CN1284726C - Reaction unit and process of continuous preparation of carbon nano-tube - Google Patents
Reaction unit and process of continuous preparation of carbon nano-tube Download PDFInfo
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- CN1284726C CN1284726C CN 02113678 CN02113678A CN1284726C CN 1284726 C CN1284726 C CN 1284726C CN 02113678 CN02113678 CN 02113678 CN 02113678 A CN02113678 A CN 02113678A CN 1284726 C CN1284726 C CN 1284726C
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Abstract
The present invention discloses a reaction device and technology for preparing carbon nanometer tubes, particularly continuous preparation of single-wall carbon nanometer tubes or multi-wall carbon nanometer tubes. The present invention has the technical scheme that the reaction device for continuously preparing carbon nanometer tubes is used, and is a tower type reactor. Simultaneously, the present invention also provides technology for continuously preparing carbon nanometer tubes by the device. The present invention has the technical scheme that the reaction device for continuously preparing carbon nanometer tubes is used, and is a tower type reactor which comprises a catalyst container, a catalyst quantitative groove, a reaction tower, a rough product outlet, a tail gas outlet, a feed gas inlet, etc., wherein a tower plate is horizontally arranged in the reaction tower. By the tower reactor, a catalyst can reach a reaction area at the fastest speed and can leave the reaction area at the fastest speed. The catalyst movement is completed under the action of mechanical force. The flow speed of the feed gas can be low, and thus, the reaction device has the advantages of low energy consumption and high conversion rate of the feed gas.
Description
Technical field
The present invention relates to a kind of reaction unit and technology for preparing carbon nanotube, be particularly suitable for the serialization preparation of Single Walled Carbon Nanotube or multi-walled carbon nano-tubes.
Background technology
Up to the present, the preparation carbon nanotube has several different methods, but topmost method has only three kinds, i.e. arc process, laser ablation method and catalystic pyrolysis.Arc process is the method for preparing carbon nanotube the earliest, is still the present method for preparing the high-crystallinity carbon nanotube.Laser ablation method is the main method for preparing Single Walled Carbon Nanotube at present, but output is difficult to industry and amplifies in the milligram level.Catalystic pyrolysis is to be catalyzer with nano-level iron, cobalt or nickel, and lower carbon number hydrocarbons, hydrocarbon or carbon monoxide are unstripped gas, and the method for catalytic cracking reaction carbon nano-tube at high temperature takes place.This method is produced carbon nano pipe purity height, specification may command, and is easy to the industry amplification, is considered to have most the method for preparing carbon nanotube of DEVELOPMENT PROSPECT.
Catalystic pyrolysis has four kinds of technologies, be fixed-bed process, ebullated bed technology, bed process and moving bed process swim, each technology all has the advantage and defect of self, simple as the fixed-bed process device, flexible and convenient operation, but the ability of handling catalyzer is little, only suitable screening of catalyst or prepare carbon nanotube on a small quantity; Ebullated bed technology can be handled a large amount of catalyzer, also can obtain good carbon nanotube productive rate, but the unstripped gas transformation efficiency is low, the energy consumption height, and the operation easier of device is big; The bed process that swims has bigger limitation, only is fit to the catalyst system that uses ferrocene, iron carbonyl etc. to gasify and decompose easily; Moving bed process is having remarkable advantages aspect the preparation design specification multi-walled carbon nano-tubes, but owing to have thermograde and translational speed aspect problem, is not suitable for the continuous preparation of Single Walled Carbon Nanotube.
Summary of the invention
The technology that the purpose of this invention is to provide a kind of catalytic cracking reaction device and adopt this device preparation carbon nanotube, realize the serialization preparation of Single Walled Carbon Nanotube or multi-walled carbon nano-tubes, obtain high unstripped gas transformation efficiency and carbon nanotube yield simultaneously, cut down the consumption of energy.
Technical scheme of the present invention is to adopt the reaction unit of preparation carbon nanotube continuously, reaction unit is a tower reactor, this tower reactor is by catalyst container 1, catalyzer quantitative slot 2, reaction tower 3, thick products export 4, tail gas outlet 5, unstripped gas six parts such as 6 grades that enter the mouth are formed, horizontally disposed column plate 8 is arranged in the reaction tower, column plate 8 is arranged from top to bottom in order, first block of column plate 13 wherein, the 3rd block of column plate 15 and other column plate that is positioned at the odd numbers sequence connect into 20, the second blocks of column plates 14 of first group of column plate with serial verb construction 9, the 4th block of column plate 16 and other column plate that is positioned at the even numbers sequence connect into second group of column plate 21 with another serial verb construction 9.
