CN109292761A - A kind of method of smooth microwave reduction graphene oxide - Google Patents
A kind of method of smooth microwave reduction graphene oxide Download PDFInfo
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- CN109292761A CN109292761A CN201811492603.2A CN201811492603A CN109292761A CN 109292761 A CN109292761 A CN 109292761A CN 201811492603 A CN201811492603 A CN 201811492603A CN 109292761 A CN109292761 A CN 109292761A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
Abstract
The present invention provides a kind of methods of smooth microwave reduction graphene oxide.The method, which can comprise the following steps that, is placed in graphene oxide in inert atmosphere；Graphene oxide is brought rapidly up to 500 DEG C or more by microwave and light wave irradiation, to decompose its band functional group of institute and reduce its number of plies, obtains redox graphene；Wherein, microwave can penetrate graphene oxide in a manner of traveling wave, and the frequency of the microwave is 300MHz~300GHz, and the frequency of the light wave is 3 × 1011~3.8 × 1014Hz.The beneficial effect comprise that light microwave to the heating speed of graphene oxide fast, homogeneous heating and without thermal inertia, energy-efficient, reduction efficiency is high, can be realized the selective oxidation to graphene oxide.
Description
Technical field
The present invention relates to the reduction fields of graphene oxide, particularly, are related to a kind of smooth microwave reduction graphene oxide
Method.
Background technique
Graphene oxide is product of the graphite after chemical oxidation, and surface has the functions such as great amount of hydroxy group, carboxyl, epoxy group
Group, specific surface area with higher, in analysis detection field, modified polymer material, biomedicine field, photoelectricity correlation neck
It is all widely used in domain, photocatalysis.Because of the characteristic of graphene oxide, chemical reagent is mostly used to restore greatly on the market at present
(such as sodium borohydride, hydrogen iodide, ascorbic acid chemical reducing agent), high temperature thermal reduction, plasma method etc..
Existing graphene oxide restoring method is had the problem that in process of production first is that also using chemical reagent
Original needs to use a large amount of chemical reagent, and bring by-product increases, and subsequent cleaning difficulty increases, and environmentally friendly risk increases, and causes
Increased costs；Second is that being heat-treated using high temperature, graphene oxide reduction temperature is higher, the product matter that different reduction temperatures obtains
Not the problems such as amount uniformity not can guarantee, while also bring along the increase of product ash content, equipment seriously corroded；Third is that using other reduction
Method (such as plasma), technology difficulties, cost can be multiplied, and be unable to get industrialization large-scale application.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to solve above-mentioned one existing in the prior art
Or multiple problems.For example, one of the objects of the present invention is to provide a kind of method of smooth microwave reduction graphene oxide, the side
Method being capable of functional group on efficient-decomposition graphene oxide.
To achieve the goals above, the present invention provides a kind of methods of smooth microwave reduction graphene oxide.The method
It can comprise the following steps that and graphene oxide is placed in inert atmosphere；Keep graphene oxide rapid by microwave and light wave irradiation
500 DEG C or more are warming up to, to decompose its band functional group of institute and reduce its number of plies, obtains redox graphene；Wherein, microwave energy
It is enough that graphene oxide is penetrated in a manner of traveling wave.
An exemplary embodiment according to the present invention, the step that graphene oxide is placed in inert atmosphere can wrap
It includes: graphene oxide being sent into the internal tubular container full of nitrogen or inert gas by gas；Wherein, the tubulose holds
The both ends of device have opening, and the gas can be flowed into from an opening of tubular container, and the gas includes nitrogen or inertia
Gas.
An exemplary embodiment according to the present invention, the method, which may further comprise the step of:, is obtaining reduction-oxidation graphite
After alkene, redox graphene is taken out from another opening of tubular container by way of suction filtration.
An exemplary embodiment according to the present invention, flow velocity of the gas in the tubular container can be in 10cm3/
S is hereinafter, such as 1~8cm3/s；The amount that the gas can be sent into graphene oxide can be in 1g/cm3Hereinafter, such as 0.5 ±
0.3g/cm3。
An exemplary embodiment according to the present invention, the power of the light wave can be 200~500W；The microwave can
For 500~5500W, such as 2000W；The irradiation time of the light wave and microwave can be in 10min hereinafter, such as 5 ± 3min.
