CN109292765B - Method for preparing reduced graphene oxide with low layer number - Google Patents
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Abstract
The invention provides a method for preparing reduced graphene oxide with a low layer number. The method may comprise the steps of: dispersing graphene oxide having a first layer number in water, and forming a graphene oxide hydrogel; placing the hydrogel at a first temperature and a first pressure to condense water molecules in the graphene oxide hydrogel into ice molecules and desublimate the ice molecules, thereby obtaining graphene oxide with a second layer number; placing the graphene oxide with the second layer number in an inert atmosphere; and (3) rapidly heating the graphene oxide with the second layer number to more than 500 ℃ through microwave and light wave irradiation so as to decompose functional groups carried by the graphene oxide and reduce the layer number of the graphene oxide, thereby obtaining the reduced graphene oxide, wherein the microwave can penetrate through the graphene oxide in a traveling wave manner. The beneficial effects of the invention include: the structure of the graphite oxide sheet layer cannot be damaged in the freeze drying process, and the obtained graphene oxide product has fewer layers and larger specific surface area; the optical microwave has the advantages of high heating speed, uniform heating and high reduction efficiency on the graphene oxide, and can realize selective oxidation on the graphene oxide.
Description
Technical Field
The invention relates to the field of reduction of graphene oxide, in particular to a method for preparing reduced graphene oxide with a low layer number.
Background
Graphene oxide is a product obtained by chemically oxidizing graphite, has a large number of functional groups such as hydroxyl, carboxyl, epoxy and the like on the surface, has a high specific surface area, and is widely applied to the fields of analysis and detection, modified polymer materials, biomedicine, photoelectric correlation and photocatalysis. The existing preparation method has a large number of graphene oxide layers, for example, tens of graphene oxide layers, which affects the quality of graphene prepared from the graphene oxide layers.
Due to the characteristics of graphene oxide, chemical reagent reduction (such as chemical reducing agents like sodium borohydride, hydrogen iodide, ascorbic acid and the like), high-temperature thermal reduction, plasma methods and the like are mostly adopted in the market at present. The existing graphene oxide reduction method has the following problems in the production process: firstly, a large amount of chemical reagents are needed for reduction by adopting the chemical reagents, so that the number of by-products is increased, the difficulty of subsequent cleaning is increased, the environmental protection risk is increased, and the cost is increased; secondly, high-temperature thermal reduction is adopted, the reduction temperature of the graphene oxide is high, the quality uniformity of products obtained at different reduction temperatures cannot be guaranteed, and meanwhile, the problems of increase of ash content of the products, serious corrosion of equipment and the like are caused; thirdly, other reduction methods (such as plasma) are adopted, the production technology difficulty and the cost are multiplied, and the industrial large-scale application cannot be obtained.
Disclosure of Invention
In view of the deficiencies in the prior art, it is an object of the present invention to address one or more of the problems in the prior art as set forth above. For example, an object of the present invention is to provide a method for producing reduced graphene oxide having a low number of layers, which is capable of efficiently decomposing functional groups on graphene oxide and obtaining reduced graphene oxide having a low number of layers.
In order to achieve the above object, the present invention provides a method for preparing reduced graphene oxide with a low number of layers. The method may comprise the steps of:
dispersing graphene oxide having a first layer number in water, and forming a graphene oxide hydrogel; placing the graphene oxide hydrogel at a first temperature and a first pressure to condense water molecules in the graphene oxide hydrogel into ice molecules and desublimate the ice molecules, so that graphene oxide with a second layer number is obtained, wherein the first layer number is tens of layers to tens of layers, the second layer number is smaller than the first layer number, the first temperature is not higher than-50 ℃ and the temperature change is not more than +/-4 ℃, and the first pressure is lower than 1 atmosphere and the pressure change is not more than +/-100 Pa; placing the graphene oxide with the second layer number in an inert atmosphere; and (3) rapidly heating the graphene oxide with the second layer number to more than 500 ℃ through microwave and light wave irradiation so as to decompose functional groups carried by the graphene oxide and reduce the layer number of the graphene oxide, thereby obtaining the reduced graphene oxide, wherein the microwave can penetrate through the graphene oxide in a traveling wave manner.
