CN105329886A - Method for preparing graphene through composite shear stress stripping of vibrating screw extruder - Google Patents
Method for preparing graphene through composite shear stress stripping of vibrating screw extruder Download PDFInfo
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Abstract
The invention provides a method for preparing graphene through composite shear stress stripping of a vibrating screw extruder, and belongs to the field of graphene materials. According to the method, an electromagnetic, ultrasonic and longitudinal mechanical vibration tensile force field is introduced into the extruder rotating at high speed, the vibration tensile force field periodically changes along with the time to enable the graphite interface to be tensioned, graphite becomes loosened under the action of a stripping agent, the graphite generates powerful shearing stripping through contact interfaces of meshing blocks of the extruder in a tensioned state, thinner graphene with the narrower thickness distribution range is obtained, and then rapid and efficient high-quality graphene preparation under the high-shearing action is achieved. The method has the advantages that the production cost of the high-quality graphene is significantly lowered, the preparation process is green and environmentally friendly, no exhaust gas or waste liquid or waste residue is generated, and scale production of the graphene is promoted.
Description
Technical field
The present invention relates to grapheme material field, be specifically related to a kind of vibration screw extrusion press combination shearing stress that utilizes and peel off the method preparing Graphene.
Background technology
Graphene is a kind of monolayer carbon atomic plane material separated from graphite material, is the two-dirnentional structure of carbon.The thickness of this graphite crystal film only has 0.335 nanometer, and 200,000 Standard graphite alkene are superimposed together, and also only has a hairline so thick.After Graphene is found, due to the performance of its excellence, start application at numerous areas such as the energy, electronic material, biomedicine and environment protection, and its Application Areas is progressively expanded.
At present existing Graphene technology of preparing comprises mechanically peel method, substrate grows nonparasitically upon another plant method, chemical Vapor deposition process, oxidation reduction process, chemical cleavage method etc.The shortcoming of oxidation reduction process is that the Graphene prepared exists certain textural defect, causes Graphene part electrical property loss of energy, the application of Graphene is restricted; Graphene prepared by the Graphene relative mechanical stripping method of vapour deposition process gained is difficult to transfer, and does not find quantum hall effect in some use vapour deposition process gained Graphenes, illustrates that vapour deposition process may affect some characteristic of Graphene; Mechanically peel method can obtain individual layer or only have the graphene film of several atomic layer level thickness, is the effective ways obtaining low-cost and high-performance Graphene at present.
Obtained the Graphene of excellent performance by the gluing layer by layer stripping of micromechanics, but this technique means is difficult to realize volume production.And then have at present and obtain Graphene by the means of mechanical mill, mechanical mill relies on powerful mechanical shock to produce shear with the Van der Waals force overcome between graphite flake layer thus obtain Graphene.But due to very big to the surging force of graphite linings, make Graphene produce textural defect, reduce the size of Graphene after peeling off.Particularly because powerful mechanical shock makes graphite linings structure compacted, causing peeling off difficulty increases.Therefore occurred arranging by auxiliary agent and device peeling off.
Chinese invention patent application numbers 201310411516.0 discloses a kind of ball-milling preparation method of grapheme material, hexa-atomic to graphite carbon and alkyl aromatic ring or condensed ring polyether nonionic surfactant and deionized water mix and are loaded on ball grinder by this invention, within ball milling 5-30 hour, obtain Graphene; Chinese invention patent application numbers 201210046788.0 discloses a kind of preparation method of grapheme material, is dissolved in by powdered graphite in organic solvent or water, forms suspension, is ceaselessly engaged, ceaselessly tear graphite flake, prepare Graphene by wheel tooth; Chinese invention patent application numbers 201410567246.7 discloses a kind of eddy current type Graphene stripping off device, driving and rotates, making to form eddy current between shear-blade, realizing the stripping of Graphene by arranging driving mechanism.Chinese invention patent application numbers 201210038258.1 discloses a kind of electric field and peels off the method that intercalated graphite prepares Graphene, by muriate intercalated graphite, in alternating electric field, peels off intercalated graphite.
