CN116002666A - Continuous production device and method for in-situ preparation and dispersion integration of carbon nanotubes - Google Patents
Continuous production device and method for in-situ preparation and dispersion integration of carbon nanotubes Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 68
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 68
- 239000006185 dispersion Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000010924 continuous production Methods 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 22
- 230000010354 integration Effects 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims description 101
- 238000003860 storage Methods 0.000 claims description 38
- 229910052799 carbon Inorganic materials 0.000 claims description 36
- 230000001681 protective effect Effects 0.000 claims description 18
- 239000012530 fluid Substances 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 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 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 239000004215 Carbon black (E152) Substances 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 abstract description 7
- 230000001360 synchronised effect Effects 0.000 abstract description 2
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- -1 methane or propylene Chemical class 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses a continuous production device and a continuous production method integrating in-situ preparation and dispersion of carbon nanotubes, wherein the continuous production device comprises a reaction unit, a dispersion unit, a collection unit and a filtration separation unit, the reaction unit is communicated with the dispersion unit, the dispersion unit is respectively communicated with the collection unit and the filtration separation unit, and the filtration separation unit is communicated with the reaction unit. The invention adopts the continuous production method of the in-situ preparation and dispersion integration of the carbon nano tube of the device, changes the traditional high-temperature normal-pressure reaction environment into the supercritical reaction environment, realizes the synchronous continuous production of the in-situ preparation and dispersion of the carbon nano tube, integrates the growth, dispersion and collection of the carbon nano tube into a whole and improves the production efficiency of the carbon nano tube.
Description
Technical Field
The invention relates to the technical field of carbon nanotube preparation, in particular to a continuous production device and a continuous production method for in-situ preparation and dispersion integration of carbon nanotubes.
Background
Carbon nanotubes, which are a new type of carbon material, are receiving increasing attention because of their superior properties to conventional materials. The demand for carbon nanotube materials in the current strategic and emerging industries of various countries is increasingly prominent, and the demand gap of carbon nanotubes in the market is rapidly enlarged with the rapid rise of the new energy automobile industry taking fuel cell conductive paste as an example.
At present, carbon nanotubes are mainly produced by adopting a chemical vapor deposition method, and because the carbon nanotubes are easy to agglomerate under the actions of Van der Waals force and the like, the produced carbon nanotubes can be applied only by carrying out dispersion treatment. Therefore, the carbon nano tube comprises two technological processes of preparation and dispersion in the actual production and application process.
However, in the chemical vapor deposition method, carbon source gas is continuously introduced into a high-temperature normal-pressure reactor to grow carbon tubes, and the growth period of the carbon nanotubes in the process is long, so that the production efficiency is limited. The problem of incomplete contact of active sites exists in the reaction process of the carbon source gas and the catalyst, and the carbon source gas which does not participate in the reaction is discharged out of the reactor, so that the cost is increased and the environment is polluted.
In addition, the carbon nanotube dispersion mainly comprises physical methods such as ball milling, stirring and vibration, and chemical methods such as strong acid and alkali treatment and dispersant treatment. However, the physical method has high cost and low efficiency, and the chemical method has the problems of complex treatment, harm to the environment of personnel and equipment, and the like. And the carbon nanotube preparation and dispersion processes in the prior art are separated, which clearly increases the complexity of the carbon nanotube production process. The above-described problems have hindered further developments in the carbon nanotube industry.
Disclosure of Invention
The invention aims to provide a continuous production device and a continuous production method integrating in-situ preparation and dispersion of carbon nanotubes, which solve the problems of discontinuous preparation and dispersion processes, low efficiency and high cost of the carbon nanotubes.
In order to achieve the above purpose, the invention provides a continuous production device integrating in-situ preparation and dispersion of carbon nanotubes, which comprises a reaction unit, a dispersion unit, a collection unit and a filtration separation unit, wherein the reaction unit is communicated with the dispersion unit, the dispersion unit is respectively communicated with the collection unit and the filtration separation unit, and the filtration separation unit is communicated with the reaction unit.
Preferably, the reaction unit comprises a feeder, a reactor, a protective gas storage tank, a carbon source gas storage tank and a heat exchanger, wherein the reactor communicated with the feeder is communicated with the heat exchanger, and the protective gas storage tank and the carbon source gas storage tank are communicated with the reactor through a booster pump, a flowmeter and the heat exchanger in sequence.
Preferably, the dispersing unit comprises a mixer, a back pressure valve, a first expansion valve, a main pressure relief tank, a second expansion valve and a secondary pressure relief tank, wherein the mixer is communicated with the reactor, the mixer is communicated with the main pressure relief tank through the back pressure valve and the first expansion valve in sequence, and the main pressure relief tank is communicated with the secondary pressure relief tank through the second expansion valve.
