CN108689402A - A kind of method that solvent graft process prepares microdilatancy graphite - Google Patents
A kind of method that solvent graft process prepares microdilatancy graphite Download PDFInfo
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- CN108689402A CN108689402A CN201810571766.3A CN201810571766A CN108689402A CN 108689402 A CN108689402 A CN 108689402A CN 201810571766 A CN201810571766 A CN 201810571766A CN 108689402 A CN108689402 A CN 108689402A
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- graphite
- microdilatancy
- intercalator
- methods
- solid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
Abstract
The invention discloses the present invention provides a kind of method that solvent graft process prepares microdilatancy graphite, include the following steps:Graphite powder is mixed with intercalator, is ultrasonically treated, obtains suspension;Suspension is separated by solid-liquid separation, solid heat treatment obtains microdilatancy graphite.The graphite material prepared by the method for the present invention has the advantages that purity is high, interlamellar spacing is controllable, defect is few, simple for process, of low cost.
Description
Technical field
The present invention relates to the sides that graphite material technical field more particularly to a kind of solvent graft process prepare microdilatancy graphite
Method.
Background technology
With the development of New-energy electric vehicle, power lithium-ion battery is in the recent and following quite a long time
Huge development prospect and market value are suffered from, and electrode material is always the important component for influencing battery performance, directly
Connect the main performance index for determining this lithium battery.Negative material is one of the key factor for determining lithium ion battery, at present business
The ion cathode material lithium of change is mainly graphite-like carbon material, is divided into natural graphite and artificial graphite, and natural graphite is because of it
It is formed under conditions of natural high-temperature high pressure, perfectly close to the structure of ideal graphite crystal, is made it have close to graphite pole
High power capacity, workability, high-pressure solid and the feature at low cost of limit.However, its fine and close interlamellar spacing structure causes it not have
The ability of quick removal lithium embedded, in the case of conventional low range charging, lithium ion can be embedded between graphite linings, but in fast charge or low
Under the conditions of temperature, because interlamellar spacing is less than normal to lead to lithium diffusion energy force difference, it cannot quickly be embedded in lithium ion, it is most likely that negative in graphite
Pole surface forms dendrite lithium, punctures diaphragm, and short circuit occurs, and generates safety problem.
Microdilatancy graphite is as a kind of graphite material handling high interlamellar spacing obtained using intercalated technique, by graphite
The entrance and abjection of insert between lamella, so that the interlamellar spacing of graphite material increases, in the base for not destroying layer structure
On plinth, superior material property has been obtained.It is existing prepare microdilatancy graphite method in have chemical method, as chemical oxidization method,
Electrochemical oxidation process etc., using strong oxidizer, such as the concentrated sulfuric acid, nitric acid, perchloric acid are as intercalator, anti-under high temperature or electric field
It answers so that the insertion and abjection of strong oxidizer molecule, this method are inserted not exclusively there is de-, there is a certain amount of oxidant element
Residual, performance and environmental protection to material have certain harm.In addition, also there is high-energy plavini, such as gas phase diffusion melts
Salt method, laser method, explosion method, these methods generally require expensive equipment, complicated working environment and higher danger, no
Easily prepared microdilatancy graphite.
Invention content
Based on background technology there are the problem of, the present invention proposes the side that a kind of solvent graft process prepares microdilatancy graphite
Method, the graphite material prepared by this method is high with purity, interlamellar spacing is controllable, defect is few, simple for process, low-cost excellent
Point.
The present invention proposes a kind of method that solvent graft process prepares microdilatancy graphite, includes the following steps:
S1, graphite powder is mixed with intercalator, is ultrasonically treated, obtains suspension;
S2, suspension is separated by solid-liquid separation, solid heat treatment obtains microdilatancy graphite.
Preferably, in S1, the graphite powder is at least one in natural graphite, spherical graphite, graphite oxide, artificial graphite
Kind.
Preferably, in S1, the intercalator is N-Methyl pyrrolidone, n,N-Dimethylformamide, tetrahydrofuran, diformazan
The solution of at least one of sulfoxide.
Preferably, in S1, the intercalator is N-Methyl pyrrolidone, n,N-Dimethylformamide, tetrahydrofuran, diformazan
At least one of sulfoxide and the solution for having dissolved alkali metal or alkali ion.
Preferably, in S1, a concentration of 1-40mg/ml of the intercalator.
