CN107827102A - A kind of method for preparing graphene - Google Patents
A kind of method for preparing graphene Download PDFInfo
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- CN107827102A CN107827102A CN201711202591.0A CN201711202591A CN107827102A CN 107827102 A CN107827102 A CN 107827102A CN 201711202591 A CN201711202591 A CN 201711202591A CN 107827102 A CN107827102 A CN 107827102A
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Abstract
The present invention relates to a kind of preparation method of graphene, and in particular to a kind of method for preparing graphene using high pressure homogenizer liquid phase stripping, including step：(1) by graphite raw material, dispersant and water using mass ratio as 3~150：100~5000：0~10 is configured to graphite slurry；(2) by the graphite slurry prepared in colloid mill grinding distribution, afterwards be sent into material barrel the graphite slurry is cooled down；(3) graphite slurry after cooling is pumped into homogeneous in high pressure homogenizer by barrier film, peels off graphite to form the few layer graphene being evenly distributed through high pressure homogenizer homogeneous；(4) the graphene slurry is continued cycling through several times in high pressure homogenizer；(5) the graphene slurry is filtered after circulating, cleaned with deionized water, is then dried in freeze drier, less than 10 layers of graphene powder is made.The present invention has simple technological process, non-environmental-pollution, is adapted to the advantages of batch production, is that graphene realizes the extraordinary approach of industrialization.
Description
Technical field
The present invention relates to a kind of preparation method of graphene, and in particular to a kind of in a series arrangement that colloid mill is equal with high pressure
Matter machine connects the method that graphene is prepared by liquid phase stripping.
Background technology
Graphene is carbon atom with SP2Hydridization forms the two-dimensional material with cellular hexaplanar structure, mono-layer graphite
Alkene thickness only has 0.335nm, has higher thermal conductivity (up to 5300Wm-1·K-1), higher specific surface area it is (reachable
2630m2·g-1), higher hardness and light transmittance, electron mobility at room temperature be up to 200000cm2·V-1·s-1, and stone
Black alkene material has the characteristics such as soft flexible, the application of graphene and the research and development of new product is enjoyed the concern of people, such as stores up
The fields such as energy material, polymer composite, Aero-Space, biomedicine, electronic material.
The preparation method of graphene can be divided into two classes：That is physical method and chemical method.Physical method mainly has mechanical stripping
From method, liquid phase stripping method, electrochemical stripping method, epitaxy method etc., chemical method mainly has oxidation-reduction method, chemical vapor deposition
Area method, silicon carbide epitaxy method, solvent-thermal method, arc discharge method, flame method, chemical synthesis etc..
The patent of invention of Application No. 201510428227 discloses a kind of preparation method of graphene, wherein by graphite and
Mechanical stripping is carried out after liquid phase medium mixing, obtains the mixture containing graphite and graphene, then mixture is subjected to centrifugation point
From collecting the supernatant liquor containing graphene so as to prepare graphene.Although this method is simple, waste time and energy, repeatability
Difference, it is difficult to accurate control, be not particularly suited for industrialized production.
He Yuan et al. (prepares graphene and sign, nonmetallic ore, 2013,36 (1) based on native graphite solvent-thermal method：15-
17) it is solvent, ammoniacal liquor for assistant reducing agent to use improved Hummers methods to prepare graphene oxide using ethylene glycol, passes through solvent
Hot method prepares redox graphene.This method can be produced in batches, but use substantial amounts of chemistry examination in process of production
Agent, there is larger harm to environment, and the electronic structure for the graphene being prepared and perfection of crystal are all by serious
Destruction.
The patent of invention of Application No. 201610841150 discloses a kind of method of preparing grapheme through oxidation reduction, specifically
Method is first to peel off graphite oxidation graphene oxide is prepared, and then adds graphene oxide into the aqueous solution of halide
Middle reaction obtains electrolyte, finally using metal as negative electrode, using inert electrode as anode, the electrolyte is electrolysed, in negative electrode
Surface obtains graphene.This method is applied to industrialized production and can provide condition for modification of the graphene in the later stage, but makes
Reducing agent is most highly corrosive and explosive, has harm to environment and personnel.
The patent of invention of Application No. 201610471854 discloses a kind of by chemical vapor deposition growth graphene
Method, specific method are that first substrate is filled in boiler tube, are re-introduced into the reacting gas of oxygen-containing carbon source into boiler tube, heating response gas
Body discharges carbon atom to decompose oxygen-containing carbon source, by the decomposition of carbon source, and carbon atom deposition forms graphite on a surface of a substrate
Alkene film.Graphene prepared by this method has the advantages of high quality and large area, but cost height, complex process, processing at this stage
The problems such as condition harshness, constrains its development.
