CN108706576A - A kind of two level temperature control pneumatic process prepares graphene powder method and apparatus - Google Patents

A kind of two level temperature control pneumatic process prepares graphene powder method and apparatus Download PDF

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Publication number
CN108706576A
CN108706576A CN201810908031.5A CN201810908031A CN108706576A CN 108706576 A CN108706576 A CN 108706576A CN 201810908031 A CN201810908031 A CN 201810908031A CN 108706576 A CN108706576 A CN 108706576A
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China
Prior art keywords
temperature control
twin
level
graphene powder
spiral shell
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CN201810908031.5A
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Inventor
张静
曾丙炎
陈永标
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Hengli Fengtai (xiamen) Graphene Technology Co Ltd
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Hengli Fengtai (xiamen) Graphene Technology Co Ltd
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Priority to CN201810908031.5A priority Critical patent/CN108706576A/en
Publication of CN108706576A publication Critical patent/CN108706576A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • C01B32/19Preparation by exfoliation

Abstract

The invention belongs to graphene powder preparing technical fields, it discloses a kind of two level temperature control pneumatic process and prepares graphene powder method and apparatus, it is provided with twin-screw, feed inlet, first air inlet, second air inlet and air pressure sensing device, twin-screw back segment spiral shell block, third air inlet, twin-screw leading portion spiral shell block, level-one temperature control (including first heater), two level temperature control (including secondary heating mechanism, third heating device, 4th heating device, 5th heating device, 6th heating device, 7th heating device), cooling section, waste gas outlet, water inlet, water outlet, discharge port, chuck storage device, boiler tube, exhaust fan, filter screen.End of the present invention, which is equipped with cooling section, can reduce that raw material goes out the temperature of boiler tube and chuck storage device is equipped with cooling solution and can greatly reduce temperature, prevent because temperature of charge is excessively high lead to rewinding when ingress of air caused by product burn the phenomenon that, tail end connection scrubbing tower can reduce exhaust gas discharge.

