CN105731423B - The integrated apparatus and method of a kind of pyrolysis of coal generation CNT - Google Patents
The integrated apparatus and method of a kind of pyrolysis of coal generation CNT Download PDFInfo
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- CN105731423B CN105731423B CN201610061512.8A CN201610061512A CN105731423B CN 105731423 B CN105731423 B CN 105731423B CN 201610061512 A CN201610061512 A CN 201610061512A CN 105731423 B CN105731423 B CN 105731423B
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Abstract
The invention discloses a kind of integrated apparatus of pyrolysis of coal generation CNT and method.The integrated apparatus body interior is sequentially provided with pyrolysis of coal unit, heating unit, synthesis unit from inside to outside, pyrolysis of coal unit unstrpped gas for needed for synthesis unit provides synthesis, the unstrpped gas that the methane gas of pyrolysis of coal unit generation is synthesized as CNT, is directly used in the synthesis of CNT；Heating unit provides heat to pyrolysis of coal unit and carbon nanotube synthesizing unit simultaneously by combustion fuel gas.The present invention being capable of continuous synthesizing carbon nanotubes；Meanwhile, the single waste that heat is provided to synthesis unit before having saved, it is ensured that the continuous production of device；Raw material is evenly distributed in reaction member in synthesis unit entrance so that catalyst is uniformly mixed with reacting gas, it is ensured that the homogenization of CNT quality.
Description
Technical field
The present invention relates to a kind of integrated apparatus of pyrolysis of coal generation CNT and method, belong to coal chemical technology neck
Domain.
Background technology
CNT is lightweight as monodimension nanometer material, and hexagonal structure connection is perfect, with many abnormal power
, electricity and chemical property.The preparation method of common CNT has：Graphite acr method, catalystic pyrolysis, laser steaming process
With others pyrolysis polymerization, ionizing radiation method, flame method, plasma method and newest method of swimming, hydro-thermal method, solid-phase thermal
Solution, gas-phase reaction method etc..
Although the preparation method for preparing CNT is a lot, the method for being used for largely preparing CNT only has graphite
Arc process, catalystic pyrolysis, other method have the shortcomings that very big and are not used to industrially prepared.
The principle that catalystic pyrolysis prepares CNT is by hydro carbons（Such as methane, ethene, propylene and benzene）Or contain
Oxycarbide is cracked in the presence of catalyst and formed.Catalyst choice it is more be transition metal etc..Make under the same conditions
Standby catalyst and synthesizing carbon nanotubes, metal composition are different, and the activity of prepared catalyst is also different.Carbon source mainly selects second
Alkynes, methane, CO, ethene, propylene, butylene, benzene and normal butane etc..It is also different in the structure and performance of synthesizing carbon nanotubes.
At present, the unstrpped gas in actual production used in synthesizing carbon nanotubes is mainly methane, carbon monoxide and benzene, and this
A little unstrpped gases are also mainly derived from natural gas and oil gas.Comparatively, the transport of these unstripped gas is also a part
Huge investment, and the pyrogenous origin methane of coal can be as the unstripped gas needed for direct synthesizing carbon nanotubes.Such one
Aspect can obtain higher income using the cheap price of coal, while also having huge promotion to the Transformation Development of coal
Effect.
The content of the invention
The present invention is intended to provide the integrated apparatus and method of a kind of pyrolysis of coal generation CNT, pyrolysis of coal is produced
Gas is directly used in synthesizing carbon nanotubes, being capable of continuous synthesizing carbon nanotubes；Concurrently there are in carbon nanotube synthesizing unit and
Heating unit between pyrolysis of coal unit can provide heat to two reaction members simultaneously, single to synthesis before having saved
Unit provides the waste of heat, also can guarantee that the continuous production of device.
