CN107887606A - The quick method for preparing graphene - Google Patents
The quick method for preparing graphene Download PDFInfo
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- CN107887606A CN107887606A CN201711028736.XA CN201711028736A CN107887606A CN 107887606 A CN107887606 A CN 107887606A CN 201711028736 A CN201711028736 A CN 201711028736A CN 107887606 A CN107887606 A CN 107887606A
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- Prior art keywords
- cetanol
- laminate
- thin ice
- deionized water
- pulverized particles
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses the method for quickly preparing graphene, including by high-purity expanded graphite, the relevant surfactant of anionic, dispersant, defoamer and solvent mechanical agitation, slurry after stirring is dried and crushed, solidified after pulverized particles and cetanol are mixed, cetanol after solidification is applied on thin ice laminate, thin ice laminate is placed in the mixture of deionized water and ethanol, thin ice laminate and hair cetanol are waved in heating, are filtered and are changed flash baking and finally give graphene powder.The beneficial effects of the invention are as follows：Production cost is low, producing efficiency is high.
Description
Technical field
The present invention relates to the energy and new material technology field, the method for particularly quickly preparing graphene.
Background technology
The charge and discharge process of lithium ion battery is exactly Li+ reversibly embedded and deintercalation processes between positive and negative pole material.
Li+ in charging in positive electrode departs from positive pole, into electrolyte, is migrated by barrier film to negative pole, in negative pole
It is upper to capture electronics and be reduced, and be stored in layer structure material；During electric discharge, the lithium in negative pole can lose electronics and form Li
+, into electrolyte, migrated through barrier film to positive extreme direction, and be stored in positive electrode.Preferable lithium ion battery should have
The qualities such as specific capacity is high, density is big, energy density is high, security is good, low temperature performance well, the good, long lifespan of high rate performance, this will
Its positive and negative pole material is asked to possess the features such as big specific surface area, good conductivity, internal resistance is small, electrolyte wellability is good.Carbon-based material
Received much concern as lithium battery positive and negative pole material.The active charcoal of carbon-based material, NACF, the charcoal-aero gel used now
And CNT etc., but above-mentioned carbon-based material is because the specific capacity reached is undesirable, purity is not high enough or preparation produced
Cheng Chengxu is complicated, cost is high and limits its application.Graphene is because of its excellent electric property, the specific surface area, excellent of superelevation
Chemical stability and thermodynamic stability and be considered as a kind of preferable lithium ion battery electrode material.
When prepared by now common graphene, graphene powder is typically placed in deionized water or is placed in deionized water
It is that graphene powder is suspended in deionized water or deionized water by stirring or the method for ultrasonic wave in the mixture of ethanol
In the mixture of ethanol, but a part of graphene powder can only be so allowed to suspend, also considerable powder does not suspend, no
Only cost is high, and many graphene powders can only extract few graphene layer every time, operating efficiency and its low.
For the above situation, the present invention provides the quick method for preparing graphene, practical, perfect and easily solve
Above mentioned problem.
The content of the invention
The shortcomings that it is an object of the invention to overcome prior art, there is provided production cost is low, producing efficiency is high quick prepares stone
The method of black alkene.
The purpose of the present invention is achieved through the following technical solutions：The quick method for preparing graphene, it includes following step
Suddenly：
S1, mixing, high-purity expanded graphite, the relevant surfactant of anionic, dispersant, defoamer and solvent are placed in reaction
30 ~ 120min of mechanical agitation in kettle, form mixed slurry；
S2, crushing, above-mentioned mixed slurry is placed in baking oven and dried, drying temperature is 100 DEG C ~ 150 DEG C, is formed after drying
Solid, above-mentioned solid is crushed, form the pulverized particles that particle diameter is less than 100 μm；
S3, mix again, choose cetanol, will warm up 50 DEG C ~ 70 DEG C, make its thawing, put into the cetanol after thawing
Above-mentioned pulverized particles, and 60min ~ 120min is stirred, after it stirs, the temperature of cetanol is reduced to 3 DEG C ~ 15 DEG C, is made
It is mixed with the cetanol solidification of pulverized particles；
S4, smearing, choose the higher glass of roughness and be placed in container bottom, a small amount of deionized water is imported into container, then drop
Temperature is to -10 DEG C ~ 15 DEG C, and deionized water forms thin ice laminate, is heated to 0 DEG C, thin ice laminate is taken out, the thin ice laminate and container
The face of bottom contact is the face with high roughness, then is placed in the environment that temperature is -20 DEG C ~ -30 DEG C, to the height of thin ice laminate
The equably cetanol of the contaminated product pulverized particles in smearing step S3 on the face of roughness；
S5, formation, the thin ice laminate for scribbling cetanol is placed in the mixture of deionized water and ethanol, is gradually heated up deionization
The solution that water and ethanol are mixed to form, thin ice laminate and cetanol is allowed gradually to melt, so as to allow the pulverized particles in cetanol to hang
The mixture surface of deionized water and ethanol is floated over, filters and flash baking obtains the graphene powder of high-purity.