An exemplary embodiment according to the present invention, the direction and the gas of the microwave and light wave irradiation are in tubulose
Flow direction can be mutually perpendicular in container.
An exemplary embodiment according to the present invention, the vacuum degree in the tubular container can be in 100Pa or less.
An exemplary embodiment according to the present invention, the tubular container may include quartz ampoule, the microwave and light wave
The graphene oxide can be irradiated through quartzy tube wall.
An exemplary embodiment according to the present invention, the light wave may include infrared ray or far infrared.
An exemplary embodiment according to the present invention, the method may further comprise the step of: to the obtained oxygen reduction
Graphite alkene carries out cooling, dry.
Compared with prior art, the beneficial effect comprise that light microwave is fast to the heating speed of graphene oxide, adds
Hot uniformly no thermal inertia is energy-efficient, and reduction efficiency is high, can be realized the selective oxidation to graphene oxide.
Detailed description of the invention
By the description carried out with reference to the accompanying drawing, above and other purpose of the invention and feature will become more clear
Chu, in which:
Fig. 1 shows a flow diagram of light microwave reduction graphene oxide method of the invention.
Fig. 2 shows microwaves of the invention, a schematic diagram of optical wavelength radiation system and tubular container positional relationship.
Main marginal data:
1- quartz ampoule；2- optical wave tube；3- microwave cavity.
Specific embodiment
Hereinafter, the side of light microwave reduction graphene oxide of the invention will be described in detail in conjunction with exemplary embodiment
Method.
Traditional heating method is first to transfer heat to body surface by heat transfer, convection current, heat radiation etc., then pass through
Heat transfer gradually increases core body temperature.And the heating method of microwave belongs to internal heating, electromagnetic energy can be done directly on
Medium molecule is converted into heat, and transmission keeps medium inside and outside while heated, does not need heat transfer, therefore can reach in a short time uniform
Heating.Microwave can uniformly penetrating, light wave also can assisted microwave synthesis quickly heat object, make to heat more uniform.
Therefore, the invention proposes a kind of methods of redox graphene for heating light wave and microwave cooperating.
Fig. 1 shows a flow diagram of light microwave reduction graphene oxide method of the invention.
Fig. 2 shows microwaves of the invention, a schematic diagram of optical wavelength radiation system and tubular container positional relationship.
In an exemplary embodiment of the present invention, the method for the smooth microwave reduction graphene oxide may include following
Step:
Graphene oxide is placed in inert atmosphere, step S01 as shown in figure 1.It is filled for example, graphene oxide can be sent into
In the container of full nitrogen or inert gas.Wherein, the container may include the tubular container that both ends have opening.Further,
It may include the tubular container that horizontal cross setting and left and right ends have opening.
It is irradiated by microwave and light wave, is brought rapidly up graphene oxide to 500 DEG C or more, to decompose its band functional group of institute
And its number of plies is reduced, redox graphene is obtained, step S02 as shown in figure 1.Wherein, microwave can be saturating in a manner of traveling wave
Peroxidating graphene, the present invention form the traveling-wave waveform constantly transmitted, this can be avoided that standing wave by microwave one-way transmission
Localized hyperthermia's phenomenon caused by effect can be improved graphene oxide uniformity for the treatment of.The frequency of microwave can for 300MHz~
300GHz can be further 800MHz~250GHz.The frequency of the light wave can be 3 × 1011~3.8 × 1014Hz, into one
Step ground can be 2 × 1012~2.5 × 1014Hz.By acting on while microwave and light wave, graphene oxide can be brought rapidly up
To 500 degree or more, band functional group of institute can be decomposed rapidly, since its band functional group is oxygen-containing functional group, can decomposed instantaneously
A large amount of gas is generated, such as vapor, carbon dioxide generate, gas expands between graphene oxide layer, can make to prepare
The number of plies of obtained material is less, and specific surface area is bigger.Further, microwave and light wave can make the temperature liter of graphene oxide
To 500~1000 DEG C, such as 800 ± 150 DEG C.The main heating source of heating process can be microwave, and light wave can play auxiliary
Effect, the two join together that the graphene oxide temperature being heated can be made to increase rapidly, are conducive to its deoxidation treatment.
