CN111498835A - Horizontal fluidizing device for gas-phase purification of carbon nano tube and fluidizing purification method - Google Patents
Horizontal fluidizing device for gas-phase purification of carbon nano tube and fluidizing purification method Download PDFInfo
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- B01J8/36—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed through which there is an essentially horizontal flow of particles
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Abstract
The invention discloses a horizontal fluidizing device and a fluidizing purification method for gas-phase purification of carbon nano tubes, wherein the horizontal fluidizing device comprises a fluidizing reaction bin which is horizontally arranged, a gas distribution plate is arranged at the bottom of the fluidizing reaction bin, a plurality of gas inlets are sequentially arranged on the fluidizing reaction bin below the gas distribution plate along the length direction of the fluidizing reaction bin, an anti-corrosion dust filter net is arranged at the top of the fluidizing reaction bin, at least one gas outlet is arranged on the fluidizing reaction bin above the anti-corrosion dust filter net, one end of the fluidizing reaction bin is provided with a blowing port, the blowing port is arranged in the horizontal direction, and the other end of the fluidizing reaction bin is provided with a discharge port. The invention can solve the problems of higher equipment setting height, complex installation and being not beneficial to the operation and treatment of high-risk gas in the traditional carbon nano tube fluidization purification device, can effectively improve the purification efficiency and the utilization rate of reaction gas, and reduces the purification treatment cost.
Description
Technical Field
The invention relates to the technical field of carbon nanotube purification, in particular to a horizontal fluidizing device and a fluidizing purification method for carbon nanotube gas-phase purification.
Background
Carbon Nanotubes (CNTs) have received a great deal of attention and use as conductive materials due to their excellent electrical and thermal properties. The carbon nano tube is used as a conductive agent applied to a lithium battery material and can obviously improve the performance of the lithium battery, so that the carbon nano tube is more and more widely applied to the lithium battery. In the application of the lithium ion battery material, the requirement on metal impurities is strict, and various metal catalyst impurities exist in the carbon nanotube powder, so that the carbon nanotube needs to be purified when being applied to the field of the lithium ion battery.
At present, the purification method of the carbon nano tube mainly comprises three methods: one is a pickling purification method, which mainly dissolves a metal catalyst by one or more of nitric acid, hydrochloric acid and sulfuric acid, and then realizes the purification of the carbon nano tube by filtering and drying, and the method can generate a large amount of waste acid, which causes the problems of environmental pollution and waste acid treatment, and the highest purity can only reach 99.8%. The second method is a high-temperature heat treatment method, which mainly comprises the step of carrying out heat treatment on the carbon nano tube under the protection of high vacuum or inert gas at the temperature of more than 1500 ℃ to ensure that a metal catalyst in the carbon nano tube is directly sublimated and separated from the carbon nano tube, so that the aim of purifying the carbon nano tube is fulfilled. The third method is a method for removing metal impurities in the carbon nano tube by using halogen-containing gas, which makes the metal catalyst in the carbon nano tube react with the halogen-containing gas by using the principle that the boiling point of the metal halide is far lower than the boiling point of a simple substance or an oxide thereof to generate the metal halide to be gasified at high temperature, and the method can also make the content of the single metal element impurities in the carbon nano tube reach below 50ppm, greatly reduce the treatment temperature by converting the metal impurities into the metal halide, and avoid the physical damage of the carbon nano tube at high temperature, so the method is an ideal purification method for the carbon nano tube in the future.
The invention patent application CN107108222A discloses a CNT purification method using a fluidized bed reactor, in which a conventional vertical fluidized bed reactor is used to react carbon nanotubes with chlorine gas in the conventional vertical fluidized bed reactor, so as to realize the purification process of carbon nanotubes. The fluidized bed can realize the full contact of the carbon nano tube and chlorine gas, and has good purification effect; however, the traditional vertical fluidized bed can not realize continuous purification and needs to build a higher equipment platform, so that the equipment has the problems of higher gravity center, difficult operation and maintenance, inconvenience for the use and treatment of high-risk gases such as chlorine and the like.
