CN108821270A - A kind of environmentally protective graphene preparation method - Google Patents
A kind of environmentally protective graphene preparation method Download PDFInfo
- Publication number
- CN108821270A CN108821270A CN201811134223.1A CN201811134223A CN108821270A CN 108821270 A CN108821270 A CN 108821270A CN 201811134223 A CN201811134223 A CN 201811134223A CN 108821270 A CN108821270 A CN 108821270A
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- Prior art keywords
- graphene
- graphite
- environmentally protective
- aggregation
- mass ratio
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000001681 protective effect Effects 0.000 title claims abstract description 7
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 24
- 239000010439 graphite Substances 0.000 claims abstract description 24
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000002776 aggregation Effects 0.000 claims abstract description 8
- 238000004220 aggregation Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims abstract description 6
- 229910052786 argon Inorganic materials 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 239000011261 inert gas Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000138 intercalating agent Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 abstract description 17
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 description 8
- 230000002687 intercalation Effects 0.000 description 7
- 238000009830 intercalation Methods 0.000 description 7
- 239000010410 layer Substances 0.000 description 5
- 230000005284 excitation Effects 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 238000005411 Van der Waals force Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 208000018380 Chemical injury Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000004177 carbon cycle Methods 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000013500 performance material Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
Abstract
The invention discloses a kind of preparation methods of graphene, belong to field of new materials.This method is characterized in that：3% hydrogen peroxide and hexamethylene reagent for using certain mass ratio are as intercalator；Under argon gas or other inert gas shieldings, intercalated graphite certain time is motivated using plasma device, obtains the aggregation of expanded graphite and graphene；Aggregation is mixed with deionized water according to certain mass ratio, adjusting pH value to neutrality, and ultrasonic disperse is for a period of time, it is then dry to obtain graphene.The present invention uses plasma producing apparatus as energy source, and plasma can quickly transmit energy, and heating rate is up to 100 DEG C/s.Compared with existing graphene preparation technology, the present invention has the characteristics that environmentally protective, at low cost, easy to operate.
Description
Technical field
The invention belongs to new material technology field, in particular to a kind of preparation method of graphene.
Background technique
The bi-dimensional cellular structural plan crystal that graphene is made of carbon atom is a kind of carbon nanometer material haveing excellent performance
Material, in multiple fields such as supercapacitor, sea water desalination, solar batteries, there are huge application prospects.
British scientist Andre Geim and Russian scientist Konstantin Novoselov was in discovery stone in 2004
After black alkene, the preparation method of graphene emerges one after another, main method have micromechanics stripping method, oxidation-reduction method, liquid phase stripping method,
CVD method etc..Micromechanics stripping method yield is few in the above method, poor controllability is unsuitable is mass produced；Liquid phase stripping method needs
Ultrasonic some time, yield are relatively low, and the later period is also comparatively laborious for the removal of the surfactant on graphene, resulting stone
The size of black alkene is also smaller (general≤5 μm)；CVD method technique is cumbersome, equipment is expensive, energy consumption is high and reaction condition is wanted
Ask harsh, at present large-scale production difficult to realize.Oxidation-reduction method is to prepare one of most common method of graphene, this method
The problem is that control reducing degree, purifying products, most importantly problem of environmental pollution, this promotes green hair with China
Exhibition, the policy for establishing the economic system of low-carbon cycle development are opposite.Currently, lacking the preparation of a kind of low-carbon green and simple process
Method.
Therefore, the non-oxide reduction preparation of graphene is a kind of urgent green technology yet-to-be developed, is also become domestic and international
Study a big hot spot of graphene preparation.
Summary of the invention
The present invention provides a kind of environmentally protective method for preparing graphene for the deficiency in the prior art.This side
Method is characterized in that：
(1) 3% hydrogen peroxide and hexamethylene for using certain mass ratio are as intercalator.
(2) under argon gas or other inert gas shieldings, intercalated graphite certain time is motivated using plasma device, is obtained
To the aggregation of expanded graphite and graphene.
(3) aggregation is mixed with deionized water according to certain mass ratio, adjusting pH value to neutrality, and one section of ultrasonic disperse
It is time, then dry to obtain graphene.
