CN105329886B - A kind of utilize vibrates the method that screw extruder combination shearing stress stripping prepares graphene - Google Patents
A kind of utilize vibrates the method that screw extruder combination shearing stress stripping prepares graphene Download PDFInfo
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Abstract
The present invention provides a kind of using the method that screw extruder combination shearing stress stripping prepares graphene is vibrated, and belongs to grapheme material field.This method introduces electromagnetism in the extruder of high speed rotation, ultrasound, longitudinal mechanical oscillation stretch the field of force, this vibration drawing field of force is with time cyclically-varying, stretch graphite interface, graphite becomes loose under remover effect, make graphite produce powerful shearing by extruder gear block contact interface in a stretched state to peel off, obtain thinner, the smaller graphene of thickness distribution scope, it is achieved thereby that quick under high shear forces, efficiently prepare high-quality graphene, considerably reduce the production cost of high-quality graphene, preparation process environmental protection, there is no waste gas, waste liquid, waste residue is produced, the large-scale production of graphene is promoted.
Description
Technical field
The present invention relates to grapheme material field, and in particular to one kind is shelled using screw extruder combination shearing stress is vibrated
From the method for preparing graphene.
Background technology
Graphene is a kind of single layer of carbon atom facestock material separated from graphite material, is the two-dimensional structure of carbon.It is this
The thickness of graphite crystal film only has 0.335 nanometer, and 200,000 Standard graphite alkene are superimposed together, also only one hairline
It is so thick.After graphene is found, due to its excellent performance, in the energy, electronic material, biomedicine and environment
The numerous areas such as protection start application, and its application field is progressively expanded.
The technology of preparing of graphene is had at present include mechanical stripping method, substrate grow nonparasitically upon another plant method, chemical vapour deposition technique, oxidation
Reducing process, chemical cleavage method etc..The shortcoming of oxidation-reduction method is that the graphene prepared has certain fault of construction, causes graphite
Alkene part electrical property loss of energy, is restricted the application of graphene；Graphene relative mechanical stripping obtained by vapour deposition process
The graphene prepared from method is difficult to shift, and some are using no discovery quantum Hall is not imitated in graphene obtained by vapour deposition process
Should, illustrate that vapour deposition process may influence some characteristics of graphene；Mechanical stripping method can obtain individual layer or only several
The graphene film of atomic layer level thickness, is the current effective ways for obtaining low-cost and high-performance graphene.
The graphene of excellent performance is obtained by the stripping gluing layer by layer of micromechanics, but this technological means is difficult to reality
Existing volume production.And then, graphene is obtained by the means of mechanical lapping at present, mechanical lapping is by powerful machinery punching
Hit and produce shearing to overcome the Van der Waals force between graphite flake layer to obtain graphene.But it is due to the impulsive force pole to graphite linings
Greatly, graphene is made to produce fault of construction, the size of graphene after reduction is peeled off.Especially because powerful mechanical shock makes graphite
Rotating fields are compacted, and cause to peel off difficulty increase.Therefore occur in that to set by auxiliary agent and device and peeled off.
Chinese invention patent application number 201310411516.0 discloses a kind of ball-milling preparation method of grapheme material, should
Invention mixes the hexa-atomic aromatic ring of graphitic carbon and alkyl or condensed ring polyether nonionic surfactant and deionized water loaded on ball milling
Tank, ball milling obtains graphene in 5-30 hours；Chinese invention patent application number 201210046788.0 discloses a kind of graphene material
The preparation method of material, powdered graphite is dissolved in organic solvent or water, is formed suspension, is ceaselessly engaged by gear teeth,
Graphite flake is ceaselessly torn, graphene is prepared；Chinese invention patent application number 201410567246.7 discloses a kind of eddy current type
Graphene stripping off device, by setting drive mechanism driving rotation, makes to form vortex between shear-blade, realizes the stripping of graphene
From.Chinese invention patent application number 201210038258.1 discloses a kind of electric field and peels off the side that intercalated graphite prepares graphene
Method, by chloride intercalated graphite, in alternating electric field, is peeled off to intercalated graphite.
Above technological means accelerates stripping, but low yield to a certain extent, and shearing force is weak, it is difficult to overcome graphite layers
Van der Waals force, thus reaction time length, efficiency are low, and the graphene number of plies particularly obtained is difficult to control to.
