CN105523553A - Method for preparing graphene through single cold side frozen single-molecule water expansion - Google Patents
Method for preparing graphene through single cold side frozen single-molecule water expansion Download PDFInfo
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Abstract
The invention discloses a method for preparing graphene through single cold side frozen single-molecule water expansion. Blocky expanded graphite is fully immersed in deionized water, hydrogen bonds among water molecules are broken through low-frequency oscillation, the hydrogen bonds among the water molecules are broken through low-frequency electromagnetic oscillation produced by a low-frequency resonator, activated water molecules are obtained, the size of water molecular groups is reduced, the water molecules and polar additive molecules enter space among graphite layers freely, then the graphite and the water are frozen by the aid of a single cold side, the water is frozen into ice among the graphite layers, the size is increased, and the distance of the graphite layers is increased; finally, cutting and stripping are performed by the aid of a mechanical machine, and graphene products are produced through water evaporation after stripping. According to the method, deionized water and a small amount of additive are used for preparing the graphene, usage of toxic organic micromolecules is avoided, the graphene is physically stripped with the method at the low temperature, secondary defects of the graphene are reduced, besides, pollution caused by other impurity elements is reduced, and the method is environment-friendly and suitable for large-scale production.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, particularly a kind of by the anxious method of freezing the expansion of unit molecule water and preparing Graphene of single cold junction.
Background technology
Graphene has that intrinsic mobility is high, specific surface area is large, Young's modulus is high and the advantage such as rupture stress is large, is the ideal chose of conducting host materials in lithium ion battery, ultracapacitor.The Graphene preparing stable existence is on a large scale the precondition of Graphene industrialization.At present, the preparation method of Graphene mainly contains, the method such as mechanically peel method, epitaxial growth method, graphite oxide reduction method, chemical vapour deposition.Because the preparation process of graphite oxide reduction method is relatively simple, the use that its studied person is a large amount of.But defect and the oxide group of the Graphene synthesized by this method are more, limit its application in electron device.Now, liquid phase stripping method have also been obtained investigators and pays close attention to greatly, also has benefited from preparation process simple, can produce in a large number and the Graphene quality of synthesizing is higher, may be used for the fields such as electron device, becomes a kind of method of Worth Expecting.But owing to employing organic molecule in a large number as organic solvent, there is potential toxicity and synthesis complicacy, there is the problem being difficult to remove residual solvent.
In prior art, China Patent Publication No. 103623741A provides a kind of graphene dispersion agent and stripper, is made up of naphthalenetetracarbimidec imidec unit, anionic group and alkyl chain three parts.Use Graphene that described graphite dispersing agent is prepared by ultrasonic method not through the process of oxidation-reduction, defect content is low, and preparation cost is low.Although this dispersion agent is water miscible, still there is naphthalenetetracarbacidic acidic dicarboxylic anhydride unit, expensive raw material price, cost is still very high.
China Patent Publication No. 103771400A provides a kind of method utilizing pyrenyl phenylformic acid polyethers fat parents reagent to prepare graphene dispersing solution, with poly glycol monomethyl ether, para-amino benzoic acid and 1-pyrene boric acid for raw material, the para-amino benzoic acid polyether acid fat of hydrophilic long-chain is obtained by esterification, introduce the HBr with 1-pyrene acid reaction again, prepare 3,5-dibromo-benzene formic acid poly glycol monomethyl ether fat, has synthesized the graphite stripper of two property (hydrophilic and oleophilic) then again with 1-pyrene acid reaction; This compound and Graphene are dissolved in H
2in O/EtOH solution, carry out twice ultrasonic, after leaving standstill process, then obtain stable graphene dispersing solution through centrifugal.The present invention is without the need to carrying out redox to Graphene, therefore minimum to the destructiveness of graphene-structured, can give full play to conduction and the heat conductivility of Graphene uniqueness; The dispersion liquid of preparation has good aqueous phase stability, for Graphene provides an effective approach in the application of field of compound material.But still use pyrenyl phenylformic acid polyethers fat parents reagent as important source material in the method, environmental pollution is serious, reclaim complicated, cost intensive.
In sum, a kind of water miscible Graphene stripping means of pollution-free, good stability is not also had in present existing method.
