CN108569689A - A kind of preparation method for the graphene that purity is high, performance is stablized - Google Patents
A kind of preparation method for the graphene that purity is high, performance is stablized Download PDFInfo
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
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Abstract
The present invention discloses a kind of preparation method of high, performance stabilization the graphene of purity, includes the raw material of following parts by weight proportioning：48 parts of potassium hydroxide, 50 70 parts of expanded graphite, 10 14 parts of threonine, 13 parts of dioxanes, 12 18 parts of the concentrated sulfuric acid, 21 25 parts of concentrated nitric acid, 35 parts of diethyl hydroxylamine, 11 13 parts of vinyl bis-stearamides, 35 parts of N methylformamide, 19 21 parts of tetramethyl ammonium hydrogen carbonate, 1 butyl, 313 parts of methylimidazole bis-trifluoromethylsulfoandimide salt, 0.1 0.3 parts of octafluoro toluene, 57 parts of calcium hypochlorite, 15 parts of hydrazine hydrate, 12 16 parts of naphthalenetetracarbacidic acidic dianhydride；The preparation method for the graphene that the purity is high, performance is stablized can produce the graphene that purity is higher, performance is stablized.
Description
Technical field
The preparation method for the graphene that high, performance that the present invention relates to a kind of purity is stablized.
Background technology
Graphene (Graphene) is a kind of cellular flat film formed with sp2 hybrid forms by carbon atom, is one
There are one the quasi- two-dimensional material of atomic layer level thickness, monoatomic layer graphite only is done so being called for kind.Its thickness is about
0.335nm, according to the difference of preparation method, there are different fluctuatings, usually in height about 1nm of vertical direction or so, water
Square to width about 10nm to 25nm, be in addition to diamond all carbon crystals (zero dimension fullerene, one-dimensional carbon nanotube, three
Body is tieed up to graphite) basic structural unit.
Mechanical stripping method is to obtain graphene layer material using the friction and relative motion between object and graphene
Method.This method is easy to operate, and obtained graphene generally remains complete crystal structure [3].Two, Britain in 2004
Scientifical use adhesive tape carries out natural graphite the method that stripping layer by layer obtains graphene, is also classified as mechanical stripping method, this
Method is once considered low production efficiency, can not industrial volume production.
Oxidation-reduction method is by using the oxidants such as the chemical reagent such as sulfuric acid, nitric acid and potassium permanganate, hydrogen peroxide by day
Right graphite oxidation increases the spacing between graphite linings, oxide is inserted between layers in graphite, and graphite oxide is made
(Graphite Oxide).Then reactant is washed, and low temperature drying is carried out to the solid after cleaning, oxidation stone is made
Ink powder body.Graphite oxide powder is removed by the methods of physics stripping, high-temperature expansion, graphene oxide is made.Finally
Graphene oxide is restored by chemical method, obtains graphene (RGO).This method is easy to operate, and yield is high, but product matter
It measures relatively low [4].Oxidation-reduction method is using strong acid such as sulfuric acid, nitric acid, and there are larger danger, and must be carried out using a large amount of water
Cleaning, the big larger environmental pollution of band.
The graphene prepared using oxidation-reduction method, it is easily modified containing more rich oxygen-containing functional group.But due to right
When graphene oxide is restored, it is more difficult to which the oxygen content of graphene after control reduction, simultaneous oxidation graphene is in sunlight, fortune
It can constantly be restored under the influence of high temperature etc. is every extraneous in compartment when defeated, therefore the graphene of oxidation-reduction method production is by batch product
Quality it is often inconsistent, it is difficult to Control platform.
Many people obscure graphite oxide, graphene oxide, redox graphene conceptual understanding at present.Graphite oxide is in
Brown is graphite and oxide condensate.Graphene oxide system removes graphite oxide to the production after single layer, bilayer or few layer
Object, containing a large amount of oxygen-containing group, therefore graphene oxide is non-conductive, and graphene oxide property is active, special in use
It is not to participate in high-temperature material process, can constantly restores and release the gases such as sulfur dioxide.By by graphene oxide
Product after reduction could be known as graphene (redox graphene).
