CN104843688B - Graphene preparation method - Google Patents
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- CN104843688B CN104843688B CN201510186512.6A CN201510186512A CN104843688B CN 104843688 B CN104843688 B CN 104843688B CN 201510186512 A CN201510186512 A CN 201510186512A CN 104843688 B CN104843688 B CN 104843688B
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Abstract
The invention discloses a graphene preparation method. The method comprises the processes of liquid phase expansion treatment, ultrasonic peeling and drying, and the ultrasonic peeling process comprises the following steps: adding a peeling solution and wormlike graphene aggregation obtained after the liquid phase expansion treatment into a tank body provided with a plurality of ultrasonic vibration rods in proportion, introducing compressed air into the tank body to bubble and stir in order to make the wormlike graphene aggregation dispersed and suspending in the peeling solution, and controlling the ultrasonic vibration rods to carry out ultrasonic vibration treatment for 0.5-20h in order to obtain a flocculent graphene suspension. The method allows the wormlike graphene aggregation to be uniformly dispersed in the peeling solution, so the peeling effect is improved, and the peeling time is shortened.
Description
Technical field
The present invention relates to Graphene field, relate in particular to a kind of method of preparing Graphene.
Background technology
Since 2004 are found, Graphene receives much concern as a kind of new carbon. It is one completely bysp 2 The thickness that the carbon atom of hydridization forms is only the accurate two dimensional crystal material of monoatomic layer or several monoatomic layers, has high light transmittanceWith the excellent performance such as electric conductivity, high-specific surface area, high strength and pliability, be expected at high-performance nanometer electronic device, phototubeThe fields such as part, gas sensor, composite, field emmision material and stored energy obtain extensive use.
At present, the preparation method of Graphene has a variety of, and wherein " liquid phase expansion stripping method " is a kind of low cost, quality canControl, and is easy to industrialized preparation method, and the method is mainly taking graphite intercalation compound as raw material, through liquid phase expansion process,Ultrasonic wave is peeled off and is dried and processes after three operations, finally obtains graphene powder. As China Patent No." 201110282370.5 " disclose " a kind of method of preparing high-quality graphene " on May 2nd, 2012, and its technical scheme isFirst the graphite intercalation compound taking halogen or metal halide as intercalator, as raw material, enters in oxalic acid or hydrogenperoxide steam generatorRow expansion process obtains the quasiflake graphite alkene aggregation of high level expansion, then by quasiflake graphite alkene aggregation at organic solventOr in the aqueous solution of various surfactants or organic solvent solution, carry out ultrasonic oscillation processing, thereby obtain high-quality graphiteAlkene. In actual fabrication process, the effect that ultrasonic wave is peeled off by directly affect quasiflake graphite alkene aggregation peel off effect andThe quality of final products obtained therefrom, but in prior art, do not have the concrete stripping means of quasiflake graphite alkene aggregation, cause wrigglingThe stripping process of worm shape Graphene aggregation is uncontrolled, is unfavorable for peeling off of quasiflake graphite alkene aggregation.