The invention provides the integrated apparatus that a kind of pyrolysis of coal generates CNT, it is characterised in that：The integration
Apparatus main body is cylindrical structure, it is upper and lower be respectively truncated cone-shaped structure, cylindrical inside be sequentially provided with from inside to outside pyrolysis of coal unit,
Heating unit, synthesis unit；Pyrolysis of coal unit unstrpped gas for needed for synthesis unit provides synthesis, the first of pyrolysis of coal unit generation
The unstrpped gas that alkane gas is synthesized as CNT, is directly used in the synthesis of CNT；Heating unit passes through burning fuel
Gas provides heat to pyrolysis of coal unit and carbon nanotube synthesizing unit simultaneously, by controlling fuel gas to enter each heat supply list
The flow velocity of first layer provides the heat needed for pyrolysis of coal unit and carbon nanotube synthesizing unit；
The pyrolysis of coal unit is cylindrical structure, and top connects coal-supplying pipe, and bottom is provided with coke discharge pipeline；Pyrolysis of coal
The cylindrical wall on unit top is provided with uniform steam vent, the exhaust that the unstrpped gas that pyrolysis of coal unit is produced passes through top
Hole enters synthesis unit；
The heating unit is double-layer circular tubular, and inside and outside layer bottom of cylinder connects fuel gas pipeline respectively, and inner layer cylinder is
Internal layer is heated, outer layer cylinder is heating outer layer, and heating unit is enclosed on the outside of pyrolysis of coal unit, and heating internal layer connects with pyrolysis of coal unit
Touch and heat supply, heating outer layer is contacted and heat supply with the synthesis unit of CNT；
It is respectively equipped with the top of integrated apparatus at the top of catalyst inlet and inert gas entrance, synthesis unit and is provided with raw material
Distribution grid, distribution grid is a Circular Plate, and coal-supplying pipe is passed through from the center of distribution grid, and hole is uniformly provided with distribution grid, and synthesis is single
First bottom is provided with the opening and closing of Valve controlling floss hole.
In said apparatus, blender is provided with below the distribution grid.Blender be an agitating device, the agitating device be with
It is centered on one cylinder axis and multiple located at the axial blade of cylinder.Raw material can be uniformly dispersed in by the rotation of blade
The inside of synthesis unit.The number of blender can be set according to specific device size, it is ensured that can be by unstripped gas and catalysis
Agent is evenly distributed in synthesis unit.
In said apparatus, metallic rod is vertically provided with the synthesis unit, synthesis carbon is scribbled above metallic rod shaped object and is received
Metallic catalyst needed for mitron.Further, the metallic rod is provided with the device that can be moved up and down, and the device is a metal
Disk is enclosed in metallic rod, and the outside of disk is zigzag, rosette respectively with steel wire rope and motor connection, during by setting
Between, move up and down once, the CNT accumulated in metallic rod can be cleared up per disk every other hour, anti-locking apparatus
Block.
In said apparatus, cyclone separator is provided with the synthesis unit connecting carbon nanotube outlet, passes through carbon nanometer
The cyclone separator point that CNT and metallic catalyst are passed through cylindrical structure shape by the difference of pipe and metallic catalyst density
Open, the catalyst after separation is recycled.
The invention provides a kind of method that pyrolysis of coal generates CNT, using above-mentioned integrated apparatus, including it is following
Step：
（1）Coal-supplying pipe provides the coal dust that particle size diameter is 0-3cm, then provides fuel gas to coal heat to heating unit
Solution unit is heated, and temperature is reached 600 DEG C to 1200 DEG C；The unstrpped gas that pyrolysis of coal unit is produced passes through on coal supply unit
Portion enters synthesis unit；
（2）Heating unit is heated, when temperature reaches 650 DEG C to 1000 DEG C, catalyst and inert gas led to
The top that distribution grid enters synthesis unit is crossed, is entered together after the blended device mixing of the unstrpped gas then produced again with pyrolysis of coal
Synthesis unit；The catalyst that is floated in reacting gas and gas and and the catalysis that is arranged in the metallic rod inside synthesis unit
Agent is reacted and generates CNT；Air supply unit serialization is supplied；
（3）When it is about 5cm CNT that thickness is have accumulated in metallic rod, moving up and down on shaft is arranged at
Device will be moved up and down, and the CNT that will build up on is cleared up, and the CNT of synthesis just drops in synthesis unit together
The conical lower portion of bottom；When conical lower portion have accumulated the CNT that thickness is 20-30cm, the valve of its underpart can be received in carbon
Opened under mitron Action of Gravity Field, outside the CNT discharger that will build up on by floss hole, it is ensured that the continuous production of device；
（4）The metallic catalyst being mixed with CNT, which is separated catalyst by catalyst separation device, to be recycled to
Catalyst inlet is reused.