Wherein, column plate 8 numbers in the described reaction tower 3 are 1～120, preferred 1～40.The top of catalyzer quantitative slot 2 is provided with upper flashboard 11, and the bottom is provided with lower flashboard 12.
Further, described reaction unit can be formed by connecting from beginning to end by two tower reactors, and the thick products export 4 of the tower reactor 30 on top is connected with the catalyst container 1 of the tower reactor 31 of bottom.
The material of above-mentioned reaction tower 3 and column plate 8 is quartz, superalloy, metal molybdenum or corundum.
The present invention also provides the technology that adopts this device preparation carbon nanotube, the steps include:
(1) catalyzer is fallen on the 1st block of column plate 13 by catalyzer quantitative slot 2 from catalyst container 1, when stopping at level attitude, first group of column plate 20 ask when setting that the back begins turning by connection mechanism 9, topple over the 1st whole catalysis systems on the column plate 13 when forwarding the vertical position to, got back to level attitude through upset again;
(2) in first group of column plate 20 umklapp process, second group of column plate 21 is horizontal, and catalyzer is fallen on the 2nd block of column plate 14 by the 1st block of column plate 13;
(3) after first group of column plate 20 turns back to level attitude, second group of column plate 21 begins turning by connection mechanism (9), and the catalyzer on the 2nd block of column plate 14 is fallen on the 3rd block of column plate 15, and live catalyst is fallen on the 1st block of column plate 13 simultaneously;
(4) after second group of column plate 21 turns back to level attitude, first group of column plate 20 begins turning, and the catalyzer on the catalyzer on the 1st block of column plate 13 and the 3rd block of column plate 15 is fallen respectively on the 2nd block of column plate 14, the 4th block of column plate 16;
(5) the above step that circulates, when catalyzer leaves last piece column plate 8, catalyzer falls into thick products export 4 together with carbon nanotubes grown thereon.
Wherein, catalyzer is closed lower flashboard 12 when falling into catalyzer quantitative slot 2, open upper flashboard 11, after catalyzer falls into catalyzer quantitative slot 2, closes upper flashboard 11, opens lower flashboard 12.
Comprise also that in step (3), (4) and/or (5) 8 first groups of column plates 20 of column plate and second group of column plate 21 are driven the motion that moves forward and backward of the level of doing respectively by corresponding connection mechanism 9, in fallback procedures, the material on the column plate 8 is stopped by scraper 10 to be fallen on next column plate 8.
The working temperature of tower reactor is in 400～1300 ℃ of scopes.
Tower reactor provided by the invention, catalyzer can arrive conversion zone and leave conversion zone with the fastest speed with the fastest speed, is particularly suitable for adopting solid catalyst to prepare Single Walled Carbon Nanotube continuously.In tower reactor, the motion of catalyzer is finished under mechanical force, and feed gas flow rates can be very low, thereby energy consumption is low, unstripped gas transformation efficiency height.
Description of drawings
Below in conjunction with accompanying drawing the present invention is described in further detail.
Fig. 1 is the tower reactor structural representation;
Fig. 2 is the tower reactor structural representation of combination.
Embodiment
Technical scheme of the present invention is to adopt the reaction unit of preparation carbon nanotube continuously, reaction unit is a tower reactor, this tower reactor is made up of six parts such as catalyst container, catalyzer quantitative slot, reaction tower, thick products export, tail gas outlet, unstripped gas inlets, and horizontally disposed column plate 8 is arranged in the reaction tower.
