CN105731423A - Integrated device and method for generating carbon nano tube through coal pyrolysis - Google Patents
Integrated device and method for generating carbon nano tube through coal pyrolysis Download PDFInfo
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- CN105731423A CN105731423A CN201610061512.8A CN201610061512A CN105731423A CN 105731423 A CN105731423 A CN 105731423A CN 201610061512 A CN201610061512 A CN 201610061512A CN 105731423 A CN105731423 A CN 105731423A
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Abstract
The invention discloses an integrated device and method for generating a carbon nano tube through coal pyrolysis. A main body of the integrated device is sequentially provided with a coal pyrolysis unit, a heating unit and a synthesis unit from the inside to the outside, wherein the coal pyrolysis unit provides a raw material gas required for synthesis to the synthesis unit; a methane gas generated by the coal pyrolysis unit is directly applied to synthesis of the carbon nano tube as the raw material gas synthesized by the carbon nano tube; and the heating unit simultaneously provides heat to the coal pyrolysis unit and the carbon nano tube synthesis unit through burning a fuel gas. The carbon nano tube can be continuously synthesized; meanwhile, the waste for individually providing heat to the synthesis unit in the past is reduced, and continuous production of the device is ensured; and the raw materials are evenly distributed into the reaction unit at the inlet of the synthesis unit, and then a catalyst is mixed with a reaction gas evenly, so that the quality homogenization of the carbon nano tube is ensured.
Description
Technical field
The present invention relates to a kind of pyrolysis of coal and generate integrated apparatus and the method for CNT, belong to technical field of coal chemical industry.
Background technology
CNT is as monodimension nanometer material, lightweight, and hexagonal structure connects perfection, has many abnormal mechanics, electricity and chemical property.The preparation method of common CNT has: graphite acr method, catalystic pyrolysis, laser steaming process and other thermal depolymerization is legal, ionizing radiation method, flame method, plasma method and up-to-date method of swimming, hydro-thermal method, solid-phase pyrolysis, gas-phase reaction method etc..
Although the preparation method preparing CNT is a lot, but the method being used to prepare in a large number CNT only has graphite acr method, catalystic pyrolysis, and additive method has very big shortcoming to be not used to industrially prepared.
It is crack under the effect of catalyst and form by hydro carbons (such as methane, ethylene, propylene and benzene etc.) or containing oxycarbide that catalystic pyrolysis prepares the principle of CNT.What catalyst choice was more is transition metal etc..Preparing catalyst and synthesizing carbon nanotubes under the same conditions, metal composition difference, the activity of prepared catalyst is also different.Carbon source mainly selects acetylene, methane, CO, ethylene, propylene, butylene, benzene and normal butane etc..Also different in structure and the performance of synthesizing carbon nanotubes.
At present, in actual production, the unstrpped gas used by synthesizing carbon nanotubes is mainly methane, carbon monoxide and benzene, and these unstrpped gases are also mainly derived from natural gas and oil gas.Comparatively speaking, the transport of these unstripped gas is also a part of huge investment, and the pyrogenous origin methane of coal can as the unstripped gas being directly synthesized needed for CNT.The price that coal is cheap can be utilized so on the one hand to obtain higher income, the Transformation Development of coal is also had huge impetus simultaneously.
Summary of the invention
It is desirable to provide a kind of pyrolysis of coal generates integrated apparatus and the method for CNT, the gas that pyrolysis of coal produces is directly used in synthesizing carbon nanotubes, it is possible to continuous print synthesizing carbon nanotubes；Concurrently there are the heating unit between carbon nanotube synthesizing unit and pyrolysis of coal unit can provide heat to two reaction members simultaneously, the single waste that heat is provided to synthesis unit before having saved, also can guarantee that the continuous prodution of device.
