CN110272040A - A kind of preparation method of high-purity graphene oxide - Google Patents
A kind of preparation method of high-purity graphene oxide Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of high-purity graphene oxide, belong to nano material and preparation method field.Purpose is to solve the problems, such as the preparation of high-purity graphene oxide, provides a kind of simple process, the graphene oxide preparation method of high, economic and environment-friendly, the easy scale of degree of oxidation.This method is that the electrode runs parallel of graphite material is inserted into deionized water；Promote the oxidation and removing of graphite linings by the effect of electrochemical oxidation under conditions of hydro jet and DC voltage, the graphene aqueous solution of acquisition is after dry up to high-purity graphene oxide.The method of the present invention has many advantages, such as simple process, the graphene oxide purity is high of easy prepare with scale and preparation, degree of oxidation height, good water solubility, easily dispersion, be especially suitable for the electrode material or conductive additive of energy storage device, catalyst carrier and for fields such as bio-imaging, probe/sensing, therapeutic treatments.
Description
Technical field
The present invention relates to a kind of preparation methods of high-purity graphene oxide, belong to nano material and preparation field.
Background technique
Graphene is by the performances such as its unique optics, machinery, electricity, quantum, such as high conductance, highly thermally conductive, high rigidity
With high intensity etc., extensive concern is caused in fields such as electronics, information, the energy, material and biological medicines, with micro- sodium or original
The fast development of sub- rank manufacture processing technology, electronic device chip research relevant to graphene are also deepening continuously and are having phase
It closes product to release, such as graphene chip.Meanwhile graphene itself is used as a kind of structural material, derives because of its structure difference
A variety of different functional materials, including graphene oxide, graphene ribbon, graphene nano pipe etc..In these materials, stone is aoxidized
Contain-OH and C-O-C in black alkene plane, and contains C=O and COOH at its lamella edge, compared with graphene, these oxidations official
It can roll into a ball and impart the richer physical and chemical performance of graphene oxide, not only there is good wettability and surface-active,
And can be removed after small molecule or polyalcohol intercalation, semiconductor band gap is adjustable, in calorifics, electricity, the mechanics for improving material
Etc. play a very important role in terms of comprehensive performances, be widely used for energy storage, chemisorption, catalysis, biology
The fields such as medicine, drug controlled release.For example, graphene oxide have specific surface area abundant, can to gold, iron rhodium alloy,
The nanocatalysts such as palladium, platinum provide sufficient load space.And load percentage and modification mode etc. can regulate and control, therefore its
Catalytic performance also can be adjusted and optimize, and can be used as the catalysis electrode of chemical sensitisation electrode and fuel cell.Graphene
It can be with the electrode material (LiFePO in numerous energy storage devices4、LiNi0.5Mn1.5O4、Li4Ti5O12、Si、Sn、FeOxDeng) mixed
It closes, constitutes highly conductive advanced electrode, graphene oxide can promote the capacity of electrode active material to obtain greatly playing and delaying
The bulk effect in active material charge and discharge process is solved, therefore, this kind of electrodes tend to show excellent stable circulation
Property, high power or high specific energy performance.If graphene oxide is carried out partial reduction, itself can also be used as lithium ion/sodium ion
The Fabrication of High Specific Capacitance negative electrode material of battery also can be used for solar battery or electronic component as semiconductor.In terms of biology, Shanghai is answered
Graphene oxide is applied in round pcr with physics Institute's discovery, is remarkably improved specificity, sensitivity and the expansion of PCR
Units increased in production, and the primer dimer formed in amplification can be eliminated, and optimization section is wide, is widely portable to various concentration and complexity
The DNA profiling of degree.Compared with the carbon nanomaterial that other have been applied in round pcr, graphene oxide has the optimization of PCR
There is more excellent resultant effect.In addition, the toxicity of graphene is extremely low and bio-compatibility is high, it can be used as pharmaceutical carrier and exist
Medicament slow release is realized in organism, may also pass through surface-functionalized infrared as the targeted drug for the treatment of cancer or realization later
Heat cure.Certain metamaterial structure is carried out to it and processes it due to the machinability of graphene oxide in structure design aspect
It can be used as the absorbing material haveing excellent performance afterwards, be applied to national defense construction.In conclusion graphene oxide has very extensive use
On the way, there is very important researching value.
