CN109292761B - Method for reducing graphene oxide by optical microwave - Google Patents

Method for reducing graphene oxide by optical microwave Download PDF

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Publication number
CN109292761B
CN109292761B CN201811492603.2A CN201811492603A CN109292761B CN 109292761 B CN109292761 B CN 109292761B CN 201811492603 A CN201811492603 A CN 201811492603A CN 109292761 B CN109292761 B CN 109292761B
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graphene oxide
microwave
gas
tubular container
light wave
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CN109292761A (en
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李星
刘长虹
蔡雨婷
漆长席
蒋虎南
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Daying Juneng Technology And Development Co ltd
Sichuan Juchuang Shimoxi Technology Co ltd
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Daying Juneng Technology And Development Co ltd
Sichuan Juchuang Shimoxi Technology Co ltd
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    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00Structure or properties of graphene
    • C01B2204/04Specific amount of layers or specific thickness

Abstract

The invention provides a method for reducing graphene oxide by using light microwaveThe method of (1). The method may comprise the steps of: placing graphene oxide in an inert atmosphere; rapidly heating the graphene oxide to more than 500 ℃ through microwave and light wave irradiation so as to decompose functional groups carried by the graphene oxide and reduce the number of layers of the graphene oxide, thereby obtaining reduced graphene oxide; wherein the microwave can penetrate through the graphene oxide in a traveling wave manner, the frequency of the microwave is 300 MHz-300 GHz, and the frequency of the optical wave is 3 multiplied by 1011~3.8×1014Hz. The beneficial effects of the invention include: the optical microwave has the advantages of high heating speed, uniform heating, no thermal inertia, energy conservation, high efficiency and high reduction efficiency of the graphene oxide, and can realize selective oxidation of the graphene oxide.