In addition, although China Patent No. " 201320116823.1 " discloses " a kind of Graphene system on August 14th, 2013Intercalation peel-off device for subsequent use ", its technical scheme be described equipment comprise supersonic generator, ultrasonic wave dispersion tank and for to pointThe agitating device that graphite suspension in loose tank disperses, described agitating device comprises stirring motor, stirs rotating shaft and stirMix rotating vane, stir rotating shaft one end and connect stirring motor other end connection stirring rotating vane, described ultrasonic wave dispersion tankSidewall a plurality of ultrasonic transducers are installed, the bottom of ultrasonic wave dispersion tank presents infundibulate, bottom is provided with discharge gate,Drainage conduit is installed on discharge gate, is provided with and opens valve in drainage conduit, whole Graphene preparation is placed on intercalation peel-off deviceIn frame, the supersonic generator that electricity is converted to the high-frequency ac signal of telecommunication matching with ultrasonic transducer by cable withUltrasonic transducer is connected. But the prior art taking this patent document as representative, in actual use, still exist asLower defect: one, ultrasonic transducer is arranged on the outer wall of hexahedron structure tank body, and each transducer is to the distance at tank body centerDifference, causes the cavitation effect in each region in tank body inhomogeneous, not only affects the effect of peeling off of Graphene, has also reduced GrapheneThe quality of the utilization rate of raw material and Graphene product. Two, ultrasonic transducer is arranged on the outer wall of tank body, due to hyperacousticSwept area is limited, this structural limitations the size of tank body, cause using the ultrasonic stripping off device of this structure certainly will can not be largeScale is prepared Graphene product. Three, the transducer in this patent forms vibration plate by being bonded on tank wall, when needs are advised greatlyWhen molded standby Graphene, in every one side of tank body, need sticky dozens or even hundreds of transducer, due to the radiation of each transducerArea is little, and this mode has not only increased the volume of equipment, also exists and peels off weak effect, poor stability and awkward lackingPoint, is difficult to meet preparation of industrialization.
Summary of the invention
The object of the invention is to solve the above-mentioned problems in the prior art, a kind of side of preparing Graphene is providedMethod, the present invention can make quasiflake graphite alkene aggregation be distributed in stripper comparatively equably, peels off thereby reach to improve simultaneouslyThe object of effect and minimizing splitting time.
For achieving the above object, the technical solution used in the present invention is as follows:
Prepare a method for Graphene, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, itsBe characterised in that: described ultrasonic wave stripping process is that the quasiflake graphite alkene first obtaining by stripper with through liquid phase expansion process is assembledBody joins in the tank body that is provided with many ultrasound wave vibrating bars in proportion, then passes into the stirring of compressed air bubbling in tank body,Make quasiflake graphite alkene aggregation dispersion suspension in stripper, and then control the processing of ultrasound wave vibrating bar sonic oscillation0.5-20 hours, finally obtain cotton-shaped graphene suspension.
Described stripper is water or complex liquid, described complex liquid be by following component by mass percentage evenly mix andBecome: complexing of metal ion agent 5-20 %, surface tension modifier 1-5 %, all the other are water.
Complexing of metal ion agent in described complex liquid is sodium potassium tartrate tetrahydrate, sodium pyrophosphate, disodium edta, PortugalAnswering of one or more in grape sodium saccharate, ethylenediamine tetraacetic methene sodium phosphate, oxalic acid, oxalates, diethanol amine, triethanolamineClose, surface tension modifier is methyl alcohol, ethanol, propyl alcohol, lauryl sodium sulfate, neopelex, cetyl threeOne or more in methyl ammonium bromide, fluorocarbon surfactant compound.
In described tank body, the mass ratio of quasiflake graphite alkene aggregation and stripper is 1:5-1:100.
The ultrasonic frequency of described ultrasound wave vibrating bar is 25-40KHz, the sonic oscillation place of described ultrasound wave vibrating barThe reason time is 6-13 hours.
Described tank body is circular, and many ultrasound wave vibrating bars that are arranged in circular tank are many in same frontal plane of projectionAnnular distribution.
Many described ultrasound wave vibrating bars are vertical layered to be arranged in tank body, the lower end of upper strata ultrasound wave vibrating bar with underThe upper end dislocation of layer ultrasound wave vibrating bar is intersected, and on every ring, the quantity of ultrasound wave vibrating bar is the whole of the ultrasound wave vibrating bar number of pliesSeveral times.
In described tank body, the quantity of every layer of ultrasound wave vibrating bar is all identical, and the ultrasound wave vibrating bar of every layer evenly arranges tankIn body.
Described compressed air is by being arranged on the nozzle ejection on inner tank wall and bottom.
