree is to use cheap graphite as raw material through intercalation and exfoliation of graphite layers. For this technical route, a high intrinsic degree is the prerequisite for its application in all aspects, and at the same time, the environmental protection and safety of the preparation system and process should also be taken into account. However, it is still a ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19
CPCC01B2204/04C01B2204/30C01B2204/32C01B32/19
Inventor 陈杰骆艳华裴晓东
Owner SINOSTEEL NANJING NEW MATERIALS RES INST CO LTD
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