In the above method, the catalyst can be the metallic vapour for metal dust or evaporation, or contain magnetisable material
Organo-metallic compound.Further, the metallic element is any of iron, cobalt, nickel, molybdenum.The catalyst is gold
Belong to powder or the metallic vapour of evaporation, or the organo-metallic compound containing magnetisable material.
The apparatus and method that the present invention is provided, the beneficial effect brought：
（1）Inner most pyrolysis of coal unit can be continuously provided to carbon nanotube synthesizing unit needed for synthesizing carbon nanotubes
Unstrpped gas.The unstrpped gas that pyrolysis of coal is produced ensure that the continuous production of carbon nanotube synthesizing unit.
（2）Internal heating unit can provide heat, heating to pyrolysis of coal unit and carbon nanotube synthesizing unit simultaneously
Unit can be divided into two parts, realize that CNT synthesis is single by adjusting fuel gas into the speed of each heating unit
The temperature requirements of member and pyrolysis of coal unit.
（3）Install to have in the metallic rod for scribbling catalyst, metallic rod in the inside of apparatus for synthesizing carbon nanotubes and moved down on one
Dynamic device timely can clear up the CNT synthesized on the position, realize the continuous metaplasia of CNT
Production.
（4）It is uniform porous distribution located at the unstrpped gas on synthesis unit top and the distribution grid of metallic catalyst
Mixed unstrpped gas and metallic catalyst, can be dispersed in inside synthesis unit, so as to improve combined coefficient by plate.
Brief description of the drawings
Fig. 1 is the structural representation that pyrolysis of coal of the present invention generates CNT integrated apparatus.
Fig. 2 is the sectional view that pyrolysis of coal of the present invention generates CNT integrated apparatus.
Fig. 3 is the distribution grid schematic diagram that catalyst and inert gas enter reaction member.
1 is pyrolysis of coal unit in figure, and 2 be heating unit, and 2a is heating internal layer, and 2b is heating outer layer, and 3 be synthesis unit, 4
It is catalyst inlet for coal-supplying pipe, 5,6 be inert gas entrance, and 7 be coke discharge pipeline, and 8 be floss hole, and 9 be metallic rod,
10 device to move up and down, 11 be blender, and 12 be distribution grid.
Embodiment
The present invention is further illustrated below by embodiment, but is not limited to following examples.
Embodiment：
As shown in Fig. 1 ~ 3, a kind of pyrolysis of coal generates the integrated apparatus of CNT, and apparatus main body is cylindrical structure, upper,
It is respectively truncated cone-shaped structure down, cylindrical inside is sequentially provided with pyrolysis of coal unit 1, heating unit 2, synthesis unit 3 from inside to outside；Coal
The unstrpped gas for needed for synthesis unit 3 provides synthesis of pyrolysis unit 1, the methane gas that pyrolysis of coal unit 1 is generated is used as carbon nanometer
The unstrpped gas of pipe synthesis, is directly used in the synthesis of CNT；Heating unit 2 is by combustion fuel gas simultaneously to pyrolysis of coal
Unit 1 and carbon nanotube synthesizing unit 3 provide heat, are carried by controlling fuel gas to enter the flow velocity of each heating unit layer
Heat needed for coal supply pyrolysis unit 1 and carbon nanotube synthesizing unit 3；
The pyrolysis of coal unit 1 is cylindrical structure, and top connects coal-supplying pipe 4, and bottom is provided with coke discharge pipeline 7；Coal
The cylindrical wall on pyrolysis unit top is provided with uniform steam vent, and the unstrpped gas that pyrolysis of coal unit is produced passes through top
Steam vent enters synthesis unit；
The heating unit 2 is double-layer circular tubular, and inside and outside layer bottom of cylinder connects fuel gas pipeline, inner layer cylinder respectively
For heating internal layer 2a, outer layer cylinder is heating outer layer 2b, and heating unit 2 is enclosed on the outside of pyrolysis of coal unit 1, heating internal layer 2a and coal
The contact of pyrolysis unit 1 and heat supply, heating outer layer 2b are contacted and heat supply with the synthesis unit 3 of CNT；
It is respectively equipped with the top of integrated apparatus at the top of catalyst inlet 5 and inert gas entrance 6, synthesis unit provided with original
Expect distribution grid 12, distribution grid is a Circular Plate, and the center of coal-supplying pipe 4 from distribution grid 12 passes through, is uniformly provided with distribution grid 12
Hole, the bottom of synthesis unit 3 is provided with the opening and closing of Valve controlling floss hole 8.
