CN112028056A - Method for efficiently purifying carbon nanotubes by microwave heating - Google Patents
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/17—Purification
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- C—CHEMISTRY; METALLURGY
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- 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
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- C01B32/159—Carbon nanotubes single-walled
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- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/04—Nanotubes with a specific amount of walls
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- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/30—Purity
Abstract
The invention discloses a method for purifying carbon nano tubes with high efficiency by microwave heating, which comprises the steps of firstly utilizing the strong oxidizing property of chlorine, reacting residual metal catalyst in the carbon nano tubes at a certain temperature to generate chloride, and utilizing the characteristic that the gasification temperature of the metal chloride is far lower than that of metal and oxides thereof to gasify the metal chloride and separate the metal chloride from the carbon nano tubes by heating; and then removing carbon impurities such as amorphous carbon, carbon particles and the like in the carbon nano tube by microwave selective heating oxidation in the atmosphere of oxygen or air so as to achieve the purpose of purifying the carbon nano tube. The method does not influence the original appearance of the carbon nano tube basically, is suitable for removing various residual metals in the carbon nano tube, can improve the purity of the carbon nano tube to more than 99.5 percent, has the characteristics of simple method, easy operation, energy conservation, environmental protection, high purification efficiency and the like, and is a technology which is easy to industrialize and can continuously purify the carbon nano tube in batches.
Description
Technical Field
The invention relates to the technical field of purification of carbon nanotubes, in particular to a method for efficiently purifying carbon nanotubes by microwave heating.
Background
The carbon nano tube has excellent performances in various aspects such as mechanics, electricity, thermal, optics and the like, is a novel material which is noticed by the world, and has wide application prospect in the fields of lithium ion battery conductive agents, catalyst carriers, drug carriers, reinforced blending materials, electronic devices and the like. From its discovery, it has attracted the great interest of the disciplines of physics, chemistry and materials. At present, the chemical vapor deposition method is the main method for preparing carbon nanotubes, but the product contains a large amount of impurities such as metal catalyst particles (mainly including Fe, Ni, Co, etc.), amorphous carbon, carbon nanoparticles, etc., and the presence of these impurities seriously affects the performance of carbon nanotubes, restricting the application of carbon nanotubes.
At present, the existing carbon nanotube purification methods mainly include two types: one is an acid cleaning purification method, which mainly uses hydrochloric acid, nitric acid and other strong acids to dissolve residual metal catalysts, but the method is difficult to completely remove the metal catalysts with thicker carbon layer coatings, and generates a large amount of waste acid and waste water to cause environmental pollution; the other method is to adopt a high-temperature heat treatment purification method to carry out heat treatment on the carbon nano tube at about 3000 ℃ so as to gasify the residual metal catalyst, the carbon nano tube obtained by the method has high purity but high energy consumption, and the excessive treatment temperature causes the carbon atoms in the carbon nano tube to be rearranged to cause some unpredictable property changes.
Chlorine gas is used as a strong oxidizing gas, metal catalyst particles are subjected to oxidation reaction at a certain temperature to generate metal chloride, and the metal chloride can be gasified and separated from the carbon nano tube at a lower temperature by utilizing the characteristic that the boiling points of the chloride (such as the boiling points of iron chloride, nickel chloride and cobalt chloride are 315 ℃, 987 ℃ and 1049 ℃ respectively) are far lower than those of a metal simple substance and the oxidation boiling point thereof. Amorphous carbon, carbon nanoparticles and the like are less stable than carbon nanotubes and are easily oxidized, and carbon dioxide or carbon monoxide is generated by oxidation by oxygen or air at a certain temperature and is separated from the carbon nanotubes, so that the high-purity carbon nanotubes are obtained.
In recent years, the application of microwave radiation in chemical reaction is gradually increased due to the penetrability, selectivity and instant heating effect of the microwave radiation, and the carbon nano tube purified by the microwave radiation does not obviously heat a tube layer, and can directly act with metal points on the surface of a catalyst, so that amorphous carbon is oxidized and unnecessary side reactions are reduced. The microwave heating mechanism is different from the conventional heating mechanism, the processing time can be reduced by utilizing microwave assistance, the damage degree of the processing to the carbon nano tube is reduced, and therefore, the microwave heating mechanism plays an important role in the aspect of carbon nano tube purification.
