CN105752972A - Method for preparing graphene material from inorganic laminates through high-pressure draft stripping - Google Patents
Method for preparing graphene material from inorganic laminates through high-pressure draft stripping Download PDFInfo
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- CN105752972A CN105752972A CN201610189839.3A CN201610189839A CN105752972A CN 105752972 A CN105752972 A CN 105752972A CN 201610189839 A CN201610189839 A CN 201610189839A CN 105752972 A CN105752972 A CN 105752972A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses a method for preparing a graphene material from inorganic laminates through high-pressure draft stripping and belongs to the preparation technology of carbon nanomaterial graphene.The process route comprises the steps that the inorganic laminar materials are a graphite material are ground through a ball mill; the inorganic laminar materials are inserted into a graphite layer through a high-temperature furnace in a vacuum glove box under inert gas shielding, and a graphite intercalation compound is formed; finally, the graphite is shorn and stripped through high-pressure draft circulation in a high-pressure draft pulverizer; washing is carried out with deionized water, filtering and drying are carried out, and then graphene is obtained.Compared with other modes, the method has the advantages that the raw materials are wide in source and low in cost, the process is simple, large-scale production can be achieved, acid or base or other chemical materials are not used, and graphene preparation is stable and safe.
Description
Technical field
The invention belongs to a kind of carbon nanomaterial preparation technology, more particularly say, refer to a kind of method utilizing inorganic synusia to prepare Graphene by high pressure draught stripping.
Background technology
After CNT, Graphene (also referred to as mono-layer graphite or graphene) becomes the low-dimensional Carbon Materials got most of the attention.Graphene is by waiting monolayer hexagonal carbon atom cellular to constitute, and atom is honeycomb arrangement, has good mechanics and electric property.In Graphene, carrier has ballistic transport characteristic, under room temperature, the mean free path of carrier and coherence length reach micron dimension, mobility is about 100 times of silicon, be conducive to manufacturing and there is higher fusing point and high thermal conductivity, so graphene device likely at high temperature works, these character all become the ideal material of following nano electron device and nanometric circuit, have broad application prospects.
It is reported, electronics movement velocity in Graphene has reached the 1/300 of the light velocity, considerably beyond electronics movement velocity in general conductor.In plastics, mix centesimal Graphene, plastics just can be made to possess good electric conductivity；Add millesimal Graphene, the heat resistanceheat resistant performance of plastics can be made to improve 30 degrees Celsius.Thin, light, the good and superpower tough new material of draftability can be developed on this basis, be used for manufacturing automobile, aircraft and satellite.On the other hand, new forms of energy battery is also the big key areas that Graphene is commercial the earliest.Massachusetts Institute Technology successfully develops the surface flexible photovoltaic battery plate with graphene nano coating before, can greatly reducing the cost manufacturing transparent deformable solaode, this battery is likely applied in the small size digital equipment such as night vision goggles, camera.It addition, the successful research and development of Graphene superbattery, also solve the off-capacity of new energy car battery and the problem of charging interval length, greatly accelerate the development of new forms of energy battery industry.
For a long time, people think that thermodynamics fluctuation does not allow any two dimensional crystal to exist at limited temperature always, so while the research of the zero dimension of carbon and one-dimentional structure is carried out relatively early, but until Two-dimensional Carbon structure in 2004---Graphene is just found by Novose and Geim etc..From then on, because the characteristic of its excellence rapidly becomes one of investigation of materials focus in recent years, exposing huge application prospect in the exhibition of the field such as new forms of energy, new material, electronics, but its complex manufacturing, yielding poorly and selling at exorbitant prices is always up limiting the bottleneck of its industrialized development.
At present, the main method preparing Graphene has oxidation-reduction method, chemical vapour deposition technique, microcomputer stripping method etc..Although microcomputer stripping method technique is simple, but there is the problem that productivity is too low and cost is high；, there is expensive cost high in chemical vapour deposition technique, although can meet scale and prepare the requirement of high-quality graphene, but process route is more complicated and needs fuel gas and monocrystalline nickel etc., and has the shortcomings such as potential safety hazard in the process of generation Graphene；Oxidation-reduction method, it is generally required to react generation in a solvent, the if desired material under drying regime, follow-up also need to increase and dry, prevent the techniques such as reunion, although production cost relative moderate, but exist and use the problem using soda acid etc. to easily cause environmental pollution etc. in limitation and preparation process.
