CN104843688A - Graphene preparation method - Google Patents
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- CN104843688A CN104843688A CN201510186512.6A CN201510186512A CN104843688A CN 104843688 A CN104843688 A CN 104843688A CN 201510186512 A CN201510186512 A CN 201510186512A CN 104843688 A CN104843688 A CN 104843688A
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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 field of graphene, relate in particular to a kind of method preparing Graphene.
Background technology
Since being found from 2004, Graphene receives much concern as a kind of new carbon.It is a kind of completely by
sp 2 the thickness of the carbon atom formation of hydridization is only the accurate two dimensional crystal material of monoatomic layer or several monoatomic layer, there is the performance that high light transmittance and electroconductibility, high-specific surface area, high strength and snappiness etc. are excellent, be expected to obtain widespread use in fields such as high-performance nanometer electronic device, photoelectric device, gas sensor, matrix material, field emmision material and stored energies.
At present, the preparation method of Graphene has a variety of, wherein " liquid phase expansion stripping method " is a kind of low cost, quality controllable, and be easy to industrialized preparation method, the method is mainly raw material with graphite intercalation compound, peel off through liquid phase expansion process, ultrasonic wave and after drying treatment three operations, finally obtain graphene powder.As China Patent No. " 201110282370.5 " disclosed " a kind of method preparing high-quality graphene " on May 2nd, 2012, its technical scheme be first with halogen or the metal halide graphite intercalation compound that is intercalator for raw material, the quasiflake graphite alkene aggregate that expansion process obtains high level expansion is carried out in oxalic acid or superoxol, then quasiflake graphite alkene aggregate is carried out ultrasonic oscillation process in the aqueous solution or organic solvent solution of organic solvent or various tensio-active agent, thus obtain high-quality graphene.In actual fabrication process, the effect that ultrasonic wave is peeled off is by the quality of the peeling effect and final products obtained therefrom that directly affect quasiflake graphite alkene aggregate, but there is not the concrete stripping means of quasiflake graphite alkene aggregate in prior art, cause the stripping process of quasiflake graphite alkene aggregate uncontrolled, be unfavorable for the stripping of quasiflake graphite alkene aggregate.
In addition, although China Patent No. " 201320116823.1 " disclosed " a kind of Graphene preparation intercalation peel-off device " on August 14th, 2013, its technical scheme is that described equipment comprises ultrasonic generator, ultrasonic wave dispersion tank and the whipping appts for disperseing the graphite suspension in dispersion tank, described whipping appts comprises agitator motor, stir turning axle and stir rotating paddle, stir turning axle one end and connect agitator motor the other end connection stirring rotating paddle, the sidewall of described ultrasonic wave dispersion tank is provided with a plurality of ultrasonic transducer, the bottom of ultrasonic wave dispersion tank presents doline, bottom is provided with discharge gate, discharge gate is provided with drainage conduit, drainage conduit is provided with and opens valve, whole Graphene preparation intercalation peel-off device is placed in frame, ultrasonic generator electricity being converted to the high-frequency ac electrical signal matched with ultrasonic transducer is connected with ultrasonic transducer by cable.But with the prior art that this patent document is representative, in actual use, still there is following defect: one, ultrasonic transducer is arranged on the outer wall of hexahedron structure tank body, each transverter is different to the distance at tank body center, cause the cavitation effect in each region in tank body uneven, not only affect the peeling effect of Graphene, also reduce the utilization ratio of Graphene raw material and the quality of graphene product.Two, ultrasonic transducer is arranged on the outer wall of tank body, and because hyperacoustic swept area is limited, this structural limitations size of tank body, causes using the ultrasonic stripping off device of this structure certainly will can not prepare graphene product on a large scale.Three, the transverter in this patent forms vibration plate by being bonded on tank wall, when Graphene prepared on a large scale by needs, every one side of tank body needs sticky dozens or even hundreds of transverter, because the swept area of each transverter is little, this mode not only increases the volume of equipment, also there is peeling effect difference, poor stability and awkward shortcoming, be 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 method preparing Graphene is provided, the present invention can make quasiflake graphite alkene aggregate be distributed in stripping liquid comparatively equably, thus reaches the object improving peeling effect and reduce splitting time simultaneously.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of method preparing Graphene, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, it is characterized in that: described ultrasonic wave stripping process is first by stripping liquid with join in proportion through the quasiflake graphite alkene aggregate that liquid phase expansion process obtains and be provided with in the tank body of many ultrasound wave vibrating bars, pressurized air burst agitation is passed into again in tank body, make quasiflake graphite alkene aggregate dispersion suspension in stripping liquid, and then control ultrasound wave vibrating bar sonic oscillation process 0.5-20 hours, finally obtain cotton-shaped graphene suspension.