Disclosure of Invention
The invention aims to solve the problems that the existing carbon nano tube fluidization purification device cannot realize continuous purification, has higher equipment setting height and complex installation, and is not beneficial to the operation and treatment of high-risk gas, and provides a horizontal fluidization device and a fluidization purification method for gas-phase purification of carbon nano tubes.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a horizontal fluidizer for carbon nanotube gas phase purification, including being the fluidization reaction storehouse of horizontal arrangement, fluidization reaction storehouse bottom is provided with gas distribution plate, and the fluidization reaction storehouse is last to be located gas distribution plate below along fluidization reaction storehouse length direction and has set gradually a plurality of air inlets, fluidization reaction storehouse top is provided with anticorrosive filter dust net, and fluidization reaction storehouse is last to be located anticorrosive filter dust net top and is provided with at least one gas outlet, fluidization reaction storehouse one end is provided with blows the mouth, it is the horizontal direction setting to blow the mouth, and the fluidization reaction storehouse other end is provided with the discharge gate.
Among the above-mentioned technical scheme, furtherly, be provided with the storehouse of fluidizing in advance between blowing mouth and the fluidization reaction storehouse, the blowing mouth sets up in storehouse one end of fluidizing in advance, and the storehouse of fluidizing in advance sets up in fluidization reaction storehouse one end and the intercommunication of fluidization reaction storehouse, the storehouse bottom of fluidizing in advance is provided with gas distribution plate, and it is provided with the air inlet of fluidizing in advance to lie in gas distribution plate below on the storehouse of fluidizing in advance.
In the above technical solution, further, a feed inlet is arranged on the pre-fluidizing bin; preferably, a quantitative feeding device is arranged at the feeding port.
Among the above-mentioned technical scheme, further, the fluidization reaction storehouse includes a plurality of reaction branch storehouses, the reaction divides the storehouse level to set up side by side, and the reaction divides between the storehouse to communicate the connection in proper order at the tip.
In the above technical scheme, further, the reaction sub-bin bottom has two air inlets in proper order respectively, the air inlet that is close to one side of the blowing port is used for letting in reaction gas, another air inlet is used for letting in fluidizing gas, the reaction sub-bin top has an air outlet respectively.
In the above technical scheme, further, the gas outlet is located on one side of the reaction sub-bin, which is close to the gas inlet through which the reaction gas is introduced.
In the above technical scheme, further, a tail gas treatment bin is arranged on one side of the fluidization reaction bin, the tail gas treatment bin is communicated with a gas outlet of the fluidization reaction bin, and a gas outlet and a solid matter recovery port are arranged on the tail gas treatment bin; preferably, a closed cavity is formed between the tail gas treatment bin and the fluidization reaction bin, and the gas outlet is positioned in the cavity; preferably, a condensed gas inlet is arranged at the position of the gas outlet on the tail gas treatment bin; preferably, the condensed gas inlet is arranged in the horizontal direction and is vertical to the direction of the gas outlet; preferably, the top of the reaction sub-bin is provided with an inclined surface structure, and the inclined surface is inclined upwards relatively towards the direction of the air outlet; preferably, a heat insulation layer is arranged on the reaction sub-bin and positioned outside the inclined plane; preferably, a heating device is arranged between the reaction sub-bin and the heat insulation layer.
In the above technical scheme, further, a flow guide plate is arranged in the tail gas treatment bin, one end of the flow guide plate is fixed on the tail gas treatment bin, and the other end of the flow guide plate is arranged towards the solid matter recovery port; preferably, the guide plate is arranged opposite to the condensed gas inlet and is vertical to the airflow direction of the condensed gas inlet; preferably, the deflector is located between the condensate gas inlet and the vent.
In the above technical solution, further, the blowing port is connected to a pulse gas conveying device, and two adjacent gas inlets of the gas inlets are respectively connected to the reaction gas conveying device and the fluidizing gas conveying device in sequence.
