CN109065884A - The preparation method and material of acid wash purification resistance material artificial graphite pore-creating negative electrode material - Google Patents
The preparation method and material of acid wash purification resistance material artificial graphite pore-creating negative electrode material Download PDFInfo
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- CN109065884A CN109065884A CN201810939044.9A CN201810939044A CN109065884A CN 109065884 A CN109065884 A CN 109065884A CN 201810939044 A CN201810939044 A CN 201810939044A CN 109065884 A CN109065884 A CN 109065884A
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- 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
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Abstract
The invention discloses the preparation methods of acid wash purification resistance material artificial graphite pore-creating negative electrode material, including blocky resistance material is crushed micronized processing, resistance powder and acid solution are added reaction tank and impregnate, it is heated, stirring, after separation, resistance powder high temperature is dried, after dispersion, it is compound by mass parts ratio 99:1~99:15 progress will to disperse powder and modifying agent, high speed fusion dispersion, heating, the fully dispersed high temperature carbonization at 800-1300 DEG C later, it crushes powder surface reconditioning and forms core-shell structure, mixed on low speed is dispersed later, artificial graphite pore-creating negative electrode material is obtained after screening.The present invention thoroughly eliminates the impurity in material, substantially increase the purity of raw material, solving causes material some security risks such as bring short circuit, self discharge, bulge in the application because impurities of materials factor influences, porous structure is formed, these cavernous structures make material rate charge-discharge performance and material volume expansion be able to be promoted and improve.
Description
Technical field
The present invention relates to artificial graphite cathode material for lithium ion batteries technical field, in particular to acid wash purifies resistance
Expect the preparation method and material of artificial graphite pore-creating negative electrode material.
Background technique
Lithium electric energy industry is quickly grown in recent years, and lithium electricity related industry is also synchronous to be rapidly developed, wherein graphite cathode material
Expect that demand is also increasing, and one of the important link in graphite cathode material precursor preparation technique is exactly to be graphitized,
Negative electrode material presoma is graphitized in process, is processed with product, and the resistance material in furnace can also be synchronized by related graphite
Change, but such material due in graphitizing process function be resistance material, generally have that degree of graphitization is relatively low, and impurity, ash content contains
It measures higher and unstable.At present in industry, such resistance material is mechanically pulverized to micron order, after do the processing of simple pattern,
Except magnetic, then applied as a kind of negative electrode material, due to material structure and metal, magnetic impurity ash grading factors shadow
It rings, can only be applied in low side negative electrode material field, using in the battery, there is short circuit in battery, and self discharge is very risky,
Simultaneously because material surface pattern is impaired serious, and specific surface area active increases at multiple, and active site is at double after machining
Number increases, these active sites are during charge and discharge, and acutely with electrolyte reaction, meeting constantly consumption is decomposed electrolyte battery and produced
Tympanites packet, seriously affects circulation storage performance and security performance, causes battery spontaneous combustion, explosion etc., and battery life is short, application
It is at high cost.
In view of this, it is necessory to provide battery short circuit caused by developing a kind of solution graphitization impurity and content of ashes,
The preparation method and its material of the acid wash purification resistance material artificial graphite pore-creating negative electrode material of the problems such as self discharge.
Summary of the invention
It is an object of the present invention to be directed to the above-mentioned deficiency of the prior art, acid wash purification resistance material artificial graphite is provided
The preparation method and material of pore-creating negative electrode material, thoroughly eliminate the impurity in material, substantially increase the purity of raw material, solve
Cause material some security risks such as bring short circuit, self discharge, bulge in the application because impurities of materials factor influences,
Porous structure is formed, these cavernous structures make material rate charge-discharge performance and material volume expansion be able to be promoted and change
It is kind.