A kind of inorganic synusia is utilized to prepare in the process of Graphene by high pressure draught recirculation gas stripper, owing to not using the media such as soda acid chemical substance, it is only nano ply is inserted in the molten state in graphite and promote the collision mutually of storeroom by high pressure draught, shear, reduce Van der Waals force, make material reach the purpose of broken stripping.Therefore, the advantage such as have that raw material sources is wide, process route simple, product uses extensively and safety and stability is pollution-free, yield is high and can the production of large-scale.
Summary of the invention
The order of the present invention is in that, it is provided that a kind of utilize inorganic synusia to insert the method preparing Graphene in crystalline flake graphite and by high pressure draught stripping.Being inserted in graphite material by inorganic synusia, then pass through high pressure draught stripping and prepare Graphene, have raw material sources extensive, less costly, technique is simple, it is possible to realizes large-scale production, and does not use the chemical materials such as soda acid, prepares Graphene and stablize safety.
Inorganic layer sheet material is inserted in graphite material by the present invention by vacuum glove box in high temperature, obtains compound between graphite layers；Then, by compound between graphite layers in high pressure draught pulverizer, peeled off by high pressure draught circulation shear；Being finally 6.4-7.1 by product deionized water wash to pH value, filtration drying obtains Graphene.
The process chart of preparation method provided by the invention is as it is shown in figure 1, Fig. 2 is product TEM figure, including step in detail below:
(1) start ball mill, after temperature is to 20-50 DEG C, weighs inorganic layer sheet material and graphite material according to the mass ratio of 9 ~ 10:2 ~ 3, and put in ball mill, run 30 120 minutes；
(2) composite material of (1st) step is put in the vacuum glove box of full noble gas, be then placed in 400 DEG C of-500 DEG C of high temperature furnaces, react 5 ~ 8 hours；Product is cooled down and namely obtains compound between graphite layers with deionized water wash filtering drying；
(3) starting high pressure draught pulverizer, air pressure adjustment to 1.0-1.7 MPa, temperature was adjusted to 30-80 DEG C, is put into by compound between graphite layers in high pressure draught pulverizer, by high pressure draught recirculation gas stripper compound between graphite layers 50-200 minute；
(4) step (3) gained material is spent filtering drying after ionized water cleaning is 6.4-7.1 to pH value, namely obtains Graphene.
In above-mentioned preparation method provided by the invention, it is preferable that in step (1), described graphite material is expanded graphite, the one of crystalline flake graphite or both mixture.
In above-mentioned preparation method provided by the invention, it is preferable that the particle diameter of described graphite material is 20-100 μm.
In above-mentioned preparation method provided by the invention, it is preferable that in step (1), described inorganic layer sheet material is at least one in the nano imvite of aggregated thing intercalation modifying, nanomete talc powder, nano zeolite；The thickness of described inorganic layer sheet material is 100-1000nm.
In above-mentioned preparation method provided by the invention, preferably, described polymer is at least one in double hydroxyethyl Dodecyl trimethyl ammonium chloride, octadecyl trimethyl ammonium chloride, vinyl benzyl-dimethyl hexadecyl ammonium chloride, 3,5-dimethylphenyl octadecyl ammonium chloride.
In above-mentioned preparation method provided by the invention, it is preferable that in step (2), described noble gas is the one in helium, neon, argon, krypton, xenon.
In above-mentioned preparation method provided by the invention, it is preferable that ball mill is the one in the ultra-fine lamination grinding machine of the tube mill of dry type, the bar type ball mill of dry type, dry type in step (1)；Steel ball in described ball mill is 20-100mm steel ball
In above-mentioned preparation method provided by the invention, it is preferable that, it is characterised in that, in step (3), described high pressure draught pulverizer is that spiral jet pulverizer, fluid bed are to the one in spray formula airflow milling, circulating tube type airflow milling.