Currently, the method for preparing graphene oxide is more, it is generally divided into top-down approach and Bottom-up approach two
Major class.The former thinking is to split crystalline flake graphite etc. by strong oxidation to prepare graphene oxide, with traditional Brodie,
Tri- methods of Staudenmaier and Hummers are representative.The latter is passed through with the small organic molecules carbon source such as various ethylene, propane
Chemical vapor deposition forms.Currently, Brodie method, Staudenmaier method and Hummers method prepare the preparation of graphene oxide
Technique relative maturity, now still continue to use and Part Methods in each method on the basis of slightly improve.The system of these methods
Standby principle is that graphite is formed compound between graphite layers under the collective effect of strong acid and a small amount of strong oxidizer, then this interlayer
Compound continues that depth liquid phase oxidation reaction occurs under the action of excessive strong oxidizer, graphite oxide is obtained after hydrolysis, finally
Can be obtained graphene oxide by the mixture of ultrasound or long agitation graphite oxide and water, the degree of oxidation of product and
Synthesis technology is related with the reaction time, can be measured by the atomic ratio of C, O.Brodie method and Staudenmaier method oxygen
Change degree is high, but ClO can be generated in reaction process2、NO2Or N2O4It waits pernicious gases and the reaction time is long；Though Hummers method
The right reaction time is short, without toxic gas ClO2It generates, but needs the technological factor of control more in this reaction process, excessive height
Mangaic acid ion will cause potential pollution, therefore be needed in preparation process with a large amount of H2O, uneconomical environmental protection lead to acquisition
Graphene higher cost.In view of the above-mentioned problems, having many scholars in recent years in order to obtain graphene oxide and exploring preferably
Preparation method.For example, Matsuoy uses electrochemical method by graphite in strong acid, with Hg/Hg2SO4After electrode electrolysis oxidation
It puts into water, obtains graphene oxide after dry.Daniela C Marcano etc. is with KMnO4With the H of 9: 1 (volume ratios)2SO4/
H3PO4For oxidant, using being added without NaNO3Method also prepare graphene oxide, the method increase having for oxidation process
Effect property, the enhancing of products therefrom hydrophily, reaction process do not generate toxic gas, and environmental pollution is small, and reaction temperature is easy to control.
Shen Jianfeng etc. is oxidant with benzoyl peroxide, quickly prepares graphene oxide, shortens preparation time.Na
Liu et al. utilizes [C8mim]+[PF6]-Solution with water is as electrolyte, using graphite rod as electrode, by electrochemical oxidation side
Method is prepared for the graphene oxide of Ionic Liquid Modified.The above method is required to introduce it when carrying out electrochemical oxidation
His conductive ion.Although the introducing of conductive ion can accelerate the formation of graphene, as the introducing of conductive ion will lead to
The electrolytic decomposition of water quickly generates hydrogen and oxygen on the electrode, and it is blocked up to thereby result in the graphene removed from electrode, and
Aoxidize that insufficient, degree of oxidation is not high.Also, the above method obtain graphene oxide solution in often containing other impurities from
Son, i.e. conductive ion, the graphene powder that this often results in final dry acquisition is impure, will as raw material thus to obtain graphene
Without universality.So far, the simple and easy method that batch prepares high-purity graphene oxide is had not yet to see.Based on considerations above, originally
The cutting of patent combination electrochemical oxidation and water flow promotes graphite to aoxidize and remove in high-purity aqueous systems, due to electrochemistry oxygen
Water used in the process of change is deionization high purity water, and graphite is also the material of analysis and the above purity, determines graphite obtained
Alkene solution has high purity, can be used as high pure raw material and is applied among other kinds production and research.And this patent is set
The graphene degree of oxidation height of the method preparation of meter, good water solubility, surface functional group is abundant, the number of plies is few, in energy storage, urges
Change, bioprobe/imaging, medicament slow release, the treatment of cancer infrared emanation, chemical sensitisation, absorption/wastewater treatment etc. will
There is wide application space.
Summary of the invention
Present invention aim to address the preparation problem of high-purity graphene oxide, provide a kind of simple process, finished product uniformly,
The preparation method of high-purity graphene oxide of easy scale.
