CN110436450A - A method of removing graphite oxide prepares graphene oxide - Google Patents
A method of removing graphite oxide prepares graphene oxide Download PDFInfo
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- CN110436450A CN110436450A CN201910830123.0A CN201910830123A CN110436450A CN 110436450 A CN110436450 A CN 110436450A CN 201910830123 A CN201910830123 A CN 201910830123A CN 110436450 A CN110436450 A CN 110436450A
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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
- C01B32/198—Graphene oxide
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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
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The invention discloses a kind of methods that removing graphite oxide prepares graphene oxide, graphite oxide dispersion is prepared first, obtained graphite oxide dispersion is filtered, filter cake dilute hydrochloric acid and ultrapure water wash respectively, graphite oxide is obtained after drying, graphite oxide is then configured to suspension with ultrapure water, using dynamic high-pressure microjet lift-off processing, dispersion liquid centrifuge separation is taken into clear liquid again, so that it may obtain graphene oxide suspension.Operation of the present invention is convenient, and at low cost, effect is good, is easy to serialization large-scale production.
Description
Technical field
The present invention relates to a kind of methods that removing graphite oxide prepares graphene oxide, belong to new and high technology preparation nanometer material
Expect technical field.
Background technique
Graphene oxide (Graphene oxide, GO) is the oxide of graphene, the allusion quotation as plane polycyclic aromatic hydrocarbon race
Type substance because of hydbridized carbon atoms containing sp2, and is closely connected with covalent bond and forms honeycomb two dimensional crystal structure, rich in
Oxygen-containing functional group possesses unique electricity, optics, calorifics and mechanical performance, meanwhile, graphene oxide can be convenient by function
Change and be modified, and prepare the intermediate of graphene, it has also become domestic and international novel carbon-based material research hotspot causes very big pass
Note.Currently, to be used in sewage treatment, antibacterial and medicament slow release, nanocomposite, electrochemistry etc. many for graphene oxide
Domain variability achieves good research achievement.In recent years, market increases the demand of graphene oxide year by year, though scale,
The demand of high benefit installation is also very urgent.
The method that tradition prepares graphene oxide has Hummer, Brodie, Staudenmaier, usually by graphite or stone
Black alkene is used as and prepares raw material, wherein two methods of Brodie and Staudenmaier, although degree of oxidation is high, the oxygen used
Agent KClO3, smoke HNO3There is insecurity factor during the reaction, can also generate ClO2, NO2, N2O4Equal pernicious gases.
Hummers method is nineteen fifty-seven, and one kind that Hummers and Offeman are developed is safer, quickly and effectively prepares graphene oxide
Method, first prepare graphite oxide using the mixture processing graphite of sulfuric acid, sodium nitrate and potassium permanganate, then shelled again
From preparing graphene oxide.Hummers method is still widely used now, and product is with the complete carbon frame of height and Minimum Residual
Stay the maximum single-layer graphene oxide of impurity concentration.
The mode for removing generation graphene oxide from graphite oxide generallys use ultrasonication at present, and there are also documents
Report uses hot stripping method.Wherein, the product purity height of ultrasonic lift-off technology preparation, simple process, but it is not easy to serialization rule
Mould production；Hot stripping method includes that direct heating, microwave, flash of light, laser, plasma, electron beam, electric current etc. give thermal energy side
With the removing of oxygen-containing group reduction process can occur for formula, process, be prepare a kind of effective ways of graphene, meanwhile,
Heat treatment parameter can make functional form graphene oxygen content, functional group, crystal structure, lamellar structure, specific capacitance and conductivity
Generate different variations, it is more difficult to control；Hot exfoliation temperature is generally greater than 200 DEG C, and is higher than after 500 DEG C in order to avoid graphite oxide
Burning also needs inert gas, reducing atmosphere or vacuum to carry out starvation, operates more demanding.Therefore, a kind of efficient, operation letter
New method that is single, being able to achieve continuous scale removing graphite oxide production graphene oxide has good market application space.