The content of the invention
In order to reduce the impact to graphite Rotating fields when high shear is peeled off, the shearing peeling effect of graphite, this hair are improved
It is bright to propose that a kind of utilize vibrates the method that screw extruder combination shearing stress stripping prepares graphene.This method passes through to graphite
Intercalation pretreatment, graphite is sent into the vibration screw extruder with the rotational shear field of force and the vibration drawing field of force, makes graphite
It is stretched while rotational shear is peeled off, overcomes graphite linings and be compacted, realizes large-scale production under high shear conditions.
High-quality graphene.
To solve the above problems, the present invention uses following technical scheme：
A kind of utilize vibrates the method that screw extruder combination shearing stress stripping prepares graphene, it is characterised in that use
Vibration Extrusion machine with the rotational shear field of force and the vibration drawing field of force, makes graphite be stretched while rotational shear is peeled off,
Graphite is peeled off by combination shearing stress and obtains graphene, is comprised the following steps：
(1) graphite is added to the water with excessive intercalator, homogenous disperse 10-25 minutes, then with deionized water repeatedly
Wash and be filtered dry and obtain Graphite Cake；
（2）By step（1）The Graphite Cake being filtered dry under the conditions of 80-120 DEG C with stearate, remover dispersion mixing
30-45 minutes, Graphite Cake, stearate, the mass ratio of remover were 100:1-2：0.5-1；
（3）By step（2）Obtained mixture feeding vibration screw extruder, vibrating screw extruder setting 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
Obtain graphene；
The vibration screw extruder is the electromagnetic dynamic plasticizing extruder of multiscrew rotating Vortex, ultrasonic vibration extruder or
Person's longitudinal direction mechanical oscillation extruder, multiscrew refers to two and above screw rod, is engaged in block gap and existed simultaneously using extruder
The rotational shear field of force and the vibration drawing field of force, rotational shear and vibrating motion realize rapidly and efficiently stripping and prepare graphite
Alkene, overcomes graphene and occurs lattice defect because of extruding；
The screw rod of the vibration screw extruder is assembled by gear block in building blocks form, wherein the alternate angle between gear block
For 30 °, 45 °, 60 °, 90 °, reverse 30 °, reverse 45 °, reverse 60 °, the graphite conveying of 90 ° of gear blocks is zero, reverse gear block
Opposite direction conveys graphite in shear history, and delay graphite is fed forward, and graphite is made in shear action and the vibration drawing field of force
Under, stripping is periodically sheared, so as to obtain the high-quality graphene that thickness is small, the number of plies is evenly distributed.
The impulsive magnetic field that described electromagnetic dynamic plasticizing extruder is produced by magnet coil makes screw rod make pulsation rotation, it is preferred that
Described electromagnetic dynamic plasticizing extruder vibration frequency is 20-80Hz, and amplitude is 0.1-1mm.
It is preferred that, described electromagnetic dynamic plasticizing extruder is three screw rods electromagnetic dynamic plasticizing extruder in the same direction.
Described ultrasonic vibration extruder is, by introducing high-frequency ultrasonic, the cycle to be obtained using different ultrasonic vibration parts
Property the stretching field of force shearing, it is preferred that described ultrasonic vibration extruder, supersonic frequency is 20kHz, and power is continuous in 2-3KW
It is adjustable.
Described longitudinal mechanical oscillation extruder, the rotating mandrel in extruder head sets different frequency to vibrate, preferably
, described longitudinal mechanical oscillation extruder sets frequency 50Hz, amplitude is 1-3mm.
Described intercalator is C12-C18Long-chain organic quaternary ammonium salt or C12-C18The organic diamine of long-chain.
One kind that described stearate is selected in odium stearate, calcium stearate, zinc stearate, magnesium stearate.
One kind that described remover is selected in sulfamic acid, sodium gluconate, poly (sodium aspartate), diethyl thiourea.
Extruder is the plant equipment commonly used in a kind of plastic processing, is widely used in the blending of polymer, filling and changes
Property and extrusion molding.Strong shear is continuously rotated by extruder makes shear surface occur shearing stripping acquisition graphene with graphite.
