CN106809821A - The preparation method of Graphene - Google Patents
The preparation method of Graphene Download PDFInfo
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- CN106809821A CN106809821A CN201710038194.8A CN201710038194A CN106809821A CN 106809821 A CN106809821 A CN 106809821A CN 201710038194 A CN201710038194 A CN 201710038194A CN 106809821 A CN106809821 A CN 106809821A
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Abstract
The invention belongs to technical field of graphene, more particularly to a kind of preparation method of Graphene mainly comprises the following steps:Step one, with class graphite mass as raw material, prepares class graphite oxide, stand-by;Step 2, makes A end entrance, B end outflow of the class graphite oxide that step one is prepared by pipeline;The pipeline is divided into n sections from A ends to B ends, and the equivalent-effect transistor radius of each segment pipe is followed successively by R1... ..., Rn, and there is Ri+1>RiSituation;Temperature in each segment pipe is followed successively by T1... ..., Tn, and there is Ti+1>TiSituation;Wherein, n is the integer more than or equal to 2;Step 3, the material that collection is obtained from step 2 B ends, that is, obtain Graphene.The beneficial effects of the present invention are:The pipe design (caliber becomes suddenly big) of optimization, can allow class graphite oxide to be moved in flow process more fully, and thermally equivalent, the state consistency of the instantaneous oxidation graphite of cleavage is more preferable, therefore obtained graphene product consistency of performance is more preferably.
Description
Technical field
The invention belongs to technical field of graphene, more particularly to a kind of preparation method of Graphene.
Background technology
2004, strong K seas nurse (Andre K.Geim) of peace moral of Univ Manchester UK etc. used mechanical stripping method
Graphene (Graphene) is prepared first, has thus pulled open material preparation, the prelude of operational research.So-called Graphene,
Refer to a kind of plates in hexagonal annular arrangement between carbon atom, be generally made up of single or multiple lift graphite flake layer, can be two
Dimension space infinitely extends, it may be said that be proper two-dimensional structure material.It has that specific surface area is big, electrical and thermal conductivity performance
The low outstanding advantages of excellent, thermal coefficient of expansion.Specifically, its advantage at least includes:Specific surface area (calculated value high:
2630m2/g);High conductivity, carrier transport rate (200000cm2/V•s);High heat conductance (5000W/mK);High intensity is high
Young's modulus (1100GPa), fracture strength (125GPa).Therefore it leads in energy storage field, heat transfer field and Materials with High Strength
Domain have greatly use prospect.
The existing method for preparing Graphene mainly has micromechanics stripping method, ultrahigh vacuum Graphene epitaxial growth method, oxygen
Change-reducing process, chemical vapour deposition technique (CVD), solvent stripping method, electrolysis and solvent-thermal method.In this serial of methods, oxygen
Change-reducing process is most prepared on a large scale at present in the method for Graphene with widest method.
However, when preparing Graphene using oxidation-reduction method, in reduction phase, in order to sufficiently peel off graphene oxide sheet
Layer simultaneously removes the oxygen-containing functional group on lamella, often during the course of the reaction, it is necessary to apply the atmosphere of high temperature, high vacuum, high temperature
During high vacuum, it is necessary to equipment cost it is higher, the production cost during simultaneous reactions is also of a relatively high, so that the method
The relatively costly of Graphene is prepared, Graphene is limited and is widely used.
In view of this, it is necessory to develop a kind of preparation method of new Graphene, the method can substantially reduce graphite
The production cost of alkene, to promote Graphene more widely to use.
The content of the invention
It is an object of the invention to:In view of the shortcomings of the prior art, a kind of preparation method of the Graphene for providing, the party
Method can substantially reduce the production cost of Graphene, to promote Graphene more widely to use.