The inner diameter of the vertical carbon nanotube fluidizing device of the current mainstream is generally not more than 500mm, and due to the influence of an anticorrosive material arranged in the vertical carbon nanotube fluidizing device and the setting height, the volume of a reaction bin of the vertical carbon nanotube fluidizing device is difficult to be large, so that the carbon nanotube purification treatment capacity of the fluidizing device is seriously influenced. Meanwhile, the horizontal structure can reduce the setting height of the fluidizing device, thereby reducing the requirements for a factory building, reducing the construction and matching cost of equipment setting, and reducing the safety of the use of the fluidizing gas in the purification treatment process.
In addition, compared with a vertical fluidized bed, the horizontal fluidizing device is much smaller in height, so that the required fluidizing gas velocity is relatively low, the consumption of reaction gas and fluidizing gas in the fluidizing and purifying process can be reduced, and the safety problem caused by overpressure in a bin due to blockage of an anti-corrosion dust filter caused by gathering of carbon nano tubes on the anti-corrosion dust filter due to overhigh gas velocity can be avoided.
The fluidizing device of the invention respectively and sequentially introduces the reaction gas and the fluidizing gas at different positions in the fluidizing reaction bin, divides the interior of the fluidizing reaction bin into different treatment stages, realizes the full purification of the carbon nano tubes, and pushes the carbon nano tubes in the fluidized state to horizontally move in the fluidizing reaction bin by the pulse gas, so that the carbon nano tubes can continuously move in the fluidizing reaction bin, the purification effect of the carbon nano tubes is improved, meanwhile, the continuous treatment of the carbon nano tubes can be realized, and the purification treatment efficiency of the device is improved.
The invention also relates to a carbon nano tube fluidization purification method adopting the horizontal fluidization device, which comprises the following steps:
1) heating the fluidized reaction bin to a required temperature under the inert gas atmosphere; the temperature is preferably 400-1300 ℃, and more preferably 900-1200 ℃;
2) adding carbon nano tubes to be treated into the pre-fluidization bin, and introducing fluidization gas into the pre-fluidization bin from a pre-fluidization gas inlet to enable the carbon nano tubes entering the pre-fluidization bin to be in a fluidization state; the flow rate of the fluidizing gas is preferably 0.02 to 0.12 m/s;
3) respectively introducing reaction gas and fluidizing gas into the fluidized reaction bin from each gas inlet to ensure that the carbon nano tubes entering the fluidized reaction bin are in a fluidized state all the time; preferably, the flow rate of the introduced reaction gas is 0.01 to 0.038m/s, and the flow rate of the introduced fluidizing gas is 0.02 to 0.12 m/s;
4) introducing pulse airflow into the pre-fluidization bin and the fluidization reaction bin from the blowing port, wherein the pulse airflow pushes the carbon nanotubes in the pre-fluidization bin and the fluidization reaction bin to move in the horizontal direction; preferably, the pulse frequency of the pulse air flow is that the air is blown once every 3-30min, and further preferably 5-7 min; preferably, while the pulse gas flow pushes the carbon nano tubes in the pre-fluidization bin into the fluidization reaction bin, the carbon nano tubes to be treated are continuously added into the pre-fluidization bin; preferably, the acting force provided by each pulse airflow can enable the carbon nano tube to move and displace in the horizontal direction to be the distance between two adjacent air inlets;
the reaction gas in the steps 2), 3) and 4) is halogen-containing gas, and the fluidizing gas and the pulse gas flow are inert gases.
According to the invention, by using the principle of a small amount of times in a chemical extraction method for reference, through controlling the horizontal movement of the carbon nano tube, the carbon nano tube is fluidized by alternately circulating halogen-containing gas and inert gas, so that the formed metal halide gas is rapidly discharged while catalyst metal in the carbon nano tube and the halogen gas are fully reacted, the partial pressure of the metal halide gas in a fluidized reaction bin is reduced, and the gasification efficiency of the metal halide is further improved; meanwhile, the exposure time of the carbon nano tube in the metal halide atmosphere is reduced, the problem that the carbon nano tube is exposed in the metal halide atmosphere for a long time and adsorbs metal halide gas to cause subsequent purging treatment by adopting a large amount of inert gas is avoided, the purification efficiency is further improved, and the purification quality is improved.