Described stripping liquid is water or complex liquid, described complex liquid be by following component by mass percentage Homogeneous phase mixing form: 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 one or more the compound in Seignette salt, trisodium phosphate, disodium edta, Sunmorl N 60S, ethylenediamine tetraacetic methene sodium phosphate, oxalic acid, oxalate, diethanolamine, trolamine, and surface tension modifier is one or more the compound in methyl alcohol, ethanol, propyl alcohol, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide, fluorocarbon surfactant.
In described tank body, the mass ratio of quasiflake graphite alkene aggregate and stripping liquid is 1:5-1:100.
The ultrasonic frequency of described ultrasound wave vibrating bar is 25-40KHz, and the sonic oscillation treatment time of described ultrasound wave vibrating bar is 6-13 hours.
Described tank body is circular, is arranged on the many ultrasound wave vibrating bars distribution in polycyclic in same frontal plane of projection in circular tank.
Many described ultrasound wave vibrating bars are vertical layered to be arranged in tank body, and the lower end of upper strata ultrasound wave vibrating bar misplaces crossing with the upper end of lower floor's ultrasound wave vibrating bar, and on every ring, the quantity of ultrasound wave vibrating bar is the integral multiple of the ultrasound wave vibrating bar number of plies.
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 is evenly arranged in tank body.
Described pressurized 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 is before startup ultrasound wave vibrating bar carries out ultrasonic wave stripping, by pressurized air, agitation treatment is carried out to the quasiflake graphite alkene aggregate in tank body and stripping liquid in advance, this just can make quasiflake graphite alkene aggregate be distributed to comparatively equably in stripping liquid, thus reach the object improving peeling effect and reduce splitting time simultaneously, both improve the utilization ratio of raw material, turn improve the quality of obtained graphene product.
Two, in the present invention, stripping liquid both can be water, can be also complex liquid, when stripping liquid is water, had the advantage reducing production cost; When stripping liquid is complex liquid, complexing of metal ion agent in complex liquid can adsorb the metal ion be dissolved in solution, it is made to lose catalytic activity, surface tension modifier in complex liquid then can adjust the wetting property of stripping liquid to graphite and Graphene, to promote that swelling agent is to the diffusion of graphite layers, and then strengthen peeling effect.Compared with prior art, adopt the complex liquid of specific components that the final graphene product number of plies obtained can be made lower than 10 layers, and mostly concentrate on 1-5 layers, the trash content of graphene product, lower than 2%, improves the quality of product.
Three, in the present invention, the mass ratio of quasiflake graphite alkene aggregate and stripping liquid is 1:5-1:100, adopts this proportioning parameter can ensure effective stripping of quasiflake graphite alkene aggregate, is conducive to the abundant degree improving the stripping of quasiflake graphite alkene aggregate.
Four, in the present invention, because the height of ultrasonic frequency is comparatively large on ultrasonic peeling effect impact, frequency is lower, and ultrasonic cavitation is stronger, easily cause sheet damage layer, and noise is larger; Frequency is higher, ultrasound waves be about short, energy is more concentrated, but in stripping liquid, energy decrement is comparatively large, operating distance is shorter, cavitation intensity is more weak, and charge stripping efficiency is also lower.Therefore employing ultrasonic frequency is the ultrasound wave vibrating bar stripping Graphene of 25-40KHz, can ensure that peeling effect is better and ensure that peeling rate is faster.
