CN104609413A - Machine-like stripping device for ton-scale production of graphene and production method of machine-like stripping device - Google Patents
Machine-like stripping device for ton-scale production of graphene and production method of machine-like stripping device Download PDFInfo
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Abstract
The invention discloses a machine-like stripping device for ton-scale production of graphene and a production method of the machine-like stripping device. The machine-like stripping device is characterized by comprising one or more stages of stripping devices which are connected in series, wherein each stripping device comprises a material bin, a rotor, a material distribution bin and the like, the lower part of the rotor is matched with that of the material bin, and when the rotor rotates, relative friction is formed at the matching position between the outer surface of the rotor and the inner surface of the material bin. During use, graphite raw material receives the shearing action of a friction force at the matching position, and Van der Waals forces among graphite layers of the graphite collapse so that the graphite is stripped and thinned into graphene which is fed into the material distribution bin. The machine-like stripping device for ton-scale production of graphene is simple to operate and can realize batch production of graphene, and the obtained graphene has a perfect crystal structure, a large specific surface area and good conductivity.
Description
Technical field
The present invention relates to mass production facilities and the production method of Graphene.
Background technology
Graphene (Graphene), also known as mono-layer graphite, be a kind of by carbon atom with sp
2hybridized orbital composition hexangle type is the flat film of honeycomb lattice, is the two-dimension nano materials only having a carbon atom thickness.Although the discovery of Graphene only about 10 years, cause the research and development tide of the another ripple of a ripple have swept the globe.Graphene is a kind of two dimensional crystal tightly packed by carbon atom, has the features such as magical electric transmission, conduction, heat conduction and machinery.The physicist An Deliehaimu of Univ Manchester UK in 2004 and Constantine Nuo Woxiaoluofu, successfully from graphite, Graphene has been separated in laboratory, demonstrating Graphene can Individual existence, therefore win Nobel Prize in physics in 2010, thus start the global research boom of Graphene preparation, modification and application.Graphene is used for the application prospect of the aspects such as ultracapacitor, transparency electrode, lithium ion battery, sensor, functional paint and polymer nanocomposites, opens the New Times of grapheme material.
As there being scholar to say, 19th century were epoch of ironware, and 20th century were epoch of silicon, and 21 century is epoch of carbon.Carbon is one of element that distributed in nature is the most general, is to form the most important element of all life body on the earth.The characteristic of carbon material almost contains the character of all substances on the earth.Advanced carbon material has novel texture and excellent physical and chemical performance, is to have novel material that is great and decision meaning to future development.
New material industry, as one of the emphasis of emerging strategic industries, is also foundation stone and the guide of following Hi-tech Industry Development, is the important foundation that China becomes production power of the world.Graphene is as advanced carbon material, and it is the current top quality in the world material found.It has following characteristics: the thinnest, and 0.35nm is called as the material that the world is the thinnest now; Specific surface area is maximum, 2620m
2/ g; The hardest, rigidity is better than diamond, is the material that mankind's known strength is the highest, harder than iron and steel 100 times; Most tension, can elastic stretching 20%; Thermal conductivity is the highest, 5300W/m.k; Most high mobility 200,000cm
2/ v.s (300k); High light transmittance, transmittance is 97.7%/individual layer; High current carrying capacity: high 6 orders of magnitude of current density ratio copper; The most peculiar, Graphene is two-dimentional quantum material, linear band dispersion, and carrier effective mass is zero, can observe quantum hall effect under greenhouse; Also there is room temperature ballistic transport characteristic.