Disclosure of Invention
The invention aims to provide a method for efficiently purifying carbon nano tubes by microwave heating, which enables a metal catalyst to generate chloride by strong oxidizing property of chlorine and oxygen, utilizes the characteristics of low gasification temperature of the metal chloride and easy oxidation of carbon impurities such as amorphous carbon, carbon nano particles and the like of the carbon nano tubes, simultaneously utilizes the penetrability, selectivity and instant heating effect of microwave radiation, can directly act with metal points on the surface of the catalyst, enables the amorphous carbon to be oxidized, reduces unnecessary side reactions and can reduce the treatment time, and reduces the damage degree of the treatment on the carbon nano tubes by microwave radiation heating, thereby achieving the purpose of efficiently purifying the carbon nano tubes and filling the blank in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for efficiently purifying carbon nanotubes by microwave heating comprises the following steps:
s1: placing the carbon nano tube in a microwave heating device, heating the carbon nano tube by microwave radiation under the atmosphere of nitrogen or inert gas, and preserving heat;
s2: keeping the temperature unchanged, introducing chlorine or chlorine mixed gas to enable the chlorine to fully react with the residual metal catalyst in the carbon nano tube to generate metal chloride, continuously introducing the chlorine or the chlorine-containing mixed gas, heating by adopting microwave radiation to enable the generated metal chloride to volatilize from the carbon nano tube, and treating tail gas in the reaction process by using a sodium hydroxide solution;
s3: stopping introducing chlorine gas or mixed gas containing chlorine gas, performing nitrogen gas or inert gas replacement on the device, removing unreacted excessive chlorine gas, introducing oxygen gas or air, heating by adopting microwave, keeping the temperature, stopping heating, cooling the carbon nano tube to room temperature, and taking out the carbon nano tube to obtain the purified carbon nano tube.
Furthermore, the whole process from S1 to S3 is carried out under a gas environment, and the gas used comprises one or more of nitrogen or inert gas, chlorine or chlorine gas mixture and oxygen or air.
Furthermore, the carbon nanotubes in the S1 are one or more of multi-walled carbon nanotubes, single-walled carbon nanotubes and double-walled carbon nanotubes, and the purity thereof is 90-95%.
Furthermore, the residual metal catalyst in the carbon nanotubes in S2 is one or more of Fe system, Ni system and Co system.
Further, the microwave heating process in S1 is performed in a specially-made microwave irradiation apparatus.
Further, the microwave output power of the microwave radiation heating process in S1 is 100W-6000W, and the microwave frequency is 0.3-300 GHz.
Further, the carbon nano tube in the S1 is heated to 100-400 ℃ by microwave radiation for 1-15min under the atmosphere of nitrogen or inert gas and is then insulated for 5-20min
Furthermore, the flow rate of the chlorine or the chlorine mixed gas introduced for the first time in the S2 is 30-80sccm, and the reaction time is 20-60 min; then introducing chlorine or chlorine mixed gas with the flow rate of 10-20 and the reaction time of 5-20 min; the microwave radiation is heated to 350-800 ℃ and kept for 60-90 min.
Furthermore, the flow rate of the introduced oxygen or air in S3 is 30-50sccm, the temperature is controlled at 300-500 ℃ by microwave heating, and the temperature is maintained for 10-30 min.
Compared with the prior art, the invention has the beneficial effects that:
1. the method for efficiently purifying the carbon nano tube by microwave heating has the advantages of simple process, short treatment process, high efficiency, safety, reliability, environmental friendliness and high purification degree of the carbon nano tube after microwave treatment.
2. The method for efficiently purifying the carbon nano tube by microwave heating effectively improves the structural integrity, has high crystallinity, can effectively remove impurities such as metal catalyst, amorphous carbon, carbon nano particles and the like, and effectively improves the purity of the carbon nano tube.