Above technique means accelerates stripping to a certain extent, but productive rate is low, and shearing force is weak, is difficult to the Van der Waals force overcoming graphite layers, and thus long reaction time, efficiency are low, and the Graphene number of plies particularly obtained is difficult to control.
Summary of the invention
In order to reduce the impact to graphite linings structure when high-shear is peeled off, improve the shearing peeling effect of graphite, the present invention proposes a kind of vibration screw extrusion press combination shearing stress that utilizes and peels off the method preparing Graphene.The method is by the intercalation pre-treatment to graphite; graphite is sent into the vibration screw extrusion press with the rotational shear field of force and the vibration drawing field of force; graphite is stretched while rotational shear is peeled off; overcome graphite linings compacted, achieve large-scale production high-quality graphene under high shear conditions..
For solving the problem, the present invention by the following technical solutions:
A kind of vibration screw extrusion press combination shearing stress that utilizes peels off the method preparing Graphene, it is characterized in that adopting the Vibration Extrusion machine with the rotational shear field of force and the vibration drawing field of force, graphite is stretched while rotational shear is peeled off, peel off graphite by combination shearing stress and obtain Graphene, comprise the steps:
(1) graphite and excessive intercalator are added to the water, homogenous disperse 10-25 minute, are then filtered dry obtain Graphite Cake with deionized water repetitive scrubbing;
(2) Graphite Cake step (1) is filtered dry under 80-120 DEG C of condition with stearate, stripper dispersing and mixing 30-45 minute, the mass ratio of Graphite Cake, stearate, stripper is 100:1-2:0.5-1;
(3) mixture step (2) obtained sends into vibration screw extrusion press, vibration screw extrusion press set temperature is 300-400 DEG C, rotating speed 500-1200rpm, by the high-speed revolution shearing field of force and the vibration drawing field of force, makes graphite be sheared stripping and obtains Graphene;
Described vibration screw extrusion press is the homodromal electromagnetic dynamic plasticizing extruder of multiscrew, ultrasonic vibration forcing machine or longitudinal mechanical vibration forcing machine, multiscrew refers to two and above screw rod, utilize in forcing machine gear block gap and there is the rotational shear field of force and the vibration drawing field of force simultaneously, rotational shear and vibrating motion achieve rapidly and efficiently to peel off prepares Graphene, overcomes Graphene, because of extruding, lattice imperfection occurs;
The screw rod of described vibration screw extrusion press is assembled with building blocks form by gear block, alternate angle wherein between gear block is 30 °, 45 °, 60 °, 90 °, reverse 30 °, reverse 45 °, reverse 60 °, the graphite conveying of 90 ° of gear blocks is zero, reverse gear block carries graphite in the other direction in shear history, postpone graphite to be fed forward, make graphite under shearing action and vibration drawing force field, periodically be sheared stripping, thus obtain the high-quality graphene that thickness is little, the number of plies is evenly distributed.
The impulsive magnetic field that described electromagnetic dynamic plasticizing extruder is produced by solenoid makes screw rod do pulsation rotation, and preferably, described electromagnetic dynamic plasticizing extruder vibrational frequency is 20-80Hz, and amplitude is 0.1-1mm.
Preferably, described electromagnetic dynamic plasticizing extruder is three screw rod electromagnetic dynamic plasticizing extruders in the same way.
Described ultrasonic vibration forcing machine is by introducing high-frequency ultrasonic, and utilize different Under Ultrasonic Vibration moving parts to obtain the periodic stretching field of force and shear, preferably, described ultrasonic vibration forcing machine, ultrasonic frequency is 20kHz, and power is at 2-3KW continuously adjustabe.
Described longitudinal mechanical vibration forcing machine, the rotation plug in extruder head arranges different frequency vibration, and preferably, described longitudinal mechanical vibration forcing machine, arranges frequency 50Hz, and amplitude is 1-3mm.
