CN117285032A - Carbon nanotube preparation system and single-walled carbon nanotube preparation process - Google Patents
Carbon nanotube preparation system and single-walled carbon nanotube preparation process Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 57
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 54
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 54
- 239000002109 single walled nanotube Substances 0.000 title claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 40
- 238000002347 injection Methods 0.000 claims abstract description 29
- 239000007924 injection Substances 0.000 claims abstract description 29
- 238000000889 atomisation Methods 0.000 claims abstract description 11
- 238000010924 continuous production Methods 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 52
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 17
- 239000012159 carrier gas Substances 0.000 claims description 15
- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical compound SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 13
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 229910052717 sulfur Inorganic materials 0.000 claims description 9
- 239000011593 sulfur Substances 0.000 claims description 9
- 239000007795 chemical reaction product Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- 229930192474 thiophene Natural products 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- 229960002089 ferrous chloride Drugs 0.000 claims description 3
- 150000002505 iron Chemical class 0.000 claims description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 3
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 12
- 239000000047 product Substances 0.000 description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 7
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- 238000004050 hot filament vapor deposition Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 238000001237 Raman spectrum Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000004964 aerogel Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
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- 230000001105 regulatory effect Effects 0.000 description 2
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 239000011825 aerospace material Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000009530 blood pressure measurement Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 ethanesulfide Chemical compound 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000006199 nebulizer Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/02—Single-walled nanotubes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a carbon nanotube preparation system and a single-wall carbon nanotube preparation process, and relates to the technical field of carbon nanotube material preparation. The carbon nanotube preparation system of the present invention includes: the device comprises a liquid sample injection system, an atomization chamber, a pressure control system, an air inlet, a furnace body, a collecting box and a tail gas treatment device; the liquid sample injection system, the atomizing chamber, the furnace body, the collecting box and the tail gas treatment device are sequentially communicated through pipelines; the pressure control system is arranged outside the atomizing chamber; the air inlet is communicated with the atomizing chamber; the tail end of the pipeline of the atomizing chamber which is led into the furnace body is connected with a bell mouth. The invention can realize continuous production of the carbon nano tube on the basis of the preparation system, improves the quality and stability of the product, and can realize high-yield preparation of the high-quality single-wall carbon nano tube by combining with a specific preparation process.
Description
Technical Field
The invention relates to the technical field of carbon nanotube material preparation, in particular to a carbon nanotube preparation system and a single-wall carbon nanotube preparation process.
Background
The carbon nanotube material has great application potential in the fields of electron transmission, heat transmission, mechanical property, electromagnetic wave absorption and the like, and provides new possibility for scientific research and industrial application in a plurality of fields. In the field of electron transport, carbon nanotubes have excellent electrical conductivity and electrical conductivity properties, and can be used as one of the basic elements of high-performance electronic devices. Due to their ultra-thin and high surface charge density characteristics, carbon nanotubes can also be used to fabricate flexible electronic devices, such as flexible displays and wearable devices. In the field of heat transmission, the carbon nano tube has excellent heat conductivity, can be used as a high-performance heat dissipation material for heat dissipation and thermal management of electronic devices, and effectively improves the working stability and service life of the devices. In the field of mechanical properties, the carbon nanotubes have extremely high strength and rigidity, and can enhance the mechanical properties of the composite material. The tensile strength, the rigidity and the wear resistance of the material can be obviously improved by adding a proper amount of carbon nanotubes, and the material is further applied to the fields of automobile tires, aerospace materials and the like. As an electromagnetic wave absorbing material, carbon nanotubes have a wide range of frequency band absorbing ability, and particularly have important applications in the military field. The carbon nanotubes can be used for preparing radar stealth materials, electromagnetic wave absorption coatings and the like, and are beneficial to improving stealth performance and detection recognition capability of military equipment. In the field of chip fabrication, conventional silicon materials gradually approach their physical limits, while carbon nanotubes have excellent electrical properties and dimensional controllability, and are considered as one of candidates for next-generation chip materials. The carbon nano tube can be used for preparing nano-scale transistors, thermoelectric devices and the like, and is hopeful to promote the development of microelectronic technology.