Cetanol in described step S3 can also be replaced as other effumability alcohols.
The relevant surfactant of described anionic is sodium soap and titanate esters；Dispersant is polyvinyl alcohol.
Described flash baking concrete mode is microwave drying or vacuum drying.
The present invention has advantages below：By first mixing pulverized particles and cetanol, mixed cetanol is smeared
On thin ice laminate, thin ice laminate is placed in the mixture of deionized water and ethanol, can be achieved without stirring or ultrasonic wave
Pulverized particles are suspended in the mixture surface of deionized water and ethanol, allow more pulverized particles to suspend, pulverized particles will not be light
Easily fall in the mixture of deionized water and ethanol, the utilization rate of pulverized particles is high, has saved cost；The side smeared and mixed
Formula is very easy to realization, and whole work step spends the time few, improves operating efficiency suddenly,.
Embodiment
【Embodiment one】
The quick method for preparing graphene, it comprises the following steps：
S1, mixing, high-purity expanded graphite, the relevant surfactant of anionic, dispersant, defoamer and solvent are placed in reaction
Mechanical agitation 50min in kettle, form mixed slurry；
S2, crushing, above-mentioned mixed slurry being placed in baking oven and dried, drying temperature is 100 DEG C, and solid is formed after drying,
Above-mentioned solid is crushed, forms the pulverized particles that particle diameter is less than 100 μm；
S3, mix again, choose cetanol, will warm up 55 DEG C, make its thawing, above-mentioned powder is put into the cetanol after thawing
Broken particle, and 60min is stirred, after it stirs, the temperature of cetanol is reduced to 3 DEG C, makes the spermaceti for being mixed with pulverized particles
Alcohol solidifies；
S4, smearing, choose the higher glass of roughness and be placed in container bottom, a small amount of deionized water is imported into container, then drop
Temperature is to -10 DEG C, and deionized water forms thin ice laminate, is heated to 0 DEG C, thin ice laminate is taken out, the thin ice laminate and container bottom
The face of contact is the face with high roughness, then it is in -20 DEG C of environment, on the face of the high roughness of thin ice laminate to be placed in temperature
The equably cetanol of the contaminated product pulverized particles in smearing step S3；
S5, formation, the thin ice laminate for scribbling cetanol is placed in the mixture of deionized water and ethanol, is gradually heated up deionization
The solution that water and ethanol are mixed to form, thin ice laminate and cetanol is allowed gradually to melt, so as to allow the pulverized particles in cetanol to hang
The mixture surface of deionized water and ethanol is floated over, filters and fast vacuum dries to obtain the graphene powder of high-purity.
【Embodiment two】
S1, mixing, high-purity expanded graphite, the relevant surfactant of anionic, dispersant, defoamer and solvent are placed in reaction
Mechanical agitation 110min in kettle, form mixed slurry；
S2, crushing, above-mentioned mixed slurry being placed in baking oven and dried, drying temperature is 140 DEG C, and solid is formed after drying,
Above-mentioned solid is crushed, forms the pulverized particles that particle diameter is less than 100 μm；
S3, mix again, choose cetanol, will warm up 70 DEG C, make its thawing, above-mentioned powder is put into the cetanol after thawing
Broken particle, and 120min is stirred, after it stirs, the temperature of cetanol is reduced to 5 DEG C, makes the spermaceti for being mixed with pulverized particles
Alcohol solidifies；
S4, smearing, choose the higher glass of roughness and be placed in container bottom, a small amount of deionized water is imported into container, then drop
Temperature is to -15 DEG C, and deionized water forms thin ice laminate, is heated to 0 DEG C, thin ice laminate is taken out, the thin ice laminate and container bottom
The face of contact is the face with high roughness, then is placed in the environment that temperature is -30 DEG C, to the face of the high roughness of thin ice laminate
On equably contaminated product pulverized particles in smearing step S3 cetanol；
S5, formation, the thin ice laminate for scribbling cetanol is placed in the mixture of deionized water and ethanol, is gradually heated up deionization
The solution that water and ethanol are mixed to form, thin ice laminate and cetanol is allowed gradually to melt, so as to allow the pulverized particles in cetanol to hang
The mixture surface of deionized water and ethanol is floated over, filters and rapid microwave dries to obtain the graphene powder of high-purity.