SiC epitaxys are by under the hot environment of ultrahigh vacuum, making silicon atom distillation be detached from material, and remaining C is former
Son is by group Reconfiguration of form certainly, to obtain the graphene based on SiC substrate.This method can obtain the graphite of high quality
Alkene, but this method is higher to equipment requirement.
But the preparation method of graphene now produces the graphene that purity is relatively low, performance is unstable.
Invention content
In view of this, this is to provide with goal of the invention a kind of can produce purity is higher, performance is stablized graphene
Preparation method.
In order to solve the above-mentioned technical problem, the technical scheme is that：
A kind of preparation method for the graphene that purity is high, performance is stablized includes the raw material of following parts by weight proportioning：Hydrogen-oxygen
Change 4-8 parts of potassium, 50-70 parts of expanded graphite, 10-14 parts of threonine, 1-3 parts of dioxanes, 12-18 parts of the concentrated sulfuric acid, concentrated nitric acid 21-25
Part, 3-5 parts of diethyl hydroxylamine, 11-13 parts of vinyl bis-stearamides, 3-5 parts of N-METHYLFORMAMIDE, tetramethyl ammonium hydrogen carbonate
19-21 parts, 1-3 parts of 1- butyl -3- methylimidazoles bis-trifluoromethylsulfoandimide salt, 0.1-0.3 parts of octafluoro toluene, calcium hypochlorite 5-
7 parts, 1-5 parts of hydrazine hydrate, 12-16 parts of naphthalenetetracarbacidic acidic dianhydride.
Further, the graphene that purity height, performance are stablized includes the raw material of following parts by weight proportioning：Hydrogen
4 parts of potassium oxide, 50 parts of expanded graphite, 10 parts of threonine, 1 part of dioxanes, 12 parts of the concentrated sulfuric acid, 21 parts of concentrated nitric acid, diethyl hydroxylamine 3
Part, 11 parts of vinyl bis-stearamides, 3 parts of N-METHYLFORMAMIDE, 19 parts of tetramethyl ammonium hydrogen carbonate, 1- butyl -3- methylimidazoles
1 part of bis-trifluoromethylsulfoandimide salt, 0.1 part of octafluoro toluene, 5 parts of calcium hypochlorite, 1 part of hydrazine hydrate, 12 parts of naphthalenetetracarbacidic acidic dianhydride.
Further, the graphene that purity height, performance are stablized includes the raw material of following parts by weight proportioning：Hydrogen
8 parts of potassium oxide, 70 parts of expanded graphite, 14 parts of threonine, 3 parts of dioxanes, 18 parts of the concentrated sulfuric acid, 25 parts of concentrated nitric acid, diethyl hydroxylamine 5
Part, 13 parts of vinyl bis-stearamides, 5 parts of N-METHYLFORMAMIDE, 21 parts of tetramethyl ammonium hydrogen carbonate, 1- butyl -3- methylimidazoles
3 parts of bis-trifluoromethylsulfoandimide salt, 0.3 part of octafluoro toluene, 7 parts of calcium hypochlorite, 5 parts of hydrazine hydrate, 16 parts of naphthalenetetracarbacidic acidic dianhydride.
Further, the graphene that purity height, performance are stablized includes the raw material of following parts by weight proportioning：Hydrogen
6 parts of potassium oxide, 60 parts of expanded graphite, 12 parts of threonine, 2 parts of dioxanes, 15 parts of the concentrated sulfuric acid, 23 parts of concentrated nitric acid, diethyl hydroxylamine 4
Part, 12 parts of vinyl bis-stearamides, 4 parts of N-METHYLFORMAMIDE, 20 parts of tetramethyl ammonium hydrogen carbonate, 1- butyl -3- methylimidazoles
2 parts of bis-trifluoromethylsulfoandimide salt, 0.2 part of octafluoro toluene, 6 parts of calcium hypochlorite, 3 parts of hydrazine hydrate, 14 parts of naphthalenetetracarbacidic acidic dianhydride.