Description

A kind of two level temperature control pneumatic process prepares graphene powder method and apparatus
Technical field
The invention belongs to graphene powder preparing technical fields more particularly to a kind of two level temperature control pneumatic process to prepare graphene Powder method and apparatus.
Background technology
Currently, the prior art commonly used in the trade is such:
Common small lot graphene powder apparatus for preparation is tube type high-temperature furnace, by being added graphene presoma into boiler tube In, certain temperature control program is set under inert gas protection, can be taken off obtaining graphite after completing to set heating cooling process Alkene powder.
Common tube type high-temperature furnace prepares graphene powder trivial operations, and each spent material is sent into and discharging is inconvenient, is needed Addition graphene presoma fixes two end connection devices again, and there is still a need for remove two end connection devices can will just expect after finally cooling down It takes out;
Tube type high-temperature furnace prepares graphene end and needs to access exhaust gas for handling exhaust gas in buck, in graphene forerunner Body expand when due to instantaneous pressure it is excessive, furnace body gas moment discharge after, in the body of road air pressure reduce rapidly, cause buck suck-back Phenomenon influences to test;
Tube type high-temperature furnace heats for interlude, and furnace body cannot be overturn, and uneven heating is even after the addition of graphene presoma, such as short Then products obtained therefrom is second-rate for time experiment, need prolonged high temperature just can guarantee obtained by graphene quality, and cooling rate compared with Slowly, researcher's more quality time is wasted.
High-volume graphene apparatus for preparation is rotary kiln, by kiln heating overturning so that graphene presoma moves simultaneously Expanded by heating is reduced into graphene, though it can produce in enormous quantities, products obtained therefrom unstable quality, and due to that can not observe in stove Mass expanded restores situation, and a large amount of graphene presoma is needed to be debugged for device parameter, and waste is larger.
In conclusion problem of the existing technology is:
Inconvenience is operated with for tube furnace;
Easily there is suck-back disadvantage, influences entire experiment effect;
Uneven heating is even after the addition of graphene presoma, and prolonged high-temperature expansion is needed just to can guarantee gained graphene matter Amount, and cooling rate is slower, wastes the more quality time;
Rotary kiln produces graphene products obtained therefrom unstable quality in enormous quantities, needs a large amount of graphene presoma for setting Standby parameter testing, waste are larger.
Solve the difficulty and meaning of above-mentioned technical problem:
Difficulty:The heated uniformity of material, the discharge of exhaust gas and processing, the observation of the heated variation phenomenon of material, product matter The stability of amount and effective device parameter of replacing in time reduce material waste.
Meaning:The stability for increasing product quality improves the production efficiency of graphene, and reducing production cost can increase simultaneously Add the research for graphene preparation method.
Invention content
In view of the problems of the existing technology, the present invention provides a kind of two level temperature control pneumatic processes to prepare graphene powder Equipment.Graphene oxide powder, which is sent into the equipment, in conjunction with Dual-screw feeding and two level temperature control pneumatic process principle makes production make Standby graphene technique is more convenient, process temperature control is uniformly heated, and restores products obtained therefrom better quality, and raising grinds life to graphene The monitoring power of production.
The invention is realized in this way a kind of two level temperature control pneumatic process prepares Graphene powder body method, before graphene Drive body be sent to level-one temperature controlled region, material is preheated, remove graphene presoma in partial moisture, and by inert gas with Certain pressure is sent into level-one temperature controlled region, and in level-one temperature controlled region, part intercalation enters graphite to inert gas under pressure In piece lamellar spacing;A low pressure temperature controlled region for being passed through two level is then proceeded to, gradually heating expansion, indifferent gas during heating Body also partly serves as expansion;Graphene presoma restores the carbon dioxide generated, water vapor gas in graphene film simultaneously Interlayer generates huge internal pressure force effect so that graphite flake layer is peeled away, and is most obtained and is obtained graphene powder eventually.
Another object of the present invention is to provide a kind of two level temperature control pneumatic process prepare Graphene powder body method equipment, according to It is secondary to be provided with:
Twin-screw leading portion spiral shell block, angle are 30 °~60 °;Speed and material for adjusting material are heated evenly;
First heater, set temperature are 60-120 DEG C, are preheated for material;
Secondary heating mechanism, set temperature are 120-320 DEG C, moisture content and residual solvent evaporation in material;
Third heating device, set temperature are 150-520 DEG C, and material starts high temperature reduction;
4th heating device, set temperature are 200-720 DEG C, improve material reduction effect;