In the present embodiment, as the number of plies of the graphene oxide of raw material can be more than tens of layers, such as 30~50.As
The number of plies of " redox graphene " of product can be for 10 layers hereinafter, such as 5~8 layers.
The removal efficiency of functional group is up to 85%% or more, such as 95% on graphene oxide.The graphene oxide number of plies reduces
Percentage can be 80% or more, such as can be reduced to 6 layers by 40 layers.
In the present embodiment, graphene oxide can be sent into tubular container by air-flow.It can also will be obtained by air-flow
Redox graphene sends out tubular container.In other words, can be passed through load in an opening of tubular container has graphite oxide
The air-flow of alkene；The air-flow can carry the cavity that (or promotion) material flows through tubular container；In flow process, graphite oxide
Alkene can be reduced to redox graphene；Final air-flow load (or promotion) redox graphene from the another of tubular container
One opening outflow.Gas in the air-flow may include nitrogen or inert gas.
Wherein, flow velocity of the gas in pipe container can be 10cm3/ s is hereinafter, the flow control of gas in the range can
It enough can smoothly enter into graphene oxide in tubular container, so that it is sufficiently restored by microwave.Further, gas flow rate can be
0.01~8cm3/ s, still further, can be 2~5cm3/s。
The amount of the graphene oxide loaded on the air-flow can be 10g/cm3Hereinafter, such as 0.1~10g/cm3, further
Ground can be 2~10g/cm3。
For above-mentioned graphene oxide, the power of the light wave can be 200~500W；The microwave is 500~
5500W, such as 2000W.Light wave is identical with the processing time of microwave, can be controlled in 10mim hereinafter, may be, for example, 30s, 2min or
7min etc..
In the present embodiment, two openings of tubular container may be provided with valve, and graphene oxide is sent into it in gas
Afterwards, valve can be closed.Then it can adjust the vacuum degree in tubular container, avoid the influence of air.
In the present embodiment, the method may further comprise the step of: after obtaining redox graphene, pass through suction filtration
Mode takes out redox graphene from another opening of tubular container.After suction filtration, the method also includes steps
It is rapid: and redox graphene can be separated with gas, the gas isolated is recyclable to be recycled.
In the present embodiment, the present invention can be realized by the time of the power of light microwave, processing to graphene oxide
Selective oxidation, the redox graphene of different oxygen content can be obtained according to demand.
In the present embodiment, the direction of the microwave and light wave irradiation can be mutually perpendicular to the direction of the air-flow.In this way
Light wave and microwave can be enable preferably to penetrate graphene oxide, sufficiently irradiate, avoid because volume of material becomes larger cause it is micro-
Wave reflection, and then influence the irradiation of deep layer particle.
In the present embodiment, the tubular container may include being horizontally installed on quartz ampoule.Quartz ampoule be it is transparent, will not be every
The uninterrupted characteristic for penetrating effect, having to light wave, microwave of exhausted light and microwave, i.e., the described microwave and light wave can penetrate stone
English tube wall irradiates the graphene oxide.Quartz ampoule high temperature resistant, thermal expansion coefficient are extremely low, chemical stability is fabulous, electrical isolation
Property is excellent, microwave is permeable high.Quartz ampoule of the invention can high temperature resistant, rapid heat cycle can be born；It can bear positive and negative
Pressure is greater than the impact of 1Mpa.
The present invention can emit microwave by microwave system, and microwave system may include microwave source, microwave cavity and microwave
Anti-leakage mechanism composition.Wherein, microwave source is the electronic device for generating microwave energy, can be by magnetron, high-tension transformer, high repoussage
Flow back to the devices compositions such as road, cooling fan, overcurrent protection, abnormal temperature protection and waveguide.Microwave cavity is microwave energy
Bulk storage containers and the main region of microwave bulking reaction.Anti-leakage mechanism can prevent the leakage of microwave.