The floating catalytic chemical vapor deposition method is a potential macro preparation process for preparing high-quality single-wall carbon nanotubes and few-wall carbon nanotubes. The floating catalytic chemical vapor deposition method is a potential macro preparation process for preparing high-quality single-wall carbon nanotubes and few-wall carbon nanotubes. The method is characterized in that carbon source gas and catalyst pre-driving particles are injected into a high-temperature furnace together, and the carbon source gas is catalytically decomposed on a catalyst to generate carbon nanotubes. The catalyst particles and the carbon source gas are in a gas phase, so that new catalytic active centers can be continuously provided in the whole reaction process, and the growth of the carbon nano tube is promoted, thereby realizing the preparation with high yield. The floating catalytic chemical vapor deposition method can control the structure and the quantity of the carbon nanotubes by adjusting the proportion of the carbon source gas and the catalyst, and is expected to realize macro preparation of single-wall carbon nanotubes and few-wall carbon nanotubes. The temperature, time and other reaction conditions of the reaction can be controlled to realize the precise control of the quality and structure of the carbon nanotubes.
The floating catalytic chemical vapor deposition method has relatively low cost and high expansibility, and can be used for industrial production. However, the research on the floating catalytic chemical vapor deposition method at the present stage is still in the primary stage, and there are some problems to be solved in practical application. For example, further research into the design and optimization of catalysts is required to improve the quality and yield of carbon nanotubes. In addition, there is a need to solve the problems of separation and purification of carbon nanotubes to obtain a high purity product. In general, although the macro-scale preparation process of the carbon nanotubes still faces challenges, the floating catalytic chemical vapor deposition method has potential to break through in the field as a promising method, and promotes the large-scale application and research and development of the carbon nanotubes.
Disclosure of Invention
The invention aims to provide a carbon nano tube preparation system and a single-wall carbon nano tube preparation process, so as to solve the problems in the prior art and realize high-yield and high-quality preparation of the single-wall carbon nano tube.
In order to achieve the above object, the present invention provides the following solutions:
one of the technical schemes of the invention is as follows: provided is a carbon nanotube preparation system including: the device comprises a liquid sample injection system, an atomization chamber, a pressure control system, an air inlet, a furnace body, a collecting box and a tail gas treatment device;
the liquid sample injection system, the atomizing chamber, the furnace body, the collecting box and the tail gas treatment device are sequentially communicated through pipelines;
the air inlet is communicated with the atomizing chamber;
the pressure control system is arranged outside the atomizing chamber and is used for pressurizing carrier gas entering the atomizing chamber through the air inlet;
the tail end of a pipeline of the atomizing chamber, which is led into the furnace body, is connected with a bell mouth.
The second technical scheme of the invention is as follows: a continuous carbon nanotube preparing system is provided, which uses the carbon nanotube preparing system as a repeating unit, and the tail gas treating device of the previous repeating unit is communicated with the gas inlet of the next repeating unit.
The number of repeating units is not less than 2, preferably the number of repeating units is 2.
The diameter of the upper end opening of the bell mouth is equal to the diameter of the feeding pipeline, and the diameter of the lower end opening is smaller than or equal to the inner diameter of the furnace body and larger than the diameter of the upper end opening.
An atomizer is arranged at the top end of the atomizing chamber; and a heating sleeve is arranged at the bottom of the atomizing chamber.