5th heating device, set temperature are 200-1000 DEG C, ensure that material restores completely;
Twin-screw back segment spiral shell block, angle are 30 °~120 °;Speed and material for adjusting material are heated evenly;
6th heating device, set temperature are 200-1000 DEG C, ensure that material restores completely;
7th heating device, set temperature are 200-1000 DEG C, ensure that material restores completely;
Cooling section, surface are coated with the ceramics of High temperature resistant heat radiation paint;It is cooled down for material initial stage.
The chuck storage device that cooling section rear end is accepted, for carrying out material cooling.
Further, the twin-screw leading portion spiral shell block angle is 30 °~60 °.
Further, twin-screw back segment spiral shell block, angle are 60 °~90 °.
Further, twin-screw, twin-screw back segment spiral shell block, twin-screw leading portion spiral shell block be high temperature resistant, acidproof metal material or Person's nonmetallic materials;
The front upper part of the twin-screw leading portion spiral shell block is provided with feed inlet;The rear portion of the feed inlet is provided with the first air inlet; First air inlet leads to inert gas.
Further, the front upper part of the twin-screw back segment spiral shell block is provided with the second air inlet;Second air inlet is located at institute State the first air scoop aft of twin-screw leading portion spiral shell block;
The rear portion of 7th heating device is located at twin-screw back segment spiral shell block upper back and is equipped with third air inlet;
Second air inlet leads to inert gas mixed gas, including:One or both of nitrogen or argon gas mix, and The volume ratio of hydrogen mixing is 92-98: 2-8.
Further, the twin-screw is sleeved on inside boiler tube;
The side of the chuck storage device is provided with water inlet, and the other side is provided with water outlet;The water outlet connection washing Tower;
It is provided with waste gas outlet at the top of the chuck storage device;The waste gas outlet is connected to scrubbing tower;The chuck storage The bottom of material device is provided with discharge port.
In conclusion advantages of the present invention and good effect are:
Be compared with the prior art the present invention has by design improvement laboratory tube furnace apparatus production graphene powder equipment Following advantages:
(1) it is more convenient to prepare graphene by screw design, and screw flight spiral shell block can be designed so that raw material rolls Batch mixing so that raw material is heated evenly products obtained therefrom better quality, and raw material can be controlled and add by controlling spiral shell block angle and screw speed The hot time;
(2) compartment heating can observe raw material in each temperature section cosmetic variation, facilitate quality control;
(3) end is equipped with cooling section and chuck storage device is equipped with cooling water and can greatly reduce material temperature;It reduces former Expect take-off time, and then reduces experimental period;
(4) exhaust gas discharge is passed through the kind sour gas that soda lye wash tower can be effectively treated in tail gas
(5) tube furnace high temperature reduction graphene presoma is used, the required recovery time is long, inconvenient for operation, with tubular type height Warm stove comparison, the recovery time of the invention is few, is heated evenly, easy to operate, greatly increases the production efficiency and produce quality.
Description of the drawings
Fig. 1 is the device systems signal that two level temperature control pneumatic process provided in an embodiment of the present invention prepares Graphene powder body method Figure.
In figure:1, twin-screw;2, twin-screw leading portion spiral shell block;3, first heater;4, secondary heating mechanism;5, third adds Thermal;6, the 4th heating device;7, the 5th heating device;8, the 6th heating device;9, the 7th heating device;10, cooling section; 11, water inlet;12, chuck section;13, storage device;14, discharge port;15, discharge outlet;16, waste gas outlet;17, exhaust fan;18, Filter screen;19, third air inlet;20, twin-screw back segment spiral shell block;21, boiler tube;22, the second air inlet;23 first air inlets;24, Feed inlet.
Fig. 2 is that two level temperature control pneumatic process provided in an embodiment of the present invention prepares graphene powder method schematic.
Specific implementation mode
In order to further understand the content, features and effects of the present invention, the following examples are hereby given, and coordinate attached drawing Detailed description are as follows.
The present invention can easily continuous production graphene, and end setting cooling section can reduce the temperature of product, if Chuck storage device is counted, chuck internal layer, which leads to alkaline solution, can play cooling effect, and water outlet is connected to Waste gas outlet and washes The sedimentation of solid particle in the sour gas in removing exhaust gas and exhaust gas can be gone by washing tower.
Two level temperature control pneumatic process provided in an embodiment of the present invention prepares Graphene powder body method, is sent by graphene presoma Enter to level-one temperature controlled region, material is preheated, removes partial moisture in graphene presoma, and by inert gas with certain Pressure is sent into level-one temperature controlled region, and inert gas is between in level-one temperature controlled region, part intercalation enters graphite flake layer under pressure In gap;A low pressure temperature controlled region for being passed through two level is then proceeded to, gradually heating expansion, inert gas also portion during heating Divide and serves as expansion;Carbon dioxide, the water vapor gas of the generation of graphene presoma reduction simultaneously are produced in graphene film interlayer Raw huge internal pressure force effect so that graphite flake layer is peeled away, and is most obtained and is obtained graphene powder eventually.Such as Fig. 2.