Graphene has infinitely wide application prospect, although the present potential stage, generally application does not also open up new prospect with industrialization, but from the angle of scientific forecasting, has become very important major fields.Such as, it is alternative and solve the drawbacks such as traditional lithium cell charging speed is slow, power reservoir capacity is poor, the life-span is short, pollution, can solve the crucial problem of Development of Electric Vehicles, make New-energy electric vehicle flourish.For another example can substituted for silicon, manufacture future new era supercomputer; Substitute ITO transparent conductive film, be applied to the electronics industry such as touch-screen, Flexible Displays, solar cell; Also can be applicable to sea water desaltination, degradable plastics, heat dissipation film, corrosion protection coating, biomaterial, matrix material, panel computer, wrist-watch calendar, mobile telephone, photodetector, graphene paper, Graphene cloth and space flight military project, ultralight flak jackets, ultra-thin and ultra-light aircraft, ultra-thin folding cell phone, the sky elevator etc. that even has imagination.The demand that Graphene is created, very likely starts a subversiveness new technology new industrial revolution of have swepting the globe.From global development trend, no one is ready that losing Graphene develops the major opportunity brought.
The mode preparing the current comparative maturity of Graphene has Physical and chemical method, wherein the Typical Representative of Physical obtains from graphite crystal by the mode of adhesive tape sticking, this method can take structure very perfectly Graphene crystal, relatively be applicable to exploitation electron device or physical study, cannot volume production.Volume production mainly relies on chemical method, a kind of for film former shape Graphene " from bottom to top " method, is namely assembled into graphene film from small molecules or carbon atom by approach such as chemical vapour deposition, epitaxy or organic syntheses.This method scale is relatively easily done greatly, to obtain the crystalline structure of Graphene relatively complete, be more suitable for the transparent conductive film doing touch-screen or solar cell, and be difficult to the preparation being applied to powder Graphene.Another kind of mode is exactly " from top to bottom " method, is sometimes also chemical stripping method, utilizes intercalator that the Van der Waals force of each for the graphite crystal of three-dimensional interlayer is disintegrated exactly, graphite is disassembled out layer by layer, shells into which floor graphene product of individual layer or minority.Operational path and the intercalator used of current each producer are differentiated.Some salt intercalations then liquid phase are peeled off, and Graphene oxygen level prepared by this method is low, conduct electricity very well, but extent of exfoliation is relatively lower, and specific surface area is not too large; Then some initial oxidation intercalations are peeled off, and this method extent of exfoliation is high, and specific surface area is large, but the Graphene defect made is many, and oxygen level is large, constrains the process of industrialization of Graphene.
Summary of the invention
The present invention is the weak point for avoiding existing for above-mentioned prior art, a kind of tonne is provided to produce the class mechanically peel device of Graphene and production method thereof, to pollution-free, zero release, the mass production high-specific surface area of less energy-consumption, zero defect Graphene can be realized.
The present invention is that technical solution problem adopts following technical scheme:
The present invention tonne produces the class mechanically peel device of Graphene, and its feature is: described device is in series by one or more levels peel-off device;
The structure of described peel-off device is: the upper end of a material bin is provided with two opening for feeds, lower end is provided with discharge port, be communicated with below described discharge port and a point feed bin, filter screen is provided with in described point of feed bin, described point of feed bin is divided into coarse fodder storehouse and fines storehouse by described filter screen, after in material bin, material enters point feed bin by discharge port, through strainer filtering, material by filter screen enters fines storehouse, does not enter coarse fodder storehouse by the material of filter screen; A rotor is provided with in described material bin; Match with the below of described material bin in the below of described rotor, when making described rotor turns, the outside surface of rotor and the internal surface of material bin form Relative friction at mated position place;
The coarse fodder storehouse of peel-off device at different levels is by being provided with another opening for feed of pipeline communication and the first step peel-off device taking out pump; The fines storehouse of upper level peel-off device is by being provided with the opening for feed of pipeline communication and the next stage peel-off device taking out pump, and the fines storehouse of last step peel-off device is by being provided with the pipeline communication and finished product receptacle of taking out pump;
The outside surface of described rotor is made up of identical material high hardness material at mated position place with the internal surface of material bin, and described high hardness material is the material that hardness is greater than graphite.
Preferably, described hardness is greater than the material of graphite is marble, granite, diamond, smart steel, carbon steel, high mangaenese steel, wolfram varbide or stainless steel.
The outside surface of described rotor and the internal surface of material bin are plane or the Alveolus type flour milling being provided with multiple teeth groove at mated position place.
