CN108609616A - The preparation method of single-layer graphene with modified by ionic liquid cation group - Google Patents
The preparation method of single-layer graphene with modified by ionic liquid cation group Download PDFInfo
- Publication number
- CN108609616A CN108609616A CN201810416085.XA CN201810416085A CN108609616A CN 108609616 A CN108609616 A CN 108609616A CN 201810416085 A CN201810416085 A CN 201810416085A CN 108609616 A CN108609616 A CN 108609616A
- Authority
- CN
- China
- Prior art keywords
- ionic liquid
- modified
- cation group
- layer graphene
- liquid cation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/02—Single layer graphene
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to graphite flake preparing technical fields, more particularly to a kind of preparation method of the single-layer graphene with modified by ionic liquid cation group, the obtained low defect of success and the considerable single-layer graphene of yield, this method is easy to operate, mild condition, without the harsh conditions such as high temperature and pressure or strong oxidizer, be more convenient for practical operation and large-scale production.In addition, single-layer graphene made from this method not only there is oleophylic performance and high molecular polymer to dissolve each other, but also there is good electric conductivity.
Description
Technical field
The invention belongs to graphite flake preparing technical fields more particularly to a kind of with modified by ionic liquid cation group
The preparation method of single-layer graphene.
Background technology
Graphene is as a kind of new material, the upsurge for causing people to study, and all has potential application in many fields
Value, but extensive, low cost the graphene for preparing morphology controllable is still current urgent problem to be solved.
Currently, the method for preparing graphene have micromechanics stripping method, chemical vapour deposition technique, redox graphene method and
Liquid phase stripping method etc..Wherein, micromechanics stripping method is difficult to realize the industrialized actual requirement of graphene；Chemical vapour deposition technique energy
Large scale, whole continuous and with excellent properties graphene film material are enough prepared, but chemical vapour deposition technique prepares stone
The method of black alkene is not perfect and of high cost, very big the large-scale application for limiting graphene；Although redox graphene method
Achievable low cost prepares a large amount of graphene, however the method prepares the strong oxidizer used in the process of graphene and can make stone
The crystal structure of black alkene is seriously destroyed, and graphene overall performance is caused to decline；Liquid phase stripping method is generally possible to obtain crystal
The graphene of structural integrity, but that there are commonly solvents is often expensive, and also the method yield is relatively low.
Therefore, how to prepare the high single-layer graphene material of a large amount of quality on a low-cost basis becomes the weight of research
Point.
Invention content
It is an object of the invention to：In view of the deficiencies of the prior art, it provides a kind of with ionic liquid cation group
The preparation method of the single-layer graphene of modification, low defect and the considerable single-layer graphene of yield is made.
To achieve the goals above, the present invention uses following technical scheme：
The preparation method of single-layer graphene with modified by ionic liquid cation group, includes the following steps：
Step 1, using metal lithium sheet as battery cathode, graphite electrode as anode, with diaphragm by battery cathode and
Anode separates, and anode and battery cathode are dipped in completely in the electrolyte containing ionic liquid；
Step 2 carries out short circuit dischange to battery made from step 1, obtains carrying modified by ionic liquid cation group
LiCx；
Step 3 is added stripper into obtained by step 2, carries modified by ionic liquid cation group LiCxWith stripping
Liquid reacts, and the dispersion liquid with modified by ionic liquid cation group single-layer graphene is made；
Step 4 sets the dispersion liquid of the single-layer graphene with modified by ionic liquid cation group obtained by step 4
It is dried in baking oven, obtains the single-layer graphene with modified by ionic liquid cation group.
One of preparation method as the single-layer graphene of the present invention with modified by ionic liquid cation group
Kind is improved, and the ionic liquid is at least one of Formulas I, Formula II, formula III and formula IV compound represented；
Wherein, R1、R2、R3、R4、R5、R6、R7、R8Separately one kind in H atom and alkyl.Ionic liquid is
It is composed entirely of ions, it is pollution-free, nonflammable, stability is good, good conductivity and cheap.The present invention adds in the electrolytic solution
Ionic liquid be imidazoles, according to actual conditions, the ionic liquid of addition can also be pyridines, quaternary amines, pyrrolidines
With croak pyridine class.
One of preparation method as the single-layer graphene of the present invention with modified by ionic liquid cation group
Kind is improved, and the electrolyte further includes lithium salts and non-aqueous organic solvent, and the lithium salts is LiPF6And/or di-oxalate lithium borate
(LiBOB), it is 1 that the non-aqueous organic solvent, which includes volume ratio,:1:1 vinyl carbonate (EC), methyl ethyl carbonate (EMC) and carbon
Dimethyl phthalate (DMC).