And the technology that adopts this device preparation carbon nanotube, the steps include:
(1) catalyzer is fallen on the 1st block of column plate 13 by catalyzer quantitative slot 2 from catalyst container 1, when first group of column plate 20 begins turning by connection mechanism 9 after level attitude stops setting-up time, topple over the 1st whole catalyzer on the column plate 13 when forwarding the vertical position to, got back to level attitude through upset again;
(2) in first group of column plate 20 umklapp process, second group of column plate 21 is horizontal, and catalyzer is fallen on the 2nd block of column plate 14 by the 1st block of column plate 13;
(3) after first group of column plate 20 turns back to level attitude, second group of column plate 21 begins turning by connection mechanism 9, and the catalyzer on the 2nd block of column plate 14 is fallen on the 3rd block of column plate 15, and live catalyst is fallen on the 1st block of column plate 13 simultaneously;
(4) after second group of column plate 21 turns back to level attitude, first group of column plate 20 begins turning, and the catalyzer on the catalyzer on the 1st block of column plate 13 and the 3rd block of column plate 15 is fallen respectively on the 2nd block of column plate 14, the 4th block of column plate 16:
(5) the above step that circulates, when catalyzer leaves last piece column plate 8, catalyzer falls into thick product together with carbon nanotubes grown thereon and goes out
Embodiment one: in synoptic diagram 1, the 1st, catalyst container is used to deposit live catalyst, and the 2nd, the catalyzer quantitative slot, the catalytic amount that control is thrown in to column plate at every turn, the 3rd, reaction tower, the 4th, thick products export, the 5th, reaction end gas outlet, the 6th, the unstripped gas inlet, the 7th, valve, the 8th, column plate, the 9th, connection mechanism, by it column plate is connected with mechanical means, the motion of control column plate, the 10th, scraper is responsible for material on the column plate is transferred on next column plate, the 11st, catalyzer quantitative slot upper flashboard, the 12nd, catalyzer quantitative slot lower flashboard, 13 represent the 1st block of column plate, and 14 represent the 2nd block of column plate, 15 represent the 3rd block of column plate, 16 represent the 4th block of column plate, and 20 is first group of column plate, and 21 is second group of column plate.
Illustrate that below in conjunction with Fig. 1 reaction tower prepares the process of carbon nanotube continuously: the column plate 8 in the reaction tower 3 is arranged from top to bottom in order, each column plate 8 is all for being horizontally disposed with, wherein first block of column plate 13, the 3rd block of column plate 15 and other column plate that is positioned at the odd numbers sequence connect into 20, the second blocks of column plates 14 of first group of column plate, the 3rd block of column plate 16 and other column plate that is positioned at the even numbers sequence with serial verb construction 9 and connect into second group of column plate 21 with another serial verb construction 9.Catalyzer is fallen on the 1st block of column plate 13 by catalyzer quantitative slot 2 from catalyst container 1, when being in, first group of column plate 20 begin turning by connection mechanism 9 after level attitude stops setting-up time, topple over the 1st whole catalyzer on the column plate when forwarding the vertical position to, got back to level attitude through upset again.In first group of column plate 20 umklapp process, second group of column plate 21 is horizontal, and catalyzer is fallen on the 2nd block of column plate 14 by the 1st block of column plate 13.After first group of column plate 20 turned back to level attitude, second group of column plate 21 began turning by connection mechanism 9, and the catalyzer on the 2nd block of column plate 14 is fallen on the 3rd block of column plate 15, and live catalyst is fallen on the 1st block of column plate 13 simultaneously.On first block of column plate 13 of first group of column plate 20 and the 3rd block of column plate 15 catalyzer is arranged at this moment, do not have catalyzer on second group of column plate 21.After second group of column plate 21 turned back to level attitude, first group of column plate 20 began turning, and the catalyzer on the catalyzer on the 1st block of column plate 13 and the 3rd block of column plate 15 is fallen respectively on the 2nd block of column plate 14, the 4th block of column plate 16.Later column plate moving process is undertaken by this rule.Catalyzer descends the position in the moving process of column plate gradually, contacts with reaction atmosphere simultaneously, grows carbon nanotube on catalyzer.When catalyzer leaves last piece column plate, catalyzer falls into thick products export 4 together with carbon nanotubes grown thereon.
The residence time of catalyzer in reaction tower 3 can be controlled by the quantity and the column plate 8 upset speed of control column plate 8.Stage number in the reaction tower 3 is the amount doesn't matter, a minimum column plate, and number is not limit at most.But in actual production, column plate 8 numbers generally are no more than 120.This is that promptly the residence time of catalyzer in reaction tower 3 is no more than 2 hours because the time of catalyzer carbon nano-tube generally can not surpass 2 hours.If stage number surpasses 120, the residence time less than of catalyzer on every block of column plate 1 minute, the column plate movement velocity is too fast, and operation has certain difficulty.For Single Walled Carbon Nanotube, about 10 minutes reaction times, generally use 10 blocks of column plates 8 just enough.To multi-walled carbon nano-tubes, stage number is proper 40 left and right sides, and this can guarantee to obtain maximum space-time yield.
