CN108910869A - The preparation method of graphene slurry - Google Patents
The preparation method of graphene slurry Download PDFInfo
- Publication number
- CN108910869A CN108910869A CN201811026213.6A CN201811026213A CN108910869A CN 108910869 A CN108910869 A CN 108910869A CN 201811026213 A CN201811026213 A CN 201811026213A CN 108910869 A CN108910869 A CN 108910869A
- Authority
- CN
- China
- Prior art keywords
- graphite
- granularity
- obtains
- graphene
- paper
- 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
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
-
- 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
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/22—Intercalation
- C01B32/225—Expansion; Exfoliation
Abstract
The invention discloses a kind of preparation methods of graphene slurry, include the following steps：1）High temperature puffing is carried out to expansible graphite, then passes through the isolated graphite worm of object gas, then mat formation, is finally rolled into paper；2）Step 1）Obtained graphite paper is crushed, and reaches graphite powder, granularity is at 200-500 μm；3）Step 2）Obtained graphite powder further crushes, and obtains granularity in 5 μm of graphite microparticles below；4）Graphite microparticles are mixed with solvent, stirs evenly, is then handled using high-speed shearing machine, ultrasonic treatment is recycled, obtains graphene slurry.The present invention carries out subsequent preparation after roll off after high magnification expansible graphite extruding is increased its bulk density at paper again, removes more abundant；It is separated by high temperature puffing and object gas, exhaust gas and impurity therein can be removed, improve the quality of graphene slurry.
Description
Technical field
The invention belongs to technical field of graphene, and in particular to a kind of preparation method of graphene slurry.
Background technique
Graphene is a kind of Two-dimensional Carbon nanometer material for forming hexangle type in honeycomb lattice with sp2 hybridized orbit by carbon atom
Material.Graphene slurry can be used ultrasonic wave dispersion, sand mill and grinding distribution machine and be prepared.
The preparation method of existing common graphene slurry
1. obtaining graphite oxide by strong oxidizer, graphene oxide is obtained after ultrasonic oscillation, reducing agent is added and is gone back
Original obtains graphene.Strong oxidizer generally has strong corrosive, has certain risk, and strong oxidizer carries out natural graphite
Other nonmetalloids are remained after oxidation in graphite and are difficult to remove clean, and also needs to additionally incorporate reducing agent later and be restored
Reaction.General pollution is bigger in the oxidation-reduction process of this technique, is usually directed to danger compound product, and technical process is more multiple
It is miscellaneous, the graphene oxide of high quality is first prepared, it is restored again, process is complicated, and error and poor controllability aoxidize stone
The quality of black quality directly influences the quality of graphene, or even determines whether graphene is capable of forming, and general Strong oxdiative
Agent, which carries out oxidation to graphite, will cause the fault of construction of graphene, influence graphene performance.
2. liquid phase stripping method：Corresponding organic solvent and surfactant are added into crystalline flake graphite or expansible graphite, then
By ultrasonic wave up-stripping, the organic solvent and surfactant of such method design are subsequent there are certain environment pollution
Residual solvent is difficult to be removed in graphene in treatment process, seriously affects graphene performance.And graphite layers opening is not filled
Point, difficulty is big in subsequent stripping process, and removing is insufficient, and the single-layer graphene quantity that can be obtained is few.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of preparation methods of graphene slurry, and peeling effect is good,
Removing is thinner more sufficiently, and obtained graphene number of plies is lower, and the piece diameter of graphene is bigger.
The technical solution adopted by the present invention is that a kind of preparation method of graphene slurry, includes the following steps：
1）High temperature puffing is carried out to expansible graphite, then passes through the isolated graphite worm of object gas, then mat formation, finally grinds
It is pressed into paper；
2）Step 1）Obtained graphite paper is crushed, and obtains graphite powder, granularity is at 100-300 μm；
3）Step 2）Obtained graphite powder further crushes, and obtains granularity in 5 μm of graphite microparticles below；
4）Graphite microparticles are mixed with solvent, stirs evenly, is then handled using high-speed shearing machine, are recycled at ultrasound
Reason, obtains graphene slurry.
Further, the expansible graphite be high magnification expansible graphite, expansion multiple at 1000 times -1500 times,
Swelling temperature is 800 DEG C or more.
Further, to be mechanically pulverized when the step 2) crushes, step 3）It is air-flow crushing when crushing.
Further, step 3）After middle crushing, impurity and big granularity powder are removed through cyclone dust removal, three-level bag-type dust,
Screening machine screen size is relied on simultaneously, obtains 99% or more carbon amounts, granularity 5um graphite microparticles below.