One of preparation method as the single-layer graphene of the present invention with modified by ionic liquid cation group
Kind is improved, and the stripper includes water and ethyl alcohol.
One of preparation method as the single-layer graphene of the present invention with modified by ionic liquid cation group
Kind is improved, and in step 4, the drying temperature is 65~90 DEG C.
The beneficial effects of the present invention are：The present invention provides a kind of single layer stone with modified by ionic liquid cation group
Low defect and the considerable single-layer graphene of yield is successfully made in the preparation method of black alkene, and this method is easy to operate, mild condition,
Without the harsh conditions such as high temperature and pressure or strong oxidizer, be more convenient for practical operation and large-scale production.In addition, single made from this method
Layer graphene not only there is oleophylic performance and high molecular polymer to dissolve each other, but also have good electric conductivity.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention are simultaneously
It is without being limited thereto.
Embodiment 1
The preparation method of single-layer graphene with modified by ionic liquid cation group, includes the following steps：
Step 1, using metal lithium sheet as battery cathode, graphite electrode as anode, with diaphragm by battery cathode and
Anode separates, and anode and battery cathode are dipped in completely in the electrolyte containing ionic liquid；
Step 2 carries out short circuit dischange to battery made from step 1, obtains carrying modified by ionic liquid cation group
LiCx；
Step 3 is added stripper into obtained by step 2, carries modified by ionic liquid cation group LiCxWith stripping
Liquid reacts, and the dispersion liquid with modified by ionic liquid cation group single-layer graphene is made；
Step 4 sets the dispersion liquid of the single-layer graphene with modified by ionic liquid cation group obtained by step 4
It is dried in baking oven, obtains the single-layer graphene with modified by ionic liquid cation group.
Wherein, the compound that ionic liquid is as follows；R1、R2Separately one in H atom and alkyl
Kind.
Electrolyte further includes lithium salts and non-aqueous organic solvent, lithium salts LiPF6, non-aqueous organic solvent includes that volume ratio is 1:
1:1 vinyl carbonate (EC), methyl ethyl carbonate (EMC) and dimethyl carbonate (DMC)；Stripper includes water and ethyl alcohol.
Embodiment 2
The preparation method of single-layer graphene with modified by ionic liquid cation group, includes the following steps：
Step 1, using metal lithium sheet as battery cathode, graphite electrode as anode, with diaphragm by battery cathode and
Anode separates, and anode and battery cathode are dipped in completely in the electrolyte containing ionic liquid；
Step 2 carries out short circuit dischange to battery made from step 1, obtains carrying modified by ionic liquid cation group
LiCx；
Step 3 is added stripper into obtained by step 2, carries modified by ionic liquid cation group LiCxWith stripping
Liquid reacts, and the dispersion liquid with modified by ionic liquid cation group single-layer graphene is made；
Step 4 sets the dispersion liquid of the single-layer graphene with modified by ionic liquid cation group obtained by step 4
It is dried in baking oven, obtains the single-layer graphene with modified by ionic liquid cation group.
Wherein, the compound that ionic liquid is as follows；R3、R4Separately one in H atom and alkyl
Kind.
Electrolyte further includes lithium salts and non-aqueous organic solvent, and lithium salts is di-oxalate lithium borate (LiBOB), non-aqueous organic solvent
It is 1 including volume ratio:1:1 vinyl carbonate (EC), methyl ethyl carbonate (EMC) and dimethyl carbonate (DMC)；Stripper includes
Water and ethyl alcohol.
Embodiment 3
The preparation method of single-layer graphene with modified by ionic liquid cation group, includes the following steps：
Step 1, using metal lithium sheet as battery cathode, graphite electrode as anode, with diaphragm by battery cathode and
Anode separates, and anode and battery cathode are dipped in completely in the electrolyte containing ionic liquid；
Step 2 carries out short circuit dischange to battery made from step 1, obtains carrying modified by ionic liquid cation group
LiCx；
Step 3 is added stripper into obtained by step 2, carries modified by ionic liquid cation group LiCxWith stripping
Liquid reacts, and the dispersion liquid with modified by ionic liquid cation group single-layer graphene is made；
Step 4 sets the dispersion liquid of the single-layer graphene with modified by ionic liquid cation group obtained by step 4
It is dried in baking oven, obtains the single-layer graphene with modified by ionic liquid cation group.