In order to achieve the above object, the present invention is adopted the following technical scheme that:
A kind of preparation method of Graphene, mainly comprises the following steps:
Step one, with class graphite mass as raw material, prepares class graphite oxide, stand-by;
Step 2, makes A end entrance, B end outflow of the class graphite oxide that step one is prepared by pipeline;The pipeline is from A ends
N sections is divided into B ends, also, from A ends to B ends, the equivalent-effect transistor radius of each segment pipe is followed successively by R1, R2... ..., Rn, and exist
Ri+1>RiSituation, wherein, 1≤i≤n;From A ends to B ends, the temperature in each segment pipe is followed successively by T1, T2... ..., Tn, and deposit
In Ti+1>TiSituation, wherein, 1≤i≤n;From A ends to B ends, flow velocity of the class graphite oxide in each segment pipe is followed successively by V1, V2
... ..., Vn;Wherein, n is the integer more than or equal to 2;
Step 3, the material that collection is obtained from step 2 B ends, that is, obtain Graphene.
Improved as a kind of the of preparation method of Graphene of the present invention, in step 2, Ri+1≥2Ri, wherein, 1≤i≤n.
Improved as a kind of the of preparation method of Graphene of the present invention, in step 2, Ti≤ 180 DEG C, 180 DEG C<Ti+1, its
In, 1≤i≤n.
Improved as a kind of the of preparation method of Graphene of the present invention, in step 2, Ri+1≥4Ri, wherein, 1≤i≤n.
Improved as a kind of the of preparation method of Graphene of the present invention, 100 DEG C≤Ti≤ 150 DEG C, 250 DEG C≤Ti+1, its
In, 1≤i≤n.
Improved as a kind of the of preparation method of Graphene of the present invention, class graphite oxide described in step 1 be graphite oxide or/
And graphene oxide.
Improved as a kind of the of preparation method of Graphene of the present invention, be inert gas atmosphere in the pipeline described in step 2
Enclose, the inert gas is nitrogen or argon gas.
Improved as a kind of the of preparation method of Graphene of the present invention, 0.1m/s≤Vi, 1≤i≤n.
Improved as a kind of the of preparation method of Graphene of the present invention, pressurizeed at pipeline A ends or/and applied at pipeline B ends
Negative pressure so that i-th section flowing velocity with Vi of the class graphite oxide in pipeline.
It is prepared by raw material with class graphite mass in a kind of improvement step one as the preparation method of Graphene of the present invention
The method of class graphite oxide is:Hummers methods, Staudenmaier methods or Brodie methods.The preparation of class graphite oxide can be adopted
With various methods of the prior art, do not limited by the above method.
The beneficial effects of the present invention are:It is different from traditional graphene preparation method, Graphene is prepared using this method
When:
First, designed by pipeline configuration, allow class graphite oxide to automatically generate subnormal ambient during being flowed in pipeline, saved
The extra cost for increasing negative pressure is saved, so that reduction prepares the cost of Graphene;The principle of its foundation is:
1), perfect gas state equation:PVm=RT, quality m, volume V, pressure p, temperature T in formula;
2), bernoulli principle:P1+1/2 ρ v12+ ρ gh1=p2+1/2 ρ v22+ ρ gh2, p is the pressure of certain point in fluid in formula, and v is
The flow velocity of the fluid point, ρ is fluid density, and g is acceleration of gravity, and h is height where the point, and C is a constant h2;
3), continuity equation:A ρ U=constants, cross-sectional area A in formula, flow velocity is U, density p;
By three above formula, can obtain, when fluid flows in pipeline, if caliber becomes suddenly big, internal fluid pressure
Good general reduces suddenly;Now the fluid in Large Diameter Pipeline will produce pressure differential with the fluid in pipe with small pipe diameter, that is, form negative pressure.
Secondly, the pipe design (caliber becomes suddenly big) of optimization, can allow class graphite oxide to be moved more in flow process
Fully, thermally equivalent, the state consistency of the instantaneous oxidation graphite of cleavage is more preferable, therefore obtained graphene product performance is consistent
Property is more preferably;
Finally, the place for increasing suddenly in caliber, temperature is raised simultaneously so that class graphite oxide moment reaches negative pressure and cleavage temperature
Under the double action effect of degree, farthest there is cleavage, prepare the less graphene product of the graphite flake number of plies.
