CN107364855A - A kind of preparation technology for improving graphene purity - Google Patents
A kind of preparation technology for improving graphene purity Download PDFInfo
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- CN107364855A CN107364855A CN201710799206.9A CN201710799206A CN107364855A CN 107364855 A CN107364855 A CN 107364855A CN 201710799206 A CN201710799206 A CN 201710799206A CN 107364855 A CN107364855 A CN 107364855A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- 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 technology for improving graphene purity, comprise the following steps：（1）Metallic catalyst, metal agent for capturing and carbon materials, glucan, vinyl acetate maleic anhydride multipolymer, starch acrylonitrile graft copolymer, cellulose graft acrylonitrile hydrolysis product are stirred, adsorbed, obtain being adsorbed with the carbon source mixture of metallic catalyst；（2）Reducing agent is heated with being adsorbed with after the carbon source mixture of metallic catalyst mixes, obtains graphene first product；（3）Grinding；（4）Graphene first product and magnetic draw point abrasive body are put into closed grinding container, grinding container is inserted in conversion magnetic field space, peeled off；（5）Draw point is separated, after settling, centrifuging, the graphene transperent suspension liquid of high-purity is made.Preparation technology of the present invention is simple, and graphene purity is high, and yield is high, pollution-free.
Description
Technical field
The present invention relates to carbon material technical field, more particularly to a kind of preparation technology for improving graphene purity.
Background technology
Graphene (Graphene) is the only one layer of atomic thickness for being stripped out from graphite material, being made up of carbon atom
Two dimensional crystal.2004, Univ Manchester UK physicist An Deliegaimu and Constantine's Nuo Woxiao loves,
Graphene is isolated in success from graphite, it was demonstrated that therefore it can also obtain Nobel's thing in 2010 jointly with individualism, two people
Neo-Confucianism prize.Graphene is both most thin material, and most tough material, 200 times more taller than best steel of fracture strength.
It has good elasticity again simultaneously, and stretch range can reach the 20% of own dimensions.It is that current nature is most thin, intensity highest
Material, if making hammock with the graphene of one piece of 1 square metre of area, weight itself can be to bear one less than 1 milligram
One kilogram of cat.Graphene most potential application at present is the substitute as silicon, ultra micro transistor npn npn is manufactured, for producing
Following supercomputer.Substitute silicon with graphene, the speed of service of computer processor will be fast hundreds times.In addition, graphite
Alkene is almost fully transparent, only absorbs 2.3% light.On the other hand, it is very fine and close, even minimum gas atom (helium
Atom) it can not also penetrate.These features cause it to be highly suitable as the raw material of transparent electron product, and such as transparent touch is shown
Screen, luminescent screen and solar panel.
A kind of novel nano-material most strong as the most thin, maximum intensity, electrical and thermal conductivity performance that have now been found that, graphene
It is referred to as " dark fund ", is " king of new material ", scientist even foretells that graphene " will thoroughly change 21 century ".Very likely lift
Play a subversiveness new technology new industrial revolution have swept the globe.
At present, grapheme material powder can be prepared using a variety of methods, as mechanical stripping method, oxidation-reducing process,
Crystal epitaxy method, chemical vapour deposition technique, organic synthesis method and stripping CNT method etc..In these methods, it is mechanical
Stripping method and epitaxial growth method preparation efficiency are very low, it is difficult to meet large-scale needs.Although chemical vapour deposition technique can obtain
The continuous graphene film of large scale is obtained, but is applied to micro-nano electronic device or transparent conductive film, can not but meet energy storage material
Material and the extensive demand in functional composite material field.Oxidation-reducing process prepares grapheme material powder and is relatively easy to realize,
It is the common method for preparing grapheme material powder, but this method uses a large amount of strong acid and oxygen during graphene is prepared
Agent, graphenic surface is destroyed seriously, and easily pollute environment, therefore be not suitable for the graphene system of extensive industrialization
It is standby.
