CN107032338A - A kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene - Google Patents
A kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene Download PDFInfo
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Abstract
The present invention relates to grapheme material preparation field, and in particular to a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene.Graphite powder and paraffin are thermally formed liquid dispersion in advance first, then continuously sprayed to by high-pressure atomization between two electrodes pre-set, atomization graphite occurs Explosive Solutions under heavy impulse current effect and is cleaved into graphene, later fall into chilling pond, be fixed as in the paraffin that chilling is condensed under graphene is completely dispersed state powdered.The present invention realizes continuous parallel off and prepares graphene, and effectively overcomes the reunion of graphene, and obtained graphene has good dispersiveness in plastics, rubber.This method peels off graphene by high pressure draught and electric current blast, can not only efficiently utilize raw material, reduces cost, and preparation process is simple, does not introduce impurity.
Description
Technical field
The present invention relates to grapheme material preparation field, and in particular to a kind of continuous discharge-induced explosion parallel off preparing graphite alkene
Method.
Background technology
Come into the graphene in the popular visual field suddenly because of the Nobel Prize, be intensity highest material known to the mankind.Graphite
Alkene is the graphite film of monoatomic layer, and its lattice is the bi-dimensional cellular structure being made up of carbon atom.The material has many novelties
Physical characteristic, it is to be currently known the best material of electric conductivity at normal temperatures, and the movement velocity of electronics wherein reaches
The 1/300 of the light velocity, considerably beyond general conductor.In addition, also can use graphene to manufacture composite, battery/super capacitor, storage
Hydrogen material, field emmision material, hypersensor etc..
The preparation method of graphene mainly includes chemical vapour deposition technique, oxidation intercalation and restores method, liquid phase stripping method, machine
Tool stripping method.Wherein chemical vapour deposition technique can obtain high-quality graphene, but low yield, require high to substrate, turn
Move and there is greatly difficulty；Oxidation intercalation, which restores method, can realize batch production graphene, but be due to stone in oxidizing process
The structure of black alkene is destroyed, it is difficult to obtain high-quality graphene product；Liquid phase stripping method is in a suitable solvent, to utilize
Ultrasonic energy is dissociated to graphite flake layer, is difficult to remove asking for residual solvent however, solvent stripping method prepares graphene presence
Topic, and solvent stripping yield is general very low.By contrast, mechanical stripping method is that one kind can prepare high-quality stone with low cost
The method simple and easy to apply of black alkene.However, directly mechanical stripping efficiency is low, and high energy consumption, obtained graphene number of plies distribution is not
, quality stability is poor.
Chinese invention patent application number 201510230893.3 discloses a kind of utilization discharge-induced explosion and prepares grapheme material
Method, graphite rod is fixed between electrode；Distilled water is added into discharge-induced explosion tank, discharge-induced explosion tank is sealed；To discharge-induced explosion system
High-voltage capacitance group charging in system, it is rear to start discharge-induced explosion system；Electric discharge opens discharge-induced explosion tank after terminating, and collects in discharge-induced explosion tank
Suspension；Suspension is carried out to stand after ultrasonic disperse processing, filtering；Hydrochloric acid is added into filtrate, is filtered, is washed to neutrality,
Vacuum drying obtains the grapheme material.But, this discharge-induced explosion prepares graphene method can only be interrupted work in blasting cartridge
Make, cause preparation process discontinuous.
Chinese invention patent application number 201510230895.2 discloses one kind and prepares nitrogen-doped graphene using discharge-induced explosion
The method of material, belongs to technology field.Methods described is assembling and graphite rod is fixed on into electricity after debugging discharge-induced explosion system
Between pole；Nitrogen source solution is added into discharge-induced explosion tank, discharge-induced explosion tank is sealed；High-voltage capacitance group into discharge-induced explosion system is filled
Electricity, it is rear to start discharge-induced explosion system；Electric discharge opens discharge-induced explosion tank after terminating, and collects the suspension in discharge-induced explosion tank；Suspension is entered
Stood after the processing of row ultrasonic disperse, filtering；Hydrochloric acid is added into filtrate, is filtered, washing to neutrality, vacuum drying obtains the nitrogen
Doped graphene material.But the program needs liquid phase environment, cause graphenic surface to carry impurity, reduce graphene performance.