A kind of preparation method for the graphene that purity is high, performance is stablized is as follows：
1) it to 60 parts of 6 parts of potassium hydroxide of addition of expanded graphite, is placed in ultrasonic disperse machine, ultrasonic power 750, oxygen is formed after 2h
Graphite alkene suspension；
2) 12 parts of threonine, 2 parts of dioxanes, 4 parts of diethyl hydroxylamine, vinyl will be added in the graphene suspension in step 1)
12 parts of bis-stearamides, 4 parts of N-METHYLFORMAMIDE, 20 parts of tetramethyl ammonium hydrogen carbonate, are placed in a centrifuge, centrifugation rate is
3200r/min, time 20min, temperature are maintained at 25 DEG C, obtain graphene oxide colloidal solution；
3) it by 23 parts of 15 parts of the concentrated sulfuric acid, concentrated nitric acid mixing, is placed in blender, stir speed (S.S.) 300r/min, time 1h, temperature
Degree is maintained at 30 DEG C, obtains mixed liquor；
4) it will be added in the mixed liquor in step 3) in the graphene colloidal solution in step 2), by the effect of dryer,
By moisture evaporation, graphene oxide colloid is obtained；
5) by 2 parts of 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimides salt, 0.2 part of octafluoro toluene, 6 parts of calcium hypochlorite, naphthalene four
14 parts of formic acid dianhydride is added in centrifuge, centrifugation rate 2000r/min, centrifugation time 30min, and temperature is maintained at 75
DEG C, obtain mixed liquor；
6) mixed liquor of step 5) is added in the graphene colloid of step 4), is filtered after being heated to 90 DEG C, it is cooling, it obtains
To graphene oxide；
7) 3 parts of hydrazine hydrate will be added in the graphene oxide in step 6), heating is stirred to obtained system, until yellow
Cotton-shaped graphene oxide becomes black suspension in solution, is filtered with 0.35 μm of filter wash after cooling, and filter cake is cold
Dry 48h is lyophilized to get to graphene.
The technology of the present invention effect major embodiment is in the following areas：By the way that potassium hydroxide, expanded graphite, threonine, two are added
Oxane, the concentrated sulfuric acid, concentrated nitric acid, diethyl hydroxylamine, vinyl bis-stearamides can produce the higher graphene of purity, pass through
Be added N-METHYLFORMAMIDE, tetramethyl ammonium hydrogen carbonate, 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimides salt, octafluoro toluene,
Calcium hypochlorite, hydrazine hydrate, naphthalenetetracarbacidic acidic dianhydride are capable of the graphene of production performance stabilization.
Specific implementation mode
Embodiment 1
The graphene that a kind of purity is high, performance is stablized includes the raw material of following parts by weight proportioning：4 parts of potassium hydroxide, expansion stone
50 parts of ink, 10 parts of threonine, 1 part of dioxanes, 12 parts of the concentrated sulfuric acid, 21 parts of concentrated nitric acid, 3 parts of diethyl hydroxylamine, vinyl are double stearic
11 parts of amide, 3 parts of N-METHYLFORMAMIDE, 19 parts of tetramethyl ammonium hydrogen carbonate, 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimides
1 part of salt, 0.1 part of octafluoro toluene, 5 parts of calcium hypochlorite, 1 part of hydrazine hydrate, 12 parts of naphthalenetetracarbacidic acidic dianhydride.
