CN115536005A - Carbon nano tube purification method - Google Patents
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- CN115536005A CN115536005A CN202211347132.2A CN202211347132A CN115536005A CN 115536005 A CN115536005 A CN 115536005A CN 202211347132 A CN202211347132 A CN 202211347132A CN 115536005 A CN115536005 A CN 115536005A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 115
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 115
- 238000000034 method Methods 0.000 title claims abstract description 53
- 238000000746 purification Methods 0.000 title claims abstract description 28
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 40
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000007789 gas Substances 0.000 claims abstract description 35
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 18
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 46
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- 230000035484 reaction time Effects 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 4
- 238000005243 fluidization Methods 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 238000005406 washing Methods 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 2
- 230000009471 action Effects 0.000 description 12
- 239000012299 nitrogen atmosphere Substances 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000011852 carbon nanoparticle Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002079 double walled nanotube Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000006181 electrochemical material Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/159—Carbon nanotubes single-walled
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/17—Purification
Abstract
The invention relates to the technical field of carbon nanotubes, in particular to a carbon nanotube purification method. The method comprises the following steps: (1) Mixing the carbon nano tube with ammonium chloride solid powder in a first container, and reacting at 350-400 ℃; (2) The carbon nano tube treated in the step (1) is in contact with fluidizing gas, oxygen and carbon dioxide in a second container, and the reaction temperature is 640 to 690 ℃; (3) And (3) mixing the carbon nano tubes treated in the step (2) with fluidizing gas in a third container for cooling. The purification method of the invention has no procedures of acid washing, water treatment and high energy consumption drying, avoids the problems of high energy consumption and serious damage to the conductivity of the carbon nano tube caused by high-temperature purification, has simple and convenient process and low operation energy consumption, can realize continuous large-scale purification of the carbon nano tube, and can ensure that the purity of the carbon nano tube can reach more than 99.9 percent.
Description
Technical Field
The invention relates to the technical field of carbon nanotubes, in particular to a carbon nanotube purification method.
Background
Preparation of C from vacuum arc evaporation of graphite electrode by Lijima since 1991 60 The experimental products of (a) unexpectedly found that since the multi-walled carbon nanotube, the carbon nanotube, as a one-dimensional nanomaterial, has been widely developed and applied due to its high mechanical strength, excellent electrical conductivity, and high specific surface area. The carbon nanotube is mainly a single-layer or multi-layer coaxial circular tube formed by hexagonally arranged carbon atoms. It has a very large aspect ratio, typically between 1-100nm in diameter and several microns to hundreds of microns in length. Due to the large length-diameter ratio, the carbon nano tube has excellent mechanical, electrical, electric conduction and heat conduction performances. The carbon nano tube has wide potential application prospect in the fields of lithium ion batteries, coatings, catalyst carriers, rubber plastic composite materials, electrochemical materials, photoelectric sensing and the like.
The preparation method of the carbon nano tube comprises the following steps: graphite arc process, chemical vapor deposition process, laser evaporation graphite process, template process, condensed phase electrolysis process, organic plasma jet process, etc. Among them, the graphite arc method and the chemical vapor deposition method are the most widely used preparation methods at present. The carbon nanotubes prepared by these methods are accompanied by considerable amounts of impurities such as carbon nanoparticles, amorphous carbon, catalysts, and the like. The existence of these impurities has greatly hindered the application of carbon nanotubes in various fields, and therefore, research on the purification technology of carbon nanotubes is urgent. The existing industrialized batch purification method of the carbon nano tube mainly comprises the following steps: chemical oxidation, gas phase oxidation, liquid phase acid washing, high temperature purification, etc. However, these methods have various problems, and the purity of purification by chemical oxidation and gas phase oxidation is limited; the acid washing method needs to be repeatedly washed by purified water until the pH value is close to neutral, so that more waste water is generated, the using amount of water resources is large, and the waste water needs to be dried again after being washed, so that a large amount of electric energy or natural gas energy is consumed, and the energy conservation and emission reduction are not facilitated; the purification of carbon nanotubes by the high-temperature purification method requires high temperature of 1800-2500 ℃, has extremely high energy consumption and extremely high damage to the conductivity of the carbon nanotubes, so the invention of the method for continuously purifying the carbon nanotubes in batches with low energy consumption is urgently needed.
Disclosure of Invention
Aiming at the technical problems of non-ideal purification effect, large resource and energy consumption and loss of carbon nano tube performance of the existing industrialized mass purification method of the carbon nano tube, the invention provides the purification method of the carbon nano tube, which has no procedures of acid washing, water treatment and high energy consumption drying, avoids the problems of high energy consumption and serious damage of carbon nano tube conductivity caused by high-temperature purification, has simple and convenient process and low operation energy consumption, can realize continuous mass purification of the carbon nano tube, and can achieve the purity of the carbon nano tube of more than 99.9 percent.