The patent of invention of Application No. 201310194548 discloses the side that a kind of ultrasonic wave peels off preparing graphite alkene
Method, graphite is uniformly mixed in organic solvent by a certain percentage with intercalator, preparing graphite alkene is peeled off using ultrasonic wave,
The higher graphene solution of concentration can be made in the method.Although the graphene crystal structure that this method is prepared is complete, it is difficult to
Purifies and separates cause product quality low.
The patent of invention of Application No. 201310411516 discloses a kind of ball-milling preparation method of graphene, by graphite,
Surfactant and water mixing are loaded in ball grinder, and graphene is prepared using high-energy ball milling.This method has simple to operate, operation
The advantages that safe, but to be typically prepared the time longer for this method, power consumption is larger, therefore is not suitable for industrialized production.
At present, although the preparation method of some graphenes has been disclosed, for preparing low cost, low stain, high-quality
The batch production of amount graphene there is also some problems.For example preparing graphite alkene is by mechanically pulling off, the method is not suitable for
Batch production；The graphene prepared using chemical vapour deposition technique, although having complete single layer structure, the method pair is set
Standby and substrate requires high, the problems such as long preparation period, low yield, high production cost be present；Current widely used oxidation
It is to peel off graphite by the process of oxidation as intercalator by the use of acid, alkali, metal etc. and restore that reducing process, which prepares graphene, this
Not only environmental pollution is larger for method, and the graphene defect prepared is more.Recently, grown up ultrasonic stripping and ball milling again
The method that stripping prepares graphene, ultrasonic stripping means need to use substantial amounts of organic solvent, pollute environment, and be prepared
Graphene is difficult to purifies and separates, so as to cause product quality to reduce.Ball milling stripping method prepares graphene, is rushed because powerful when peeling off
Hit power and be easily caused graphene generation lattice defect, reduce the crystalline size of graphene, additionally due to milling time is long, cost is high
High, therefore, it is difficult to realize industrialization large-scale production.
The content of the invention
In view of yielding poorly in the presence of above-mentioned prior art, time-consuming, the number of plies is more, cost is high, pollution is big, technological process
The problems such as complicated, the present invention provide a kind of in a series arrangement connect colloid mill and high pressure homogenizer and made by liquid phase stripping
The method of standby graphene.
The concrete technical scheme of the present invention is as follows：
A kind of method for preparing graphene, comprises the following steps：
By graphite raw material, dispersant and water using mass ratio as 3~150：100~5000：0~10 is configured to graphite slurry；
By the graphite slurry prepared in colloid mill grinding distribution, be then fed into material barrel and the graphite slurry cooled down；Will
Graphite slurry after cooling is pumped into homogeneous in high pressure homogenizer by barrier film, graphite is peeled off shape through high pressure homogenizer homogeneous
Uniformly lack layer graphene into distribution；The graphene slurry is continued cycling through several times in high pressure homogenizer；Will after circulation
The graphene slurry filters, and is cleaned with deionized water, is then dried in freeze drier, and less than 10 layers of graphene is made
Powder.
On the basis of above-mentioned prior art, it can also increase following technical characteristic and further be limited：
One or more of the graphite raw material in expanded graphite, thermal cracking graphite or quasiflake graphite powder.
Dispersant is selected from polyvinylpyrrolidone, the polyacrylate solution of amido, polyacrylate kind block polymer
Solution (HD-2008), the one or more of polysiloxane-polyether copolymer solution.Wherein, polyacrylate kind block polymer
Solution (HD-2008) is bought in Guangzhou Hou Huan chemical assistants Co., Ltd, is a kind of hydrophily high score of affinity groups containing pigment
Sub- block copolymer, belongs to anionic dispersing agents, and pH is about 6.5~7.
The rotating speed of colloid mill is 5400~9000r/min, and milling time is 30~60min.
The flow rate set that graphite slurry enters high pressure homogenizer is 40~60L/h.
The pressure of the pressure valve of high pressure homogenizer is 300~800bar.
Graphene slurry circulates 3~15 times in high pressure homogenizer.
In the 5th step, graphene slurry is cleaned 2~3 times with deionized water.