Five, in the present invention, tank body is set to circle, has ultrasound wave vibrating bar to the inner tank wall advantage that radiation effect is identical everywhere, is conducive to improving peeling effect; Many ultrasound wave vibrating bars in tank body are the distribution in polycyclic in same frontal plane of projection, further increases the effect of Omnidirectional radiation tank interior and further increases hyperacoustic power density, also improves the amount that single batch is peeled off material simultaneously.
Six, in the present invention, many ultrasound wave vibrating bars are vertical layered to be arranged in tank body, and the quantity of ultrasound wave vibrating bar is the integral multiple of the ultrasound wave vibrating bar number of plies on every ring, this structure make the ultrasonic radiation effect of ultrasound wave vibrating bar in tank body and stability better, improve the peeling effect of material and the quality of final products obtained therefrom.Compared with the prior art be " 201320116823.1 " with China Patent No. being representative, the structure that ultrasound wave vibrating bar layering is arranged not only further increases the amount that single batch is peeled off material, also reduce volume and the floor space of tank body, there is easy for installation and practical advantage.And the lower end of upper strata ultrasound wave vibrating bar misplaces crossing with the upper end of lower floor ultrasound wave vibrating bar, then can avoid the white space occurred in tank body without ultrasonic radiation.
Seven, in the present invention; every layer of ultrasound wave vibrating bar is evenly arranged at the structure in tank body, makes tank body internal upper part, middle part identical with the ultrasonic radiation effect of bottom, namely when mass-producing material handling; fully material can be peeled off completely at short notice, be conducive to the quality improving graphene product.
Eight, in the present invention, pressurized air, by being arranged on the nozzle ejection on inner tank wall and bottom, has the advantage that stirring effect is good and agitation speed is fast.
Nine, after adopting the present invention, the high-quality graphene product that single batch of turnout reaches hundreds of kilograms can be obtained.
Accompanying drawing explanation
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;
Be labeled as in figure: 1, tank body, 2, ultrasound wave vibrating bar, 3, nozzle, 4, wedged bottom, 5, cover plate, 6, steel pipe.
Embodiment
Embodiment 1
Prepare a method for Graphene, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, described liquid phase expansion process operation expands for being placed in expansion solutions by graphite intercalation compound, finally obtains quasiflake graphite alkene aggregate; Described ultrasonic wave stripping process is first be provided with in the tank body 1 of many ultrasound wave vibrating bars 2 for the ratio of 5:1 joins in mass ratio by water and quasiflake graphite alkene aggregate, pressurized air burst agitation is passed into again in tank body 1, make quasiflake graphite alkene aggregate comparatively equably dispersion suspension in stripping liquid, and then control the ultrasound wave vibrating bar 2 sonic oscillation process 0.5 hour that ultrasonic frequency is 25KHz, finally obtain cotton-shaped graphene suspension; Described drying process is the moisture that employing expansion drying or cryodesiccated method remove in cotton-shaped graphene suspension, finally obtains graphene powder.The experiment proved that, after the present embodiment adopts aforesaid method, in gained graphene powder, the number of plies of graphene film concentrates on 3-8 layers, and foreign matter 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, described liquid phase expansion process operation expands for being placed in expansion solutions by graphite intercalation compound, finally obtains quasiflake graphite alkene aggregate; Described ultrasonic wave stripping process is first be provided with in the tank body 1 of many ultrasound wave vibrating bars 2 for the ratio of 5:1 joins in mass ratio by complex liquid and quasiflake graphite alkene aggregate, pressurized air burst agitation is passed into again in tank body 1, make quasiflake graphite alkene aggregate comparatively equably dispersion suspension in stripping liquid, and then control the ultrasound wave vibrating bar 2 sonic oscillation process 1 hour that ultrasonic frequency is 28KHz, finally obtain cotton-shaped graphene suspension; Described drying process is the moisture that employing expansion