CN108394890A - The method that compression ignition method prepares graphene - Google Patents
The method that compression ignition method prepares graphene Download PDFInfo
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- CN108394890A CN108394890A CN201710077369.6A CN201710077369A CN108394890A CN 108394890 A CN108394890 A CN 108394890A CN 201710077369 A CN201710077369 A CN 201710077369A CN 108394890 A CN108394890 A CN 108394890A
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Abstract
The present invention provides a kind of preparation method of graphene, using purified acetylene and oxygen as raw material, in four stroke reciprocating piston internal combustion engine combustion chambers graphene is generated under oxygen debt compression ignition reaction, cool down in vacuum tank through quick throttle, it is drawn into the water containing graphene dispersion agent by water-ring vacuum pump, rubble ink alkene is made, 85% or more content is obtained after purified, thickness 3.0nm is hereinafter, piece diameter is mainly distributed on 0.5~3 μm of grapheme material.
Description
Technical field
The invention belongs to technical field of graphene preparation, are related to a kind of preparation method of graphene.
Background technology
Graphene is a kind of honey comb like quasi- two-dimensional structure formed after sp2 electron orbit hydridization by carbon atom, is carbon
Another allotrope of element.It is the only one layer of atom for being stripped out from graphite material, being made of carbon atom
The two dimensional crystal of thickness.
Graphene is a kind of material studied the most extensively in world wide.In structure, it is one layer of hexagonal honeycomb knot
The carbon atom thin slice of structure composition.As a kind of new material, it has a variety of excellent specific properties, such as high intensity, ultra-thin, impermeable
Water, electrical and thermal conductivity performance are good, flexibility is good.Graphene is that current nature is most thin, the highest material of intensity, and fracture strength ratio is most
Taller 200 times good of steel, while it has good elasticity, stretch range that can reach the 20% of own dimensions again.In addition, stone
Black 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) can not also penetrate.
Graphene as presently found most thin, maximum intensity, a kind of strongest novel nano-material of electrical and thermal conductivity performance,
It is referred to as " dark fund ".Compared with other new materials, graphene have the characteristics that it is numerous excellent, as carrier mobility is high, electric current
Density is big, intensity is high, thermal conductivity is high, ultra-thin and ultra-light is superhard, at the same have high-performance sensors, can strengthening electronic conveying, catalysis
Agent inhales hydrogen, bipolar semiconductor, without functions such as heat dissipation transmission.Be bound to one graphene technological revolution of outburst in coming 10 years.
The production of graphene film, it is of high cost, also rest on laboratory stage；The customary preparation methods packet of existing graphene
It includes：Micromechanics stripping method, epitaxial growth method, chemical gaseous phase deposition CVD, graphite oxide reduction method, induced with laser phase separation etc..
Micromechanics stripping method, although easy to operate, the quality of graphene prepared is high, and the graphene size obtained is smaller, and imitates
Rate is low, of high cost, poor controllability；Chemical gaseous phase deposition CVD method and epitaxial growth method, are required for high temperature and catalysts conditions；And
Graphite oxide reduction method then needs the strong oxidizer concentrated sulfuric acid, concentrated nitric acid, potassium permanganate and reducing agent hydrazine hydrate, sodium borohydride etc.
A variety of chemical substances, preparation time is also longer, there is certain safety and environmental risk.
Current domestic realization graphene rests on graphene powder production in a daily output tonne other volume production technology, and method is
Physics stripping method, at 1000 DEG C or so, hydrogen does protective gas, makees cathode plate using metal Ru, high-purity lamellar graphite stick does sun
Pole, high voltage direct current electric arc stripped laminar graphite, separates 1~10nm thickness graphenes；Wherein thickness 3nm graphenes below go out
Piece rate is more than 80%, and piece diameter is mainly distributed on 5~20 μm, and graphene lattice is complete, defect is few；In high temperature ring after graphene stripping
The shortcomings of folded, caliper recovery easily occurs back in border during graphene purifying technique behind, can also occur back folded, dispatch from the factory
The usual number of plies of product near 13 layers, piece diameter is mainly distributed on 5~10 μm, and conductivity reaches as high as 105~106S/m, the production
Product can be in the purposes such as electrically conductive ink.That there are goods batch is long for the method for the volume production, product high-temperature time is long, graphene powder
Collection mode etc., which returns in folded and reunion graphene, to have a great impact.The present invention can solve graphene physics stripping method volume production
When too long in flow, the shortcomings of temperature fall time is long, meanwhile, when hidden fire-fighting danger and equipment being avoided to run throughout the year, compression pressure tight metal is set
Preparation gives birth to " hydrogen embrittlement " corrosion, the defect for causing bearing device metal strength to decline at any time.