Chinese invention patent application number 201210160242.8 discloses a kind of method that blast prepares graphene, first
Reactor interior sealing is added to after decomposition explosion material is mixed with expanded graphite, then reactor is heated to 400 DEG C~600
DEG C, kept for 3~5 minutes, naturally cool to room temperature, collect product, obtain the graphene.But this method needs decomposition explosion
Property material, has potential safety hazard for operating personnel, and the impurity of explosive substance can also influence the performance of graphene.
In summary, had using discharge-induced explosion and do not introduce the advantageous of chemical impurity, but be the failure to realize continuous production.And
And obtained graphene is difficult to effectively disperse, therefore, there is presently no a kind of continuous discharge-induced explosion parallel off preparing graphite alkene
Method.
The content of the invention
It is discontinuous for parallel off preparing graphite alkene process of exploding in the prior art, require higher to preparing environmental condition
Defect, graphene is difficult to scattered defect, and the present invention proposes a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene,
By the way that by paraffin melting and the continuous injection of graphite atomization, between electrode, graphite occurs Explosive Solutions under heavy impulse current effect and split
Into graphene, chilling pond is later fallen into, the wax that chilling is condensed in the case where graphene is completely dispersed state is fixed as powdered.Not only
Realize continuous parallel off and prepare graphene, and effectively overcome the reunion of graphene, obtained graphene is in plastics, rubber
With good dispersiveness.
To solve the above problems, the present invention uses following technical scheme：
A kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene, using graphite powder as raw material, paraffin is used as graphene
Surface protectant, comprises the following steps：
（1）Graphite powder is cleaned, is removed after impurity, argon gas protection dry for standby；
（2）Graphite powder material and paraffin are mixed and are put into milling apparatus, sets the temperature of milling apparatus to 60~100 DEG C, grinds
Mill speed is 20~50 rpm/min, by heating paraffin, forms liquid, and thinner solid product is obtained after grinding for graphite
Fine powder, and graphite powder material is dispersed in liquid paraffin, obtains graphite powder paraffin homogeneous dispersion；
（3）The graphite powder paraffin homogeneous dispersion is atomized with high pressure draught, sprayed between two electrodes pre-set, it is described
10-20 A alternating current is provided between two electrodes, the graphite powder paraffin homogeneous dispersion is quick-fried under heavy impulse current effect
It is fried to be cracked into graphene, chilling pond is then fallen into, graphene in paraffin, forms stable grapheme material by rapid condensation.
It is preferred that, the graphite powder material is crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, oxidation stone
At least one of ink.
It is preferred that, the paraffin is any one in fully refined paraffin wax, semi-refined paraffin wax and scale wax.
It is preferred that, the mass ratio of the graphite powder and paraffin is 1:0.1-1.
It is preferred that, the cleaning graphite powder comprises the following steps：
Ultrasound 0.5 ~ 1 minute first in HF solution, removes graphite surface impurity, finally with deionized water rinsing, removes HF residual
Liquid is stayed, graphite powder is dried under 80 ~ 90 DEG C of argon gas protection；The HF solution concentrations are 3.5 ~ 5%；The argon gas protects drying
Argon gas be that purity is 99.9%, the ambient pressure of argon gas is 100 ~ 1000 Pa.
It is preferred that, the milling apparatus is ball mill, sand mill or engagement screws extruder in the same direction.
It is preferred that, the spout pressure of the high pressure draught is 0.08-0.12MPa, and exit velocity is 20.8-24.4 meter per seconds.
It is preferred that, the length of described two electrodes is 1-2 meters, and the distance between two-plate is 10-20cm, and material is anaerobic
Any one in copper coin, anaerobic nickel plate, anaerobic platinum sheet, anaerobic zine plate.
It is preferred that, the alternating electric field between described two electrodes is that voltage is 1-5KV, and alternative frequency is 100Hz-1MHz.
It is preferred that, the temperature in the chilling pond is -50 ~ -10 DEG C that liquid nitrogen is controlled.
The present invention proposes a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene, compared with prior art, and it is dashed forward
The characteristics of going out and excellent effect are：
1st, the present invention provides a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene, by the way that atomization graphite is continuously sprayed
To between electrode, generation Explosive Solutions are cleaved into graphene under heavy impulse current effect
2nd, the present invention is using paraffin as liquid, the graphene dispersion that complete blast is peeled off, and further quick chilling, is condensed
Wax is fixed as powdered, effectively overcomes the reunion of graphene, and obtained graphene has good scattered in plastics, rubber
Property.
3rd, the present invention is not directed to chemical reaction in preparation process, it is to avoid destruction of the chemical reaction to graphene-structured,
The product quality of acquisition is higher, environment is polluted few.