Preferably, the collecting unit comprises a collector, and the main pressure relief tank and the secondary pressure relief tank are both communicated with the collector.
Preferably, the filtering and separating unit comprises a filter and a gas separator, the secondary pressure release tank is communicated with the gas separator through the filter, and the gas separator is respectively communicated with the carbon source gas storage tank and the protection gas storage tank.
The continuous production method for in-situ preparation and dispersion integration of the carbon nano tube comprises the following steps:
s1, a catalyst enters the reactor through the feeder and heats the reactor;
s2, heating and pressurizing the carbon source gas in the carbon source gas storage tank and the protective gas in the protective gas storage tank to be above a critical point to form a supercritical fluid, and then conveying the supercritical fluid to the reactor to obtain the carbon nano tube;
s3, conveying the carbon nanotubes obtained in the step S2 in the reactor into the mixer through the heat exchanger, and forming uniformly mixed suspended matters in the mixer;
s4, enabling the suspended matters obtained in the S3 in the mixer to sequentially enter the main pressure relief tank through the back pressure valve and the first expansion valve, and then enter the secondary pressure relief tank through the second expansion valve;
s5, sending the carbon nanotubes obtained after being dispersed in the main pressure relief tank and the secondary pressure relief tank in the S4 into a collecting tank;
and S6, enabling the mixed gas in the secondary pressure release tank to enter the gas separator through the filter, separating the mixed gas through the gas separator, and then respectively returning the mixed gas to the protective gas storage tank and the carbon source gas storage tank to participate in the next cyclic reaction.
Preferably, the catalyst in S1 is a metal supported catalyst of iron, cobalt, nickel, manganese, aluminum, copper, magnesium, platinum and the like, and the particle size range is 50-100 mu m.
Preferably, the carbon source gas in S2 is one of hydrocarbons, alcohols, ethers, ketones and phenols, and the shielding gas is one of inert gas, nitrogen and carbon dioxide.
Therefore, the continuous production device and the continuous production method for in-situ preparation and dispersion integration of the carbon nanotubes by adopting the method have the beneficial effects that:
1. by means of the special property of the supercritical fluid and technological integration innovation, the in-situ preparation and dispersion synchronous continuous production of the carbon nanotubes is realized, the growth, dispersion and collection of the carbon nanotubes are integrated, and the production efficiency of the carbon nanotubes is improved;
2. the recycling of the carbon source gas and the shielding gas improves the utilization efficiency of the carbon source gas and the shielding gas, realizes heat recovery through the heat exchanger, and effectively reduces the production cost;
3. the traditional high-temperature normal-pressure reaction environment is changed into a supercritical reaction environment, the reaction temperature is reduced to make the reaction condition tend to be mild, and the carbon nano tube is dispersed through the supercritical fluid phase transition process, so that harmless, simplified and efficient dispersion is realized;
4. the heat and mass transfer efficiency of the carbon source gas is higher in the supercritical state, and the advantages of high reaction efficiency of the reactor are added, so that the growth rate of the carbon nano tube is effectively improved;
5. the method has the advantages of high integration level, high operation elasticity, high production efficiency, low operation cost and environmental friendliness, meets the current development requirements of green chemical industry, and provides a brand new approach for solving the problem of large-scale production of the carbon nanotubes.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a schematic diagram of an in-situ preparation and dispersion integrated continuous production apparatus for carbon nanotubes according to the present invention.
Reference numerals
1. A reactor; 2. a heat exchanger; 3. a mixer; 4. a main pressure relief tank; 5. a second-stage pressure release tank; 6. a filter; 7. a gas separator; 8. a carbon source gas storage tank; 9. a protective gas storage tank; 10. a pressurizing pump; 11. a collector; 12. a feeder; 13. a flow meter; 14. a back pressure valve; 15. a first expansion valve; 16. and a second expansion valve.
Detailed Description
The technical scheme of the invention is further described below through the attached drawings and the embodiments.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The terms "first," "second," and the like, as used herein, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof, but does not exclude other elements or items. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate relative positional relationships, which may also be changed when the absolute position of the object to be described is changed.
Example 1
The continuous production device integrating in-situ preparation and dispersion of the carbon nano tube comprises a reaction unit, a dispersion unit, a collection unit and a filtering separation unit. The reaction unit is communicated with the dispersing unit, the dispersing unit is respectively communicated with the collecting unit and the filtering and separating unit, and the filtering and separating unit is communicated with the reaction unit.
The reaction unit comprises a feeder 12, a reactor 1, a protective gas storage tank 9, a carbon source gas storage tank 8 and a heat exchanger 2, wherein the reactor 1 communicated with the feeder 12 is communicated with the heat exchanger 2. The protective gas storage tank 9 and the carbon source gas storage tank 8 are communicated with the reactor 1 through a booster pump 10, a flowmeter 13 and the heat exchanger 2 in sequence.
