CN105540574A - Method for preparing graphene micro-sheets by using counter-jet jet mill - Google Patents
Method for preparing graphene micro-sheets by using counter-jet jet mill Download PDFInfo
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Abstract
The invention relates to the field of graphene materials, particularly relates to preparation methods for graphene micro-sheets and particularly relates to a method for preparing the graphene micro-sheets by using a counter-jet jet mill. According to the method, the graphene sheets are obtained through enabling melted ferric chloride and potassium chloride to enter an interlayer of graphite, enabling the powder materials to be in collision through high-speed airflow in the counter-jet jet mill by using the characteristic of brittleness of ferric chloride and potassium chloride crystal grains and the characteristics of good fluidity and difficulty in agglomeration of talcum powder, delaminating the graphite and the talcum powder by generated impact force, shearing force and frictional force, carrying out further separation by a grading room, refluxing unqualified powder material to a crushing chamber, and yielding delaminated graphite and talcum powder as well as gas together. The continuous and large-scale production of the graphene micro-sheets, which are uniform in layer number dispersion and good in fluidity and are not prone to agglomeration, is achieved, the yield is high, the cost is low, no pollution is caused, and the layer thickness meets the requirements of use in the fields of rubber reinforcing, plastic reinforcing, coating material anticorrosion, lubrication and sewage treatment, so that the promotion of the large-scale application of graphene is facilitated.
Description
Technical field
The present invention relates to grapheme material field, be specifically related to the preparation method of graphene film, particularly relate to a kind of graphene microchip is prepared in utilization method to spray formula micronizer mill.
Background technology
Graphene is the another Novel Carbon Nanomaterials be found after carbon nanotube, its appearance makes the crystalline structure of carbon define the integral framework comprising soccerballene, carbon nanotube, Graphene, graphite and diamond, establishes from zero to the carbon normal form of three-dimensional.Because Graphene possesses excellent electricity, mechanics, optical property, the preparation technology of Graphene is received much concern all the time, the main technique preparing Graphene at present takes vapour deposition process, catalytic growth after utilizing gaseous carbon source at high temperature to decompose on matrix surface prepares Graphene, and the method prepares the important method of high quality and big area single-layer graphene.But its working condition is comparatively harsh, power consumption is large, and cost is high.And, directly adopt gaseous carbon sources to add the danger of production to a great extent.And another kind of adopt graphite oxide reduction method to be prepare the method for Graphene, mainly graphite is carried out Strong oxdiative process, after obtaining graphite oxide, then stripping is carried out to it prepare graphene oxide, eventually pass reduction treatment and obtain Graphene; But because this preparation method can destroy graphene-structured, and energy consumption is large in preparation process, and efficiency is low, the high and contaminate environment of cost, is difficult to promote.
Chinese invention patent application numbers 201310097659.9 discloses the preparation method of Graphene, comprise: Graphene presoma and amino-complex are mixed, ball milling obtains the Graphene that mixes and amino-complex mixed powder for 8 ~ 20 hours, wherein utilize amino-complex to be peeled off by graphite presoma in ball milling and obtain Graphene, the mass ratio of described graphite presoma and amino-complex is 1:(1 ~ 10); By described Graphene and amino-complex mixed powder dispersion solvent, so that amino-complex is dissolved; Filter, adopt described solvent wash filter cake to obtain Graphene wet-milling; And described Graphene wet-milling is placed in vacuum drying oven in 60 ~ 120 DEG C, dry 5 ~ 12 hours, obtained Graphene dry powder.Preparation method's technique of this invention is simple, and process is easy to control, but the Graphene quality of preparation is uneven, is difficult to ensure repeatability.