The technical scheme adopted by the invention to achieve the purpose is as follows:
The preparation method of acid wash purification resistance material artificial graphite pore-creating negative electrode material, comprising the following steps:
S1: blocky resistance material is crushed into micronized processing and obtains resistance powder；
S2: being added reaction tank for resistance powder together with acid solution and impregnate, and heated, stirring, reaction after a certain period of time will
Acid solution is separated with resistance powder；
S3: carrying out high temperature drying for resistance powder, disperse later to drying material, obtains dispersion powder；
S4: dispersion powder is carried out to compound, high speed fusion dispersion with modifying agent by mass parts ratio 99:1~99:15, together
When be heated to 100-300 DEG C, to modifying agent and dispersion powder carry out it is fully dispersed, obtain comminuting matter；
S5: by comminuting matter, high temperature carbonization, crushing powder surface reconditioning simultaneously form core-shell structure at 800-1300 DEG C,
Mixed on low speed dispersion is carried out later, obtains artificial graphite pore-creating negative electrode material after screening.
Further, the partial size of the micronized processing to blocky resistance material is 10-50 μm.
Further, the acid solution is at least one of hydrofluoric acid, sulfuric acid.
Further, in the S2 heating temperature to 60-100 DEG C；Stirring frequency is 5-40r/min；Reaction time is
6-12h。
Further, high temperature drying carries out under inert gas protection；The temperature of high temperature drying is 800-1300
℃；The carbon content of resistance powder after high temperature drying is 98%~99.99%.
Further, the granularity D50 of the modifying agent is 1-15 μm.
Further, the modifying agent is modified pitch.
Further, the modified pitch is that formaldehyde occurs under the action of oxalic acid with the polycyclic aromatic hydrocarbon in coal tar pitch
Electrophilic substitution reaction, further cyclisation and aromatisation, form the modified pitch of the big polynuclear aromatic hydrocarbons structure containing molecular weight.
A kind of artificial stone that the preparation method of above-mentioned acid wash purification resistance material artificial graphite pore-creating negative electrode material is prepared
Black pore-creating negative electrode material, the partial size of the artificial graphite pore-creating negative electrode material are 13-18um.
Compared with prior art, the invention has the benefit that the present invention is by carrying out pre- micronized place to resistance material
Reason causes there are the impurity exposure inside packaging type interlayer in blocky resistance material, and pickling, fully reacting thoroughly eliminates object
Impurity in material substantially increases the purity of raw material, and solving causes material band in the application because impurities of materials factor influences
The short circuit come, self discharge, a series of security risks such as bulge.Simultaneously in acid cleaning process, in micronized smashed raw material
The ash content and impurity substances contained pass through strong acid dissolution after separated with strong acid solution so that material formed it is porous
Structure, these cavernous structures make material rate charge-discharge performance and material volume expansion be able to be promoted and improve, so that
This quasi-resistance class negative electrode material is achieved in middle and high-end market application.
Above-mentioned is the general introduction of inventive technique scheme, below in conjunction with attached drawing and specific embodiment, is done further to the present invention
Explanation.
Detailed description of the invention
Fig. 1 is the resistance block stock schematic diagram of the present embodiment；
Fig. 2 is resistance material schematic diagram after the micrometer crusher of the present embodiment；
Fig. 3 is crushing resistance material schematic diagram after the pickling of the present embodiment；
Fig. 4 is resistance material schematic diagram after the surface of the present embodiment coats；
Fig. 5 is that the charging advantage of the present embodiment and charging stress improve mechanism schematic diagram；
Fig. 6 is the high rate performance test schematic diagram of the present embodiment；
Fig. 7 is the multiplying power discharging test schematic diagram of the present embodiment.
Specific embodiment:
In order to which the purpose of the present invention and technical solution and advantage is more clearly understood, make with reference to embodiments detailed
Explanation.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not intended to limit the present invention.