Described intercalator is C
12-C
18long-chain organic quaternary ammonium salt or C
12-C
18the organic diamine of long-chain.
Described stearate selects the one in sodium stearate, calcium stearate, Zinic stearas, Magnesium Stearate.
Described stripper selects the one in thionamic acid, Sunmorl N 60S, poly (sodium aspartate), diethyl thiourea.
Forcing machine is mechanical means conventional in a kind of plastic working, is widely used in the blended, filling-modified of polymkeric substance and extrusion moulding.Forcing machine continuous rotation Strong shear is relied on to make shear surface and graphite occur to shear to peel off and obtain Graphene.Regroup in order to avoid shearing graphite Graphene that is compacted or that peeled off in stripping at forcing machine, the present invention utilizes vibration screw extrusion press, the screw rod of this forcing machine except rotating, also have additional oscillator field, this oscillator field can make the material in screw rod be subject to combination shearing stress.Therefore, the forcing machine of high speed rotating produces powerful shearing at gear block contact interface, graphite is peeled off, simultaneously by introducing the vibration drawing field of force, the periodical change in time of this vibration drawing field of force, graphite interface is stretched, there is the rotational shear field of force and the vibration drawing field of force in graphite in forcing machine gear block gap simultaneously, combination shearing stress makes graphite not only become loose under stripper effect, and impel forcing machine to shear to separate thinner, that thickness distribution scope is less Graphene, thus overcome Graphene, because of extruding, lattice imperfection occurs.On the one hand, by arranging extruder screw gear block element, particularly in gear block district, the property performance period change of axial back lash, makes material while conveying, is subject to complicated shearing action, this shearing is different from grinding, but shears with material tangent plane direction; On the other hand, utilize the stretching in the additional field of force, eliminate the extruding between screw rod and barrel, graphite is stripped in a stretched state.
This by utilizing the high-shear of vibration screw extrusion press compound force field to peel off, effectively overcome the Van der Waals force of graphite layers, splitting time section, make to prepare Graphene technique simple, be easy to volume production, and by controlling the regulation and control that vibrational frequency and amplitude can realize the Graphene number of plies and size, for suitability for industrialized production Graphene provides a very feasible route.
The present invention adopts vibration screw extrusion press to prepare Graphene, with adopt at present that ball milling directly grinds, oxidization abrasive restores, liquid phase peels off and prepares compared with Graphene, all, thickness is thinner, and crystalline structure is more complete and orderly in the Graphene number of plies distribution that the inventive method obtains.Salient features contrast is as shown in table 1 below.
Table 1:
A kind of vibration screw extrusion press combination shearing stress that utilizes of the present invention peels off the method preparing Graphene, and compared with existing stripping graphite technology, its outstanding feature and excellent effect are:
1, shear by introducing the vibration drawing field of force in screw extrusion press, combination shearing stress avoids the compacted compacting of graphite, and graphite is peeled off by Strong shear under loose state, and the efficiency therefore peeled off is higher, and the Graphene thickness obtained is little, the number of plies is evenly distributed.
2, by adopting rotational shear and the vibration drawing field of force to shear, effectively prevent damage when mechanical shearing peels off graphite, graphene layer crystalline structure caused, saving the perfection of lattice of Graphene preferably.
3, peel off by vibration screw extrusion press the method preparing Graphene; achieve and prepare high-quality graphene fast, efficiently, considerably reduce the production cost of high-quality graphene, preparation process environmental protection; do not have waste gas, waste liquid, waste residue to produce, promoted the large-scale production of Graphene.
Accompanying drawing explanation
In order to understand rotational shear and the oscillator field tensile shear of vibration Screw Extrusion further, be described by diagram.
Fig. 1 is the schematic appearance of vibration screw extrusion press.1-drive-motor, 2-charging opening, 3-stretching vibration field device, 4-extruder screw.