On the basis of micromechanics stripping method, the grinding for being attempted to be carried out graphene with traditional ball grinding method is prepared greatly
Amount, the graphene or graphene oxide, Antisar M.V et al. of small area have carried out wet ball grinding in water, have obtained thickness
More than 10nm graphite nano-sheets.In order to improve graphene charge stripping efficiency, people are aided in using substantial amounts of minute solid particles
Stripping process, to increase stripping process contact area and peel off number, but the removal of fine particle and liquid exists with separating
Bigger difficulty.
The invention provides a kind of preparation technology for improving graphene purity.
The content of the invention
The technical problems to be solved by the invention are：Provide a kind of preparation technology for improving graphene purity.
In order to solve the above technical problems, the invention provides a kind of preparation technology for improving graphene purity, it is including following
Step：
（1）By metallic catalyst, metal agent for capturing and carbon materials, glucan, vinyl acetate-maleic anhydride multipolymer,
Starch acrylonitrile graft copolymer, cellulose graft acrylonitrile hydrolysis product are stirred, and are adsorbed, obtain being adsorbed with metal
The carbon source mixture of catalyst；The metallic catalyst, metal agent for capturing and carbon materials, glucan, vinyl acetate-maleic
Anhydride multipolymer, starch acrylonitrile graft copolymer, the weight part ratio of cellulose graft acrylonitrile hydrolysis product are 1：（0.4-
0.6）：（0.8-1.2）：（0.1-0.3）：（0.5-0.7）：（0.1-0.3）：（0.3-0.5）；
（2）By reducing agent and step（1）In be adsorbed with metallic catalyst carbon source mixture mixing after, be according to heating rate
12-14 DEG C/min is heated to temperature as 950-1050 DEG C, and constant temperature keeps 26-28h, obtains graphene first product；The reducing agent is
Nano-Zinc powder；
（3）By step（2）Obtained graphene first product is ground, and it is 10000 mesh to reach granularity；
（4）By the graphene first product after grinding and magnetic draw point abrasive body, it is put into closed grinding container, grinding container is put
Enter have to EDS maps formed tubular conversion magnetic field space in, carry out stripping 48-58h, after stripping be made graphite nano micro-flake-
The mixture dry powder of graphene；
（5）By step（4）The mixture dry powder separation draw point of obtained graphite nano micro-flake-graphene, by settling, centrifuging point
From rear, the graphene transperent suspension liquid of obtained high-purity.
Further, the metallic catalyst is zinc molybdate.
Further, the metal agent for capturing is diethylene triamine pentamethylene phosphonic.
Further, the step（4）The material of middle grinding container is austenitic stainless steel.
Further, the step（4）The conversion frequency of middle conversion magnetic field space is 2600-2800r/min, and magnetic induction is strong
Spend for 0.8-0.9T.
Further, comprise the following steps：
（1）By metallic catalyst, metal agent for capturing and carbon materials, glucan, vinyl acetate-maleic anhydride multipolymer,
Starch acrylonitrile graft copolymer, cellulose graft acrylonitrile hydrolysis product are stirred, and are adsorbed, obtain being adsorbed with metal
The carbon source mixture of catalyst；The metallic catalyst, metal agent for capturing and carbon materials, glucan, vinyl acetate-maleic
Anhydride multipolymer, starch acrylonitrile graft copolymer, the weight part ratio of cellulose graft acrylonitrile hydrolysis product are 1：0.5：1
：0.2：0.6：0.2：0.4；
（2）By reducing agent and step（1）In be adsorbed with metallic catalyst carbon source mixture mixing after, be according to heating rate
13 DEG C/min is heated to temperature as 1000 DEG C, and constant temperature keeps 27h, obtains graphene first product；The reducing agent is nano zinc powder
End；
（3）By step（2）Obtained graphene first product is ground, and it is 10000 mesh to reach granularity；
（4）By the graphene first product after grinding and magnetic draw point abrasive body, it is put into closed grinding container, grinding container is put
Entering has in the tubular conversion magnetic field space formed to EDS maps, carries out stripping 53h, graphite nano micro-flake-stone is made after stripping
The mixture dry powder of black alkene；
（5）By step（4）The mixture dry powder separation draw point of obtained graphite nano micro-flake-graphene, by settling, centrifuging point
From rear, the graphene transperent suspension liquid of obtained high-purity.