The invention provides a kind of pyrolysis of coal and generate the integrated apparatus of CNT, it is characterized in that: described integrated apparatus main body is column structure, upper and lower respectively truncated cone-shaped structure, cylindrical inside is sequentially provided with pyrolysis of coal unit, heating unit, synthesis unit from inside to outside；Pyrolysis of coal unit provides synthesis needed raw material gas, the unstrpped gas that the methane gas that pyrolysis of coal unit generates synthesizes as CNT for synthesis unit, is directly used in the synthesis of CNT；Heating unit provides heat by combustion fuel gas coal supply pyrolysis unit simultaneously and carbon nanotube synthesizing unit, and the flow velocity entering each heating unit layer by controlling fuel gas provides the heat needed for pyrolysis of coal unit and carbon nanotube synthesizing unit；
Described pyrolysis of coal unit is column structure, and top connects coal-supplying pipe, and bottom is provided with coke discharge pipeline；The cylindrical wall on pyrolysis of coal unit top is provided with uniform steam vent, and the unstrpped gas that pyrolysis of coal unit produces enters synthesis unit by the steam vent on top；
Described heating unit is double-layer circular tubular, inside and outside layer bottom of cylinder connects fuel gas pipeline respectively, inner layer cylinder is heating internal layer, outer layer cylinder is heating outer layer, heating unit is enclosed within outside pyrolysis of coal unit, heating internal layer contacts with pyrolysis of coal unit and heat supply, and heating outer layer contacts with the synthesis unit of CNT and heat supply；
The top of integrated apparatus is respectively equipped with catalyst inlet and inert gas entrance, synthesis unit top is provided with feed distribution plate, and distribution grid is a Circular Plate, and coal-supplying pipe passes from the center of distribution grid, distribution grid is uniformly provided with hole, bottom synthesis unit, is provided with the opening and closing of Valve controlling floss hole.
In said apparatus, described distribution grid is connected with blender.Blender is an agitating device, and this agitating device is to be located at the axial blade of cylinder with multiple centered by a cylinder axis.Raw material can be uniformly dispersed in the inside of synthesis unit by the rotation of blade.The number of blender can set according to concrete device size, it is ensured that can unstripped gas and catalyst be evenly distributed in synthesis unit.
In said apparatus, described synthesis unit is vertically provided with metallic rod, above metallic rod shaped object, scribbles the metallic catalyst needed for synthesizing carbon nanotubes.Further, described metallic rod is provided with the device that can move up and down, this device is that a rosette is enclosed within metallic rod, the outside of disk is zigzag, rosette is connected with steel wire rope and motor respectively, and by setting the time, often disk moves up and down once every other hour, accumulation CNT in metallic rod can be cleared up, it is prevented that the blocking of device.
In said apparatus, described synthesis unit connecting carbon nanotube outlet place is provided with cyclone separator, by the difference of CNT and metallic catalyst density, CNT and metallic catalyst are separated by the cyclone separator of cylindrical structure shape, the catalyst after separating is recycled.
The invention provides a kind of method that pyrolysis of coal generates CNT, adopt above-mentioned integrated apparatus, comprise the following steps:
(1) coal-supplying pipe provides particle size diameter to be the coal dust of 0-3cm, then provides fuel gas that pyrolysis of coal unit is heated to heating unit, makes temperature reach 600 DEG C to 1200 DEG C；The unstrpped gas that pyrolysis of coal unit produces enters synthesis unit by coal supply unit top；
(2) heating unit is heated, when temperature reaches 650 DEG C to 1000 DEG C, catalyst and noble gas is entered the top of synthesis unit by distribution grid, together with after the blended device mixing of unstrpped gas then produced with pyrolysis of coal again, enter synthesis unit；The catalyst that floats in reacting gas and gas and and the catalyst that is arranged in the metallic rod within synthesis unit react and generate CNT；Air supply unit serialization supplies；
(3) when metallic rod have accumulated the CNT that thickness is approximately 5cm, it is arranged at moving up and down device and will move up and down on shaft, the CNT that will build up on is cleared up, and the CNT of synthesis just drops together in the conical lower portion of synthesis unit bottom；When conical lower portion have accumulated the CNT that thickness is 20-30cm, the valve of its underpart can be opened under CNT action of gravity, by outside the CNT discharger that floss hole will build up on, it is ensured that the continuous prodution of device；
(4) metallic catalyst being mixed with in CNT by catalyst separation device catalyst separation is out recycled to catalyst inlet again with.