The technical solution adopted by the present invention: steps are as follows for the preparation method of high-purity graphene oxide:
Step 1) is 1~30M Ω cm using the graphite of fixed shape as conductivity is inserted in parallel into away from negative electrode-1Go from
In sub- water, the distance of graphite electrode remains 0.5~100cm；
Step 2) is put into a magnetic stir bar in the bottom equipped with device ion water container, by entire electrochemical reaction system
It is vertically arranged on magnetic stirring apparatus, magnetic stir bar is allowed to promote deionized water at the uniform velocity with 10~3000 revs/min of speed rotation
Rotation；
Step 3) adds the DC voltage of 1~100V using customary DC power supply between two graphite electrodes, keeps voltage
Constant with magnetic stirring speed, electrochemical reaction carries out 1~200 hour, becomes brown black suspension liquid later i.e. to deionized water
Stop reaction；
Step 4) obtains brown color aqueous solution after filtering brown black suspension liquid 1~10 time with filter paper, faces freezing or surpassing
The dry diameter that can be obtained is 0.001~10 μm of high-purity graphene oxide under the conditions of boundary；
The shape that is made of the graphite material is rodlike, cuboid or round pie；The graphite material is to analyze pure or light
It composes pure；
The length of the magnetic stir bar is 1~10cm, and diameter is 0.1~1cm；
The magnetic stir bar of one uniform rotation, magnetic stir bar and graphite are arranged at the bottom equipped with deionized water container
The distance of 1~5cm is kept between electrode, cannot be contacted with graphite electrode；
The filter paper for brown black suspension liquid filtering is qualitative or quantitative filter paper；
The method of the drying of the graphene solution is that freezing or super critical condition are dry；
A kind of high-purity graphene oxide, by the preparation method of the described in any item high-purity graphene oxides of the claims
It is made, the purity of the graphene is greater than 99.99%.
The preparation method principle of high-purity graphene oxide proposed by the present invention is: first inserting the electrode runs parallel of graphite material
Enter into deionized water；Promote the oxygen of graphite linings by the effect of electrochemical oxidation under conditions of hydro jet and DC voltage
Change and removing, the graphene solution of acquisition are high-purity graphene oxide powder after dry.
Beneficial effects of the present invention: without complicated preparation method, very high purity and degree of oxidation can be prepared in batches on a large scale
Higher graphene oxide, is easy to mass production；Without expensive instrument, it is different from the preparation side of traditional graphene oxide
The graphene oxide conductivity of method, preparation is higher, and graphene oxide possesses oxygenated functional group abundant, such as carboxyl, hydroxyl；
Therefore, this method have many advantages, such as simple process, easy prepare with scale, it is environmentally protective and preparation graphene oxide purity is high,
The number of plies is few, good water solubility, easily disperse, is particularly suitable to be used as the electrode material or conductive additive, chemistry of energy storage device
Sensor, catalyst and biomedicine etc..
Detailed description of the invention
The preparation flow figure of Fig. 1 graphene oxide
In figure: 1. DC power supplies；2. conducting wire；3. graphite electrode；4. container；5. deionized water；6. magnetic stir bar；7. magnetic
Power blender.
The infared spectrum of Fig. 2 graphene oxide
Ordinate is the infrared Absorption intensity of sample, no unit；Abscissa is the wave number of infrared spectroscopy, unit cm-1。
The Raman map of Fig. 3 graphene oxide
Ordinate is the intensity of Raman signal, no unit；Abscissa is the displacement of Raman spectrum, unit cm-1。
The transmission electron microscope picture of Fig. 4 graphene oxide
Specific embodiment
Embodiment 1
Measuring 400 milliliters of high purity water (18.4M Ω) first and taking a diameter is that the fish shape magnetic stir bar of 4cm exists
Be stamped one piece of polyfluortetraethylene plate with a thickness of 1cm in 500 milliliters of beaker, on beaker, on plate there are two at a distance of 7.5cm's and
Support jack of the hole that diameter is 0.7cm as fixed electrode, the carbon-point that two diameters are 0.6cm is connected to conducting wire respectively
On the positive and negative anodes of DC power supply, be inserted in parallel into the hole of polytetrafluoroethylene (PTFE), make graphite electrode most of not in high purity water and with
The magnetic stir bar of beaker bottom keeps certain distance.Then entire beaker device is vertically arranged on magnetic stirring apparatus, is adjusted
It saves magnetic stirring apparatus and reaches 2000 revs/min by the revolving speed of magnetic stir bar；Meanwhile the voltage on DC power supply is adjusted, make graphite
Voltage field between electrode is maintained at 30V, and due to being the low deionized water of conductivity, graphite electricity is shown on DC power supply instrumentation table
Electric current between pole is essentially 0A.