Invention content
The shortcomings that the technical problem to be solved by the present invention is to be directed to graphene physics stripping method and deficiency provide a kind of new
Can volume production, low cost, environment it is friendly prepare graphene method.
In order to solve the above technical problems, the technical solution used in the present invention is：
The present invention is by compression-ignited reactor (cylinder body, free gravity falling bodies piston, Oilless Lubrication Seal in Petroleum Gas system, pneumatic lifting
Automatically controlled securing pothook of rising stem, electromagnetism etc.), explosive-proof protector shell (and vacuum graphite alkene collecting tank function), water-ring vacuum pump, limit
Pressure valve (and safety valve, throttle expansion valve function), pond, PLC program controller, acetylene purification facility, ultrasonic wave vibration plate etc. have
Machine combines composition；
It is further, it is preferable to use offer of the acetylene as carbon source, is to be easy to purify, including but not limited to fuel gas is such as
Methane, ethane, propane, butane, ethylene, propylene, butylene etc. and methanol, ethyl alcohol, gasoline, the diesel oil etc. that can be used for compression ignition reaction.
Further, in compression ignition reactor, mixed gas is compressed through free gravity falling bodies, it is more than 10 to reach compression ratio
Shi Fasheng detonations, different according to oxygen and acetylene accounting, compression ignition reaction temperature can be between 500 DEG C~3200 DEG C, and compression ignition is quick-fried
Fried pressure is between 1.2~8.0Mpa.Acetylene content 2.0%~80.0% (vol), oxygen content 2.0%~50.0% (vol)
Since compression ignition reaction contains physical explosion and chemical explosion, the steady detonation wave that physical explosion generates, gas radiates in a short time
Property high speed swell (pressure change dramatically), detonation wave is gas expansion speed caused by explosion time higher than caused by velocity of sound.Oxygen
Explosion with the mixed gas of imflammable gas belongs to chemical explosion, and oxidation reaction occurs.Compression ignition under anoxic conditions, reaction production
Object has carbon, carbon monoxide, carbon dioxide and water.Compression ignition reacts newly-generated carbon particulate, and under the shear action of detonation wave, carbon is micro-
Grain is peeling-off, generates graphene microchip, compression ignition reaction pressure after the pressure for passing through safety valve setting more than opening, into vacuum
Chamber；The graphene that detonation reaction generates cools down rapidly in vacuum graphite alkene collecting tank, avoids graphene from returning folded and reunite, sets simultaneously
Setting vacuum graphite alkene collecting tank can be to avoid air bleeding valve carbon deposition phenomenon.Vacuum graphite alkene collecting tank is the pass of graphene volume production technology
Button apparatus.The speed of exhaust of water-ring vacuum pump is more than the deflation rate of compression ignition reactor, and blast pressure is than peace when authentic testing
Full valve pressure set points are high (see Fig. 1).
Further, the pressure of the gas explosion after compression ignition, the temperature of compression ignition room can pass through the pressure of regulation safety valve
Setting adjustment, the height that compression ignition explosive force rebound piston returns to are arranged according to 20 times of gas expansion spaces, and second of falling is again
Start safety valve to open, gravity piston is promoted by pneumatic pull rod, is returned to original state, meanwhile, secondary mixed gas is inhaled
Enter, forms one cycle, similar four-stroke engine.It repeats four-stroke cycle and keeps the operation of graphene continuous production.Complete mistake
Journey is as follows
Suction stroke：
IO Intake Valve Opens, exhaust valve closing, piston are promoted by pneumatic cylinder, are moved from lower dead center to top dead centre, on piston
The volume of cylinder of side increases, and generates vacuum degree, and inner pressure of air cylinder drops to admission pressure hereinafter, under pull of vacuum effect, passes through
The gas flowmeter of accurate measurement is separately added into acetylene and oxygen, is mixed to form combustion mixture, by air intake duct and air inlet door-inhale
Enter in cylinder.Intake process continues up to until piston crossed top dead centre IC Intake Valve Closes.Open pneumatic pull rod handgrip, downlink
Piston through gravity, start compressed mixed gas.