In said method, described catalyst can be the metallic vapour for metal dust or evaporation, or the organo-metallic compound containing magnetisable material.Further, described metallic element is any one in ferrum, cobalt, nickel, molybdenum.Described catalyst is the metallic vapour of metal dust or evaporation, or the organo-metallic compound containing magnetisable material.
Apparatus and method provided by the invention, bringBeneficial effect:
(1) inner most pyrolysis of coal unit provides the unstrpped gas needed for synthesizing carbon nanotubes can to carbon nanotube synthesizing unit continuously.The unstrpped gas that pyrolysis of coal produces ensure that the continuous prodution of carbon nanotube synthesizing unit.
(2) internal heating unit coal supply pyrolysis unit and carbon nanotube synthesizing unit can provide heat simultaneously, heating unit can be divided into two parts, and the speed entering each heating unit by regulating fuel gas realizes carbon nanotube synthesizing unit and the temperature requirements of pyrolysis of coal unit.
(3) in the internally installed metallic rod scribbling catalyst of apparatus for synthesizing carbon nanotubes, metallic rod there is a device moved up and down can be cleared up by the CNT of synthesis on this position timely, it is achieved the continuous prodution of CNT.
(4) distribution grid of the unstrpped gas and metallic catalyst of being located at synthesis unit top is the distribution grid of uniform porous, can mixed unstrpped gas and metallic catalyst be dispersed in inside synthesis unit, thus improving combined coefficient.
Accompanying drawing explanation
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 noble gas enter reaction member.
In figure, 1 is pyrolysis of coal unit, and 2 is heating unit, and 2a is heating internal layer, 2b is heating outer layer, and 3 is synthesis unit, and 4 is coal-supplying pipe, 5 is catalyst inlet, 6 is inert gas entrance, and 7 is coke discharge pipeline, and 8 is floss hole, 9 is metallic rod, 10 devices for moving up and down, 11 is blender, and 12 is distribution grid.
Detailed description of the invention
Further illustrate the present invention by the examples below, but be not limited to following example.
Embodiment:
As shown in Fig. 1 ~ 3, a kind of pyrolysis of coal generates the integrated apparatus of CNT, and apparatus main body is column structure, upper and lower respectively truncated cone-shaped structure, and cylindrical inside is sequentially provided with pyrolysis of coal unit 1, heating unit 2, synthesis unit 3 from inside to outside；Pyrolysis of coal unit 1 provides synthesis needed raw material gas, the unstrpped gas that the methane gas that pyrolysis of coal unit 1 generates synthesizes as CNT for synthesis unit 3, is directly used in the synthesis of CNT；Heating unit 2 provides heat by combustion fuel gas coal supply pyrolysis unit 1 and carbon nanotube synthesizing unit 3 simultaneously, and the flow velocity entering each heating unit layer by controlling fuel gas provides the heat needed for pyrolysis of coal unit 1 and carbon nanotube synthesizing unit 3；
Described pyrolysis of coal unit 1 is column structure, and top connects coal-supplying pipe 4, and bottom is provided with coke discharge pipeline 7；The cylindrical wall on pyrolysis of coal unit top is provided with uniform steam vent, and the unstrpped gas that pyrolysis of coal unit produces enters synthesis unit by the steam vent on top；
Described heating unit 2 is double-layer circular tubular, inside and outside layer bottom of cylinder connects fuel gas pipeline respectively, inner layer cylinder is heating internal layer 2a, outer layer cylinder is heating outer layer 2b, heating unit 2 is enclosed within outside pyrolysis of coal unit 1, heating internal layer 2a contacts with pyrolysis of coal unit 1 and heat supply, and heating outer layer 2b contacts with the synthesis unit 3 of CNT and heat supply；
The top of integrated apparatus is respectively equipped with catalyst inlet 5 and inert gas entrance 6, synthesis unit top is provided with feed distribution plate 12, distribution grid is a Circular Plate, coal-supplying pipe 4 passes from the center of distribution grid 12, being uniformly provided with hole on distribution grid 12, the bottom of synthesis unit 3 is provided with the opening and closing of Valve controlling floss hole 8.