In order to avoid the graphite graphene that is compacted or has peeled off regroups in shearing and peel off in extruder, the present invention utilizes vibration
Screw extruder, this extruder can make in screw rod except the screw rod of rotation, also additional oscillator field, this oscillator field
Material is by combination shearing stress.Therefore, the extruder of rotation produces powerful shearing in gear block contact interface at a high speed, makes stone
Ink is peeled off, while by introducing the vibration drawing field of force, this vibration drawing field of force draws graphite interface with time cyclically-varying
Stretch, graphite has the rotational shear field of force and the vibration drawing field of force simultaneously in extruder engagement block gap, and combination shearing stress exists
Graphite is set not only to become loose under remover effect, and it is smaller to promote extruder shearing to separate thinner, thickness distribution scope
Graphene so that overcome graphene occurs lattice defect because of extruding.On the one hand, by setting extruder screw gear block
Element, particularly in gear block area, axial property back lash performance period change makes material while conveying, by complexity
Shear action, this shearing be different from grinding, but with material tangent plane direction shear；On the other hand, the additional field of force is utilized
Stretching, eliminates the extruding between screw rod and barrel, graphite is stripped in a stretched state.
This high shear by using vibration screw extruder compound force field is peeled off, and effectively overcomes the model of graphite layers
De Huali, splitting time section, makes to prepare graphene technique simple, it is easy to volume production, and by controlling vibration frequency and amplitude can
To realize the regulation and control to the graphene number of plies and size, a very feasible route is provided for industrialized production graphene.
The present invention prepares graphene using vibration screw extruder, with directly being ground using ball milling at present, oxidization abrasive again
Reduction, liquid phase stripping prepare graphene and compared, and the graphene number of plies distribution that the inventive method is obtained is equal, and thickness is thinner, crystal knot
Structure is more complete and orderly.Main performance contrast is as shown in table 1 below.
Table 1：
The present invention is a kind of using the method that screw extruder combination shearing stress stripping prepares graphene is vibrated, with existing stripping
Compared from graphite technology, the characteristics of it is protruded and excellent effect are：
1st, sheared by introducing the vibration drawing field of force in screw extruder, combination shearing stress avoids graphite from being compacted pressure
It is real, graphite is peeled off in the state of loose by Strong shear, therefore peel off it is more efficient, obtained graphene thickness is small, layer
Number is evenly distributed.
2nd, shear, effectively prevent when mechanical shearing peels off graphite to stone by using rotational shear and the vibration drawing field of force
The damage that black alkene layer crystal structure is caused, preferably saves the perfection of lattice of graphene.
3rd, by vibrating the method that screw extruder stripping prepares graphene, realize it is quick, efficiently prepare high-quality stone
Black alkene, considerably reduces the production cost of high-quality graphene, preparation process environmental protection, without waste gas, waste liquid, waste residue production
It is raw, promote the large-scale production of graphene.
Brief description of the drawings
Rotational shear and oscillator field tensile shear for a further understanding of vibration Screw Extrusion, by illustrating
It is bright.
Fig. 1 is the schematic appearance for vibrating screw extruder.1- motors, 2- charge doors, 3- stretching vibration field devices,
4- extruder screws.
Fig. 2 is the part gear block shearing sketch for vibrating screw extruder.Graphite is by the gear block forced shears of rotating Vortex
Cut, gear block alternate angle is 30 °, while the direction of arrow is the additional stretching vibration field of force, by the rotational shear of gear block and additional
Oscillator field the stretching field of force shearing, graphite is peeled off in the state of loose by Strong shear, thus peel off it is more efficient, obtain
Graphene thickness is small, the number of plies is evenly distributed.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention
Scope be only limitted to following example.In the case where not departing from above method thought of the present invention, according to ordinary skill
Various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
(1) by graphite and excessive intercalator C12Long-chain organic quaternary ammonium salt is added to the water, homogenous disperse 10 minutes, then
With deionized water cyclic washing and it is filtered dry and obtains Graphite Cake；
（2）By step（1）The Graphite Cake being filtered dry under the conditions of 80-120 DEG C with odium stearate, sulfamic acid dispersion mixing
30 minutes, Graphite Cake, odium stearate, the mass ratio of sulfamic acid were 100:1：0.5；
（3）By step（2）Obtained mixture feeding parallel dual-screw electromagnetic dynamic plasticizing extruder, Vibration Extrusion machine sets temperature
Spend for 300-400 DEG C, rotating speed 800rpm, vibration frequency is 80Hz, amplitude is 0.1mm.Wherein extruder screw is between gear block
Alternate angle be 30 °, 45 °, 60 °, 90 °, reverse 30 °, reverse 45 °, reverse 60 °, pass through the high-speed revolution shearing field of force and vibration draw
Stretch, makes graphite be sheared stripping and obtains graphene.