According to an exemplary embodiment of the present invention, the first number of layers may be 20 to 30 layers, and the second number of layers may be 5 to 7 layers.
According to an exemplary embodiment of the invention, the first temperature may be selected in the range of-55 to-65 ℃ and the temperature may not vary by more than ± 2 ℃.
According to an exemplary embodiment of the present invention, the first pressure may be selected within a range of 10 to 100Pa and a variation of the pressure is not more than + -10 Pa.
According to an exemplary embodiment of the present invention, the graphene oxide hydrogel may have a solid content of 0.1 to 50 wt%.
According to an exemplary embodiment of the present invention, the step of placing the graphene oxide having the second number of layers in an inert atmosphere may include: feeding the graphene oxide with the second layer number into a tubular container filled with nitrogen or inert gas through gas; wherein both ends of the tubular container have openings, the gas is capable of flowing in from one opening of the tubular container, and the gas comprises nitrogen or inert gas.
According to an exemplary embodiment of the present invention, the method may further comprise the steps of: after obtaining the reduced graphene oxide, taking the reduced graphene oxide out of the other opening of the tubular container by means of suction filtration.
According to an exemplary embodiment of the invention, the flow rate of the gas in the tubular container may be at 10cm3Less than s, e.g. 1 to 8cm3S; the amount of the gas capable of being fed into the graphene oxide can be 1g/cm3Below, for example, 0.5. + -. 0.3g/cm3。
According to an exemplary embodiment of the present invention, the irradiation time of the light waves and microwaves may be below 10min, for example, 5 ± 3 min.
According to an exemplary embodiment of the present invention, the direction of the microwave and light wave irradiation and the direction of the gas flow within the tubular container may be perpendicular to each other.
According to an exemplary embodiment of the present invention, a degree of vacuum inside the tubular container may be below 100 Pa.
According to an exemplary embodiment of the present invention, the tubular container may include a quartz tube, and the microwave and light waves may irradiate the graphene oxide through a wall of the quartz tube.
According to an exemplary embodiment of the present invention, the light wave may include infrared rays or far infrared rays.
According to an exemplary embodiment of the present invention, the method may further comprise the steps of: and cooling and drying the obtained reduced graphene oxide.
Compared with the prior art, the invention has the beneficial effects that: the structure of the graphite oxide sheet layer cannot be damaged in the freeze drying process, the layer-to-layer distance of the freeze-dried graphene oxide sheet is larger than that of the graphene oxide product dried by other drying methods, and the graphene oxide sheet has fewer layers and larger specific surface area; the heating speed in the optical microwave reduction process is high, the heating is uniform, the thermal inertia is avoided, the energy is saved, the efficiency is high, the reduction efficiency is high, and the selective oxidation of the graphene oxide can be realized.
Drawings
The above and other objects and features of the present invention will become more apparent from the following description taken in conjunction with the accompanying drawings, in which:
fig. 1 shows a schematic flow diagram of a method for preparing reduced graphene oxide with a low number of layers in an exemplary embodiment of the invention;
FIG. 2 is a schematic diagram illustrating the positional relationship of a microwave and lightwave radiation system with a tubular container in an exemplary embodiment of the invention.
The main illustration is as follows:
1-a quartz tube; 2-a light wave tube; 3-microwave cavity.
Detailed Description
Hereinafter, the method for preparing reduced graphene oxide with a low number of layers according to the present invention will be described in detail with reference to the accompanying drawings and exemplary embodiments.
Graphene oxide can be used as a raw material for preparing graphene, and the quality of the prepared graphene is influenced by the high graphene oxide number. The conventional heating method is that heat is firstly transferred to the surface of an object through heat conduction, convection, heat radiation and the like, and then the central temperature of the object is gradually raised through heat conduction. Therefore, the invention provides a method for preparing reduced graphene oxide with a low layer number by using low-temperature cold drying and optical microwave reduction.