Employing the invention has the advantages that:
One, the present invention carries out before ultrasonic wave peels off starting ultrasound wave vibrating bar, in advance by compressed air in tank bodyQuasiflake graphite alkene aggregation and stripper carry out agitation treatment, this just can make quasiflake graphite alkene aggregation comparatively equablyBe distributed in stripper, improve thereby reach simultaneously the object of peeling off effect and reducing splitting time, both improved the profit of raw materialBy rate, improve again the quality of the Graphene product making.
Two, in the present invention, stripper can be both water, can be also complex liquid, when stripper is water, had to reduce and producedThe advantage of cost; When stripper is complex liquid, the complexing of metal ion agent in complex liquid can be adsorbed the gold being dissolved in solutionBelong to ion, make it lose catalytic activity, the surface tension modifier in complex liquid can be adjusted stripper to graphite and graphiteThe wellability of alkene, to promote the diffusion of swelling agent to graphite layers, and then effect is peeled off in enhancing. Compared with prior art, adoptThe complex liquid of specific components can make the final Graphene product number of plies obtaining lower than 10 layers, and mostly concentrates on 1-5 layers, graphiteThe percentage of impurity of alkene product, lower than 2%, has improved the quality of product.
Three, in the present invention, the mass ratio of quasiflake graphite alkene aggregation and stripper is 1:5-1:100, adopts this proportioningParameter can ensure effectively peeling off of quasiflake graphite alkene aggregation, is conducive to improve filling that quasiflake graphite alkene aggregation peels offDivide degree.
Four, in the present invention, due to the height of ultrasonic frequency, to peel off influential effect larger to ultrasonic, and frequency is lower, ultrasonicCavitation is stronger, easily cause sheet damage layer, and noise is larger; Frequency is higher, and that ultrasound waves is about is short, energy is more concentrated,But in stripper, energy attenuation is large, operating distance is shorter, cavitation intensity a little less than, charge stripping efficiency is also lower. Therefore adopt superFrequency of sound wave is that the ultrasound wave vibrating bar of 25-40KHz is peeled off Graphene, can ensure to peel off better effects and if speed is peeled off in guaranteeSpend faster.
Five, in the present invention, tank body is set to circle, and radiation effect is identical everywhere to inner tank wall to have ultrasound wave vibrating barAdvantage, be conducive to improve and peel off effect; Many ultrasound wave vibrating bars in tank body are polycyclic and divide in same frontal plane of projectionCloth, has further improved the effect of Omnidirectional radiation tank interior and has further improved hyperacoustic power density, also simultaneouslyImprove the single batch of amount of peeling off material.
Six, in the present invention, many vertical layered being arranged in tank body of ultrasound wave vibrating bar, and ultrasound wave vibrating bar on every ringQuantity be the integral multiple of the ultrasound wave vibrating bar number of plies, this structure makes the ultrasonic radiation effect of ultrasound wave vibrating bar in tank bodyBetter with stability, improve the quality of peeling off effect and final products obtained therefrom of material. With China Patent No. beThe prior art that " 201320116823.1 " are representative is compared, and the structure that ultrasound wave vibrating bar layering arranges not only further increasesThe single batch of amount of peeling off material, also reduced volume and the floor space of tank body, have easy for installation and practical excellentPoint. And the lower end of upper strata ultrasound wave vibrating bar is crossing with the upper end dislocation of lower floor ultrasound wave vibrating bar, can avoid at tank bodyInterior appearance is without the white space of ultrasonic radiation.
Seven,, in the present invention, every layer of ultrasound wave vibrating bar is evenly arranged at the structure in tank body, make tank body internal upper part, inThe ultrasonic radiation effect of portion and bottom is identical, in the time of scale material handling, and can be fully that material is complete at short noticePeel off, be conducive to improve the quality of Graphene product.
Eight,, in the present invention, compressed air, by being arranged on the nozzle ejection on inner tank wall and bottom, has stirring effectGet well and the fast advantage of agitation speed.
Nine, adopt after the present invention, can obtain the high-quality graphene product that single batch of output reaches hundreds of kilograms.