The fluidized purification method can effectively reduce the adsorption of the carbon nano tube to the metal halide in the fluidized purification treatment process, and compared with the existing fluidized purification process, the purification efficiency is improved by 60 percent, the utilization rate of the halogen-containing reaction gas can be improved by 30 percent, and the cost of fluidized purification of the carbon nano tube is reduced.
Drawings
FIG. 1 is a schematic view of the structure of the present invention.
FIG. 2 is a schematic sectional view taken along line A-A in FIG. 1.
FIG. 3 is a schematic structural view of the arrangement of the heat-insulating layer and the heating device on the top of the reaction sub-bin.
In the figure: 1. reaction sub-bins, 2, a gas distribution plate, 3, a gas inlet, 4, an anticorrosive dust filtering net, 5, a gas outlet, 6, a pre-fluidization bin, 7, a blowing port, 8, a pre-fluidization gas inlet, 9, a discharge port, 10, a tail gas treatment bin, 11, a solid matter recycling port, 12, a condensed gas inlet, 13, a gas outlet, 14, a quantitative feeding device, 15, a heat preservation and insulation layer, 16, a heating pipe, 17 and a guide plate.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
The horizontal fluidizing device in the embodiment comprises a fluidizing reaction bin which is horizontally arranged, wherein the fluidizing reaction bin is composed of a plurality of reaction sub-bins 1, each reaction sub-bin 1 is horizontally arranged side by side, and the reaction sub-bins 1 are sequentially communicated and connected at the end parts. As shown in fig. 1, the fluidized reaction bin in this embodiment is composed of three reaction sub-bins 1, the reaction sub-bins 1 are all cavity structures with openings at two ends, and the three reaction sub-bins 1 are connected in parallel in sequence to form a completely communicated cavity structure.
The bottom of each reaction sub-bin 1 of the fluidization reaction bin is respectively provided with a gas distribution plate 2 for fluidization, two gas inlets 3 are arranged below the gas distribution plate on each reaction sub-bin 1, the gas inlet on the left side of the two gas inlets 3 is used for introducing reaction gas, and the gas inlet on the right side is used for introducing fluidization gas, so that the carbon nano tubes in the fluidization reaction bin are in a fluidization state.
An anti-corrosion dust filter 4 is arranged at the top of each reaction sub-bin 1, and an air outlet 5 is arranged above the anti-corrosion dust filter on each reaction sub-bin 1 and used for discharging reaction tail gas in the bin. Wherein, the gas outlets 5 on the reaction sub-bin 1 are all positioned on one side of the reaction sub-bin close to the gas inlet for introducing the reaction gas; the arrangement mode is adopted because the content of the metal halide gas in the tail gas at the side where the reaction gas is introduced into the reaction sub-bin is higher, so that the discharge of the metal halide gas can be effectively accelerated, the retention time and the partial pressure of the metal halide gas in the bin are reduced, and the adsorption of the carbon nano tube on the metal halide gas is reduced and the discharge of the metal halide gas is accelerated.
The fluidized reaction zones in the reaction sub-bins are made of high-temperature-resistant and anti-corrosion materials such as quartz, corundum or graphite; because the mode of sequentially splicing and combining the reaction sub-bins to form the fluidized reaction bin is adopted, the volume of the fluidized reaction bin can be well ensured, and the requirement on the size of each reaction sub-bin can be reduced. The gas distribution plate and the anti-corrosion dust filter screen are the prior art in the prior fluidization device, the structures of the gas distribution plate and the anti-corrosion dust filter screen can adopt the prior conventional structures, and the gas distribution plate and the anti-corrosion dust filter screen are both made of anti-corrosion materials due to the special requirements of the fluidization and purification treatment of the carbon nano tubes, wherein the anti-corrosion dust filter screen is woven by quartz fibers or carbon fibers.