Fig. 2 is that the part gear block of vibration screw extrusion press shears sketch.Graphite is by homodromal gear block strong shear, gear block alternate angle is 30 °, the direction of arrow is the additional stretching vibration field of force simultaneously, sheared by the rotational shear of gear block and the stretching field of force of applied vibration field, graphite is peeled off by Strong shear under loose state, therefore the efficiency peeled off is higher, and the Graphene thickness obtained is little, the number of plies is evenly distributed.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should be interpreted as scope of the present invention is only limitted to following example.When not departing from aforesaid method thought of the present invention, the various replacement made according to ordinary skill knowledge and customary means or change, all should be within the scope of the present invention.
embodiment 1
(1) by graphite and excessive intercalator C
12long-chain organic quaternary ammonium salt is added to the water, homogenous disperse 10 minutes, is then filtered dry obtains Graphite Cake with deionized water repetitive scrubbing;
(2) Graphite Cake step (1) is filtered dry under 80-120 DEG C of condition with sodium stearate, thionamic acid dispersing and mixing 30 minutes, the mass ratio of Graphite Cake, sodium stearate, thionamic acid is 100:1:0.5;
(3) mixture step (2) obtained sends into parallel dual-screw electromagnetic dynamic plasticizing extruder, and Vibration Extrusion machine set temperature is 300-400 DEG C, rotating speed 800rpm, and vibrational frequency is 80Hz, and amplitude is 0.1mm.Wherein extruder screw is 30 °, 45 °, 60 °, 90 °, reverse 30 °, reverse 45 °, reverse 60 ° by the alternate angle between gear block, by the high-speed revolution shearing field of force and the vibration drawing field of force, makes graphite be sheared stripping and obtains Graphene.
Analyze by detecting, the Graphene thickness that embodiment 1 obtains accounts for 80% within 3nm, and thickness accounts for 95% within 5nm, and the number of plies is evenly distributed.
embodiment 2
(1) by graphite and excessive intercalator C
16long-chain organic quaternary ammonium salt is added to the water, homogenous disperse 25 minutes, is then filtered dry obtains Graphite Cake with deionized water repetitive scrubbing;
(2) Graphite Cake step (1) is filtered dry under 80-120 DEG C of condition with calcium stearate, poly (sodium aspartate) dispersing and mixing 45 minutes, the mass ratio of Graphite Cake, calcium stearate, hard poly (sodium aspartate) is 100:1.5:1;
(3) mixture step (2) obtained sends into four screw rod ultrasonic vibration forcing machines in the same way, and Vibration Extrusion machine set temperature is 300-400 DEG C, rotating speed 1200rpm, and ultrasonic frequency is 20kHz, and power is at 2KW continuously adjustabe.By the high-speed revolution shearing field of force and the ultrasonic vibration stretching field of force, make graphite be sheared stripping and obtain Graphene.
embodiment 3
(1) by graphite and excessive intercalator C
18the organic diamine of long-chain is added to the water, homogenous disperse 10 minutes, is then filtered dry obtains Graphite Cake with deionized water repetitive scrubbing;
(2) Graphite Cake step (1) is filtered dry under 80-120 DEG C of condition with Zinic stearas, diethyl thiourea dispersing and mixing 35 minutes, the mass ratio of Graphite Cake, Zinic stearas, diethyl thiourea is 100:1:0.5;
(3) mixture step (2) obtained sends into the longitudinal mechanical vibration forcing machine of three screw rods in the same way, and Vibration Extrusion machine set temperature is 300-400 DEG C, and rotating speed 600rpm, arranges frequency 50Hz, and amplitude is 3mm.By the high-speed revolution shearing field of force and the vibration drawing field of force, make graphite be sheared stripping and obtain Graphene.
