KR20170047486A - Method for purifying CNT using a fluidized bed reactor - Google Patents
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- KR20170047486A KR20170047486A KR1020150147657A KR20150147657A KR20170047486A KR 20170047486 A KR20170047486 A KR 20170047486A KR 1020150147657 A KR1020150147657 A KR 1020150147657A KR 20150147657 A KR20150147657 A KR 20150147657A KR 20170047486 A KR20170047486 A KR 20170047486A
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- B01J8/24—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
Abstract
The present invention relates to a CNT purification method, wherein carbon nanotubes containing an impurity containing a residual metal are reacted and removed with a halogen-containing gas under an inert gas atmosphere in a fluidized bed reactor. The method according to the present invention can operate the reactor at a higher density than the CNT purification method using the conventional heating furnace by using the flow condition and the sealing condition in combination, thereby shortening the time required for the purification process of the CNT, Impurities such as metal catalysts can be effectively purified.
Description
The present invention relates to a method for purifying carbon nanotubes (CNTs) using a fluidized bed reactor.
CNT is widely used as a conductive additive in electronic products such as batteries, conductive ink, and conductive polymers. In the case of fine chemical products, when impurities other than CNT are added together, the quality of the products may be deteriorated and unexpected defects may be caused. Therefore, it is important to remove impurities such as amorphous carbon which may occur during CNT synthesis or CNT synthesis process in order to improve product quality. In particular, the problem of quality and defects can be prevented before the metal catalyst is removed.
The metal removal process in the conventional CNT purification process employs a wet fixation layer using liquid acid and a dry fixation layer in which a chlorine gas is injected into a box-type furnace at a high temperature.
Specifically, the metal removing method using the liquid acid may generate a waste acid as a by-product, and may cause problems such as environmental pollution and waste acid treatment. Further, the metal removing method using the heating furnace has a disadvantage in that the production amount of the product may be lowered because the raw material such as the cooling gas and the time are consumed in controlling the heating and cooling of the heating furnace.
Therefore, there is a need to develop a technique for CNT purification that can shorten the process time while minimizing the production of byproducts.
It is an object of the present invention to provide a method for purifying CNT using a fluidized bed reactor.
Another object of the present invention is to provide a CNT treated by the above method.
According to an aspect of the present invention, there is provided a carbon nanotube-containing carbon nanotube, including a gas inlet and an outlet, and a carbon nanotube (CNT) inlet and outlet, A method for purifying carbon nanotubes (CNTs) which is removed by reacting with a halogen-containing gas.
The purification method includes a first step of heating a carbon nanotube containing an impurity including a residual metal to a first temperature (T1) in an inert gas atmosphere and reacting the carbon nanotube with a halogen-containing gas to halogenize the impurity; And a second step of heating the carbon nanotube to a second temperature (T2) higher than the first temperature to evaporate the halogenated impurity and remove the carbon nanotube through a gas outlet, and obtaining the purified carbon nanotube through a CNT outlet .
According to one embodiment, the first temperature T1 may be 600 ° C to 1000 ° C.
Also, the second temperature T2 may be T1 + 100 deg.
According to one embodiment, the purification process can be carried out in a continuous process using one fluidized bed reactor.
Also, the purification method may be carried out in a continuous process using two fluidized bed reactors, the first step being carried out in a first fluidized bed reactor, and the second step being carried out in a second fluidized bed reactor.
According to one embodiment, the method may further include cooling the purified CNT discharged through the CNT outlet.
According to one embodiment, the halogen-containing gas may be a gas containing fluorine, chlorine, bromine, iodine or a mixture thereof.
Further, the halogen-containing gas may be a gas containing chlorine gas or trichloromethane gas or a mixed component thereof.
According to one embodiment, the inert gas may be a gas containing nitrogen, helium, neon, argon, krypton, xenon, radon or a mixture thereof.
According to one embodiment, the injection method of the gas may be a purging method, a pulse method, a continuous injection method, or a combination injection method.
According to one embodiment, the pressure of the inert gas may be between 500 torr and 800 torr.
According to one embodiment, the pressure of the halogen-containing gas may be from 500 torr to 900 torr.