As shown in fig. 1, a pre-fluidizing chamber 6 is disposed at one end of the fluidized reaction chamber, and the pre-fluidizing chamber 6 is used for fluidizing the carbon nanotubes entering the apparatus to make them in a fluidized state; specifically, the pre-fluidizing bin 6 is a closed cavity structure with an opening at one end, and the opening end of the pre-fluidizing bin 6 is connected with one end of the fluidizing reaction bin, so that the pre-fluidizing bin and the fluidizing reaction bin are communicated; the other end of the pre-fluidization bin 6 is provided with a blowing port 7, the blowing port 7 is arranged in the horizontal direction, and the arrangement position of the blowing port 7 is preferably the middle position of the end part of the pre-fluidization bin and is used for introducing pulse airflow in the horizontal direction into the pre-fluidization bin and the fluidization reaction bin and pushing the carbon nano tubes in the fluidization state in the pre-fluidization bin and the fluidization reaction bin to move in the horizontal direction. The bottom of the pre-fluidization bin 6 is provided with a gas distribution plate 2, a pre-fluidization air inlet 8 is arranged on the pre-fluidization bin 6 and below the gas distribution plate, and fluidization gas is introduced into the pre-fluidization bin through the pre-fluidization air inlet so that the carbon nano tubes entering the pre-fluidization bin are in a fluidization state.
One end of the reaction sub-bin 1 positioned at the rightmost side is closed, and the end part of the section is provided with a discharge hole 9 for discharging, so that the purified carbon nano tubes are transferred out of the fluidized reaction bin.
As shown in fig. 1 and 2, a tail gas treatment bin 10 is arranged at one side of the fluidized reaction bin, the tail gas treatment bin 10 is communicated with a gas outlet of the fluidized reaction bin, and a gas outlet 13 and a solid matter recovery port 11 are arranged on the tail gas treatment bin 10; and tail gas discharged from the gas outlet 5 in the fluidization reaction bin enters a tail gas treatment bin, metal halide particles obtained by desublimation of the tail gas in the tail gas treatment bin are discharged from a solid matter recovery port under the action of cooling gas, and the rest gas is discharged from a gas outlet. In this embodiment, as shown in fig. 2, the tail gas treatment bin 10 is disposed at one side of the fluidized reaction bin, and a closed cavity is formed between the tail gas treatment bin and the fluidized reaction bin, and the gas outlet 5 is located in the cavity, so that gas exhausted from the fluidized reaction bin can be directly exhausted into the tail gas treatment bin.
A condensed gas inlet 12 is arranged above the gas outlet or in a horizontal position on the tail gas treatment bin 10, and the condensed gas inlet 12 is arranged in a horizontal direction and is vertical to the direction of the gas outlet. And introducing low-temperature condensed gas into the tail gas treatment bin from the condensed gas inlet, and cooling the high-temperature tail gas discharged from the gas outlet, so that the metal halide in the high-temperature tail gas can be rapidly sublimated into metal halide solid particles. The condensing gas lets in the flow direction that can change high-temperature gas in the tail gas treatment storehouse from the horizontal direction, forms one deck inert gas film simultaneously above the tail gas treatment storehouse to can reduce the direct contact between exhaust high temperature corrosive gas and the tail gas treatment storehouse inner wall, reduce the corruption of high temperature corrosive gas to the tail gas treatment storehouse.
For avoiding condensing gas to react the influence of dividing the storehouse top, prevent that it from reducing the reaction and divide the temperature of position department in the storehouse, make high temperature tail gas because the reduction of temperature makes metal halide gas desublimate into solid particle in advance before discharging from the gas outlet, divide 1 top in the storehouse to set up to the inclined plane structure with the reaction, the inclined plane sets up towards the relative top slope of gas outlet orientation for carry out the water conservancy diversion to high temperature gas. Meanwhile, as shown in fig. 3, a heat insulation layer 15 is arranged on the reaction sub-bin 1 and positioned outside the inclined surface, and the heat insulation layer 15 is made of the existing heat insulation material and is used for reducing the influence of condensed gas on the temperature inside the reaction sub-bin; further, a heating device is arranged between the top of the reaction sub-bin 1 and the heat insulation layer 15, the heating device can adopt the existing heating pipe 16 to heat the top of the reaction sub-bin, and the temperature of the top position in the reaction sub-bin is ensured.
