CN107381565A - A kind of purification treating method of micro crystal graphite - Google Patents

A kind of purification treating method of micro crystal graphite Download PDF

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Publication number
CN107381565A
CN107381565A CN201610322801.9A CN201610322801A CN107381565A CN 107381565 A CN107381565 A CN 107381565A CN 201610322801 A CN201610322801 A CN 201610322801A CN 107381565 A CN107381565 A CN 107381565A
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CN
China
Prior art keywords
graphite
micro crystal
concentration
acid
crystal graphite
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CN201610322801.9A
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Chinese (zh)
Inventor
林前锋
李丽萍
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Hunan Guosheng Graphite Technology Co Ltd
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Hunan Guosheng Graphite Technology Co Ltd
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Priority to CN201610322801.9A priority Critical patent/CN107381565A/en
Publication of CN107381565A publication Critical patent/CN107381565A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/20Graphene characterized by its properties
    • C01B2204/30Purity

Abstract

The invention discloses a kind of purification treating method of micro crystal graphite, selection particle diameter is the natural micro crystal graphite of 150 250 purposes as raw material, the sulfuric acid that hydrochloric acid that the hydrofluoric acid for being 35% with concentration, concentration are 40%, concentration are 98% mixes 10 15min, 2h is reacted at room temperature afterwards, after reaction terminates, when by graphite washing pH value being 5.5 7, under vacuo, graphite oxide is radiated using microwave, impure graphene is heated cleavage, obtains the higher graphene of purity.The purification treating method of micro crystal graphite provided by the invention, method is simple, can significantly reduce the impurity content in graphite.

Description

A kind of purification treating method of micro crystal graphite
Technical field
The present invention relates to micro crystal graphite technical field, is to be related to a kind of purification process side of micro crystal graphite more specifically Method.
Background technology
Natural micro crystal graphite is also known as aphanitic graphite, amorphous graphite or amorphous graphite, by many small in structure Graphite crystal is formed, and degree of graphitization is higher, but mineral impurity content is high, as negative electrode of lithium ion battery Material has good cycle performance, but the shortcomings such as coulombic efficiency is low, reversible capacity is low first be present.
The content of the invention
In view of this, it is an object of the invention to propose a kind of purification treating method of micro crystal graphite.
To achieve these goals, technical scheme is as follows:
A kind of purification treating method of micro crystal graphite, comprises the following steps:
(1) choose particle diameter be the natural micro crystal graphite of 150-250 purposes be used as raw material, with concentration for 35% hydrogen fluorine Acid, concentration be 40% hydrochloric acid, concentration be 98% sulfuric acid mix 10-15min, afterwards at room temperature React 2h,
(2) reaction terminate after, by graphite washing pH value be 5.5-7 when, under vacuo, using microwave to oxygen Graphite is radiated, and impure graphene is heated cleavage, obtains the higher graphene of purity.
Further, the graphite, hydrofluoric acid, hydrochloric acid, the volume ratio of sulfuric acid are 6: 3: 2: 2, the hydrofluoric acid Density be 1.45, the density of the sulfuric acid is 1.67, and the density of the hydrochloric acid is 2.00.
Compared with prior art, beneficial effects of the present invention are as follows:At the purifying of micro crystal graphite proposed by the present invention Reason method, method is simple, can significantly reduce the impurity content in graphite.
Embodiment
With reference to specific embodiment, the invention will be further described, to more fully understand the present invention.
Embodiment 1
A kind of purification treating method of micro crystal graphite, step are as follows:
(1) choose particle diameter be the natural micro crystal graphite of 150 purposes be used as raw material, with concentration for 35% hydrofluoric acid, The sulfuric acid that hydrochloric acid that concentration is 40%, concentration are 98% mixes 10min, reacts 2h at room temperature afterwards,
(2) reaction terminate after, by graphite washing pH value be 7 when, under vacuo, using microwave to aoxidize stone Ink is radiated, and impure graphene is heated cleavage, obtains the higher graphene of purity.
It is 6: 3: 2: 2 by the volume ratio of graphite, hydrofluoric acid, hydrochloric acid, sulfuric acid, the density of hydrofluoric acid is 1.45, The density of sulfuric acid is 1.67, and the density of hydrochloric acid is 2.00.
Embodiment 2
A kind of purification treating method of micro crystal graphite, step are as follows:
(1) choose particle diameter be the natural micro crystal graphite of 200 purposes be used as raw material, with concentration for 35% hydrofluoric acid, The sulfuric acid that hydrochloric acid that concentration is 40%, concentration are 98% mixes 10min, reacts 2h at room temperature afterwards,
(2) reaction terminate after, by graphite washing pH value be 7 when, under vacuo, using microwave to aoxidize stone Ink is radiated, and impure graphene is heated cleavage, obtains the higher graphene of purity.
It is 6: 3: 2: 2 by the volume ratio of graphite, hydrofluoric acid, hydrochloric acid, sulfuric acid, the density of hydrofluoric acid is 1.45, The density of sulfuric acid is 1.67, and the density of hydrochloric acid is 2.00.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, all essences in the present invention Within god and principle, any modification for being made, equivalent substitution etc., should be included in protection scope of the present invention it It is interior.