Summary of the invention
Block expanded graphite is fully immersed in deionized water by the present invention, the hydrogen bond interrupted between water molecules is obtained by low-frequency oscillation, interrupt the hydrogen bond between water molecules by low-frequency resonance instrument generation low frequency electromagnetic oscillation, obtain activated water molecule, reduce the size of water clusters, water molecules and polar additive molecule is made freely to enter graphite layers, then use single cold junction, freezing graphite and water, water is frozen into ice in graphite layers, volume increases, and increases graphite layers distance.Finally, sheared by mechanical machine and peel off, after peeling off, vaporize water produces graphene product.
The invention provides a kind of by the anxious method of freezing the expansion of unit molecule water and preparing Graphene of single cold junction, it is characterized in that, said method comprising the steps of:
A. using block expanded graphite as raw material, described raw material and polar additive are placed in the stainless steel vessel that deionized water is housed, the mass ratio of described raw material and described polar additive, described deionized water three is 1:0.01 ~ 0.2:10 ~ 25, be uniformly mixed solution to be uniformly distributed to raw material, low frequency electromagnetic oscillation is produced by low-frequency resonance instrument, reduce the size of water clusters, make water molecules and described polar additive freely enter graphite layers, constantly stir in low frequency electromagnetic oscillation process;
B. by lowering the temperature rapidly to one end of described container, deionized water in described container is solidified, obtain low temperature solid-state composite graphite material, by low temperature solid-state composite graphite material described in screw extrusion press or Counter-impact flow pulverizer mechanically peel, obtain mechanically peel product;
C., under the condition passing into shielding gas, described mechanically peel product is warming up to 200 ~ 300 DEG C, deionized water is vaporized, after cooling, obtains Graphene.
Preferably, described polar additive be sheet footpath size the graphene oxide quantum dot of 20 ~ 80nm or with phenyl ring, naphthalene nucleus or pyridine ring for main body rack, comprise one or more hydroxyl or organic molecule that is amino and carboxyl.
Preferably, the frequency of described low frequency electromagnetic oscillation is 7.2 ~ 8.2Hz.
Preferably, employing temperature is that the cold head of-200 ~-100 DEG C is lowered the temperature to described container, and cooling rate is 10 ~ 50 DEG C/s.
Preferably, the screw speed of described screw extrusion press is 100 ~ 600 revs/min.
Preferably, the gas velocity of described Counter-impact flow pulverizer is 2.5 ~ 5 Mach.
Above-mentioned one or more technical scheme in the embodiment of the present application, at least has one or more technique effects following:
1, adopt deionization and a small amount of additive to prepare Graphene in the program, avoid the use of toxicity organic molecule, and program physics stripping Graphene at low temperatures, reduce the secondary defect of Graphene.
2, the program adopts the water of the freezing graphite layers of single cold junction, water molecules is solidified and has directivity, avoid the homogeneous nucleation growth process that even refrigerating process causes, the volume orientation that water cure is caused expands, strut graphite layers distance, interrupt Van der Waals key.
3, the deionized water that the program uses can recycle, and technique is simple, with low cost, decreases the pollution of other impurity elements, environmental protection, applicable scale operation.
Accompanying drawing explanation
Fig. 1 is a kind of by the anxious Method And Principle schematic diagram freezing the expansion of unit molecule water and prepare Graphene of single cold junction in the embodiment of the present application.
