CN106744895A - A kind of preparation method of high-purity multi-layer graphene - Google Patents
A kind of preparation method of high-purity multi-layer graphene Download PDFInfo
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- CN106744895A CN106744895A CN201611235101.2A CN201611235101A CN106744895A CN 106744895 A CN106744895 A CN 106744895A CN 201611235101 A CN201611235101 A CN 201611235101A CN 106744895 A CN106744895 A CN 106744895A
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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
- C01B2204/04—Specific amount of layers or specific thickness
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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
- C01B2204/30—Purity
Abstract
The invention discloses a kind of preparation method of high-purity multi-layer graphene; including smashing, shaping, cutting, liquid oxidation, solid oxidation, ultrasonically treated, reduction, purifying preparation process; it is raw material that the present invention uses high-purity compact crystal shape graphite; solid oxidizer is respectively adopted and liquid oxidizer is aoxidized twice; peel off graphite abundant; by a series of preparation method; finally give purity multi-layer graphene high; the present invention is easy to operate; production equipment is few; it is with low cost, it is easy to utilize, it is suitable to large-scale production.
Description
Technical field
The invention belongs to carbon material technical field, a kind of preparation method of high-purity multi-layer graphene is specifically related to.
Background technology
Graphene is the receiving with hexagonal lattice alveolate texture bonded together to form with sp2 hybrid forms by single layer of carbon atom
Rice carbon material, belongs to a kind of new two dimensional crystal material.Graphene have good electric conductivity, thermal conductivity, mechanical performance, thoroughly
Photosensitiveness and electronics property, are with a wide range of applications in energy stores, opto-electronic device and field of compound material.Therefore,
Graphene has become the study hotspot of the multiple ambit such as materialogy, physics and chemistry at present.In terms of industrialization, by
In the development of various technologies of preparing, the exploitation of graphene product also achieves significantly be in progress in recent years.
The preparation method of graphene product is various, mainly including micromechanics stripping method, epitaxial growth method, chemical gaseous phase deposition
CVD and graphite oxide reducing process, micromechanics stripping means controllability are poor, and obtained Graphene size is smaller and exists very big
Uncertainty；Epitaxial growth method high energy consumption, device therefor needs to keep ultrahigh vacuum at high temperature, and this is the design system of equipment
Make and bring great difficulty；Chemical gaseous phase deposition CVD is in the preparation later stage, and the transfer process for Graphene is more complicated,
And preparation cost is higher；Graphite oxide reducing process is also considered as preparing one of best approach of Graphene at present, the method
Simple to operate, preparation cost is low, can on a large scale prepare Graphene, it has also become effective way prepared by Graphene.But
In the presence of some drawbacks, product quality and purity than relatively low, therefore, a kind of graphene preparation method of high-purity is explored, to reality
The extensive use of existing Graphene has highly important value.
The content of the invention
For above-mentioned existing technologies problem, the invention discloses a kind of preparation method of high-purity multi-layer graphene, have
It is easy to operate, the features such as product purity is high.
Mesh of the present invention solves the technical scheme that above-mentioned technical problem taken：A kind of preparation of high-purity multi-layer graphene
Method, comprises the following steps：
(1) crush：It is raw material to use compact crystal shape graphite, compact crystal shape graphite is placed in pulverizer and is crushed, mistake
200-300 eye mesh screens, obtain powdered graphite；
(2) it is molded：Powdered graphite is processed using individual layer flat board continuous rolled-on method, first by powdered graphite load to
It is uniform to trickle down on the conveyor belt in material device, rolled using pressure roll, the graphite bed of material is formed, the graphite bed of material is heated, finally
By in the roller of the graphite bed of material feeding control thickness of first one-step forming, pressed again once by required thickness, to obtain thickness
Uniform graphite cake；
(3) cut：Graphite cake is cut with graphite cutting machine, the graphite flake of required size is cut into；
(4) liquid oxidation：Graphite flake, liquid oxidizer are well mixed, are placed in closed reaction vessel, it is anti-in frozen water
After answering 1-4h, stirring reaction 0.5-2h under normal temperature obtains the first suspension, and the first suspension is washed with deionized into suction filtration extremely
Neutrality, is placed in baking oven and dries, and obtains dry product；
(5) solid oxidation：Dry product, solid oxidizer, solvent are well mixed, are added to magnetic stirrer
Closed container in, be placed on magnetic stirring apparatus, be warming up to 30-70 DEG C stirring mixing 2-4h, the second suspension is obtained, by second
Suspension is washed with deionized suction filtration to neutrality, is placed in baking oven and dries, and obtains graphite oxide；
(6) it is ultrasonically treated：Graphite oxide is placed in supersonic wave cleaning machine, carries out ultrasonically treated, obtain graphene oxide；
(7) reduce：Graphene oxide, reducing agent, solvent are well mixed, the closed appearance with magnetic stirrer is added to
In device, it is placed on magnetic stirring apparatus, is warming up to 40-60 DEG C of stirring mixing 2-5h, obtains the 3rd suspension；
(8) purify：By the 3rd suspension suction filtration, cleaned with ethanol after suction filtration, centrifugal sedimentation 3 times, by precipitum spend from
Finally be placed in precipitum in baking oven and dried by sub- water washing, centrifugal sedimentation 3 times with ethanol centrifugal sedimentation 3 times again, obtains multilayer
Graphene.