According to one embodiment, the method may further include a step of neutralizing the halogenated impurities recovered from the gas outlet.
In addition, the neutralization process, silver nitrate (AgNO 3), sodium thiosulfate (Na 2 S 2 O 3) , sodium chloride (NaCl), thiocyanate of potassium (KSCN), thio when thio Ansan ammonium (NH 4 SCN), an aluminum salt-based compound , Sodium hydroxide (NaOH), calcium hydroxide (Ca (OH) 2 ), or a combination thereof.
According to one embodiment, the purified CNT can be provided by such a method.
Other details of the embodiments of the present invention are included in the following detailed description.
According to the CNT purification method using the fluidized bed reactor according to the present invention, by performing the purification reaction of the CNTs using the fluidized bed, the reactor is operated at a higher density than the conventional CNT purification method using a furnace such as a box furnace The contact between the powder and the gas can be effectively performed. Therefore, it is possible to effectively purify the impurities such as the metal catalyst in the CNT while shortening the time required for the CNT purification process.
1 is a schematic view of a carbon nanotube purification system according to the present invention.
2 is an SEM image of CNT according to Production Example 1 and Example 1. Fig.
BRIEF DESCRIPTION OF THE DRAWINGS The present invention is capable of various modifications and various embodiments, and specific embodiments are illustrated in the drawings and described in detail in the description. It is to be understood, however, that the invention is not to be limited to the specific embodiments, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.
As used herein, the term " input "may be used interchangeably with" inflow, infusion "herein, and may be understood to mean the inflow or outflow of liquid, gas, have.
Hereinafter, a CNT (carbon nanotube) purification method according to an embodiment of the present invention will be described in detail.
In order to obtain high purity CNTs, impurities can be removed through a purification step which is a post-treatment of CNT synthesis. As the impurities that can be included in the synthesized CNT, amorphous carbon material, fullerene, graphite, metal catalyst, etc. may be contained. In general, CNTs are purified by removing such impurities by a chemical method or physical method.
The CNT purification method using the fluidized bed reactor according to the present invention is characterized in that in a fluidized bed reactor having a gas inlet and an outlet and a carbon nanotube (CNT) inlet and outlet, the carbon nanotube containing the residual metal is inert And is reacted with a halogen-containing gas under a gaseous atmosphere to remove the halogen-containing gas.
1 schematically shows a carbon nanotube purification system as one embodiment of the present invention.
According to one embodiment, the purification method according to the present invention is a purification method comprising: heating a carbon nanotube containing an impurity including a residual metal to a first temperature (T1) in an inert gas atmosphere to react with a halogen-containing gas to halogenate the impurity; Stage 1; And a second step of heating the carbon nanotube to a second temperature (T2) higher than the first temperature to evaporate the halogenated impurity and remove the carbon nanotube through the gas outlet, and to obtain the purified carbon nanotube through the CNT outlet.
In the first step, the amount of the halogen-containing gas and the inert gas is fed into the fluidized bed reactor at a constant concentration according to the flow conditions, and then the temperature is raised to the first temperature (T1) .
In the first step, the inert gas is introduced into the fluidized bed reactor, the introduction of the inert gas is stopped, the halogen-containing gas is introduced, and the temperature is raised to the first temperature (T1) And purging the reactor after the reaction for a predetermined time in a sealed state.
The closed state may mean a closed state of the fluidized bed reactor or a state of no gas in and out of the reactor, and may include a vacuum atmosphere, which means a pressure of 1 torr or less .
The transferring step may be purging with one or more gases selected from a halogen-containing gas or an inert gas, and may be purged with an inert gas, for example, after the step of reacting in the flow condition, But it is not limited to this.
The step of introducing the halogen-containing gas, the introduction of the inert gas and the step of raising the temperature to the first temperature (T1) may be carried out in the first step regardless of the order. In addition, the first step may include appropriately selecting the order and the number of the steps of reacting in the flow condition and reacting in the hermetic condition.
According to one embodiment, the first temperature T1 may be 600 ° C to 1000 ° C. When the first temperature T1 is less than the above-mentioned temperature range, the chlorination reaction with metal impurities including a catalytic metal or the like in the carbon material may not be smooth.