Beneficial effects of the present invention：The present invention provides a kind of preparation technology for improving graphene purity, and preparation technology is simple,
Graphene purity is high, and yield is high, and present invention process is not using environmental pollutions such as strong acid or oxidants
Serious raw material, acted on by ion exchange, chelating, absorption etc., realize uniform graphitization, improve graphitization journey
Degree, meanwhile, using superfine magnetic draw point as abrasive body, caused impact force is minimum each other but collision frequency is very high, enters
One step removes fine particle and liquid, can effectively weaken the destruction of the lattice because of collision and to graphene, is adapted to use just
In the stripping of flaky graphite, graphene purity is improved.
Embodiment
Describe embodiments of the present invention in detail below with reference to embodiment, whereby to the present invention how application technology hand
Section solves technical problem, and the implementation process for reaching technique effect can fully understand and implement according to this.
It should be noted that writing length to save specification, unnecessary repetition and waste are avoided, in the feelings not conflicted
Under condition, the feature in embodiment and embodiment in the application can be mutually combined.
A kind of preparation technology for improving graphene purity, comprises the following steps：
（1）By metallic catalyst, metal agent for capturing and carbon materials, glucan, vinyl acetate-maleic anhydride multipolymer,
Starch acrylonitrile graft copolymer, cellulose graft acrylonitrile hydrolysis product are stirred, and are adsorbed, obtain being adsorbed with metal
The carbon source mixture of catalyst；The metallic catalyst, metal agent for capturing and carbon materials, glucan, vinyl acetate-maleic
Anhydride multipolymer, starch acrylonitrile graft copolymer, the weight part ratio of cellulose graft acrylonitrile hydrolysis product are 1：（0.4-
0.6）：（0.8-1.2）：（0.1-0.3）：（0.5-0.7）：（0.1-0.3）：（0.3-0.5）；
（2）By reducing agent and step（1）In be adsorbed with metallic catalyst carbon source mixture mixing after, be according to heating rate
12-14 DEG C/min is heated to temperature as 950-1050 DEG C, and constant temperature keeps 26-28h, obtains graphene first product；The reducing agent is
Nano-Zinc powder；
（3）By step（2）Obtained graphene first product is ground, and it is 10000 mesh to reach granularity；
（4）By the graphene first product after grinding and magnetic draw point abrasive body, it is put into closed grinding container, grinding container is put
Enter have to EDS maps formed tubular conversion magnetic field space in, carry out stripping 48-58h, after stripping be made graphite nano micro-flake-
The mixture dry powder of graphene；
（5）By step（4）The mixture dry powder separation draw point of obtained graphite nano micro-flake-graphene, by settling, centrifuging point
From rear, the graphene transperent suspension liquid of obtained high-purity.
As the priority scheme of the present invention, the metallic catalyst is zinc molybdate.
As the priority scheme of the present invention, the metal agent for capturing is diethylene triamine pentamethylene phosphonic.
As the priority scheme of the present invention, the step（4）The material of middle grinding container is austenitic stainless steel.
As the priority scheme of the present invention, the step（4）The conversion frequency of middle conversion magnetic field space is 2600-2800r/
Min, magnetic induction intensity 0.8-0.9T.