A kind of preparation method for the graphene that purity is high, performance is stablized is as follows：
1) it to 50 parts of 4 parts of potassium hydroxide of addition of expanded graphite, is placed in ultrasonic disperse machine, ultrasonic power 750, oxygen is formed after 2h
Graphite alkene suspension；
2) 10 parts of threonine, 1 part of dioxanes, 3 parts of diethyl hydroxylamine, vinyl will be added in the graphene suspension in step 1)
11 parts of bis-stearamides, 3 parts of N-METHYLFORMAMIDE, 19 parts of tetramethyl ammonium hydrogen carbonate, are placed in a centrifuge, centrifugation rate is
3200r/min, time 20min, temperature are maintained at 25 DEG C, obtain graphene oxide colloidal solution；
3) it by 21 parts of 12 parts of the concentrated sulfuric acid, concentrated nitric acid mixing, is placed in blender, stir speed (S.S.) 300r/min, time 1h, temperature
Degree is maintained at 30 DEG C, obtains mixed liquor；
4) it will be added in the mixed liquor in step 3) in the graphene colloidal solution in step 2), by the effect of dryer,
By moisture evaporation, graphene oxide colloid is obtained；
5) by 1 part of 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimides salt, 0.5 part of octafluoro toluene, 5 parts of calcium hypochlorite, naphthalene four
12 parts of formic acid dianhydride is added in centrifuge, centrifugation rate 2000r/min, centrifugation time 30min, and temperature is maintained at 75
DEG C, obtain mixed liquor；
6) mixed liquor of step 5) is added in the graphene colloid of step 4), is filtered after being heated to 90 DEG C, it is cooling, it obtains
To graphene oxide；
7) 1 part of hydrazine hydrate will be added in the graphene oxide in step 6), heating is stirred to obtained system, until yellow
Cotton-shaped graphene oxide becomes black suspension in solution, is filtered with 0.35 μm of filter wash after cooling, and filter cake is cold
Dry 48h is lyophilized to get to graphene.
Embodiment 2
A kind of graphene for the graphene that purity is high, performance is stablized includes the raw material of following parts by weight proportioning：Potassium hydroxide 8
Part, 70 parts of expanded graphite, 14 parts of threonine, 3 parts of dioxanes, 18 parts of the concentrated sulfuric acid, 25 parts of concentrated nitric acid, 5 parts of diethyl hydroxylamine, ethylene
The double fluoroforms of 13 parts of base bis-stearamides, 5 parts of N-METHYLFORMAMIDE, 21 parts of tetramethyl ammonium hydrogen carbonate, 1- butyl -3- methylimidazoles
3 parts of sulfimide salt, 0.3 part of octafluoro toluene, 7 parts of calcium hypochlorite, 5 parts of hydrazine hydrate, 16 parts of naphthalenetetracarbacidic acidic dianhydride.
A kind of preparation method for the graphene that purity is high, performance is stablized is as follows：
1) it to 70 parts of 8 parts of potassium hydroxide of addition of expanded graphite, is placed in ultrasonic disperse machine, ultrasonic power 750, oxygen is formed after 2h
Graphite alkene suspension；
2) 14 parts of threonine, 3 parts of dioxanes, 5 parts of diethyl hydroxylamine, vinyl will be added in the graphene suspension in step 1)
13 parts of bis-stearamides, 5 parts of N-METHYLFORMAMIDE, 21 parts of tetramethyl ammonium hydrogen carbonate, are placed in a centrifuge, centrifugation rate is
3200r/min, time 20min, temperature are maintained at 25 DEG C, obtain graphene oxide colloidal solution；
3) it by 25 parts of 18 parts of the concentrated sulfuric acid, concentrated nitric acid mixing, is placed in blender, stir speed (S.S.) 300r/min, time 1h, temperature
Degree is maintained at 30 DEG C, obtains mixed liquor；
4) it will be added in the mixed liquor in step 3) in the graphene colloidal solution in step 2), by the effect of dryer,
By moisture evaporation, graphene oxide colloid is obtained；
5) by 3 parts of 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimides salt, 0.3 part of octafluoro toluene, 7 parts of calcium hypochlorite, naphthalene four
16 parts of formic acid dianhydride is added in centrifuge, centrifugation rate 2000r/min, centrifugation time 30min, and temperature is maintained at 75
DEG C, obtain mixed liquor；
6) mixed liquor of step 5) is added in the graphene colloid of step 4), is filtered after being heated to 90 DEG C, it is cooling, it obtains
To graphene oxide；
7) 5 parts of hydrazine hydrate will be added in the graphene oxide in step 6), heating is stirred to obtained system, until yellow
Cotton-shaped graphene oxide becomes black suspension in solution, is filtered with 0.35 μm of filter wash after cooling, and filter cake is cold
Dry 48h is lyophilized to get to graphene.