3rd, reaction condition of the present invention is controllable, and raw materials for production are recyclable, and preparation efficiency is high, production cost reduction, possesses continuous
Large-scale industrial production condition.
Brief description of the drawings
Fig. 1 is scattered electron microscope of the obtained graphene of the embodiment of the present invention 1 in butadiene-styrene rubber.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention
Scope be only limitted to following example.In the case where not departing from above method thought of the present invention, according to ordinary skill
Various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
（1）Mass ratio is used for 1:0.8 crystalline graphite powder is raw material with fully refined paraffin wax, and fully refined paraffin wax is used as graphene table
Face protective agent, by crystalline graphite powder solution concentration for 5% HF solution in ultrasound 1 minute, remove graphite surface impurity, finally
With deionized water rinsing, HF Liquid Residues are removed, are 1000 Pa in ambient pressure, 80 DEG C of purity protect lower dry for 99.9% argon gas
Drystone ink powder, is removed after impurity, argon gas protection dry for standby；
（2）Graphite powder material and paraffin are mixed and are put into ball mill, sets the temperature of ball mill to 60 DEG C, grinding rate is 50
Rpm/min, by heating paraffin, forms liquid, and thinner solid product is obtained after grinding for graphite fine powder, and graphite powder
Material is dispersed in liquid paraffin, obtains graphite powder paraffin homogeneous dispersion；
（3）The graphite powder paraffin homogeneous dispersion is atomized with high pressure draught, the spout pressure of high pressure draught is 0.08MPa,
Exit velocity is 24.4 meter per seconds, is sprayed between two electrodes pre-set, electrode material is no-oxygen copper plate, two no-oxygen copper plates
Length be 1 meter, the distance between two-plate is 20cm, and 20 A alternating current is provided between two no-oxygen copper plate, described
Graphite powder paraffin homogeneous dispersion is under heavy impulse current effect, and blast is cracked into graphene, then falls into chilling pond, chilling pond
Temperature be -10 DEG C, graphene in paraffin, forms stable grapheme material by rapid condensation.
The graphene prepared in embodiment is carried out after performance test, data are obtained as shown in table 1.
Embodiment 2
（1）Mass ratio is used for 1:1 thermal cracking graphite powder is raw material with fully refined paraffin wax, and fully refined paraffin wax is used as graphene table
Face protective agent, by thermal cracking graphite powder solution concentration for 3.5% HF solution in ultrasound 0.5 minute, remove thermal cracking graphite table
Face impurity, finally with deionized water rinsing, removes HF Liquid Residues, is 100 Pa, the argon that 90 DEG C of purity are 99.9% in ambient pressure
Thermal cracking graphite powder is dried under gas shielded, is removed after impurity, argon gas protection dry for standby；
（2）Thermal cracking graphite powder material and paraffin are mixed and are put into sand mill, the temperature of sand mill is set to 80 DEG C, grinding speed
Spend for 25 rpm/min, by heating paraffin, form liquid, thinner solid product is obtained after grinding for graphite fine powder, and
And graphite powder material is dispersed in liquid paraffin, graphite powder paraffin homogeneous dispersion is obtained；
（3）The graphite powder paraffin homogeneous dispersion is atomized with high pressure draught, the spout pressure of high pressure draught is 0.09MPa,
Exit velocity is 21 meter per seconds, is sprayed between two electrodes pre-set, and electrode material is no-oxygen copper plate, two no-oxygen copper plates
Length is 2 meters, and the distance between two-plate is the alternating current that 15 A are provided between 12cm, two no-oxygen copper plate, the stone
Ink powder paraffin homogeneous dispersion is under heavy impulse current effect, and blast is cracked into graphene, then falls into chilling pond, chilling pond
Temperature is -15 DEG C, and graphene in paraffin, forms stable grapheme material by rapid condensation.
The graphene prepared in embodiment is carried out after performance test, data are obtained as shown in table 1.