The technical scheme of the invention is as follows:
a carbon nano tube purification method comprises the following steps:
(1) Mixing the carbon nano tube with ammonium chloride solid powder in a first container, and reacting at 350-400 ℃;
(2) The carbon nano tube treated in the step (1) is contacted with fluidizing gas, oxygen and carbon dioxide in a second container, and the reaction temperature is 640-690 ℃;
(3) And (3) mixing the carbon nano tubes treated in the step (2) with fluidizing gas in a third container for cooling.
Furthermore, the purification method is suitable for single-wall carbon nanotubes, double-wall carbon nanotubes or multi-wall carbon nanotubes; the carbon nano tube can be in the form of powder, granules, blocks or the mixture of the powder, the granules, the blocks and the mixture of the three; the carbon nanotubes may be prepared by a graphite arc method, a chemical vapor deposition method, a laser evaporation graphite method, a template method, a condensed phase electrolysis method, an organic plasma spray method, with or without a metal catalyst, such as iron, cobalt, nickel, magnesium, aluminum, manganese, molybdenum, vanadium, etc.
Further, in the step (1), the reaction is carried out in a fluidizing gas atmosphere, ammonium chloride accounts for 0.5-2% of the weight of the carbon nano tube, and the reaction time is 20-40min.
Further, in the step (1), preferably, the carbon nanotubes are placed in a fluidizing gas atmosphere in a first container, and ammonium chloride solid powder is added, wherein the ammonium chloride accounts for 1% of the weight of the carbon nanotubes, the reaction temperature is 370 ℃, and the reaction time is 30min.
Further, the carbon nanotubes are processed in the step (1) and then enter the second container under the action of the thrust force of the fluidizing gas flow.
Further, in the step (2), continuously introducing fluidizing gas, oxygen and carbon dioxide into the second container, wherein the flow speed of the fluidizing gas is 500 to 600m 3 The flow rate of oxygen is 200 to 300m 3 The flow rate of the carbon dioxide is 300 to 350m 3 The reaction time is 10 to 30min.
Further, the reaction temperature in the step (2) is preferably 670 ℃, and the reaction time is preferably 20min.
Further, the carbon nanotubes are processed in the step (2) and then enter a third container under the action of the pushing force of the fluidizing gas flow.
Further, in the step (3), continuously introducing fluidizing gas into the third container, wherein the flow speed of the fluidizing gas is 300-350m 3 And h, cooling for about 30min until the temperature of the carbon nano tube is reduced to room temperature.
Further, the fluidizing gas flow rate in the step (3) is preferably 320m 3 /h。
Further, the fluidizing gas is nitrogen or argon.
The invention has the beneficial effects that:
according to the invention, ammonium chloride powder is used as a reaction reagent, and metal impurities of the carbon nano tube are effectively removed at the temperature of 350-400 ℃; nitrogen or argon is used as fluidizing gas, carbon dioxide is used as reducing gas, and oxygen is used as oxidizing gas, so that the impure carbon substances are effectively removed;
according to the invention, impurities can be removed on the premise of not damaging the carbon tube, a pickling method is avoided, a large amount of water washing purification is avoided, the waste of water resources is effectively reduced, the subsequent sewage treatment process is also avoided, and the cost is saved; high energy consumption of the high-temperature purification method is avoided. The method has the advantages of simple process, convenient and quick operation, low cost and the like, has good product purity uniformity and good batch stability, is suitable for continuous batch purification of the carbon nanotubes, and ensures that the purity of the obtained carbon nanotubes reaches over 99.9 percent.
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
Fig. 1 is a TEM image of a low purity carbon nanotube in the prior art.
Fig. 2 is a TEM image of the high purity carbon nanotube purified in example 1.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The method for purifying the low-purity carbon nano tube by using the fluidized bed comprises the following steps:
(1) Placing the carbon nano tube in a first storage tank of a fluidized bed, and adding ammonium chloride solid powder in the nitrogen atmosphere, wherein the weight of the ammonium chloride is 1 percent of that of the carbon nano tube, the reaction temperature is 370 ℃, and the reaction time is 20min.
(2) After the carbon nano tube is treated in the step (1), the carbon nano tube enters a second storage tank of the fluidized bed under the action of the thrust force of nitrogen airflow, and nitrogen, oxygen and carbon dioxide are continuously introduced into the second storage tank, wherein the flow velocity of the nitrogen is 550m 3 Flow rate of oxygen gas of 250m 3 Flow rate of carbon dioxide at 330 m/h 3 The reaction temperature is 680 ℃ and the reaction time is 20min.