The present invention can emit light wave by several optical wave tubes.The effect of light wave mainly plays heat temperature raising.It is described
Light wave may include infrared ray or far infrared.
As shown in Fig. 2, the microwave cavity 3 of microwave system can surround quartz ampoule 2, such microwave can be through quartz ampoule
Tube wall sufficiently and uniformly irradiation oxidation graphene in a manner of traveling wave；Two optical wave tubes 2 can be distributed in the two sides of quartz ampoule, this
Sample light wave also can pass through quartzy tube wall sufficiently and uniformly irradiation oxidation graphene.Under the synergistic effect of light wave and microwave, oxygen
Graphite alkene can quickly heat up.
In the present embodiment, the reduction of graphene oxide can carry out under vacuum conditions, can be avoided the shadow of air in this way
It rings, because air is easy thermal conductivity to walk.Vacuum degree in container can be in 100Pa or less.The also settable vacuum meter of the present invention,
To facilitate control vacuum degree.
In the present embodiment, the method may further comprise the step of: the obtained graphene oxide is carried out it is cooling, dry
It is dry.Wherein, cooling step may include water cooling, air-flow cooling etc..
The above exemplary embodiments for a better understanding of the present invention carry out further it below with reference to specific example
Explanation.
Example 1 (blank example)
Using graphene oxide as raw material, the number of plies of graphene oxide is 30, functional group's weight accounting in graphene oxide
It is 0.82%.
Microwave reduction is carried out to graphene oxide, obtains redox graphene.Wherein, the frequency of microwave is 5GHz, micro-
The time of wave processing is 8min.
Through detecting, the number of plies of redox graphene is 10, and functional group's weight accounting is 0.27%, functional group's removal rate
It is 67%.
Example 2
Using graphene oxide as raw material, the number of plies of graphene oxide is 30, functional group's weight accounting in graphene oxide
It is 0.82%.
Graphene oxide is restored using light microwave reduction method of the invention, and obtains redox graphene.
Wherein, the frequency of microwave is 5GHz, and the frequency of light wave is 5 × 1013The time of Hz, light wave and microwave treatment is 5min,.
Through detecting, the number of plies of redox graphene is 7, and the weight accounting of functional group is 0.04%, functional group's removal rate
It is 95.1%.
In conclusion light microwave reduction graphene oxide of the invention has the advantage that
(1) heating speed is fast
Conventional heating (such as flame, hot wind, electric heating, steam) all be using heat transfer, convection current, heat radiation by heat first
The surface of heating object is passed to, then so that central temperature is increased (the external heating both often claimed) by heat transfer.It will make
Centre reaches required temperature, needs certain heat conduction time, and just to the time needed for the object of pyroconductivity difference
It is longer.Microwave heating then belongs to internal heating method, and electromagnetic energy directly acts on medium molecule and is converted into heat, and transmission makes in medium
It is outer while heated, heat transfer is not needed, therefore can reach in a short time and be evenly heated.
(2) it is evenly heated
When being heated with external heating method, to improve heating speed, elevated external temperatures are just needed, increase temperature gradient.So
And it is easy for generating scorched outside and underdone inside phenomenon therewith.No matter shape when microwave heating, microwave can uniformly penetrating, generate heat
Amount, therefore uniformity substantially improves.
(3) energy-efficient
Different material has different absorptivities to microwave, and the substance containing moisture content is easy to absorb microwave energy.Glass, gathers ceramics
Propylene, polyethylene, fluoroplastics etc. then seldom absorb microwave, and metal all cannot be by microwave heating by reflection wave, these substances.It is micro-
When Wave heating, being heated material is typically all to be placed on interior is heated, and heating room is a closed cavity, electricity for electromagnetic wave
Magnetic wave cannot leak, can only heating object absorb, heating indoor air and cell therefor will not all be heated, so hot
It is high-efficient.Therefore the environment temperature for working at the same time place will not increase, production environment is obviously improved.
(4) corrosion-resistant, no thermal inertia.