In said apparatus, the lower section of distribution grid 12 is provided with blender 11.Blender is an agitating device, the agitating device
It is centered on a cylinder axis and multiple located at the axial blade of cylinder.Raw material can uniformly be divided by the rotation of blade
It is dispersed in the inside of synthesis unit.The number of blender can be set according to specific device size, it is ensured that can by unstripped gas and
Catalyst is evenly distributed in synthesis unit.
In said apparatus, metallic rod 9 is vertically provided with the synthesis unit 3, metal bar surface scribbles synthesizing carbon nanotubes
Required metallic catalyst.Further, the metallic rod 9 is provided with the device 10 that can be moved up and down, and the device is a metal
Disk is enclosed in metallic rod, and the outside of disk is zigzag, rosette respectively with steel wire rope and motor connection, during by setting
Between, move up and down once, the CNT accumulated in metallic rod can be cleared up per disk every other hour, anti-locking apparatus
Block.
In said apparatus, cyclone separator is provided with the synthesis unit connecting carbon nanotube outlet（Do not show in figure
Go out）, CNT and metallic catalyst are passed through by cylindrical structure shape by the difference of CNT and metallic catalyst density
Cyclone separator separate, by after separation catalyst recycle.
The operation principle of the present invention：
（1）Pyrolysis of coal unit is in the bosom of whole device, the coal of crushing from coal-supplying pipe enters pyrolysis of coal unit,
The speed for controlling fuel gas to enter heating unit by flow control valve arrives to set the temperature of pyrolysis of coal unit at 600 DEG C
Between 1200 DEG C.Coal isolation air separation, the appropriate pressure of control pyrolysis of coal unit under conditions of heating unit provides heat
And temperature, the production rate of unstrpped gas methane needed for improving CNT synthesis.The gas that pyrolysis of coal is produced is through pyrolysis unit
Pyrolysis of coal unit is discharged on top, and the coke that pyrolysis of coal is produced then is discharged by the coke discharge pipeline of the unit bottom.
（2）Heating unit is located at the middle part of synthesis unit and pyrolysis of coal unit, and heating unit is divided into inside and outside two layers, passed through
Control enters the speed of heating unit fuel gas to control the technological temperature needed for synthesis unit synthesizing carbon nanotubes, and coal is warm
The temperature of unit is solved between 600 DEG C to 1200 DEG C.
（3）Metallic catalyst and inert gas can first pass through a distribution grid, will be catalyzed when entering synthesis unit top
Agent and inert gas are evenly distributed in synthesis unit, and the outer wall of synthesis unit is made up of heat proof material such as quartz or graphite.
Catalyst is powder or the metal of evaporation, and it is preferably the Organometallic compounds containing magnetic material such as iron, cobalt, nickel, molybdenum
Thing.Fig. 3 is the horizontal cross of distribution grid, and the distribution grid is every 10 ° centered on the center of circle and a row diameter is provided with distribution grid
Size identical circular hole, the diameter of circular hole can be changed according to specific output, be adjusted by adjusting the diameter of circular hole
Unstrpped gas and catalyst enter the speed of synthesis unit, can also adjust the stream of gas by changing the distribution density of circular hole
Amount, it is ensured that metallic catalyst and inert gas, which can equably divide, to be sprinkling upon in synthesis unit.