Embodiment 3
（1）Mass ratio is used for 1:0.5 graphite oxide powder is raw material with scale wax, and scale wax is protected as graphenic surface
Agent, by graphite oxide powder solution concentration for 4.5% HF solution in ultrasound 0.7 minute, remove graphite oxide surface impurity, most
Deionized water rinsing is used afterwards, HF Liquid Residues are removed, and is 500 Pa in ambient pressure, 85 DEG C of purity is under 99.9% argon gas protections
Graphite powder is dried, is removed after impurity, argon gas protection dry for standby；
（2）Graphite oxide powder material and scale wax are mixed and are put into engagement screws extruder in the same direction, engagement screws in the same direction are set
The temperature of extruder is to 100 DEG C, and extruded velocity is 30 rpm/min, by heating paraffin, forms liquid, is obtained more after extrusion
Thin solid product is graphite fine powder, and graphite powder material is dispersed in liquid paraffin, obtains graphite powder paraffin uniform
Dispersion；
（3）The graphite powder paraffin homogeneous dispersion is atomized with high pressure draught, the spout pressure of high pressure draught is 0.1MPa,
Exit velocity is 22.4 meter per seconds, is sprayed between two electrodes pre-set, electrode material is anaerobic nickel plate, two anaerobic nickel plates
Length be 1.5 meters, the distance between two-plate is 20cm, and 15 A alternating current, institute are provided between the two anaerobics nickel plate
Graphite powder paraffin homogeneous dispersion is stated under heavy impulse current effect, blast is cracked into graphene, then falls into chilling pond, chilling
The temperature in pond is -30 DEG C, and graphene in paraffin, forms stable grapheme material by rapid condensation.
The graphene prepared in embodiment is carried out after performance test, data are obtained as shown in table 1.By obtained stone
Black alkene makes an addition to the direct banburying mixing 5min of butadiene-styrene rubber with 5% ratio, and its dispersiveness, such as Electronic Speculum of accompanying drawing 1 is tested using Electronic Speculum
Shown in figure, graphene has good dispersiveness with butadiene-styrene rubber, and routinely equipment and technique are that disperseing for graphene can be achieved.
Embodiment 4
（1）Mass ratio is used for 1:0.3 expanded graphite powder is raw material with semi-refined paraffin wax, and semi-refined paraffin wax is used as graphene table
Face protective agent, by expanded graphite powder solution concentration for 4% HF solution in ultrasound 0.7 minute, remove graphite surface impurity, most
Deionized water rinsing is used afterwards, HF Liquid Residues are removed, and is 500 Pa in ambient pressure, 85 DEG C of purity is under 99.9% argon gas protections
Graphite powder is dried, is removed after impurity, argon gas protection dry for standby；
（2）Expanded graphite powder material and paraffin are mixed and are put into reverse engagement screws extruder, sets reverse engagement screws to squeeze
Go out the temperature of machine to 85 DEG C, extruded velocity is 40 rpm/min, by heating paraffin, forms liquid, obtains thinner after grinding
Solid product be graphite fine powder, and graphite powder material is dispersed in liquid paraffin, is obtained graphite powder paraffin and is uniformly divided
Granular media；
（3）The graphite powder paraffin homogeneous dispersion is atomized with high pressure draught, the spout pressure of high pressure draught is 0.11MPa,
Exit velocity is 22 meter per seconds, is sprayed between two electrodes pre-set, and electrode material is anaerobic zine plate, two anaerobic zine plates
Length is 1.6 meters, and the distance between two-plate is the alternating current that 12 A are provided between 18cm, the two anaerobics zine plate, described
Graphite powder paraffin homogeneous dispersion is under heavy impulse current effect, and blast is cracked into graphene, then falls into chilling pond, chilling pond
Temperature be -50 DEG C, graphene in paraffin, forms stable grapheme material by rapid condensation.
The graphene prepared in embodiment is carried out after performance test, data are obtained as shown in table 1.
Embodiment 5
（1）Mass ratio is used for 1:0.8 crystalline flake graphite is raw material with thermal cracking graphite mixed powder and fully refined paraffin wax, full essence
Paraffin is refined as graphenic surface protective agent, by mixing graphite powder in solution concentration is 5% HF solution ultrasound 0.5 minute, go
Except graphite surface impurity, finally with deionized water rinsing, HF Liquid Residues are removed, are 1000 Pa in ambient pressure, 89 DEG C of purity are
The 99.9% lower drying graphite powder of argon gas protection, is removed after impurity, argon gas protection dry for standby；
（2）Graphite powder material and paraffin are mixed and are put into ball mill, sets the temperature of ball mill to 90 DEG C, grinding rate is 20
Rpm/min, by heating paraffin, forms liquid, and thinner solid product is obtained after grinding for graphite fine powder, and graphite powder
Material is dispersed in liquid paraffin, obtains graphite powder paraffin homogeneous dispersion；
（3）The graphite powder paraffin homogeneous dispersion is atomized with high pressure draught, the spout pressure of high pressure draught is 0.08MPa,
Exit velocity is 21 meter per seconds, is sprayed between two electrodes pre-set, and electrode material is anaerobic platinum sheet, two anaerobic platinum sheets
Length is 1.2 meters, and the distance between two-plate is the alternating current that 20 A are provided between 18cm, the two anaerobics platinum sheet, described
Graphite powder paraffin homogeneous dispersion is under heavy impulse current effect, and blast is cracked into graphene, then falls into chilling pond, chilling pond
Temperature be -45 DEG C, graphene in paraffin, forms stable grapheme material by rapid condensation.