Compression travel
Inlet and exhaust valve Close All, combustion mixture in compression ignition cylinder, mixture temperature increase, and pressure rises.Piston closes on
Before bottom dead center, combustion mixture pressure rises to 0.6~1.2MPa or so, and temperature causes gaseous mixture up to 430 DEG C~650 DEG C
Body detonation.
Stroke is reacted in detonation
When compression travel is close to lower dead center, cause mixed gas detonation, a large amount of heat is released after combustion mixture detonation
Amount, In-cylinder Combustion Pressure and temperature rise rapidly, and maximum combustion pressure is up to 3~8MPa, and maximum combustion temperature is up to 1500 DEG C
~3200 DEG C.High-temperature high-pressure fuel gas pushes piston quickly to be moved to top dead centre, and when expansion space stroke starts, inlet valve is turned off, row
What valve reason compression spring was adjusted, there is mechanical time delay to be converted from closing to open state.
Instroke
Expansion space stroke is close to when ending, the semi-open state of exhaust valve, due to shearing oxygen debt burning through detonation at this moment cylinder
Carbon black is partially converted to graphene, and in-cylinder pressure enters vacuum tank through exhaust safety valve, and after throttling, high-temp waste gas is discharged rapidly
, it can be achieved that fast cooling, this stage belong to the free exhaust stage, high-temp waste gas is discharged with velocity of sound by exhaust valve cylinder.With
Final vacuum process is crossed top dead centre and is moved to lower dead center into forced exhaust stage, piston is advanced into, and exhaust gas inside cylinder is discharged for pressure,
When piston is reached near lower dead center, exhaust process terminates, and completes a cycle.
Because acetylene is purified and high purity oxygen gas generates mixed gas, variable factor is few, can be started using four-cycle diesel
Machine is transformed into graphene production equipment, how to avoid the quick-fried mechanical damage of the shake of bent axle, just under study for action.
Further, since the moisture formation steam in vacuum tank, reacting generation takes away heat and generation throttle effect
The throttling action of equivalent Carnot cycle, the graphene that detonation reaction generates are cooled down rapidly, are tested obtaining as a result, high temperature and pressure
It is also easy to produce graphene, but is also easy to back fold and forms carbon dust or carbon distribution, the graphene yield that rapid cooling obtains is best.
Nano level graphene forms flying dust, is extracted through water-ring vacuum pump, the water of water-ring vacuum pump, is to be added to divide
Powders composition, the graphene in dispersant solution, it is not easy to occur back to fold, condition is provided (see figure for subsequent purifying technique
2)。
Further, when certain products, need low-grade graphene, can between vacuum tank and water-ring vacuum pump,
Low-melting-point resin graphene adsorption tower is added, this method may be implemented low cost and obtain graphene product (see Fig. 3).To push away early
Wide graphene application provides selection.
Description of the drawings
Fig. 1：Graphene compression ignition structure of reactor schematic diagram
1. 2. 3. gravity drop hammer 4. 5. 6. 7. fix air bleeding valve (safety valve) throttle pipe by sliding shaft sleeve for piston and connecting rod for compression ignition room
Holder 8. airlift grapple 9. pneumatic cylinder 10. vacuum graphite alkene collecting tank (and explosion-proof, sound insulation function)Intake valve
Fig. 2：Graphene collects figure
1. 2. 3. gravity drop hammer 4. 5. 6. 7. fix air bleeding valve (safety valve) throttle pipe by sliding shaft sleeve for piston and connecting rod for compression ignition room
Holder 8. airlift grapple 9. pneumatic cylinder 10. vacuum graphite alkene collecting tank (and explosion-proof, sound insulation function)Intake valveWater ring
Formula vacuum pumpUltrasonic activation plateDispersant solution pondAcetylene gas measuring instrumentOxygen gas measuring instrument
Fig. 3：Graphene resin adsorption products application schematic diagram
1. 2. 3. gravity drop hammer 4. 5. 6. 7. fix air bleeding valve (safety valve) throttle pipe by sliding shaft sleeve for piston and connecting rod for compression ignition room
Holder 8. airlift grapple 9. pneumatic cylinder 10. vacuum graphite alkene collecting tank (and explosion-proof, sound insulation function)Intake valveWater ring
Formula vacuum pumpUltrasonic activation plateDispersant solution pondAcetylene gas measuring instrumentOxygen gas measuring instrument
Low-temperature melting point resin graphene adsorption tower
The beneficial effects of the invention are as follows：
The present invention is volume production graphene preparation technology, a kind of graphene powder of low cost, is carried for graphene extensive use
For a kind of method prepared.The application of form the few-layer graphene alkene powder, although there is significant limitation, at present can volume production graphene life
Production technology, the number of plies of the invention is best, due to the growth course of two dimensional crystal be under suitable condition, by nucleation,
The present invention may provide a kind of one of material of nucleus for the volume production of large area form the few-layer graphene alkene film.