Further, step 4）In graphite microparticles and solvent weight ratio be 3-10:97-90.It can according to need and add
Enter dispersing agent and suspending agent.
Further, step 4）In solvent according to graphene application field determine.
Further, step 4）When middle ultrasonic treatment, supersonic frequency is the KHz of 30KHz~60.
The carbon content of the expansible graphite is in 99.5wt% or more.
The invention has the advantages that：
1, use high magnification expansible graphite for raw material, expansion multiplying power reaches 1000-1500 times, which breaks tradition
Acid group intercalation theory, as shown in Figure 1, by coating to crystalline flake graphite, when heating expansion, it is swollen that large volume occurs for clad
Swollen expansive force distending atom interlayer has obtained adequately as shown in Fig. 2, obtaining high magnification expansible graphite between interlayer
It opens, substantially reduces graphene removing difficulty, established solid raw material supply basis for the production of graphene, increased
Graphene production efficiency, reduces costs.
2, by the way that graphite paper will be prepared after expansible graphite high temperature puffing, then by pulverizer graphite paper membrane is crushed
At graphite powder, granularity 200-500um, the basic material as production graphene.Due to production graphene when interlayer it
Between open more more more more advantageous sufficiently as basic material, and to open more sufficient expansible graphite multiplying power higher for interlayer, this
The basic material bulk density meeting very little of sample is either still cut at a high speed by the concussion removing of ultrasonic wave wave band to subsequent
The machine mechanical stripping of cutting is unfavorable, and high magnification expanded graphite density is bigger in unit volume, and removing contact surface is more intensive, and removing is more filled
Point, the present invention carries out subsequent system after obtained high magnification expansible graphite roll off is increased its bulk density at paper again
It is standby, it removes more abundant.In addition, either air-flow is removed, by equipment during mechanical shearing removing or ultrasonic wave up-stripping
Generated gas shock power direction, mechanical shear stress direction, ultrasonic frequency vibratory forces direction are all to prolong a direction substantially
It is changeless, and in the present invention during by expansible graphite extruding, simultaneously roll off is at graphite paper, the roll off power of application makes
It obtains the most of structure in the form of sheets of graphite and prolongs a horizontal direction arrangement, so that more big sheet knots can be obtained in removing
Structure graphene nano material.
3, due to, through the isolated graphite worm of object gas, being subsequently used for preparing graphite paper after expansible graphite extruding, lead to
High temperature puffing and the separation of object gas are crossed, exhaust gas and impurity therein can be removed, improve the quality of graphene slurry.It selects inflatable
Graphitic carbon content is 99% or more, and impurity is mainly silicate mineral, and exhaust gas is to need giving up for heating while puffing burning natural gas generation
Gas.Further the carbon content of preferred expansible graphite is in 99.5wt% or more.
Detailed description of the invention
Fig. 1 is that classical acid root cutting stratification reads schematic diagram.
Fig. 2 is the extruding schematic diagram of high magnification expansible graphite used in the present invention.
Fig. 3 is the made grapheme material Electronic Speculum phenogram of conventional method.
Fig. 4 is the made grapheme material Electronic Speculum phenogram of embodiment 1.
Fig. 5 is the made grapheme material Electronic Speculum phenogram of conventional method.
Fig. 6 is the made grapheme material Electronic Speculum phenogram of embodiment 1.
Specific embodiment
The present invention is further illustrated below with reference to embodiment, but the scope of protection of present invention is not limited to implement
The range of example statement.
Embodiment 1：
Applied to the graphene slurry of water paint, specific preparation step is：
1）Using high magnification expansible graphite as raw material（The high magnification expanded graphite is that Yichang is newly produced at graphite limited liability company
Product, for export trade, expansion multiple is 1500 times）, then compacted through the isolated graphite of object gas in 1000 DEG C of progress extrudings
Worm, then mat formation, it is rolled into paper, finally with a thickness of 0.1mm, density 1.25g/cm3；
2）Step 1）Obtained graphite paper is mechanically pulverized, and obtains graphite powder, granularity is at 100-300 μm；
3）Step 2）Obtained graphite powder is crushed by airslide disintegrating mill, by cyclone dust removal, three-level bag-type dust
Impurity and big granularity powder are removed, while relying on screening machine screen size, obtains 99% or more carbon amounts, granularity 5um graphite below
Micro mist；
4）Graphite microparticles are mixed with water, wherein graphite microparticles solid content is 6wt%, is stirred evenly, and high-speed shearing machine is then utilized
It is handled, recycles ultrasonic treatment, obtain graphene slurry.