A guide plate 17 is arranged in the tail gas treatment bin 10, one end of the guide plate 17 is fixed on the tail gas treatment bin 10, and the other end of the guide plate 17 is arranged towards the direction of the solid matter recovery port 11; the guide plate 17 is arranged opposite to the condensed gas inlet 12 and is vertical to the airflow direction of the condensed gas inlet. The setting of guide plate is used for guiding the direction of motion of tail gas in the tail gas treatment storehouse, and tail gas is through condensation treatment back, and the metal halide granule that the desublimation formed is discharged from the solid matter recovery opening along the guide plate direction under the effect of guide plate, realizes the recovery of catalyst metal and recycles. Wherein, guide plate 17 sets up between condensation gas entry 12 and gas vent 13, makes the air current in the tail gas treatment storehouse move along the guide plate to the dwell time of extension air current in the tail gas treatment storehouse realizes the abundant condensation to metal halide in the tail gas, realizes the gas-solid separation of tail gas better, and all the other gases in the tail gas are discharged from the gas vent.
The pre-fluidizing bin 6 is provided with a feeding port, the feeding port is provided with a quantitative feeding device 14 for adding the carbon nano tubes to be treated into the pre-fluidizing bin, and the quantitative feeding device can adopt existing conveying equipment such as pneumatic conveying or spiral conveying.
The blowing port 7 is connected with a pulse gas conveying device and is used for introducing pulse gas into the pre-fluidization bin and the fluidization reaction bin at a certain pulse frequency; the two gas inlets 3 of each reaction sub-bin 1 are respectively connected with a reaction gas conveying device and a fluidizing gas conveying device for respectively providing reaction gas and fluidizing gas into the reaction sub-bins.
Certainly, in order to ensure the operation of fluidized purification of the carbon nano tube, heating devices are arranged in each reaction sub-bin to provide required reaction treatment temperature for fluidized purification; meanwhile, in order to ensure the uniformity of the temperature in the whole fluidized reaction bin, heat insulation materials such as asbestos fiber and the like are arranged in each reaction sub-bin.
The following description will be made with reference to the horizontal fluidization device in the above embodiment to describe the fluidization purification process, specifically as follows:
and introducing inert gas into the horizontal fluidizing device to perform replacement operation, and detecting the oxygen content in the horizontal fluidizing device to enable the oxygen content to meet the technological requirements.
Under the inert gas atmosphere, the interior of the fluidized reaction bin is heated to the temperature (400-1300 ℃) required by purification treatment.
The carbon nano tube to be purified is quantitatively added into the pre-reaction bin through a quantitative feeding device, fluidizing gas is introduced into the pre-fluidizing bin from the pre-fluidizing gas inlet, so that the carbon nano tube entering the pre-fluidizing bin is in a fluidizing state, and the flow velocity of the introduced fluidizing gas is 0.02-0.12 m/s.
Respectively introducing reaction gas and fluidizing gas into the fluidized reaction bin from each gas inlet to ensure that the carbon nano tubes entering the fluidized reaction bin are in a fluidized state all the time, wherein the flow velocity of the introduced reaction gas is 0.01-0.038m/s, and the flow velocity of the introduced fluidizing gas is 0.02-0.12 m/s; the fluidized reaction bin is divided into a plurality of reaction treatment sections and fluidized treatment sections by sequentially and alternately introducing reaction gas and fluidizing gas into the fluidized reaction bin, the catalyst metal in the carbon nano tubes in the reaction treatment sections reacts with halogen gas, and the carbon nano tubes are subjected to purging treatment by inert gas in the fluidized treatment sections.