Specific implementation mode
To make technical scheme of the present invention and advantage be more clear, below technical solution in the present invention carry out it is clear, complete
Site preparation describes, and described embodiments are some of the embodiments of the present invention, instead of all the embodiments, based in the present invention
Embodiment, all embodiments that those of ordinary skill in the art are obtained under the premise of no creative work, belongs to this hair
Bright protection domain.
Embodiment 1：The operation principle of reciprocating piston internal combustion engine, the very close present invention, since the burning point of acetylene is low, directly
Connect will produce in the way of four stroke reciprocating piston internal combustion engine compression ignitions shake it is quick-fried, it is serious to mechanical damage, utilize the present invention pressure
Combustion mode and principle produce graphene, test best working condition, and improved four strokes compression-ignition engine can implement this
Invention steals the technical data of the present invention and manufactures graphene with the graphene preparation technology of the present invention, belongs to direct infringement.
The present invention due to compression ignition mode high temperature and high pressure condition and realize fast cooling, the advantages that technological process is short, can be with
Realize prepared by continuity output graphene.
Embodiment 2：Notice that the course of work of four-stroke gasoline engine is a complicated process, it is by air inlet, compression, combustion
Burn four expansion, exhaust stroke (stroke) compositions.
Suction stroke
It is moved by the downward top dead centre of top dead centre at this point, piston is driven by bent axle, meanwhile, IO Intake Valve Opens, exhaust valve closing.
When piston is moved from top dead centre to lower dead center, the volume above piston increases, and the gas pressure in cylinder declines, and is formed certain
Vacuum degree.Due to IO Intake Valve Opens, cylinder is communicated with air inlet pipe, and gaseous mixture is inhaled into cylinder.When piston is moved to lower dead center
When, incoming mixture and the undischarged exhaust gas of a upper working cycles are filled in cylinder.
Compression travel
Piston is moved to top dead centre by lower dead center, and inlet and exhaust valve is closed.Bent axle drives under the action of the inertia force such as flywheel
Rotation pushes piston to move up by connecting rod, and cylinder interior gas volume is gradually reduced, and gas is compressed, the mixing in cylinder
Atmospheric pressure is with temperature with raising.
Expansion space stroke
At this point, inlet and exhaust valve simultaneously closes off, plug ignition, gaseous mixture vigorous combustion, temperature, pressure in cylinder are drastically
Rise, high temperature, high pressure gas push piston to move down, and are rotated by connecting rod band dynamic crankshaft.In four rows of engine work
Cheng Zhong, only this just realize that thermal energy is converted into mechanical energy in stroke.
When power output shaftless using petrol engine, is run under the conditions of oxygen debt using acetylene, is used to prepare graphene,
The adjusting plug ignition time avoids shaking quick-fried mechanical damage, the utilization of this method, although cannot reach graphene prepares high temperature
The best applications condition of high pressure, but can also realize with this method and prepare graphene, but can be easy to generate carbon distribution and cause
Valve fails, and vacuum plant of the invention may be implemented the key equipment of decarbonizing, prepare graphene in this way, belongs to and invade
Violate the present invention.
Claims (7)
1. the method that compression ignition method prepares graphene is obtained through experiment, shelled using Physical under Detonation Shock Wave and high temperature and pressure
The process conditions to cool down from graphene and rapidly prepare graphene mechanism, it is characterised in that are：By compression-ignited reactor, graphene
Vacuum colletor, water-ring vacuum pump, throttling expansion pipe, pond, PLC program controller, acetylene purification facility, acetylene-oxygen meter
Measure the combinations such as instrument, ultrasonic wave vibration plate composition.
2. the method that compression ignition method according to claim 1 prepares graphene, it is characterised in that：It is anti-using the oxygen debt compression ignition of acetylene
The carbon source that should be generated, preferably acetylene are that graphene carbon source provides, including but not limited to fuel gas for example methane, ethane, propane,
Butane, ethylene, propylene, butylene etc. and methanol, ethyl alcohol, gasoline, the diesel oil etc. that can be used for compression ignition reaction.