Brief description of the drawings
Fig. 1 is the main TV structure schematic diagram of tank body in embodiment 8;
Fig. 2 is the plan structure schematic diagram of tank body in embodiment 8;
Fig. 3 is the structural representation of ultrasound wave vibrating bar in embodiment 8;
In figure, be labeled as: 1, tank body, 2, ultrasound wave vibrating bar, 3, nozzle, 4, wedged bottom, 5, cover plate, 6, steel pipe.
Detailed description of the invention
Embodiment 1
Prepare a method for Graphene, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, instituteState liquid phase expansion process operation and expand for graphite intercalation compound is placed in expansion solutions, finally obtain quasiflake graphite alkene poly-Collective; Described ultrasonic wave stripping process be first by water and quasiflake graphite alkene aggregation in mass ratio for the ratio of 5:1 joinsBe provided with in the tank body 1 of many ultrasound wave vibrating bars 2, then pass into the stirring of compressed air bubbling in tank body 1, make quasiflake graphiteAlkene aggregation comparatively equably dispersion suspension in stripper, and then to control ultrasonic frequency be 25KHz ultrasonic vibrationRod 2 sonic oscillations are processed 0.5 hour, finally obtain cotton-shaped graphene suspension; Described drying process for adopt expansion drying orCryodesiccated method is removed the moisture in cotton-shaped graphene suspension, finally obtains graphene powder. The experiment proved that this realityExecute example and adopt after said method, in gained graphene powder, the number of plies of graphene film concentrates on 3-8 layers, and impurity content is 2.0
wt%。
Embodiment 2
Prepare a method for Graphene, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, instituteState liquid phase expansion process operation and expand for graphite intercalation compound is placed in expansion solutions, finally obtain quasiflake graphite alkene poly-Collective; Described ultrasonic wave stripping process be first by complex liquid and quasiflake graphite alkene aggregation in mass ratio for the ratio of 5:1 addsEnter to being provided with in the tank body 1 of many ultrasound wave vibrating bars 2, then pass into the stirring of compressed air bubbling in tank body 1, make vermiformGraphene aggregation comparatively equably dispersion suspension in stripper, and then to control ultrasonic frequency be 28KHz ultrasonic waveVibrating head 2 sonic oscillations are processed 1 hour, finally obtain cotton-shaped graphene suspension; Described drying process is for adopting expansion dryingOr cryodesiccated method removes the moisture in cotton-shaped graphene suspension, finally obtain graphene powder. Wherein, complex liquid isEvenly mixed by mass percentage by following component: complexing of metal ion agent 20%, surface tension modifier 4%, all the other areWater, further, described complexing of metal ion agent is evenly to be mixed by sodium potassium tartrate tetrahydrate and sodium pyrophosphate, surface tension agentEvenly to be mixed by methyl alcohol and ethanol. The experiment proved that, the present embodiment adopts after said method, gained graphene powderIn, the number of plies of graphene film concentrates on 3-8 layers, and impurity content is 1.8 wt%.
Embodiment 3
Prepare a method for Graphene, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, instituteState liquid phase expansion process operation and expand for graphite intercalation compound is placed in expansion solutions, finally obtain quasiflake graphite alkene poly-Collective; Described ultrasonic wave stripping process be first by complex liquid and quasiflake graphite alkene aggregation in mass ratio for the ratio of 10:1 addsEnter to being provided with in the tank body 1 of many ultrasound wave vibrating bars 2, then pass into the stirring of compressed air bubbling in tank body 1, make vermiformGraphene aggregation comparatively equably dispersion suspension in stripper, and then to control ultrasonic frequency be 30KHz ultrasonic waveVibrating head 2 sonic oscillations are processed 6 hours, finally obtain cotton-shaped graphene suspension; Described drying process is for adopting expansion dryingOr cryodesiccated method removes the moisture in cotton-shaped graphene suspension, finally obtain graphene powder. Wherein, complex liquid isEvenly mixed by mass percentage by following component: complexing of metal ion agent 15%, surface tension modifier 5%, all the other areWater, further, described complexing of metal ion agent is evenly to be mixed by disodium edta and gluconic acid sodium salt, tableSurface tension conditioning agent is evenly to be mixed by propyl alcohol and lauryl sodium sulfate. The experiment proved that, the present embodiment adopts above-mentionedAfter method, in gained graphene powder, the number of plies of graphene film concentrates on 2-7 layers, and impurity content is 2.0 wt%.