(3) After the carbon nano tube is treated in the step (2), the carbon nano tube enters a third storage tank of the fluidized bed under the action of the thrust force of nitrogen airflow, and nitrogen is continuously introduced into the third storage tank to ensure that the carbon nano tube is kept at the flow velocity of 330m 3 And in the nitrogen atmosphere, cooling for about 30min until the temperature of the carbon nano tube is reduced to room temperature, and obtaining the carbon nano tube with the purity of more than 99.9 percent.
Example 2
The method for purifying the low-purity carbon nano tube by using the fluidized bed comprises the following steps:
(1) Placing the carbon nano tube in a first storage tank of a fluidized bed, and adding ammonium chloride solid powder in the nitrogen atmosphere, wherein the weight of the ammonium chloride is 1 percent of that of the carbon nano tube, the reaction temperature is 370 ℃, and the reaction time is 20min.
(2) After the carbon nano tube is treated in the step (1), the carbon nano tube enters a second storage tank under the action of the pushing force of argon gas flow, argon gas, oxygen and carbon dioxide are continuously introduced into the second storage tank, and the flow velocity of the argon gas is 500m 3 The flow rate of oxygen is 250m 3 Flow rate of carbon dioxide at 330 m/h 3 The reaction temperature is 680 ℃ and the reaction time is 20min.
(3) After the carbon nano tube is treated in the step (2), the carbon nano tube enters a third storage tank under the action of the pushing force of argon gas flow, and argon gas is continuously introduced into the third storage tank, so that the carbon nano tube is kept at the flow velocity of 330m 3 And in the argon atmosphere, cooling for about 30min until the temperature of the carbon nano tube is reduced to room temperature to obtain the carbon nano tube with the purity of more than 99.9 percent.
Example 3
The method for purifying the low-purity carbon nano tube by using the fluidized bed comprises the following steps:
(1) Placing the carbon nano tube in a first storage tank of a fluidized bed, and adding ammonium chloride solid powder in a nitrogen atmosphere, wherein the weight of the ammonium chloride is 0.5 percent of that of the carbon nano tube, the reaction temperature is 370 ℃, and the reaction time is 20min.
（2）After the carbon nano tube is treated in the step (1), the carbon nano tube enters a second storage tank under the action of the thrust force of nitrogen airflow, and nitrogen, oxygen and carbon dioxide are continuously introduced into the second storage tank, wherein the flow rate of the nitrogen is 550m 3 H, flow rate of oxygen 250m 3 Flow rate of carbon dioxide at 330 m/h 3 The reaction temperature is 690 ℃ and the reaction time is 20min.
(3) After the carbon nano tube is treated in the step (2), the carbon nano tube enters a third storage tank under the action of the pushing force of the nitrogen airflow, and the nitrogen is continuously introduced into the third storage tank, so that the carbon nano tube is kept at the flow velocity of 320m 3 And in the nitrogen atmosphere, cooling for about 30min until the temperature of the carbon nano tube is reduced to room temperature, and obtaining the carbon nano tube with the purity of more than 99.9 percent.
Example 4
Purifying the low-purity carbon nano tube by using a fluidized bed, wherein the purification method comprises the following steps:
(1) Placing the carbon nano tube in a first storage tank of a fluidized bed, and adding ammonium chloride solid powder in the nitrogen atmosphere, wherein the weight of the ammonium chloride is 2 percent of that of the carbon nano tube, the reaction temperature is 350 ℃, and the reaction time is 40min.
(2) After the carbon nano tube is treated in the step (1), the carbon nano tube enters a second storage tank under the action of the pushing force of the nitrogen airflow, and nitrogen, oxygen and carbon dioxide are continuously introduced into the second storage tank, wherein the flow velocity of the nitrogen is 600m 3 H, flow rate of oxygen gas 200m 3 Flow rate of carbon dioxide is 350m 3 The reaction temperature is 645 ℃ and the reaction time is 30min.
(3) After the carbon nano tube is treated in the step (2), the carbon nano tube enters a third storage tank under the action of the pushing force of the nitrogen airflow, and the nitrogen is continuously introduced into the third storage tank, so that the carbon nano tube is kept at the flow velocity of 300m 3 And in the nitrogen atmosphere, cooling for about 30min until the temperature of the carbon nano tube is reduced to room temperature, and obtaining the carbon nano tube with the purity of more than 99.9 percent.
Example 5
Purifying the low-purity carbon nano tube by using a fluidized bed, wherein the purification method comprises the following steps:
(1) Placing the carbon nano tube in a first storage tank of a fluidized bed, and adding ammonium chloride solid powder in a nitrogen atmosphere, wherein the weight of the ammonium chloride is 1 percent of that of the carbon nano tube, the reaction temperature is 370 ℃, and the reaction time is 30min.