Electron microscope analysis is carried out to obtained graphene slurry, as shown in Fig. 4 and Fig. 6, it is possible to find the made graphite of the present embodiment
Obvious more made than the conventional method graphene nano material removing of alkene nano material it is more sufficiently thinner, the number of plies is lower.And this hair
The piece diameter of the obvious graphene nano material more made than conventional method of bright made graphene nano material is generally bigger.
During high magnification expansible graphite extruding prepares graphite paper, authorization can be obtained using applicant
Patent equipment and technique are produced（It is directed to expansible graphite worm object air separation ZL201220720146X, high power
The flattening device ZL2012207201489 that mats formation, the ultra-thin graphite guide hotting mask of rate expansible graphite raw material heat pressure-sizing device
ZL2012207200804 and a kind of ultra-thin high thermal conductivity membrane material of high purity graphite high-tensile and production equipment
ZL2012105673225）, can also be produced using existing graphite paper production technology and equipments on the market.
Embodiment 2：
Applied to the graphene slurry of field of lithium, specific preparation step is：
1）The high magnification expansible graphite for being 1000 times using expansion multiple is raw material（The high magnification expanded graphite is the new Cheng Shi in Yichang
The product of black limited liability company's production, for export trade）, then compacted through the isolated graphite of object gas in 900 DEG C of progress extrudings
Worm, then mat formation, it is rolled into paper, finally with a thickness of 0.08mm, density 1.20g/cm3；
2）Step 1）Obtained graphite paper is mechanically pulverized, and obtains graphite powder, granularity is at 100-300 μm；
3）Step 2）Obtained graphite powder is crushed by airslide disintegrating mill, by cyclone dust removal, three-level bag-type dust
Impurity and big granularity powder are removed, while relying on screening machine screen size, obtains 99% or more carbon amounts, granularity 5um graphite below
Micro mist；
4）5 μm of graphite microparticles below are mixed with NMP, solid content passes through high-speed shearing machine in 4 wt% after mixing evenly（It is high
Shearing grinding homogenizer, cutting can（Shanghai）Mechanical equipment Co., Ltd）It was handled with 10000r/ minutes, passes through the liquid of the equipment
Circulation repeatedly grinds scissors to raw material progress mechanical water and cuts, and obtains 10-30 layers of graphene nanos addition property slurry, finally passes through ultrasonic wave
Emulsion dispersion machine（Hangzhou is far at Supersonic Tech Corp.）, slurry recycles special by the high-frequency vibration of ultrasonic wave in a reservoir
Property, up-stripping is carried out to the graphene nano material in slurry, and promote the dispersion of graphene nano material, finally obtains 5-
20 layers of graphene nano addition property slurry.
The above embodiments are only the preferred technical solution of the present invention, and are not construed as limitation of the invention, this hair
Bright protection scope should be with the technical solution of claim record, technical characteristic in the technical solution recorded including claim
Equivalents are protection scope.Equivalent replacement i.e. within this range is improved, also within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of graphene slurry, which is characterized in that include the following steps：
1）High temperature puffing is carried out to expansible graphite, then passes through the isolated graphite worm of object gas, then mat formation, finally grinds
It is pressed into paper；
2）Step 1）Obtained graphite paper is crushed, and obtains graphite powder, granularity is at 100-300 μm；
3）Step 2）Obtained graphite powder further crushes, and obtains granularity in 5 μm of graphite microparticles below；
4）Graphite microparticles are mixed with solvent, stirs evenly, is then handled using high-speed shearing machine, are recycled at ultrasound
Reason, obtains graphene slurry.
2. according to the method described in claim 1, it is characterized in that：The expansible graphite is high magnification expansible graphite,
For expansion multiple at 1000 times -1500 times, swelling temperature is 800 DEG C or more.
3. according to the method described in claim 1, it is characterized in that：To be mechanically pulverized when the step 2) crushes, step 3）
It is air-flow crushing when crushing.
4. according to the method described in claim 1, it is characterized in that：Step 3）After middle crushing, removed through cyclone dust removal, three-level cloth bag
Dirt removes impurity and big granularity powder, while relying on screening machine screen size, obtains 99% or more carbon amounts, granularity 5um stone below
Black micro mist.
5. according to the method described in claim 1, it is characterized in that：Step 4）In graphite microparticles and solvent weight ratio be 3-
10:97-90。
6. according to the method described in claim 1, it is characterized in that：Step 4）In solvent it is true according to graphene application field
It is fixed.