In described fines storehouse, the below that is positioned at described filter screen is provided with filter screen brush;
The pipeline that in the end the fines storehouse of one-level peel-off device is communicated with finished product receptacle is provided with drying plant.
Utilize the production method of tonne production Graphene of above-mentioned class mechanically peel device, its feature is:
Start the rotor of peel-off device at different levels and take out pump;
Rotary rotor, makes the outside surface of rotor and the internal surface of material bin form frictional force at mated position place;
Graphite and liquid adjuvants are mixed and stirs, then join the material bin of first step peel-off device from opening for feed, graphite is subject to the shearing action of frictional force in the position that rotor matches with material bin, in graphite, the Van der Waals force of each graphite layers is disintegrated, thus make graphite be stripped thinning acquisition Graphene, a point feed bin is entered from feed opening, sieve through filter screen, next stage peel-off device is entered by the material (comprising the unstripped graphite raw material meeting filter screen order number and the Graphene peeling off acquisition) of filter screen, again peel off thinning, peel off obtained finished product Graphene layer by layer through multistage peel-off device and enter finished product receptacle, the material bin that material not by filter screen in peel-off device at different levels returns first step peel-off device continues to peel off.
Wherein said liquid adjuvants is one or more mixing in deionized water, alcohol, N-Methyl pyrrolidone, DMF, peruscabin.
The quality of described graphite and the volume ratio of described liquid adjuvants are 0.01 ~ 150:100g/ml.
The present invention utilizes the Relative friction of class mechanically peel device rotor and material bin, graphite raw material is peeled off layer by layer, thus acquisition Graphene, the material that the outside surface of rotor and the internal surface of material bin are greater than graphite at mated position place by hardness is formed, to reduce the wearing and tearing of device.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, to produce the class mechanically peel device of Graphene simple to operate for the present invention tonne, and gained Graphene crystalline structure is perfect, specific surface area is large, conduct electricity very well, and can realize the mass production of Graphene.
2, the Graphene extent of exfoliation prepared of the present invention is relatively adjustable, can according to splitting time and the number of plies peeling off number of times and adjust gained Graphene;
3, the Graphene that prepared by the present invention does not almost have defect, and oxygen level is extremely low;
4, the present invention prepares the middle any tramp material particle that do not induce one of method of Graphene, maintain the purity of Graphene to the full extent, substantially having accomplished zero destruction to Graphene, achieved zero damage, no pollution, zero release, less energy-consumption, high yield, is the inevitable choice of Graphene volume production from now on;
5, the method for Graphene of the present invention's synthesis is simple, reliable and stable, produces line and copies simply, can the demand of fast responding market.
Accompanying drawing explanation
Fig. 1 is the structural representation that the present invention tonne produces the class mechanically peel device of Graphene;
Fig. 2 is the schematic diagram that the present invention tonne produces material bin and rotor mated position place in the class mechanically peel device of Graphene;
Fig. 3 is that the graphene dispersion of the embodiment of the present invention 1 preparation is to the microscope figure on silicon oxide;
Fig. 4 is the TEM figure of Graphene prepared by the embodiment of the present invention 1;
Fig. 5 is the purity table of Graphene prepared by the embodiment of the present invention 1;
Fig. 6 is the photo of the embodiment of the present invention 2 marble mill;
Fig. 7 is that the graphene dispersion of the embodiment of the present invention 2 preparation is to the microscope figure on silicon oxide;
Fig. 8 is the TEM figure of Graphene prepared by the embodiment of the present invention 2;
Fig. 9 is the purity table of Graphene prepared by the embodiment of the present invention 3;
Number in the figure: 1a opening for feed; 1b discharge port; 2 material bins; 3 rotors; 4a coarse fodder storehouse; 4b fines storehouse; 5 filter screens; 6 filter screen brushes; 7 take out pump; 8 finished product receptacles.