Chinese invention patent application numbers 201410286173.4 discloses a kind of preparation method of Graphene, and it comprises the following steps: the mode of graphite oxide mechanical shearing or ball milling is broken into small shreds by (1); (2) under hydrogen nitrogen or hydrogen argon atmospher, be 1 ~ 19% by hydrogen volume concentration, the concentration of nitrogen or argon gas is 99 ~ 81%, gas flow rate is 10 ~ 100mL/min, with 5 ~ 35 DEG C/min temperature rise rate, above-mentioned graphite oxide small shreds is warming up to 250 ~ 500 DEG C, soaking time is 5 ~ 120min, and hydrogen nitrogen or hydrogen argon gas stream drop to room temperature or naturally cool to room temperature, obtain Graphene.The preparation method of this invention is simple to operate, and the Graphene reducing degree obtained is higher, but the graphene dispersion of preparation is poor, and quality is uncontrollable.
Chinese invention patent application numbers 201410226056.9 discloses the technique and the device that adopt comminution by gas stream stripping means to prepare Graphene presoma two-dimensional nano Graphite Powder 99, and this contrive equipment comprises air supply system, pulverizes the gentle solid separation system of stripping system; In pulverizing stripping system, A return line, B return line and upcast constitute the Matter Transfer loop of comminution by gas stream stripping process; A air entraining pipe, B air entraining pipe and C air entraining pipe constitute the comminution by gas stream passage of comminution by gas stream stripping process.Preparing Graphene presoma two-dimensional nano Graphite Powder 99 adopts three bursts of supersonic jets jointly to carry graphite granule, by collision and the friction of band material jet, realize high-purity pulverizing and the stripping of graphite granule, pulverize stripping continuously by the circulation of graphite granule, obtain two-dimensional nano Graphite Powder 99 thus.This invention utilizes the mutual collision between graphite granule to realize pulverizing and the stripping of Graphite Powder 99 with friction, and obtain highly purified two-dimensional nano Graphite Powder 99, but preparation method's productive rate of this invention is low, quality product is uncontrollable.
Mechanically peel method be a kind of can with low cost, the pollution-free method preparing high-quality graphene, now conventional mechanical-physical stripping method comprises conventional ball mill, stirring ball-milling, grinding etc., but in the process of abrading-ball grinding graphite, because local applying pressure is large, powerful surging force can make Graphene produce textural defect, reduces the size of Graphene after peeling off.Therefore, invent a kind of preparation technology simply, production safety environmental protection, production cost is low, and output is high, the graphene preparation method of constant product quality, to the application promoting grapheme material, promotes that the development of Graphene industry is significant.
Summary of the invention
High for current Graphene production cost, complicated process of preparation, the shortcoming that output is little, the present invention proposes a kind of method that low cost prepares graphene microchip.The method utilizes prepares the graphene microchip that be evenly distributed of the number of plies at 500-200 layer to spray formula micronizer mill, the graphene microchip of preparation can be applicable in the matrix materials such as rubber, plastics, coating, lubricating oil, sewage disposal, or as preparing the raw material of Graphene further, the preparation cost of current Graphene significantly can be reduced.
For solving the problem, the present invention by the following technical solutions:
A kind of utilization prepares the method for graphene microchip to spray formula micronizer mill, it is characterized in that: first by Graphite Powder 99 thermal treatment, add talcum powder and N,N-DIMETHYLACETAMIDE in heat treatment process and carry out dispersed with stirring, then make Graphite Powder 99 interlayer brittle by intercalator process, by the impact force, shearing force, the frictional force stripping graphite that produce pulverizing nozzle and the feed introduction of spray formula micronizer mill, obtain the number of plies in being uniformly dispersed of 50-200 layer, good fluidity, the graphene microchip of not easily reuniting, concrete grammar is as follows:
(1) be the Graphite Powder 99 of 80-90 by weight part, weight part be the talcum powder of 1-5 and weight part is that the N,N-DIMETHYLACETAMIDE of 0.5-1.5 is in high-speed mixing reaction machine, mix under Heating temperature is 250-300 DEG C of condition, with the rotating speed dispersed with stirring 30-60min of 300-600rpm, obtain mixed powder;
(2) iron(ic) chloride, Repone K, polyoxyethylene glycol are mixed with intercalator with mass ratio 2-3:2-3:1, then the mixed powder that step (1) obtains are soaked more than 48h in intercalator, be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in spray formula micronizer mill, two nozzles are arranged to spray formula micronizer mill, pulverize nozzle for one and spray into crushiing chamber with the pressure of 3.0-4.0MPa, a feed introduction sprays into crushiing chamber with the pressure of 2.0-2.8MPa, powder produces the impact force of high strength in crushiing chamber with the collision of the form of jet, shearing force, frictional force, powder is repeated stock in high velocity air, in the process of cutting rubbing, talcum powder and graphite linings are constantly peeled off, by the screening of grading room, the crushiing chamber that is back to defective macrobead powder continues collision and peels off, reach the product of stripping requirement from products export output, obtain the number of plies being uniformly dispersed at 50-200 layer, good fluidity, not easily reunite Graphene material.