Embodiment
By 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 one
Fig. 1 is a kind of by the anxious Method And Principle schematic diagram freezing the expansion of unit molecule water and prepare Graphene of single cold junction in the embodiment of the present application, and 1 is container, 2 ice solidify to form for water molecules, and 3 is graphite synusia, and 4 is freezing end.Concrete implementation step is as follows:
Get block expanded graphite 1kg as raw material, the graphene oxide quantum dot that block for 1kg expanded graphite and 15g sheet footpath are of a size of 20nm is placed in the stainless steel vessel that 10kg is equipped with deionized water, constantly be uniformly mixed solution to be uniformly distributed to raw material, the low-frequency resonance instrument generation low frequency electromagnetic oscillation being 7.2Hz by the frequency of electromagnetic oscillation interrupts the hydrogen bond between deionized water water molecules, deionized water is activated, obtain activated water molecule, and then reduce the size of deionized water water clusters, allow water molecules easily carry graphene oxide quantum dot further and freely enter graphite layers, constantly stir in low frequency electromagnetic oscillation process.Next, by lowering the temperature rapidly to one end of container, in an embodiment, container can be cylindrical vessel, cuboid container, square container, does not just illustrate one by one at this.The vessel faces at freezing end place is set according to the shape of container, in the present embodiment, cylindrical vessel is selected to be the device holding raw material, freezing end is arranged on cylindrical chamber rounded bottom or circular top is preferred version, certainly, freezing end also as required, can be arranged on a certain region of cylindrical cylinder by those skilled in the art.Freezing end temperature is the copper cold head of-200 DEG C, be that 10 DEG C/s lowers the temperature to cylindrical vessel with cooling rate, deionized water in container is solidified, like this due to thermograde, one end close to copper cold head is solidified at the deionized water of graphite layers, volume increases, the spacing of graphite layers increases because deionized water solidifies, along with the time increases, due to thermograde, raw material away from freezing end also solidifies gradually, and the directive directional freeze of tool makes graphite slowly softened in an orderly manner, obtains whole low temperature solid-state composite graphite material.Next, arranging screw speed is 100 revs/min, by low temperature solid-state composite graphite material described in screw extrusion press mechanically peel, obtains mechanically peel product.Mechanically peel product is taken out, is passing into N
2condition under, mechanically peel product is warming up to 200 DEG C, deionized water is vaporized, after cooling, obtains Graphene.
Embodiment two
Fig. 1 is a kind of by the anxious Method And Principle schematic diagram freezing the expansion of unit molecule water and prepare Graphene of single cold junction in the embodiment of the present application, and 1 is container, 2 ice solidify to form for water molecules, and 3 is graphite synusia, and 4 is freezing end.Concrete implementation step is as follows:
Get block expanded graphite 1kg as raw material, the graphene oxide quantum dot that block for 1kg expanded graphite and 200g sheet footpath are of a size of 70nm is placed in the stainless steel vessel that 20kg is equipped with deionized water, constantly be uniformly mixed solution to be uniformly distributed to raw material, the low-frequency resonance instrument generation low frequency electromagnetic oscillation being 7.2Hz by the frequency of electromagnetic oscillation interrupts the hydrogen bond between deionized water water molecules, deionized water is activated, obtain activated water molecule, and then reduce the size of deionized water water clusters, allow water molecules easily carry graphene oxide quantum dot further and freely enter graphite layers, constantly stir in low frequency electromagnetic oscillation process.Next, by lowering the temperature rapidly to one end of container, in an embodiment, container can be cylindrical vessel, cuboid container, square container, does not just illustrate one by one at this.The vessel faces at freezing end place is set according to the shape of container, in the present embodiment, cylindrical vessel is selected to be the device holding raw material, freezing end is arranged on cylindrical chamber rounded bottom or circular top is preferred version, certainly, freezing end also as required, can be arranged on a certain region of cylindrical cylinder by those skilled in the art.Freezing end temperature is the copper cold head of-200 DEG C, be that 10 DEG C/s lowers the temperature to cylindrical vessel with cooling rate, deionized water in container is solidified, like this due to thermograde, one end close to copper cold head is solidified at the deionized water of graphite layers, volume increases, the spacing of graphite layers increases because deionized water solidifies, along with the time increases, due to thermograde, raw material away from freezing end also solidifies gradually, and the directive directional freeze of tool makes graphite slowly softened in an orderly manner, obtains whole low temperature solid-state composite graphite material.Next, arranging screw speed is 100 revs/min, by low temperature solid-state composite graphite material described in screw extrusion press mechanically peel, obtains mechanically peel product.Mechanically peel product is taken out, is passing into N
2condition under, mechanically peel product is warming up to 200 DEG C, deionized water is vaporized, after cooling, obtains Graphene.