After stablizing to device, the high speed rotation had a meeting, an audience, etc. well under one's control with magnetic stir bar of direct current is kept；After power-up 96 hours, nothing
The transparent high purity water of color has gradually become dark brown solution, stops reaction immediately at this time, dark brown solution is taken out, with qualitative filter
Graphene solution is freeze-dried all over the graphene oxide solution that brown color can be obtained, high-purity oxygen can be obtained by paper filter 23
Graphite alkene powder.Infrared absorption spectrum (Fig. 2), Raman spectrum (Fig. 3) and transmission electron microscope (Fig. 4) is carried out to powder to survey
Examination, test result show that prepared graphene powder degree of oxidation is high, the number of plies is few, functional group is abundant, good water solubility.
Embodiment 2
Measuring 400 milliliters of deionized water (15.0M Ω) first and taking a diameter is that the fish shape magnetic stir bar of 4cm exists
Be stamped one piece of polyfluortetraethylene plate with a thickness of 1cm in 500 milliliters of beaker, on beaker, on plate there are two at a distance of 7.5cm's and
Support jack of the hole that diameter is 0.7cm as fixed electrode, the carbon-point that two diameters are 0.6cm is connected to conducting wire respectively
On the positive and negative anodes of DC power supply, be inserted in parallel into the hole of polytetrafluoroethylene (PTFE), make graphite electrode most of not in high purity water and with
The magnetic stir bar of beaker bottom keeps certain distance.Then entire beaker device is vertically arranged on magnetic stirring apparatus, is adjusted
It saves magnetic stirring apparatus and reaches 2000 revs/min by the revolving speed of magnetic stir bar；Meanwhile the voltage on DC power supply is adjusted, make graphite
Voltage field between electrode is maintained at 30V, due to being the lower deionized water of conductivity, shows graphite on DC power supply instrumentation table
Electric current between electrode is essentially 0A.
After stablizing to device, the high speed rotation had a meeting, an audience, etc. well under one's control with magnetic stir bar of direct current is kept；After power-up 96 hours, nothing
The transparent high purity water of color has gradually become dark brown solution, stops reaction immediately at this time, dark brown solution is taken out, with qualitative filter
Graphene solution is freeze-dried all over the graphene oxide solution that brown color can be obtained, high-purity oxygen can be obtained by paper filter 23
Graphite alkene powder.
Embodiment 3
Measuring 400 milliliters of deionized water (18.4M Ω) first and taking a diameter is that the fish shape magnetic stir bar of 4cm exists
Be stamped one piece of polyfluortetraethylene plate with a thickness of 1cm in 500 milliliters of beaker, on beaker, on plate there are two at a distance of 7.5cm's and
Support jack of the hole that diameter is 0.7cm as fixed electrode, the carbon-point that two diameters are 0.6cm is connected to conducting wire respectively
On the positive and negative anodes of DC power supply, be inserted in parallel into the hole of polytetrafluoroethylene (PTFE), make graphite electrode most of not in high purity water and with
The magnetic stir bar of beaker bottom keeps certain distance.Then entire beaker device is vertically arranged on magnetic stirring apparatus, no
Inoperative magnetic stirring apparatus is crossed, magnetic stir bar is allowed to remain stationary in solution bottom；The voltage on DC power supply is adjusted, graphite is made
Voltage field between electrode is maintained at 30V, and due to being the low deionized water of conductivity, graphite electricity is shown on DC power supply instrumentation table
Electric current between pole is essentially 0A.