Described Graphite Powder 99 is any one in crystalline flake graphite, expanded graphite, high orientation graphite, thermo-cracking graphite, and particle diameter is between 50 microns and 500 microns.
Described talcum powder is platy talc, and particle diameter is between 50 microns and 500 microns, and radius-thickness ratio is between 1:10 and 1:20.
Nozzle, feed introduction, crushiing chamber, grading room, hopper, lining, products export are pulverized in described comprising spray formula micronizer mill.The characteristic of utilize talcum powder good fluidity, not easily reuniting, by the mixed powder of talcum powder and Graphite Powder 99 in High-speed gas impacting by graphite and talcum powder delamination, further by grading room sorting, defective powder is heavy is back to crushiing chamber, peel off graphite to be separated by products export together with gas with talcum powder, obtain graphene microchip.
Describedly feed introduction is provided with to spray formula micronizer mill and pulverizes nozzle two nozzles, described feed introduction is in crushiing chamber hopper side, inlet pressure 2.0-2.8MPa, inlet diameter 6-10mm, described pulverizing nozzle is at the crushiing chamber opposite side relative with feed introduction, inlet pressure 3.0-4.0MPa, inlet diameter 6-10mm, pressure is by the rare gas element generating chamber of compression, pressure difference is there is owing to arranging the pressure pulverizing nozzle and feed introduction, in crushiing chamber, powder bumps against and moves with same direction, crushed material is sprayed into crushiing chamber with the pressure of 3.6MPa by preferred pulverizing nozzle, a feed introduction sprays into crushiing chamber with the pressure of 2.5MPa, obtain the number of plies being uniformly dispersed at 50-200 layer, good fluidity, the graphene microchip of not easily reuniting.
In order to promote the widespread use of grapheme material, the present invention proposes a kind of method preparing graphene microchip, the method can the acquisition number of plies of volume production at the graphene film of 50-200 layer, stable production process, and it is pollution-free, production cost compares the reduction that existing graphene preparation method becomes hundred times, the graphene microchip of preparation is not only uniformly dispersed, good fluidity, not easily reunites, and have excellent physical strength, conduction, heat conductivility concurrently, and good lubrication, high temperature resistant and anticorrosion properties.Because the thickness of the graphene microchip of preparation is within the scope of nanoscale, but its radial width can reach several to dozens of micron, there is the diameter/thickness ratio of super large, graphene microchip can be applied in rubber, plastics, coating, lubrication wet goods matrix material.Or as preparing the raw material of Graphene further, the preparation cost of current Graphene significantly can be reduced.
The present invention is a kind of utilizes the method being prepared by spray formula micronizer mill to graphene microchip, the characteristic of utilize talcum powder good fluidity, not easily reuniting, make powder good fluidity in the process of spraying, not easily block, and the graphene microchip of preparation is loose evenly, good fluidity, not easily reunite; In to spray formula micronizer mill, by high velocity air, material is collided simultaneously; the impact force produced, shearing force, frictional force are by graphite and talcum powder delamination; further by grading room sorting; utilization has been peeled off graphite and has been separated with macrobead material with talcous high-specific surface area characteristic; defective powder is back to crushiing chamber, achieves continuously, the large-scale production number of plies is that 50-200 is uniformly dispersed, good fluidity, the graphene microchip of not easily reuniting.