embodiment 4
(1) by graphite and excessive intercalator C
124the organic diamine of long-chain is added to the water, homogenous disperse 25 minutes, is then filtered dry obtains Graphite Cake with deionized water repetitive scrubbing;
(2) Graphite Cake step (1) is filtered dry under 80-120 DEG C of condition with Magnesium Stearate, Sunmorl N 60S dispersing and mixing 40 minutes, the mass ratio of Graphite Cake, Magnesium Stearate, Sunmorl N 60S is 100:2:1;
(3) mixture step (2) obtained sends into parallel dual-screw ultrasonic vibration forcing machine, Vibration Extrusion machine set temperature is 300-400 DEG C, rotating speed 500rpm, Vibration Extrusion machine is assembled with building blocks form by gear block, alternate angle wherein between gear block is 30 °, 45 °, 60 °, 90 °, reverse 30 °, reverse 45 °, reverse 60 °, the graphite conveying of 90 ° of gear blocks is zero, reverse gear block carries graphite in the other direction in shear history, postpone graphite to be fed forward, make graphite under shearing action and vibration drawing force field, periodically be sheared stripping, thus it is little to obtain thickness, the high-quality graphene that the number of plies is evenly distributed.
embodiment 5
(1) by graphite and excessive intercalator C
18long-chain organic quaternary ammonium salt is added to the water, homogenous disperse 20 minutes, is then filtered dry obtains Graphite Cake with deionized water repetitive scrubbing;
(2) Graphite Cake step (1) is filtered dry under 80-120 DEG C of condition with calcium stearate, poly (sodium aspartate) dispersing and mixing 45 minutes, the mass ratio of Graphite Cake, calcium stearate, poly (sodium aspartate) is 100:1:1;
(3) it is 300-400 DEG C that mixture step (2) obtained sends into three screw rod electromagnetic dynamic plasticizing extruder Vibration Extrusion machine set temperatures in the same way, rotating speed 1000rpm, due to three-screw extruder, it has two region of engagements, after graphite mixture is quantitatively sent into, drawn in gap by the motion between two screw rods and carry out high shearing action, under the effect of Vibrational force field, the intercropping periodical change at any time of this gap, shearing rate and rate of extension is made also to produce periodical change, along with the increase of vibrational frequency, in shear history, graphite is carried in the other direction by the reverse gear block arranged, postpone graphite to be fed forward, make graphite under shearing action and vibration drawing force field, periodically be sheared stripping, thus it is little to obtain thickness, the high-quality graphene that the number of plies is evenly distributed.
Analyze by detecting, the Graphene thickness that embodiment 5 obtains accounts for 86% within 3nm, and thickness accounts for 97% within 5nm, and the shearing of three screw rod electromagnetic dynamic plasticizing extruders is peeled off in the same way, the number of plies is evenly distributed more even, and the accounting of the Graphene of individual layer and several layers is more.
Claims (6)
1. one kind utilizes vibration screw extrusion press combination shearing stress to peel off the method preparing Graphene, it is characterized in that adopting the vibration screw extrusion press with the rotational shear field of force and the vibration drawing field of force, graphite is stretched while rotational shear is peeled off, comprises the steps:
(1) graphite and excessive intercalator are added to the water, homogenous disperse 10-25 minute, are then filtered dry obtain Graphite Cake with deionized water repetitive scrubbing;
(2) Graphite Cake step (1) is filtered dry under 80-120 DEG C of condition with stearate, stripper dispersing and mixing 30-45 minute, the mass ratio of Graphite Cake, stearate, stripper is 100:1-2:0.5-1;
(3) mixture step (2) obtained sends into vibration screw extrusion press, vibration screw extrusion press set temperature is 300-400 DEG C, rotating speed 500-1200rpm, by the high-speed revolution shearing field of force and the vibration drawing field of force, makes graphite be sheared stripping and obtains Graphene;
Described vibration screw extrusion press is the homodromal electromagnetic dynamic plasticizing extruder of multiscrew, ultrasonic vibration forcing machine or longitudinal mechanical vibration forcing machine, utilize in forcing machine gear block gap and there is the rotational shear field of force and the vibration drawing field of force simultaneously, achieve rapidly and efficiently to peel off and prepare Graphene;
The screw rod of described vibration screw extrusion press is assembled with building blocks form by gear block, and the alternate angle wherein between gear block is 30 °, 45 °, 60 °, 90 °, reverse 30 °, reverse 45 °, reverse 60 °;
Described intercalator is C
12-C
18long-chain organic quaternary ammonium salt or C
12-C
18the organic diamine of long-chain;
Described stripper selects the one in thionamic acid, Sunmorl N 60S, poly (sodium aspartate), diethyl thiourea.
