CN106099085A - A kind of preparation method of porous polyimide coated graphite material - Google Patents
A kind of preparation method of porous polyimide coated graphite material Download PDFInfo
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- CN106099085A CN106099085A CN201610782585.6A CN201610782585A CN106099085A CN 106099085 A CN106099085 A CN 106099085A CN 201610782585 A CN201610782585 A CN 201610782585A CN 106099085 A CN106099085 A CN 106099085A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses the preparation method of a kind of porous polyimide coated graphite material, porous polyimide is evenly coated at graphite surface by hot imidization reaction by it, graphite surface is effectively prevented to contact with the direct of liquid electrolyte, on the basis of ensureing high rate performance excellence, the generation of side reaction when suppression graphite high temperature circulation and storage, promote high temperature circulation and storage performance, improve the safety that graphite makees the lithium secondary battery of negative pole simultaneously, the final graphite 50 circulations under high temperature (55 DEG C) may be up to 98%, the preparation method of this porous polyimide coated graphite material is simple, workable, it is suitable for being prepared on a large scale.
Description
Technical field
The present invention relates to graphite material preparation field, be specifically related to the preparation of a kind of porous polyimide coated graphite material
Method.
Background technology
Material with carbon element has that chemical potential is low, good cycle, cheap, advantages of environment protection, be the most preferable,
Conventional lithium ion battery negative material.And in material with carbon element, compare with hard carbon with soft carbon, graphite material is in specific capacity, electric discharge
The aspect such as platform and cost has a more significantly advantage, but graphite uses the lithium secondary battery life-span as the power vehicle of negative pole
One of short reason is that in high temperature environments (higher than 50 DEG C) graphite can occur a lot with electrolyte in circulation and storing process
Side reaction, this is degrading the cycle performance of battery, and causes potential safety hazard.Up to now, substantial amounts of research work is mainly concentrated
Promoting on the circulation of graphite cathode and capacity boost, its circulation under high temperature (55 DEG C) and the research of high rate performance
Work the fewest.
Summary of the invention
The present invention is directed to existing technical problem, it is provided that the preparation method of a kind of porous polyimide coated graphite material,
By hot imidization reaction, porous polyimide is evenly coated at graphite surface, effectively prevents graphite surface and liquid electrolyte
The directly contact of liquid, on the basis of ensureing high rate performance excellence, sending out of side reaction when suppression graphite high temperature circulation and storage
Raw, promote high temperature circulation and storage performance, improve the safety that graphite makees the lithium secondary battery of negative pole simultaneously.
For achieving the above object, the present invention provides following technical scheme: a kind of porous polyimide coated graphite material, its
Being characterised by, it comprises the following steps:
(1) solvent of 1 part of diamine compound and 10-18 part is sequentially added in the stirred tank of band atmosphere protection, at noble gas
1-4h, stirring frequency 30-50HZ is stirred so that it is be completely dissolved under protection.Then it is dividedly in some parts 1-2 part dianhydride chemical combination by metering
Thing, continues stirring reaction 4-6 h under inert atmosphere protection, obtains the polyamic acid solution of yellow, viscous；
(2) polyamic acid solution solvent dilution step (1) obtained is the solution of 1-6% to mass concentration, is subsequently adding
The powdered graphite of 100% and 0.1-0.5% foaming agent, uniform stirring 1h.Then mixed liquor is centrifuged, and the powder obtained is existed
In air dry oven, 25 DEG C are dried 0.5-2.0h, then move to 25 DEG C of dry 10-16h in vacuum drying oven, obtain polyamic acid bag
The graphite covered.
(3) graphite of polyamic acid cladding step (2) obtained is positioned in atmosphere furnace, under inert gas shielding,
By 90 DEG C/2h, 180 DEG C/1 h, 220 DEG C/1 h, the imidization program imidization of 280 DEG C/1 h, 320 DEG C/1h, obtain polyamides
The graphite of imines cladding；
Further, preferably, the diamine compound described in step (1) is p-phenylenediamine (p-PDA), four fluoro-benzene two
One or more in amine, cyclohexane diamine (CHDA), Tetramethylene. diamidogen.