Description

Method for reducing graphene oxide by optical microwave
Technical Field
The invention relates to the field of reduction of graphene oxide, in particular to a method for reducing graphene oxide by using optical microwaves.
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. 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 optical microwave reduction of graphene oxide, which can efficiently decompose functional groups on graphene oxide.
In order to achieve the above object, the present invention provides a method for reducing graphene oxide by using optical microwave. The method may comprise the steps of: placing graphene oxide in an inert atmosphere; rapidly heating the graphene oxide to more than 500 ℃ through microwave and light wave irradiation so as to decompose functional groups carried by the graphene oxide and reduce the number of layers of the graphene oxide, thereby obtaining reduced graphene oxide; wherein the microwave can pass through the graphene oxide in a traveling wave manner.
According to an exemplary embodiment of the present invention, the step of placing the graphene oxide in an inert atmosphere may include: feeding graphene oxide 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, said gas is present in said chamberThe flow rate in the tubular container can be 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 power of the light wave may be 200-500W; the microwave can be 500-5500W, such as 2000W; the irradiation time of the light waves and microwaves can 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 optical microwave has the advantages of high heating speed, uniform heating, no thermal inertia, energy conservation, high efficiency and high reduction efficiency of the graphene oxide, and can realize selective oxidation of the graphene oxide.
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 chart of the method for reducing graphene oxide by using optical microwave according to the present invention.
FIG. 2 is a schematic diagram showing the positional relationship of the microwave and lightwave radiation system of the present invention with respect to a tubular container.
The main illustration is as follows:
1-a quartz tube; 2-a light wave tube; 3-microwave cavity.
Detailed Description
Hereinafter, the method for optical microwave reduction of graphene oxide according to the present invention will be described in detail with reference to exemplary embodiments.
The traditional heating mode is that heat is firstly transferred to the surface of an object through heat conduction, convection, heat radiation and the like, and then the temperature of the center of the object is gradually increased through the heat conduction. The heating mode of the microwave belongs to internal heating, electromagnetic energy can directly act on medium molecules to be converted into heat, the medium is heated inside and outside simultaneously through transmission, and heat conduction is not needed, so that uniform heating can be achieved in a short time. The microwave can be uniformly permeated, and the light wave can assist the microwave to heat an object quickly, so that the heating is more uniform.
Therefore, the invention provides a method for reducing graphene oxide by heating light waves and microwaves cooperatively.
Fig. 1 shows a schematic flow chart of the method for reducing graphene oxide by using optical microwave according to the present invention.
FIG. 2 is a schematic diagram showing the positional relationship of the microwave and lightwave radiation system of the present invention with respect to a tubular container.
In an exemplary embodiment of the present invention, the method for optical microwave reduction of graphene oxide may include the steps of:
the graphene oxide is placed in an inert atmosphere, as in step S01 in fig. 1. For example, graphene oxide may be fed into a vessel 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 (3) rapidly heating the graphene oxide to more than 500 ℃ through microwave and light wave irradiation to decompose functional groups carried by the graphene oxide and reduce the number of layers of the graphene oxide, so as to obtain the reduced graphene oxide, as shown in step S02 in fig. 1. The microwave can penetrate through the graphene oxide in a traveling wave mode, and the continuously 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 avoidedThe consistency of graphene oxide treatment 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 microwaves and light waves, the graphene oxide can be rapidly heated to more than 500 ℃, the carried functional groups can be rapidly decomposed, and because the carried functional groups are oxygen-containing functional groups, a large amount of gas such as water vapor, carbon dioxide and the like can be instantly generated during decomposition, and the 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 "reduced graphene oxide" as a product may be 10 or less, for example, 5 to 8 layers.
The removal rate of the functional groups on the graphene oxide can reach more than 85%, for example 95%. The percent reduction in graphene oxide count may be 80% or more, for example, from 40 layers to 6 layers.
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 10cm3Flow rate control of gas below/sIn this range, the graphene oxide can be smoothly introduced into the tubular container so as to 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 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 light wave can be 200-500W; the microwave can be 500-5500W, such as 2000W. 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, both openings of the tubular container may be provided with valves, and the valves may be closed after the gas feeds the graphene oxide. The vacuum level in the tubular container can then be adjusted to avoid the effects of air.
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 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.
The microwave system can emit microwaves, and the microwave system can comprise a microwave source, a microwave resonant cavity and a microwave leakage-proof 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 order that the above-described exemplary embodiments of the invention may be better understood, further description thereof with reference to specific examples is provided below.
Example 1 (blank comparative example)
Graphene oxide is used as a raw material, the number of layers of the graphene oxide is 30, and the weight percentage of functional groups in the graphene oxide is 0.82%.
And carrying out microwave reduction on the graphene oxide to obtain reduced graphene oxide. Wherein the frequency of the microwave is 5GHz, and the time of the microwave treatment is 8 min.
Through detection, the number of layers of the reduced graphene oxide is 10, the weight ratio of the functional groups is 0.27%, and the removal rate of the functional groups is 67%.
Example 2
Graphene oxide is used as a raw material, the number of layers of the graphene oxide is 30, and the weight percentage of functional groups in the graphene oxide is 0.82%.
And reducing the graphene oxide by adopting the optical microwave reduction method disclosed by the invention to obtain the reduced graphene oxide. Wherein the frequency of the microwave is 5GHz and the frequency of the optical wave is 5 × 1013Hz, and the time for light wave and microwave treatment is 5 min.
Through detection, the number of layers of the reduced graphene oxide is 7, the weight ratio of the functional groups is 0.04%, and the removal rate of the functional groups is 95.1%.
In summary, the optical microwave reduction of graphene oxide according to the present invention has the following advantages:
(1) the heating speed is high
Conventional heating (such as flame, hot air, electric heat, steam, etc.) is to transfer heat to the surface of an object to be heated first by heat conduction, convection, and heat radiation, and then to raise the central temperature step by heat conduction (also commonly referred to as external heating). It takes a certain heat transfer time to bring the central part to the desired temperature, while it takes longer for objects with poor heat transfer. Microwave heating belongs to an internal heating mode, electromagnetic energy directly acts on medium molecules to be converted into heat, the medium is heated inside and outside simultaneously through transmission, heat conduction is not needed, and therefore uniform heating can be achieved in a short time.
(2) Uniform heating
When the heating is carried out by an external heating mode, 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. When the microwave is heated, the microwave can uniformly permeate regardless of the shape, and heat is generated, so that the uniformity is greatly improved.
(3) Energy-saving high-efficiency
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 the air in the heating chamber and a corresponding container cannot be heated, so that the heat efficiency is high. Meanwhile, the environmental temperature of the workplace is not increased, and the production environment is obviously improved.
(4) Corrosion resistance and no thermal inertia.
The invention can adopt a corrosion-resistant optical microwave pipeline, does not react with corrosive gas thermally decomposed from graphene oxide, and meanwhile, the reaction pipeline is uniformly heated, does not form hot atmosphere gas groups and does not have thermal inertia.
(5) Clean and sanitary
When the graphene oxide is processed and dried, a large amount of dust is not generated, and the operation environment is good.
(6) Selective heating
The equipment can remove the surface functional group of the graphene oxide according to the light microwave power and the processing time, thereby realizing selective thermal reduction and preparing the reduced graphene oxide material containing different oxygen contents
(7) Safe and harmless
Generally, microwave energy is transmitted in a closed heating chamber and a wave channel pipe, so that microwave leakage can be strictly controlled within national safety standard indexes 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 (4)