The phosphorus content of compact crystal shape graphite described in step (1) is 90%~95%.
Heat time described in step (2) is 4-8h, and heating-up temperature is 200-600 DEG C；
Graphite plate thickness described in step (2) is 0.2-0.8mm.
Graphite flake described in step (3) is square, and length is 0.5-1cm.
Drying temperature is 40-80 DEG C in step (4), described in step (5), and the time is 2-4h, is dried described in step (8)
Temperature is 40-80 DEG C, and the time is 12-18h.
Liquid oxidizer described in step (4) is the concentrated sulfuric acid, hydrogen peroxide, wherein the weight ratio of the concentrated sulfuric acid, hydrogen peroxide
It is 1~3:1, liquid oxidizer is 15~20 with the weight ratio of graphite flake:1.
Solid oxidizer described in step (5) be potassium permanganate, solvent is deionized water, wherein solid oxidizer, solvent,
The weight ratio of dry product is 5:100~400:1.
Reducing agent described in step (7) is sodium hydrogensulfite, and solvent is deionized water, wherein reducing agent, solvent, oxidation stone
The weight ratio of black alkene is 5：100-200：1.
Ethanol centrifugal sedimentation condition is described in step (8)：4000~7000r/min of rotating speed, time 4-7min, deionization
Water centrifugal sedimentation condition is：Rotating speed 3000-4000r/min, time 5-9min.
The present invention has beneficial effect：It is raw material that the present invention uses high-purity compact crystal shape graphite, and solid is respectively adopted
Oxidant and liquid oxidizer are aoxidized twice, peel off graphite abundant, by a series of preparation method, finally give purity high
Multi-layer graphene, the present invention it is easy to operate, production equipment is few, with low cost, easy to utilize, is suitable to large-scale production.
Specific embodiment
With reference to specific embodiment, the present invention is described further：
Embodiment 1
(1) crush：It is raw material to use compact crystal shape graphite, compact crystal shape graphite is placed in pulverizer and is crushed, mistake
200 eye mesh screens, obtain powdered graphite；
(2) it is molded：Powdered graphite is processed using individual layer flat board continuous rolled-on method, first by powdered graphite load to
It is uniform to trickle down on the conveyor belt in material device, rolled using pressure roll, the graphite bed of material is formed, heat the graphite bed of material, heating
Temperature is 200 DEG C, and the heat time is 8h, finally by the roller of the graphite bed of material feeding control thickness of first one-step forming, is pressed
Required thickness is pressed once again, obtains the graphite cake that thickness is 0.8mm；
(3) cut：Graphite cake is cut with graphite cutting machine, the square graphite flake that length is 1cm is cut into；
(4) liquid oxidation：By graphite flake, the concentrated sulfuric acid, hydrogen peroxide is by weight 1:10:10 are well mixed, and are placed in closed
In reaction vessel, after reacting 1h in frozen water, stirring reaction 2h under normal temperature obtains the first suspension, and the first suspension is spent
Ion water washing suction filtration is placed in baking oven and dries to neutrality, and drying temperature is 40 DEG C, and the time is 4h, obtains dry product；
(5) solid oxidation：By dry product, potassium permanganate, deionized water by weight 1:5:160 are well mixed, plus
Enter in the closed container with magnetic stirrer, be placed on magnetic stirring apparatus, be warming up to 30 DEG C of stirring mixing 2h, obtain second
Suspension, suction filtration to neutrality is washed with deionized by the second suspension, is placed in baking oven and is dried, and drying temperature is 40 DEG C, when
Between be 4h, obtain graphite oxide；