The light microwave pipe-line of corrosion resistance can be used in the present invention, and the corrosive gas not thermally decomposed out with graphene oxide is anti-
It answers, is heated evenly in simultaneous reactions pipeline, do not form hot atmosphere air mass, no thermal inertia.
(5) sanitation and hygiene
When to graphene oxide dry processing, a large amount of dust will not be generated, operating environment is good.
(6) selectivity heating
Equipment can be according to light microwave power size, processing time come surface of graphene oxide functional group removal rate, thus real
Existing selective thermal reduction, preparation contain the redox graphene material of different oxygen content
(7) safe and harmless
Usual microwave energy is transmitted in closing heating room, radio frequency channel pipe, and microwave leakage can be made to be strict controlled in national peace
In full standard index, it is significantly less than the safety standard of country's formulation.And microwave is not belonging to radioactive ray, again without pernicious gas
Discharge, is a kind of foolproof heating technique.
Although those skilled in the art should be clear above by combining exemplary embodiment to describe the present invention
Chu can carry out exemplary embodiment of the present invention each without departing from the spirit and scope defined by the claims
Kind modifications and changes.
Claims (10)
1. a kind of method of smooth microwave reduction graphene oxide, which is characterized in that the described method comprises the following steps:
Graphene oxide is placed in inert atmosphere；
It is brought rapidly up graphene oxide to 500 DEG C or more by microwave and light wave irradiation, to decompose its band functional group of institute and subtract
Its few number of plies, obtains redox graphene, wherein microwave can penetrate graphene oxide in a manner of traveling wave.
2. the method for smooth microwave reduction graphene oxide according to claim 1, which is characterized in that described by graphite oxide
The step that alkene is placed in inert atmosphere includes: that graphene oxide is sent into the internal pipe full of nitrogen or inert gas by gas
In shape container, wherein the both ends of the tubular container have opening, and the gas can be flowed from an opening of tubular container
Enter, the gas includes nitrogen or inert gas.
3. the method for smooth microwave reduction graphene oxide according to claim 2, which is characterized in that the gas is described
Flow velocity in tubular container is in 10cm3/ s is hereinafter, the amount that the gas of unit volume can be sent into graphene oxide is 1g/cm3
Below.
4. the method for smooth microwave reduction graphene oxide according to claim 1, which is characterized in that the frequency of the microwave
For 300MHz~300GHz, the frequency of the light wave is 3 × 1011~3.8 × 1014Hz。
5. the method for smooth microwave reduction graphene oxide according to claim 4, which is characterized in that the power of the microwave
For 500~5500W, the power of the light wave is 200~500W, and the irradiation time of the light wave and microwave is 10min or less.
6. the method for smooth microwave reduction graphene oxide according to claim 2, which is characterized in that the microwave and light wave
The flow direction in tubular container is mutually perpendicular to the gas in the direction of irradiation.
7. the method for smooth microwave reduction graphene oxide according to claim 2, which is characterized in that in the tubular container
Vacuum degree in 100Pa or less.
8. the method for smooth microwave reduction graphene oxide according to claim 2, which is characterized in that the tubular container packet
Quartz ampoule is included, the microwave and light wave can irradiate the graphene oxide through quartzy tube wall.
9. the method for smooth microwave reduction graphene oxide according to claim 2, which is characterized in that the light wave includes red
Outside line or far infrared.
10. the method for smooth microwave reduction graphene oxide according to claim 1, which is characterized in that the method is also wrapped
It includes step: the obtained redox graphene being carried out cooling, dry.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN113086974A (en) * | 2021-04-02 | 2021-07-09 | 合肥碳艺科技有限公司 | Nitrogen-doped graphene and preparation method and application thereof |
| CN116813348A (en) * | 2023-07-11 | 2023-09-29 | 聊城冠县尚敖超硬材料有限公司 | Reduction treatment method and process for high-yield graphite column |
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| 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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| 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 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| 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 |
| CN116813348A (en) * | 2023-07-11 | 2023-09-29 | 聊城冠县尚敖超硬材料有限公司 | Reduction treatment method and process for high-yield graphite column |
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