（4）Unstrpped gas enters synthesis together after the top of synthesis unit and the mixing of metallic catalyst and inert gas
Unit, in order that unstrpped gas and metallic catalyst mixing are more abundant, can enter the blender of upper design one of synthesis unit,
Meanwhile, gas pump and flow control valve can be installed before synthesis unit is entered to control inert gas and metallic catalyst to enter
The speed of synthesis unit.
（5）Enter synthesis unit after unstrpped gas and the metallic catalyst mixing come out from pyrolysis of coal unit, into conjunction
Scribble and synthesized in the metallic rod of metallic catalyst in synthesis unit into the unstrpped gas part of unit, in metallic rod on move down
Dynamic device in time can clear up CNT above, the blocking of anti-locking apparatus.In addition, as shown in Fig. 2 synthesis is single
Be formed as to the lower tilt of member 130 cone, the CNT of synthesis can be gathered in the bottom of cone.Meanwhile,
Being gathered in the catalyst of synthesis unit bottom can also clear in time, and circulation makes again after being separated by cyclone separator
With.
In addition, according to shape, density, the size of the type of catalyst, that is, catalyst, adjustment inert gas and catalysis
The flow velocity of agent.
The method that pyrolysis of coal of the present invention generates CNT is illustrated below.
First, coal-supplying pipe provides the coal dust that particle size diameter is 0-3cm, then provides fuel gas to coal to heating unit
Pyrolysis unit is heated, and temperature is reached 600 DEG C to 1200 DEG C.The unstrpped gas that pyrolysis of coal unit is produced passes through coal supply unit
Top enters synthesis unit.
Then, heating unit is heated, when temperature reaches 650 DEG C to 1000 DEG C, by catalyst and inert gas
Enter the top of synthesis unit by distribution grid, the unstrpped gas then produced again with pyrolysis of coal（Methane）After blended device mixing
Enter synthesis unit together.The catalyst that is floated in reacting gas and gas and and it is arranged inside synthesis unit and scribbles gold
Catalyst on the bar of metal catalyst is reacted and generates CNT.
When it is about 5cm CNT that thickness is have accumulated in metallic rod, it is arranged on shaft and moves up and down dress
Putting to be moved up and down, and the CNT that will build up on is cleared up, and the CNT of synthesis just drops under synthesis unit together
The conical lower portion in portion.When conical lower portion have accumulated the CNT that thickness is 20-30cm, the valve of its underpart is in CNT
Opened under Action of Gravity Field, outside the CNT discharger that will build up on by floss hole, it is ensured that the continuous production of device.
Catalyst can be separated to be recycled to and urged by the metallic catalyst being mixed with CNT by cyclone separator
Agent input port is reused.
Claims (8)
1. a kind of pyrolysis of coal generates the integrated apparatus of CNT, it is characterised in that：The integrated apparatus main body is cylinder
Structure, upper and lower is respectively truncated cone-shaped structure, and cylindrical inside is sequentially provided with pyrolysis of coal unit, heating unit, synthesis list from inside to outside
Member, the pyrolysis of coal unit is cylindrical structure, and top connects coal-supplying pipe, and bottom is provided with coke discharge pipeline, pyrolysis of coal unit
The cylindrical wall on top is provided with uniform steam vent, and the unstrpped gas that pyrolysis of coal unit is produced is entered by the steam vent on top
Enter synthesis unit；
The heating unit is double-layer circular tubular, and inside and outside layer bottom of cylinder connects fuel gas pipeline respectively, and inner layer cylinder is heating
Internal layer, outer layer cylinder is heating outer layer, and heating unit is enclosed on the outside of pyrolysis of coal unit, and heating internal layer is contacted simultaneously with pyrolysis of coal unit
Heat supply, heating outer layer is contacted and heat supply with the synthesis unit of CNT；Catalyst is respectively equipped with the top of integrated apparatus to enter
Mouthful and inert gas entrance, be provided with feed distribution plate at the top of synthesis unit, distribution grid is a Circular Plate, coal-supplying pipe is from distribution grid
Center pass through, be uniformly provided with hole on distribution grid, blender be provided with below distribution grid；Arranged provided with Valve controlling synthesis unit bottom
Put the opening and closing of mouth；
Metallic rod is vertically provided with synthesis unit, the metallic rod is provided with the device that can be moved up and down, and the device is a metal
Disk is enclosed in metallic rod.