3. The method for efficiently purifying the carbon nano tube by microwave heating does not relate to an acid washing process, reduces the pollution of acid waste liquid treatment on the environment, and reduces the treatment cost.
4. The method for efficiently purifying the carbon nano tube by microwave heating has the advantages of simple process, short treatment period and low energy consumption, greatly reduces the production cost, and can be widely applied to industrial production.
Detailed Description
The following examples will explain the present invention in detail, however, the present invention is not limited thereto. 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.
A method for efficiently purifying carbon nanotubes by microwave heating comprises the following steps:
the first step is as follows: placing the carbon nano tube in a microwave heating device, wherein the microwave heating process is carried out in a special microwave radiation device, heating the carbon nano tube to 100-400 ℃ in the atmosphere of nitrogen or inert gas by microwave radiation for 1-15min, and then preserving heat for 5-20 min; wherein the carbon nano tube is one or more of a multi-wall carbon nano tube, a single-wall carbon nano tube and a double-wall carbon nano tube, the microwave output power in the microwave radiation heating process is 100W-6000W, and the microwave frequency is 0.3-300 GHz;
the second step is that: keeping the temperature unchanged, introducing chlorine or chlorine mixed gas, controlling the gas flow to be 30-80sccm, reacting for 20-60min, fully reacting the chlorine with the residual metal catalyst in the carbon nanotube to generate metal chloride, continuously introducing the chlorine or the chlorine-containing mixed gas, controlling the flow to be 10-20sccm, and reacting for 5-20 min; heating to 350-800 deg.C by microwave radiation, maintaining for 60-90min to volatilize the generated metal chloride from the carbon nanotube, and treating the tail gas in the reaction process with sodium hydroxide solution; wherein, the residual metal catalyst in the carbon nano tube is one or more of Fe system, Ni system and Co system;
the third step: stopping introducing chlorine gas or mixed gas containing chlorine gas, performing nitrogen gas or inert gas replacement on the device, removing unreacted excessive chlorine gas, introducing oxygen gas or air, controlling the gas flow to be 30-50sccm, keeping the temperature at 300-500 ℃ for 10-30min by microwave heating, stopping heating to cool the carbon nano tube to room temperature, and taking out the carbon nano tube to obtain the purified carbon nano tube.
In the above embodiments, the whole process is performed in a gas environment, and the gas used includes one or more of nitrogen or inert gas, chlorine or chlorine gas mixture, and oxygen or air.
The working principle is as follows: the method ensures that the metal catalyst generates chloride through the strong oxidizing property of chlorine and oxygen, utilizes the characteristics of low gasification temperature of the metal chloride and easy oxidation of carbon nano-tubes by carbon impurities such as amorphous carbon, carbon nano-particles and the like, simultaneously utilizes the penetrability, selectivity and instant heating function of microwave radiation, can directly act with metal points on the surface of the catalyst, ensures that the amorphous carbon is oxidized, reduces unnecessary side reactions and can reduce the treatment time, and reduces the damage degree of the treatment on the carbon nano-tubes through the microwave radiation heating, thereby achieving the purpose of efficiently purifying the carbon nano-tubes.
In order to further explain the above invention better, the following specific examples are also provided:
example 1:
a method for efficiently purifying carbon nanotubes by microwave heating comprises the following steps:
the method comprises the following steps: placing 10g of multi-walled carbon nanotubes synthesized by a 93% Fe catalyst in a microwave heating device, heating by microwave radiation for 5min under nitrogen atmosphere to raise the temperature to 300 ℃, and then preserving the heat for 10 min;
step two: changing chlorine gas to flow through the carbon nano tube at a flow rate of 40sccm for 30min to enable the chlorine gas to react with residual metal catalyst in the carbon nano tube to generate metal chloride, continuing to flow the chlorine gas at a flow rate of 20sccm, heating the carbon nano tube by microwave radiation for 5min to 400 ℃, keeping the temperature for 60min to enable the generated metal chloride to volatilize from the carbon nano tube, and collecting and treating tail gas in the reaction process by using a sodium hydroxide solution;
step three: stopping introducing chlorine, performing nitrogen or inert gas replacement on the device, removing unreacted excessive chlorine, introducing oxygen, controlling the gas flow to be 30min, performing microwave heating, keeping the temperature at 300 ℃ for 30min, stopping heating, cooling the carbon nano tube to room temperature, and taking out to obtain the purified carbon nano tube.