After stablizing to device, direct current is kept to have a meeting, an audience, etc. well under one's control, after power-up 96 hours, colorless and transparent high purity water is gradually become
It is simultaneously molten all over can be obtained the extremely low brown color of graphene content with qualitative filter paper filter 23 to stop reaction for the brown color of very slight color
Liquid, although high-purity graphene oxide powder equally also can be obtained in graphene solution freeze-drying, yield is extremely low, thus may be used
See that the at the uniform velocity stirring of deionized water facilitates the removing of graphene oxide layer.
Embodiment 4
The deionized water (5M Ω) of 400 milliliters of measurement and a diameter are the fish shape magnetic stir bar of 4cm in 500 millis first
In the beaker risen, it is stamped one piece of polyfluortetraethylene plate with a thickness of 1cm on beaker, there are two at a distance of 7.5cm's and diameter on plate
For support jack of the hole as fixed electrode of 0.7cm, the carbon-point that two diameters are 0.6cm is connected to direct current with conducting wire respectively
On the positive and negative anodes of power supply, be inserted in parallel into the hole of polytetrafluoroethylene (PTFE), allow graphite electrode be largely placed in high purity water and and beaker
The magnetic stirring apparatus of bottom keeps certain distance.Then entire beaker device is placed on magnetic stirring apparatus, adjusts magnetic force and stirs
It mixes device and reaches 2000rpm by the revolving speed of magnetic stir bar；Meanwhile the voltage on DC power supply is adjusted, make between graphite electrode
Voltage field is maintained at 30V, due to being the lower deionized water of conductivity, shows between graphite electrode on DC power supply instrumentation table
Electric current is essentially 0A.
After stablizing to device, the high speed rotation had a meeting, an audience, etc. well under one's control with magnetic stir bar of direct current is kept；After power-up 72 hours, nothing
The transparent high purity water of color has gradually become dark brown solution, stops reaction immediately at this time, dark brown solution is taken out, with qualitative filter
The graphene oxide solution of brown color can be obtained in paper filter 23 time, but graphene degree of oxidation at this time is not so good as embodiment 1
Middle height, and particle is larger.
Embodiment 5
400 milliliters of hydrochloric acid solution (pH=1) is measured first and a diameter is the fish shape magnetic stir bar of 4cm 500
In the beaker of milliliter, it is stamped one piece of polyfluortetraethylene plate with a thickness of 1cm on beaker, there are two at a distance of 7.5cm's and straight on plate
Support jack of the hole that diameter is 0.7cm as fixed electrode, the carbon-point that two diameters are 0.6cm is connected to directly with conducting wire respectively
On the positive and negative anodes in galvanic electricity source, be inserted in parallel into the hole of polytetrafluoroethylene (PTFE), make graphite electrode most of not in high purity water and with burning
The magnetic stir bar in bottom of a cup portion keeps certain distance.Then entire beaker vertical means are placed on magnetic stirring apparatus, are adjusted
Magnetic stirring apparatus reaches 2000 revs/min by the revolving speed of magnetic stir bar；Meanwhile the voltage on DC power supply is adjusted, keep graphite electric
Voltage field between pole is maintained at 30V, and due to being hydrochloric acid solution, the electric current between graphite electrode is shown on DC power supply instrumentation table
It beats always, and constantly there is bubble to emerge on electrode, after a period of time, solution can not be obtained at black suspension
High-purity mangesium oxide graphene, but obtained the lower graphite powder of degree of oxidation.
Embodiment 6
Measure first 400 milliliters sodium hydroxide solution (pH=14) and diameter for 4cm fish shape magnetic stir bar
It is stamped one piece of polyfluortetraethylene plate with a thickness of 1cm in 500 milliliters of beaker, on beaker, there are two at a distance of 7.5cm's on plate
And the hole that diameter is 0.7cm connects the carbon-point that two diameters are 0.6cm as the support jack for fixing electrode with conducting wire respectively
It on the positive and negative anodes of DC power supply, is inserted in parallel into the hole of polytetrafluoroethylene (PTFE), graphite electrode is allowed largely to be placed in high purity water simultaneously
Certain distance is kept with the magnetic stir bar of beaker bottom.Then entire beaker system is vertically arranged on magnetic stirring apparatus,
It adjusts magnetic stirring apparatus and reaches 2000 revs/min by the revolving speed of magnetic stir bar；Meanwhile the voltage on DC power supply is adjusted, make stone
Voltage field between electrode ink is maintained at 30V, and due to being sodium hydroxide solution, solution conductivity rate is higher, DC power supply instrumentation table
Electric current between upper display graphite electrode is beated always, and constantly has bubble to emerge on graphite electrode, after a period of time,
Solution can not obtain high-purity mangesium oxide graphene at black suspension, but obtain that degree of oxidation is lower and particle is larger
Graphite powder.