A kind of preparation technology for improving graphene purity of embodiment 1
A kind of preparation technology for improving graphene purity, comprises the following steps：
（1）By metallic catalyst, metal agent for capturing and carbon materials, glucan, vinyl acetate-maleic anhydride multipolymer,
Starch acrylonitrile graft copolymer, cellulose graft acrylonitrile hydrolysis product are stirred, and are adsorbed, obtain being adsorbed with metal
The carbon source mixture of catalyst；The metallic catalyst, metal agent for capturing and carbon materials, glucan, vinyl acetate-maleic
Anhydride multipolymer, starch acrylonitrile graft copolymer, the weight part ratio of cellulose graft acrylonitrile hydrolysis product are 1：0.5：1
：0.2：0.6：0.2：0.4；
（2）By reducing agent and step（1）In be adsorbed with metallic catalyst carbon source mixture mixing after, be according to heating rate
13 DEG C/min is heated to temperature as 1000 DEG C, and constant temperature keeps 27h, obtains graphene first product；The reducing agent is nano zinc powder
End；
（3）By step（2）Obtained graphene first product is ground, and it is 10000 mesh to reach granularity；
（4）By the graphene first product after grinding and magnetic draw point abrasive body, it is put into closed grinding container, grinding container is put
Entering has in the tubular conversion magnetic field space formed to EDS maps, carries out stripping 53h, graphite nano micro-flake-stone is made after stripping
The mixture dry powder of black alkene；
（5）By step（4）The mixture dry powder separation draw point of obtained graphite nano micro-flake-graphene, by settling, centrifuging point
From rear, the graphene transperent suspension liquid of obtained high-purity.
As the priority scheme of the present invention, the metallic catalyst is zinc molybdate.
As the priority scheme of the present invention, the metal agent for capturing is diethylene triamine pentamethylene phosphonic.
As the priority scheme of the present invention, the step（4）The material of middle grinding container is austenitic stainless steel.
As the priority scheme of the present invention, the step（4）The conversion frequency of middle conversion magnetic field space is 2700r/min,
Magnetic induction intensity is 0.85T.
All above-mentioned this intellectual properties of primarily implementation, the not this new product of implementation of setting limitation other forms
And/or new method.Those skilled in the art will utilize this important information, the above modification, to realize similar execution feelings
Condition.But all modifications or transformation belong to the right of reservation based on new product of the present invention.
Claims (6)
1. a kind of preparation technology for improving graphene purity, it is characterised in that comprise the following steps：
By metallic catalyst, metal agent for capturing and carbon materials, glucan, vinyl acetate-maleic anhydride multipolymer, starch
Acrylonitrile graft copolymer, cellulose graft acrylonitrile hydrolysis product are stirred, and are adsorbed, obtain being adsorbed with metal catalytic
The carbon source mixture of agent；The metallic catalyst, metal agent for capturing and carbon materials, glucan, vinyl acetate-maleic acid
Anhydride copolymer, starch acrylonitrile graft copolymer, the weight part ratio of cellulose graft acrylonitrile hydrolysis product are 1：（0.4-
0.6）：（0.8-1.2）：（0.1-0.3）：（0.5-0.7）：（0.1-0.3）：（0.3-0.5）；
By reducing agent and step（1）In be adsorbed with metallic catalyst carbon source mixture mixing after, be 12- according to heating rate
14 DEG C/min is heated to temperature as 950-1050 DEG C, and constant temperature keeps 26-28h, obtains graphene first product；The reducing agent is to receive
Rice zinc powder；
By step（2）Obtained graphene first product is ground, and it is 10000 mesh to reach granularity；
By the graphene first product after grinding and magnetic draw point abrasive body, it is put into closed grinding container, grinding container is inserted
With in the tubular conversion magnetic field space formed to EDS maps, stripping 48-58h is carried out, graphite nano micro-flake-stone is made after stripping
The mixture dry powder of black alkene；
By step（4）The mixture dry powder separation draw point of obtained graphite nano micro-flake-graphene, by settling, centrifuging
Afterwards, the graphene transperent suspension liquid of high-purity is made.
2. the preparation technology of a kind of raising graphene purity according to right 1, it is characterised in that the metallic catalyst is
Zinc molybdate.
3. the preparation technology of a kind of raising graphene purity according to right 1, it is characterised in that the metal agent for capturing is
Diethylene triamine pentamethylene phosphonic.
A kind of 4. preparation technology of raising graphene purity according to right 1, it is characterised in that the step（4）In grind
The material for grinding container is austenitic stainless steel.