Fig. 1 shows a schematic flow diagram of a method for preparing reduced graphene oxide with a low number of layers in an exemplary embodiment of the invention. FIG. 2 is a schematic diagram illustrating the positional relationship of a microwave and lightwave radiation system with a tubular container in an exemplary embodiment of the invention.
In an exemplary embodiment of the present invention, the method of preparing a reduced graphene oxide with a low number of layers may include the steps of:
the graphene oxide having the first number of layers is dispersed in water, and a graphene oxide hydrogel is formed, as in step S01 in fig. 1. In the dispersing process, the dispersing effect is preferably further enhanced by ultrasonic dispersion, so that water molecules fully enter a lamellar structure or folds of the graphene oxide, or are combined with functional groups on the surface of the graphene oxide to form hydrated ions, thereby forming the graphene oxide hydrogel. The graphene oxide hydrogel has a structure in which water molecules are bonded in its own sheet or wrinkle of graphene oxide. The solid content of the graphene oxide hydrogel can be 0.1-50 wt%. The water used for dispersing the graphene oxide is preferably secondary deionized water.
And placing the graphene oxide hydrogel at a first temperature and a first pressure to condense water molecules in the graphene oxide hydrogel into ice molecules and desublimate the ice molecules, so that the graphene oxide with a second layer number is obtained. And the first temperature is controlled to be not higher than-50 ℃ and the temperature variation of the first temperature is always not more than + -4 ℃, the first pressure is controlled to be lower than 1 atmosphere and the variation of the first pressure is always not more than + -100 Pa. Further, the first temperature may be selected within the range of-55 to-65 ℃ and the temperature variation does not exceed ± 2 ℃. The first pressure intensity can be selected within the range of 10-100 Pa, and the pressure intensity variation does not exceed +/-10 Pa. The second layer number is smaller than the first layer number. The second layer number is smaller than the first layer number. The second number of layers may have a significant reduction compared to the first number of layers. Here, the second number of layers may be 1/3-1/6 of the first number of layers. For example, the second number of layers may be 5 to 7.
The graphene oxide having the second layer number is placed in an inert atmosphere, as in step S03 in fig. 1. For example, the graphene oxide having the second number of layers may be fed into a container filled with nitrogen or an inert gas. Wherein the container may comprise a tubular container having openings at both ends. Further, a tubular container which is horizontally and transversely arranged and has openings at the left end and the right end can be included.
And rapidly heating the graphene oxide with the second layer number to more than 500 ℃ by microwave and light wave irradiation to decompose the functional groups carried by the graphene oxide and reduce the layer number of the graphene oxide, so as to obtain reduced graphene oxide (namely the reduced graphene oxide), as shown in step S04 in fig. 1. The microwave can penetrate through the graphene oxide in a traveling wave mode, and a constantly transmitted traveling wave waveform is formed through the unidirectional transmission of the microwave, so that the local high temperature phenomenon caused by the standing wave effect can be avoided, and the processing consistency of the graphene oxide can be improved. The frequency of the microwave can be 300MHz to 300GHz, and further can be 800MHz to 250 GHz. The frequency of the optical wave may be 3 × 1011～3.8×1014Hz, further, may be 2X 1012～2.5×1014Hz. Through the simultaneous action of microwave and light wave, the graphene oxide can be rapidly heated to more than 500 ℃, the functional group carried by the graphene oxide can be rapidly decomposed, and a large amount of gas such as water vapor, carbon dioxide and the like can be instantly generated during decomposition due to the oxygen-containing functional groupThe generated gas expands among graphene oxide sheet layers, so that the number of layers of the prepared material is smaller, and the specific surface area is larger. Further, the microwave and the light wave can enable the temperature of the graphene oxide to rise to 500-1000 ℃, such as 800 +/-150 ℃. The main heating source in the heating process can be microwaves, the light waves can play an auxiliary role, and the combination of the microwaves and the light waves can quickly raise the temperature of the heated graphene oxide, so that the deoxidation treatment is facilitated.
In this embodiment, the number of layers of graphene oxide as a raw material may be several tens of layers or more, for example, 30 to 50. The number of layers of the graphene oxide after low-temperature cold drying can be less than 10, for example, 6 to 8.