Embodiment 7
400 milliliters of dehydrated alcohol is measured first and a diameter is burning of the fish shape magnetic stir bar of 4cm at 500 milliliters
In cup, it is stamped one piece of polyfluortetraethylene plate with a thickness of 1cm on beaker, there are two at a distance of 7.5cm's and diameter is 0.7cm on plate
Support jack of the hole as fixed electrode, the carbon-point that two diameters are 0.6cm is connected to DC power supply with conducting wire respectively
On positive and negative anodes, be inserted in parallel into the hole of polytetrafluoroethylene (PTFE), make graphite electrode most of not in high purity water and with beaker bottom
Magnetic stirring apparatus keeps certain distance.Then entire beaker system is vertically arranged on magnetic stirring apparatus, adjusts magnetic agitation
Device reaches 2000 revs/min by the revolving speed of magnetic stir bar；Meanwhile the voltage on DC power supply is adjusted, make between graphite electrode
Voltage field is maintained at 30V, due to being the extremely low dehydrated alcohol of conductivity, shows between graphite electrode on DC power supply instrumentation table
Electric current is essentially 0A.
After stablizing to device, the high-speed stirred of voltage and magnetic stir bar is kept；After power-up 120 hours, solution body
It is substantially unchanged.
In above example 1,2 graphene oxide purity is high, the number of plies is few, degree of oxidation is high, good water solubility, abundance,
And reaction system can be replaced flexibly, and the size of graphene oxide can also carry out appropriate regulation, method by the conductivity of water
It is simple and easy, environmentally protective.High-purity mangesium oxide graphene system is prepared using this method to realize for the first time.
Claims (1)
1. a kind of preparation method of high-purity graphene oxide, it is characterised in that:
It is 1~30M Ω cm that the graphite of fixed shape is inserted in parallel into conductivity as positive and negative electrode (3) by step 1)-1Go from
In sub- water (5), the distance of graphite electrode remains 0.5~100cm；
Step 2) is put into a magnetic stir bar (6) in the bottom equipped with deionized water container (4), by entire electrochemical reaction system
System is vertically arranged on magnetic stirring apparatus (7), and magnetic stir bar is allowed to promote deionized water with 10~3000 revs/min of speed rotation
At the uniform velocity rotate；
Step 3) adds the direct current of 1~100V using customary DC power supply (1) and by conducting wire (2) between two graphite electrodes
Pressure keeps voltage and magnetic stirring speed constant, and electrochemical reaction carries out 1~200 hour, and it is outstanding to become brownish black to deionized water
Stop reaction after supernatant liquid；
Step 4) obtains brown color aqueous solution after filtering brown black suspension liquid 1~10 time with filter paper, in freezing or overcritical item
The dry high-purity graphene oxide that can be obtained diameter and be 0.001~10 μm under part；
The shape that is made of the graphite material is rodlike, cuboid or round pie；The graphite material is to analyze pure or spectroscopic pure；
The length of the magnetic stir bar is 1~10cm, and diameter is 0.1~1cm；
The magnetic stir bar of one uniform rotation, magnetic stir bar and graphite electrode are arranged at the bottom equipped with deionized water container
Between keep 1~5cm distance, cannot be contacted with graphite electrode；
The filter paper for brown black suspension liquid filtering is qualitative or quantitative filter paper；
A kind of high-purity graphene oxide, by the preparation method system of the described in any item high-purity graphene oxides of the claims
, the purity of the graphene is greater than 99.99%.
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| CN112158833A (en) * | 2019-12-30 | 2021-01-01 | 北京工业大学 | Safe graphene oxide preparation method without chemical addition |
| CN112655714A (en) * | 2020-12-25 | 2021-04-16 | 河南煜和科技集团有限公司 | Graphene multi-composite system sterilization disinfectant |
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