(6) it is ultrasonically treated：Graphite oxide is placed in supersonic wave cleaning machine, carries out ultrasonically treated, obtain graphene oxide；
(7) reduce：By graphene oxide, sodium hydrogensulfite, deionized water by weight 1:5:100 are well mixed, and add
To in the closed container with magnetic stirrer, it is placed on magnetic stirring apparatus, is warming up to 40 DEG C of stirring mixing 5h, obtains the 3rd and hang
Turbid liquid；
(8) purify：By the 3rd suspension suction filtration, cleaned with ethanol after suction filtration, centrifugal sedimentation 3 times, centrifuge speed
4000r/min, centrifugation time 7min, precipitum is washed with deionized, centrifugal sedimentation 3 times, centrifuge speed 4000r/
Min, centrifugation time 5min, finally use ethanol centrifugal sedimentation 3 times again, centrifuge speed 4000r/min, centrifugation time 7min will
Precipitum is placed in baking oven and dries, and drying temperature is 50 DEG C, and the time is 12h, obtains multi-layer graphene.
Embodiment 2
(1) crush：It is raw material to use compact crystal shape graphite, compact crystal shape graphite is placed in pulverizer and is crushed, mistake
250 eye mesh screens, obtain powdered graphite；
(2) it is molded：Powdered graphite is processed using individual layer flat board continuous rolled-on method, first by powdered graphite load to
It is uniform to trickle down on the conveyor belt in material device, rolled using pressure roll, the graphite bed of material is formed, heat the graphite bed of material, heating
Temperature is 400 DEG C, and the heat time is 5h, finally by the roller of the graphite bed of material feeding control thickness of first one-step forming, is pressed
Required thickness presses the graphite cake for once obtaining that thickness is 0.6mm again；
(3) cut：Graphite cake is cut with graphite cutting machine, the square graphite flake that length is 1cm is cut into；
(4) liquid oxidation：By graphite flake, the concentrated sulfuric acid, hydrogen peroxide is by weight 1:9:9 well mixed are placed in confined reaction
In container, in frozen water react 4h after, stirring reaction 0.5h under normal temperature obtains the first suspension, by the first suspension spend from
Sub- water washing suction filtration is placed in baking oven and dries to neutrality, and drying temperature is 60 DEG C, and the time is 3h, obtains dry product；
(5) solid oxidation：By dry product, potassium permanganate, deionized water by weight 1:5:200 are well mixed, plus
Enter in the closed container with magnetic stirrer, be placed on magnetic stirring apparatus, be warming up to 70 DEG C of stirring mixing 2h, obtain second
Suspension, suction filtration to neutrality is washed with deionized by the second suspension, is placed in baking oven and is dried, and drying temperature is 40 DEG C, when
Between be 4h, obtain graphite oxide；
(6) it is ultrasonically treated：Graphite oxide is placed in supersonic wave cleaning machine, carries out ultrasonically treated, obtain graphene oxide；
(7) reduce：Just graphene oxide, sodium hydrogensulfite, deionized water are by weight 1:5:150 are well mixed, plus
Enter in the closed container with magnetic stirrer, be placed on magnetic stirring apparatus, be warming up to 60 DEG C of stirring mixing 2h, obtain the 3rd
Suspension；
(8) purify：By the 3rd suspension suction filtration, cleaned with ethanol after suction filtration, centrifugal sedimentation 3 times, centrifuge speed
5000r/min, centrifugation time 5min, precipitum is washed with deionized, centrifugal sedimentation 3 times, centrifuge speed 4000r/
Min, centrifugation time 8min, finally use ethanol centrifugal sedimentation 3 times again, and centrifuge speed 5000r/min, centrifugation time 5min will
Precipitum is placed in baking oven and dries, and drying temperature is 80 DEG C, and the time is 12h, obtains multi-layer graphene.