2. pyrolysis of coal according to claim 1 generates the integrated apparatus of CNT, it is characterised in that：The blender
For an agitating device, the agitating device is centered on a cylinder axis and multiple located at the axial blade of cylinder, passes through blade
Rotation raw material is uniformly dispersed in the inside of synthesis unit；The number of blender is set according to specific device size,
Guarantee unstripped gas and catalyst being evenly distributed in synthesis unit.
3. pyrolysis of coal according to claim 1 generates the integrated apparatus of CNT, it is characterised in that：The metallic rod
The metallic catalyst needed for synthesizing carbon nanotubes is scribbled above.
4. pyrolysis of coal according to claim 1 generates the integrated apparatus of CNT, it is characterised in that：The round metal
The outside of disk is zigzag, rosette be connected with steel wire rope and and motor connection, by setting time, per disk every other hour on
Lower movement is once.
5. pyrolysis of coal according to claim 1 generates the integrated apparatus of CNT, it is characterised in that：The synthesis is single
Member is provided with cyclone separator in connection outlet.
6. a kind of method that pyrolysis of coal generates CNT, using the integrated apparatus described in any one of claim 1 ~ 5, it is special
Levy and be：Comprise the following steps：
（1）Coal-supplying pipe provides the coal dust that particle size diameter is 0-3cm, then provides fuel gas to pyrolysis of coal list to heating unit
Member is heated, and temperature is reached 600 DEG C to 1200 DEG C；The unstrpped gas that pyrolysis of coal unit is produced is entered by coal supply unit top
Enter synthesis unit；
（2）Heating unit is heated, when temperature reaches 650 DEG C to 1000 DEG C, by catalyst and inert gas by dividing
Fabric swatch enters the top of synthesis unit, enters synthesis together after the blended device mixing of the unstrpped gas then produced again with pyrolysis of coal
Unit；The catalyst that is floated in reacting gas and gas and enter with the catalyst that is arranged in the metallic rod inside synthesis unit
Row reacts and generates CNT；Air supply unit serialization is supplied；
（3）When have accumulated the CNT that thickness is 5cm in metallic rod, the device that moves up and down being arranged in metallic rod will
Move up and down, the CNT that will build up on is cleared up, the CNT of synthesis just drops in the cone of synthesis unit bottom together
Shape bottom；When conical lower portion have accumulated the CNT that thickness is 20-30cm, the valve of its underpart can be in CNT gravity
Effect is lower to open, outside the CNT discharger that will build up on by floss hole, it is ensured that the continuous production of device；
（4）Catalyst is separated and is recycled to catalysis by the metallic catalyst being mixed with CNT by catalyst separation device
Agent entrance is reused.
7. the method that pyrolysis of coal according to claim 6 generates CNT, it is characterised in that：The catalyst is metal
Powder, the metallic vapour of evaporation or the organo-metallic compound containing magnetisable material.
8. the method that pyrolysis of coal according to claim 7 generates CNT, it is characterised in that：The metallic element is
Any of iron, cobalt, nickel, molybdenum.
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| CN107986260B (en) * | 2018-01-08 | 2019-07-12 | 海门市卓维纺织品有限公司 | A kind of microwave-heating formula coal carbon nanotube device |
| CN110950322B (en) * | 2019-11-14 | 2023-01-31 | 太原理工大学 | Method for preparing carbon nanotube composite carbon material by utilizing red mud and raw coal |
| CN113353920B (en) * | 2021-07-15 | 2022-05-17 | 青岛科技大学 | Continuous preparation device and preparation method of carbon nano tube |
| CN113562722B (en) * | 2021-08-05 | 2023-06-20 | 青岛科技大学 | Method for producing carbon nano tube by using semicoke-based catalyst prepared by microfluidization bed |
| CN115028161B (en) * | 2022-06-17 | 2024-01-09 | 焦作集越纳米材料技术有限公司 | Preparation method of carbon nano tube |
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| KR20140094943A (en) * | 2013-01-23 | 2014-07-31 | 강원대학교산학협력단 | Method for synthesizing carbon nano tubes |
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