Beneficial effect
Compared with prior art; inorganic layer sheet material and graphite material are passed through ball mill grinding by the present invention; then in the vacuum glove box under inert gas shielding; by high temperature furnace, inorganic layer sheet material is intercalation into graphite layers; become graphite intercalation compound; last in jet mill, utilize high pressure draught circulation shear to peel off graphite, filter again through deionized water wash and obtain Graphene after removing inorganic layer sheet material.The advantage such as have that raw material sources is wide, process route simple, product uses extensively and safety and stability is pollution-free, yield is high and can the production of large-scale.
Accompanying drawing explanation
Fig. 1 is the process flow diagram that the present invention prepares Graphene.Wherein, A is inorganic layer sheet material；B is graphite material；C is Graphene.
Fig. 2 is the TEM figure that the present invention prepares Graphene.
Fig. 3 is that the present invention prepares the Raman spectrogram of G1, G2 and G3 in Graphene example 1,2 and 3, and wherein, abscissa is wave number, unit: cm-1, vertical coordinate is peak intensity, and unit is: absolute unit (a.u.).
Detailed description of the invention
By detailed description of the invention, the present invention is described in further detail, but this should not being interpreted as, the scope of the present invention is only limitted to Examples below.When without departing from said method thought of the present invention, the various replacements made according to ordinary skill knowledge and customary means or change, should be included in the scope of the present invention.
Embodiment 1
A kind of method utilizing inorganic synusia to prepare grapheme material by high pressure draught stripping, including step once:
(1) start ball mill, when, after temperature to 50 DEG C, weighing inorganic layer sheet material and graphite material according to the mass ratio of 10:3, and put in ball mill, run 30 120 minutes；
(2) composite material of (1st) step is put in the vacuum glove box of full noble gas, be then placed in 500 DEG C of high temperature furnaces, react 8 hours；Product is cooled down and namely obtains compound between graphite layers with deionized water wash filtering drying；
(3) starting high pressure draught pulverizer, air pressure adjustment to 1.7 MPas, temperature was adjusted to 80 DEG C, is put into by compound between graphite layers in jet mill, by high pressure draught recirculation gas stripper compound between graphite layers 200 minutes；
(4) being cleaned by above-mentioned resulting materials deionized water to pH value is filtering drying after 7.1, namely obtains product Graphene G1.
Being the Raman spectrum analysis of 532nm by using wavelength, 2D peak is biphonon resonance raman peak, and the stacking degree of its intensity reflection Graphene, its width reflects the number of plies of its Graphene.Raman spectrum analysis in Fig. 3, the G peak in G1 is positioned at 1580cm-1, 2D peak be positioned at 2630cm-1, 2D peak shape is sharp-pointed, symmetrical, it was shown that the Graphene number of plies is relatively low.
Embodiment 2
A kind of method utilizing inorganic synusia to prepare grapheme material by high pressure draught stripping, including step once:
(1) start ball mill, when, after temperature to 20 DEG C, weighing inorganic layer sheet material and graphite material according to the mass ratio of 9:3, and put in ball mill, run 30 120 minutes；
(2) composite material of (1st) step is put in the vacuum glove box of full noble gas, be then placed in 400 DEG C of high temperature furnaces, react 5 hours；Product is cooled down and namely obtains compound between graphite layers with deionized water wash filtering drying；
(3) starting high pressure draught pulverizer, air pressure adjustment to 1.0 MPas, temperature was adjusted to 30 DEG C, is put into by compound between graphite layers in jet mill, by high pressure draught recirculation gas stripper compound between graphite layers 50 minutes；
(4) being cleaned by above-mentioned resulting materials deionized water to pH value is filtering drying after 6.4, namely obtains Graphene G2.
The Graphene G2 that embodiment is obtained is analyzed, the Raman spectrum analysis in Fig. 3, and the G peak in G2 is positioned at 1570cm-1, 2D peak is positioned at 2650cm-1, 2D peak shape is more weak than G1 intensity, symmetry is relatively low, it was shown that its Graphene number of plies is more than G1.