A kind of 5. preparation technology of raising graphene purity according to right 1, it is characterised in that the step（4）Middle change
The conversion frequency for changing magnetic field space is 2600-2800r/min, magnetic induction intensity 0.8-0.9T.
6. the preparation technology of a kind of raising graphene purity according to right 1, it is characterised in that comprise the following steps：
（1）By metallic catalyst, metal agent for capturing and carbon materials, glucan, vinyl acetate-maleic anhydride multipolymer,
Starch acrylonitrile graft copolymer, cellulose graft acrylonitrile hydrolysis product are stirred, and are adsorbed, obtain being adsorbed with metal
The carbon source mixture of catalyst；The metallic catalyst, metal agent for capturing and carbon materials, glucan, vinyl acetate-maleic
Anhydride multipolymer, starch acrylonitrile graft copolymer, the weight part ratio of cellulose graft acrylonitrile hydrolysis product are 1：0.5：1
：0.2：0.6：0.2：0.4；
（2）By reducing agent and step（1）In be adsorbed with metallic catalyst carbon source mixture mixing after, be according to heating rate
13 DEG C/min is heated to temperature as 1000 DEG C, and constant temperature keeps 27h, obtains graphene first product；The reducing agent is nano zinc powder
End；
（3）By step（2）Obtained graphene first product is ground, and it is 10000 mesh to reach granularity；
（4）By the graphene first product after grinding and magnetic draw point abrasive body, it is put into closed grinding container, grinding container is put
Entering has in the tubular conversion magnetic field space formed to EDS maps, carries out stripping 53h, graphite nano micro-flake-stone is made after stripping
The mixture dry powder of black alkene；
By step（4）The mixture dry powder separation draw point of obtained graphite nano micro-flake-graphene, by settling, centrifuging
Afterwards, the graphene transperent suspension liquid of high-purity is made.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103935986A (en) * | 2014-02-28 | 2014-07-23 | 中国科学院宁波材料技术与工程研究所 | Method for high yield preparation of graphene by using biologic carbon source material |
| CN104556001A (en) * | 2014-12-19 | 2015-04-29 | 林前锋 | Method for preparing high-purity graphene |
| CN104876217A (en) * | 2015-06-01 | 2015-09-02 | 北京理工大学 | Graphene preparation method |
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- 2017-09-07 CN CN201710799206.9A patent/CN107364855B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103935986A (en) * | 2014-02-28 | 2014-07-23 | 中国科学院宁波材料技术与工程研究所 | Method for high yield preparation of graphene by using biologic carbon source material |
| CN103935986B (en) * | 2014-02-28 | 2016-03-30 | 中国科学院宁波材料技术与工程研究所 | A kind of method preparing Graphene with biological carbon source material high yield |
| CN104556001A (en) * | 2014-12-19 | 2015-04-29 | 林前锋 | Method for preparing high-purity graphene |
| CN104876217A (en) * | 2015-06-01 | 2015-09-02 | 北京理工大学 | Graphene preparation method |
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Effective date of registration: 20191204 Address after: Room c506a-19, University Business Park, No. 99, University Road, Xuzhou hi tech Industrial Development Zone, 221000, Jiangsu Province Patentee after: Xuzhou Tiancheng Intelligent Technology Co.,Ltd. Address before: 211000 Jiangsu City, Jiangning, Qilin District, science and Technology Innovation Park, Hui Chi Road, unit B, building 300, building two Patentee before: NANJING HANERS BIOTECHNOLOGY Co.,Ltd. |
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Effective date of registration: 20201109 Address after: Room 501000, Changde Industrial Park, Changchun, China Patentee after: Jilin Zhongcheng Energy Technology Co.,Ltd. Address before: Room c506a-19, University Business Park, No. 99, University Road, Xuzhou hi tech Industrial Development Zone, 221000, Jiangsu Province Patentee before: Xuzhou Tiancheng Intelligent Technology Co.,Ltd. |
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