A kind of embodiment 1: system of acid wash purification resistance material artificial graphite pore-creating negative electrode material provided in this embodiment
Method: blocky resistance material is crushed into micronized processing to 10-50 μm, resistance powder is obtained, destroys raw material interlayer in advance, make interlayer
Interior impurity is exposed；Reaction tank is added in resistance powder to impregnate together with hydrofluoric acid solution, 60 DEG C is heated to, is stirred,
Frequency reacts 8h in 5r/min, with heating hydrofluoric acid solution, later separates hydrofluoric acid solution with resistance powder；It will isolate
Resistance powder carry out being dried under the conditions of 800 DEG C of temperature under inert gas protection, so that its carbon content is reached 98%；It
Drying material is dispersed afterwards, dispersion powder is carried out with modifying agent by mass parts ratio 99:1 to compound, high speed fusion dispersion,
300 DEG C are heated to simultaneously, it is fully dispersed to modifying agent and dispersion powder progress, comminuting matter is obtained, wherein modifying agent is to be modified
Pitch, granularity D50 are 1-15um, and modified pitch is that with the polycyclic aromatic hydrocarbon in coal tar pitch parent occurs for formaldehyde under the action of oxalic acid
Electric substitution reaction, further cyclisation and aromatisation, form the modified pitch of the big polynuclear aromatic hydrocarbons structure containing molecular weight；By powder
Material carries out 800 DEG C of high temperature carbonizations after broken, repairs to powder surface is crushed, forms core-shell structure, and it is mixed to carry out low speed later
Dispersion is closed, obtains artificial graphite pore-creating negative electrode material after screening.
A kind of artificial stone that the preparation method of above-mentioned acid wash purification resistance material artificial graphite pore-creating negative electrode material is prepared
Black pore-creating negative electrode material, the partial size of the artificial graphite pore-creating negative electrode material are 13-18um.
A kind of embodiment 2: system of acid wash purification resistance material artificial graphite pore-creating negative electrode material provided in this embodiment
Method: blocky resistance material is crushed into micronized processing to 10-50 μm, resistance powder is obtained, destroys raw material interlayer in advance, make interlayer
Interior impurity is exposed；Reaction tank is added in resistance powder to impregnate together with hydrofluoric acid solution, 80 DEG C is heated to, is stirred,
Frequency reacts 12h in 20r/min, with heating hydrofluoric acid solution, later separates hydrofluoric acid solution with resistance powder；It will separation
Resistance powder out carries out being dried under the conditions of 1000 DEG C of temperature under inert gas protection, its carbon content is made to reach 98%-
99.99%；Drying material is dispersed later, dispersion powder and modifying agent are subjected to compound, height by mass parts ratio 99:15
Speed fusion dispersion, while 300 DEG C are heated to, it is fully dispersed to modifying agent and dispersion powder progress, comminuting matter is obtained, wherein
Modifying agent is modified pitch, granularity D50 is 1-15um, modified pitch be formaldehyde under the action of oxalic acid with it is more in coal tar pitch
Electrophilic substitution reaction, further cyclisation and aromatisation occur for cycloaromatics, form changing for the big polynuclear aromatic hydrocarbons structure containing molecular weight
Property pitch；Crushing rear material is subjected to 1300 DEG C of high temperature carbonizations, is repaired to powder surface is crushed, forms core-shell structure, it
Mixed on low speed dispersion is carried out afterwards, obtains artificial graphite pore-creating negative electrode material after screening.
A kind of artificial stone that the preparation method of above-mentioned acid wash purification resistance material artificial graphite pore-creating negative electrode material is prepared
Black pore-creating negative electrode material, the partial size of the artificial graphite pore-creating negative electrode material are 13-18um.
A kind of embodiment 3: system of acid wash purification resistance material artificial graphite pore-creating negative electrode material provided in this embodiment
Method: blocky resistance material is crushed into micronized processing to 10-50 μm, resistance powder is obtained, destroys raw material interlayer in advance, make interlayer
Interior impurity is exposed；Reaction tank is added in resistance powder to impregnate together with hydrofluoric acid solution, 100 DEG C is heated to, is stirred
It mixes, frequency reacts 12h in 40r/min, with heating hydrofluoric acid solution, later separates hydrofluoric acid solution with resistance powder；It will divide
The resistance powder separated out carries out being dried under the conditions of 1300 DEG C of temperature under inert gas protection, reaches its carbon content
98%-99.99%；Drying material is dispersed later, dispersion powder and modifying agent are answered by mass parts ratio 99:10
Conjunction, high speed fusion dispersion, while 200 DEG C are heated to, and it is fully dispersed to modifying agent and dispersion powder progress, obtain crushed material
Material, wherein modifying agent is modified pitch, granularity D50 is 1-15um, modified pitch be formaldehyde under the action of oxalic acid with coal tar pitch
In polycyclic aromatic hydrocarbon electrophilic substitution reaction, further cyclisation and aromatisation occurs, form the polynuclear aromatic hydrocarbons knot big containing molecular weight
The modified pitch of structure；Crushing rear material is subjected to 1000 DEG C of high temperature carbonizations, is repaired to powder surface is crushed, forms nucleocapsid
Structure carries out mixed on low speed dispersion later, obtains artificial graphite pore-creating negative electrode material after screening.