Further, preferably, the solvent described in step (1) is N,N-dimethylacetamide (DMAc), N-first
Base ketopyrrolidine (NMP), N,N-dimethylformamide (DMF) one or more.
Further, preferably, the dianhydride compound described in step (1) is free biphenyl tetracarboxylic dianhydride
(BPDA), burnt melitic acid dianhydride (PMDA), pyromellitic dianhydride (PMDA) one or more.
Further, preferably, the noble gas described in step (1) be the one in nitrogen, argon, helium or
Person is multiple.
Further, preferably, the foaming agent described in step (2) is ammonium carbonate, ammonium nilrite, azo two formyl
One or more in amine.
Further, preferably, graphite described in step (2) be the one in Delanium or native graphite or
Person is multiple.
Further, preferably, described graphite purity ＞ 99.99%, granularity D50=16-20um.
Further, preferably, the noble gas described in step (3) be the one in nitrogen, argon, helium or
Person is multiple.
Special instruction, what above-mentioned all numbers referred to is all mass fraction.
Compared with prior art, the invention has the beneficial effects as follows:
(1) present invention uses the method for hot imidization that the polyimide nano protective layer traditional carbon-coating of replacement is coated on graphite table
Face, can effectively suppress the serious side reaction in circulation and storing process of graphite and electrolyte, improve the cyclicity of battery
Can, eliminating potential safety hazard, 50 circulations under high temperature (55 DEG C) of the final graphite may be up to 98%；
(2) present invention uses addition foaming agent to prepare the clad of porous, improves the activity of negative material, thus improves stone
The high rate performance of ink negative material；
(3) preparation method of the graphite cathode material of this polyimides cladding is simple, workable, is suitable for being prepared on a large scale.
Detailed description of the invention
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, all
Belong to the scope of protection of the invention.
Embodiment one
A kind of porous polyimide coated graphite material, it comprises the following steps:
(1) DMAC N,N' dimethyl acetamide (DMAc) of 1 part of p-phenylenediamine (p-PDA) and 12 parts is sequentially added into band atmosphere protection
Stirred tank in, stir 1h, stirring frequency 30HZ under nitrogen protection so that it is be completely dissolved.Then it is dividedly in some parts 1 part by metering
Free biphenyl tetracarboxylic dianhydride (BPDA), continues stirred under nitrogen atmosphere reaction 4h, and the polyamic acid obtaining yellow, viscous is molten
Liquid；
(2) the polyamic acid solution DMAC N,N' dimethyl acetamide (DMAc) that step (1) obtains being diluted to mass concentration is 1%
Solution, be subsequently adding the purity 99.998% of 100%, the Delanium powder of granularity D50=16um and 0.1% ammonium carbonate, uniformly
Stirring 1h.Then mixed liquor is centrifuged, and the powder 25 DEG C of baking 0.5h in air dry oven that will obtain, then move to vacuum and do
25 DEG C of dry 10h in dry case, obtain the graphite of polyamic acid cladding；
(3) step (2) is obtained polyamic acid cladding graphite be positioned in atmosphere furnace, under nitrogen protection, by 90 DEG C/
2h, 180 DEG C/1 h, 220 DEG C/1 h, the imidization program imidization of 280 DEG C/1 h, 320 DEG C/1h, obtain polyimides cladding
Graphite.
Embodiment two
A kind of porous polyimide coated graphite material, it comprises the following steps:
(1) N-Methyl pyrrolidone (NMP) of 1 part of four fluoro-phenylenediamine and 12 parts is sequentially added into the stirred tank of band atmosphere protection
In, under argon shield, stir 2h, stirring frequency 40 HZ so that it is be completely dissolved.Then it is dividedly in some parts 2 parts of burnt melitics by metering
Acid dianhydride (PMDA), continues stirring reaction 5 h under argon shield, obtains the polyamic acid solution of yellow, viscous；
(2) the polyamic acid solution N-Methyl pyrrolidone (NMP) that step (1) obtains is diluted to mass concentration be 2% molten
Liquid, is subsequently adding the purity 99.995% of 100%, the Delanium powder of granularity D50=18um and 0.3% ammonium nilrite, uniformly stirs
Mix 1h.Then mixed liquor is centrifuged, and the powder 25 DEG C of baking 2.0h in air dry oven that will obtain, then move to vacuum and do
25 DEG C of dry 16h in dry case, obtain the graphite of polyamic acid cladding；
(3) step (2) is obtained polyamic acid cladding graphite be positioned in atmosphere furnace, under argon shield, by 90 DEG C/
2h, 180 DEG C/1 h, 220 DEG C/1 h, the imidization program imidization of 280 DEG C/1 h, 320 DEG C/1h, obtain polyimides cladding
Graphite.