Embodiment 3
(1) crush：It is raw material to use compact crystal shape graphite, compact crystal shape graphite is placed in pulverizer and is crushed, mistake
300 eye mesh screens, obtain powdered graphite；
(2) it is molded：Powdered graphite is processed using individual layer flat board continuous rolled-on method, first by powdered graphite load to
It is uniform to trickle down on the conveyor belt in material device, rolled using pressure roll, the graphite bed of material is formed, heat the graphite bed of material, heating
Temperature is 600 DEG C, and the heat time is 4h, finally by the roller of the graphite bed of material feeding control thickness of first one-step forming, is pressed
Required thickness is pressed once again, obtains the graphite cake that thickness is 0.7mm；
(3) cut：Graphite cake is cut with graphite cutting machine, the square graphite flake that length is 1cm is cut into；
(4) liquid oxidation：By graphite flake, the concentrated sulfuric acid, hydrogen peroxide is by weight 1:15:5 are well mixed, and are placed in closed anti-
In answering container, after reacting 3h in frozen water, stirring reaction 2h under normal temperature obtains the first suspension, by the first suspension spend from
Sub- water washing suction filtration is placed in baking oven and dries to neutrality, and drying temperature is 60 DEG C, and the time is 4h, obtains dry product；
(5) solid oxidation：By dry product, potassium permanganate, deionized water by weight 1:5:400 are well mixed, plus
Enter in the closed container with magnetic stirrer, be placed on magnetic stirring apparatus, be warming up to 50 DEG C of stirring mixing 3h, obtain second
Suspension, suction filtration to neutrality is washed with deionized by the second suspension, is placed in baking oven and is dried, and drying temperature is 60 DEG C, when
Between be 4h, obtain graphite oxide；
(6) it is ultrasonically treated：Graphite oxide is placed in supersonic wave cleaning machine, carries out ultrasonically treated, obtain graphene oxide；
(7) reduce：Just graphene oxide, sodium hydrogensulfite, deionized water are by weight 1:5:200 are well mixed, plus
Enter in the closed container with magnetic stirrer, be placed on magnetic stirring apparatus, be warming up to 50 DEG C of stirring mixing 5h, obtain the 3rd
Suspension；
(8) purify：By the 3rd suspension suction filtration, cleaned with ethanol after suction filtration, centrifugal sedimentation 3 times, centrifuge speed
4000r/min, centrifugation time 6min, precipitum is washed with deionized, centrifugal sedimentation 3 times, centrifuge speed 3000r/
Min, centrifugation time 7min, finally use ethanol centrifugal sedimentation 3 times again, and centrifuge speed 4000r/min, centrifugation time 6min will
Precipitum is placed in baking oven and dries, and drying temperature is 60 DEG C, and the time is 14h, obtains multi-layer graphene.
Preferred embodiments of the invention are the foregoing is only, is not intended to limit the invention, it is all in spirit of the invention
With any modification, equivalent and the improvement made within principle etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of high-purity multi-layer graphene, it is characterised in that comprise the following steps：
(1) crush：It is raw material to use compact crystal shape graphite, compact crystal shape graphite is placed in pulverizer and is crushed, and crosses 200-
300 eye mesh screens, obtain powdered graphite；
(2) it is molded：Powdered graphite is processed using individual layer flat board continuous rolled-on method, powdered graphite is loaded into feed dress first
It is uniform to trickle down on the conveyor belt in putting, rolled using pressure roll, the graphite bed of material is formed, the graphite bed of material is heated, finally will be just
In the roller of the graphite bed of material feeding control thickness of one-step forming, pressed again once by required thickness, it is uniform to obtain thickness
Graphite cake；
(3) cut：Graphite cake is cut with graphite cutting machine, the graphite flake of required size is cut into；
(4) liquid oxidation：Graphite flake, liquid oxidizer are well mixed, are placed in closed reaction vessel, 1- is reacted in frozen water
After 4h, stirring reaction 0.5-2h under normal temperature obtains the first suspension, and the first suspension is washed with deionized into suction filtration into
Property, it is placed in baking oven and dries, obtain dry product；
(5) solid oxidation：Dry product, solid oxidizer, solvent are well mixed, are added to the close of magnetic stirrer
Close in container, be placed on magnetic stirring apparatus, be warming up to 30-70 DEG C of stirring mixing 2-4h, obtain the second suspension, it is suspended by second
Liquid is washed with deionized suction filtration to neutrality, is placed in baking oven and dries, and obtains graphite oxide；
(6) it is ultrasonically treated：Graphite oxide is placed in supersonic wave cleaning machine, carries out ultrasonically treated, obtain graphene oxide；
(7) reduce：Graphene oxide, reducing agent, solvent are well mixed, the closed container with magnetic stirrer is added to
In, it is placed on magnetic stirring apparatus, 40-60 DEG C of stirring mixing 2-5h is warming up to, obtain the 3rd suspension；
(8) purify：By the 3rd suspension suction filtration, cleaned with ethanol after suction filtration, centrifugal sedimentation 3 times, by precipitum deionized water
Finally be placed in precipitum in baking oven and dried by washing, centrifugal sedimentation 3 times with ethanol centrifugal sedimentation 3 times again, obtains Multi-layer graphite
Alkene.