1. A method for reducing graphene oxide by optical microwave is characterized by comprising the following steps:
placing graphene oxide in an inert atmosphere;
the graphene oxide is rapidly heated to more than 500 ℃ through microwave and light wave irradiation so as to decompose functional groups carried by the graphene oxide and reduce the number of layers of the graphene oxide, and reduced graphene oxide is obtained, wherein microwaves can penetrate through the graphene oxide in a traveling wave manner;
wherein the step of placing the graphene oxide in an inert atmosphere comprises: feeding graphene oxide into a tubular container filled with nitrogen or inert gas by gas, wherein the tubular container has openings at two ends, the gas can flow in from one opening of the tubular container, and the gas comprises the nitrogen or the inert gas;
the flow rate 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;
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: cooling and drying the obtained reduced graphene oxide;
the power of the microwave is 500-5500W, the power of the light wave is 200-500W, and the irradiation time of the light wave and the microwave is less than 10 min.
2. The method for optical microwave reduction of graphene oxide according to claim 1, wherein the directions of the microwave and light wave irradiation and the gas flow direction in the tubular container are perpendicular to each other.
3. The method of claim 1, wherein the tubular container comprises a quartz tube, and the microwave and light waves are capable of irradiating the graphene oxide through the wall of the quartz tube.
4. The optical microwave graphene oxide reduction method according to claim 1, wherein the light waves include infrared rays or far infrared rays.
CN201811492603.2A 2018-12-07 2018-12-07 Method for reducing graphene oxide by optical microwave Active CN109292761B (en)

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CN110215946A (en) * 2019-05-29 2019-09-10 西南大学 A kind of novel metal test tube device for microwave heating
CN111943178A (en) * 2020-08-21 2020-11-17 伊诺福科光学技术有限公司 Method for preparing graphene material through self-sufficient reduction, graphene material, graphene film, electrode and capacitor
CN112048147A (en) * 2020-09-18 2020-12-08 高碑店市安普光电材料科技有限公司 Antibacterial and deodorant plastic master batch taking elastomer as carrier and preparation method thereof
CN113086974B (en) * 2021-04-02 2021-11-19 合肥碳艺科技有限公司 Nitrogen-doped graphene and preparation method and application thereof

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CN102107870A (en) * 2011-03-23 2011-06-29 中国科学院山西煤炭化学研究所 Method for quickly preparing reduced graphene by using microwaves
CN102730678A (en) * 2012-07-23 2012-10-17 贵州新碳高科有限责任公司 Device and method for preparing graphene powder
CN106517174A (en) * 2016-11-25 2017-03-22 西安交通大学 Quick heating method for graphene and deep processing method based on same

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN102107870A (en) * 2011-03-23 2011-06-29 中国科学院山西煤炭化学研究所 Method for quickly preparing reduced graphene by using microwaves
CN102730678A (en) * 2012-07-23 2012-10-17 贵州新碳高科有限责任公司 Device and method for preparing graphene powder
CN106517174A (en) * 2016-11-25 2017-03-22 西安交通大学 Quick heating method for graphene and deep processing method based on same

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