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A kind of preparation method of graphene composite petroleum coke-based activated carbon and super capacitor

A graphene composite, activated carbon technology, applied in hybrid capacitor electrodes, chemical instruments and methods, carbon compounds, etc., can solve the problems of unstable specific surface area, poor reproducibility, and poor graphene dispersion.

Active Publication Date: 2022-07-05
SHANDONG OBO NEW MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the performance of activated carbon prepared by the method used is still very insufficient, which is manifested in: the prepared activated carbon is mainly composed of micropores, and the pore size distribution is unreasonable; the proportion of alkali used in the preparation process is relatively high; the performance of the prepared activated carbon is still not satisfactory. Requirements for capacity; the internal resistance of the prepared activated carbon is relatively large, etc.
And there are also some technologies that use graphene modified activated carbon, but the selectivity of activated carbon sources is not strong, and there is a lack of targeted research, and the common composite paths are as follows: 1. Physical mixing of graphene and activated carbon; 2. Graphene Or blending of graphene oxide and activated carbon precursors, and then co-activation
Although some activated carbons with high specific area can be obtained, the specific surface area is not stable, the reproducibility is poor, and the dispersion of graphene is not good, resulting in unsatisfactory electrical conductivity, which makes it difficult to realize industrial production and meet application requirements.

Method used

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  • A kind of preparation method of graphene composite petroleum coke-based activated carbon and super capacitor

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preparation example Construction

[0045] The invention provides a preparation method of graphene composite petroleum coke-based activated carbon, comprising the following steps:

[0046] A) after the petroleum coke particles are coked under the condition of the first gas, obtain pre-carbonized petroleum coke;

[0047] B) after the pre-carbonized petroleum coke obtained in the above steps is mixed with the activator, activate under the condition of the third gas, and then obtain the activated carbon dispersion after washing;

[0048] C) after the activated carbon dispersion liquid, graphene oxide solution and reducing agent obtained in the above steps are mixed and chemically reduced, a semi-finished product is obtained;

[0049] D) drying the semi-finished product obtained in the above-mentioned steps after etching with hydrogen peroxide, and then performing heat treatment under the condition of protective gas to obtain graphene composite petroleum coke-based activated carbon.

[0050] In the present inventio...

Embodiment 2

[0105] Take 100 g of needle-shaped petroleum coke and pulverize it into particles of 8-12 microns, treat at 500° C. for 1 hour in a nitrogen atmosphere, and cool naturally to obtain pre-carbonized petroleum coke.

[0106] Add 250g of powdered KOH and mix them uniformly, add this mixture into a metal nickel crucible, and heat it up to 450°C at a rate of 10-20°C / min under a nitrogen atmosphere and keep it for 3h; then heat it up to a rate of 10-20°C / min Activated at 750 °C for 1 h, and then cooled to room temperature naturally. The product was dissolved in water, washed repeatedly until neutral, then added 6M hydrochloric acid to reflux for 2 h, filtered, and washed with deionized water until neutral. Deionized water was added to prepare a 0.1 g / ml water dispersion to obtain an activated carbon dispersion.

[0107] A monolayer graphene oxide solution with a solid content of 0.2 g was added to the dispersion, ultrasonically stirred for 1 h, then adjusted to pH 10.5 with ammonia wa...

Embodiment 3

[0116] Take 100 g of needle-shaped petroleum coke and pulverize it into particles of 10-15 microns, and treat at 400° C. for 2 hours in an argon atmosphere to obtain pre-carbonized petroleum coke.

[0117] Add 400g of powdered KOH and mix them uniformly. Add this mixture to a metal nickel crucible, and in a nitrogen atmosphere, the temperature is raised to 500°C at a rate of 10-20°C / min and maintained for 2 hours; then the temperature is raised to a rate of 10-20°C / min Activated at 850 °C for 1 h, and then cooled to room temperature naturally. The product was dissolved in water, washed repeatedly until neutral, then added 6M hydrochloric acid to reflux for 2 h, filtered, and washed with deionized water until neutral. Deionized water was added to prepare a 0.05 g / ml water dispersion to obtain an activated carbon dispersion.

[0118] A single-layer graphene oxide solution with a solid content of 0.3 g was added to the dispersion, ultrasonically stirred for 1 h, then adjusted to...

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Abstract

The invention provides a preparation method of graphene composite petroleum coke-based activated carbon. First, the petroleum coke particles are coked under the condition of a first gas to obtain pre-carbonized petroleum coke; and then the pre-carbonized petroleum coke is mixed with an activator. , activate under the condition of the third gas, and then wash to obtain activated carbon dispersion; then mix the activated carbon dispersion, graphene oxide solution and reducing agent for chemical reduction to obtain a semi-finished product; finally, the semi-finished product is etched by an etchant After post-drying, and then heat treatment under protective gas conditions, the graphene composite petroleum coke-based activated carbon is obtained. In the present invention, hydrogen peroxide is used for etching treatment, so that the graphene is further formed with pores, the ion migration channel is improved, and the specific surface area of ​​the graphene modified activated carbon is further improved and stabilized. In the subsequent high-temperature reduction process, the graphene The structure is restored and the electrical conductivity of the activated carbon is improved, thereby increasing the specific capacity of the supercapacitive carbon.

Description

technical field [0001] The invention belongs to the technical field of activated carbon materials, and relates to a preparation method of modified petroleum coke-based activated carbon and a supercapacitor, in particular to a preparation method of graphene composite petroleum coke-based activated carbon and a supercapacitor. Background technique [0002] Supercapacitors are a new type of energy storage device that can provide powerful pulsed power. Due to the energy storage principle of physical charge adsorption, supercapacitors have good high-power charge-discharge performance. During charging, the electrode surface charge in a polarized state attracts anisotropic ions in the electrolyte solution, so that these ions attach to the electrode surface to form an electric double layer. capacitance, thereby generating a stable potential difference between the positive and negative electrodes. Supercapacitors have the characteristics of fast charging and discharging speed, high ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/318C01B32/372H01G11/24H01G11/34H01G11/36
CPCH01G11/24H01G11/34H01G11/36Y02E60/13
Inventor 赵永彬张在忠姜彤彤程金杰
Owner SHANDONG OBO NEW MATERIAL CO LTD