Embodiment 3
The graphene that a kind of purity is high, performance is stablized includes the raw material of following parts by weight proportioning：6 parts of potassium hydroxide, expansion stone
60 parts of ink, 12 parts of threonine, 2 parts of dioxanes, 15 parts of the concentrated sulfuric acid, 23 parts of concentrated nitric acid, 4 parts of diethyl hydroxylamine, vinyl are double stearic
12 parts of amide, 4 parts of N-METHYLFORMAMIDE, 20 parts of tetramethyl ammonium hydrogen carbonate, 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimides
2 parts of salt, 0.2 part of octafluoro toluene, 6 parts of calcium hypochlorite, 3 parts of hydrazine hydrate, 14 parts of naphthalenetetracarbacidic acidic dianhydride.
A kind of preparation method for the graphene that purity is high, performance is stablized is as follows：
1) it to 60 parts of 6 parts of potassium hydroxide of addition of expanded graphite, is placed in ultrasonic disperse machine, ultrasonic power 750, oxygen is formed after 2h
Graphite alkene suspension；
2) 12 parts of threonine, 2 parts of dioxanes, 4 parts of diethyl hydroxylamine, vinyl will be added in the graphene suspension in step 1)
12 parts of bis-stearamides, 4 parts of N-METHYLFORMAMIDE, 20 parts of tetramethyl ammonium hydrogen carbonate, are placed in a centrifuge, centrifugation rate is
3200r/min, time 20min, temperature are maintained at 25 DEG C, obtain graphene oxide colloidal solution；
3) it by 23 parts of 15 parts of the concentrated sulfuric acid, concentrated nitric acid mixing, is placed in blender, stir speed (S.S.) 300r/min, time 1h, temperature
Degree is maintained at 30 DEG C, obtains mixed liquor；
4) it will be added in the mixed liquor in step 3) in the graphene colloidal solution in step 2), by the effect of dryer,
By moisture evaporation, graphene oxide colloid is obtained；
5) by 2 parts of 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimides salt, 0.2 part of octafluoro toluene, 6 parts of calcium hypochlorite, naphthalene four
14 parts of formic acid dianhydride is added in centrifuge, centrifugation rate 2000r/min, centrifugation time 30min, and temperature is maintained at 75
DEG C, obtain mixed liquor；
6) mixed liquor of step 5) is added in the graphene colloid of step 4), is filtered after being heated to 90 DEG C, it is cooling, it obtains
To graphene oxide；
7) 3 parts of hydrazine hydrate will be added in the graphene oxide in step 6), heating is stirred to obtained system, until yellow
Cotton-shaped graphene oxide becomes black suspension in solution, is filtered with 0.35 μm of filter wash after cooling, and filter cake is cold
Dry 48h is lyophilized to get to graphene.
Experimental example
It is experimental group to choose the graphene that 100 pieces of purity height of the invention, performances are stablized, and it is pair to choose 100 blocks of common graphite alkene
According to group, experimental group is as big small size used in control group, and thickness all 10cm, and record is as a result, it is tested after the test
As a result as follows：
| The specific surface area m2/g of graphene | Graphene purity wt.% | |
| Experimental group | 2100 | 99.9% |
| Control group | 1128 | 95% |
It is learnt by experimental result, the preparation method of the graphene that purity of the invention is high, performance is stablized can be produced pure
The graphene that degree is higher, performance is stablized.
The technology of the present invention effect major embodiment is in the following areas：By the way that potassium hydroxide, expanded graphite, threonine, two are added
Oxane, the concentrated sulfuric acid, concentrated nitric acid, diethyl hydroxylamine, vinyl bis-stearamides can produce the higher graphene of purity, pass through
Be added N-METHYLFORMAMIDE, tetramethyl ammonium hydrogen carbonate, 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimides salt, octafluoro toluene,
Calcium hypochlorite, hydrazine hydrate, naphthalenetetracarbacidic acidic dianhydride are capable of the graphene of production performance stabilization.