Embodiment 4
Prepare a method for Graphene, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, instituteState liquid phase expansion process operation and expand for graphite intercalation compound is placed in expansion solutions, finally obtain quasiflake graphite alkene poly-Collective; Described ultrasonic wave stripping process be first by complex liquid and quasiflake graphite alkene aggregation in mass ratio for the ratio of 30:1 addsEnter to being provided with in the tank body 1 of many ultrasound wave vibrating bars 2, then pass into the stirring of compressed air bubbling in tank body 1, make vermiformGraphene aggregation comparatively equably dispersion suspension in stripper, and then to control ultrasonic frequency be 32KHz ultrasonic waveVibrating head 2 sonic oscillations are processed 10 hours, finally obtain cotton-shaped graphene suspension; Described drying process is for adopting expansion dryingOr cryodesiccated method removes the moisture in cotton-shaped graphene suspension, finally obtain graphene powder. Wherein, complex liquid isEvenly mixed by mass percentage by following component: complexing of metal ion agent 12%, surface tension modifier 3%, all the other areWater, further, described complexing of metal ion agent is evenly to be mixed by ethylenediamine tetraacetic methene sodium phosphate and oxalic acid, surfacePower conditioning agent is neopelex. The experiment proved that, the present embodiment adopts after said method, gained graphene powderIn, the number of plies of graphene film concentrates on 1-6 layers, and impurity content is 1.5 wt%.
Embodiment 5
Prepare a method for Graphene, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, instituteState liquid phase expansion process operation and expand for graphite intercalation compound is placed in expansion solutions, finally obtain quasiflake graphite alkene poly-Collective; Described ultrasonic wave stripping process be first by complex liquid and quasiflake graphite alkene aggregation in mass ratio for the ratio of 50:1 addsEnter to being provided with in the tank body 1 of many ultrasound wave vibrating bars 2, then pass into the stirring of compressed air bubbling in tank body 1, make vermiformGraphene aggregation comparatively equably dispersion suspension in stripper, and then to control ultrasonic frequency be 34KHz ultrasonic waveVibrating head 2 sonic oscillations are processed 13 hours, finally obtain cotton-shaped graphene suspension; Described drying process is for adopting expansion dryingOr cryodesiccated method removes the moisture in cotton-shaped graphene suspension, finally obtain graphene powder. Wherein, complex liquid isEvenly mixed by mass percentage by following component: complexing of metal ion agent 8%, surface tension modifier 2%, all the other areWater, further, described complexing of metal ion agent is evenly to be mixed by oxalates and diethanol amine, surface tension modifierFor softex kw. The experiment proved that, the present embodiment adopts after said method, in gained graphene powder, and stoneThe number of plies of China ink alkene sheet concentrates on 1-5 layers, and impurity content is 1.4 wt%.
Embodiment 6
Prepare a method for Graphene, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, instituteState liquid phase expansion process operation and expand for graphite intercalation compound is placed in expansion solutions, finally obtain quasiflake graphite alkene poly-Collective; Described ultrasonic wave stripping process be first by complex liquid and quasiflake graphite alkene aggregation in mass ratio for the ratio of 50:1 addsEnter to being provided with in the tank body 1 of many ultrasound wave vibrating bars 2, then pass into the stirring of compressed air bubbling in tank body 1, make vermiformGraphene aggregation comparatively equably dispersion suspension in stripper, and then to control ultrasonic frequency be 36KHz ultrasonic waveVibrating head 2 sonic oscillations are processed 17 hours, finally obtain cotton-shaped graphene suspension; Described drying process is for adopting expansion dryingOr cryodesiccated method removes the moisture in cotton-shaped graphene suspension, finally obtain graphene powder. Wherein, complex liquid isEvenly mixed by mass percentage by following component: complexing of metal ion agent 8%, surface tension modifier 2%, all the other areWater, further, described complexing of metal ion agent is evenly to be mixed by oxalates and diethanol amine, surface tension modifierFor softex kw. The experiment proved that, the present embodiment adopts after said method, in gained graphene powder, and stoneThe number of plies of China ink alkene sheet concentrates on 1-5 layers, and impurity content is 1.2 wt%.