The second step may include a step of removing a halogenated impurity including a halogenated metal or the like from the first step and raising the temperature to a second temperature (T2). The second step may include a step of introducing a halogen-containing gas into an inert gas atmosphere or a vacuum atmosphere to react and remove impurities. The order and the number of the above-mentioned inert gas atmosphere formation or vacuum atmosphere formation and the halogen-containing gas introduction are not particularly limited, and can be alternately or repeated a suitable number of times.
According to one embodiment, the second temperature T2 may be a temperature higher than the first temperature, and specifically, T2 may be a temperature higher than T1 + 100 ° C. The second temperature T2 may range, for example, from 700 ° C to 1500 ° C, and more specifically, for example, from 900 ° C to 1400 ° C. When the second temperature (T2) is lower than the above-mentioned range or lower than the first temperature, the removal reaction of the impurities including the halogenated metal is not smooth, so that the residual metal and the halogenated metal remain in the carbon nanotube, And this may cause a deterioration of the physical properties of the carbon nanotubes. In addition, at temperatures above the range described above, graphitization of the catalyst by the residual metal occurs, and removal of impurities such as metals may not be easy.
In the first and second steps, the order and the number of the CNTs according to the present invention are not particularly limited, and depending on the crystallinity of the CNT to be purified, the kind of the catalyst metal used for CNT synthesis, As shown in FIG.
The catalyst metal is not particularly limited as long as it is a substance promoting the growth of carbon nanotubes. Examples of the catalyst metal include at least one metal selected from the group consisting of Groups 3 to 12 of the Periodic Table of Elements. (Fe), nickel (Ni), cobalt (Co), cobalt (Co), and cobalt (Co), and more preferably, at least one metal selected from the group consisting of 3, 5, 6, 8, 9, And a rare earth element selected from chromium (Cr), molybdenum (Mo), tungsten (W), vanadium (V), titanium (Ti), ruthenium (Ru), rhodium (Rh), palladium (Pd) At least one kind of metal. A material having a high boiling point with respect to the first temperature and the second temperature may require a large amount of energy, so that a material capable of being treated with a low energy in terms of efficiency may be preferable.
According to one embodiment, the carbon nanotube tablets according to the present invention may be carried out in a continuous process through one fluidized bed reactor.
The process including the first step and the second step may be carried out in a fluidized bed reactor. Specifically, the fluidized bed reactor includes a
Also, according to one embodiment, the carbon nanotube tablets of the present invention may be carried out in a continuous process using two fluidized bed reactors. Specifically, the first step may be performed in a first fluidized bed reactor, and the second step may be performed in a second fluidized bed reactor.
According to one embodiment, the reaction time of the first step may be maintained for, for example, 10 minutes to 1 hour, and the halogenation process of the residual metal may be more completely performed within the range, Carbon nanotubes and the size of the reactor.
Also, the reaction time of the second step can be maintained for 30 minutes to 300 minutes, and can be appropriately controlled within a range that can remove impurities including residual metals without affecting the carbon nanotubes.
The treatment time and temperature can be appropriately adjusted by those skilled in the art according to the crystallinity of the CNT to be purified and the kind of the catalyst metal used for CNT synthesis.
Each of the above processes may be carried out in any combination, and the specific process may be repeated.
According to an embodiment, the method may further include cooling the purified carbon nanotube through a purification method including the first step and the second step.
In addition, according to one embodiment, as shown in FIG. 1, it may further include a step of recovering the gas discharged from the
As the neutralization solution, for example, a solution containing nitric acid, sulfuric acid and the like can be used. Specifically, silver nitrate (AgNO 3 ), sodium thiosulfate (Na 2 S 2 O 3 ), sodium chloride (NaCl) The halide is removed using an aqueous solution of a material selected from potassium (KSCN), ammonium thiocyanate (NH 4 SCN), aluminum salt compound, sodium hydroxide (NAOH), calcium hydroxide (Ca (OH) 2 ) However, the present invention is not limited to the above example.
According to one embodiment, the pressure of the halogen-containing gas may be from 500 torr to 900 torr, for example, from 600 torr to 800 torr, more specifically from 600 torr to 700 torr.