An atomizer and an atomization chamber are arranged before the horn mouth is fed, and raw materials are gasified and then injected into the horn mouth. Meanwhile, the bottom end of the bell mouth is designed as an expansion pipeline, so that the pipe diameter of air flow is gradually enlarged when the air flow enters the growth pipe from the air inlet pipe, the generation of vortex is reduced, and the possibility of adhesion of products is reduced. Through the design of progressive expansion pipeline, can make the mouth of pipe diameter of gas raw materials in horn mouth department increase gradually to reduce the production of gas reflux phenomenon, thereby make the carbon nanotube that grows adhere and pile up the phenomenon that leads to the product quality bad in low temperature region. The design method of gradually expanding the pipe diameter of the horn mouth can also control the stability and the flow speed of the air flow, and ensure the uniformity and the stability of the feeding process. Secondly, the pipeline between the discharge port furnace body and the collecting box is improved, and a longer temperature buffer area of the pipeline is arranged at the outlet of the furnace tube, so that the generated single-wall carbon nano tube is collected under the condition that the temperature is gradually reduced, and the possibility of adhering to the inside of the metal tube wall is reduced.
The fine metal net is arranged in the collecting box, so that the generated single-walled carbon nanotube aerogel film is easier to fall off, and besides, the frequency of periodic sampling is reduced.
In the invention, the pressure control system consists of a sensor, a controller, an actuator and a feedback loop, and the functions comprise pressure measurement, pressure monitoring, pressure regulation, pressure protection and automatic control. The pressure control system plays an important role in ensuring stable and controlled operation of the system pressure.
The gas inlet can ensure gas supply, realize gas mixing and provide safety protection.
The atomizing chamber may introduce the liquid in a suitable manner and disperse the liquid into fine particles or mist by a nebulizer or other device. This helps to increase the liquid surface area, increase the contact area with the environment, facilitate solvent evaporation, reactant interactions and reaction progress, and thereby promote diffusion and reaction of the species. The atomizer is mainly a device for converting liquid into fine particles or liquid drops by means of ultrasonic waves, compressed air or mechanical vibration, and the like, and is a core component in an atomization chamber.
The heating jacket may provide a sufficient temperature for the liquid to atomize to form a gas.
The flange is used for connecting pipe ends and connecting equipment inlets and outlets.
The furnace body has the functions of high-temperature treatment, temperature control, heat preservation, safety protection and the like, can meet various high-temperature manufacturing and treatment requirements, and provides high-temperature reaction conditions for the single-wall carbon nanotube preparation.
The collection box may collect the sample at the source or during preparation for subsequent analysis and processing. In addition, the collection box provides a proper storage environment, so that the safety and stability of the sample can be ensured.
The tail gas treatment device generally reduces the concentration of gases with stronger interference such as sulfur dioxide and the like so as to ensure the effectiveness and stability of the gas supply device, and can purify the gases to realize the recycling of carrier gases.
The horn mouth is made of aluminum oxide; the pipeline is made of quartz.
The horn mouth can prevent the liquid sample from entering the high-temperature path body along with the carrier gas to generate a vortex effect, so that the sample with poor quality is deposited at the upper end of the high-temperature furnace tube.
More specifically, the liquid sample injection system is used as follows:
(1) Preparing a sample: according to the preparation requirements, liquid samples needing sample introduction are prepared. Ensure that the sample has been pre-treated or prepared.
(2) The connection system comprises: the liquid sample injection system is connected with the rest parts. Ensuring the connection is correct and tight.
(3) Setting sample introduction parameters: parameters such as sample injection volume, sample injection speed and the like are set, and a liquid sample injection system is usually provided with a control panel or software, so that parameter setting and adjustment can be conveniently carried out.
(4) The calibration system: depending on the preparation requirements, calibration of the system may be performed. And (3) checking the accuracy and stability of the liquid sample injection system, and ensuring the accuracy of the sample injection quantity and speed.
(5) Sample injection is carried out: and inserting the injection device into the liquid sample injection system according to the preparation requirements and the set parameters. And introducing the sample into a sample introduction device, ensuring no bubbles, and inserting the sample introduction device into a corresponding position in the liquid sample introduction system.