In above-described embodiment one and embodiment two, described cetanol can also be replaced as other effumability alcohols；Institute
The relevant surfactant of anionic stated is sodium soap and titanate esters, and dispersant is polyvinyl alcohol.
Described above is only the preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein
Form, the exclusion to other embodiment is not to be taken as, and can be used for various other combinations, modification and environment, and can be at this
In the text contemplated scope, it is modified by the technology or knowledge of above-mentioned teaching or association area.And those skilled in the art are entered
Capable change and change does not depart from the spirit and scope of the present invention, then all should be in the protection domain of appended claims of the present invention
It is interior.
Claims (4)
1. the quick method for preparing graphene, it is characterised in that：It comprises the following steps：
S1, mixing, high-purity expanded graphite, the relevant surfactant of anionic, dispersant, defoamer and solvent are placed in reaction
30 ~ 120min of mechanical agitation in kettle, form mixed slurry；
S2, crushing, above-mentioned mixed slurry is placed in baking oven and dried, drying temperature is 100 DEG C ~ 150 DEG C, is formed after drying
Solid, above-mentioned solid is crushed, form the pulverized particles that particle diameter is less than 100 μm；
S3, mix again, choose cetanol, will warm up 50 DEG C ~ 70 DEG C, make its thawing, put into the cetanol after thawing
Above-mentioned pulverized particles, and 60min ~ 120min is stirred, after it stirs, the temperature of cetanol is reduced to 3 DEG C ~ 15 DEG C, is made
It is mixed with the cetanol solidification of pulverized particles；
S4, smearing, choose the higher glass of roughness and be placed in container bottom, a small amount of deionized water is imported into container, then drop
Temperature is to -10 DEG C ~ 15 DEG C, and deionized water forms thin ice laminate, is heated to 0 DEG C, thin ice laminate is taken out, the thin ice laminate and container
The face of bottom contact is the face with high roughness, then is placed in the environment that temperature is -20 DEG C ~ -30 DEG C, to the height of thin ice laminate
The equably cetanol of the contaminated product pulverized particles in smearing step S3 on the face of roughness；
S5, formation, the thin ice laminate for scribbling cetanol is placed in the mixture of deionized water and ethanol, is gradually heated up deionization
The solution that water and ethanol are mixed to form, thin ice laminate and cetanol is allowed gradually to melt, so as to allow the pulverized particles in cetanol to hang
The mixture surface of deionized water and ethanol is floated over, filters and flash baking obtains the graphene powder of high-purity.
2. the quick method for preparing graphene according to claim 1, it is characterised in that：Spermaceti in described step S3
Alcohol can also be replaced as other effumability alcohols.
3. the quick method for preparing graphene according to claim 1, it is characterised in that：The relevant table of described anionic
Face activating agent is sodium soap and titanate esters；Dispersant is polyvinyl alcohol.
4. the quick method for preparing graphene according to claim 1, it is characterised in that：Described flash baking is specifically square
Formula is microwave drying or vacuum drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711028736.XA CN107887606A (en) | 2017-10-29 | 2017-10-29 | The quick method for preparing graphene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711028736.XA CN107887606A (en) | 2017-10-29 | 2017-10-29 | The quick method for preparing graphene |
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| Publication Number | Publication Date |
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| CN107887606A true CN107887606A (en) | 2018-04-06 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104986758A (en) * | 2015-06-25 | 2015-10-21 | 厦门凯纳石墨烯技术有限公司 | Three-dimensional network graphene for lithium battery and preparing method thereof |
| CN105948027A (en) * | 2016-05-06 | 2016-09-21 | 成都新柯力化工科技有限公司 | Method for large-scale continuous preparation of graphene precursor and graphene precursor |
| CN106315567A (en) * | 2016-08-16 | 2017-01-11 | 肖丽芳 | Preparation method of foam graphene |
-
2017
- 2017-10-29 CN CN201711028736.XA patent/CN107887606A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104986758A (en) * | 2015-06-25 | 2015-10-21 | 厦门凯纳石墨烯技术有限公司 | Three-dimensional network graphene for lithium battery and preparing method thereof |
| CN105948027A (en) * | 2016-05-06 | 2016-09-21 | 成都新柯力化工科技有限公司 | Method for large-scale continuous preparation of graphene precursor and graphene precursor |
| CN106315567A (en) * | 2016-08-16 | 2017-01-11 | 肖丽芳 | Preparation method of foam graphene |
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Application publication date: 20180406 |