Further, the inert gas may be supplied at a pressure of 500 torr to 800 torr, for example, at a pressure of 600 torr to 800 torr, more specifically 600 torr to 700 torr.
The flow rates of the halogen-containing gas and the inert gas as described above can be appropriately adjusted by the user because the purification time can be shortened under a condition of a high concentration of the halogen gas and can be prolonged under a low condition. In addition, the reactivity of the halogen gas may be affected depending on the environmental conditions such as the material of the reactor, so that it can be suitably controlled according to the environmental conditions such as the material of the reactor, the catalyst, and the reaction temperature.
According to one embodiment, the halogen-containing gas may be a gas containing fluorine, chlorine, bromine, iodine or a mixed component thereof, for example, a chlorine-containing gas may be used, Or a gas containing trichloromethane gas or a mixed component thereof. By using such a halogen-containing gas, halogen ions having a high electron affinity can be used for removing impurities, particularly metal-containing impurities. For example, halogen ions have high reactivity with iron-containing impurities. Impurities which are covalently bonded with a halogen ion and a metal ion can be selectively removed as a reaction product after the reaction.
In addition, the inert gas may include, for example, a gas containing nitrogen, helium, neon, argon, krypton, xenon, radon or a mixed component thereof, and specifically nitrogen gas may be used. Since such an inert gas is chemically very stable and has a property of not exchanging electrons or sharing it, it can serve to flow and move the CNT due to the inflow of gas without reacting with the CNT.
The gases may be heated via a preheater and then introduced into the
Further, the halogen gas, the inert gas, etc. used in the CNT purification method using the fluidized bed reactor can be recycled.
The method of injecting the gas is not particularly limited, and may include a purging method, a pulse method, a continuous injection method, or an injection method using a combination thereof. For example, the purging method may include a method of injecting gas intermittently and continuously, and the pulse method may include injecting a predetermined amount of gas at regular intervals. Also, the continuous injection method may include a method of injecting a gas at a specific speed, and the gas injection method as described above may be used in combination.
The CNT purification method according to the present invention is advantageous in that the purification process and the cooling process can be separately processed, that is, the purification process is performed and the cooling process is performed in a separate space. Herein, the refining step refers to a step in which the halogen-containing gas reacts with the impurities, and the cooling step may mean a step of lowering the temperature of the CNT after the refining step. For example, the cooling process may be performed by moving the carbon nanotubes from which the impurities have been removed according to the present invention to the cooling and
In the conventional method of cooling the natural convection by interrupting the heat supply to the furnace by the general cooling process, the time taken to lower the temperature may be prolonged, so that the consumed cooling water or the cooling gas may also be increased. On the other hand, according to the method of the present invention, the CNTs recovered after the purification process are moved and the cooling process is separated and treated so that the energy that has been heated for the purification process can be used as it is in the next batch. The recovered CNTs can be cooled, so that a sufficient cooling time can be secured. Therefore, when the purification process and the cooling process are separated and processed according to the present invention, the time required for recovery through purification of CNT and the raw materials such as cooling water and cooling gas can be saved.
The
As described above, the purification process according to the present invention can be operated under flow conditions and hermetic conditions. The purification process according to the present invention can be performed by using the inert gas and the halogen-containing gas, It is possible to efficiently carry out the process.
According to the present invention, CNTs purified in high purity can be provided by the method as described above, and such CNTs can exhibit the best performance in various fields. For example, CNT has many applications such as medical or engineering microparts, electronic devices, batteries, etc. In particular, in the case of electronic materials, when CNTs contain impurities due to their characteristics, there are disadvantages The CNT purification method according to the present invention and the CNT purified by this method can be used to minimize such problems.
The carbon nanotube according to the present invention may be one produced by growing a carbon nanotube by a chemical vapor phase synthesis (CVD) method through decomposition of a carbon source using a supported catalyst. The catalytic metal supported on the supported catalyst may be a carbon nanotube Is not particularly limited.