A kind of artificial stone that the preparation method of above-mentioned acid wash purification resistance material artificial graphite pore-creating negative electrode material is prepared
Black pore-creating negative electrode material, the partial size of the artificial graphite pore-creating negative electrode material are 13-18um.
A kind of embodiment 4: system of acid wash purification resistance material artificial graphite pore-creating negative electrode material provided in this embodiment
Method: blocky resistance material is crushed into micronized processing to 10-50 μm, resistance powder is obtained, destroys raw material interlayer in advance, make interlayer
Interior impurity is exposed；Reaction tank is added in resistance powder to impregnate together with hydrofluoric acid solution, 80 DEG C is heated to, is stirred,
Frequency reacts 6h in 30r/min, with heating hydrofluoric acid solution, later separates hydrofluoric acid solution with resistance powder；It will isolate
Resistance powder carry out being dried under the conditions of 1200 DEG C of temperature under inert gas protection, so that its carbon content is reached 98%-
99.99%；Drying material is dispersed later, dispersion powder and modifying agent are subjected to compound, height by mass parts ratio 99:5
Speed fusion dispersion, while 180 DEG C are heated to, it is fully dispersed to modifying agent and dispersion powder progress, comminuting matter is obtained, wherein
Modifying agent is modified pitch, granularity D50 is 1-15um, modified pitch be formaldehyde under the action of oxalic acid with it is more in coal tar pitch
Electrophilic substitution reaction, further cyclisation and aromatisation occur for cycloaromatics, form changing for the big polynuclear aromatic hydrocarbons structure containing molecular weight
Property pitch；Crushing rear material is subjected to 1200 DEG C of high temperature carbonizations, is repaired to powder surface is crushed, forms core-shell structure, it
Mixed on low speed dispersion is carried out afterwards, obtains artificial graphite pore-creating negative electrode material after screening.
A kind of artificial stone that the preparation method of above-mentioned acid wash purification resistance material artificial graphite pore-creating negative electrode material is prepared
Black pore-creating negative electrode material, the partial size of the artificial graphite pore-creating negative electrode material are 13-18um.
A kind of embodiment 5: system of acid wash purification resistance material artificial graphite pore-creating negative electrode material provided in this embodiment
Method: blocky resistance material is crushed into micronized processing to 10-50 μm, resistance powder is obtained, destroys raw material interlayer in advance, make interlayer
Interior impurity is exposed；Reaction tank is added in resistance powder to impregnate together with hydrofluoric acid solution, 100 DEG C is heated to, is stirred
It mixes, frequency reacts 10h in 10r/min, with heating hydrofluoric acid solution, later separates hydrofluoric acid solution with resistance powder；It will divide
The resistance powder separated out carries out being dried under the conditions of 1100 DEG C of temperature under inert gas protection, reaches its carbon content
98%-99.99%；Drying material is dispersed later, dispersion powder and modifying agent are answered by mass parts ratio 99:12
Conjunction, high speed fusion dispersion, while 300 DEG C are heated to, and it is fully dispersed to modifying agent and dispersion powder progress, obtain crushed material
Material, wherein modifying agent is modified pitch, granularity D50 is 1-15um, modified pitch be formaldehyde under the action of oxalic acid with coal tar pitch
In polycyclic aromatic hydrocarbon electrophilic substitution reaction, further cyclisation and aromatisation occurs, form the polynuclear aromatic hydrocarbons knot big containing molecular weight
The modified pitch of structure；Crushing rear material is subjected to 1100 DEG C of high temperature carbonizations, is repaired to powder surface is crushed, forms nucleocapsid
Structure carries out mixed on low speed dispersion later, obtains artificial graphite pore-creating negative electrode material after screening.