Embodiment three
Fig. 1 is a kind of by the anxious Method And Principle schematic diagram freezing the expansion of unit molecule water and prepare Graphene of single cold junction in the embodiment of the present application, and 1 is container, 2 ice solidify to form for water molecules, and 3 is graphite synusia, and 4 is freezing end.Concrete implementation step is as follows:
Get block expanded graphite 1kg as raw material, the graphene oxide quantum dot that block for 1kg expanded graphite and 200g sheet footpath are of a size of 70nm is placed in the stainless steel vessel that 20kg is equipped with deionized water, constantly be uniformly mixed solution to be uniformly distributed to raw material, the low-frequency resonance instrument generation low frequency electromagnetic oscillation being 8.2Hz by the frequency of electromagnetic oscillation interrupts the hydrogen bond between deionized water water molecules, deionized water is activated, obtain activated water molecule, and then reduce the size of deionized water water clusters, allow water molecules easily carry graphene oxide quantum dot further and freely enter graphite layers, constantly stir in low frequency electromagnetic oscillation process.Next, by lowering the temperature rapidly to one end of container, in an embodiment, container can be cylindrical vessel, cuboid container, and square describes device, does not just illustrate one by one at this.The vessel faces at freezing end place is set according to the shape of container, in the present embodiment, select long: wide: the high cuboid container for 3:2:1 is the device holding raw material, freezing end is arranged on the face at the wide high place of cuboid container, certainly, freezing end also as required, can be arranged on other faces of cuboid container by those skilled in the art.Freezing end temperature is the copper cold head of-200 DEG C, be that 10 DEG C/s lowers the temperature to cuboid container with cooling rate, deionized water in container is solidified, like this due to thermograde, one end close to copper cold head is solidified at the deionized water of graphite layers, volume increases, the spacing of graphite layers increases because deionized water solidifies, along with the time increases, due to thermograde, raw material away from freezing end also solidifies gradually, and the directive directional freeze of tool makes graphite slowly softened in an orderly manner, obtains whole low temperature solid-state composite graphite material.Next, arranging screw speed is 100 revs/min, by low temperature solid-state composite graphite material described in screw extrusion press mechanically peel, obtains mechanically peel product.Mechanically peel product is taken out, is passing into N
2condition under, mechanically peel product is warming up to 200 DEG C, deionized water is vaporized, after cooling, obtains Graphene.
Embodiment four
Fig. 1 is a kind of by the anxious Method And Principle schematic diagram freezing the expansion of unit molecule water and prepare Graphene of single cold junction in the embodiment of the present application, and 1 is container, 2 ice solidify to form for water molecules, and 3 is graphite synusia, and 4 is freezing end.Concrete implementation step is as follows:
Get block expanded graphite 1kg as raw material, the graphene oxide quantum dot that block for 1kg expanded graphite and 200g sheet footpath are of a size of 70nm is placed in the stainless steel vessel that 20kg is equipped with deionized water, constantly be uniformly mixed solution to be uniformly distributed to raw material, the low-frequency resonance instrument generation low frequency electromagnetic oscillation being 8.2Hz by the frequency of electromagnetic oscillation interrupts the hydrogen bond between deionized water water molecules, deionized water is activated, obtain activated water molecule, and then reduce the size of deionized water water clusters, allow water molecules easily carry graphene oxide quantum dot further and freely enter graphite layers, constantly stir in low frequency electromagnetic oscillation process.Next, by lowering the temperature rapidly to one end of container, in an embodiment, container can be cylindrical vessel, cuboid container, and square describes device, does not just illustrate one by one at this.The vessel faces at freezing end place is set according to the shape of container, in the present embodiment, select long: wide: the high cuboid container for 3:2:1 is the device holding raw material, freezing end is arranged on the face at the wide high place of cuboid container, certainly, freezing end also as required, can be arranged on other faces of cuboid container by those skilled in the art.Freezing end temperature is the copper cold head of-150 DEG C, be that 50 DEG C/s lowers the temperature to cuboid container with cooling rate, deionized water in container is solidified, like this due to thermograde, one end close to copper cold head is solidified at the deionized water of graphite layers, volume increases, the spacing of graphite layers increases because deionized water solidifies, along with the time increases, due to thermograde, raw material away from freezing end also solidifies gradually, and the directive directional freeze of tool makes graphite slowly softened in an orderly manner, obtains whole low temperature solid-state composite graphite material.Next, arranging screw speed is 100 revs/min, by low temperature solid-state composite graphite material described in screw extrusion press mechanically peel, obtains mechanically peel product.Mechanically peel product is taken out, is passing into N
2condition under, mechanically peel product is warming up to 200 DEG C, deionized water is vaporized, after cooling, obtains Graphene.