Compared with the conventional method, the present invention has advantages below：
(1) the optional species of graphite raw material is more, cheap, can effectively reduce production cost；
(2) pollution of the reagent to environment in experimentation can be effectively avoided from aqueous phase, effectively reduces the later stage to sample
The difficulty that product are handled；
(3) homogeneous is carried out to raw material by high pressure homogenizer, the graphene crystal structure being prepared is complete, yield it is high and
Technological process is simple.
In addition, the present invention also has simple technological process, non-environmental-pollution, is adapted to the advantages of batch production, it is graphene
Realize the extraordinary approach of industrialization.
Brief description of the drawings
Fig. 1 shows the technique general schematic view of the present invention.
Fig. 2 is the shape appearance figure that the graphene platelet prepared in embodiment 1 is characterized by SEM.
Fig. 3 is the shape appearance figure that the graphene platelet prepared in embodiment 2 is characterized by SEM.
Fig. 4 is the shape appearance figure that the graphene platelet prepared in embodiment 3 is characterized by SEM.
Fig. 5 is the shape appearance figure that the graphene platelet prepared in embodiment 4 is characterized by SEM.
Fig. 6 is the shape appearance figure that the graphene platelet prepared in embodiment 5 is characterized by SEM.
Embodiment
The present invention is described in detail with instantiation below in conjunction with the accompanying drawings.
As shown in figure 1, the present invention is first raw material by solvent, graphite of water, graphite slurry is prepared into after adding dispersant, then
Graphite slurry is passed through high pressure homogenizer, graphite is quickly peeled off under high shear power and impact force action, crystal knot is made
The form the few-layer graphene alkene slurry that structure defect is few, quality is high, obtained graphene slurry is finally made by graphite using freeze-drying
Alkene powder.Specific embodiment is as follows：
Embodiment 1
(1) by expanded graphite raw material, polyvinylpyrrolidone and water using mass ratio as 3：100：0 is configured to graphite slurry.
(2) graphite slurry of step (1) grinding distribution in colloid mill is taken, the rotating speed of colloid mill is 6200r/min, grinding
Slurry is cooled down into material barrel after 50min.
(3) graphite slurry after above-mentioned cooling is pumped into homogeneous in high pressure homogenizer by barrier film, graphite slurry with
46L/h speed enters in the cavity of high pressure homogenizer, adjusts the pressure of pressure valve to 800bar, makes through high pressure homogenizer homogeneous
Graphite peels off the few layer graphene to be formed and be evenly distributed.
(4) above-mentioned graphene slurry is continued cycling through 3~15 times in high pressure homogenizer, high pressure homogenizer device parameter with
Above-mentioned steps are consistent.
(5) slurry is filtered after circulating 3~15 times, is cleaned 2~3 times with deionized water, is then done in freeze drier
It is dry, you can 1~10 layer of graphene powder being evenly distributed is made.
Show by morphology analysis and structural analysis, obtained less than 10 layers graphene numbers of plies distribution is equal in the present embodiment
Even, fault of construction is few.
Embodiment 2
(1) by expanded graphite raw material, polyvinylpyrrolidone and water using mass ratio as 140：4500：7 are configured to black lead wash
Material.
(2) graphite slurry of step (1) grinding distribution in colloid mill is taken, the rotating speed of colloid mill is 6000r/min, grinding
Slurry is cooled down into material barrel after 50min.
(3) graphite slurry after above-mentioned cooling is pumped into homogeneous in high pressure homogenizer by barrier film, graphite slurry with
46L/h speed enters in the cavity of high pressure homogenizer, adjusts the pressure of pressure valve to 800bar, makes through high pressure homogenizer homogeneous
Graphite peels off the few layer graphene to be formed and be evenly distributed.
(4) above-mentioned graphene slurry is continued cycling through 3~15 times in high pressure homogenizer, high pressure homogenizer device parameter with
Above-mentioned steps are consistent.
(5) slurry is filtered after circulating 3~15 times, is cleaned 2~3 times with deionized water, is then done in freeze drier
It is dry, you can 1~10 layer of graphene powder being evenly distributed is made.
Show by morphology analysis and structural analysis, obtained less than 10 layers graphene numbers of plies distribution is equal in the present embodiment
Even, fault of construction is few.
Embodiment 3
(1) by expanded graphite raw material, polyvinylpyrrolidone and water using mass ratio as 30：1000：3 are configured to black lead wash
Material.
(2) graphite slurry of step (1) grinding distribution in colloid mill is taken, the rotating speed of colloid mill is 5800r/min, grinding
Slurry is cooled down into material barrel after 50min.