Preferably, in S1, the frequency of supersound process is 40-90KHz, and the time of supersound process is 0.5-6h.If at ultrasound
The frequency of reason is excessively high to cause graphite flake layer directly to be removed with the overlong time being ultrasonically treated.
Preferably, in S2, the mode of separation of solid and liquid is one kind in filtering, centrifugation.
Preferably, in S2, the concrete operations of heat treatment are:It is heated to 90-180 DEG C, isothermal holding 1-12h.
The present invention can be special at ambient temperature, using small solvent molecule or metal ion, under conditions of ultrasonic wave assists
Determine solvent molecule and slowly enter graphite linings gap, as solvent molecule infiltrates graphite flake layer, interlamellar spacing is gradually extended, then leads to
Heating removal interlayer solvent molecule or ion are crossed, the controllable microdilatancy graphite of interlamellar spacing is obtained.The present invention is poor by controlled concentration
Regulate and control the size of interlamellar spacing with propagation energy, and simple for process, of low cost, is had by graphite material prepared by the method for the present invention
Have the advantages that purity is high, interlamellar spacing is controllable, defect is few.
Description of the drawings
Fig. 1 is X-ray diffraction (XRD) figure of microdilatancy graphite and untreated graphite prepared by the present invention;
Fig. 2 is the crystallite dimension and interlamellar spacing variation relation figure of microdilatancy graphite and untreated graphite prepared by the present invention.
Specific implementation mode
Technical solution of the present invention is described in detail with reference to specific embodiment.
Embodiment 1
A kind of method that solvent graft process prepares microdilatancy graphite, includes the following steps:
S1, graphite powder is mixed with intercalator, is ultrasonically treated, obtains suspension;
S2, suspension is separated by solid-liquid separation, solid heat treatment obtains microdilatancy graphite.
Embodiment 2
A kind of method that solvent graft process prepares microdilatancy graphite, includes the following steps:By 1000mg natural flake graphites
Powder is added in the N-Methyl pyrrolidone solution of a concentration of 20mg/ml of 100ml, after simple agitation, with the frequency ultrasound of 80KHz
1h, filtering are handled, solid is put into beaker, is heated to 90 DEG C in baking oven, isothermal holding 12h, you can obtain microdilatancy
Graphite.
Embodiment 3
A kind of method that solvent graft process prepares microdilatancy graphite, becomes 4h, remaining step and reality by sonication treatment time
It is identical to apply example 2, prepares microdilatancy graphite.
Embodiment 4
A kind of method that solvent graft process prepares microdilatancy graphite, includes the following steps:100mg spherical graphite powders are added
Into the tetrahydrofuran solution dissolved with lithium metal of a concentration of 40mg/ml of 100ml, after simple agitation, with the frequency ultrasound of 40KHz
6h is handled, is centrifuged, solid is put into beaker, is heated to 90 DEG C in baking oven, isothermal holding 12h, you can obtain micro-
Expanded graphite.
Embodiment 5
A kind of method that solvent graft process prepares microdilatancy graphite, includes the following steps:4000mg graphite oxide powder is added
Enter into the n,N-Dimethylformamide solution for having dissolved alkali ion of a concentration of 1mg/ml of 100ml, after simple agitation, with
The frequency ultrasound of 90KHz handles 0.5h, centrifuges, and solid is put into beaker, is heated to 180 DEG C in baking oven, heat preservation
Handle 1h, you can obtain microdilatancy graphite.
Embodiment 6
A kind of method that solvent graft process prepares microdilatancy graphite, includes the following steps:3000mg graphous graphite powders are added
Enter into the tetrahydrofuran and dimethyl sulfoxide mixed solution of a concentration of 10mg/ml of 100ml, after simple agitation, with the frequency of 65KHz
It is ultrasonically treated 3h, filtering, solid is put into beaker, is heated to 135 DEG C in baking oven, isothermal holding 6h, you can obtain micro-
Expanded graphite.
Experimental example 1
Microdilatancy graphite and untreated graphite made from embodiment 2 and embodiment 3 are denoted as experimental group 2, experiment successively
Group 3 and contrast groups 1.X-ray diffraction (XRD) is carried out to experimental group 2, experimental group 3 and contrast groups 1 to analyze, the results are shown in Figure 1,
It will be seen from figure 1 that the diffraction spectrogram of microdilatancy graphite exists with untreated graphite in contrast groups 1 in all experimental groups 2 and 3
(002) crystallographic plane diffraction peak is all relatively more sharp, this shows that microdilatancy graphite prepared by the present invention has more complete lamella crystal knot
Structure, intercalation do not cause apparent destruction to graphite laminate structure.