Dynamic high-pressure microjet processing technique (Dynamic high pressure microfluidization, DHPM)
It is to collect a series of comprehensive function power such as intensive shear, high-speed impact, pressure instantaneous relase, the higher-order of oscillation, swollen quick-fried and air pocket in one
The emerging technology of body can be completed at the same time a variety of unit operations such as conveying, mixing, ultramicro grinding, pressurization, extruding.With tradition height
Pressure homogeneous technology compare, it has a characteristic that low temperature fast-crushing can be achieved in (1), because microjet in micropore runner flow velocity
It is exceedingly fast, mostly in 300m/s or more, crushing process moment be can be completed, thus the heating of crushing process is limited, is particularly conducive to pair
The crushing of heat sensitive material；(2) grain diameter is tiny after crushing and is evenly distributed, since 100% pulverized material must all lead to
It crosses micropore runner to be handled, the high velocity turbulent flow of accompanied by intense keeps material stress big and uniform therebetween, the dispersion of particle diameter distribution
It is small；(3) for material after ultra-fine grinding, superfine product generally all can be directly used for preparation production, be especially suitable for precious rare material
Crushing；(4) the operation is stable, long service life, jet mill chamber mostly uses diamond or structural ceramics to be made, very resistance to
Abrasion, corrosion-resistant, long service life, and runner is fixed geometry, the component that crucial pulverization is played in work will not be sent out
Raw any variation, the operation is stable.
Currently, dynamic high-pressure micro jetting technology is mainly used in food processing field, mainly include ultramicronising emulsifying homogeneous,
Liposome preparation, sterilizing and inactive enzyme and four class of big molecular modification, main function object have protein, lipid, dietary fiber and
The materials such as starch also have and are mainly used for ink, oil in chemical field applied to fields such as medicine, chemical industry, biology and cosmetics
Ink, the performance improvement of coating and fresh fuel development, the broken dispersion of inorganic pigment, various emulsifications are overlapped product etc., there are no
Report the strip applications for graphite oxide.
Graphite oxide prepares graphene oxide, and intermediate there are also an one-step desaltings to operate, and document report largely uses bag filter at present
Dialysis desalination is carried out, operating cost is high, cumbersome, amount is small, it is high to require system, is unfavorable for the needs of industrial mass production.
The present invention is directed to improve graphite oxide to prepare graphene oxide technology technology, provide it is a kind of it is novel, efficient, low at
Sheet, safety, the new method for preparing graphene oxide of continuous operation.
Summary of the invention
The object of the present invention is to provide a kind of method that removing graphite oxide prepares graphene oxide, this method is efficient, low
Cost, safely, can be continuously produced.
Inventor's discovery:
(1) divide 3 for the filter cake of glassy yellow graphite oxide dispersion using 45 DEG C of temperature, 3% dilute hydrochloric acid 150-200mL of mass concentration
After secondary washing, then with ultrapure water 150-200mL point 3 washing graphite oxide filter cakes, can sufficiently desalination removal of impurities, than using dialysis
Method desalting effect is more preferable, can make almost to contain only two kinds of elements of C, O in graphite oxide.
(2) the graphite oxide ultrapure water after desalination is prepared mass concentration is 5.0 mg/mL suspension, using 50 MPa
Operation pressure, dynamic microjet handle 4 times after, can obtain average-size be 263 nm, 91-955 nm distribution ratio be 92.5%
Graphene oxide, yield 93.4%.
A kind of method that removing graphite oxide prepares graphene oxide provided by the invention, method includes the following steps:
(1) at room temperature, it by 30 μm of graininess natural graphite 2g, sodium nitrate 1g addition 250mL there-necked flask, is placed in cryostat
It is cooled to 0 DEG C；Again the 50 mL concentrated sulfuric acids are slowly added to that 30 min are sufficiently stirred in there-necked flask, and keep the temperature of reaction system
Not higher than 5 DEG C；Then 0.3g potassium permanganate is added in there-necked flask and 30 min is sufficiently stirred, while keeping temperature of reaction system
Not higher than 10 DEG C；In 1h, then by 3 batches of addition there-necked flasks of 7g potassium permanganate point, temperature of reaction system is kept to be not higher than 20 DEG C；
(2) cryostat is withdrawn, reaction system 35 ± 3 DEG C is heated to water-bath, and 2h is sufficiently stirred, obtains brown suspension；
(3) 90 mL water are slowly added dropwise in brown suspension, it is dilute by control plus water speed control system no more than 90 DEG C
The suspension released reacts 15min at this temperature；
(4) H of mass concentration 30% is added into suspension2O2 The mixed solution of 7 mL and 45 DEG C of 55 m L of ultrapure water, obtains
Glassy yellow graphite oxide dispersion；
(5) dispersion liquid is filtered while hot, obtains yellowish-brown filter cake, the dilute hydrochloric acid 150-200mL of 45 DEG C of mass concentrations 3% of filter cake
After dividing 3 washings, then divided 3 times with ultrapure water 150-200mL and washed, then will obtain oxygen after filter cake transfer vacuum oven drying
Graphite；
(6) graphite oxide after desalination is configured to the suspension of concentration 5.0mg/mL with ultrapure water, using 50MPa operation pressure
Dynamic microjet is handled 4 times, and obtained brown dispersion liquid is centrifugated 30min at 3,000 rpm, clear liquid is collected, obtains oxygen
Graphite alkene suspension.