A kind of artificial stone that the preparation method of above-mentioned acid wash purification resistance material artificial graphite pore-creating negative electrode material is prepared
Black pore-creating negative electrode material, the partial size of the artificial graphite pore-creating negative electrode material are 13-18um.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned implementation
Mode is changed and is modified.Therefore, the invention is not limited to the specific embodiments disclosed and described above, to this hair
Bright some modifications and changes should also be as falling into the scope of the claims of the present invention.In addition, although in this specification
It uses some specific terms, these terms are merely for convenience of description, does not limit the present invention in any way.
Claims (9)
1. the preparation method of acid wash purification resistance material artificial graphite pore-creating negative electrode material, which comprises the following steps:
S1: blocky resistance material is crushed into micronized processing and obtains resistance powder；
S2: being added reaction tank for resistance powder together with acid solution and impregnate, heated, stirring, and reaction is molten by acid after a certain period of time
Liquid is separated with resistance powder；
S3: carrying out high temperature drying for resistance powder, disperse later to drying material, obtains dispersion powder；
S4: will dispersion powder and modifying agent by mass parts ratio 99:1~99:15 carry out it is compound, high speed fusion dispersion, simultaneously add
Heat is fully dispersed to modifying agent and dispersion powder progress to 100-300 DEG C, obtains comminuting matter；
S5: by comminuting matter at 800-1300 DEG C high temperature carbonization, crush powder surface reconditioning and simultaneously form core-shell structure, it is laggard
The dispersion of row mixed on low speed, obtains artificial graphite pore-creating negative electrode material after screening.
2. the preparation method of acid wash purification resistance material artificial graphite pore-creating negative electrode material as described in claim 1, which is characterized in that
The partial size of the micronized processing to blocky resistance material is 10-50 μm.
3. the preparation method of acid wash purification resistance material artificial graphite pore-creating negative electrode material as described in claim 1, which is characterized in that
The acid solution is at least one of hydrofluoric acid, sulfuric acid.
4. the preparation method of acid wash purification resistance material artificial graphite pore-creating negative electrode material as described in claim 1, which is characterized in that
Heating temperature is to 60-100 DEG C in the S2；Stirring frequency is 5-40r/min；Reaction time is 6-12h.
5. the preparation method of acid wash purification resistance material artificial graphite pore-creating negative electrode material as described in claim 1, which is characterized in that
The high temperature drying carries out under inert gas protection；The temperature of high temperature drying is 800-1300 DEG C；Electricity after high temperature drying
The carbon content for hindering powder is 98%~99.99%.
6. the preparation method of acid wash purification resistance material artificial graphite pore-creating negative electrode material as described in claim 1, which is characterized in that
The granularity D50 of the modifying agent is 1-15 μm.
7. the preparation method of acid wash purification resistance material artificial graphite pore-creating negative electrode material as described in claim 1, which is characterized in that
The modifying agent is modified pitch.
8. the preparation method of acid wash purification resistance material artificial graphite pore-creating negative electrode material as claimed in claim 7, which is characterized in that
The modified pitch be formaldehyde under the action of oxalic acid in coal tar pitch polycyclic aromatic hydrocarbon occur electrophilic substitution reaction and into
The modified pitch of the big polynuclear aromatic hydrocarbons structure containing molecular weight is formed after the cyclisation and aromatisation of one step.
9. the preparation method preparation that acid wash described in a kind of one of claim 1-8 purifies resistance material artificial graphite pore-creating negative electrode material
Obtained by artificial graphite pore-creating negative electrode material, the partial size of the artificial graphite pore-creating negative electrode material is 13-18um.
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| CN112645320A (en) * | 2020-12-22 | 2021-04-13 | 东莞市和鸿升新材料科技有限公司 | Method for preparing low-cost negative electrode material by recycling graphite crucible |
| CN112694087A (en) * | 2020-12-23 | 2021-04-23 | 东莞市和鸿升新材料科技有限公司 | Method for preparing low-cost negative electrode material by recycling resistance material |
| CN112875695A (en) * | 2021-01-29 | 2021-06-01 | 广东凯金新能源科技股份有限公司 | Artificial graphite as resistance material and preparation method thereof |
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Application publication date: 20181221 |
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| RJ01 | Rejection of invention patent application after publication |