The present invention utilizes the graphene microchip prepared spray formula micronizer mill, not only be uniformly dispersed, good fluidity, not easily reunite, and pollution-free, output is high, cost is low, meet the requirement in fields such as rubber reinforcement, plastics enhancing, anticorrosion with coat, lubrication, sewage disposals, be conducive to the large-scale application promoting Graphene.Its salient features advantage is as shown in table 1.
Table 1.
The present invention is a kind of utilizes the method being prepared by spray formula micronizer mill to graphene microchip, and compared with prior art, its outstanding feature and excellent effect are:
The characteristic of 1, utilize talcum powder good fluidity, not easily reuniting, makes that the graphene microchip of preparation is loose evenly, good fluidity, not easily to reunite.
2, utilize the nozzle to spray formula micronizer mill two different operating pressure, allow powder peel off in crushiing chamber collision, obtain by the sorting of grading room the graphene microchip that the number of plies is controlled, be evenly distributed.
3, preparation method of the present invention be easy to control, the closed production of serialization can be realized, drop into little, cost is low, non-environmental-pollution, output are high, has significant market using value.
Accompanying drawing explanation
For further illustrating the method utilizing and prepared by spray formula micronizer mill to graphene microchip, be described by accompanying drawing.
Accompanying drawing 1: for spray formula micronizer mill schematic diagram.1-products export; 2-grading room; 3-lining; 4-hopper; 5-feed introduction; 6-crushiing chamber; 7-pulverizes nozzle.
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
A kind of utilization prepares the method for graphene microchip to spray formula micronizer mill:
(1) by weight part be 80 expanded graphite powder, weight part be 1 talcum powder and weight part be that the N,N-DIMETHYLACETAMIDE of 0.5 is in high-speed mixing reaction machine, mix under Heating temperature is 250 DEG C of conditions, with the rotating speed dispersed with stirring 30-60min of 300rpm, obtain mixed powder;
(2) iron(ic) chloride, Repone K, polyoxyethylene glycol are mixed with intercalator with mass ratio 2:2:1, then the mixed powder that step (1) obtains are soaked more than 48h in intercalator, be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in spray formula micronizer mill, two nozzles are arranged to spray formula micronizer mill, pulverize nozzle for one and spray into crushiing chamber with the pressure of 3.0MPa, a feed introduction sprays into crushiing chamber with the pressure of 2.0MPa, powder produces the impact force of high strength in crushiing chamber with the collision of the form of jet, shearing force, frictional force, powder is repeated stock in high velocity air, in the process of cutting rubbing, talcum powder and graphite linings are constantly peeled off, by the screening of grading room, the crushiing chamber that is back to defective macrobead powder continues collision and peels off, reach the product of stripping requirement from products export output, obtain the number of plies being uniformly dispersed at 50-200 layer, good fluidity, not easily reunite graphene microchip.
embodiment 2
A kind of utilization prepares the method for graphene microchip to spray formula micronizer mill:
(1) by weight part be 90 high orientation Graphite Powder 99, weight part be 5 talcum powder and weight part be that the N,N-DIMETHYLACETAMIDE of 1.5 is in high-speed mixing reaction machine, mix under Heating temperature is 300 DEG C of conditions, with the rotating speed dispersed with stirring 30min of 600rpm, obtain mixed powder;
(2) iron(ic) chloride, Repone K, polyoxyethylene glycol are mixed with intercalator with mass ratio 3:3:1, then the mixed powder that step (1) obtains are soaked more than 48h in intercalator, be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in spray formula micronizer mill, two nozzles are arranged to spray formula micronizer mill, pulverize nozzle for one and spray into crushiing chamber with the pressure of 4.0MPa, a feed introduction sprays into crushiing chamber with the pressure of 2.8MPa, powder produces the impact force of high strength in crushiing chamber with the collision of the form of jet, shearing force, frictional force, powder is repeated stock in high velocity air, in the process of cutting rubbing, talcum powder and graphite linings are constantly peeled off, by the screening of grading room, the crushiing chamber that is back to defective macrobead powder continues collision and peels off, reach the product of stripping requirement from products export output, obtain the number of plies being uniformly dispersed at 50-200 layer, good fluidity, not easily reunite graphene microchip.