In step (5), 40 DEG C of drying temperature, drying time is for 24 hours.
Compared with prior art, the invention has the following advantages that
1, the present invention replaces the salinity impurity introduced in bag filter removing graphite oxide preparation process, operation side using ultrapure water
Just, at low cost, effect is good, is suitable for extensive desalting processing.
2, it is usually used in the method for graphite oxide removing for ultrasound removing and hot lift-off technology, wherein ultrasonic lift-off technology technique
Simply, but it is not easy to serialization large-scale production；Hot stripping method is a kind of effective ways for preparing graphene, but heat treatment parameter meeting
So that functional form graphene oxygen content, functional group, crystal structure, lamellar structure, specific capacitance and conductivity generate different variations,
It is more difficult to control, it operates more demanding.The present invention prepares graphene oxide using dynamic high-pressure micro jetting technology removing graphite oxide,
Have the advantages that it is efficient, easy to operate, be able to achieve continuous large-scale production.
Detailed description of the invention
Fig. 1 is scanning electron microscope power spectrum (EDS) figure of raw graphite.
Fig. 2 is scanning electron microscope power spectrum (EDS) figure without the graphite oxide of any desalting processing.
Fig. 3 is scanning electron microscope power spectrum (EDS) figure of the graphite oxide by the processing of dialysis desalting for 24 hours.
Fig. 4 is scanning electron microscope power spectrum (EDS) figure of the graphite oxide by washing three times.
Fig. 5 is dynamic high-pressure microjet number of processes to material particle size and distribution map.
Fig. 6 is the infared spectrum of raw graphite (a) and graphene oxide (b).
Fig. 7 is the Raman spectrogram of raw graphite and product graphene oxide.
Fig. 8 is the XRD diagram of raw graphite and product graphene oxide.
Fig. 9 is the uv-spectrogram of product graphene oxide.
Figure 10 is the atomic force microscopy figure of product graphene oxide.
Figure 11 is two-dimensional-thickness chart of product graphene oxide.
Specific embodiment
Embodiment:
At room temperature, it by 30 μm of graininess natural graphite 2g, sodium nitrate 1g addition 250mL there-necked flask, is placed in cold in cryostat
But to 0 DEG C；It is slowly added to the concentrated sulfuric acid of 50 mL mass fractions 98% that 30min to be sufficiently stirred in there-necked flask again, and keeps reacting
The temperature of system is not higher than 5 DEG C；Then 0.3g potassium permanganate is added in there-necked flask and is sufficiently stirred 30min, while keeping anti-
Answer system temperature not higher than 10 DEG C；In 1h, then by 3 batches of addition there-necked flasks of 7g potassium permanganate point, keep temperature of reaction system
Not higher than 20 DEG C；This stage is low-temp reaction.
Cryostat is withdrawn, reaction system 35 ± 3 DEG C is heated to water-bath, and 2h is sufficiently stirred, obtains brown suspension；This
Stage is medium temperature reaction.
90 mL water are slowly added dropwise in brown suspension, it is dilute by control plus water speed control system no more than 90 DEG C
The suspension released reacts 15min at this temperature；This stage is pyroreaction.