3. the method that compression ignition method according to claim 1 prepares graphene, it is characterised in that：In compression ignition reactor, warp
Free gravity falling bodies compress mixed gas, reach when compression ratio is more than 10 and detonation occurs, different according to oxygen and acetylene accounting,
Compression ignition reaction temperature can be between 500 DEG C~3200 DEG C, and compression ignition blast pressure is between 1.2~8.0Mpa.Acetylene content
Between 2.0%~80.0% (vol), between oxygen content 2.0%~50.0% (vol).
4. the method that compression ignition method according to claim 1 prepares graphene, it is characterised in that：Gas explosion after compression ignition
Pressure, the temperature of compression ignition room can be set by the pressure of regulation safety valve and be adjusted, the height that compression ignition explosive force rebound piston returns to
Degree is arranged according to 20 times of gas expansion spaces, and second of falling is again started up safety valve unlatching, and promoting gravity by pneumatic pull rod lives
Plug, is returned to original state, meanwhile, secondary mixed gas sucking forms one cycle, similar four-stroke engine.Weight
Multiple four-stroke cycle keeps the operation of graphene continuous production.
5. the method that compression ignition method according to claim 1 prepares graphene, it is characterised in that：The vacuum graphite alkene of setting is received
Collect in tank, the moisture that compression ignition reaction that acetylene is oxygen debt generates, which forms steam and takes away heat and generate throttle effect, is equal to Carnot cycle
Throttling action, the graphene that detonation reaction generates cool down rapidly in vacuum graphite alkene collecting tank, and graphene is avoided to return folded and reunite,
Vacuum graphite alkene collecting tank is arranged simultaneously can be to avoid air bleeding valve carbon deposition phenomenon.Vacuum graphite alkene collecting tank is graphene volume production skill
The key equipment of art.
6. the method that compression ignition method according to claim 1 prepares graphene, it is characterised in that：Nano level graphene is formed
Flying dust is extracted through water-ring vacuum pump, the water of water-ring vacuum pump, is that dispersion. formulation is added, in dispersant solution
Graphene, it is not easy to folded phenomenon occur back, condition is provided for subsequent purifying technique.
7. the method that compression ignition method according to claim 1 prepares graphene, it is characterised in that：Utilize four stroke reciprocating-pistons
Formula internal combustion engine and using test data and vacuum avoid carbon distribution weakness be transformed after substitute compression ignition reactor, graphene can be met
Continuous production processes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020144710A1 (en) * | 2019-01-08 | 2020-07-16 | Indian Institute Of Technology Delhi | A method of preparation of reduced graphene oxide nanoparticles |
| CN112279241A (en) * | 2020-11-25 | 2021-01-29 | 德阳烯碳科技有限公司 | Rapid preparation method of low-layer-number small-size graphene |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103420361A (en) * | 2012-05-22 | 2013-12-04 | 海洋王照明科技股份有限公司 | A method of preparing graphene by explosion |
| US20140335010A1 (en) * | 2013-05-10 | 2014-11-13 | Kansas State University Research Foundation | Process for high-yield production of graphene via detonation of carbon-containing material |
| CN105752964A (en) * | 2016-01-25 | 2016-07-13 | 肖荣阁 | High-temperature high-pressure bursting method for producing graphene and equipment |
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2017
- 2017-02-06 CN CN201710077369.6A patent/CN108394890A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420361A (en) * | 2012-05-22 | 2013-12-04 | 海洋王照明科技股份有限公司 | A method of preparing graphene by explosion |
| US20140335010A1 (en) * | 2013-05-10 | 2014-11-13 | Kansas State University Research Foundation | Process for high-yield production of graphene via detonation of carbon-containing material |
| CN105752964A (en) * | 2016-01-25 | 2016-07-13 | 肖荣阁 | High-temperature high-pressure bursting method for producing graphene and equipment |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020144710A1 (en) * | 2019-01-08 | 2020-07-16 | Indian Institute Of Technology Delhi | A method of preparation of reduced graphene oxide nanoparticles |
| CN112279241A (en) * | 2020-11-25 | 2021-01-29 | 德阳烯碳科技有限公司 | Rapid preparation method of low-layer-number small-size graphene |
| CN112279241B (en) * | 2020-11-25 | 2022-04-12 | 德阳烯碳科技有限公司 | Rapid preparation method of low-layer-number small-size graphene |
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Application publication date: 20180814 |