(2) After the carbon nano tube is treated in the step (1), the carbon nano tube enters a second storage tank under the action of the pushing force of the nitrogen airflow, nitrogen, oxygen and carbon dioxide are continuously introduced into the second storage tank, and the flow rate of the nitrogen is 530m 3 H, flow rate of oxygen 270m 3 Flow rate of carbon dioxide at 340 m/h 3 H, the reaction temperature is 670 ℃, and the reaction time is 20min.
(3) After the carbon nano tube is treated in the step (2), the carbon nano tube enters a third storage tank under the action of the pushing force of the nitrogen airflow, and the nitrogen is continuously introduced into the third storage tank, so that the carbon nano tube is kept at the flow velocity of 320m 3 In nitrogen atmosphere, cooling for about 30min until the temperature of the carbon nano tube is reduced to room temperature, and obtaining the carbon nano tube with the purity of more than 99.9 percent.
Although the present invention has been described in detail by referring to the drawings in connection with the preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and these modifications or substitutions are within the scope of the present invention/any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention.
Claims (10)
1. A carbon nanotube purification method is characterized by comprising the following steps:
(1) Mixing the carbon nano tube with ammonium chloride solid powder in a first container, and reacting at 350-400 ℃;
(2) The carbon nano tube treated in the step (1) is in contact with fluidizing gas, oxygen and carbon dioxide in a second container, and the reaction temperature is 640 to 690 ℃;
(3) And (3) mixing the carbon nano tubes treated in the step (2) with fluidizing gas in a third container for cooling.
2. The method for purifying carbon nanotubes in claim 1, wherein in the step (1), the reaction is performed in a fluidized gas atmosphere, the weight of ammonium chloride is 0.5-2% of the weight of the carbon nanotubes, and the reaction time is 20-40min.
3. The method of claim 1, wherein the step (1) comprises placing the carbon nanotubes in a fluidized gas atmosphere in a first container, adding ammonium chloride solid powder, wherein the ammonium chloride is 1% of the weight of the carbon nanotubes, the reaction temperature is 370 ℃, and the reaction time is 30min.
4. The method for purifying carbon nanotubes recited in claim 1, wherein the carbon nanotubes are introduced into the second container by the driving force of the fluidizing gas stream after being treated in the step (1).
5. The carbon nanotube purification method of claim 1, wherein in the step (2), the fluidizing gas, the oxygen and the carbon dioxide are continuously introduced into the second container, and the flow rate of the fluidizing gas is 500 to 600m 3 The flow rate of oxygen is 200 to 300m 3 The flow rate of the carbon dioxide is 300 to 350m 3 The reaction time is 10 to 30min.
6. The method for purifying carbon nanotubes in claim 5, wherein the reaction temperature in step (2) is 670 ℃ and the reaction time is 20min.
7. The method for purifying carbon nanotubes as claimed in claim 1, wherein the carbon nanotubes are introduced into the third container by the thrust of the fluidizing gas stream after being treated in step (2).
8. The method for purifying carbon nanotubes as claimed in claim 1, wherein in the step (3), the fluidization is continuously introduced into the third containerThe flow rate of the fluidizing gas is 300 to 350m 3 And/h, until the temperature of the carbon nano tube is reduced to the room temperature.
9. The carbon nanotube purification method of claim 8, wherein the fluidizing gas flow rate of step (3) is 320m 3 /h。
10. The method for purifying carbon nanotubes as claimed in claim 1, wherein the fluidizing gas is nitrogen or argon.
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| CN202211347132.2A CN115536005B (en) | 2022-10-31 | Carbon nano tube purification method |
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| CN202211347132.2A CN115536005B (en) | 2022-10-31 | Carbon nano tube purification method |
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| CN115536005B CN115536005B (en) | 2024-04-19 |
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|---|---|---|---|---|
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| CN101941691A (en) * | 2010-09-21 | 2011-01-12 | 上海大学 | Preparation method of single-walled carbon nanotube |
| CN106315560A (en) * | 2016-08-22 | 2017-01-11 | 赖世权 | Carbon nanotube purification method |
| CN112978717A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Method for shortening carbon nano tube |
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041427A (en) * | 2006-03-22 | 2007-09-26 | 索尼株式会社 | Manufacturing method of carbon material, carbon material and manufacturing method of electronic components |
| CN101941691A (en) * | 2010-09-21 | 2011-01-12 | 上海大学 | Preparation method of single-walled carbon nanotube |
| CN106315560A (en) * | 2016-08-22 | 2017-01-11 | 赖世权 | Carbon nanotube purification method |
| CN112978717A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Method for shortening carbon nano tube |
Non-Patent Citations (1)
| Title |
|---|
| YUN CHEN等: "Purification of double-walled carbon nanotube macro-films", 《NEWJ.CHEM》, pages 542 * |
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