Method for preparing high-carbon graphite by using middle-carbon crystalline flake graphite as raw material

A medium-carbon flake and graphite technology, applied in the field of high-carbon graphite preparation, can solve problems such as high production costs, and achieve the effects of improving utilization, reducing corrosion, and lowering reaction temperature

Active Publication Date: 2015-08-19
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the current alkaline-acid method still has the problem of high production cost due to high energy consumption and high requirements of the process on production equipment.

Method used

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  • Method for preparing high-carbon graphite by using middle-carbon crystalline flake graphite as raw material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Material preparation: medium carbon flake graphite: the fixed carbon content is 95wt.%, and the particle size is 100 orders; Sodium hydroxide: the solid form is powder; Hydrochloric acid: the mass concentration is 4%, and the mass ratio of the three is 3 :10:170.

[0023] (2) After mixing and stirring the medium carbon flake graphite and sodium hydroxide, place it in a powder tablet press, press it into a block under a pressure of 20MPa, and maintain the pressure for 9min to obtain a density of 1.9g / cm 3 graphite prefabricated blocks.

[0024] (3) Embed the prefabricated graphite block in powdery medium carbon flake graphite, and place it in a box-type resistance furnace, maintain it at 500°C for 3 hours, then dissolve the graphite block that has been taken out and cleaned the surface into water, stir and filter, repeat Wash until the pH of the filtrate = 7.0, and collect the powder for later use.

[0025] (4) Dissolve the graphite powder obtained in step (3) in h...

Embodiment 2

[0028] (1) Material preparation: medium carbon flake graphite: the fixed carbon content is 95wt.%, and the particle size is 100 orders; Sodium hydroxide: the solid form is powder; Hydrochloric acid: the mass concentration is 9%, and the mass ratio of the three is 2 :10:60.

[0029] (2) After mixing and stirring the medium carbon flake graphite and sodium hydroxide, place it in a powder tablet press, press it into a block under a pressure of 30MPa, and maintain the pressure for 10min to obtain a density of 2.0g / cm 3 graphite prefabricated blocks.

[0030] (3) Embed the prefabricated graphite block in powdery medium carbon flake graphite, and place it in a box-type resistance furnace, maintain it at 450°C for 3 hours, then dissolve the graphite block that has been taken out and cleaned the surface into water, stir and filter, repeat Wash until the pH of the filtrate = 7.0, and collect the powder for later use.

[0031] (4) Dissolve the graphite powder obtained in step (3) in h...

Embodiment 3

[0034] (1) Material preparation: medium carbon flake graphite: the fixed carbon content is 88wt.%, and the particle size is 32 orders; Sodium hydroxide: solid form is powder; Hydrochloric acid: mass concentration is 15%, and the mass ratio of the three is 2 :10:60.

[0035] (2) After mixing and stirring the medium carbon flake graphite and sodium hydroxide, place it in a powder tablet press, press it into a block under a pressure of 30MPa, and maintain the pressure for 10min to obtain a density of 2.0g / cm 3 graphite prefabricated blocks.

[0036] (3) Embed the prefabricated graphite block in powdery medium carbon flake graphite, and place it in a box-type resistance furnace, maintain it at 450°C for 3 hours, then dissolve the graphite block that has been taken out and cleaned the surface into water, stir and filter, repeat Wash until the pH of the filtrate = 7.0, and collect the powder for later use.

[0037] (4) Dissolve the graphite powder obtained in step (3) in hydrochlo...

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Abstract

The invention relates to the technical field of graphite purification, in particular to a method for preparing high-carbon graphite by using middle-carbon crystalline flake graphite as a raw material. The method disclosed by the invention comprises the steps: the middle-carbon crystalline flake graphite and sodium hydroxide are mixed and are pressed into blocks in a mold, high-temperature calcination is carried out under the condition that the middle-carbon crystalline flake graphite is embedded, washing is carried out, then the obtained graphite powder is subjected to acid leaching and washing in sequence, drying is carried out, thus high-carbon graphite of which the fixed carbon content is more than 99.5 wt.% is obtained. The graphite and the sodium hydroxide are mixed and are pressed into blocks in the mold, thus the contact degree of impurities and sodium hydroxide and the heat conduction efficiency of a system are improved, and material and energy consumption is reduced; a high-purity nitrogen protection method is replaced with the middle-carbon crystalline flake graphite embedded method, the purification quantity is ensured, meanwhile, the corrosion to equipment in the production process is reduced, and thus the production cost is reduced. According to the invention, the reaction speed of impurities and sodium hydroxide is accelerated, the use ratio of sodium hydroxide is improved, the reaction temperature is reduced, the operation is simple and the cost is low.

Description

technical field [0001] The invention relates to the technical field of graphite purification, in particular to a method for preparing high-carbon graphite from medium-carbon flake graphite as a raw material. Background technique [0002] Graphite is a material with extremely high utilization value, which plays a pivotal role in various fields of science and technology. Especially since the discovery of graphene, people's research on it has continued to heat up in recent years. Therefore, the purity of graphite as a raw material for graphene has become a key indicator of its economic and application value, and the purification of graphite has always been a top priority for scientific researchers. [0003] At present, the preparation methods of high-purity graphite generally include alkali-acid method, hydrofluoric acid method, chlorination roasting method, and high-temperature method. Among them, the hydrofluoric acid method and the chlorination roasting method can produce ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 赵增典何志伟季海滨刘然升冯柳王英王志国王永在张丽鹏
Owner SHANDONG UNIV OF TECH
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