drying or cryodesiccated method remove in cotton-shaped graphene suspension, finally obtains graphene powder.Wherein, complex liquid be by following component by mass percentage Homogeneous phase mixing form: complexing of metal ion agent 20%, surface tension modifier 4%, all the other are water, further, described complexing of metal ion agent is formed by Seignette salt and trisodium phosphate Homogeneous phase mixing, and surface tension agent is formed by methyl alcohol and ethanol Homogeneous phase mixing.The experiment proved that, after the present embodiment adopts aforesaid method, in gained graphene powder, the number of plies of graphene film concentrates on 3-8 layers, and foreign matter 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, described liquid phase expansion process operation expands for being placed in expansion solutions by graphite intercalation compound, finally obtains quasiflake graphite alkene aggregate; Described ultrasonic wave stripping process is first be provided with in the tank body 1 of many ultrasound wave vibrating bars 2 for the ratio of 10:1 joins in mass ratio by complex liquid and quasiflake graphite alkene aggregate, pressurized air burst agitation is passed into again in tank body 1, make quasiflake graphite alkene aggregate comparatively equably dispersion suspension in stripping liquid, and then control the ultrasound wave vibrating bar 2 sonic oscillation process 6 hours that ultrasonic frequency is 30KHz, finally obtain cotton-shaped graphene suspension; Described drying process is the moisture that employing expansion drying or cryodesiccated method remove in cotton-shaped graphene suspension, finally obtains graphene powder.Wherein, complex liquid be by following component by mass percentage Homogeneous phase mixing form: complexing of metal ion agent 15%, surface tension modifier 5%, all the other are water, further, described complexing of metal ion agent is formed by disodium edta and Sunmorl N 60S Homogeneous phase mixing, and surface tension modifier is formed by propyl alcohol and sodium lauryl sulphate Homogeneous phase mixing.The experiment proved that, after the present embodiment adopts aforesaid method, in gained graphene powder, the number of plies of graphene film concentrates on 2-7 layers, and foreign matter 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, described liquid phase expansion process operation expands for being placed in expansion solutions by graphite intercalation compound, finally obtains quasiflake graphite alkene aggregate; Described ultrasonic wave stripping process is first be provided with in the tank body 1 of many ultrasound wave vibrating bars 2 for the ratio of 30:1 joins in mass ratio by complex liquid and quasiflake graphite alkene aggregate, pressurized air burst agitation is passed into again in tank body 1, make quasiflake graphite alkene aggregate comparatively equably dispersion suspension in stripping liquid, and then control the ultrasound wave vibrating bar 2 sonic oscillation process 10 hours that ultrasonic frequency is 32KHz, finally obtain cotton-shaped graphene suspension; Described drying process is the moisture that employing expansion drying or cryodesiccated method remove in cotton-shaped graphene suspension, finally obtains graphene powder.Wherein, complex liquid be by following component by mass percentage Homogeneous phase mixing form: complexing of metal ion agent 12%, surface tension modifier 3%, all the other are water, further, described complexing of metal ion agent is formed by ethylenediamine tetraacetic methene sodium phosphate and oxalic acid Homogeneous phase mixing, and surface tension modifier is Sodium dodecylbenzene sulfonate.The experiment proved that, after the present embodiment adopts aforesaid method, in gained graphene powder, the number of plies of graphene film concentrates on 1-6 layers, and foreign matter 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, described liquid phase expansion process operation expands for being placed in expansion solutions by graphite intercalation compound, finally obtains quasiflake graphite alkene aggregate; Described ultrasonic wave stripping process is first be provided with in the tank body 1 of many ultrasound wave vibrating bars 2 for the ratio of 50:1 joins in mass ratio by complex liquid and quasiflake graphite alkene aggregate, pressurized air burst agitation is passed into again in tank body 1, make quasiflake graphite alkene aggregate comparatively equably dispersion suspension in stripping liquid, and then control the ultrasound wave vibrating bar 2 sonic oscillation process 13 hours that ultrasonic frequency