Embodiment three
A kind of porous polyimide coated graphite material, it comprises the following steps:
(1) N,N-dimethylformamide (DMF) of 1 part of cyclohexane diamine (CHDA) and 18 parts is sequentially added into band atmosphere protection
Stirred tank in, helium protect under stir 3h, stirring frequency 50HZ so that it is be completely dissolved.Then it is dividedly in some parts 1 part by metering
Pyromellitic dianhydride (PMDA), continues helium protection lower stirring reaction 6 h, obtains the polyamic acid solution of yellow, viscous；
(2) the polyamic acid solution N,N-dimethylformamide (DMF) that step (1) obtains being diluted to mass concentration is 5%
Solution, be subsequently adding 100% 100% purity 99.996%, the natural graphite powder of granularity D50=17um and 0.5% azo diformazan
Amide, uniform stirring 1h.Then mixed liquor is centrifuged, and the powder 25 DEG C of baking 0.9h in air dry oven that will obtain, then
Move to 25 DEG C of dry 12h in vacuum drying oven, obtain the graphite of polyamic acid cladding；
(3) graphite of polyamic acid cladding step (2) obtained is positioned in atmosphere furnace, under helium, by 90 DEG C/2h,
180 DEG C/1 h, 220 DEG C/1 h, the imidization program imidization of 280 DEG C/1 h, 320 DEG C/1h, obtain the stone of polyimides cladding
Ink.
Embodiment four
A kind of porous polyimide coated graphite material, it comprises the following steps:
(1) N,N-dimethylformamide (DMF) of 1 part of Tetramethylene. diamidogen and 14 parts is sequentially added into the stirred tank of band atmosphere protection
In, stir 4h, stirring frequency 40 HZ so that it is be completely dissolved under nitrogen protection.Then it is dividedly in some parts 2 parts of equal benzene four by metering
Formic anhydride (PMDA), continues stirring reaction 5h under inert atmosphere protection, obtains the polyamic acid solution of yellow, viscous；
(2) the polyamic acid solution N,N-dimethylformamide (DMF) that step (1) obtains being diluted to mass concentration is 3%
Solution, is subsequently adding purity 99.996%, the natural graphite powder of granularity D50=16um and 0.4% azodicarbonamide of 100%,
Uniform stirring 1h.Then mixed liquor is centrifuged, and the powder 25 DEG C of baking 1.5h in air dry oven that will obtain, then move to
25 DEG C of dry 14h in vacuum drying oven, obtain the graphite of polyamic acid cladding；
(3) step (2) is obtained polyamic acid cladding graphite be positioned in atmosphere furnace, under nitrogen protection, by 90 DEG C/
2h, 180 DEG C/1 h, 220 DEG C/1 h, the imidization program imidization of 280 DEG C/1 h, 320 DEG C/1h, obtain polyimides cladding
Graphite.
Comparative example one
Use the natural spherical plumbago powder raw material as a comparison case 1 of phosphorus content 99.95%.
Comparative example two
The Delanium powder raw material of comparative example 2 phosphorus content 99.95% as a comparison case 2.