In said apparatus, described distribution grid 12 is connected with blender 11.Blender is an agitating device, and this agitating device is to be located at the axial blade of cylinder with multiple centered by a cylinder axis.Raw material can be uniformly dispersed in the inside of synthesis unit by the rotation of blade.The number of blender can set according to concrete device size, it is ensured that can unstripped gas and catalyst be evenly distributed in synthesis unit.
In said apparatus, being vertically provided with metallic rod 9 in described synthesis unit 3, metal bar surface scribbles the metallic catalyst needed for synthesizing carbon nanotubes.Further, described metallic rod 9 is provided with the device 10 that can move up and down, this device is that a rosette is enclosed within metallic rod, the outside of disk is zigzag, rosette is connected with steel wire rope and motor respectively, and by setting the time, often disk moves up and down once every other hour, accumulation CNT in metallic rod can be cleared up, it is prevented that the blocking of device.
In said apparatus, described synthesis unit connecting carbon nanotube outlet place is provided with cyclone separator (not shown), by the difference of CNT and metallic catalyst density, CNT and metallic catalyst are separated by the cyclone separator of cylindrical structure shape, the catalyst after separating is recycled.
The operation principle of the present invention:
(1) pyrolysis of coal unit is in the bosom of whole device, and the coal of pulverizing enters pyrolysis of coal unit from coal-supplying pipe, and the speed being controlled fuel gas entrance heating unit by flow control valve sets the temperature of pyrolysis of coal unit between 600 DEG C to 1200 DEG C.The Coal Under isolation air separation of heat is provided at heating unit, controls the pressure and temperature that pyrolysis of coal unit is suitable, improve the production rate of CNT synthesis needed raw material gases methane.The gas that pyrolysis of coal produces discharges pyrolysis of coal unit through the top of pyrolysis unit, and the coke that pyrolysis of coal produces then is discharged by the coke discharge pipeline of this unit bottom.
(2) heating unit is positioned at synthesis unit and the middle part of pyrolysis of coal unit, heating unit is divided into inside and outside two-layer, control the technological temperature needed for synthesis unit synthesizing carbon nanotubes by controlling to enter the speed of heating unit fuel gas, and the temperature of pyrolysis of coal unit is between 600 DEG C to 1200 DEG C.
(3) metallic catalyst and noble gas are when entering synthesis unit top, it is possible to first pass through a distribution grid, be evenly distributed in synthesis unit by catalyst and noble gas, the outer wall of synthesis unit by heat proof material as quartz or graphite are made.Catalyst is the metal of powder or evaporation, and it is preferably the organo-metallic compound containing magnetic material such as ferrum, cobalt, nickel, molybdenum.Fig. 3 is the horizontal cross of distribution grid, this distribution grid be centered by the center of circle every 10 ° on distribution grid, be provided with the circular hole that string diameter is identical, the diameter of circular hole can be changed according to concrete volume of production, unstrpped gas and the speed of catalyst entrance synthesis unit is regulated by regulating the diameter of circular hole, the flow of gas can also be regulated by changing the distribution density of circular hole, it is ensured that metallic catalyst and indifferent gas physical ability are divided equably and be sprinkling upon in synthesis unit.
(4) unstrpped gas enters synthesis unit together with after the top of synthesis unit mixes with metallic catalyst and noble gas, in order to make unstrpped gas and metallic catalyst mixing more abundant, upper design one blender of synthesis unit can entered, simultaneously, it is possible to gas pump is installed before entering synthesis unit and flow control valve controls noble gas and the speed of metallic catalyst entrance synthesis unit.