is 34KHz, finally obtain cotton-shaped graphene suspension; Described drying process is the moisture that employing expansion drying or cryodesiccated method remove in cotton-shaped graphene suspension, finally obtains graphene powder.Wherein, complex liquid be by following component by mass percentage Homogeneous phase mixing form: complexing of metal ion agent 8%, surface tension modifier 2%, all the other are water, further, described complexing of metal ion agent is formed by oxalate and diethanolamine Homogeneous phase mixing, and surface tension modifier is cetyl trimethylammonium bromide.The experiment proved that, after the present embodiment adopts aforesaid method, in gained graphene powder, the number of plies of graphene film concentrates on 1-5 layers, and foreign matter 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, described liquid phase expansion process operation expands for being placed in expansion solutions by graphite intercalation compound, finally obtains quasiflake graphite alkene aggregate; Described ultrasonic wave stripping process is first be provided with in the tank body 1 of many ultrasound wave vibrating bars 2 for the ratio of 50:1 joins in mass ratio by complex liquid and quasiflake graphite alkene aggregate, pressurized air burst agitation is passed into again in tank body 1, make quasiflake graphite alkene aggregate comparatively equably dispersion suspension in stripping liquid, and then control the ultrasound wave vibrating bar 2 sonic oscillation process 17 hours that ultrasonic frequency is 36KHz, finally obtain cotton-shaped graphene suspension; Described drying process is the moisture that employing expansion drying or cryodesiccated method remove in cotton-shaped graphene suspension, finally obtains graphene powder.Wherein, complex liquid be by following component by mass percentage Homogeneous phase mixing form: complexing of metal ion agent 8%, surface tension modifier 2%, all the other are water, further, described complexing of metal ion agent is formed by oxalate and diethanolamine Homogeneous phase mixing, and surface tension modifier is cetyl trimethylammonium bromide.The experiment proved that, after the present embodiment adopts aforesaid method, in gained graphene powder, the number of plies of graphene film concentrates on 1-5 layers, and foreign matter 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, described liquid phase expansion process operation expands for being placed in expansion solutions by graphite intercalation compound, finally obtains quasiflake graphite alkene aggregate; Described ultrasonic wave stripping process is first be provided with in the tank body 1 of many ultrasound wave vibrating bars 2 for the ratio of 100:1 joins in mass ratio by complex liquid and quasiflake graphite alkene aggregate, pressurized air burst agitation is passed into again in tank body 1, make quasiflake graphite alkene aggregate comparatively equably dispersion suspension in stripping liquid, and then control the ultrasound wave vibrating bar 2 sonic oscillation process 20 hours that ultrasonic frequency is 40KHz, finally obtain cotton-shaped graphene suspension; Described drying process is the moisture that employing expansion drying or cryodesiccated method remove in cotton-shaped graphene suspension, finally obtains graphene powder.Wherein, complex liquid be by following component by mass percentage Homogeneous phase mixing form: complexing of metal ion agent 5%, surface tension modifier 1%, all the other are water, and further, described complexing of metal ion agent is trolamine, and surface tension agent is fluorocarbon surfactant.The experiment proved that, after the present embodiment adopts aforesaid method, in gained graphene powder, the number of plies of graphene film concentrates on 1-3 layers, and foreign matter content is 1.0 wt%.
Embodiment 8
A kind of method preparing Graphene, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, described ultrasonic wave stripping process is first by stripping liquid with join in proportion through the quasiflake graphite alkene aggregate that liquid phase expansion process obtains and be provided with in the tank body 1 of many ultrasound wave vibrating bars 2, pressurized air burst agitation is passed into again in tank body 1, make quasiflake graphite alkene aggregate dispersion suspension in stripping liquid, and then control ultrasound wave vibrating bar 2 sonic oscillation process 0.5-20 hours, 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 the many ultrasound wave vibrating bars 2 be arranged in circular tank 1 distribution in polycyclic in same frontal plane of projection.