The crystallite dimension and interlamellar spacing of graphite, crystallite dimension and interlayer in test experience group 2, experimental group 3 and contrast groups 1
Away from variation as shown in Fig. 2, figure it is seen that the size of the interlamellar spacing of microdilatancy graphite can be regulated and controled under the conditions of the present invention,
Crystallite dimension La and Lc variation is little, illustrates that microdilatancy graphite is smaller to the extent of the destruction of graphite particle, keeps as far as possible
Its original pattern.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of method that solvent graft process prepares microdilatancy graphite, which is characterized in that include the following steps:
S1, graphite powder is mixed with intercalator, is ultrasonically treated, obtains suspension;
S2, suspension is separated by solid-liquid separation, solid heat treatment obtains microdilatancy graphite.
2. according to the method described in claim 1, it is characterized in that, in S1, the graphite powder be natural graphite, spherical graphite,
At least one of graphite oxide, artificial graphite.
3. method according to claim 1 or 2, which is characterized in that in S1, the intercalator be N-Methyl pyrrolidone,
The solution of at least one of N,N-dimethylformamide, tetrahydrofuran, dimethyl sulfoxide.
4. according to claim 1-3 any one of them methods, which is characterized in that in S1, the intercalator is N- methylpyrroles
At least one of alkanone, N,N-dimethylformamide, tetrahydrofuran, dimethyl sulfoxide and the molten of alkali metal or alkali ion is dissolved
Liquid.
5. according to claim 1-4 any one of them methods, which is characterized in that in S1, a concentration of 1- of the intercalator
40mg/ml。
6. according to claim 1-5 any one of them methods, which is characterized in that in S1, the frequency of supersound process is 40-
The time of 90KHz, supersound process are 0.5-6h.
7. according to claim 1-6 any one of them methods, which is characterized in that in S2, the mode of separation of solid and liquid be filtering, from
One kind in heart separation.
8. according to claim 1-7 any one of them methods, which is characterized in that in S2, the concrete operations of heat treatment are:Add
Heat arrives 90-180 DEG C, isothermal holding 1-12h.
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| CN201810571766.3A CN108689402A (en) | 2018-06-01 | 2018-06-01 | A kind of method that solvent graft process prepares microdilatancy graphite |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114408916A (en) * | 2021-12-16 | 2022-04-29 | 广东邦普循环科技有限公司 | Expanded graphite and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102769139A (en) * | 2012-08-10 | 2012-11-07 | 深圳市斯诺实业发展有限公司永丰县分公司 | Preparation method of high power capacity lithium ion battery cathode material |
| CN103723708A (en) * | 2013-11-22 | 2014-04-16 | 盐城纳新天地新材料科技有限公司 | Preparation method of organic single-layer graphene solution |
| KR20140112826A (en) * | 2013-03-14 | 2014-09-24 | 국립대학법인 울산과학기술대학교 산학협력단 | Expanded Graphite or Graphene Fabricated by Physical Process And Method for Fabricating the same |
-
2018
- 2018-06-01 CN CN201810571766.3A patent/CN108689402A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102769139A (en) * | 2012-08-10 | 2012-11-07 | 深圳市斯诺实业发展有限公司永丰县分公司 | Preparation method of high power capacity lithium ion battery cathode material |
| KR20140112826A (en) * | 2013-03-14 | 2014-09-24 | 국립대학법인 울산과학기술대학교 산학협력단 | Expanded Graphite or Graphene Fabricated by Physical Process And Method for Fabricating the same |
| CN103723708A (en) * | 2013-11-22 | 2014-04-16 | 盐城纳新天地新材料科技有限公司 | Preparation method of organic single-layer graphene solution |
Non-Patent Citations (1)
| Title |
|---|
| 李学文: "《中国袖珍百科全书》", 30 September 2001, 长城出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114408916A (en) * | 2021-12-16 | 2022-04-29 | 广东邦普循环科技有限公司 | Expanded graphite and preparation method thereof |
| CN114408916B (en) * | 2021-12-16 | 2023-07-07 | 广东邦普循环科技有限公司 | Expanded graphite and preparation method thereof |
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