By detection and analysis, the graphene thickness that embodiment 1 is obtained accounts for 80% within 3nm, and thickness is within 5nm
95% is accounted for, the number of plies is evenly distributed.
Embodiment 2
(1) by graphite and excessive intercalator C16Long-chain organic quaternary ammonium salt is added to the water, homogenous disperse 25 minutes, then
With deionized water cyclic washing and it is filtered dry and obtains Graphite Cake；
（2）By step（1）The Graphite Cake being filtered dry is disperseed under the conditions of 80-120 DEG C with calcium stearate, poly (sodium aspartate)
Mixing 45 minutes, Graphite Cake, calcium stearate, the mass ratio of hard poly (sodium aspartate) are 100:1.5：1；
（3）By step（2）Obtained mixture sends into four screw rods ultrasonic vibration extruder in the same direction, and Vibration Extrusion machine sets temperature
Spend for 300-400 DEG C, rotating speed 1200rpm, supersonic frequency is 20kHz, and power is in 2KW continuously adjustabes.Pass through high-speed revolution shearing
The 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 C18The organic diamine of long-chain is added to the water, homogenous disperse 10 minutes, then
With deionized water cyclic washing and it is filtered dry and obtains Graphite Cake；
（2）By step（1）The Graphite Cake being filtered dry is scattered mixed with zinc stearate, diethyl thiourea under the conditions of 80-120 DEG C
Close 35 minutes, Graphite Cake, zinc stearate, the mass ratio of diethyl thiourea are 100:1：0.5；
（3）By step（2）Obtained mixture sends into the longitudinal mechanical oscillation extruder of three screw rod in the same direction, and Vibration Extrusion machine is set
It is 300-400 DEG C to put temperature, and rotating speed 600rpm sets frequency 50Hz, amplitude is 3mm.By the high-speed revolution shearing field of force and shaking
The dynamic stretching field of force, makes graphite be sheared stripping and obtains graphene.
Embodiment 4
(1) by graphite and excessive intercalator C124The organic diamine of long-chain is added to the water, homogenous disperse 25 minutes, then
With deionized water cyclic washing and it is filtered dry and obtains Graphite Cake；
（2）By step（1）The Graphite Cake being filtered dry is scattered mixed with magnesium stearate, sodium gluconate under the conditions of 80-120 DEG C
Close 40 minutes, Graphite Cake, magnesium stearate, the mass ratio of sodium gluconate are 100:2：1；
（3）By step（2）Obtained mixture feeding parallel dual-screw ultrasonic vibration extruder, Vibration Extrusion machine sets temperature
Spend for 300-400 DEG C, rotating speed 500rpm, Vibration Extrusion machine is assembled by gear block in building blocks form, wherein between gear block
Alternate angle is 30 °, 45 °, 60 °, 90 °, reverse 30 °, reverse 45 °, reverse 60 °, and the graphite conveying of 90 ° of gear blocks is zero, is reversely nibbled
Close block opposite direction in shear history and convey graphite, delay graphite is fed forward, and makes graphite in shear action and vibration drawing power
Under field action, stripping is periodically sheared, so as to obtain the high-quality graphene that thickness is small, the number of plies is evenly distributed.
Embodiment 5
(1) by graphite and excessive intercalator C18Long-chain organic quaternary ammonium salt is added to the water, homogenous disperse 20 minutes, then
With deionized water cyclic washing and it is filtered dry and obtains Graphite Cake；
（2）By step（1）The Graphite Cake being filtered dry is disperseed under the conditions of 80-120 DEG C with calcium stearate, poly (sodium aspartate)
Mixing 45 minutes, Graphite Cake, calcium stearate, the mass ratio of poly (sodium aspartate) are 100:1：1；
（3）By step（2）Obtained mixture sends into three screw rods electromagnetic dynamic plasticizing extruder Vibration Extrusion machine in the same direction and sets temperature
Spend for 300-400 DEG C, rotating speed 1000rpm, due to three-screw extruder, it there are two region of engagements, and graphite mixture is quantitatively sent into
Afterwards, gap is pulled by the motion between two screw rods and carries out high shear action, in the presence of Vibrational force field, the gap is with the time
Make cyclically-varying so that shear rate and rate of extension also produce cyclically-varying, with the increase of vibration frequency, by setting
The reverse gear block put opposite direction in shear history conveys graphite, and delay graphite is fed forward, make graphite in shear action and
Under vibration drawing force field, stripping is periodically sheared, so as to obtain the high-quality graphite that thickness is small, the number of plies is evenly distributed
Alkene.