In the present embodiment, many ultrasound wave vibrating bars 2 are vertical layered to be arranged in tank body 1, the quantity of every layer of ultrasound wave vibrating bar 2 is all identical, and the ultrasound wave vibrating bar 2 of every layer is evenly arranged in tank body 1, and on every ring, the quantity of ultrasound wave vibrating bar 2 is integral multiples of ultrasound wave vibrating bar 2 number of plies.Such set-up mode can not only make ultrasound wave vibrating bar 2 homogeneous radiation tank body 1 inner, avoid occurring the white space without ultrasonic radiation, the internal diameter of tank body 1 can also be reduced, namely reduce the internal diameter of tank body 1 with the height increasing tank body 1, be conducive to the floor space reducing whole tank body 1.
Further, in preferred tank body 1, the number of plies of ultrasound wave vibrating bar 2 is 4 layers, certainly, different according to the preparative-scale of Graphene, and in tank body 1, the degree of depth of ultrasound wave vibrating bar 2 and the number of plies also can be arranged according to practical situation.
In the present embodiment, due to ultrasound wave vibrating bar 2 be radial 360 degree without dead angle radiation, therefore in order to prevent the interior appearance of tank body 1 without the white space of ultrasonic radiation, need the lower end of upper strata ultrasound wave vibrating bar 2 to misplace crossing with the upper end of lower floor ultrasound wave vibrating bar 2.
In the present embodiment, because material enters in tank body 1 above tank body 1, the material density at liquid level place in tank body 1 is caused to be greater than the material density at place bottom tank body 1, in order to ensure the abundant stripping of material, preferably in tank body 1, place of the superiors increases multiple ultrasound wave vibrating bar 2, and these ultrasound wave vibrating bars 2 increased evenly are arranged in tank body 1 equally circlewise.
In the present embodiment, conveniently tank body 1 is fixed, and tank body 1 surrounding is provided with hangers.
In order to the set-up mode of ultrasound wave vibrating bar 2 in tank body 1 can be clearly described, it is 4 layers with the number of plies of ultrasound wave vibrating bar 2 below, number of rings in same frontal plane of projection is 2 rings is example, as shown in Figure 2, ultrasound wave vibrating bar 2 quantity in inner ring is 4, ultrasound wave vibrating bar 2 quantity on outer shroud is 24, and on inner ring and outer shroud, the quantity of ultrasound wave vibrating bar 2 is the integral multiple of ultrasound wave vibrating bar 2 number of plies.Wherein, 4 ultrasound wave vibrating bar 2 correspondences in inner ring are distributed in 4 layers in tank body 1,24 ultrasound wave vibrating bars 2 on outer shroud are distributed in tank body 1 in the mode of every 6 corresponding one decks equally, and in same frontal plane of projection, ultrasound wave vibrating bar 2 on ring is arranged in order by the number of plies, namely 4 ultrasound wave vibrating bars 2 in inner ring arrange by the order of the 1st layer, the 2nd layer, the 3rd layer and the 4th layer successively, and 24 ultrasound wave vibrating bars 2 on outer shroud continue arrangement by 1 layer, the 2nd layer, the 3rd layer and the 4th layer of order successively.This makes it possible to ensure that the ultrasonic radiation effect in each region in tank body 1 is more even.
Further, because the material density at liquid level place in tank body 1 is greater than the material density at place bottom tank body 1, in order to ensure the abundant stripping of material, preferably in tank body 1, increasing at least 4 ultrasound wave vibrating bars 2 between the outer shroud of the 1st layer and inner ring, ensureing that material can be fully stripped.
In the present embodiment, described pressurized air is sprayed by the nozzle 3 be 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, and during installation, ultrasound wave vibrating bar 2 is fixed on the cover plate 5 of tank body 1 by steel pipe 6.