Because the number of layers of the reduction object by the optical microwave is low, the number of layers of the reduced graphene oxide obtained by the reaction can be lower, such as less than 4 layers, even less than 3 layers; and functional groups on the graphene oxide can be fully removed, and the removal rate can reach more than 95%.
In the embodiment, the first temperature is controlled to be not higher than-50 ℃ and the first pressure is controlled to be not higher than 1 standard atmospheric pressure, so that water molecules can be changed into ice molecules, and the lamellar structure of the graphite is further widened through volume expansion; and the ice can be desublimated and volatilized at low temperature and low pressure, the temperature is low, the entropy value is low, the strutted structure of the graphene oxide can be maintained, and the prepared graphene oxide material has good dispersibility and large specific surface area. Moreover, the relatively constant low temperature (for example, not higher than-50 ℃ and the temperature variation in the cavity of the whole cold dry cavity is controlled not to exceed +/-4 ℃) and the relatively constant vacuum degree (for example, lower than 1 atmosphere and the pressure variation in the whole cavity is controlled not to exceed +/-100 Pa) are beneficial to relatively stabilizing the condensation speed and degree of water molecules, so that the 'opening' effect on the graphene oxide layer is stable; but also the ice molecule desublimation speed and degree are relatively stable, thus being beneficial to avoiding local defects caused by the local stress of the graphene oxide layer to a certain degree. Furthermore, the temperature control unit and the pressure control unit are used for controlling the atmosphere of the cold drying cavity to be within the range of-55 to-65 ℃, the temperature change in the whole cavity is controlled not to exceed +/-2 ℃, the pressure is controlled to be 10 to 100Pa, the pressure change in the whole cavity is controlled not to exceed +/-10 Pa, the condensation speed and the degree of water molecules are further stabilized, and the opening effect of the graphene oxide layer is stabilized; but also the ice molecule desublimation speed and degree are further stabilized, thereby further avoiding local defects caused by the local stress of the graphene oxide layer.
In this embodiment, the graphene oxide may be fed into the tubular container by a gas flow. The resulting reduced graphene oxide may also be conveyed out of the tubular vessel by a gas stream. In other words, the gas flow loaded with graphene oxide can be introduced into one opening of the tubular container; the gas stream can carry (or push) the material through the cavity of the tubular container; during the flowing process, the graphene oxide can be reduced into reduced graphene oxide; the resulting gas stream carries (or pushes) the reduced graphene oxide out of the other opening of the tubular vessel. The gas in the gas stream may comprise nitrogen or an inert gas.
Wherein the flow rate of gas in the pipe container can be 10cm3The flow rate of the gas is controlled to be in the range below the second temperature range, so that the graphene oxide can be sufficiently reduced by the microwave. Further, the gas flow velocity can be 0.01-8 cm3And/s, and further, 2 to 5cm3/s。
The amount of graphene oxide loaded (or carried) on the gas stream may be 10g/cm3Below, for example, 0.1 to 10g/cm3Further, it may be 2 to 10g/cm3。
Aiming at the graphene oxide, the power of the microwave can be 45-55 KW. The treatment time of the light wave and the microwave is the same, and can be controlled below 10mim, such as 30s, 2min or 7 min.
In this embodiment, the selective oxidation of graphene oxide can be realized through the power of optical microwaves and the processing time, that is, reduced graphene oxide with different oxygen contents can be obtained according to the requirement.
In this embodiment, the directions of the microwave and light wave irradiation may be perpendicular to the direction of the gas flow. Can make light wave and microwave can be better pierce through graphite oxide like this, abundant irradiation avoids leading to the microwave reflection because of the material volume grow, and then influences the irradiation of deep granule.
In this embodiment, the tubular container may comprise a quartz tube disposed laterally. The quartz tube is transparent, cannot isolate the penetrating effect of light and microwaves, and has the non-blocking characteristic to light waves and microwaves, namely, the microwaves and the light waves can penetrate through the wall of the quartz tube to irradiate the graphene oxide. The quartz tube is high temperature resistant, has extremely low thermal expansion coefficient, excellent chemical stability, excellent electrical insulation and extremely high microwave permeability. The quartz tube can resist high temperature and can bear rapid cooling and rapid heating; can bear the impact of positive and negative pressure more than 1 Mpa.