Embodiment five
Fig. 1 is a kind of by the anxious Method And Principle schematic diagram freezing the expansion of unit molecule water and prepare Graphene of single cold junction in the embodiment of the present application, and 1 is container, 2 ice solidify to form for water molecules, and 3 is graphite synusia, and 4 is freezing end.Concrete implementation step is as follows:
Get block expanded graphite 1kg as raw material, the graphene oxide quantum dot that block for 1kg expanded graphite and 200g sheet footpath are of a size of 70nm is placed in the stainless steel vessel that 20kg is equipped with deionized water, constantly be uniformly mixed solution to be uniformly distributed to raw material, the low-frequency resonance instrument generation low frequency electromagnetic oscillation being 8.2Hz by the frequency of electromagnetic oscillation interrupts the hydrogen bond between deionized water water molecules, deionized water is activated, obtain activated water molecule, and then reduce the size of deionized water water clusters, allow water molecules easily carry graphene oxide quantum dot further and freely enter graphite layers, constantly stir in low frequency electromagnetic oscillation process.Next, by lowering the temperature rapidly to one end of container, in an embodiment, container can be cylindrical vessel, cuboid container, and square describes device, does not just illustrate one by one at this.The vessel faces at freezing end place is set according to the shape of container, in the present embodiment, select long: wide: the high cuboid container for 3:2:1 is the device holding raw material, freezing end is arranged on the face at the wide high place of cuboid container, certainly, freezing end also as required, can be arranged on other faces of cuboid container by those skilled in the art.Freezing end temperature is the copper cold head of-150 DEG C, be that 50 DEG C/s lowers the temperature to cuboid container with cooling rate, deionized water in container is solidified, like this due to thermograde, one end close to copper cold head is solidified at the deionized water of graphite layers, volume increases, the spacing of graphite layers increases because deionized water solidifies, along with the time increases, due to thermograde, raw material away from freezing end also solidifies gradually, and the directive directional freeze of tool makes graphite slowly softened in an orderly manner, obtains whole low temperature solid-state composite graphite material.Next, arranging screw speed is 100 revs/min, by low temperature solid-state composite graphite material described in screw extrusion press mechanically peel, obtains mechanically peel product.Mechanically peel product is taken out, is passing into N
2condition under, mechanically peel product is warming up to 200 DEG C, deionized water is vaporized, after cooling, obtains Graphene.
Embodiment six
Fig. 1 is a kind of by the anxious Method And Principle schematic diagram freezing the expansion of unit molecule water and prepare Graphene of single cold junction in the embodiment of the present application, and 1 is container, 2 ice solidify to form for water molecules, and 3 is graphite synusia, and 4 is freezing end.Concrete implementation step is as follows:
Get block expanded graphite 1kg as raw material, the graphene oxide quantum dot that block for 1kg expanded graphite and 200g sheet footpath are of a size of 70nm is placed in the stainless steel vessel that 20kg is equipped with deionized water, constantly be uniformly mixed solution to be uniformly distributed to raw material, the low-frequency resonance instrument generation low frequency electromagnetic oscillation being 8.2Hz by the frequency of electromagnetic oscillation interrupts the hydrogen bond between deionized water water molecules, deionized water is activated, obtain activated water molecule, and then reduce the size of deionized water water clusters, allow water molecules easily carry graphene oxide quantum dot further and freely enter graphite layers, constantly stir in low frequency electromagnetic oscillation process.Next, by lowering the temperature rapidly to one end of container, in an embodiment, container can be cylindrical vessel, cuboid container, and square describes device, does not just illustrate one by one at this.The vessel faces at freezing end place is set according to the shape of container, in the present embodiment, select long: wide: the high cuboid container for 3:2:1 is the device holding raw material, freezing end is arranged on the face at the wide high place of cuboid container, certainly, freezing end also as required, can be arranged on other faces of cuboid container by those skilled in the art.Freezing end temperature is the copper cold head of-150 DEG C, be that 50 DEG C/s lowers the temperature to cuboid container with cooling rate, deionized water in container is solidified, like this due to thermograde, one end close to copper cold head is solidified at the deionized water of graphite layers, volume increases, the spacing of graphite layers increases because deionized water solidifies, along with the time increases, due to thermograde, raw material away from freezing end also solidifies gradually, and the directive directional freeze of tool makes graphite slowly softened in an orderly manner, obtains whole low temperature solid-state composite graphite material.Next, the gas velocity arranging Counter-impact flow pulverizer is 2.5 Mach, by Counter-impact flow pulverizer mechanically peel low temperature solid-state composite graphite material, obtains mechanically peel product.Mechanically peel product is taken out, is passing into N
2condition under, mechanically peel product is warming up to 200 DEG C, deionized water is vaporized, after cooling, obtains Graphene.