Main thought is solvent to be inserted into graphite layers with physical method, then make solvent that phase occur by outside energy excitation
Become, generate bulk gas, Van der Waals force removes graphite in turn between destroying graphite using the pressure that the gas of interlayer generates, and generates stone
Black alkene.Graphite layers Van der Waals force is 2.5MPa, and theoretically the pressure of graphite layers produce anger body is greater than this numerical value energy
Graphite is removed.In addition graphite layers object needs heated fast, and when heating rate is less than 1 DEG C/min, cracking reaction rate is low,
Gas can be overflowed from interlayer, and as 5 DEG C/min of heating rate >, cracked gas generates rate and is higher than gas from interlayer spilling speed
Rate, removing can occur, so the present invention selects plasma to motivate as external energy, plasma device can fast quick-release
Exoergic amount, heating rate is up to 100 DEG C/s.When solvent intercalation, the structure and size of graphite will affect intercalation depth, some experiment tables
Bright, the graphite number of plies and size are smaller, intercalation resistance with regard to smaller, so the preferred graphite of the present invention be 325 mesh and its more than
Expanded graphite.
Detailed description of the invention
Fig. 1 is graphene scanning electron microscope (SEM) photograph prepared by the present invention.
Specific embodiment
The present invention provides a kind of preparation method of graphene, includes the following steps：：
(1) graphite, 3% hydrogen peroxide, hexamethylene are 1 according to mass ratio：3：1 ratio is prepared, by 2.5 mass parts 325
Purpose expanded graphite, 7.5 mass parts, 3% hydrogen peroxide and 2.5 mass parts hexamethylenes are put into beaker and mix, and stir evenly.Its
What middle hydrogen peroxide played the role of is pre-oxidation, and hexamethylene introduces graphite layers as main solvent molecule.
(2) mixture of step (1) is stood into 48h, infiltrates the intercalation depth and intercalation for guaranteeing solvent for a long time
Then mass fraction is filtered by sintered filter funnel, leaves solid portion.
(3) under argon gas or other inert gas shieldings, solid 120s is motivated using plasma device, is filled in plasma
Under the excitation set, solid can be rapidly heated and then expand, and be cooled to room temperature, and obtain the aggregation of expanded graphite and graphene
Body.
(4) by aggregation and deionized water according to 1：5 mass ratio mixing, adjusts pH value to neutrality, pH value influences whether
Coherent condition of its graphene in dispersion liquid should carry out the adjusting of pH, then ultrasonic disperse in order to avoid this soft-agglomerated
1h is dry to obtain graphene.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
The present invention has the following advantages that compared with original technology：
1, intercalation directly is carried out to expanded graphite with solvent, recycles plasma excitation solvent to undergo phase transition later, benefit
Interlayer power, which is destroyed, with the gas pressure that phase transformation generates completes removing, it is easy to operate.
2, strong oxidizer and strong acid are not used, reduces the pollution to environment, while also avoiding toxic and corrosive
Injury of the reagent to operator.
3, plasma excitation can quickly heat up, and heating rate is up to 100 DEG C/s.
4, the intercalation of solvent can be controlled by the time, it can be ensured that the number of plies distribution of graphene concentrates on certain fixation
The number of plies.
Claims (3)
1. a kind of environmentally protective graphene preparation method, it is characterised in that：Including
(1) use 3% hydrogen peroxide and hexamethylene according to certain mass ratio as intercalator；
(2) under argon gas or other inert gas shieldings, intercalated graphite certain time is motivated using plasma device, is obtained swollen
The aggregation of swollen graphite and graphene；
(3) aggregation is mixed with deionized water according to certain mass ratio, adjusts pH value to neutrality, and at one section of ultrasonic disperse
Between, it is then dry to obtain graphene.
2. environmentally protective graphene preparation method according to claim 1, it is characterised in that：The plasma device
Can quick release of energy, heating rate is up to 100 DEG C/s.
3. environmentally protective graphene preparation method according to claim 1, it is characterised in that：The graphite is 325 mesh
And its above expanded graphite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811134223.1A CN108821270A (en) | 2018-09-27 | 2018-09-27 | A kind of environmentally protective graphene preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811134223.1A CN108821270A (en) | 2018-09-27 | 2018-09-27 | A kind of environmentally protective graphene preparation method |
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| Publication Number | Publication Date |
|---|---|
| CN108821270A true CN108821270A (en) | 2018-11-16 |
Family
ID=64149885
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811134223.1A Pending CN108821270A (en) | 2018-09-27 | 2018-09-27 | A kind of environmentally protective graphene preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108821270A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102431999A (en) * | 2011-09-22 | 2012-05-02 | 中国科学院金属研究所 | Method for preparing high-quality graphene |
| CN103359713A (en) * | 2012-03-31 | 2013-10-23 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
-
2018
- 2018-09-27 CN CN201811134223.1A patent/CN108821270A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102431999A (en) * | 2011-09-22 | 2012-05-02 | 中国科学院金属研究所 | Method for preparing high-quality graphene |
| CN103359713A (en) * | 2012-03-31 | 2013-10-23 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
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