The upset speed of column plate 8 is that the residence time in reaction tower determines by column plate quantity and catalyzer.In apparatus of the present invention, the motion of column plate 8 is interrupted, and promptly begins turning after level attitude stays for some time again, and turning back to stays for some time behind the level attitude again begins turning again.Per first group of column plate should be equal to or greater than the time of its upset in the time that level attitude stops.
Adopt tower reactor, can guarantee to obtain the high unstripped gas transformation efficiency and the utilization ratio of catalyzer.Catalyzer is constantly accepted by column plate and is toppled in reaction tower during free-falling, catalyzer is constantly stirred, and has guaranteed fully contacting of catalyzer and reaction atmosphere.Unstripped gas is entered by the unstripped gas 6 of reaction tower bottommost simultaneously, and reaction end gas is discharged by reaction end gas outlet 5 topmost, can guarantee the unstripped gas and active minimum catalyst action of concentration maximum, helps obtaining maximum carbon nanotube yield.The unstripped gas of concentration minimum (reaction end gas) contacts with the highest active catalyzer, can guarantee to obtain maximum unstripped gas transformation efficiency.This gas reactor flow direction from bottom to top near piston flow, helps atmosphere control simultaneously.
Embodiment two: adopt tower reactor also can realize the serialization preparation of different size multi-walled carbon nano-tubes.As shown in Figure 2, top tower reactor 30 is placed on the bottom reaction tower 31, form the reaction tower of combination, the activation of catalyzer and the different positions that is grown in of carbon nanotube are carried out simultaneously, realize the serialization preparation of different size multi-walled carbon nano-tubes.In the tower reactor of combination, be positioned at top tower reactor 30 and be used for deactivated catalyst, bottom tower reactor 31 is used to prepare carbon nanotube.Be connected with catalyzer quantitative slot 2 by catalyst container 1 between two tower reactors.Catalyzer falls into the catalyst container 1 of bottom tower reactor 31 after top tower reactor 3 () activation, quantitative 2 through the catalyzer quantitative slot, gradation is added on the column plate 8 of next bottom tower reactor 31.Because the buffer action of catalyzer quantitative slot 2, the atmosphere of two tower reactors is isolated fully about making.
Catalyzer quantitative slot 2 quantitative processes are as follows: close lower flashboard 12, open a flashboard 11, catalyzer falls into catalyzer quantitative slot 2.Close upper flashboard 11, open lower flashboard 12, catalyzer is fallen on the 1st block of column plate 13 of reaction tower 3, the growth response of beginning carbon nanotube.The regular movement of flashboard is realized under HYDRAULIC CONTROL SYSTEM.
The front is mentioned and is adopted the mode of upset column plate that material is transferred on next column plate from a last column plate.Sometimes, this mode is not very effective, as be combined into piece behind the catalyzer carbon nano-tube, sticks on the column plate 8, just can not realize the transfer of material by upset column plate 8.Can take the mode of push-and-pull column plate 8 to shift material in this case: i.e. the motion of column plate is carried out in the plane, only does to advance or setback, and in fallback procedures, the material on the column plate 8 is stopped by scraper 10 to be fallen on next column plate 8.In this case, column plate also is that grouping is moved, and promptly first group of column plate 20 moves simultaneously by connection mechanism 9, second group of also motion simultaneously of column plate 21.The motion of each group is all organized at another and is carried out when static, and each group immobilized time should be equal to or greater than the time of motion.
Tower reactor is particularly suitable for the serialization preparation of Single Walled Carbon Nanotube: the Single Walled Carbon Nanotube growth time is extremely short, generally about 10 minutes, and the thermograde process can not be arranged, otherwise grow multi-walled carbon nano-tubes or other carbon material on the catalyzer easily.Adopt reaction tower, can make catalyzer arrive conversion zone, contact growing single-wall carbon nano tube with reaction atmosphere with the fastest speed.When catalyzer after the conversion zone residence time reaches setting-up time, catalyzer is deviate from from column plate together with the Single Walled Carbon Nanotube of growth thereon, shifts out through thick products export.Adopt this reaction tower to prepare Single Walled Carbon Nanotube, can avoid the necessary intensification of pre-existing reactors, temperature-fall period, improved production efficiency, reduced energy consumption.