Embodiment 3
A kind of method utilizing inorganic synusia to prepare grapheme material by high pressure draught stripping, including step once:
(1) start ball mill, when, after temperature to 40 DEG C, weighing inorganic layer sheet material and graphite material according to the mass ratio of 9:2, and put in ball mill, run 80 minutes；
(2) composite material of (1st) step is put in the vacuum glove box of full noble gas, be then placed in 450 DEG C of high temperature furnaces, react 6 hours；Product is cooled down and namely obtains compound between graphite layers with deionized water wash filtering drying；
(3) starting high pressure draught pulverizer, air pressure adjustment to 1.5 MPas, temperature was adjusted to 75 DEG C, is put into by compound between graphite layers in jet mill, by high pressure draught recirculation gas stripper compound between graphite layers 130 minutes；
(4) being cleaned by above-mentioned resulting materials deionized water to pH value is filtering drying after 6.8, namely obtains Graphene.
Claims (8)
1. one kind utilizes the method that inorganic synusia prepares grapheme material by high pressure draught stripping, it is characterised in that comprise the technical steps that:
(1) start ball mill, after temperature is to 20-50 DEG C, weighs inorganic layer sheet material and graphite material according to the mass ratio of 9 ~ 10:2 ~ 3, and put in ball mill, run 30 120 minutes；
(2) composite material of (1st) step is put in the vacuum glove box of full noble gas, be then placed in 400 DEG C of-500 DEG C of high temperature furnaces, react 5 ~ 8 hours；Product is cooled down and namely obtains compound between graphite layers with deionized water wash filtering drying；
(3) starting high pressure draught pulverizer, air pressure adjustment to 1.0-1.7 MPa, temperature was adjusted to 30-80 DEG C, is put into by compound between graphite layers in high pressure draught pulverizer, by high pressure draught recirculation gas stripper compound between graphite layers 50-200 minute；
(4) step (3) gained material is spent filtering drying after ionized water cleaning is 6.4-7.1 to pH value, namely obtains Graphene.
2. a kind of method utilizing inorganic synusia to prepare grapheme material by high pressure draught stripping according to claim 1, it is characterised in that in step (1), described graphite material is expanded graphite, the one of crystalline flake graphite or both mixture.
3. a kind of method utilizing inorganic synusia to prepare grapheme material by high pressure draught stripping according to claim 2, it is characterised in that the particle diameter of described graphite material is 20-100 μm.
4. a kind of method utilizing inorganic synusia to prepare grapheme material by high pressure draught stripping according to claim 1, it is characterized in that, in step (1), described inorganic layer sheet material is at least one in the nano imvite of aggregated thing intercalation modifying, nanomete talc powder, nano zeolite；The thickness of described inorganic layer sheet material is 100-1000nm.
5. a kind of method utilizing inorganic synusia to prepare grapheme material by high pressure draught stripping according to claim 4, it is characterized in that, described polymer is at least one in double hydroxyethyl Dodecyl trimethyl ammonium chloride, octadecyl trimethyl ammonium chloride, vinyl benzyl-dimethyl hexadecyl ammonium chloride, 3,5-dimethylphenyl octadecyl ammonium chloride.
6. a kind of method utilizing inorganic synusia to prepare grapheme material by high pressure draught stripping according to claim 1, it is characterised in that in step (2), described noble gas is the one in helium, neon, argon, krypton, xenon.
7. a kind of method utilizing inorganic synusia to prepare grapheme material by high pressure draught stripping according to claim 1, it is characterized in that, ball mill is the one in the ultra-fine lamination grinding machine of the tube mill of dry type, the bar type ball mill of dry type, dry type in step (1)；Steel ball in described ball mill is 20-100mm steel ball.