Specific embodiment
The present invention and its advantage are described in detail with reference to specific embodiment, but embodiment party of the invention
Formula not limited to this.
Comparative example 1
It is prepared by graphite oxide:According to graphite:Potassium permanganate:The concentrated sulfuric acid (mass concentration is 98%):Sodium nitrate=2.5:4.5:50:1
Relationship between quality, in 6 DEG C of reactor, add the concentrated sulfuric acid (concentration is 98%), sodium nitrate, graphite and potassium permanganate, stirring is equal
It is even;Pre-reaction slurry obtained above is placed in 4h is reacted in the environment of 6 DEG C, that is, obtain low-temp reaction product;According to deionization
Water:Low-temp reaction product=0.5:1 relationship between quality, the deionized water of 25 DEG C of selection is produced as diluent to above-mentioned low-temp reaction
Dilution is slowly added in thing, the phenomenon of feed time, temperature of charge change and dilution is observed and record;Finally obtained above-mentioned
To dilution be warming up to 90 DEG C, keeping temperature carries out the pyroreaction of 2h afterwards, that is, obtain be grafted oxygenated functional group oxidation
Graphite slurry;Washing à is carried out to the product after above-mentioned oxidation reaction with deionized water and filters à washing à filtering à ... operations, will
Heteroion removal therein, obtains pure graphite oxide, and dry afterwards, smashing obtains graphite oxide powder;
It is prepared by Graphene:Above-mentioned graphite oxide powder is placed in isometrical electron tubes type reacting furnace, is evacuated to -98kPa, heated up
To 300 DEG C, graphene powder is obtained after reaction 2h.
Embodiment 1
Step one, the preparation of graphite oxide:It is identical with comparative example;
Step 2, the preparation of Graphene:Vertical tubular furnace of the selection with two-stage structure, it includes the first paragraph stove being connected with each other
Pipe and second segment boiler tube, one end away from second segment boiler tube of first paragraph boiler tube is A ends, second segment boiler tube away from first paragraph stove
One end of pipe is B ends, and first paragraph boiler tube is provided with the valve whether both control connects with the junction of second segment boiler tube,
First paragraph boiler tube and second segment boiler tube are connected with nitrogen as protective gas;Wherein first paragraph boiler tube radius is 10cm, second segment
Boiler tube radius is 20cm;It is 180 DEG C to control first paragraph furnace tube temperature, and second segment furnace tube temperature is 250 DEG C;By graphite oxide from
The A ends of primary reformer pipe are added in first paragraph boiler tube, heat 3min so that graphite oxide is warming up to 180 DEG C, then opens valve,
Vacuumized at B ends simultaneously so that flow velocity of the graphite oxide in first paragraph boiler tube reaches 1m/s, afterwards into second segment stove
Pipe, and flow velocity of the graphite oxide in second segment boiler tube is 2m/s;Because boiler tube diameter moment becomes big so that graphite oxide is entering
Enter second segment boiler tube moment formation negative pressure, and graphite oxide fully flows in second segment boiler tube, is fully contacted with tube wall, is heated
Fully, it is expanded complete, obtain the graphene powder of function admirable.
Embodiment 2
Difference from Example 1 is:
Second segment boiler tube radius is 40cm;Remaining is same as Example 1, repeats no more.
Embodiment 3
Difference from Example 1 is:
Second segment boiler tube radius is 80cm, and flow velocity of the graphite oxide in second segment boiler tube is 1.5m/s;Protective gas is argon
Gas;Remaining is same as Example 1, repeats no more.
Embodiment 4
Difference from Example 1 is:
Second segment boiler tube radius is 40cm;First paragraph furnace tube temperature is 100 DEG C, while opening valve, is pressurizeed at A ends;Its
It is remaining same as Example 1, repeat no more.
Embodiment 5
Difference from Example 1 is:
Second segment boiler tube radius is 40cm;First paragraph furnace tube temperature is 140 DEG C, and flow velocity of the graphite oxide in second segment boiler tube
It is 3m/s;Remaining is same as Example 1, repeats no more.