Examples of the catalytic metal include at least one kind of metal selected from the group consisting of Groups 3 to 12 of the 18-element type periodic table recommended by IUPAC in 1990. Among them, at least one kind of metal selected from the group consisting of 3, 5, 6, 8, 9 and 10 is preferable, and iron (Fe), nickel (Ni), cobalt (Co), chromium (Cr) At least one metal selected from the group consisting of Mo, W, V, Ti, Ru, Rh, Pd, Pt and rare- Particularly preferred. Examples of the catalyst metal precursor include inorganic salts such as nitrates, sulfates and carbonates of catalyst metals, organic salts such as nitrates and acylates, organic complexes such as acetylacetone complexes, organic metal compounds and the like And is not particularly limited as long as it is a compound containing a catalytic metal.
It is widely known to control the reaction activity by using two or more of these catalytic metals and catalytic metal precursor compounds. For example, at least one element selected from iron (Fe), cobalt (Co), and nickel (Ni) and at least one element selected from titanium (Ti), vanadium (V), and chromium (Cr), molybdenum (Mo), and tungsten (W) can be exemplified. The metal catalyst may preferably be cobalt (Co) as a main component and further include at least one metal selected from iron (Fe), molybdenum (Mo), chromium (Cr), and vanadium (V).
Hereinafter, embodiments of the present invention will be described in detail so that those skilled in the art can easily carry out the present invention. The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Production Example 1: Preparation of carbon nanotube (CNT)
Carbon nanotubes were synthesized in a laboratory scale fluidized bed reactor using a Co / Fe / Mo / V / Al containing metal catalyst for CNT synthesis. Specifically, the CNT synthesis catalyst prepared in the above process and CNT were mixed and placed in a middle portion of a quartz tube having an inner diameter of 55 mm. Then, the catalyst was heated to 700 ° C. in a nitrogen atmosphere, Gas was synthesized for 2 hours while flowing at a flow rate of 900 sccm to synthesize an entangled carbon nanotube agglomerate. A photograph of the produced CNT is shown in Production Example 1 of Fig.
Examples 1 to 2 and Comparative Example 1: Purification of carbon nanotubes
Example 1
20 g of the carbon nanotubes prepared in Preparation Example 1 were placed in a fluidized bed reactor. N 2 was injected at a flow rate of 1000 sccm to raise the internal temperature of the reactor to 900 캜. Next, the halogen-containing gases Cl 2 and N 2 were fed in a 1: 1 ratio at a flow rate of 1000 sccm for 30 minutes.
Thereafter, only N 2 was injected, the sample was transferred to a second high-temperature reactor at 1200 ° C, and then maintained in a flowing condition of N 2 gas atmosphere for 30 minutes and then cooled. The photograph of the CNT after this step is shown in the photograph of Example 1 of Fig.
Example 2
20 g of the carbon nanotubes prepared in Preparation Example 1 were placed in a fluidized bed reactor.
N 2 was injected at a flow rate of 1000 sccm to raise the internal temperature of the reactor to 900 캜. Next, the halide-containing gases Cl 2 and N 2 are injected at a flow rate of 1000 sccm for 5 minutes at a 1: 1 ratio, followed by supplying N 2 gas at 1000 sccm for 10 minutes. The process of injecting Cl 2 gas and N 2 mixed gas again and then supplying N 2 gas is repeated three times. After injecting only N 2 , the sample is transferred to a high-temperature reactor at a second temperature of 1200 ° C., and the sample is maintained in a flowing condition of N 2 gas atmosphere for 30 minutes, followed by cooling.
Comparative Example 1
20 g of the carbon nanotubes prepared in Preparation Example 1 were placed in a fluidized bed reactor.
The inside of the reactor was purged with an inert gas atmosphere of N 2 , and then the temperature was raised to 1500 ° C. After 1 hour, the substrate was spontaneously cooled under a fixed bed condition of N 2 atmosphere, and a metal debris removal process using only heat treatment was performed.
The contents of Fe, Co, Mo, V, and Cr in carbon nanotubes were measured by ICP (inductively coupled plasma spectrometry) analysis of the carbon nanotubes of the examples and comparative examples.
Continuous infusion
Pulse injection
As can be seen from the above, according to the CNT purification method of the present invention, it can be confirmed that the gas raw material and time consumed in the process can be saved, and an efficient process can be performed.
It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention. something to do. It is therefore intended that the scope of the invention be defined by the claims appended hereto and their equivalents.