Embodiment
Embodiment 1
As shown in Figure 1, the class mechanically peel device of the present embodiment tonne production Graphene is in series by three grades of peel-off devices;
The structure of peel-off device is: the upper end of a material bin 2 is provided with two opening for feed 1a, lower end is provided with discharge port 1b, be communicated with below discharge port 1b and a point feed bin, filter screen 5 is provided with in point feed bin, filter screen 5 will divide feed bin to be divided into coarse fodder storehouse 4a and fines storehouse 4b, after in material bin 2, material enters point feed bin by discharge port 1b, filter through filter screen 5, material by filter screen 5 enters fines storehouse 4b, does not enter coarse fodder storehouse 4a by the material of filter screen 5; A rotor 3 is provided with in material bin 2; Match with the below of material bin 2 in the below of rotor 3, when rotor 3 is rotated, the outside surface of rotor 3 and the internal surface of material bin 2 form Relative friction at mated position place;
The coarse fodder storehouse 4a of peel-off device at different levels is by being provided with another opening for feed 1a of pipeline communication and the first step peel-off device taking out pump 7; The fines storehouse of upper level peel-off device is by being provided with the opening for feed 1a of pipeline communication and the next stage peel-off device taking out pump 7, and the fines storehouse of last step peel-off device is by being provided with the pipeline communication and finished product receptacle 8 of taking out pump 7;
The outside surface of rotor 3 is made up of identical material high hardness material at mated position place with the internal surface of material bin 2, and high hardness material is the material that hardness is greater than graphite.The present embodiment selects marble material.In concrete enforcement, the size of the position that rotor matches with material bin can adjust arbitrarily according to the needs of output.
As shown in Figure 2, the outside surface of described rotor (3) and the internal surface of material bin (2) are plane or the Alveolus type flour milling being provided with multiple teeth groove at mated position place.The structure formation being set to Alveolus type flour milling is a kind of structure being similar to mill, can add the frictional force of ectotrochanter and material bin compared to plane, is easier to the multi-layer graphene of composition graphite to disassemble out layer by layer, to obtain more Graphenes.
In concrete enforcement, in described fines storehouse 4b, the below that is positioned at filter screen 5 is provided with filter screen brush 6, so that clean filter screen 5.
In use, by the powdery graphite alkene sheet selecting the graphite raw material of different meshes to obtain different size, the Graphene of required order number can also can be obtained by the filter screen of selection different meshes.
In addition, graphite raw material can be peeled off for single or multiple lift Graphene by the stripping of every one-level peel-off device, again through the filtration of filter screen, the Graphene that meets order number demand is mingled with unstripped graphite raw material and enters next stage peel-off device, multi-layer graphene may be stripped as single-layer graphene in next stage peel-off device, graphite raw material continues to be stripped into Graphene, and the stripping layer by layer through multistage peel-off device can peel off into single-layer graphene by as much as possible for graphite raw material.
In concrete enforcement, because raw material is graphite and the mixing of liquid adjuvants, what therefore obtain in finished product receptacle is the dispersion liquid of Graphene, the pipeline that is communicated with finished product receptacle of the fines storehouse of in the end one-level peel-off device can arrange drying plant as required, dry to the graphene dispersing solution obtained after peel-off device stripping at different levels by drying plant, remove liquid adjuvants, in finished product receptacle, collect dry graphene powder.
Utilize the method for the class mechanically peel device of the present embodiment production tonne production Graphene as follows:
Start the rotor of peel-off device at different levels and take out pump;
Rotary rotor, makes the outside surface of rotor and the internal surface of material bin form frictional force at mated position place;
1000g blocky graphite and 1000mL deionized water are mixed and stir, join the material bin of first step peel-off device from opening for feed, graphite is subject to the shearing action of frictional force in the position that rotor matches with material bin, Van der Waals force in graphite between each layer graphene is disintegrated, thus make graphite be peeled off thinning acquisition Graphene layer by layer, a point feed bin is entered from feed opening, sieve through filter screen, the Graphene meeting filter screen order number is mingled with the fines storehouse that the graphite raw material meeting filter screen order number enters first step peel-off device, enter second stage peel-off device taking out under pumping action, again peel off thinning, and then through third stage peel-off device, the finished product graphene dispersing solution obtained in the fines storehouse of third stage peel-off device enters finished product receptacle, the material bin that material not by filter screen in peel-off device at different levels returns first step peel-off device continues to peel off.