Introducing pulse airflow into the pre-fluidization bin and the fluidization reaction bin from the blowing ports, wherein the pulse airflow pushes the carbon nano tubes in the pre-fluidization bin and the fluidization reaction bin to move in the horizontal direction, the pulse frequency of the introduced pulse airflow is that the carbon nano tubes are blown once every 3-30min, namely, high-speed airflow is introduced once every 3-30min, the high-speed airflow provides an acting force in the horizontal direction for the carbon nano tubes, so that the carbon nano tubes move rightwards for a certain distance, the positions of the carbon nano tubes in the fluidization reaction bin are changed, and preferably, the acting force provided by the high-speed airflow can enable the carbon nano tubes to move in the horizontal direction to be the distance between two adjacent air inlets; thus, the carbon nano tube in the fluidized state moves along the horizontal direction along with the pulse airflow introduced at a certain frequency in the reaction bin, and the carbon nano tube horizontally moves one fluidization position under the action of each pulse airflow. Therefore, the carbon nano tube sequentially passes through the reaction treatment sections and the fluidization treatment section, the carbon nano tube is ensured to be fully contacted with the reaction gas and the fluidization gas, the fluidization purification treatment effect is ensured, and the utilization rate of the reaction gas is improved.
The reaction gas is a halogen-containing gas, and preferably one or more of chlorine, hydrogen chloride, freon, and the like, or a mixed gas of these gases with an inert gas, and the like.
The fluidizing gas and the pulse gas flow adopt inert gas, preferably one or more of nitrogen, argon and helium.
And while the pulse airflow pushes the carbon nano tubes in the pre-fluidization bin into the fluidization reaction bin, the carbon nano tubes to be treated are continuously added into the pre-fluidization bin, so that the continuous purification operation of the carbon nano tubes can be realized.
And when the carbon nano tube intermittently and horizontally moves to the position of the discharge hole in the fluidized reaction bin, the fluidized purification process is completed, and the carbon nano tube subjected to fluidized purification treatment is discharged from the discharge hole.
Tail gas in the fluidization reaction bin enters the tail gas treatment bin through each gas outlet, and metal halides in the tail gas are rapidly sublimated into solid particles under the action of condensed gas flow introduced from a condensed gas inlet; the condensed gas can be helium gas with light weight.
The present specification and figures are to be regarded as illustrative rather than restrictive, and it is intended that all such alterations and modifications that fall within the true spirit and scope of the invention, and that all such modifications and variations are included within the scope of the invention as determined by the appended claims without the use of inventive faculty.
Claims (10)
1. A horizontal fluidizing device for carbon nanotube gas-phase purification, its characterized in that: including the fluidization reaction storehouse that is the level and arranges, fluidization reaction storehouse bottom is provided with gas distribution plate, and the fluidization reaction storehouse is last to be located gas distribution plate below along fluidization reaction storehouse length direction and has set gradually a plurality of air inlets, fluidization reaction storehouse top is provided with anticorrosive dirt net of straining, and it is provided with at least one gas outlet to lie in anticorrosive dirt net of straining top on the fluidization reaction storehouse, fluidization reaction storehouse one end is provided with blows the mouth, blow the mouth and be the horizontal direction setting, and the fluidization reaction storehouse other end is provided with the discharge gate.
2. The horizontal fluidizing device for vapor-phase purification of carbon nanotubes according to claim 1, wherein: be provided with the storehouse of fluidizing in advance between blowing mouth and the fluidization reaction storehouse, the blowing mouth sets up in the storehouse one end of fluidizing in advance, and the storehouse of fluidizing in advance sets up in fluidization reaction storehouse one end and fluidization reaction storehouse intercommunication, the storehouse bottom of fluidizing in advance is provided with gas distribution plate, and it is provided with the air inlet of fluidizing in advance to lie in gas distribution plate below on the storehouse of fluidizing in advance.
3. The horizontal fluidizing device for vapor-phase purification of carbon nanotubes according to claim 1, wherein: a feed inlet is formed in the pre-fluidization bin; preferably, a quantitative feeding device is arranged at the feeding port.
4. The horizontal fluidizing device for vapor-phase purification of carbon nanotubes according to claim 1, wherein: the fluidization reaction bin comprises a plurality of reaction sub-bins, the reaction sub-bins are horizontally arranged side by side, and the reaction sub-bins are sequentially communicated and connected at the end parts.