Claims (2)

1. a kind of purification treating method of micro crystal graphite, it is characterised in that comprise the following steps:
(1) choose particle diameter be the natural micro crystal graphite of 150-250 purposes be used as raw material, with concentration for 35% hydrofluoric acid, The sulfuric acid that hydrochloric acid that concentration is 40%, concentration are 98% mixes 10-15min, reacts 2h at room temperature afterwards,
(2) reaction terminate after, by graphite washing pH value be 5.5-7 when, under vacuo, using microwave to aoxidize Graphite is radiated, and impure graphene is heated cleavage, obtains the higher graphene of purity.
2. the purification treating method of micro crystal graphite according to claim 1, it is characterised in that the stone Ink, hydrofluoric acid, hydrochloric acid, the volume ratio of sulfuric acid are 6: 3: 2: 2, and the density of the hydrofluoric acid is 1.45, the sulphur The density of acid is 1.67, and the density of the hydrochloric acid is 2.00.
CN201610322801.9A 2016-05-17 2016-05-17 A kind of purification treating method of micro crystal graphite Pending CN107381565A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610322801.9A CN107381565A (en) 2016-05-17 2016-05-17 A kind of purification treating method of micro crystal graphite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610322801.9A CN107381565A (en) 2016-05-17 2016-05-17 A kind of purification treating method of micro crystal graphite

Publications (1)

Publication Number Publication Date
CN107381565A true CN107381565A (en) 2017-11-24

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CN201610322801.9A Pending CN107381565A (en) 2016-05-17 2016-05-17 A kind of purification treating method of micro crystal graphite

Country Status (1)

Country Link
CN (1) CN107381565A (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101948107A (en) * 2010-09-15 2011-01-19 天津大学 Method for preparing and purifying graphene by microwave radiation under vacuum
CN102107870A (en) * 2011-03-23 2011-06-29 中国科学院山西煤炭化学研究所 Method for quickly preparing reduced graphene by using microwaves
CN102502611A (en) * 2011-11-15 2012-06-20 东南大学 Method for rapidly preparing graphene in large quantities by utilizing graphite oxides
CN104591143A (en) * 2013-10-30 2015-05-06 青岛泰浩达碳材料有限公司 Purifying processing method for microcrystalline graphite

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101948107A (en) * 2010-09-15 2011-01-19 天津大学 Method for preparing and purifying graphene by microwave radiation under vacuum
CN102107870A (en) * 2011-03-23 2011-06-29 中国科学院山西煤炭化学研究所 Method for quickly preparing reduced graphene by using microwaves
CN102502611A (en) * 2011-11-15 2012-06-20 东南大学 Method for rapidly preparing graphene in large quantities by utilizing graphite oxides
CN104591143A (en) * 2013-10-30 2015-05-06 青岛泰浩达碳材料有限公司 Purifying processing method for microcrystalline graphite

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Application publication date: 20171124