(5) after pyrolysis of coal unit unstrpped gas out and metallic catalyst mixing, synthesis unit is entered, the unstrpped gas part entering synthesis unit scribbles synthesis in the metallic rod of metallic catalyst in synthesis unit, moving up and down device and can in time CNT above be cleared up in metallic rod, it is prevented that the blocking of device.Additionally, as in figure 2 it is shown, the lower tilt ground of synthesis unit 130 is formed as a cone, it is possible to the CNT of synthesis is gathered in the bottom of cone.Meanwhile, being gathered in the catalyst bottom synthesis unit can also clear in time, again recycles after being separated by cyclone separator.
It addition, the type according to catalyst, namely the shape of catalyst, density, size, adjust the flow velocity of noble gas and catalyst.
The method that pyrolysis of coal of the present invention generates CNT below illustrates.
First, coal-supplying pipe provides particle size diameter to be the coal dust of 0-3cm, then provides fuel gas that pyrolysis of coal unit is heated to heating unit, makes temperature reach 600 DEG C to 1200 DEG C.The unstrpped gas that pyrolysis of coal unit produces enters synthesis unit by coal supply unit top.
Then, heating unit is heated, when temperature reaches 650 DEG C to 1000 DEG C, catalyst and noble gas are entered the top of synthesis unit by distribution grid, together with after the blended device mixing of unstrpped gas (methane) then produced with pyrolysis of coal again, enter synthesis unit.The catalyst that floats in reacting gas and gas and and the catalyst that is arranged on the bar scribbling metallic catalyst within synthesis unit react and generate CNT.
When have accumulated the CNT that thickness is approximately 5cm in metallic rod, being arranged at moving up and down device and will move up and down on shaft, the CNT that will build up on is cleared up, and the CNT of synthesis just drops together in the conical lower portion of synthesis unit bottom.When conical lower portion have accumulated the CNT that thickness is 20-30cm, the valve of its underpart is opened under CNT action of gravity, by outside the CNT discharger that floss hole will build up on, it is ensured that the continuous prodution of device.
The metallic catalyst being mixed with in CNT can pass through cyclone separator catalyst separation is out recycled to catalyst input port again with.
Claims (8)
1. the integrated apparatus of a pyrolysis of coal generation CNT, it is characterized in that: described integrated apparatus main body is column structure, upper and lower respectively truncated cone-shaped structure, cylindrical inside is sequentially provided with pyrolysis of coal unit, heating unit, synthesis unit from inside to outside, described pyrolysis of coal unit is column structure, top connects coal-supplying pipe, bottom is provided with coke discharge pipeline, the cylindrical wall on pyrolysis of coal unit top is provided with uniform steam vent, and the unstrpped gas that pyrolysis of coal unit produces enters synthesis unit by the steam vent on top；
Described heating unit is double-layer circular tubular, inside and outside layer bottom of cylinder connects fuel gas pipeline respectively, inner layer cylinder is heating internal layer, outer layer cylinder is heating outer layer, heating unit is enclosed within outside pyrolysis of coal unit, heating internal layer contacts with pyrolysis of coal unit and heat supply, and heating outer layer contacts with the synthesis unit of CNT and heat supply；The top of integrated apparatus is respectively equipped with catalyst inlet and inert gas entrance, synthesis unit top is provided with feed distribution plate, and distribution grid is a Circular Plate, and coal-supplying pipe passes from the center of distribution grid, distribution grid is uniformly provided with hole, bottom synthesis unit, is provided with the opening and closing of Valve controlling floss hole.
2. pyrolysis of coal according to claim 1 generates the integrated apparatus of CNT, it is characterised in that: described distribution grid is connected with blender；Blender is an agitating device, and this agitating device is to be located at the axial blade of cylinder with multiple centered by a cylinder axis, and raw material is uniformly dispersed in the inside of synthesis unit by the rotation of blade；The number of blender can set according to concrete device size, it is ensured that can unstripped gas and catalyst be evenly distributed in synthesis unit.