The H of mass concentration 30% is added into suspension2O2 The mixed solution of 7mL and 45 DEG C of ultrapure water 55mL, obtains bright
Oxide yellow graphite dispersing solution；
Dispersion liquid is filtered while hot, obtains yellowish-brown filter cake, the dilute hydrochloric acid 150mL of 45 DEG C of mass concentrations 3% of filter cake, which divides 3 times, to be washed
After washing, then divided 3 times with ultrapure water 150mL and washed, the drying at 40 DEG C of filter cake transfer vacuum oven is then obtained into oxygen afterwards for 24 hours
Graphite；
By raw graphite, without the graphite oxide, the graphite oxide by the processing of dialysis desalting for 24 hours, warp of any desalting processing
It crosses the graphite oxide of washing three times and carries out the observation of SEM Electronic Speculum and power spectrum EDS analysis, the result is shown in Figure 1 to Fig. 4 and subordinate list 1.Fig. 1 is extremely
Fig. 4 shows that raw graphite contains only two kinds of elements of C, O substantially, and purity is very high；Graphite oxide is converted to by Hummer method
Afterwards, more metallic element is introduced, is illustrated to obtain the graphene oxide of high-purity, it is necessary to carry out desalting processing.Comparison
Dialysis treatment and washing EDS figure three times and two kinds are operated element contained by obtained graphite oxide and percentage arranges for 24 hours
In table 1.Table 1 shows that washing and dialysis can effectively remove impurity, washes more preferable than the impurity-eliminating effect of dialysis, it was demonstrated that washing behaviour
Make it is feasible and low in cost, easy to operate, be more suitable for industrial scale production.
Graphite oxide after desalination is configured to the suspension of concentration 5.0mg/mL with ultrapure water, is operated and is pressed using 50MPa
Strong dynamic microjet is handled 4 times, and obtained brown dispersion liquid is centrifugated 30min at 3,000 rpm, clear liquid is collected, obtains
Graphene oxide suspension.Graphene oxide yield is calculated, yield is 93.4% at this time.
Size distribution measurement is carried out to the product for handling different numbers by high pressure microjet, as a result sees Fig. 5 and table 2.From
Fig. 5 and table 2 are it is found that after 2 times, 3 times, 4 processing, and the granularity of product is obviously reduced, and effect is obvious；Number of processes is more,
Particle diameter distribution is more biased to zonule.
The product obtained after high pressure microjet is handled 4 times is subjected to serial characterization, as a result sees Fig. 6-Figure 11.
The infared spectrum of natural flake graphite and product GO is compared, as shown in figure 3, the infared spectrum of product and raw material is poor
Unobvious, product is in 3438cm-1And 1405cm-1Locate the vibration absorption peak of appearance-OH respectively and deformation absorption peak, in 1726cm-1
There is the stretching vibration absworption peak of carbonyl C=O, 1052cm in place-1There is the stretching vibration peak of alkoxy C-O, 1620cm in place-1Place
There is the deformation vibration peak of adsorbed water molecule, it can be seen that, the flexible vibration for not occurring epoxy group (C-O) is removed in product infared spectrum
Outside dynamic peak, remaining characteristic peak occurs.
The Raman spectrogram of graphite raw material and product GO is compared, as shown in fig. 7, product GO is in 1340cm-1And 1592cm-1There are two apparent characteristic peaks in place, very close with document report.
As shown in figure 8, there is one on the diffraction pattern of graphite, sharp peak, 2 θ=26.4 °, corresponding interlamellar spacing are by force
3.35, by the typical diffractive peak for the graphite plane that orderly graphene forms；On the diffraction pattern of GO, the characteristic peak of graphite
It disappears, nearby wider diffraction maximum occurs in 2 θ=10.2 °, the interlamellar spacing of product is about 7.94, this explanation contains after reaction
Oxygen functional group is introduced into every layer of graphene surface, and graphite is transformed to graphene oxide.
According to the literature, there are two characteristic absorption peaks at about 230 and 300nm for graphite oxide (GO) aqueous solution, right respectively
Answer the transition of fragrance C-C key and the transition of C=O key；And the characteristic absorption peak of graphene (GN) corresponds to virtue at about 270nm
The transition of fragrant C-C key.Accordingly, the spectrogram of unknown product UV spectrum resulting under the conditions of same test and GO or GN are carried out pair
Than can determine that whether product is alternative one.The uv-spectrogram of this experiment products therefrom as shown in figure 9, in 229nm and
Occur two apparent absorption peaks at 300nm, it is consistent with document report, illustrate that product is graphene oxide.
The atomic force microscope images of product graphene oxide are as shown in Figure 10, it is seen that and the thickness of product is about 1.0 ~
1.2nm, the characteristics of meeting single-layer graphene oxide, lateral two-dimensional is about hundreds of nanometers.
Fig. 6-Figure 11 characterization result shows to be successfully prepared single-layer graphene oxide using high pressure micro jetting technology.