By detection and analysis, the graphene thickness that embodiment 5 is obtained accounts for 86% within 3nm, and thickness is within 5nm
97% is accounted for, the shearing of three screw rods electromagnetic dynamic plasticizing extruder in the same direction is peeled off, and the number of plies, which is evenly distributed, to be more uniformly distributed, and individual layer and several layers
Graphene accounting it is more.
Claims (6)
1. a kind of utilize vibrates the method that screw extruder combination shearing stress stripping prepares graphene, it is characterised in that using tool
There is the vibration screw extruder in the rotational shear field of force and the vibration drawing field of force, graphite is drawn while rotational shear is peeled off
Stretch, comprise the following steps：
(1) graphite is added to the water with excessive intercalator, then homogenous disperse 10-25 minutes is washed repeatedly with deionized water
Wash and be filtered dry and obtain Graphite Cake；
（2）By step（1）The Graphite Cake being filtered dry under the conditions of 80-120 DEG C with stearate, remover dispersion mixing 30-45
Minute, Graphite Cake, stearate, the mass ratio of remover are 100:1-2 ：0.5-1 ；
（3）By step（2）Obtained mixture feeding vibration screw extruder, vibration screw extruder sets temperature to be 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 obtained
Graphene；
The vibration screw extruder is electromagnetic dynamic plasticizing extruder, ultrasonic vibration extruder or the longitudinal direction of multiscrew rotating Vortex
Mechanical oscillation extruder, is engaged in block gap using extruder and there is the rotational shear field of force and vibration drawing field of force stripping system simultaneously
Standby graphene；
The screw rod of the vibration screw extruder is assembled by gear block in building blocks form, and wherein the alternate angle between gear block is
30 °, 45 °, 60 °, 90 °, reverse 30 °, reverse 45 °, reverse 60 °；
The intercalator is C12-C18Long-chain organic quaternary ammonium salt or C12-C18The organic diamine of long-chain；
One kind that the remover is selected in sulfamic acid, sodium gluconate, poly (sodium aspartate), diethyl thiourea.
2. a kind of utilization according to claim 1 vibrates screw extruder combination shearing stress stripping and prepares graphene
Method, it is characterised in that：The impulsive magnetic field that described electromagnetic dynamic plasticizing extruder is produced by magnet coil makes screw rod make pulsation rotation,
Vibration frequency is 20-80Hz, and amplitude is 0.1-1mm.
3. a kind of utilization according to claim 1 vibrates screw extruder combination shearing stress stripping and prepares graphene
Method, it is characterised in that：Described electromagnetic dynamic plasticizing extruder is three screw rods electromagnetic dynamic plasticizing extruder in the same direction.
4. a kind of utilization according to claim 1 vibrates screw extruder combination shearing stress stripping and prepares graphene
Method, it is characterised in that：Described ultrasonic vibration extruder is, by introducing high-frequency ultrasonic, to utilize different ultrasonic vibration parts
Periodically stretching field of force shearing is obtained, supersonic frequency is 20kHz, and power is in 2-3KW continuously adjustabes.
5. a kind of utilization according to claim 1 vibrates screw extruder combination shearing stress stripping and prepares graphene
Method, it is characterised in that：Rotating mandrel of the described longitudinal mechanical oscillation extruder in extruder head sets vibration frequency
50Hz, amplitude is 1-3mm.
6. a kind of utilization according to claim 1 vibrates screw extruder combination shearing stress stripping and prepares graphene
Method, it is characterised in that：Described stearate is from one in odium stearate, calcium stearate, zinc stearate, magnesium stearate
Kind.
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| KR102176629B1 (en) * | 2017-04-28 | 2020-11-09 | 주식회사 엘지화학 | Method for preparing a graphene |
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| 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 |
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