embodiment 3
A kind of utilization prepares the method for graphene microchip to spray formula micronizer mill:
(1) by weight part be 85 crystalline graphite powder, weight part be 3 talcum powder and weight part be that the N,N-DIMETHYLACETAMIDE of 0.8 is in high-speed mixing reaction machine, mix under Heating temperature is 260 DEG C of conditions, with the rotating speed dispersed with stirring 45min of 400rpm, obtain mixed powder;
(2) iron(ic) chloride, Repone K, polyoxyethylene glycol are mixed with intercalator with mass ratio 2.1:2.5:1, then the mixed powder that step (1) obtains are soaked more than 48h in intercalator, be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in spray formula micronizer mill, two nozzles are arranged to spray formula micronizer mill, pulverize nozzle for one and spray into crushiing chamber with the pressure of 3.6MPa, a feed introduction sprays into crushiing chamber with the pressure of 2.5MPa, powder produces the impact force of high strength in crushiing chamber with the collision of the form of jet, shearing force, frictional force, powder is repeated stock in high velocity air, in the process of cutting rubbing, talcum powder and graphite linings are constantly peeled off, by the screening of grading room, the crushiing chamber that is back to defective macrobead powder continues collision and peels off, reach the product of stripping requirement from products export output, obtain the number of plies being uniformly dispersed at 50-200 layer, good fluidity, not easily reunite graphene microchip.
embodiment 4
A kind of utilization prepares the method for graphene microchip to spray formula micronizer mill:
(1) by weight part be 84 thermo-cracking Graphite Powder 99, weight part be 4 talcum powder and weight part be that the N,N-DIMETHYLACETAMIDE of 1.2 is in high-speed mixing reaction machine, mix under Heating temperature is 280 DEG C of conditions, with the rotating speed dispersed with stirring 45min of 500rpm, obtain mixed powder;
(2) iron(ic) chloride, Repone K, polyoxyethylene glycol are mixed with intercalator with mass ratio 2.3:2.8:1, then the mixed powder that step (1) obtains are soaked more than 48h in intercalator, be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in spray formula micronizer mill, two nozzles are arranged to spray formula micronizer mill, pulverize nozzle for one and spray into crushiing chamber with the pressure of 3.4MPa, a feed introduction sprays into crushiing chamber with the pressure of 2.6MPa, powder produces the impact force of high strength in crushiing chamber with the collision of the form of jet, shearing force, frictional force, powder is repeated stock in high velocity air, in the process of cutting rubbing, talcum powder and graphite linings are constantly peeled off, by the screening of grading room, the crushiing chamber that is back to defective macrobead powder continues collision and peels off, reach the product of stripping requirement from products export output, obtain the number of plies being uniformly dispersed at 50-200 layer, good fluidity, not easily reunite graphene microchip.
embodiment 5
A kind of utilization prepares the method for graphene microchip to spray formula micronizer mill:
(1) by weight part be 81 expanded graphite powder, weight part be 2 talcum powder and weight part be that the N,N-DIMETHYLACETAMIDE of 1.3 is in high-speed mixing reaction machine, mix under Heating temperature is 260 DEG C of conditions, with the rotating speed dispersed with stirring 35min of 360rpm, obtain mixed powder;
(2) iron(ic) chloride, Repone K, polyoxyethylene glycol are mixed with intercalator with mass ratio 2:2.5:1, then the mixed powder that step (1) obtains are soaked more than 48h in intercalator, be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in spray formula micronizer mill, two nozzles are arranged to spray formula micronizer mill, pulverize nozzle for one and spray into crushiing chamber with the pressure of 3.9MPa, a feed introduction sprays into crushiing chamber with the pressure of 2.2MPa, powder produces the impact force of high strength in crushiing chamber with the collision of the form of jet, shearing force, frictional force, powder is repeated stock in high velocity air, in the process of cutting rubbing, talcum powder and graphite linings are constantly peeled off, by the screening of grading room, the crushiing chamber that is back to defective macrobead powder continues collision and peels off, reach the product of stripping requirement from products export output, obtain the number of plies being uniformly dispersed at 50-200 layer, good fluidity, not easily reunite graphene microchip.