(3) graphite slurry after above-mentioned cooling is pumped into homogeneous in high pressure homogenizer by barrier film, graphite slurry with
46L/h speed enters in the cavity of high pressure homogenizer, adjusts the pressure of pressure valve to 800bar, makes through high pressure homogenizer homogeneous
Graphite peels off the few layer graphene to be formed and be evenly distributed.
(4) above-mentioned graphene slurry is continued cycling through 3~15 times in high pressure homogenizer, high pressure homogenizer device parameter with
Above-mentioned steps are consistent.
(5) slurry is filtered after circulating 3~15 times, is cleaned 2~3 times with deionized water, is then done in freeze drier
It is dry, you can 1~10 layer of graphene powder being evenly distributed is made.
Show by morphology analysis and structural analysis, obtained less than 10 layers graphene numbers of plies distribution is equal in the present embodiment
Even, fault of construction is few.
Embodiment 4
(1) by expanded graphite raw material, polyvinylpyrrolidone and water using mass ratio as 67：3000：10 are configured to black lead wash
Material.
(2) graphite slurry of step (1) grinding distribution in colloid mill is taken, the rotating speed of colloid mill is 5800r/min, grinding
Slurry is cooled down into material barrel after 40min.
(3) graphite slurry after above-mentioned cooling is pumped into homogeneous in high pressure homogenizer by barrier film, graphite slurry with
46L/h speed enters in the cavity of high pressure homogenizer, adjusts the pressure of pressure valve to 800bar, makes through high pressure homogenizer homogeneous
Graphite peels off the few layer graphene to be formed and be evenly distributed.
(4) above-mentioned graphene slurry is continued cycling through 3~15 times in high pressure homogenizer, high pressure homogenizer device parameter with
Above-mentioned steps are consistent.
(5) slurry is filtered after circulating 3~15 times, is cleaned 2~3 times with deionized water, is then done in freeze drier
It is dry, you can 1~10 layer of graphene powder being evenly distributed is made.
Show by morphology analysis and structural analysis, obtained less than 10 layers graphene numbers of plies distribution is equal in the present embodiment
Even, fault of construction is few.
Embodiment 5
(1) by expanded graphite raw material, polyvinylpyrrolidone and water using mass ratio as 5：160：1 is configured to graphite slurry.
(2) graphite slurry of step (1) grinding distribution in colloid mill is taken, the rotating speed of colloid mill is 5400r/min, grinding
Slurry is cooled down into material barrel after 40min.
(3) graphite slurry after above-mentioned cooling is pumped into homogeneous in high pressure homogenizer by barrier film, graphite slurry with
45L/h speed enters in the cavity of high pressure homogenizer.The pressure of pressure valve is adjusted to 750bar, is made through high pressure homogenizer homogeneous
Graphite peels off the few layer graphene to be formed and be evenly distributed.
(4) above-mentioned graphene slurry is continued cycling through 3~15 times in high pressure homogenizer, high pressure homogenizer device parameter with
Above-mentioned steps are consistent.
(5) slurry is filtered after circulating 3~15 times, is cleaned 2~3 times with deionized water, is then done in freeze drier
It is dry, you can 1~10 layer of graphene powder being evenly distributed is made.
Show by morphology analysis and structural analysis, obtained less than 10 layers graphene numbers of plies distribution is equal in the present embodiment
Even, fault of construction is few.
The present invention is raw material using cheap plurality of specifications graphite, and graphene is prepared in the method peeled off using liquid phase.
The cheap and more specification of raw material makes this method be more suitable for industrialized production, and can effectively reduce industrialized production graphene
Cost.
The present invention selects solvent of the aqueous phase as graphite, can effectively reduce the difficulty that the later stage handled sample, together
When avoid the injury of pollution and staff of the solvent to environment in process of production.
Present invention selection colloid mill and high pressure homogenizer are used in conjunction, and wherein colloid mill is as pre-dispersed equipment early stage so that stone
Black slurry is uniformly dispersed in aqueous phase, while graphite slurry lamella during glue mill is more, and the big part of particle is broken, shape
Into precrushing slurry, the effective efficiency for improving high pressure homogenizer homogeneous graphite, two equipment, which are used in conjunction, to be more suitable for producing graphite in batches
Alkene.
The technological process of the present invention is simple, while can carry out circulation homogeneous to material, makes the graphene film being prepared
Layer is few, and crystal structure is complete, and yield is high.