Wherein, the compound that ionic liquid is as follows；R5、R6Separately one in H atom and alkyl
Kind.
Electrolyte further includes lithium salts and non-aqueous organic solvent, lithium salts LiPF6It is non-aqueous with di-oxalate lithium borate (LiBOB)
Organic solvent includes that volume ratio is 1:1:1 vinyl carbonate (EC), methyl ethyl carbonate (EMC) and dimethyl carbonate (DMC)；Stripping
Chaotropic includes water and ethyl alcohol.
Embodiment 4
The preparation method of single-layer graphene with modified by ionic liquid cation group, includes the following steps：
Step 1, using metal lithium sheet as battery cathode, graphite electrode as anode, with diaphragm by battery cathode and
Anode separates, and anode and battery cathode are dipped in completely in the electrolyte containing ionic liquid；
Step 2 carries out short circuit dischange to battery made from step 1, obtains carrying modified by ionic liquid cation group
LiCx；
Step 3 is added stripper into obtained by step 2, carries modified by ionic liquid cation group LiCxWith stripping
Liquid reacts, and the dispersion liquid with modified by ionic liquid cation group single-layer graphene is made；
Step 4 sets the dispersion liquid of the single-layer graphene with modified by ionic liquid cation group obtained by step 4
It is dried in baking oven, obtains the single-layer graphene with modified by ionic liquid cation group.
Wherein, the compound that ionic liquid is as follows；R7、R8Separately one in H atom and alkyl
Kind.
Electrolyte further includes lithium salts and non-aqueous organic solvent, lithium salts LiPF6It is non-aqueous with di-oxalate lithium borate (LiBOB)
Organic solvent includes that volume ratio is 1:1:1 vinyl carbonate (EC), methyl ethyl carbonate (EMC) and dimethyl carbonate (DMC)；Stripping
Chaotropic includes water and ethyl alcohol.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula is changed and is changed.Therefore, the invention is not limited in above-mentioned specific implementation mode, every those skilled in the art exist
Made any conspicuously improved, replacement or modification all belongs to the scope of protection of the present invention on the basis of the present invention.This
Outside, although having used some specific terms in this specification, these terms are merely for convenience of description, not to the present invention
Constitute any restrictions.
Claims (5)
1. the preparation method of the single-layer graphene with modified by ionic liquid cation group, which is characterized in that including following step
Suddenly：
Step 1, using metal lithium sheet as battery cathode, graphite electrode as anode, with diaphragm by battery cathode and battery
Anode separates, and anode and battery cathode are dipped in completely in the electrolyte containing ionic liquid；
Step 2 carries out short circuit dischange to battery made from step 1, obtains with modified by ionic liquid cation group
LiCx；
Step 3 is added stripper into obtained by step 2, carries modified by ionic liquid cation group LiCxIt is anti-with stripper
It answers, the dispersion liquid with modified by ionic liquid cation group single-layer graphene is made；
The dispersion liquid of the single-layer graphene with modified by ionic liquid cation group obtained by step 4 is placed in baking by step 4
It is dried in case, obtains the single-layer graphene with modified by ionic liquid cation group.
2. the preparation method of the single-layer graphene according to claim 1 with modified by ionic liquid cation group,
It is characterized in that：The ionic liquid is at least one of Formulas I, Formula II, formula III and formula IV compound represented；
Wherein, R1、R2、R3、R4、R5、R6、R7、R8Separately one kind in H atom and alkyl.
3. the preparation method of the single-layer graphene according to claim 1 with modified by ionic liquid cation group,
It is characterized in that：The electrolyte further includes lithium salts and non-aqueous organic solvent, and the lithium salts is LiPF6And/or di-oxalate lithium borate
(LiBOB), it is 1 that the non-aqueous organic solvent, which includes volume ratio,:1:1 vinyl carbonate (EC), methyl ethyl carbonate (EMC) and carbon
Dimethyl phthalate (DMC).
4. the preparation method of the single-layer graphene according to claim 1 with modified by ionic liquid cation group,
It is characterized in that：The stripper includes water and ethyl alcohol.