The graphene prepared in embodiment is carried out after performance test, data are obtained as shown in table 1.
Table 1：
| Performance indications | 90% graphene thickness | Charge stripping efficiency | It is dispersed in butadiene-styrene rubber |
| Embodiment one | 0.5-2nm | 34.5% | Well |
| Embodiment two | 1.5-2nm | 33.4% | Well |
| Embodiment three | 0.8-1.6nm | 30.8% | Well |
| Example IV | 2.5-3.7nm | 37.1% | Well |
| Embodiment five | 2.9-4.0nm | 42.1% | Well |
Claims (10)
1. a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene, using graphite powder as raw material, paraffin is used as graphite
Alkene surface protectant, comprises the following steps：
（1）Graphite powder is cleaned, is removed after impurity, argon gas protection dry for standby；
（2）Graphite powder material and paraffin are mixed and are put into milling apparatus, sets the temperature of milling apparatus to 60~100 DEG C, grinds
Mill speed is 20~50 rpm/min, by heating paraffin, forms liquid, and thinner solid product is obtained after grinding for graphite
Fine powder, and graphite powder material is dispersed in liquid paraffin, obtains graphite powder paraffin homogeneous dispersion；
（3）The graphite powder paraffin homogeneous dispersion is atomized with high pressure draught, sprayed between two electrodes pre-set, it is described
10-20 A alternating current is provided between two electrodes, the graphite powder paraffin homogeneous dispersion is quick-fried under heavy impulse current effect
It is fried to be cracked into graphene, chilling pond is then fallen into, graphene in paraffin, forms stable grapheme material by rapid condensation.
2. a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene according to claim 1, it is characterised in that：It is described
Graphite powder material is at least one of crystalline flake graphite, expanded graphite, highly oriented graphite, thermal cracking graphite, graphite oxide.
3. a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene according to claim 1, it is characterised in that：It is described
Paraffin is any one in fully refined paraffin wax, semi-refined paraffin wax and scale wax.
4. a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene according to claim 1, it is characterised in that：It is described
The mass ratio of graphite powder and paraffin is 1:0.1-1.
5. a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene according to claim 1, it is characterised in that：It is described
Cleaning graphite powder comprises the following steps：
Ultrasound 0.5 ~ 1 minute first in HF solution, removes graphite surface impurity, finally with deionized water rinsing, removes HF residual
Liquid is stayed, graphite powder is dried under 80 ~ 90 DEG C of argon gas protection；The HF solution concentrations are 3.5 ~ 5%；The argon gas protects drying
Argon gas be that purity is 99.9%, the ambient pressure of argon gas is 100 ~ 1000 Pa.
6. a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene according to claim 1, it is characterised in that：It is described
Milling apparatus is ball mill, sand mill or engagement screws extruder in the same direction.
7. a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene according to claim 1, it is characterised in that：It is described
The spout pressure of high pressure draught is 0.08-0.12MPa, and exit velocity is 20.8-24.4 meter per seconds.
8. a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene according to claim 1, it is characterised in that：It is described
The length of two electrodes is 1-2 meters, and the distance between two-plate is 10-20cm, and material is no-oxygen copper plate, anaerobic nickel plate, anaerobic
Any one in platinum sheet, anaerobic zine plate.
9. a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene according to claim 1, it is characterised in that：It is described
Alternating electric field between two electrodes is that voltage is 1-5KV, and alternative frequency is 100Hz-1MHz.
10. a kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene according to claim 1, it is characterised in that：Institute
The temperature for stating chilling pond is -50 ~ -10 DEG C that liquid nitrogen is controlled.
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| CN110255530A (en) * | 2019-06-24 | 2019-09-20 | 兰州理工大学 | A kind of device of constraint electric detonation graphite preparation low-dimensional nano-sized carbon |
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