Certainly, the representative instance of the above only present invention, in addition to this, the present invention can also have other a variety of specific implementations
Mode, all technical solutions formed using equivalent substitution or equivalent transformation, is all fallen within the scope of protection of present invention.
Claims (3)
1. a kind of preparation method for the graphene that purity is high, performance is stablized, it is characterised in that：Match including following parts by weight
The raw material of ratio：4-8 parts of potassium hydroxide, 50-70 parts of expanded graphite, 10-14 parts of threonine, 1-3 parts of dioxanes, concentrated sulfuric acid 12-18
Part, 21-25 parts of concentrated nitric acid, 3-5 parts of diethyl hydroxylamine, 11-13 parts of vinyl bis-stearamides, 3-5 parts of N-METHYLFORMAMIDE, four
19-21 parts of methyl carbonic acid hydrogen ammonium, 1-3 parts of 1- butyl -3- methylimidazoles bis-trifluoromethylsulfoandimide salt, octafluoro toluene 0.1-0.3
Part, 5-7 parts of calcium hypochlorite, 1-5 parts of hydrazine hydrate, 12-16 parts of naphthalenetetracarbacidic acidic dianhydride.
1) it to 60 parts of 6 parts of potassium hydroxide of addition of expanded graphite, is placed in ultrasonic disperse machine, ultrasonic power 750, oxygen is formed after 2h
Graphite alkene suspension；
2) 12 parts of threonine, 2 parts of dioxanes, 4 parts of diethyl hydroxylamine, vinyl will be added in the graphene suspension in step 1)
12 parts of bis-stearamides, 4 parts of N-METHYLFORMAMIDE, 20 parts of tetramethyl ammonium hydrogen carbonate, are placed in a centrifuge, centrifugation rate is
3200r/min, time 20min, temperature are maintained at 25 DEG C, obtain graphene oxide colloidal solution；
3) it by 23 parts of 15 parts of the concentrated sulfuric acid, concentrated nitric acid mixing, is placed in blender, stir speed (S.S.) 300r/min, time 1h, temperature
Degree is maintained at 30 DEG C, obtains mixed liquor；
4) it will be added in the mixed liquor in step 3) in the graphene colloidal solution in step 2), by the effect of dryer,
By moisture evaporation, graphene oxide colloid is obtained；
5) by 2 parts of 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimides salt, 0.2 part of octafluoro toluene, 6 parts of calcium hypochlorite, naphthalene four
14 parts of formic acid dianhydride is added in centrifuge, centrifugation rate 2000r/min, centrifugation time 30min, and temperature is maintained at 75
DEG C, obtain mixed liquor；
6) mixed liquor of step 5) is added in the graphene colloid of step 4), is filtered after being heated to 90 DEG C, it is cooling, it obtains
To graphene oxide；
7) 3 parts of hydrazine hydrate will be added in the graphene oxide in step 6), heating is stirred to obtained system, until yellow
Cotton-shaped graphene oxide becomes black suspension in solution, is filtered with 0.35 μm of filter wash after cooling, and filter cake is cold
Dry 48h is lyophilized to get to graphene.