3. pyrolysis of coal according to claim 1 generates the integrated apparatus of CNT, it is characterised in that: described synthesis unit is vertically provided with metallic rod, above metallic rod shaped object, scribbles the metallic catalyst needed for synthesizing carbon nanotubes.
4. pyrolysis of coal according to claim 3 generates the integrated apparatus of CNT, it is characterized in that: described metallic rod is provided with the device that can move up and down, this device is that a rosette is enclosed within metallic rod, the outside of disk is zigzag, rosette is connected with steel wire rope and also connects with motor, by setting the time, often disk moves up and down once every other hour.
5. pyrolysis of coal according to claim 1 generates the integrated apparatus of CNT, it is characterised in that: described synthesis unit is provided with cyclone separator in connecting carbon nanotube outlet.
6. the method that pyrolysis of coal generates CNT, adopts the integrated apparatus described in any one of claim 1 ~ 5, it is characterised in that: comprise the following steps:
(1) coal-supplying pipe provides particle size diameter to be the coal dust of 0-3cm, then provides fuel gas that pyrolysis of coal unit is heated to heating unit, makes temperature reach 600 DEG C to 1200 DEG C；The unstrpped gas that pyrolysis of coal unit produces enters synthesis unit by coal supply unit top；
(2) heating unit is heated, when temperature reaches 650 DEG C to 1000 DEG C, catalyst and noble gas is entered the top of synthesis unit by distribution grid, together with after the blended device mixing of unstrpped gas then produced with pyrolysis of coal again, enter synthesis unit；The catalyst that floats in reacting gas and gas and and the catalyst that is arranged in the metallic rod within synthesis unit react and generate CNT；Air supply unit serialization supplies；
(3) when metallic rod have accumulated the CNT that thickness is approximately 5cm, it is arranged at moving up and down device and will move up and down on shaft, the CNT that will build up on is cleared up, and the CNT of synthesis just drops together in the conical lower portion of synthesis unit bottom；When conical lower portion have accumulated the CNT that thickness is 20-30cm, the valve of its underpart can be opened under CNT action of gravity, by outside the CNT discharger that floss hole will build up on, it is ensured that the continuous prodution of device；
(4) metallic catalyst being mixed with in CNT by catalyst separation device catalyst separation is out recycled to catalyst inlet again with.
7. the method that pyrolysis of coal according to claim 6 generates CNT, it is characterised in that: described catalyst is the metallic vapour of metal dust or 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: described metallic element is any one in ferrum, cobalt, nickel, molybdenum.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107986260A (en) * | 2018-01-08 | 2018-05-04 | 匡玉华 | A kind of microwave-heating formula coal carbon nanotube device |
| CN110950322A (en) * | 2019-11-14 | 2020-04-03 | 太原理工大学 | Method for preparing carbon nanotube composite carbon material by utilizing red mud and raw coal |
| CN113353920A (en) * | 2021-07-15 | 2021-09-07 | 青岛科技大学 | Continuous preparation device and preparation method of carbon nano tube |
| CN113562722A (en) * | 2021-08-05 | 2021-10-29 | 青岛科技大学 | Method for producing carbon nano tube by using semicoke-based catalyst prepared by microfluidization bed |
| CN115028161A (en) * | 2022-06-17 | 2022-09-09 | 焦作集越纳米材料技术有限公司 | Preparation method of carbon nano tube |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107986260A (en) * | 2018-01-08 | 2018-05-04 | 匡玉华 | A kind of microwave-heating formula coal carbon nanotube device |
| CN110950322A (en) * | 2019-11-14 | 2020-04-03 | 太原理工大学 | Method for preparing carbon nanotube composite carbon material by utilizing red mud and raw coal |
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Granted publication date: 20171024 Termination date: 20220129 |