The two pressurizing pumps 10 respectively pressurize the protective gas in the protective gas storage tank 9 and the carbon source gas in the carbon source gas storage tank 8 to be above the critical pressure, and the pressurized mixed gas exchanges heat with the mixture of the supercritical fluid and the carbon nano tube in the heat exchanger 2. The heated and pressurized mixed gas reaches a supercritical state, and the supercritical mixed fluid enters the reactor 1 and is mixed with the catalyst to complete the growth of the carbon nano tube in the fluidization process of the reactor 1. The supercritical mixed fluid provides a carbon source for growth of the carbon nano tube, and simultaneously provides a circulating power source for the whole circulating production process, and the carbon nano tube is carried out of the reactor 1 by the supercritical mixed fluid and then enters the mixer 3 through the heat exchanger 2.
The heat exchanger 2 exchanges heat with the mixture of the supercritical fluid and the carbon nano tube in the reactor 1, and simultaneously heats the mixed gas to reach a supercritical state after the temperature of the mixed gas is raised. The carbon source gas and the shielding gas are mixed through the bottom of the reactor 1 and then enter the reactor 1 to be mixed with the catalyst fed by the feeder 12.
The dispersion unit comprises a mixer 3, a back pressure valve 14, a first expansion valve 15, a main pressure relief tank 4, a second expansion valve 16 and a secondary pressure relief tank 5, and the mixer 3 is communicated with the reactor 1. The mixer 3 is communicated with the main pressure relief tank 4 through the back pressure valve 14 and the first expansion valve 15 in sequence, and the main pressure relief tank 4 is communicated with the secondary pressure relief tank 5 through the second expansion valve 16.
The mixer 3 is used for stirring the supercritical mixed fluid and the carbon nano tubes at a high speed to form carbon nano tube suspended matters, the carbon nano tube suspended matters are subjected to primary expansion and dispersion in the main pressure release tank 4, and secondary expansion and pressure release are performed in the secondary pressure release tank 5, so that the dispersion process of the carbon nano tubes is completed.
The collecting unit comprises a collector 11, and the main pressure relief tank 4 and the secondary pressure relief tank 5 are communicated with the collector 11. The dispersed carbon nanotubes enter the collector 11 through the bottom of the main pressure relief tank 4 and the bottom of the secondary pressure relief tank 5, so that the dispersed carbon nanotubes are collected.
The filtering and separating unit comprises a filter 6 and a gas separator 7, the secondary pressure release tank 5 is communicated with the gas separator 7 through the filter 6, and the gas separator 7 is respectively communicated with a carbon source gas storage tank 8 and a protection gas storage tank 9. The supercritical fluid is depressurized and becomes a mixed gas, and the mixed gas separates residual carbon nanotubes through a filter 6 to realize gas purification. After the mixed gas is separated by the gas separator 7, the carbon source gas returns to the carbon source gas storage tank 8, and the protection gas returns to the protection gas storage tank 9.
The pressing force of the whole production device is divided into a high-pressure circuit and a low-pressure circuit in the circulation process, wherein the high-pressure circuit starts from the booster pump 10 and stops at the back pressure valve 14. The pressure is regulated by the booster pump 10, the heating process in the reactor 1 and the back pressure valve 14. The low-pressure loop starts from the main pressure release tank 4 and ends at the carbon source gas storage tank 8 and the protection gas storage tank 9.
Example 2
The continuous production method for in-situ preparation and dispersion integration of the carbon nano tube comprises the following steps:
s1, the catalyst enters the reactor through a feeder and heats the reactor. The catalyst is a metal supported catalyst of iron, cobalt, nickel, manganese, aluminum, copper, magnesium, platinum and the like, and the particle size range is 50-100 mu m.
S2, heating and pressurizing the carbon source gas in the carbon source gas storage tank and the protective gas in the protective gas storage tank to be above a critical point, forming a supercritical fluid, and then conveying the supercritical fluid to a reactor to obtain the carbon nano tube, wherein the reaction time is 0.5-0.8h.
The reactor is a fluidized bed reactor or a kettle type reaction furnace, the heating temperature is 500-600 ℃, and the fluidization speed is regulated by using a flowmeter. The carbon source gas is hydrocarbon, such as methane or propylene, and the pressure in the reactor is 5-10Mpa. The protecting gas is one or more of inert gas, nitrogen and carbon dioxide, and the pressure in the reactor is 5-10Mpa.
And S3, conveying the carbon nanotubes obtained in the step S2 in the reactor into a mixer through a heat exchanger, and forming a uniformly mixed suspension in the mixer.
The heat exchanger is a shell-and-tube heat exchanger, and the mixer is a stirring mixer. The supercritical fluid after the reaction passes through a tube pass after being mixed with the carbon nano tube, and the supercritical fluid before the reaction passes through a shell pass and reaches a supercritical state.