Embodiment 6
Difference from Example 1 is:
Second segment boiler tube radius is 40cm;First paragraph furnace tube temperature is 160 DEG C, and first paragraph furnace tube temperature is 185 DEG C, graphite oxide
Flow velocity in first paragraph boiler tube is 10m/s, and protective gas is argon gas;Remaining is same as Example 1, repeats no more.
Embodiment 7
Difference from Example 1 is:
Second segment boiler tube radius is 40cm;First paragraph furnace tube temperature is 160 DEG C, and first paragraph furnace tube temperature is 240 DEG C, opens valve
While, pressurizeed at A ends;;Remaining is same as Example 1, repeats no more.
Embodiment 8
Difference from Example 1 is:
Step one is the preparation of graphene oxide:By the natural flake graphite of the mesh of 20g 50,50g sodium nitrate, 100g potassium permanganate
1h is cooled down respectively at 2 DEG C~4 DEG C with the concentrated sulfuric acid that 800g mass concentrations are 98%, is then added to be placed in stainless steel still shell
In ptfe autoclave, 1min is slowly stirred, covers tightly kettle cover, in 1h is stood at 2 DEG C~4 DEG C, then in 100 DEG C of baking ovens
Reaction 1h;After sufficiently cool, ptfe autoclave is taken out from stainless steel still shell, reactant mixture therein is slow
To in entering 6L deionized waters, the aqueous hydrogen peroxide solution that 90mL mass concentrations are 20% is stirring evenly and then adding into, stirring is to suspended
Liquid is glassy yellow, by the suspension suction filtration, washing to pH values to obtain graphene oxide after 7.
Step 2, the preparation of Graphene:Vertical tubular furnace of the selection with two-stage structure, it includes be connected with each other first
Section boiler tube and second segment boiler tube, one end away from second segment boiler tube of first paragraph boiler tube is A ends, second segment boiler tube away from first
One end of section boiler tube is B ends, and first paragraph boiler tube is provided with what whether both control connected with the junction of second segment boiler tube
Valve, first paragraph boiler tube and second segment boiler tube are connected with nitrogen as protective gas;Wherein first paragraph boiler tube radius is 10cm, the
Secondary reformer pipe radius is 40cm;It is 160 DEG C to control first paragraph furnace tube temperature, and second segment furnace tube temperature is 300 DEG C;By graphite oxide
Alkene is added in first paragraph boiler tube from the A ends of first paragraph boiler tube, heats 3min so that graphene oxide is warming up to 180 DEG C, then beats
Valve opening door, while being vacuumized at B ends so that flow velocity of the graphene oxide in first paragraph boiler tube reaches 1m/s, enters afterwards
Second segment boiler tube, and flow velocity of the graphene oxide in second segment boiler tube is 0.5m/s;Because boiler tube diameter moment becomes big so that
Graphene oxide fully flows into second segment boiler tube moment formation negative pressure, and graphene oxide in second segment boiler tube, with
Tube wall is fully contacted, and is heated fully, expanded complete, obtains the graphene powder of function admirable.
Embodiment 9
Difference from Example 8 is:
Flow velocity of the graphite oxide in first paragraph boiler tube is 0.1m/s in step 2;Remaining is same as Example 8, repeats no more.
Embodiment 10
Difference from Example 8 is:
Flow velocity of the graphite oxide in first paragraph boiler tube is 0.5m/s in step 2;Remaining is same as Example 8, repeats no more.