Example 2:
a method for efficiently purifying carbon nanotubes by microwave heating comprises the following steps:
the method comprises the following steps: placing 10g of multi-walled carbon nanotubes synthesized by a Fe and Co catalyst with the purity of 95% in a microwave heating device, heating the multi-walled carbon nanotubes by microwave radiation for 8min under the atmosphere of inert gas to raise the temperature to 450 ℃, and then preserving the heat for 15 min;
step two: changing chlorine gas into chlorine gas at a flow rate of 35sccm for 50min to enable the chlorine gas to react with residual metal catalyst in the carbon nano tube to generate metal chloride, continuing to introduce the chlorine gas at a flow rate of 10sccm, heating by microwave radiation for 10min to 800 ℃ for 60min to enable the generated metal chloride to volatilize from the carbon nano tube, and collecting and treating tail gas in the reaction process by using a sodium hydroxide solution;
step three: stopping introducing chlorine, performing nitrogen or inert gas replacement on the device, removing unreacted excessive chlorine, introducing oxygen, controlling the gas flow to be 30min, performing microwave heating, keeping the temperature at 300 ℃ for 30min, stopping heating, cooling the carbon nano tube to room temperature, and taking out to obtain the purified carbon nano tube.
Example 3:
a method for efficiently purifying carbon nanotubes by microwave heating comprises the following steps:
the method comprises the following steps: placing 10g of multi-walled carbon nanotubes synthesized by Fe and Ni catalysts with the purity of 94% in a microwave heating device, heating by microwave radiation for 5min under the nitrogen atmosphere to raise the temperature to 400 ℃, and then preserving the heat for 15 min;
step two: changing chlorine gas to flow through the carbon nano tube at a flow rate of 50sccm for 30min to enable the chlorine gas to react with residual metal catalyst in the carbon nano tube to generate metal chloride, continuing to flow the chlorine gas at a flow rate of 10sccm, heating the carbon nano tube by microwave radiation for 5min to 650 ℃, keeping the temperature for 80min to enable the generated metal chloride to volatilize from the carbon nano tube, and collecting and treating tail gas in the reaction process by using a sodium hydroxide solution;
step three: stopping introducing chlorine gas, performing nitrogen gas or inert gas replacement on the device, removing unreacted redundant chlorine gas, introducing oxygen gas, controlling the gas flow to be 30sccm, performing microwave heating, controlling the temperature to be 500 ℃, keeping the temperature for 15min, stopping heating, cooling the carbon nano tube to the room temperature, and taking out the carbon nano tube to obtain the purified carbon nano tube.
Example 4:
a method for efficiently purifying carbon nanotubes by microwave heating comprises the following steps:
the method comprises the following steps: placing 10g of multi-walled carbon nanotubes synthesized by Co catalyst with purity of 95% in a microwave heating device, heating by microwave radiation for 5min under nitrogen atmosphere to raise the temperature to 400 ℃, and then preserving heat for 20 min;
step two: changing chlorine gas to flow through the carbon nano tube at a flow rate of 60sccm for 25min to enable the chlorine gas to react with residual metal catalyst in the carbon nano tube to generate metal chloride, continuing to flow the chlorine gas at a flow rate of 15sccm, heating the carbon nano tube by microwave radiation for 15min to 800 ℃ and keeping the temperature for 80min to enable the generated metal chloride to volatilize from the carbon nano tube, and collecting and treating tail gas in the reaction process by using a sodium hydroxide solution;
step three: stopping introducing chlorine gas, performing nitrogen gas or inert gas replacement on the device, removing unreacted redundant chlorine gas, introducing oxygen gas, controlling the gas flow to be 40sccm, performing microwave heating, controlling the temperature to be 450 ℃, keeping the temperature for 20min, stopping heating, cooling the carbon nano tube to the room temperature, and taking out the carbon nano tube to obtain the purified carbon nano tube.