Embodiment 7
Prepare a method for Graphene, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, instituteState liquid phase expansion process operation and expand for graphite intercalation compound is placed in expansion solutions, finally obtain quasiflake graphite alkene poly-Collective; Described ultrasonic wave stripping process is to be first the ratio of 100:1 in mass ratio by complex liquid and quasiflake graphite alkene aggregationJoin in the tank body 1 that is provided with many ultrasound wave vibrating bars 2, then pass into the stirring of compressed air bubbling in tank body 1, make wormDispersion suspension is in stripper comparatively equably for shape Graphene aggregation, and then that to control ultrasonic frequency be 40KHz is ultrasonicRipple vibrating head 2 sonic oscillations are processed 20 hours, finally obtain cotton-shaped graphene suspension; Described drying process is for adopting flash distillation dryDry or cryodesiccated method is removed the moisture in cotton-shaped graphene suspension, finally obtains graphene powder. Wherein, complex liquidEvenly to be mixed by mass percentage by following component: complexing of metal ion agent 5%, surface tension modifier 1%, all the other areWater, further, described complexing of metal ion agent is triethanolamine, surface tension agent is fluorocarbon surfactant. Through experiment cardBright, the present embodiment adopts after said method, and in gained graphene powder, the number of plies of graphene film concentrates on 1-3 layers, and impurity containsAmount is 1.0 wt%.
Embodiment 8
Prepare a method for Graphene, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, instituteStating ultrasonic wave stripping process is that the quasiflake graphite alkene aggregation first obtaining by stripper with through liquid phase expansion process adds in proportionEnter to being provided with in the tank body 1 of many ultrasound wave vibrating bars 2, then pass into the stirring of compressed air bubbling in tank body 1, make vermiformGraphene aggregation dispersion suspension is in stripper, and then it is little to control ultrasound wave vibrating bar 2 sonic oscillations processing 0.5-20Time, finally obtain cotton-shaped graphene suspension.
In the present embodiment, described tank body 1 is circular, and the bottom surface of circular tank 1 is wedged bottom 4, and is arranged in circular tank 1Many ultrasound wave vibrating bars 2 in same frontal plane of projection, be polycyclic distribute.
In the present embodiment, many vertical layered being arranged in tank body 1 of ultrasound wave vibrating bar 2, every layer of ultrasound wave vibrating bar 2Quantity is all identical, and the ultrasound wave vibrating bar 2 of every layer evenly arranges in tank body 1, and on every ring, the quantity of ultrasound wave vibrating bar 2 is superThe integral multiple of acoustic vibration rod 2 numbers of plies. Such set-up mode can not only make ultrasound wave vibrating bar 2 homogeneous radiation tank body 1 inside,Avoid occurring the white space without ultrasonic radiation, can also reduce the internal diameter of tank body 1, reduce with the height that increases tank body 1The internal diameter of tank body 1, is conducive to reduce the floor space of whole tank body 1.
Further, preferably the number of plies of the interior ultrasound wave vibrating bar 2 of tank body 1 is 4 layers, certainly, and according to the preparation rule of GrapheneMould difference, the degree of depth of the interior ultrasound wave vibrating bar 2 of tank body 1 and the number of plies also can be according to actual conditions settings.