As shown in Figure 1, the equipment that two level temperature control pneumatic process provided in an embodiment of the present invention prepares Graphene powder body method, packet It includes:
Twin-screw 1;Twin-screw leading portion spiral shell block 2;First heater 3;Secondary heating mechanism 4;Third heating device 5;The Four heating devices 6;5th heating device 7;6th heating device 8;7th heating device 9;Cooling section 10;Water inlet 11;Chuck Section 12;Storage device 13;Discharge port 14;Discharge outlet 15;Waste gas outlet 16;Exhaust fan 17;Filter screen 18;Third air inlet 19; Twin-screw back segment spiral shell block 20;Boiler tube 21;Second air inlet 22;First air inlet 23;Feed inlet 24.
The end of twin-screw 1 is set with cooling section 10;
The cooling section rear end undertakes storage device 13.
The front upper part of the twin-screw leading portion spiral shell block 2 is provided with feed inlet 24;The rear portion of the feed inlet is provided with the first air inlet Mouth 23;
The rear sleeve of the twin-screw leading portion spiral shell block 2 is equipped with first heater 3.
The front upper part of the twin-screw back segment spiral shell block 19 is provided with the second air inlet 22;Second air inlet 22 is located at described 23 rear portion of the first air inlet of twin-screw leading portion spiral shell block;
The multistage heating device includes:
Level-one temperature control device includes:First heater 3, two level temperature control device include:Secondary heating mechanism 4, third add Thermal 5, the 4th heating device 6, the 5th heating device 7, the 6th heating device 8, the 7th heating device 9 are simultaneously sleeved on stove successively Guan Shang;
The rear portion of 7th heating device 9 is provided with the third air inlet 19 positioned at twin-screw back segment spiral shell block upper back.
The twin-screw is sleeved on inside boiler tube 21;
The chuck section side of the storage device is provided with water inlet, and the other side is provided with water outlet;The water outlet connection is washed Wash tower;
It is provided with waste gas outlet at the top of the storage device;The waste gas outlet is connected to scrubbing tower;
The bottom of the storage device is provided with discharge port 14.
With reference to operation principle, the invention will be further described.
Graphene presoma is entered by feed inlet 24 in boiler tube 21, is moved backward by twin-screw 1;By setting twin-screw The speed of spiral shell block angle adjustable material and being heated evenly for material of leading portion spiral shell block 2 and twin-screw back segment spiral shell block 20;The One air inlet 23 and third air inlet 19 are passed through inert gas, and the second air inlet 22 is passed through inert gas or inert gas and hydrogen The mixed gas of gas;Material passes through 3 pre-add heat abstraction department volatile substances of first heater;Add again by the second of setting The bringing-up section of thermal 4 to 9 temperature of the 7th heating device carries out high temperature reduction, and material carries out initial stage by cooling section 10 after reduction Cooling, last material enters jacketed section of storage device and is cooled down, and material is discharged by reserved discharge port 14 after cooling, whole Generated exhaust gas is connected to scrubbing tower processing by waste gas outlet 16 and discharge outlet 15.
Twin-screw 1, twin-screw back segment spiral shell block 20, twin-screw leading portion spiral shell block 2 be high temperature resistant, acidproof nonmetallic materials, it is excellent It is selected as high temperature ceramic material;
First air inlet 23, third air inlet 19 lead to inert gas, and preferably nitrogen or argon gas is one or two kinds of mixed It closes;
Second air inlet 22 leads to inert gas mixed gas, preferably nitrogen hydrogen mixeding gas (96: 4) or argon hydrogen gaseous mixture Body (96: 4);
Twin-screw leading portion spiral shell block 2, spiral shell block design angle be 30-60 °, preferably 50-60 °, twin-screw back segment spiral shell block 20, spiral shell Block design angle be 30-120, preferably 80-90 °;
Solution used in water inlet 11 is alkaline aqueous solution, the preferably sodium hydrate aqueous solution of 10% mass fraction;
The set temperature of first heater 3 is 60-120 DEG C, and the set temperature of secondary heating mechanism 4 is 120-320 DEG C, The set temperature of third heating device 5 is 150-520 DEG C, and the set temperature of the 4th heating device 6 is 200-720 DEG C, slender acanthopanax The set temperature of thermal 7 is 200-1000 DEG C, and the set temperature of the 6th heating device 8 is 200-1000 DEG C, the 7th heating dress The set temperature for setting 9 is 200-1000 DEG C,
Surface carried out by cooling section 10 is coated with the ceramics of High temperature resistant heat radiation paint;
Boiler tube 21 is resistance to high, acidproof metal or nonmetallic materials, the preferably transparency silica glass of high temperature-resistant acid-resistant Material.
The above is only the preferred embodiments of the present invention, and is not intended to limit the present invention in any form, Every any simple modification made to the above embodiment according to the technical essence of the invention, equivalent variations and modification, belong to In the range of technical solution of the present invention.