For checking the performance of graphite cathode material, test by half-cell method of testing, with the porous polyimide of the present invention
Coated graphite material: SBR (solid content 50%): CMC:SP=95.5:2.0:1.5:1.0 (weight ratio), add appropriate deionization
Water mixing furnishing pulpous state, coats on Copper Foil and is dried in vacuum drying oven and make negative plate in 12 hours；To electrode metal
Lithium sheet composition half-cell, electrolyte is 1M liPF6/ EC+DEC+DMC=1:1:1, and charge-discharge magnification is 0.2 C/3C, charge and discharge
Piezoelectric voltage scope is 0-1.5V, and the discharge and recharge cabinet computerizedd control carries out collection and the control of data, the results are shown in Table 1
The graphite material that table 1 lists the embodiment of the present invention prepared compares with the performance parameter of comparative example material,
。
As can be seen from the above results: high rate performance and the high temperature of the graphite of the polyimides cladding that the embodiment of the present invention prepares follow
Ring performance substantially increases compared with comparative example, and reason can be attributed to polyimide nano protective layer and replace traditional carbon-coating cladding
At graphite surface, can effectively suppress the serious side reaction in circulation and storing process of graphite and electrolyte, improve battery
Cycle performance, eliminate potential safety hazard, meanwhile, made the clad porous of preparation by foaming agent, negative pole can be effectively improved
The activity of material, thus improve the high rate performance of graphite cathode material.
Special instruction, what above-mentioned all numbers referred to is all mass fraction.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, permissible
Understand and these embodiments can be carried out multiple change without departing from the principles and spirit of the present invention, revise, replace
And modification, the scope of the present invention be defined by the appended.
Claims (9)
1. the preparation method of a porous polyimide coated graphite material, it is characterised in that it comprises the following steps:
(1) solvent of 1 part of diamine compound and 10-18 part is sequentially added in the stirred tank of band atmosphere protection, at noble gas
1-4h, stirring frequency 30-50HZ is stirred so that it is be completely dissolved under protection；
Then it is dividedly in some parts 1-2 part dianhydride compound by metering, continues stirring reaction 4-6 h under inert atmosphere protection, obtain Huang
The polyamic acid solution that color is thick；
(2) polyamic acid solution solvent dilution step (1) obtained is the solution of 1-6% to mass concentration, is subsequently adding
The powdered graphite of 100% and 0.1-0.5% foaming agent, uniform stirring 1h；
Then mixed liquor is centrifuged, and the powder 25 DEG C of baking 0.5-2.0h in air dry oven that will obtain, then move to vacuum
25 DEG C of dry 10-16h in drying baker, obtain the graphite of polyamic acid cladding；
(3) graphite of polyamic acid cladding step (2) obtained is positioned in atmosphere furnace, under inert gas shielding, by 90
DEG C/2h, 180 DEG C/1 h, 220 DEG C/1 h, the imidization program imidization of 280 DEG C/1 h, 320 DEG C/1h, obtain polyimides bag
The graphite covered.
The preparation method of a kind of porous polyimide coated graphite material the most according to claim 1, it is characterised in that: step
Suddenly the diamine compound described in (1) is p-phenylenediamine (p-PDA), four fluoro-phenylenediamines, cyclohexane diamine (CHDA), ring fourth
One or more in alkane diamidogen.
The preparation method of a kind of porous polyimide coated graphite material the most according to claim 1, it is characterised in that: step
Suddenly solvent described in (1) is DMAC N,N' dimethyl acetamide (DMAc), N-Methyl pyrrolidone (NMP), N,N-dimethylformamide
(DMF) one or more.
The preparation method of a kind of porous polyimide coated graphite material the most according to claim 3, it is characterised in that: step
Suddenly dianhydride compound described in (1) is free biphenyl tetracarboxylic dianhydride (BPDA), burnt melitic acid dianhydride (PMDA), equal benzene tetramethyl
One or more of anhydride (PMDA).
The preparation method of a kind of porous polyimide coated graphite material the most according to claim 1, it is characterised in that: step
Suddenly one or more during noble gas is nitrogen, argon, helium described in (1).
The preparation method of a kind of porous polyimide coated graphite material the most according to claim 1, it is characterised in that: step
Suddenly one or more during the foaming agent described in (2) is ammonium carbonate, ammonium nilrite, azodicarbonamide.
The preparation method of a kind of porous polyimide coated graphite material the most according to claim 1, it is characterised in that: step
Suddenly one or more during the graphite described in (2) is Delanium or native graphite.