High pressure microjet treatment effect and efficiency of pcr product also have relationship with operating condition, and experiment compared using orthogonal test
Three graphite oxide mass concentration, operation pressure and number of operations conditions the results are shown in Table 3 to the reciprocal effect of efficiency of pcr product.It is logical
Crossing range analysis final optimization pass and obtaining optimal operating condition be graphite oxide mass concentration is 5 mg/mL, operation pressure 50
MPa is handled 4 times, and yield is up to 93.04%.
Table 1 is that scanning electron microscope power spectrum (EDS) element of sample desalting effect compares:
Table 2 is the influence that dynamic high-pressure microjet number of processes is distributed material two-dimensional:
3 dynamic high-pressure microjet of table removing graphite oxide prepares graphene oxide process conditions orthogonal experiments:
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, it is possible to understand that
These embodiments can be carried out with a variety of variations, modification, replacement, this hair without departing from the principles and spirit of the present invention
Bright range is defined by the following claims.
Claims (2)
1. a kind of method that removing graphite oxide prepares graphene oxide, which is characterized in that method includes the following steps:
(1) at room temperature, it by 30 μm of graininess natural graphite 2g, sodium nitrate 1g addition 250mL there-necked flask, is placed in cryostat
It is cooled to 0 DEG C；Again the 50 mL concentrated sulfuric acids are slowly added to that 30 min are sufficiently stirred in there-necked flask, and keep the temperature of reaction system
Not higher than 5 DEG C；Then 0.3g potassium permanganate is added in there-necked flask and 30 min is sufficiently stirred, while keeping temperature of reaction system
Not higher than 10 DEG C；In 1h, then by 3 batches of addition there-necked flasks of 7g potassium permanganate point, temperature of reaction system is kept to be not higher than 20 DEG C；
(2) cryostat is withdrawn, reaction system 35 ± 3 DEG C is heated to water-bath, and 2h is sufficiently stirred, obtains brown suspension；
(3) 90 mL water are slowly added dropwise in brown suspension, it is dilute by control plus water speed control system no more than 90 DEG C
The suspension released reacts 15min at this temperature；
(4) H of mass concentration 30% is added into suspension2O2 The mixed solution of 7 mL and 45 DEG C of 55 m L of ultrapure water, obtains
Glassy yellow graphite oxide dispersion；
(5) dispersion liquid is filtered while hot, obtains yellowish-brown filter cake, the dilute hydrochloric acid 150-200mL of 45 DEG C of mass concentrations 3% of filter cake
After dividing 3 washings, then divided 3 times with ultrapure water 150-200mL and washed, then will obtain oxygen after filter cake transfer vacuum oven drying
Graphite；
(6) graphite oxide after desalination is configured to the suspension of concentration 5.0mg/mL with ultrapure water, using 50MPa operation pressure
Dynamic microjet is handled 4 times, and obtained brown dispersion liquid is centrifugated 30min at 3,000 rpm, clear liquid is collected, obtains oxygen
Graphite alkene suspension.
2. a kind of method that removing graphite oxide prepares graphene oxide according to claim 1, which is characterized in that in step
Suddenly in (5), 40 DEG C of drying temperature, drying time is for 24 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111498839A (en) * | 2020-04-29 | 2020-08-07 | 青岛科技大学 | Ultrathin sheet layer reduced graphene oxide and synthesis method thereof |
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| CN102701199A (en) * | 2012-07-15 | 2012-10-03 | 桂林理工大学 | Method for preparing graphene oxide by dispersed emulsion assisted with Hummers method |
| CN106976870A (en) * | 2017-03-29 | 2017-07-25 | 天津工业大学 | Efficiently peel off the method that graphite powder prepares big size graphene |
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2019
- 2019-09-04 CN CN201910830123.0A patent/CN110436450A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701199A (en) * | 2012-07-15 | 2012-10-03 | 桂林理工大学 | Method for preparing graphene oxide by dispersed emulsion assisted with Hummers method |
| CN106976870A (en) * | 2017-03-29 | 2017-07-25 | 天津工业大学 | Efficiently peel off the method that graphite powder prepares big size graphene |
Non-Patent Citations (1)
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| SHUAISHUAI LIANG ET AL.: "Effects of Processing Parameters on Massive Production of Graphene by Jet Cavitation", 《J. NANOSCI. NANOTECHNOL.》 * |
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| CN111498839A (en) * | 2020-04-29 | 2020-08-07 | 青岛科技大学 | Ultrathin sheet layer reduced graphene oxide and synthesis method thereof |
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