In the present embodiment, due to ultrasound wave vibrating bar 2 be radially 360 degree without dead angle radiation, therefore in order to prevent in tank body 1Occur without the white space of ultrasonic radiation, need to be by the lower end of upper strata ultrasound wave vibrating bar 2 and lower floor's ultrasound wave vibrating bar 2 upperEnd dislocation is intersected.
In the present embodiment, because material enters in tank body 1 from tank body 1 top, cause the material density at the interior liquid level of tank body 1 placeBe greater than the material density at tank body 1 bottom place, in order to ensure fully peeling off of material, preferably increase many at place of the interior the superiors of tank body 1Individual ultrasound wave vibrating bar 2, the ultrasound wave vibrating bar 2 of these increases is evenly arranged in tank body 1 equally circlewise.
In the present embodiment, in order to facilitate tank body 1 fixing, be provided with hangers in tank body 1 surrounding.
For the set-up mode of the interior ultrasound wave vibrating bar 2 of tank body 1 can be clearly described, below with ultrasound wave vibrating bar 2The number of plies is 4 layers, and the number of rings in same frontal plane of projection is that 2 rings are example, as shown in Figure 2, and ultrasound wave vibrating bar 2 quantity on interior ringBe 4, ultrasound wave vibrating bar 2 quantity on outer shroud are 24, and on interior ring and outer shroud, the quantity of ultrasound wave vibrating bar 2 is ultrasonic waveThe integral multiple of vibrating head 2 numbers of plies. Wherein, 4 ultrasound wave vibrating bar 2 correspondences on interior ring are distributed in 4 layers in tank body 1, outer shroudOn 24 ultrasound wave vibrating bars 2 be distributed in tank body 1 in the mode of every 6 corresponding one decks equally, and at same frontal plane of projectionIn, the ultrasound wave vibrating bar 2 on ring is arranged in order by the number of plies, in 4 ultrasound wave vibrating bars 2 on ring successively by the 1st layer, theThe order of 2 layers, the 3rd layer and the 4th layer is arranged, and 24 ultrasound wave vibrating bars 2 on outer shroud are successively by 1 layer, the 2nd layer, the 3rd layer and the4 layers of order continue to arrange. The ultrasonic radiation effect that so just can ensure tank body 1 interior each region is more even.
Further, because the material density at the interior liquid level of tank body 1 place is greater than the material density at tank body 1 bottom place, in order to protectFully peeling off of exhibit material preferably increases at least 4 ultrasound wave vibrating bars 2 in tank body 1 between the outer shroud of the 1st layer and interior ring,Ensure that material can be fully stripped.
In the present embodiment, described compressed air sprays by the nozzle 3 being arranged on tank body 1 inwall and bottom.
In the present embodiment, described ultrasound wave vibrating bar 2 is dumbbell rod type tubular ultrasonic radiator in prior art, installsTime, ultrasound wave vibrating bar 2 is fixed on the cover plate 5 of tank body 1 by steel pipe 6.
Claims (8)
1. prepare a method for Graphene, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, its spyLevy and be: described ultrasonic wave stripping process is the quasiflake graphite alkene aggregation first obtaining by stripper with through liquid phase expansion processJoin in proportion in the tank body (1) that is provided with many ultrasound wave vibrating bars (2), then pass into compressed air drum in tank body (1)Bubble stirs, and makes quasiflake graphite alkene aggregation dispersion suspension in stripper, and then controls ultrasound wave vibrating bar (2) Under Ultrasonic VibrationSwing and process 0.5-20 hours, finally obtain cotton-shaped graphene suspension;
Described tank body (1) is circular, is arranged on the interior many ultrasound wave vibrating bars (2) of circular tank (1) at same frontal plane of projectionInside being polycyclic distributes.
2. a kind of method of preparing Graphene as claimed in claim 1, is characterized in that: described stripper is water or compoundLiquid, described complex liquid is that following component is evenly mixed by mass percentage: complexing of metal ion agent 5-20 %, surfaceTension regulator 1-5 %, all the other are water.