Carry out drying to graphene dispersing solution and remove ionized water, then the Graphene of drying is carried out specific surface area test, the specific surface area of the Graphene that known the present embodiment obtains can reach 200 ~ 300m
2/ g.
Graphene is configured to the spirituous solution of 0.01mg/mL, is dispersed in silicon oxide substrate, examines under a microscope pattern, as shown in Figure 3, can find out that the present embodiment gained graphene film footpath is at 1 ~ 10 μm, and be all individual layer.
The graphene dispersion of the present embodiment is done on TEM copper mesh TEM test, as shown in Figure 4, can see that gained Graphene is single layer structure equally.
Do purity check with dried dry powder Graphene, as shown in Figure 5, known Graphene content is more than 99.7% for analytical results.
Meanwhile, known by analytical test, the specific conductivity of the present embodiment gained Graphene is greater than 30000S/m.
According to the demand of output and strength of solution, can be realized by the ratio of regulating rotary rotor speed and initial auxiliary agent and Graphene, this device can realize the transformation efficiency of graphite to Graphene more than 90%, and the Graphene that can complete 100 kilograms per hour is produced.Embodiment 2
When class mechanically peel device of the present invention only has one-level peel-off device to form, mill structure can be reduced to, be equivalent to the circular marble mill of two panels of marble stone mill by material bin 2 and rotor 3, the contact surface of two fan mills arranges well-regulated groove, as shown in Figure 6.During use, 500g crystalline flake graphite is joined between two panels circular millstone that diameter is 1m marble stone mill, rotate counterclockwise mill, while add alcohol from mill top, the all well-regulated groove in the inside of the upper lower fan of stone mill, and middle dark outside is shallow, and certain gap is also left in centre.Along with the rotation that upper prochlorite grinds, graphite first enters in the gap of middle portion according to the skewed slot passage carved between two panels mill, progress in the groove of rule afterwards, the Van der Waals force of graphite layers is disintegrated by frictional shearing in the process, graphite is peeled off into individual layer or multi-layer graphene layer by layer, rotating grinding board 30 minutes, just obtains the Graphene spirituous solution of solid content 500g.
The spirituous solution that takes a morsel drops in respectively on oxidized silicon chip and TEM copper mesh and observes, as shown in Figure 7, gained graphene film footpath is greater than 100 μm to the optical microphotograph picture obtained, and has individual layer and few layer to exist, TEM characterizes as shown in Figure 8, demonstrates gained Graphene and has individual layer and few Rotating fields.Test by analysis, the specific surface area of gained Graphene is at 45m
2about/g, specific conductivity is greater than 10000S/m.
Compared with the embodiment 1 class mechanically peel device be made up of three grades of peel-off devices used, the specific surface area of the present embodiment gained Graphene is little, specific conductivity is little, and gained Graphene not all is individual layer.
Embodiment 3
As a comparison, the present embodiment adopts chemical method to prepare graphene powder, specific as follows: in the flask of 250mL, to add 5mL oleum, and ice bath adds 2g Graphite Powder 99 and 1g NaNO under stirring
3mixture, point add 6g potassium permanganate three times after stirring, period temperature can not more than 20 DEG C.Continue to be stirred to temperature and rise to 35 DEG C, Keep agitation adds deionized water in 30 minutes, stir again and make dissolution homogeneity in 20 minutes, add 5mL hydrogen peroxide, now solution is gradually in glassy yellow, filtered while hot, by products therefrom successively with 5% hydrochloric acid and washed with de-ionized water until solution is in neutrality, product after cleaning is put into vacuum drying oven dry at 60 DEG C, obtain graphite oxide.Get 100mg graphite oxide to be dispersed in 100mL water and to obtain brown color suspension, liquid is placed on ultrasonic disperse 1h in ultrasonic cleaning machine and obtains stable dispersions.Moved into heating in water bath to 80 DEG C in flask subsequently, drip 2mL hydrazine hydrate, filter after reaction 24h, products therefrom methyl alcohol and deionized water respectively rinse 6 times, with 60 DEG C of dryings in vacuum drying oven, obtain Graphene.