For the present invention by experiment, and graphene powder is prepared, effect is highly desirable, and prepares the expection of scheme
Unanimously.
Claims (8)
1. a kind of method for preparing graphene, comprises the following steps：
(1) by graphite raw material, dispersant and water using mass ratio as 3~150：100~5000：0~10 is configured to graphite slurry；
(2) by the graphite slurry prepared in colloid mill grinding distribution, be then fed into material barrel to the graphite slurry carry out
Cooling；
(3) graphite slurry after cooling is pumped into homogeneous in high pressure homogenizer by barrier film, made through high pressure homogenizer homogeneous
Graphite peels off the few layer graphene to be formed and be evenly distributed；
(4) the graphene slurry is continued cycling through several times in high pressure homogenizer；
(5) the graphene slurry is filtered after circulating, cleaned with deionized water, is then dried in freeze drier, is made
Less than 10 layers of graphene powder.
2. the method according to claim 1 for preparing graphene, it is characterised in that：The graphite raw material is selected from expansion stone
One or more in ink, thermal cracking graphite or quasiflake graphite powder.
3. the method according to claim 1 for preparing graphene, it is characterised in that：The dispersant is selected from polyvinyl pyrrole
Alkanone powder, the polyacrylate solution of amido, polyacrylate block polymer solution, polysiloxane-polyether copolymer
One or more in solution.
4. the method according to claim 1 for preparing graphene, it is characterised in that：The rotating speed of the colloid mill be 5400~
9000r/min, milling time are 30~60min.
5. the method according to claim 1 for preparing graphene, it is characterised in that：The graphite slurry enters high-pressure homogeneous
The flow rate set of machine is 40~60L/h.
6. the method according to claim 1 for preparing graphene, it is characterised in that：The pressure valve of the high pressure homogenizer
Pressure is 300~800bar.
7. the method according to claim 1 for preparing graphene, it is characterised in that：The graphite slurry is in high pressure homogenizer
It is middle to circulate 3~15 times.
8. the method according to claim 1 for preparing graphene, it is characterised in that：In the 5th step, deionized water is used
Clean graphene slurry 2~3 times.
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| EP3192822A4 (en) * | 2014-12-12 | 2018-07-04 | LG Chem, Ltd. | Block copolymer and method for preparing graphene by using same |
| CN108423664A (en) * | 2018-04-26 | 2018-08-21 | 昆明理工大学 | A kind of preparation method of phosphorus alkene-graphene composite material |
| CN108630338A (en) * | 2018-03-08 | 2018-10-09 | 北京地泽科技有限公司 | A kind of method, apparatus for producing graphene conductive slurry in batches and graphene conductive slurry prepared therefrom |
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| US11192085B2 (en) | 2014-12-12 | 2021-12-07 | Lg Chem, Ltd. | Block copolymer, and method for preparing graphene using same |
| EP3192822A4 (en) * | 2014-12-12 | 2018-07-04 | LG Chem, Ltd. | Block copolymer and method for preparing graphene by using same |
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| CN109147988A (en) * | 2018-08-02 | 2019-01-04 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | A kind of preparation method of thin graphene slurry |
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| CN109461936A (en) * | 2018-09-25 | 2019-03-12 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | A kind of environment-friendly preparation method thereof of the aqueous composite mortar of graphene |
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| CN110070996A (en) * | 2019-05-28 | 2019-07-30 | 中山大学 | Nickel sulfide/graphene composite material preparation method and application |
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| CN112143072A (en) * | 2020-09-02 | 2020-12-29 | 新奥（内蒙古）石墨烯材料有限公司 | Graphene/polyethylene heat conduction material, preparation method thereof, pipe using heat conduction material and ground source heat pump |
| CN112573510A (en) * | 2020-12-30 | 2021-03-30 | 中国科学院过程工程研究所 | Graphene slurry and preparation method and application thereof |
| CN113019659A (en) * | 2021-04-02 | 2021-06-25 | 严冬梅 | Graphene powder preparation and processing method |
| CN115231561A (en) * | 2021-04-22 | 2022-10-25 | 中国石油化工股份有限公司 | Powder graphene and preparation method and application thereof |
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| CN115231561B (en) * | 2021-04-22 | 2023-09-29 | 中国石油化工股份有限公司 | Powder graphene and preparation method and application thereof |
| RU2829790C2 (en) * | 2021-04-22 | 2024-11-05 | Чайна Петролеум Энд Кемикал Корпорейшн | Graphene powder, method for production thereof and use thereof |
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