7. income approach according to claim 1, it is characterised in that：Step 4）When middle ultrasonic treatment, supersonic frequency is 30KHz~60
KHz。
8. income approach according to claim 1, it is characterised in that：The carbon content of the expansible graphite is in 99.5wt% or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811026213.6A CN108910869A (en) | 2018-09-04 | 2018-09-04 | The preparation method of graphene slurry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811026213.6A CN108910869A (en) | 2018-09-04 | 2018-09-04 | The preparation method of graphene slurry |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108910869A true CN108910869A (en) | 2018-11-30 |
Family
ID=64408267
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811026213.6A Pending CN108910869A (en) | 2018-09-04 | 2018-09-04 | The preparation method of graphene slurry |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108910869A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113563773A (en) * | 2021-07-26 | 2021-10-29 | 宝泰隆新材料股份有限公司北京技术研发中心 | Preparation method of graphene heat dissipation coating |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105110318A (en) * | 2015-07-23 | 2015-12-02 | 深圳市国创新能源研究院 | Graphene aqueous slurry, and preparation method thereof |
| CN107572511A (en) * | 2017-09-15 | 2018-01-12 | 兰州大学 | A kind of method of green large-scale production graphene |
| CN108083265A (en) * | 2017-02-27 | 2018-05-29 | 苏州鼎烯聚材纳米科技有限公司 | A kind of dry type of graphene nano powder removes production technology |
-
2018
- 2018-09-04 CN CN201811026213.6A patent/CN108910869A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105110318A (en) * | 2015-07-23 | 2015-12-02 | 深圳市国创新能源研究院 | Graphene aqueous slurry, and preparation method thereof |
| CN108083265A (en) * | 2017-02-27 | 2018-05-29 | 苏州鼎烯聚材纳米科技有限公司 | A kind of dry type of graphene nano powder removes production technology |
| CN107572511A (en) * | 2017-09-15 | 2018-01-12 | 兰州大学 | A kind of method of green large-scale production graphene |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113563773A (en) * | 2021-07-26 | 2021-10-29 | 宝泰隆新材料股份有限公司北京技术研发中心 | Preparation method of graphene heat dissipation coating |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108630338B (en) | A kind of method, apparatus for producing graphene conductive slurry in batches and graphene conductive slurry prepared therefrom | |
| CN106587027A (en) | Method for rapidly preparing small-dimensional graphene | |
| CN106882795B (en) | A kind of scale ultrasound stripping prepares the method for graphene and the application of graphene | |
| CN104658757B (en) | The process for dispersing of combined conductive agent in a kind of lithium-ion capacitor electrode slurry | |
| CN105819437B (en) | A kind of method that scale cleaning prepares graphene | |
| CN106744877B (en) | A kind of method that dry grinding removing prepares the device of graphene and produces graphene | |
| CN110143586A (en) | A kind of preparation method of the graphene of single layer or few layer | |
| CN107973293A (en) | The preparation method and graphene of graphene | |
| CN107716002B (en) | Device and method for preparing hexagonal boron nitride nanosheet through pure shear ball milling and ultrasonic cooperation | |
| CN109860548B (en) | Preparation method and application of nano silicon material | |
| CN110203913A (en) | A method of preparing graphene | |
| CN106582994A (en) | Device for continuously preparing graphene slurry and production method | |
| CN108264046A (en) | A kind of graphene-asphalt based active carbon and its preparation method and application | |
| CN110330012A (en) | The preparation method of high concentration graphene aqueous liquid dispersion and self-dispersing graphene powder | |
| CN111320150A (en) | Method for preparing hexagonal boron nitride nanosheets by ion insertion ultrasonic stripping of alkali metal salt | |
| CN108910869A (en) | The preparation method of graphene slurry | |
| CN113611438B (en) | Crushing method of carbon nanotube fiber bundle and conductive slurry | |
| CN107235495B (en) | A kind of method that depolymerization clay mineral crystalline substance beam prepares high length-diameter ratio monodimension nanometer material | |
| CN107188192B (en) | A kind of method that ionic liquid cooperates with high-pressure homogeneous processing to prepare monocrystalline dispersion nano-attapulgite stone | |
| CN106410210A (en) | Preparation method of metal hydride/nano carbon composite materials | |
| CN206352051U (en) | A kind of closed continuous complexes for preparing grapheme material | |
| CN111389530B (en) | Pressing cracking device and method of biomass power generation system | |
| CN110386597A (en) | Large-scale production thin graphene equipment and large-scale production thin graphene method | |
| CN106629687A (en) | Method for preparing graphene by jet mill and graphene | |
| CN109626360A (en) | Preparation method of carbon nano tube dispersion liquid and products thereof and application |
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 |