Although describe the preferred embodiments of the present invention, those skilled in the art once obtain the basic creative concept of cicada, then can make other change and amendment to these embodiments.So claims are intended to be interpreted as comprising preferred embodiment and falling into all changes and the amendment of the scope of the invention.
Obviously, those skilled in the art can carry out various change and modification to the present invention and not depart from the spirit and scope of the present invention.Like this, if these amendments of the present invention and modification belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these change and modification.
Claims (6)
1., by the anxious method of freezing the expansion of unit molecule water and preparing Graphene of single cold junction, it is characterized in that, said method comprising the steps of:
A. using block expanded graphite as raw material, described raw material and polar additive are placed in the stainless steel vessel that deionized water is housed, the mass ratio of described raw material and described polar additive, described deionized water three is 1:0.01 ~ 0.2:10 ~ 25, be uniformly mixed solution to be uniformly distributed to raw material, low frequency electromagnetic oscillation is produced by low-frequency resonance instrument, reduce the size of water clusters, make water molecules and described polar additive freely enter graphite layers, constantly stir in low frequency electromagnetic oscillation process;
B. by lowering the temperature rapidly to one end of described container, deionized water in described container is solidified, obtain low temperature solid-state composite graphite material, by low temperature solid-state composite graphite material described in screw extrusion press or Counter-impact flow pulverizer mechanically peel, obtain mechanically peel product;
C., under the condition passing into shielding gas, described mechanically peel product is warming up to 200 ~ 300 DEG C, deionized water is vaporized, after cooling, obtains Graphene.
2. according to claim 1 a kind of by the anxious method of freezing the expansion of unit molecule water and preparing Graphene of single cold junction, it is characterized in that, described polar additive be sheet footpath size the graphene oxide quantum dot of 20 ~ 80nm or with phenyl ring, naphthalene nucleus or pyridine ring for main body rack, comprise one or more hydroxyl or organic molecule that is amino and carboxyl.
3. according to claim 1 a kind of by the anxious method of freezing the expansion of unit molecule water and preparing Graphene of single cold junction, it is characterized in that, the frequency of described low frequency electromagnetic oscillation is 7.2 ~ 8.2Hz.
4. according to claim 1ly a kind ofly expanded prepared the method for Graphene by the anxious unit molecule water that freezes of single cold junction, it is characterized in that, adopt temperature to be that the cold head of-200 ~-100 DEG C is lowered the temperature to described container, cooling rate is 10 ~ 50 DEG C/s.
5. according to claim 1 a kind of by the anxious method of freezing the expansion of unit molecule water and preparing Graphene of single cold junction, it is characterized in that, the screw speed of described screw extrusion press is 100 ~ 600 revs/min.
6. according to claim 1 a kind of by the anxious method of freezing the expansion of unit molecule water and preparing Graphene of single cold junction, it is characterized in that, the gas velocity of described Counter-impact flow pulverizer is 2.5 ~ 5 Mach.
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| CN114455575A (en) * | 2022-01-28 | 2022-05-10 | 中安新材料(深圳)有限公司 | Graphene and preparation method and application thereof |
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