2. a kind of vibration screw extrusion press combination shearing stress that utilizes according to claim 1 peels off the method preparing Graphene, it is characterized in that: the impulsive magnetic field that described electromagnetic dynamic plasticizing extruder is produced by solenoid makes screw rod do pulsation rotation, vibrational frequency is 20-80Hz, and amplitude is 0.1-1mm.
3. a kind of vibration screw extrusion press combination shearing stress that utilizes according to claim 1 peels off the method preparing Graphene, it is characterized in that: described electromagnetic dynamic plasticizing extruder is three screw rod electromagnetic dynamic plasticizing extruders in the same way.
4. a kind of vibration screw extrusion press combination shearing stress that utilizes according to claim 1 peels off the method preparing Graphene, it is characterized in that: described ultrasonic vibration forcing machine is by introducing high-frequency ultrasonic, utilize different Under Ultrasonic Vibration moving parts to obtain the periodic stretching field of force to shear, ultrasonic frequency is 20kHz, and power is at 2-3KW continuously adjustabe.
5. a kind of vibration screw extrusion press combination shearing stress that utilizes according to claim 1 peels off the method preparing Graphene, it is characterized in that: the described rotation plug of longitudinal mechanical vibration forcing machine in extruder head arranges vibrational frequency 50Hz, and amplitude is 1-3mm.
6. a kind of vibration screw extrusion press combination shearing stress that utilizes according to claim 1 peels off the method preparing Graphene, it is characterized in that: described stearate selects the one in sodium stearate, calcium stearate, Zinic stearas, Magnesium Stearate.
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| GB2585545A (en) * | 2018-02-02 | 2021-01-13 | Univ Kingston | Graphene nanoplatelets derived from thermomechanical exfoliation of graphite |
| GB2585545B (en) * | 2018-02-02 | 2022-08-17 | Univ Kingston | A method for manufacturing an exfoliated product from a layered material |
| US11760639B2 (en) | 2018-02-02 | 2023-09-19 | Queen's University At Kingston | Graphene nanoplatelets derived from thermomechanical exfoliation of graphite |
| CN111875881A (en) * | 2020-07-16 | 2020-11-03 | 广东工业大学 | Method for selectively distributing layered nanosheets at incompatible blend interface and nanocomposite |
| CN111875881B (en) * | 2020-07-16 | 2023-05-09 | 广东工业大学 | Method for selectively distributing lamellar nano-sheets at interface of incompatible blend and nano-composite material |
| CN115842848A (en) * | 2023-03-01 | 2023-03-24 | 成都远峰科技发展有限公司 | Dynamic monitoring system based on industrial Internet of things and control method thereof |
| CN115842848B (en) * | 2023-03-01 | 2023-04-28 | 成都远峰科技发展有限公司 | Dynamic monitoring system based on industrial Internet of things and control method thereof |
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Denomination of invention: A Method of Preparing Graphene by Compound Shear Stress Stripping with Vibrating Screw Extruder Effective date of registration: 20230609 Granted publication date: 20170725 Pledgee: Zhejiang Tailong Commercial Bank Co.,Ltd. Zhoushan Jintang Small and Micro Enterprise Specialized Branch Pledgor: ZHEJIANG ZHONGYANG SCREW MANUFACTURING Co.,Ltd. Registration number: Y2023330001141 |