Example 5:
a method for efficiently purifying carbon nanotubes by microwave heating comprises the following steps:
the method comprises the following steps: placing 10g of double-wall carbon nano tube synthesized by Ni and Co catalysts with the purity of 91 percent in a microwave heating device, heating the double-wall carbon nano tube by microwave radiation for 5min under the nitrogen atmosphere and keeping the temperature for 15min after the temperature is raised to 400 ℃;
step two: keeping the temperature unchanged, changing chlorine gas mixed gas, controlling the flow rate to be 80sccm, controlling the time to be 30min to enable the chlorine gas to react with the residual metal catalyst in the carbon nano tube to generate metal chloride, continuously introducing the chlorine gas/nitrogen gas mixed gas (the volume ratio of the chlorine gas to the nitrogen gas is 1:9), controlling the flow rate to be 10sccm, heating by microwave radiation for 5min to 800 ℃, keeping the temperature for 70min to enable the generated metal chloride to volatilize from the carbon nano tube, and collecting and treating tail gas in the reaction process by using a sodium hydroxide solution;
step three: stopping introducing chlorine gas, performing nitrogen gas or inert gas replacement on the device, removing unreacted redundant chlorine gas, introducing oxygen gas, controlling the gas flow to be 30sccm, performing microwave heating, controlling the temperature to be 450 ℃, keeping the temperature for 10min, stopping heating, cooling the carbon nano tube to the room temperature, and taking out the carbon nano tube to obtain the purified carbon nano tube.
Example 6:
a method for efficiently purifying carbon nanotubes by microwave heating comprises the following steps:
the method comprises the following steps: placing 10g of single-walled carbon nanotubes synthesized by a Ni catalyst with the purity of 90% in a microwave heating device, heating the single-walled carbon nanotubes by microwave radiation for 5min under the nitrogen atmosphere and with the gas flow of 40sccm to 400 ℃, and then preserving the heat for 15 min;
step two: keeping the temperature unchanged, introducing a chlorine/argon gas mixture (the volume ratio of chlorine to argon is 5:95), controlling the flow rate to be 65sccm, reacting the chlorine gas with the residual metal catalyst in the carbon nano tube for 40min to generate metal chloride, continuously introducing the chlorine/argon gas mixture, controlling the flow rate to be 20sccm, heating by microwave radiation for 10min to 600 ℃, keeping the temperature for 50min to volatilize the generated metal chloride from the carbon nano tube, and collecting and treating tail gas in the reaction process by using a sodium hydroxide solution;
step three: stopping introducing chlorine gas, performing nitrogen gas or inert gas replacement on the device, removing unreacted excessive chlorine gas, introducing air, controlling the gas flow to be 50sccm, performing microwave heating, controlling the temperature to be 350 ℃, keeping the temperature for 10min, stopping heating, cooling the carbon nano tube to the room temperature, and taking out the carbon nano tube to obtain the purified carbon nano tube.
Index testing
The index tests of the above examples 1-6 were carried out by the following specific test methods:
a. and (3) detecting the metal content: weighing a certain mass of purified carbon nanotubes, placing the purified carbon nanotubes in prepared aqua regia, heating and boiling for 1h, cooling and filtering, diluting the filtrate, detecting the amount of metal ions in the diluent by adopting an atomic absorption method, calculating the metal content in the purified carbon nanotubes, and detecting results are shown in table 1.
b. Ash content: weighing 3 parts of purified carbon nano tube with a certain mass, placing the purified carbon nano tube into a crucible, placing the crucible into a muffle furnace, calcining at 900 ℃ for 4 hours, taking out the crucible, weighing the residual mass, calculating the ash content, and detecting results are shown in table 1.