The third technical scheme of the invention: providing a single-walled carbon nanotube preparation process, and adopting the carbon nanotube preparation system; the preparation process comprises the following steps:
setting the temperature in the furnace body to be 800-1300 ℃, introducing carrier gas into the carbon nano tube preparation system through the air inlet, adding reaction raw materials into the liquid sample injection system, atomizing through the atomizing chamber, and entering the furnace body through the bell mouth;
collecting reaction products by utilizing the collecting box, and treating tail gas by utilizing the tail gas treatment device;
the pressure control system is used for controlling the pressure of the atomizing chamber to be 10-100atm in the preparation process.
The fourth technical scheme of the invention: providing a continuous preparation process of carbon nanotubes, wherein the continuous preparation system of the carbon nanotubes is adopted; the preparation process comprises the following steps:
setting the temperature in the furnace body to be 800-1300 ℃, introducing carrier gas into the carbon nano tube continuous preparation system through the air inlet, adding reaction raw materials into the liquid sample injection system, atomizing through the atomizing chamber, and entering the furnace body through the bell mouth;
collecting reaction products by utilizing the collecting box, and treating tail gas by utilizing the tail gas treatment device;
the pressure control system is used for controlling the pressure of the atomizing chamber to be 10-100atm in the preparation process;
and (3) introducing the tail gas treated by the tail gas treatment device into an air inlet of the next repeating unit, and continuously preparing the carbon nano tube.
As a further preference of the invention, the reaction raw materials used in the preparation process are mixed solutions of liquid carbon source, ferric salt and sulfur source; the carrier gas is mixed gas of hydrogen and nitrogen in a volume ratio of 2:1. The flow rate in the preparation process is preferably 100-600 mu L/min.
The liquid carbon source comprises ethanol, toluene, cyclohexane or other liquid carbon-containing organic matters; the ferric salt plays a role of a catalyst, and is specifically one or more of ferric chloride, ferrous chloride, ferric acetate, ferric nitrate and ferrocene; the sulfur source plays a role of a cocatalyst, and is specifically a compound capable of providing a sulfur source, such as thiophene, ethanethiol, ethanesulfide, thiophenol and the like.
Preferably toluene is the liquid carbon source, ferrocene or ferric chloride is the ferric salt, and thiophene is the sulfur source.
The liquid carbon source, iron salt and sulfur source were mixed in a ratio of 100mL:5g:10 mL.
The liquid sample injection system introduces the pretreated liquid sample in an accurate and controllable mode, realizes automatic sample injection of the sample through sample injection volume control and sample injection speed control, and improves experimental efficiency.
According to the invention, the tail gas generated in the preparation process of the carbon nanotubes is introduced into the sodium hydroxide solution of the tail gas treatment device, and the tail gas contains impurities such as sulfur dioxide, so that the generated sulfur dioxide impurities can be removed by introducing the tail gas into the sodium hydroxide solution for absorption and reaction.
The invention discloses the following technical effects:
the invention can optimize the airflow in the process of preparing the carbon nano tube, adjust the flow speed and the flow state of the airflow by gradually expanding or narrowing the caliber of the pipeline, reduce the generation of vortex and the possibility of blocking products, ensure the smooth flow of the gas and avoid the confusion and the blocking of the airflow by reasonably designing the pipeline structure.
The invention aims at the continuous preparation of the carbon nano tube, and the preparation systems are connected in series, so that the production efficiency can be improved, the waste of energy and materials can be reduced, the manual operation and management cost can be reduced, and the product quality and consistency can be improved. The serial use can better control and monitor the production process, discover and solve the problems in time, improve the quality and stability of the product, and is an effective production optimization mode.
The invention solves the problem of adhesion of products in the pipeline in the preparation process of the carbon nanotubes, improves the production efficiency of the carbon nanotubes, and further meets the production requirement of industry on the carbon nanotubes. The preparation system and the preparation method can be used for preparing the high-yield and high-quality single-wall carbon nanotubes (G/D value can reach more than 50).