In this embodiment, the method may further include the steps of: after obtaining the reduced graphene oxide, taking the reduced graphene oxide out of the other opening of the tubular container by means of suction filtration. After suction filtration, the method further comprises the steps of: and the reduced graphene oxide can be separated from the gas, and the separated gas can be recycled.
In this embodiment, the present invention can emit microwaves through a microwave system, and the microwave system can include a microwave source, a microwave cavity, and a microwave leakage prevention mechanism. The microwave source is an electronic device for generating microwave energy and can be composed of a magnetron, a high-voltage transformer, a high-voltage rectification loop, a heat dissipation fan, an over-current protection device, an abnormal temperature protection device, a waveguide and the like. The microwave cavity is the primary storage vessel for microwave energy and is also the primary region of the microwave puffing reaction. The leakage prevention mechanism can prevent leakage of microwaves.
The invention can emit light waves through a plurality of light wave tubes. The light wave mainly plays a role in heating and warming. The light wave may include infrared rays or far infrared rays.
As shown in fig. 2, the microwave cavity 3 of the microwave system may surround the quartz tube 2, so that the microwave may sufficiently and uniformly irradiate the graphene oxide through the tube wall of the quartz tube in a traveling wave manner; the two light wave tubes 2 can be distributed on two sides of the quartz tube, so that light waves can penetrate through the wall of the quartz tube to irradiate the graphene oxide fully and uniformly. Under the synergistic effect of light waves and microwaves, the graphene oxide can be rapidly heated.
In this embodiment, the reduction of the graphene oxide can be performed in a vacuum environment, which can avoid the influence of air, because the air easily conducts heat away. The vacuum degree in the container may be 100Pa or less. The invention can also be provided with a vacuum meter to conveniently control the vacuum degree.
In this embodiment, the method may further include the steps of: and cooling and drying the obtained graphene oxide. Wherein the step of cooling may comprise water cooling, air cooling, or the like.
In summary, the method for preparing reduced graphene oxide with a low number of layers has the following advantages:
(1) according to the invention, the purified graphene oxide lamella can be further expanded in the drying process, and meanwhile, the lower entropy value of the graphene oxide material is kept at a low temperature, which is beneficial to keeping the microstructure of the expanded graphene oxide lamella, so that the graphene oxide product with higher quality can be obtained. For example, the graphene prepared by the method has a complete microstructure, and the number of layers of the graphene oxide can be reduced to 1/3-1/6 in the prior art, for example, the number of layers can be reduced from 20-30 to 5-7; the specific surface area of the graphene oxide is increased to 1.5 to 2.5 times of the original specific surface area, for example, the specific surface area is from 100 to 200m2The/g is increased to 200-400 m2/g。
(2) The heating speed of the optical microwave reduction is high, and the heating is uniform. If an external heating mode is used for heating, in order to increase the heating speed, the external temperature needs to be increased, and the temperature difference gradient is increased. However, this is accompanied by the generation of exogenous or endogenous phenomena. And no matter how the shape is, the microwave can uniformly permeate to generate heat, so that the uniformity is greatly improved.
(3) Different materials have different absorptivity to microwave, and substances containing moisture can easily absorb microwave energy. Glass, ceramic, polypropylene, polyethylene, fluoroplastic, etc. rarely absorb microwaves, metals reflect waves, and none of these materials can be heated by microwaves. In microwave heating, the heated material is generally placed in a heating chamber, the heating chamber is a closed cavity for electromagnetic waves, the electromagnetic waves cannot be leaked out and only can be absorbed by a heated object, and air in the heating chamber and a corresponding container cannot be heated, so that the heat efficiency is high. Meanwhile, the environmental temperature of a working place cannot be increased, the production environment is obviously improved, and the energy conservation and the high efficiency are realized.