The preparation method for the graphene that 2. purity as described in claim 1 is high, performance is stablized, it is characterised in that：1) to
50 parts of 4 parts of potassium hydroxide of addition of expanded graphite, are placed in ultrasonic disperse machine, ultrasonic power 750, graphene oxide are formed after 2h
Suspension；
2) 10 parts of threonine, 1 part of dioxanes, 3 parts of diethyl hydroxylamine, vinyl will be added in the graphene suspension in step 1)
11 parts of bis-stearamides, 3 parts of N-METHYLFORMAMIDE, 19 parts of tetramethyl ammonium hydrogen carbonate, are placed in a centrifuge, centrifugation rate is
3200r/min, time 20min, temperature are maintained at 25 DEG C, obtain graphene oxide colloidal solution；
3) it by 21 parts of 12 parts of the concentrated sulfuric acid, concentrated nitric acid mixing, is placed in blender, stir speed (S.S.) 300r/min, time 1h, temperature
Degree is maintained at 30 DEG C, obtains mixed liquor；
4) it will be added in the mixed liquor in step 3) in the graphene colloidal solution in step 2), by the effect of dryer,
By moisture evaporation, graphene oxide colloid is obtained；
5) by 1 part of 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimides salt, 0.5 part of octafluoro toluene, 5 parts of calcium hypochlorite, naphthalene four
12 parts of formic acid dianhydride is added in centrifuge, centrifugation rate 2000r/min, centrifugation time 30min, and temperature is maintained at 75
DEG C, obtain mixed liquor；
6) mixed liquor of step 5) is added in the graphene colloid of step 4), is filtered after being heated to 90 DEG C, it is cooling, it obtains
To graphene oxide；
7) 1 part of hydrazine hydrate will be added in the graphene oxide in step 6), heating is stirred to obtained system, until yellow
Cotton-shaped graphene oxide becomes black suspension in solution, is filtered with 0.35 μm of filter wash after cooling, and filter cake is cold
Dry 48h is lyophilized to get to graphene.
The preparation method for the graphene that 3. purity as described in claim 1 is high, performance is stablized, it is characterised in that：1) to
70 parts of 8 parts of potassium hydroxide of addition of expanded graphite, are placed in ultrasonic disperse machine, ultrasonic power 750, graphene oxide are formed after 2h
Suspension；
2) 14 parts of threonine, 3 parts of dioxanes, 5 parts of diethyl hydroxylamine, vinyl will be added in the graphene suspension in step 1)
13 parts of bis-stearamides, 5 parts of N-METHYLFORMAMIDE, 21 parts of tetramethyl ammonium hydrogen carbonate, are placed in a centrifuge, centrifugation rate is
3200r/min, time 20min, temperature are maintained at 25 DEG C, obtain graphene oxide colloidal solution；
3) it by 25 parts of 18 parts of the concentrated sulfuric acid, concentrated nitric acid mixing, is placed in blender, stir speed (S.S.) 300r/min, time 1h, temperature
Degree is maintained at 30 DEG C, obtains mixed liquor；
4) it will be added in the mixed liquor in step 3) in the graphene colloidal solution in step 2), by the effect of dryer,
By moisture evaporation, graphene oxide colloid is obtained；
5) by 3 parts of 1- butyl -3- methylimidazole bis-trifluoromethylsulfoandimides salt, 0.3 part of octafluoro toluene, 7 parts of calcium hypochlorite, naphthalene four
16 parts of formic acid dianhydride is added in centrifuge, centrifugation rate 2000r/min, centrifugation time 30min, and temperature is maintained at 75
DEG C, obtain mixed liquor；
6) mixed liquor of step 5) is added in the graphene colloid of step 4), is filtered after being heated to 90 DEG C, it is cooling, it obtains
To graphene oxide；
7) 5 parts of hydrazine hydrate will be added in the graphene oxide in step 6), heating is stirred to obtained system, until yellow
Cotton-shaped graphene oxide becomes black suspension in solution, is filtered with 0.35 μm of filter wash after cooling, and filter cake is cold
Dry 48h is lyophilized to get to graphene.
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| CN103861472A (en) * | 2014-03-28 | 2014-06-18 | 东华大学 | Preparation method of amino-modified graphene oxide composite positive permeable film |
| WO2016045035A1 (en) * | 2014-09-25 | 2016-03-31 | 深圳粤网节能技术服务有限公司 | Method for preparing graphene |
| CN104891482A (en) * | 2015-06-03 | 2015-09-09 | 盐城纳新天地新材料科技有限公司 | Method for preparing graphene oxide in alkaline water phase |
| CN105601914A (en) * | 2015-12-29 | 2016-05-25 | 上海第二工业大学 | Preparing method of ionic liquid functionalized graphene/conductive polyaniline nanowire composition material |
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