Embodiment 11
Difference from Example 1 is:
Step 2, the preparation of Graphene:Vertical tubular furnace of the selection with three-stage structure, it includes the first paragraph stove being sequentially connected
Pipe, second segment boiler tube and the 3rd section of boiler tube, one end away from second segment boiler tube of first paragraph boiler tube is A ends, the 3rd section of boiler tube
Away from second segment boiler tube one end be B ends, and first paragraph boiler tube and second segment boiler tube junction be provided with control the two connect
The junction of the first valve for whether leading to, second segment boiler tube and the 3rd section of boiler tube is provided with the second valve whether both control connects
Door, first paragraph boiler tube, second segment boiler tube and the 3rd section of boiler tube are connected with nitrogen as protective gas;Wherein first paragraph boiler tube radius
It is 10cm, second segment boiler tube radius is 40cm, and the 3rd section of boiler tube radius is 80cm;First paragraph furnace tube temperature is controlled for 180 DEG C, the
Secondary reformer pipe temperature is 250 DEG C, and the 3rd section of furnace tube temperature is 300 DEG C;Graphite oxide is added first from the A ends of first paragraph boiler tube
In section boiler tube, 3min is heated so that graphite oxide is warming up to 180 DEG C, the first valve and the second valve is then opened, while in B
Vacuumized at end so that flow velocity of the graphite oxide in first paragraph boiler tube reaches 1m/s, afterwards into second segment boiler tube, it is
Flow velocity in secondary reformer pipe is 2m/s, and the flow velocity in the 3rd section of boiler tube is 3m/s;Because boiler tube diameter moment becomes big so that oxygen
Graphite is entering second segment boiler tube and the 3rd section of boiler tube moment forms negative pressure, and graphite oxide is in second segment boiler tube and the 3rd section
Fully flowed in boiler tube, be fully contacted with tube wall, be heated fully, it is expanded complete, obtain the graphene powder of function admirable.
Embodiment 12
Difference from Example 1 is:
Step 2, the preparation of Graphene:Vertical tubular furnace of the selection with four segment structures, it includes the first paragraph stove being sequentially connected
Pipe, second segment boiler tube, the 3rd section of boiler tube and the 4th section of boiler tube, one end away from second segment boiler tube of first paragraph boiler tube is A ends, the
Four sections of boiler tubes are B ends away from the 3rd section of one end of boiler tube, and the junction of first paragraph boiler tube and second segment boiler tube is provided with
The junction of control the two first valve for whether connect, second segment boiler tube and the 3rd section of boiler tube be provided with the two connection of control and
The junction of the second no valve, the 3rd section of boiler tube and the 4th section of boiler tube is provided with the 3rd valve whether both control connects,
First paragraph boiler tube, second segment boiler tube, the 3rd section of boiler tube and the 4th section of boiler tube are connected with nitrogen as protective gas;Wherein first paragraph
Boiler tube radius is 10cm, and second segment boiler tube radius is 40cm, and the 3rd section of boiler tube radius is 80cm, and the 4th section of boiler tube radius is
100cm;It is 180 DEG C to control first paragraph furnace tube temperature, and second segment furnace tube temperature is 250 DEG C, and the 3rd section of furnace tube temperature is 300 DEG C,
4th section of furnace tube temperature is 320 DEG C;Graphite oxide is added in first paragraph boiler tube from the A ends of first paragraph boiler tube, 3min is heated, made
Obtain graphite oxide and be warming up to 180 DEG C, then open the first valve, the second valve and the 3rd valve, while vacuumized at B ends,
So that flow velocity of the graphite oxide in first paragraph boiler tube reaches 1m/s, afterwards into second segment boiler tube, it is in second segment boiler tube
Flow velocity be 2m/s, flow velocity in the 3rd section of boiler tube is 2.5m/s, and the flow velocity in the 4th section of boiler tube is 3.5m/s;Due to stove
Pipe diameter moment becomes big so that graphite oxide is forming negative into second segment boiler tube, the 3rd section of boiler tube and the 4th section of boiler tube moment
Press, and graphite oxide fully flows in second segment boiler tube, the 3rd section of boiler tube and the 4th section of boiler tube, is fully contacted with tube wall, receives
It is hot abundant, it is expanded complete, obtain the graphene powder of function admirable.
Product quality uniformity is characterized:With same condition, the experiment 3 of comparative example 1 and 1 ~ embodiment of embodiment 12 is repeated
Secondary, experiment sampling one, carries out specific surface area test every time, and test result is as shown in Table 1 and Table 2.
Table 1:The reaction condition and specific surface area test result of comparative example 1 and embodiment 1 to 10.
Table 2:The reaction condition and specific surface area test result of embodiment 11 and embodiment 12.