Claims (9)
1. prepare the method for Graphene for one kind, comprise liquid phase expansion process operation, ultrasonic wave stripping process and drying process, it is characterized in that: described ultrasonic wave stripping process be first by stripping liquid and through the quasiflake graphite alkene aggregate that liquid phase expansion process obtains join in proportion be provided with many ultrasound wave vibrating bars (2) tank body (1) in, pressurized air burst agitation is passed into again in tank body (1), make quasiflake graphite alkene aggregate dispersion suspension in stripping liquid, and then control ultrasound wave vibrating bar (2) sonic oscillation process 0.5-20 hours, finally obtain cotton-shaped graphene suspension.
2. a kind of method preparing Graphene as claimed in claim 1, it is characterized in that: described stripping liquid is water or complex liquid, described complex liquid be by following component by mass percentage Homogeneous phase mixing form: complexing of metal ion agent 5-20 %, surface tension modifier 1-5 %, all the other are water.
3. a kind of method preparing Graphene as claimed in claim 2, it is characterized in that: the complexing of metal ion agent in described complex liquid is one or more the compound in Seignette salt, trisodium phosphate, disodium edta, Sunmorl N 60S, ethylenediamine tetraacetic methene sodium phosphate, oxalic acid, oxalate, diethanolamine, trolamine, and surface tension modifier is one or more the compound in methyl alcohol, ethanol, propyl alcohol, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide, fluorocarbon surfactant.
4. a kind of method preparing Graphene according to any one of claim 1-3, is characterized in that: the mass ratio of described tank body (1) interior quasiflake graphite alkene aggregate and stripping liquid is 1:5-1:100.
5. a kind of method preparing Graphene as described in claim 1,2 or 3, is characterized in that: the ultrasonic frequency of described ultrasound wave vibrating bar (2) is 25-40KHz, and the sonic oscillation treatment time of described ultrasound wave vibrating bar (2) is 6-13 hours.
6. a kind of method preparing Graphene as claimed in claim 1, is characterized in that: described tank body 1, for circular, is arranged on many ultrasound wave vibrating bars (2) distribution in polycyclic in same frontal plane of projection in circular tank (1).
7. a kind of method preparing Graphene as claimed in claim 6, it is characterized in that: described many ultrasound wave vibrating bars (2) are vertical layered to be arranged in tank body (1), the lower end of upper strata ultrasound wave vibrating bar (2) misplaces crossing with the upper end of lower floor's ultrasound wave vibrating bar (2), 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.
8. a kind of method preparing Graphene as claimed in claim 7, is characterized in that: in described tank body (1), the quantity of every layer of ultrasound wave vibrating bar (2) is all identical, and the ultrasound wave vibrating bar of every layer (2) is evenly arranged in tank body (1).
9. a kind of method preparing Graphene as described in claim 1,6,7 or 8, is characterized in that: described pressurized air is by being arranged on nozzle (3) ejection on tank body (1) inwall and bottom.
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| CN105601154A (en) * | 2015-12-28 | 2016-05-25 | 四川碳世界科技有限公司 | Graphene enhancer and preparation method thereof |
| CN105819437A (en) * | 2016-05-06 | 2016-08-03 | 成都新柯力化工科技有限公司 | Method for large-scale clean graphene preparation |
| 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 |
| CN107673335A (en) * | 2017-01-04 | 2018-02-09 | 柯良节 | Graphene preparation method based on the reaction of multiphase quantum self coupling |
| CN109502580A (en) * | 2018-12-07 | 2019-03-22 | 四川聚创石墨烯科技有限公司 | A kind of purification devices 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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| CN102431999A (en) * | 2011-09-22 | 2012-05-02 | 中国科学院金属研究所 | Method for preparing high-quality graphene |
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| CN107673335A (en) * | 2017-01-04 | 2018-02-09 | 柯良节 | Graphene preparation method based on the reaction of multiphase quantum self coupling |
| WO2018126780A1 (en) * | 2017-01-04 | 2018-07-12 | 柯良节 | Method for preparing graphene based on multi-phase quantum self-coupling reaction |
| CN109502580A (en) * | 2018-12-07 | 2019-03-22 | 四川聚创石墨烯科技有限公司 | A kind of purification devices of graphene oxide |
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