5. the preparation method of the single-layer graphene according to claim 1 with modified by ionic liquid cation group,
It is characterized in that：In step 4, the drying temperature is 65~90 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810416085.XA CN108609616A (en) | 2018-05-03 | 2018-05-03 | The preparation method of single-layer graphene with modified by ionic liquid cation group |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810416085.XA CN108609616A (en) | 2018-05-03 | 2018-05-03 | The preparation method of single-layer graphene with modified by ionic liquid cation group |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108609616A true CN108609616A (en) | 2018-10-02 |
Family
ID=63662009
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810416085.XA Pending CN108609616A (en) | 2018-05-03 | 2018-05-03 | The preparation method of single-layer graphene with modified by ionic liquid cation group |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108609616A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101214954A (en) * | 2008-01-22 | 2008-07-09 | 东北师范大学 | Method for preparing conductive single-layer graphite sheet modified by ionic liquid cation group |
| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
| CN102868006A (en) * | 2012-09-21 | 2013-01-09 | 华东理工大学 | Method for preparing graphene through waste lithium batteries |
| CN103626165A (en) * | 2012-08-28 | 2014-03-12 | 海洋王照明科技股份有限公司 | Graphene preparation method |
-
2018
- 2018-05-03 CN CN201810416085.XA patent/CN108609616A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101214954A (en) * | 2008-01-22 | 2008-07-09 | 东北师范大学 | Method for preparing conductive single-layer graphite sheet modified by ionic liquid cation group |
| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
| CN103626165A (en) * | 2012-08-28 | 2014-03-12 | 海洋王照明科技股份有限公司 | Graphene preparation method |
| CN102868006A (en) * | 2012-09-21 | 2013-01-09 | 华东理工大学 | Method for preparing graphene through waste lithium batteries |
Non-Patent Citations (2)
| Title |
|---|
| HAIPING LEI等: "Exfoliation Mechanism of Geaphite Cathode in Ionic Liquids", 《ACS APPLIED MATERIALS & INTERFACES》 * |
| 娄文勇: "《离子液体中生物催化不对称反应研究》", 31 May 2017, 华南理工大学出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107777688B (en) | Preparation method of sheet-like Mxene sheet material | |
| US11631886B2 (en) | Quasi-solid-state electrolyte based on ionic liquid for use in lithium battery and preparation method thereof | |
| CN107017432B (en) | Nonaqueous electrolytic solution and lithium ion battery | |
| CN109103488B (en) | Polymer sodium battery and preparation method and application thereof | |
| CN103811802B (en) | A kind of polymer Li-ion battery and manufacture method thereof | |
| CN103181003A (en) | Electrode plate, preparing method therefor, super capacitor and lithium ion battery | |
| CN106532113A (en) | Lithium battery electrolyte film-forming additive and preparation method | |
| CN108682824A (en) | A kind of composite negative electrode material of lithium ion battery, preparation method and the purposes in lithium ion battery | |
| CN104098785A (en) | Pvdf gel polymer electrolyte and preparation method thereof | |
| CN112599774A (en) | Flexible all-solid-state organic secondary battery and preparation method and application thereof | |
| CN105261789B (en) | electrolyte and lithium ion battery including the electrolyte | |
| CN109103500B (en) | Polymer lithium selenium battery and preparation method thereof | |
| CN107793564B (en) | Low-Tg polyether all-solid-state single-ion conductive polymer and preparation method thereof | |
| CN109037658A (en) | A kind of lithium iron phosphate positive material preparation method of polymer overmold | |
| CN105742711B (en) | A kind of electrolyte and a kind of lithium ion battery | |
| CN110474051B (en) | Application of common dye rhodamine B as organic anode material of lithium ion battery | |
| CN108609616A (en) | The preparation method of single-layer graphene with modified by ionic liquid cation group | |
| CN108711624A (en) | More carbonyl azacyclo- organic compounds of organic positive electrode for lithium battery and preparation method thereof | |
| TWI730924B (en) | Cathode material of lithium-ion battery and fabricating method thereof, and lithium-ion battery | |
| JP2003040885A (en) | Glycerol dicarbonate derivative, non-aqueous electrolyte solution produced by using the same, polymer electrolyte and cell | |
| CN103450610B (en) | Gel polymer electrolyte membrane, and preparation method and application thereof | |
| CN110336080B (en) | Preparation and application method of composite single-ion solid electrolyte | |
| CN108630987B (en) | Gel polymer electrolyte and preparation method and application thereof | |
| CN111116388A (en) | Preparation method of polyether-based ionic liquid, preparation method and application of high-voltage electrolyte | |
| CN111477383B (en) | Environment-friendly graphene conductive film for touch screen and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181002 |