S4, enabling the suspended matters obtained in the S3 in the mixer to sequentially enter the main pressure relief tank through the back pressure valve and the first expansion valve, and then enter the secondary pressure relief tank through the second expansion valve.
Taking primary expansion dispersion in the main pressure release tank as a leading, and carrying out secondary expansion dispersion in the secondary pressure release tank to intercept the carbon nano tube.
S5, enabling the carbon nanotubes obtained after the dispersion of the main pressure release tank and the secondary pressure release tank in the S4 to enter a collecting tank, and enabling the carbon nanotubes after the dispersion to enter a collector through collecting ports at the bottom of the main pressure release tank and the bottom of the secondary pressure release tank for collection.
And S6, enabling the mixed gas in the second-stage pressure release tank in S4 to enter a gas separator through a filter, separating the mixed gas through the gas separator, and respectively returning the mixed gas to a protective gas storage tank and a carbon source gas storage tank to participate in the next cyclic reaction. The filter is used for filtering the residual carbon nano tube to purify the mixed gas, and the gas separator is a membrane type gas separator.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (8)
1. The continuous production device integrating in-situ preparation and dispersion of carbon nanotubes is characterized in that: the device comprises a reaction unit, a dispersing unit, a collecting unit and a filtering and separating unit, wherein the reaction unit is communicated with the dispersing unit, the dispersing unit is respectively communicated with the collecting unit and the filtering and separating unit, and the filtering and separating unit is communicated with the reaction unit.
2. The continuous production device integrating in-situ preparation and dispersion of carbon nanotubes according to claim 1, wherein: the reaction unit comprises a feeder, a reactor, a protective gas storage tank, a carbon source gas storage tank and a heat exchanger, wherein the reactor communicated with the feeder is communicated with the heat exchanger, and the protective gas storage tank and the carbon source gas storage tank are communicated with the reactor through a booster pump, a flowmeter and the heat exchanger in sequence.
3. The continuous production apparatus of in-situ preparation and dispersion integration of carbon nanotubes according to claim 2, wherein: the dispersing unit comprises a mixer, a back pressure valve, a first expansion valve, a main pressure relief valve, a second expansion valve and a secondary pressure relief tank, wherein the mixer is communicated with the reactor, the mixer is communicated with the main pressure relief tank through the back pressure valve and the first expansion valve in sequence, and the main pressure relief tank is communicated with the secondary pressure relief tank through the second expansion valve.
4. The continuous production apparatus for in-situ preparation and dispersion integration of carbon nanotubes according to claim 3, wherein: the collecting unit comprises a collector, and the main pressure relief tank and the secondary pressure relief tank are both communicated with the collector.
5. The continuous production apparatus of in-situ preparation and dispersion integration of carbon nanotubes according to claim 4, wherein: the filtering and separating unit comprises a filter and a gas separator, the secondary pressure release tank is communicated with the gas separator through the filter, and the gas separator is respectively communicated with the carbon source gas storage tank and the protection gas storage tank.
6. The continuous production method of in-situ preparation and dispersion integration of carbon nanotubes according to any one of claims 1-5, wherein:
s1, a catalyst enters the reactor through the feeder and heats the reactor;
s2, heating and pressurizing the carbon source gas in the carbon source gas storage tank and the protective gas in the protective gas storage tank to be above a critical point to form a supercritical fluid, and then conveying the supercritical fluid to the reactor to obtain the carbon nano tube;
s3, conveying the carbon nanotubes obtained in the step S2 in the reactor into the mixer through the heat exchanger, and forming uniformly mixed suspended matters in the mixer;
s4, enabling the suspended matters obtained in the S3 in the mixer to sequentially enter the main pressure relief tank through the back pressure valve and the first expansion valve, and then enter the secondary pressure relief tank through the second expansion valve;
s5, sending the carbon nanotubes obtained after being dispersed in the main pressure relief tank and the secondary pressure relief tank in the S4 into a collecting tank;
and S6, enabling the mixed gas in the secondary pressure release tank to enter the gas separator through the filter, separating the mixed gas through the gas separator, and then respectively returning the mixed gas to the protective gas storage tank and the carbon source gas storage tank to participate in the next cyclic reaction.
7. The continuous production method of in-situ preparation and dispersion integration of carbon nanotubes according to claim 6, wherein the method comprises the steps of: the catalyst in S1 is a metal supported catalyst of iron, cobalt, nickel, manganese, aluminum, copper, magnesium, platinum and the like, and the particle size range is 50-100 mu m.
8. The continuous production method of in-situ preparation and dispersion integration of carbon nanotubes according to claim 6, wherein the method comprises the steps of: the carbon source gas in S2 is one of hydrocarbon, alcohol, ether, ketone and phenol, and the shielding gas is one of inert gas, nitrogen and carbon dioxide.
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