The a small amount of Graphene getting the present embodiment does specific surface area test, and the specific surface area of known the present embodiment gained Graphene is 550 ~ 650m
2/ g.The Graphene that takes a morsel does purity check, as shown in Figure 9, can see that wherein sulphur content reaches about 5%, and carbon content is about 94%, and specific conductivity is about 850S/m.Therefore, although the Graphene prepared in this way has larger specific surface area, purity is low, and specific conductivity is low, and employs highly toxic substance hydrazine hydrate etc., contaminate environment.
Claims (7)
1. a class mechanically peel device for tonne production Graphene, is characterized in that: described device is in series by one or more levels peel-off device;
The structure of described peel-off device is: the upper end of a material bin (2) is provided with two opening for feeds (1a), lower end is provided with discharge port (1b), described discharge port (1b) below is communicated with and a point feed bin, filter screen (5) is provided with in described point of feed bin, described point of feed bin is divided into coarse fodder storehouse (4a) and fines storehouse (4b) by described filter screen (5), after material bin (2) interior material enters point feed bin by discharge port (1b), filter through filter screen (5), material by filter screen (5) enters fines storehouse (4b), do not enter coarse fodder storehouse (4a) by the material of filter screen (5), a rotor (3) is provided with in described material bin (2), match with the below of described material bin (2) in the below of described rotor (3), when described rotor (3) is rotated, the outside surface of rotor (3) and the internal surface of material bin (2) form Relative friction at mated position place,
The coarse fodder storehouse (4a) of peel-off device at different levels is by being provided with another opening for feed (1a) of pipeline communication and the first step peel-off device taking out pump (7); The fines storehouse (4b) of upper level peel-off device is by being provided with the opening for feed (1a) of pipeline communication and the next stage peel-off device taking out pump (7), and the fines storehouse (4b) of last step peel-off device is by being provided with the pipeline communication and finished product receptacle (8) of taking out pump (7);
The outside surface of described rotor (3) is made up of identical material high hardness material at mated position place with the internal surface of material bin (2), and described high hardness material is the material that hardness is greater than graphite.
2. class mechanically peel device according to claim 1, is characterized in that: the material that described hardness is greater than graphite is marble, granite, diamond, smart steel, carbon steel, high mangaenese steel, wolfram varbide or stainless steel.
3. class mechanically peel device according to claim 1, is characterized in that: the outside surface of described rotor (3) and the internal surface of material bin (2) are plane or the Alveolus type flour milling being provided with multiple teeth groove at mated position place.
4. class mechanically peel device according to claim 1, is characterized in that: in described fines storehouse (4b), the below that is positioned at described filter screen (5) is provided with filter screen brush (6);
The pipeline that in the end the fines storehouse of one-level peel-off device is communicated with finished product receptacle (8) is provided with drying plant.
5. utilize the class mechanically peel device described in claim 1 tonne to produce a production method for Graphene, it is characterized in that:
Start the rotor of peel-off device at different levels and take out pump;
Rotary rotor, makes the outside surface of rotor and the internal surface of material bin form frictional force at mated position place;
Graphite and liquid adjuvants are mixed and stirs, then join the material bin of first step peel-off device from opening for feed, graphite is subject to the shearing action of frictional force in the position that rotor matches with material bin, in graphite, the Van der Waals force of each graphite layers is disintegrated, thus make graphite be stripped thinning acquisition Graphene, a point feed bin is entered from feed opening, sieve through filter screen, next stage peel-off device is entered by the material of filter screen, again peel off thinning, peel off obtained finished product Graphene layer by layer through multistage peel-off device and enter finished product receptacle; The material bin that material not by filter screen in peel-off device at different levels returns first step peel-off device continues to peel off.
6. method according to claim 5, is characterized in that: described liquid adjuvants is deionized water, alcohol, N-Methyl pyrrolidone, DMF mix with one or more in peruscabin.
7. method according to claim 5, is characterized in that: the quality of described graphite and the volume ratio of described liquid adjuvants are 0.01 ~ 150:100g/mL.
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