8. a kind of method utilizing inorganic synusia to prepare grapheme material by high pressure draught stripping according to claim 1, it is characterized in that, in step (3), described high pressure draught pulverizer is that spiral jet pulverizer, fluid bed are to the one in spray formula airflow milling, circulating tube type airflow milling.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241789A (en) * | 2016-08-28 | 2016-12-21 | 桂林新艺制冷设备有限责任公司 | A kind of method preparing Graphene |
| CN106587027A (en) * | 2017-01-05 | 2017-04-26 | 苏州高通新材料科技有限公司 | Method for rapidly preparing small-dimensional graphene |
| CN106829940A (en) * | 2017-03-31 | 2017-06-13 | 长沙蓝态尔电子科技有限公司 | The production equipment and its production technology of a kind of grapheme material |
| CN107022190A (en) * | 2017-04-20 | 2017-08-08 | 成都新柯力化工科技有限公司 | One kind is used for the enhanced graphene microchip masterbatch of engineering plastics and preparation method |
| CN107032336A (en) * | 2017-06-16 | 2017-08-11 | 成都新柯力化工科技有限公司 | The alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state |
| CN107416810A (en) * | 2017-06-19 | 2017-12-01 | 成都新柯力化工科技有限公司 | A kind of method that graphene is peeled off using alternating electric field vibro-grinding |
| CN107879331A (en) * | 2016-09-29 | 2018-04-06 | 河南烯碳合成材料有限公司 | The method for manufacturing graphene of the basal plane lateral dimensions more than 50 nanometers |
| CN111422858A (en) * | 2020-04-13 | 2020-07-17 | 鹤岗市振金石墨烯新材料研究院 | Method for efficiently preparing graphene |
| CN112174122A (en) * | 2020-09-30 | 2021-01-05 | 李素红 | Antibacterial graphene nano knife and preparation method and application thereof |
| CN115536033A (en) * | 2022-08-16 | 2022-12-30 | 浙江工业大学 | Preparation method of ultrathin black talc nanosheet |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106241789A (en) * | 2016-08-28 | 2016-12-21 | 桂林新艺制冷设备有限责任公司 | A kind of method preparing Graphene |
| CN107879331A (en) * | 2016-09-29 | 2018-04-06 | 河南烯碳合成材料有限公司 | The method for manufacturing graphene of the basal plane lateral dimensions more than 50 nanometers |
| CN106587027A (en) * | 2017-01-05 | 2017-04-26 | 苏州高通新材料科技有限公司 | Method for rapidly preparing small-dimensional graphene |
| CN106829940A (en) * | 2017-03-31 | 2017-06-13 | 长沙蓝态尔电子科技有限公司 | The production equipment and its production technology of a kind of grapheme material |
| CN107022190A (en) * | 2017-04-20 | 2017-08-08 | 成都新柯力化工科技有限公司 | One kind is used for the enhanced graphene microchip masterbatch of engineering plastics and preparation method |
| CN107022190B (en) * | 2017-04-20 | 2019-04-05 | 江苏华曼复合材料科技有限公司 | A kind of graphene microchip masterbatch and preparation method for engineering plastics enhancing |
| CN107032336B (en) * | 2017-06-16 | 2018-03-13 | 成都新柯力化工科技有限公司 | The alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state |
| CN107032336A (en) * | 2017-06-16 | 2017-08-11 | 成都新柯力化工科技有限公司 | The alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state |
| CN107416810A (en) * | 2017-06-19 | 2017-12-01 | 成都新柯力化工科技有限公司 | A kind of method that graphene is peeled off using alternating electric field vibro-grinding |
| CN111422858A (en) * | 2020-04-13 | 2020-07-17 | 鹤岗市振金石墨烯新材料研究院 | Method for efficiently preparing graphene |
| CN112174122A (en) * | 2020-09-30 | 2021-01-05 | 李素红 | Antibacterial graphene nano knife and preparation method and application thereof |
| CN115536033A (en) * | 2022-08-16 | 2022-12-30 | 浙江工业大学 | Preparation method of ultrathin black talc nanosheet |
| CN115536033B (en) * | 2022-08-16 | 2024-02-13 | 浙江工业大学 | Preparation method of ultrathin black talcum nano-sheet |
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