The preparation method of a kind of porous hollow graphite material the most according to claim 7, it is characterised in that: described graphite is pure
Degree ＞'s 99.99%, granularity D50=16-20um.
The preparation method of a kind of porous polyimide coated graphite material the most according to claim 1, it is characterised in that: step
Suddenly one or more during the noble gas described in (3) is nitrogen, argon, helium.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109088062A (en) * | 2018-08-14 | 2018-12-25 | 河北省科学院能源研究所 | A kind of preparation method of the modified nickel ion doped material of polyimides cladding, Dopants |
| CN109280385A (en) * | 2017-07-21 | 2019-01-29 | 达胜科技股份有限公司 | Composite material containing artificial graphite, graphite sheet and method for producing same |
| CN110518229A (en) * | 2019-09-17 | 2019-11-29 | 东莞赣锋电子有限公司 | A kind of lithium cobaltate cathode material of modification and preparation method thereof |
| WO2020155846A1 (en) * | 2019-01-31 | 2020-08-06 | 常德力元新材料有限责任公司 | Graphite adhesive tape and preparation method therefor |
| CN111525117A (en) * | 2020-05-11 | 2020-08-11 | 喻明兵 | Three-dimensional porous carbon coated Co3O4The negative electrode material of the sodium ion battery and the preparation method thereof |
| CN111599998A (en) * | 2020-05-15 | 2020-08-28 | 宁波锋成纳米科技有限公司 | Electrode active material and preparation method and application thereof |
| CN112447959A (en) * | 2020-12-10 | 2021-03-05 | 山东丰元化学股份有限公司 | Surface treatment method of high-nickel ternary cathode material |
| CN113135566A (en) * | 2021-03-19 | 2021-07-20 | 广东邦普循环科技有限公司 | Modification method of lithium battery negative electrode material graphite and modified graphite |
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| CN103682247A (en) * | 2012-09-24 | 2014-03-26 | 华为技术有限公司 | Composite negative plate for lithium ion battery as well as preparation method of composite negative plate and lithium ion battery |
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| JP2004247233A (en) * | 2003-02-17 | 2004-09-02 | Sanyo Electric Co Ltd | Nonaqueous electrolyte secondary battery |
| CN103682247A (en) * | 2012-09-24 | 2014-03-26 | 华为技术有限公司 | Composite negative plate for lithium ion battery as well as preparation method of composite negative plate and lithium ion battery |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280385A (en) * | 2017-07-21 | 2019-01-29 | 达胜科技股份有限公司 | Composite material containing artificial graphite, graphite sheet and method for producing same |
| CN109088062A (en) * | 2018-08-14 | 2018-12-25 | 河北省科学院能源研究所 | A kind of preparation method of the modified nickel ion doped material of polyimides cladding, Dopants |
| WO2020155846A1 (en) * | 2019-01-31 | 2020-08-06 | 常德力元新材料有限责任公司 | Graphite adhesive tape and preparation method therefor |
| CN110518229A (en) * | 2019-09-17 | 2019-11-29 | 东莞赣锋电子有限公司 | A kind of lithium cobaltate cathode material of modification and preparation method thereof |
| CN111525117A (en) * | 2020-05-11 | 2020-08-11 | 喻明兵 | Three-dimensional porous carbon coated Co3O4The negative electrode material of the sodium ion battery and the preparation method thereof |
| CN111599998A (en) * | 2020-05-15 | 2020-08-28 | 宁波锋成纳米科技有限公司 | Electrode active material and preparation method and application thereof |
| CN111599998B (en) * | 2020-05-15 | 2021-07-27 | 宁波锋成纳米科技有限公司 | Electrode active material and preparation method and application thereof |
| CN112447959A (en) * | 2020-12-10 | 2021-03-05 | 山东丰元化学股份有限公司 | Surface treatment method of high-nickel ternary cathode material |
| CN113135566A (en) * | 2021-03-19 | 2021-07-20 | 广东邦普循环科技有限公司 | Modification method of lithium battery negative electrode material graphite and modified graphite |
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