CN108910869A - The preparation method of graphene slurry - Google Patents
The preparation method of graphene slurry Download PDFInfo
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- 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
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 137
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 47
- 239000002002 slurry Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 70
- 239000010439 graphite Substances 0.000 claims abstract description 70
- 239000011859 microparticle Substances 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 230000001007 puffing effect Effects 0.000 claims abstract description 7
- 238000010008 shearing Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000000428 dust Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- 239000003595 mist Substances 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 2
- 230000008961 swelling Effects 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims 1
- 239000000463 material Substances 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000002086 nanomaterial Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 238000007796 conventional method Methods 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000007800 oxidant agent Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 241000549556 Nanos Species 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Carbon And Carbon Compounds (AREA)
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.
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Cited By (1)
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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 |
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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 |
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