The results of the index test of each example are shown in table 1:
TABLE 1
| Serial number | Total metal content after purification (ppm) | Ash content (%) |
| Example 1 | 9.2 | 0.1 |
| Example 2 | 12.35 | 0.15 |
| Example 3 | 10.28 | 0.11 |
| Example 4 | 10.8 | 0.12 |
| Example 5 | 8.64 | 0.098 |
| Example 6 | 7.25 | 0.095 |
As can be seen from the data in table 1, the method for efficiently purifying carbon nanotubes by microwave heating provided by the present invention has a significant effect on the purification of various types of carbon nanotubes, and the purity of the carbon nanotubes after purification reaches more than 99.5%, so that the present invention is suitable for the purification of carbon nanotubes of various metal catalyst systems, and can effectively remove carbon impurities such as amorphous carbon, carbon nanoparticles, etc., to obtain high-purity carbon nanotubes, and the process is simple and easy for industrial production.
Appropriate changes and modifications to the embodiments described above will become apparent to those skilled in the art from the disclosure and teachings of the foregoing description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (9)
1. A method for efficiently purifying carbon nanotubes by microwave heating is characterized by comprising the following steps:
s1: placing the carbon nano tube in a microwave heating device, heating the carbon nano tube by microwave radiation under the atmosphere of nitrogen or inert gas, and preserving heat;
s2: keeping the temperature unchanged, introducing chlorine or chlorine mixed gas to enable the chlorine to fully react with the residual metal catalyst in the carbon nano tube to generate metal chloride, continuously introducing the chlorine or the chlorine-containing mixed gas, heating by adopting microwave radiation to enable the generated metal chloride to volatilize from the carbon nano tube, and treating tail gas in the reaction process by using a sodium hydroxide solution;
s3: stopping introducing chlorine gas or mixed gas containing chlorine gas, performing nitrogen gas or inert gas replacement on the device, removing unreacted excessive chlorine gas, introducing oxygen gas or air, heating by adopting microwave, keeping the temperature, stopping heating, cooling the carbon nano tube to room temperature, and taking out the carbon nano tube to obtain the purified carbon nano tube.
2. The method for microwave heating efficient purification of carbon nanotubes as claimed in claim 1, wherein the whole process of S1-S3 is performed under a gas environment, and the gas used comprises one or more of nitrogen or inert gas, chlorine or chlorine mixture, and oxygen or air.
3. The method for microwave heating highly efficient purification of carbon nanotubes as claimed in claim 1, wherein the carbon nanotubes in S1 are one or more of multi-walled carbon nanotubes, single-walled carbon nanotubes, double-walled carbon nanotubes, and the purity thereof is 90-95%.
4. The method for microwave heating efficient purification of carbon nanotubes as claimed in claim 1, wherein the residual metal catalyst in the carbon nanotubes in S2 is one or more of Fe system, Ni system and Co system.
5. The method for microwave heating highly efficient purification of carbon nanotubes as claimed in claim 1, wherein the microwave heating process in S1 is performed in a specially prepared microwave irradiation apparatus.
6. The method for microwave heating highly effective purification of carbon nanotubes as claimed in claim 1, wherein the microwave radiation heating process in S1 has microwave output power of 100W-6000W and microwave frequency of 0.3-300 GHz.
7. The method for microwave heating high-efficiency purification of carbon nanotubes as claimed in claim 1, wherein the carbon nanotubes in S1 are heated to 100-400 ℃ by microwave radiation for 5-20min under nitrogen or inert gas atmosphere for 1-15 min.
8. The method for microwave heating efficient purification of carbon nanotubes as claimed in claim 1, wherein the flow rate of the chlorine gas or the chlorine gas mixture introduced for the first time in S2 is 30-80sccm, and the reaction time is 20-60 min; then introducing chlorine or chlorine mixed gas with the flow rate of 10-20 and the reaction time of 5-20 min; the microwave radiation is heated to 350-800 ℃ and kept for 60-90 min.
9. The method for purifying carbon nanotubes by microwave heating as claimed in claim 1, wherein the flow rate of the introduced oxygen or air in S3 is 30-50sccm, the temperature of microwave heating is controlled at 300-500 ℃ and the temperature is maintained for 10-30 min.
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