Claims (6)
1. one kind utilizes the method being prepared by spray formula micronizer mill to graphene microchip, it is characterized in that: first Graphite Powder 99 thermal treatment is disperseed, then interlayer is brittle, by the impact force, shearing force, the frictional force stripping graphite that produce pulverizing nozzle and the feed introduction of spray formula micronizer mill, obtain the number of plies in being uniformly dispersed of 50-200 layer, good fluidity, the graphene microchip of not easily reuniting, concrete grammar is as follows:
(1) be the Graphite Powder 99 of 80-90 by weight part, weight part be the talcum powder of 1-5 and weight part is that the N,N-DIMETHYLACETAMIDE of 0.5-1.5 is in high-speed mixing reaction machine, mix under Heating temperature is 250-300 DEG C of condition, with the rotating speed dispersed with stirring 30-60min of 300-600rpm, obtain mixed powder;
(2) iron(ic) chloride, Repone K, polyoxyethylene glycol are mixed with intercalator with mass ratio 2-3:2-3:1, then the mixed powder that step (1) obtains are soaked more than 48h in intercalator, be filtered dry by whizzer, drying obtains pre-intercalation powder;
(3) pre-intercalation powder step (2) obtained is sent in spray formula micronizer mill, two nozzles are arranged to spray formula micronizer mill, pulverize nozzle for one and spray into crushiing chamber with the pressure of 3.0-4.0MPa, a feed introduction sprays into crushiing chamber with the pressure of 2.0-2.8MPa, powder produces the impact force of high strength in crushiing chamber with the collision of the form of jet, shearing force, frictional force, powder is repeated stock in high velocity air, in the process of cutting rubbing, talcum powder and graphite linings are constantly peeled off, by the screening of grading room, the crushiing chamber that is back to defective macrobead powder continues collision and peels off, reach the product of stripping requirement from products export output, obtain the number of plies being uniformly dispersed at 50-200 layer, good fluidity, not easily reunite graphene microchip.
2. the method for graphene microchip is prepared in a kind of utilization to spray formula micronizer mill according to claim 1, it is characterized in that: Graphite Powder 99 is any one in crystalline flake graphite, expanded graphite, high orientation graphite, thermo-cracking graphite, and particle diameter is between 50 microns and 500 microns.
3. the method for graphene microchip is prepared in a kind of utilization to spray formula micronizer mill according to claim 1, it is characterized in that: talcum powder is platy talc, and particle diameter is between 50 microns and 500 microns, and radius-thickness ratio is between 1:10 and 1:20.
4. the method for graphene microchip is prepared in a kind of utilization to spray formula micronizer mill according to claim 1, it is characterized in that: nozzle, feed introduction, crushiing chamber, grading room, hopper, lining, products export are pulverized in described comprising spray formula micronizer mill.
5. the method for graphene microchip is prepared in a kind of utilization to spray formula micronizer mill according to claim 1, it is characterized in that: described is provided with feed introduction to spray formula micronizer mill and pulverizes nozzle two nozzles, described feed introduction is in crushiing chamber hopper side, inlet pressure 2.0-2.8MPa, inlet diameter 6-10mm, described pulverizing nozzle at the crushiing chamber opposite side relative with feed introduction, inlet pressure 3.0-4.0MPa, inlet diameter 6-10mm, pressure is produced by the rare gas element of compression.
6. the method for graphene microchip is prepared in a kind of utilization to spray formula micronizer mill according to claim 1, it is characterized in that: graphene microchip prepared by described method meets the application at rubber reinforcement, plastics enhancing, anticorrosion with coat, lubrication, sewage treatment area.
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