Claims (10)

1. a kind of two level temperature control pneumatic process prepares Graphene powder body method, which is characterized in that prepared by the two level temperature control pneumatic process Graphene powder body method includes:It is sent to level-one temperature controlled region by graphene presoma, material is preheated, removes graphene Partial moisture in presoma, and inert gas is sent into level-one temperature controlled region with certain pressure, inert gas is in level-one temperature controlled region Part intercalation enters in graphite flake layer gap under pressure;A low pressure temperature controlled region for being passed through two level is then proceeded to, Gradually heating expansion, inert gas also partly serves as expansion during heating;Graphene presoma also originates in simultaneously Raw carbon dioxide, water vapor gas generate huge internal pressure force effect in graphene film interlayer so that and graphite flake layer is peeled away, It most obtains and obtains graphene powder eventually.
2. a kind of equipment that two level temperature control pneumatic process as described in claim 1 prepares Graphene powder body method, which is characterized in that institute The equipment that two level temperature control pneumatic process prepares Graphene powder body method is stated to be disposed with:
Twin-screw leading portion spiral shell block, angle are 30 °~60 °;Speed and material for adjusting material are heated evenly;
Level-one temperature control first heater, set temperature are 60-120 DEG C, are preheated for material;
Two level temperature control secondary heating mechanism, set temperature are 120-320 DEG C, moisture content and residual solvent evaporation in material;
Two level temperature control third heating device, set temperature are 150-520 DEG C, and material starts high temperature reduction;
The 4th heating device of two level temperature control, set temperature are 200-720 DEG C, improve material reduction effect;
The 5th heating device of two level temperature control, set temperature are 200-1000 DEG C, ensure that material restores completely;
Twin-screw back segment spiral shell block, angle are 30 °~120 °;Speed and material for adjusting material are heated evenly;
The 6th heating device of two level temperature control, set temperature are 200-1000 DEG C, ensure that material restores completely;
The 7th heating device of two level temperature control, set temperature are 200-1000 DEG C, ensure that material restores completely;
Cooling section, surface are coated with the ceramics of High temperature resistant heat radiation paint;It is cooled down for material initial stage;
The chuck storage device that cooling section rear end is accepted, for carrying out material cooling.
3. the equipment that two level temperature control pneumatic process as claimed in claim 2 prepares Graphene powder body method, which is characterized in that described Twin-screw leading portion spiral shell block angle is 30 °~60 °.
4. the equipment that two level temperature control pneumatic process as claimed in claim 2 prepares Graphene powder body method, which is characterized in that double spiral shells Bar back segment spiral shell block, angle are 60 °~90 °.
5. the equipment that two level temperature control pneumatic process as claimed in claim 2 prepares Graphene powder body method, which is characterized in that
Twin-screw, twin-screw back segment spiral shell block, twin-screw leading portion spiral shell block are high temperature resistant, acidproof metal material or nonmetallic materials;
The front upper part of the twin-screw leading portion spiral shell block is provided with feed inlet;The rear portion of the feed inlet is provided with the first air inlet;First Air inlet leads to inert gas.
6. the equipment that two level temperature control pneumatic process as claimed in claim 2 prepares Graphene powder body method, which is characterized in that
The front upper part of the twin-screw back segment spiral shell block is provided with the second air inlet;Second air inlet is located at the twin-screw leading portion First air scoop aft of spiral shell block;
The rear portion of 7th heating device is located at twin-screw back segment spiral shell block upper back and is equipped with third air inlet,;
Second air inlet leads to the mixed gas of inert gas and hydrogen, and third air inlet leads to inert gas.
7. the equipment that two level temperature control pneumatic process as claimed in claim 2 prepares Graphene powder body method, which is characterized in that
The twin-screw is sleeved on inside boiler tube;
The side of the chuck storage device is provided with water inlet, and the other side is provided with water outlet;The water outlet is connected to scrubbing tower;
It is provided with waste gas outlet at the top of the chuck storage device;The waste gas outlet is connected to scrubbing tower;
The bottom of the chuck storage device is provided with discharge port.
8. the equipment that two level temperature control pneumatic process as claimed in claim 2 prepares Graphene powder body method, which is characterized in that described The boiler tube that uses of equipment be heat safe transparent quartz glass tube material.
9. the equipment that two level temperature control pneumatic process as claimed in claim 5 prepares Graphene powder body method, which is characterized in that described The inert gas of the first air inlet be nitrogen, the mixing of one or both of argon gas.
10. the equipment that two level temperature control pneumatic process as claimed in claim 6 prepares Graphene powder body method, which is characterized in that institute The inert gas for the second air inlet stated is the mixing of one or both of nitrogen, argon gas mixed gas and hydrogen, indifferent gas The volume ratio of body and hydrogen is 90-98: 2-10, and the inert gas of third air inlet is that one or both of nitrogen, argon gas are mixed It closes.
CN201810908031.5A 2018-08-10 2018-08-10 A kind of two level temperature control pneumatic process prepares graphene powder method and apparatus Pending CN108706576A (en)

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CN109579517A (en) * 2019-01-21 2019-04-05 南京工程学院 A kind of screw propulsion atmosphere sintering furnace producing ternary lithium electric material
CN112010293A (en) * 2020-09-09 2020-12-01 宁波益德新材料有限公司 Graphene double-cylinder linkage equipment
CN115448302A (en) * 2022-09-29 2022-12-09 深圳烯材科技有限公司 Method for preparing graphene oxide through continuous electrolysis based on pressure regulation

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CN115448302A (en) * 2022-09-29 2022-12-09 深圳烯材科技有限公司 Method for preparing graphene oxide through continuous electrolysis based on pressure regulation
CN115448302B (en) * 2022-09-29 2023-07-21 深圳烯材科技有限公司 Method for preparing graphene oxide based on pressure regulation and continuous electrolysis

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Application publication date: 20181026