Claims (16)
Wherein the carbon nanotubes containing the residual metal are reacted with the halogen-containing gas under an inert gas atmosphere to remove the CNTs.
The purification method
A first step of raising the temperature of the carbon nanotube containing impurities including the residual metal to a first temperature (T1) in an inert gas atmosphere to react with the halogen-containing gas to halogenize the impurities; And
A second step of heating at a second temperature (T2) higher than the first temperature to evaporate the halogenated impurities and remove the carbon nanotubes through a gas outlet, and obtaining purified carbon nanotubes through a CNT outlet;
(CNT). ≪ / RTI >
Wherein the first temperature (T1) is 600 占 폚 to 1000 占 폚.
And the second temperature (T2) is T1 + 100 DEG C or more.
Wherein the purification method is carried out in a continuous process using one fluidized bed reactor.
Wherein the purification method is carried out in a continuous process using two fluidized bed reactors, wherein the first step is carried out in a first fluidized bed reactor and the second step is carried out in a second fluidized bed reactor.
And cooling the purified CNT discharged through the CNT outlet.
Wherein the halogen-containing gas is a gas containing fluorine, chlorine, bromine, iodine or a mixed component thereof.
Wherein the halogen-containing gas is a gas containing chlorine gas or trichloromethane gas or a mixed component thereof.
Wherein the inert gas is a gas containing nitrogen, helium, neon, argon, krypton, xenon, radon or a mixture thereof.
Wherein the gas injection method includes a purge method, a pulse method, a continuous injection method, or an injection method in which a combination thereof is used.
Wherein the pressure of the inert gas is 500 torr to 800 torr.
Wherein the pressure of the halogen-containing gas is 500 torr to 900 torr.
And neutralizing the halogenated impurities recovered from the gas outlet.
The neutralization treatment is preferably carried out in the presence of at least one selected from the group consisting of silver nitrate (AgNO 3 ), sodium thiosulfate (Na 2 S 2 O 3 ), sodium chloride (NaCl), potassium thiocyanate (KSCN), ammonium thiocyanate (NH 4 SCN) (NaOH), calcium hydroxide (Ca (OH) 2 ), or a combination thereof.
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| PCT/KR2016/009568 WO2017069393A1 (en) | 2015-10-23 | 2016-08-29 | Cnt purification method using fluidized bed reactor |
| CN201680004658.7A CN107108222A (en) | 2015-10-23 | 2016-08-29 | Utilize the CNT purification process of fluidized-bed reactor |
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| CN108946704B (en) * | 2018-08-20 | 2020-03-31 | 山东晶石大展纳米科技有限公司 | Method and device for continuously preparing high-purity carbon nano tube |
| CN110655063A (en) * | 2019-11-07 | 2020-01-07 | 赛福纳米科技(徐州)有限公司 | Carbon nanotube purification device and purification method |
| CN111362255B (en) * | 2020-03-10 | 2021-10-22 | 内蒙古骏成新能源科技有限公司 | Carbon nano tube fluidization purification process method and fluidized bed reaction device |
| CN111498835A (en) * | 2020-04-27 | 2020-08-07 | 内蒙古骏成新能源科技有限公司 | Horizontal fluidizing device for gas-phase purification of carbon nano tube and fluidizing purification method |
| CN115215327B (en) * | 2022-02-23 | 2023-10-03 | 无锡东恒新能源科技有限公司 | Device and method for purifying carbon nano tube |
| CN116281964B (en) * | 2023-05-22 | 2023-08-11 | 湖南科晶新能源科技有限公司 | Efficient carbon nano tube purification method and purification equipment |
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| CN103407984A (en) * | 2013-07-16 | 2013-11-27 | 清华大学 | Carbon nano-tube purification method based on weak oxidizing atmosphere oxidation assisted acid treatment |
| CN104401963A (en) * | 2014-10-27 | 2015-03-11 | 山东诚合新材料有限公司 | Carbon nanotube purification method capable of removing residual metals |
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| US20020159944A1 (en) * | 2001-02-12 | 2002-10-31 | William Marsh Rice University | Gas-phase process for purifying single-wall carbon nanotubes and compositions thereof |
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