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a system for preparing single-walled carbon nanotubes according to an embodiment of the present invention; wherein: 1. the device comprises a liquid sample injection system, an air inlet, a pressure control system, an atomization chamber, an atomizer, a heating sleeve, a flange, a bell mouth, a high-temperature furnace body, a collecting box and an exhaust gas treatment device, wherein the liquid sample injection system, the air inlet, the pressure control system, the atomization chamber, the atomizer, the heating sleeve, the flange, the bell mouth, the high-temperature furnace body, the collecting box and the exhaust gas treatment device are arranged in sequence, and the liquid sample injection system, the air inlet, the pressure control system, the atomization chamber, the atomizer, the heating sleeve, the flange, the horn mouth, the high-temperature furnace body, the collecting box and the exhaust gas treatment device are arranged in sequence.
FIG. 2 shows the Raman spectrum of the product obtained in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of the product obtained in example 1 of the present invention;
FIG. 4 is a Raman spectrum of the product obtained in example 2 of the present invention;
FIG. 5 is a scanning electron microscope image of the product obtained in example 2 of the present invention.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
Fig. 1 is a schematic structural diagram of a system for preparing single-walled carbon nanotubes according to an embodiment of the present invention.
Example 1
The temperature in the furnace body 9 is regulated to 1300 ℃, then mixed gas of hydrogen and nitrogen with the volume ratio of 2:1 is taken as carrier gas (100 mu L/min) to be introduced from the air inlet 2, mixed solution of toluene, ferrocene and thiophene (toluene: ferrocene: thiophene=100 mL:5g:10 mL) is added into an injector, the mixed solution in the injector is added into a preparation system by utilizing the liquid injection system 1, atomization (heating treatment is carried out by the heating sleeve 6) is realized in the atomizing chamber 4 after the mixed solution passes through the atomizer 5, and after the mixed solution is mixed with the carrier gas, the mixed solution enters the furnace body 9 at the horn mouth 8 through a pipeline and is uniformly diffused in the downward transmission process. The reaction generates single-wall carbon nanotube aerogel, reaction products are discharged from the lower end of the furnace body 9 (the temperature of the part is higher than 800 ℃), enter the collecting box 10, and tail gas enters the tail gas treatment device 11 (the concentration of sodium hydroxide solution is 0.3M) and is sequentially connected with 2 machines for reaction and treatment.
In the above-described process for producing single-walled carbon nanotubes, the pressure of the atomizing chamber is maintained at 10 to 100atm by the pressure control system 3.
The raman spectrum of the obtained product is shown in fig. 2, G/d=71, and has a distinct RBM peak, indicating that the product is a high quality single-walled carbon nanotube (SWCNT-1); the scanning electron microscope photograph of the product is shown in fig. 3, and the product is slender and pure and uniformly distributed.
Example 1 consumption of 1g ferrocene can produce 0.3-0.4g single wall carbon nanotubes.
Example 2
The temperature in the furnace body 9 is regulated to 1300 ℃, then mixed gas of hydrogen and nitrogen with the volume ratio of 2:1 is taken as carrier gas (600 mu L/min) to be introduced from the air inlet 2, mixed solution of toluene, ferrocene and thiophenol (toluene: ferrocene: thiophenol=100 mL:5g:10 mL) is added into an injector, the mixed solution in the injector is added into a preparation system by utilizing a liquid sample injection system 1, atomization (heating treatment is carried out by a heating sleeve 6) is realized in an atomization chamber 4 after the mixed solution passes through an atomizer 5, and after the mixed solution is mixed with the carrier gas, the mixed solution enters the furnace body 9 at a bell mouth 8 through a pipeline and is uniformly diffused in the downward transmission process. The reaction produces single-wall carbon nanotube aerogel, reaction products are discharged from the lower end of the furnace body 9 (the temperature of the part is higher than 800 ℃), the reaction products enter the collecting box 10, and tail gas enters the tail gas treatment device 11 (the concentration of sodium hydroxide solution is 0.3M) for treatment.
In the above-described process for producing single-walled carbon nanotubes, the pressure of the atomizing chamber is maintained at 10 to 100atm by the pressure control system 3.