5. The horizontal fluidizing device for vapor-phase purification of carbon nanotubes according to claim 4, wherein: the reaction sub-bin is provided with two air inlets at the bottom in sequence, one air inlet close to one side of the blowing port is used for introducing reaction gas, the other air inlet is used for introducing fluidizing gas, and the top of the reaction sub-bin is provided with an air outlet respectively.
6. The horizontal fluidizing device for vapor-phase purification of carbon nanotubes according to claim 5, wherein: the gas outlet is positioned on one side of the reaction sub-bin, which is close to the gas inlet for introducing the reaction gas.
7. The horizontal fluidizing device for vapor-phase purification of carbon nanotubes according to any one of claims 1 to 6, wherein: a tail gas treatment bin is arranged on one side of the fluidization reaction bin, the tail gas treatment bin is communicated with a gas outlet of the fluidization reaction bin, and a gas outlet and a solid matter recovery port are formed in the tail gas treatment bin; preferably, a closed cavity is formed between the tail gas treatment bin and the fluidization reaction bin, and the gas outlet is positioned in the cavity; preferably, a condensed gas inlet is arranged at the position of the gas outlet on the tail gas treatment bin; preferably, the condensed gas inlet is arranged in the horizontal direction and is vertical to the direction of the gas outlet; preferably, the top of the reaction sub-bin is provided with an inclined surface structure, and the inclined surface is inclined upwards relatively towards the direction of the air outlet; preferably, a heat insulation layer is arranged on the reaction sub-bin and positioned outside the inclined plane; preferably, a heating device is arranged between the reaction sub-bin and the heat insulation layer.
8. The horizontal fluidizing device for vapor-phase purification of carbon nanotubes according to claim 7, wherein: a guide plate is arranged in the tail gas treatment bin, one end of the guide plate is fixed on the tail gas treatment bin, and the other end of the guide plate is arranged towards the direction of the solid matter recovery port; preferably, the guide plate is arranged opposite to the condensed gas inlet and is vertical to the airflow direction of the condensed gas inlet; preferably, the deflector is located between the condensate gas inlet and the vent.
9. The horizontal fluidizing device for vapor-phase purification of carbon nanotubes according to claim 1, wherein: the blowing port is connected with a pulse gas conveying device, and two adjacent gas inlets in the gas inlets are respectively connected with the reaction gas conveying device and the fluidizing gas conveying device in sequence.
10. The carbon nano tube fluidization purification method adopting the horizontal fluidization device is characterized by comprising the following steps of:
1) heating the fluidized reaction bin to a required temperature under the inert gas atmosphere; the temperature is preferably 400-1300 ℃, and more preferably 900-1200 ℃;
2) adding carbon nano tubes to be treated into the pre-fluidization bin, and introducing fluidization gas into the pre-fluidization bin from a pre-fluidization gas inlet to enable the carbon nano tubes entering the pre-fluidization bin to be in a fluidization state; the flow rate of the fluidizing gas is preferably 0.02 to 0.12 m/s;
3) respectively introducing reaction gas and fluidizing gas into the fluidized reaction bin from each gas inlet to ensure that the carbon nano tubes entering the fluidized reaction bin are in a fluidized state all the time; preferably, the flow rate of the introduced reaction gas is 0.01 to 0.038m/s, and the flow rate of the introduced fluidizing gas is 0.02 to 0.12 m/s;
4) introducing pulse airflow into the pre-fluidizing bin and the fluidizing reaction bin from the blowing port, wherein the pulse airflow pushes the carbon nanotubes in the pre-fluidizing bin and the fluidizing reaction bin to move in the horizontal direction; preferably, the pulse frequency of the pulse air flow is that the air is blown once every 3-30min, and further preferably 5-7 min; preferably, while the pulse gas flow pushes the carbon nano tubes in the pre-fluidization bin into the fluidization reaction bin, the carbon nano tubes to be treated are continuously added into the pre-fluidization bin; preferably, the acting force provided by each pulse airflow can enable the carbon nano tube to move and displace in the horizontal direction to be the distance between two adjacent air inlets;
the reaction gas in the steps 2), 3) and 4) is halogen-containing gas, and the fluidizing gas and the pulse gas flow are inert gases.
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