(4) The equipment in the optical microwave reduction process can adopt a corrosion-resistant optical microwave pipeline, does not react with corrosive gas thermally decomposed from graphene oxide, is uniformly heated in the reaction pipeline, does not form hot atmosphere gas mass, and does not have thermal inertia.
(5) When the optical microwave reduction is carried out, a large amount of dust is not generated, and the operation environment is good.
(6) According to the invention, the removal rate of the surface functional groups of the graphene oxide can be determined according to the power of optical microwave and the processing time, so that selective thermal reduction is realized, and reduced graphene oxide materials containing different oxygen contents are prepared
(7) The microwave energy is transmitted in a closed heating chamber and a wave channel pipe, so that the microwave leakage can be strictly controlled within the national safety standard index and is greatly lower than the safety standard established by the country. And the microwave does not belong to radioactive rays and has no harmful gas emission, thereby being a very safe heating technology.
Although the present invention has been described above in connection with exemplary embodiments, it will be apparent to those skilled in the art that various modifications and changes may be made to the exemplary embodiments of the present invention without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. A method for preparing reduced graphene oxide with a low layer number is characterized by comprising the following steps:
dispersing graphene oxide having a first layer number in water, and forming a graphene oxide hydrogel;
placing the graphene oxide hydrogel at a first temperature and a first pressure to condense water molecules in the graphene oxide hydrogel into ice molecules and desublimate the ice molecules, so that graphene oxide with a second layer number is obtained, wherein the first layer number is tens of layers to tens of layers, the second layer number is smaller than the first layer number, the second layer number is 1/3-1/6 of the first layer number, the first temperature is not higher than-55 ℃, the temperature change is not more than +/-4 ℃, and the first pressure is lower than 1 atmosphere and the pressure change is not more than +/-100 Pa;
placing the graphene oxide with the second layer number in an inert atmosphere;
rapidly heating the graphene oxide with the second layer number to more than 500 ℃ by microwave and light wave irradiation to decompose functional groups carried by the graphene oxide and reduce the layer number of the graphene oxide, so as to obtain reduced graphene oxide, wherein the microwave can penetrate through the graphene oxide in a traveling wave manner;
wherein the step of placing the graphene oxide having the second number of layers in an inert atmosphere comprises: feeding the graphene oxide with the second layer number into a tubular container filled with nitrogen or inert gas through gas, wherein the two ends of the tubular container are provided with openings, the gas can flow in from one opening of the tubular container, and the gas comprises the nitrogen or the inert gas;
the vacuum degree in the tubular container is below 100 Pa;
the method may further comprise the steps of: after obtaining the reduced graphene oxide, taking the reduced graphene oxide out of the other opening of the tubular container in a suction filtration mode; after suction filtration, separating the reduced graphene oxide from the gas, and recycling the separated gas;
the method further comprises the steps of: and cooling and drying the obtained reduced graphene oxide.
2. The method for preparing reduced graphene oxide with a low number of layers according to claim 1, wherein the first number of layers is 20 to 30 layers, and the second number of layers is 5 to 7 layers.
3. The method for preparing reduced graphene oxide with a low number of layers according to claim 1, wherein the first temperature is selected within a range of-55 ℃ to-65 ℃ and the temperature variation is not more than ± 2 ℃.
4. The method for preparing reduced graphene oxide with a low number of layers according to claim 1, wherein the first pressure is selected within a range of 10-100 Pa and a variation of the pressure is not more than +/-10 Pa.
5. The method for preparing reduced graphene oxide with a low number of layers according to claim 1, wherein the graphene oxide hydrogel has a solid content of 0.1-50 wt%.
6. The method for preparing reduced graphene oxide with a low number of layers according to claim 1, wherein the flow velocity of the gas in the tubular container is 10cm3Less than or equal to s, the amount of graphene oxide that can be fed per unit volume of the gas is 1g/cm3The following.
7. The method for preparing reduced graphene oxide with low number of layers according to claim 1, wherein the directions of the microwave and light wave irradiation and the gas flowing direction in the tubular container are perpendicular to each other.
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