The raman spectrum of the obtained product is shown in fig. 4, G/d=128, and has a distinct RBM peak, indicating that the product is a high quality single-walled carbon nanotube (SWCNT-2); the scanning electron microscope photograph of the product is shown in fig. 5, and the product is slender and pure and uniformly distributed.
Example 2 consumption of 1g ferrocene can produce 0.3-0.4g single wall carbon nanotubes.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (8)
1. A carbon nanotube production system, comprising: the device comprises a liquid sample injection system, an atomization chamber, a pressure control system, an air inlet, a furnace body, a collecting box and a tail gas treatment device;
the liquid sample injection system, the atomizing chamber, the furnace body, the collecting box and the tail gas treatment device are sequentially communicated through pipelines;
the air inlet is communicated with the atomizing chamber;
the pressure control system is arranged outside the atomizing chamber and is used for pressurizing carrier gas entering the atomizing chamber through the air inlet;
the tail end of a pipeline of the atomizing chamber, which is led into the furnace body, is connected with a bell mouth.
2. A continuous carbon nanotube preparing system, which is characterized in that the carbon nanotube preparing system of claim 1 is used as a repeating unit, and the tail gas treating device of the previous repeating unit is communicated with the gas inlet of the next repeating unit.
3. A process for preparing single-walled carbon nanotubes, characterized in that the system for preparing carbon nanotubes according to claim 1 is used; the preparation process comprises the following steps:
setting the temperature in the furnace body to be 800-1300 ℃, introducing carrier gas into the carbon nano tube preparation system through the air inlet, adding reaction raw materials into the liquid sample injection system, atomizing through the atomizing chamber, and entering the furnace body through the bell mouth;
collecting reaction products by utilizing the collecting box, and treating tail gas by utilizing the tail gas treatment device;
the pressure control system is used for controlling the pressure of the atomizing chamber to be 10-100atm in the preparation process.
4. A single-walled carbon nanotube continuous preparation process, characterized in that the carbon nanotube continuous preparation system of claim 2 is adopted; the preparation process comprises the following steps:
setting the temperature in the furnace body to be 800-1300 ℃, introducing carrier gas into the carbon nano tube continuous preparation system through the air inlet, adding reaction raw materials into the liquid sample injection system, atomizing through the atomizing chamber, and entering the furnace body through the bell mouth;
collecting reaction products by utilizing the collecting box, and treating tail gas by utilizing the tail gas treatment device;
the pressure control system is used for controlling the pressure of the atomizing chamber to be 10-100atm in the preparation process;
and (3) introducing the tail gas treated by the tail gas treatment device into an air inlet of the next repeating unit, and continuously preparing the carbon nano tube.
5. The process for preparing single-walled carbon nanotubes according to claim 3, wherein the reaction raw material is a mixed solution of a liquid carbon source, an iron salt and a sulfur source; the carrier gas is mixed gas of hydrogen and nitrogen in a volume ratio of 2:1.
6. The process of claim 5, wherein the liquid carbon source comprises ethanol, toluene, or cyclohexane; the ferric salt comprises one or more of ferric chloride, ferrous chloride, ferric acetate, ferric nitrate and ferrocene; the sulfur source comprises thiophene, ethanethiol, ethanesulfide or thiophenol.
7. The continuous preparation process of single-walled carbon nanotubes according to claim 4, wherein the reaction raw material is a mixed solution of a liquid carbon source, an iron salt and a sulfur source; the carrier gas is mixed gas of hydrogen and nitrogen in a volume ratio of 2:1.
8. The continuous process for preparing single-walled carbon nanotubes according to claim 7, wherein the liquid carbon source comprises ethanol, toluene or cyclohexane; the ferric salt comprises one or more of ferric chloride, ferrous chloride, ferric acetate, ferric nitrate and ferrocene; the sulfur source comprises thiophene, ethanethiol, ethanesulfide and thiophenol.
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