3. a kind of method of preparing Graphene as claimed in claim 2, is characterized in that: the metal ion in described complex liquidComplexing agent is sodium potassium tartrate tetrahydrate, sodium pyrophosphate, disodium edta, gluconic acid sodium salt, ethylenediamine tetraacetic methene sodium phosphate, grassOne or more in acid, oxalates, diethanol amine, triethanolamine compound, surface tension modifier is methyl alcohol, ethanol, thirdIn alcohol, lauryl sodium sulfate, neopelex, softex kw, fluorocarbon surfactant oneKind or multiple compound.
4. a kind of method of preparing Graphene as described in any one in claim 1-3, is characterized in that: described tank body (1)The mass ratio of interior quasiflake graphite alkene aggregation and stripper is 1:5-1:100.
5. a kind of method of preparing Graphene as described in any one in claim 1-3, is characterized in that: described ultrasonic waveThe ultrasonic frequency of vibrating head (2) is 25-40KHz, and the sonic oscillation processing time of described ultrasound wave vibrating bar (2) is 6-13Hour.
6. a kind of method of preparing Graphene as claimed in claim 1, is characterized in that: many described ultrasound wave vibrating bars(2) vertical layered being arranged in tank body (1), the lower end of upper strata ultrasound wave vibrating bar (2) and lower floor's ultrasound wave vibrating bar (2) upperEnd dislocation is intersected, and on every ring, the quantity of ultrasound wave vibrating bar (2) is the integral multiple of ultrasound wave vibrating bar (2) number of plies.
7. a kind of method of preparing Graphene as claimed in claim 6, is characterized in that: in described tank body (1) every layer ultrasonicThe quantity of ripple vibrating head (2) is all identical, and the ultrasound wave vibrating bar of every layer (2) evenly arranges in tank body (1).
8. a kind of method of preparing Graphene as described in any one in claim 1,6 or 7, is characterized in that: described compressionAir is by being arranged on nozzle (3) ejection on tank body (1) inwall and bottom.
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Families Citing this family (7)
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| CN105601154B (en) * | 2015-12-28 | 2017-08-04 | 四川碳世界科技有限公司 | A kind of graphene reinforcing agent and preparation method thereof |
| CN105523549B (en) * | 2016-01-28 | 2017-10-27 | 成都新柯力化工科技有限公司 | A kind of remover and application that graphene is prepared for mechanical stripping method |
| CN105819437B (en) * | 2016-05-06 | 2018-01-30 | 成都新柯力化工科技有限公司 | A kind of method that scale cleaning prepares graphene |
| CN106672949A (en) * | 2016-11-29 | 2017-05-17 | 上海利物盛纳米科技有限公司 | Method for preparing graphene by assisting in stripping graphite based on gas solubilization |
| CN107673335B (en) * | 2017-01-04 | 2019-03-05 | 柯良节 | Graphene preparation method based on the reaction of multiphase quantum self coupling |
| CN109502580B (en) * | 2018-12-07 | 2021-01-22 | 四川聚创石墨烯科技有限公司 | Purification device of graphene oxide |
| CN109553094A (en) * | 2019-01-03 | 2019-04-02 | 深圳天元羲王材料科技有限公司 | A kind of grapheme platelet liquid phase ultrasonic dispersing method |
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| US8501318B2 (en) * | 2008-09-03 | 2013-08-06 | Nanotek Instruments, Inc. | Dispersible and conductive nano graphene platelets |
| CN102431999B (en) * | 2011-09-22 | 2014-07-02 | 中国科学院金属研究所 | Method for preparing high-quality graphene |
| CN203128206U (en) * | 2013-03-14 | 2013-08-14 | 上海第二工业大学 | Intercalation peeling device for graphene preparation |
| CN104477892B (en) * | 2014-12-12 | 2016-08-24 | 盐城市新能源化学储能与动力电源研究中心 | Flaky graphite alkene device prepared by the preparation method of a kind of flaky graphite alkene and use the method |
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2015
- 2015-04-20 CN CN201510186512.6A patent/CN104843688B/en active Active
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