By Tables 1 and 2 it can be seen that:The specific surface area of the graphene powder prepared using the method for the present invention is consistent
Property very good, and the method very simple, it is easy to operate, the production cost of Graphene can be substantially reduced, be easy to promote stone
Large-scale, the wider application of black alkene.
The announcement and teaching of book according to the above description, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula is changed and changed.Therefore, the invention is not limited in above-mentioned specific embodiment, every those skilled in the art exist
On the basis of of the invention it is done it is any conspicuously improved, replace or modification belongs to protection scope of the present invention.This
Outward, although having used some specific terms in this specification, these terms merely for convenience of description, not to the present invention
Constitute any limitation.
Claims (10)
1. a kind of preparation method of Graphene, it is characterised in that mainly comprise the following steps:
Step one, with class graphite mass as raw material, prepares class graphite oxide, stand-by;
Step 2, makes A end entrance, B end outflow of the class graphite oxide that step one is prepared by pipeline;The pipeline is from A ends
N sections is divided into B ends, also, from A ends to B ends, the equivalent-effect transistor radius of each segment pipe is followed successively by R1, R2... ..., Rn, and exist
Ri+1>RiSituation, wherein, 1≤i≤n;From A ends to B ends, the temperature in each segment pipe is followed successively by T1, T2... ..., Tn, and deposit
In Ti+1>TiSituation, wherein, 1≤i≤n;From A ends to B ends, flow velocity of the class graphite oxide in each segment pipe is followed successively by V1, V2
... ..., Vn;Wherein, n is the integer more than or equal to 2;
Step 3, the material that collection is obtained from step 2 B ends, that is, obtain Graphene.
2. the preparation method of the Graphene described in a kind of claim 1, it is characterised in that in step 2, Ri+1≥2Ri, wherein, 1
≤i≤n。
3. the preparation method of the Graphene described in a kind of claim 1, it is characterised in that in step 2, Ti≤ 180 DEG C, 180 DEG C<
Ti+1, wherein, 1≤i≤n.
4. the preparation method of the Graphene described in a kind of claim 1 or 2, it is characterised in that in step 2, Ri+1≥4Ri, its
In, 1≤i≤n.
5. the preparation method of the Graphene described in a kind of claim 3, it is characterised in that 100 DEG C≤Ti≤ 150 DEG C, 250 DEG C≤
Ti+1, wherein, 1≤i≤n.
6. the preparation method of the Graphene described in a kind of claim 1, it is characterised in that class graphite oxide described in step 1 is oxygen
Graphite or/and graphene oxide.
7. the preparation method of the Graphene described in a kind of claim 1, it is characterised in that be inertia in the pipeline described in step 2
Atmosphere, the inert gas is nitrogen or argon gas.
8. the preparation method of the Graphene described in a kind of claim 1, it is characterised in that 0.1m/s≤Vi, 1≤i≤n.
9. the preparation method of the Graphene described in a kind of claim 1, it is characterised in that pressurizeed at pipeline A ends or/and in pipeline
B ends apply negative pressure so that i-th section flowing velocity with Vi of the class graphite oxide in pipeline.
10. the preparation method of the Graphene described in a kind of claim 1, it is characterised in that in step one, be with class graphite mass
Raw material prepare class graphite oxide method be:Hummers methods, Staudenmaier methods or Brodie methods.
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CN109250709A (en) * | 2018-12-07 | 2019-01-22 | 四川聚创石墨烯科技有限公司 | A kind of production system preparing graphene using low layer number graphene oxide |
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CN109305671B (en) * | 2018-12-07 | 2021-03-19 | 四川聚创石墨烯科技有限公司 | Method for preparing graphene by using low-layer graphene oxide |
CN109264701B (en) * | 2018-12-07 | 2021-03-19 | 四川聚创石墨烯科技有限公司 | Graphene and continuous production method thereof |
CN109264699B (en) * | 2018-12-07 | 2021-05-04 | 四川聚创石墨烯科技有限公司 | Preparation method of low-layer graphene |
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