2. a kind of preparation method of high-purity multi-layer graphene as claimed in claim 1, it is characterised in that institute in step (1)
The phosphorus content for stating compact crystal shape graphite is 90%~95%.
3. a kind of preparation method of high-purity multi-layer graphene as claimed in claim 1, it is characterised in that institute in step (2)
The heat time stated is 4-8h, and heating-up temperature is 200-600 DEG C.
4. a kind of preparation method of high-purity multi-layer graphene as claimed in claim 1, it is characterised in that institute in step (2)
The graphite plate thickness stated is 0.2-0.8mm.
5. a kind of preparation method of high-purity multi-layer graphene as claimed in claim 1, it is characterised in that institute in step (3)
It is square to state graphite flake, and length is 0.5-1cm.
6. a kind of preparation method of high-purity multi-layer graphene as claimed in claim 1, it is characterised in that in step (4), step
Suddenly drying temperature described in (5) is 40-80 DEG C, and the time is 2-4h, and drying temperature described in step (8) is 40-80 DEG C, and the time is
12-18h。
7. a kind of preparation method of high-purity multi-layer graphene as claimed in claim 1, it is characterised in that institute in step (4)
Liquid oxidizer is stated for the concentrated sulfuric acid, hydrogen peroxide, wherein the concentrated sulfuric acid, the weight ratio of hydrogen peroxide are 1~3:1, liquid oxidizer
It is 15~20 with the weight ratio of graphite flake:1.
8. a kind of preparation method of high-purity multi-layer graphene as claimed in claim 1, it is characterised in that institute in step (5)
Solid oxidizer is stated for potassium permanganate, solvent is deionized water, wherein the weight ratio of solid oxidizer, solvent, dry product
It is 5:100~400:1.
9. a kind of preparation method of high-purity multi-layer graphene as claimed in claim 1, it is characterised in that institute in step (7)
Reducing agent is stated for sodium hydrogensulfite, solvent is deionized water, wherein reducing agent, solvent, the weight ratio of graphene oxide are 5：
100-200：1.
10. a kind of preparation method of high-purity multi-layer graphene as claimed in claim 1, it is characterised in that institute in step (8)
Stating ethanol centrifugal sedimentation condition is：4000~7000r/min of rotating speed, time 4-7min, deionized water centrifugal sedimentation condition is：Turn
Fast 3000-4000r/min, time 5-9min.
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2016
- 2016-12-28 CN CN201611235101.2A patent/CN106744895A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102088819A (en) * | 2009-12-07 | 2011-06-08 | 耿世达 | Novel electronic circuit substrate and manufacturing process thereof |
| CN102167314A (en) * | 2011-05-23 | 2011-08-31 | 浙江大学 | Method for preparing graphene |
| CN105645384A (en) * | 2014-12-02 | 2016-06-08 | 中国科学院过程工程研究所 | Preparation method of graphene |
| CN105752977A (en) * | 2016-04-29 | 2016-07-13 | 江苏超电新能源科技发展有限公司 | Preparation method of high-conductivity graphene powder |
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