The tower reactor that the present invention is designed, its reaction tower material and column plate material can be quartz material, superalloy, metal molybdenum, silicon carbide or corundum etc.
The tower reactor that the present invention is designed, the flip-flop movement of its column plate can be by connection mechanism's 9 manual operations, also can be by gear drive.The motion that moves forward and backward of column plate can realize under HYDRAULIC CONTROL SYSTEM.
The tower reactor that the present invention is designed, its working temperature can heat by resistance wire heating or silicon carbon-point and reach in 400～1300 ℃ of scopes.
Adopting the designed tower reactor of the present invention, is catalyzer with the composite oxides of iron and rare earth element, and methane, benzene, carbon monoxide or acetylene are unstripped gas, can prepare Single Walled Carbon Nanotube continuously.Composite oxides with iron, cobalt or nickel and rare earth (or alkaline earth) element are catalyzer, and lower carbon number hydrocarbons, hydrocarbon, benzene, carbon monoxide etc. are unstripped gas, can realize the continuous preparation of multi-walled carbon nano-tubes.
Claims (11)
1, a kind of reaction unit of continuous preparation carbon nanotube, it is characterized in that: described reaction unit is a tower reactor, and above-mentioned tower reactor is made up of catalyst container (1), catalyzer quantitative slot (2), reaction tower (3), thick products export (4), tail gas outlet (5), unstripped gas inlet (6); Horizontally disposed column plate (8) is arranged in the reaction tower (3), column plate (8) is arranged from top to bottom in order, wherein first block of column plate (13), the 3rd block of column plate (15) and other column plate that is positioned at the odd numbers sequence connect into first group of column plate (20) with serial verb construction (9), and second block of column plate (14), the 4th block of column plate (16) and other column plate that is positioned at the even numbers sequence connect into second group of column plate (21) with another serial verb construction (9).
2, according to the reaction unit of the described a kind of continuous preparation carbon nanotube of claim 1, it is characterized in that: column plate (8) number in the described reaction tower (3) is 1～120.
3, a kind of continuous preparation carbon nanotube reaction unit according to claim 2, it is characterized in that: stage number is 1～40.
4, a kind of continuous preparation carbon nanotube reaction unit according to claim 1, it is characterized in that: be provided with upper flashboard (11) on the top of catalyzer quantitative slot (2), the bottom is provided with lower flashboard (12).
5, a kind of continuous preparation carbon nanotube reaction unit according to claim 1, it is characterized in that: described reaction unit is formed by connecting from beginning to end by two tower reactors, and the thick products export (4) of the tower reactor on top (30) is connected with the catalyst container (1) of the tower reactor (31) of bottom.
6, a kind of continuous preparation carbon nanotube reaction unit according to claim 1 is characterized in that: the material of described reaction tower (3) and column plate (8) is quartz, superalloy, metal molybdenum or corundum.
7, a kind of continuous preparation carbon nanotube reaction unit according to claim 1 is characterized in that unstripped gas inlet (6) is positioned at the bottom of tower reactor, and reaction end gas outlet (5) is positioned at the top of tower reactor.
8, adopt the preparation carbon nanotube technology of the described continuous preparation carbon nanotube reaction unit of claim 1, the steps include:
(1) catalyzer is fallen on the 1st block of column plate (13) by catalyzer quantitative slot (2) from catalyst container (1), when stopping at level attitude, first group of column plate (20) ask when setting that the back begins turning by connection mechanism (9), topple over the whole catalysis systems on the 1st block of column plate (13) when forwarding the vertical position to, got back to level attitude through upset again;
(2) in first group of column plate (20) umklapp process, second group of column plate (21) is horizontal, and catalyzer is fallen on the 2nd block of column plate (14) by the 1st block of column plate (13);
(3) after first group of column plate (20) turns back to level attitude, second group of column plate (21) begins turning by connection mechanism (9), and the catalyzer on the 2nd block of column plate (14) is fallen on the 3rd block of column plate (15), and live catalyst is fallen on the 1st block of column plate (13) simultaneously;
(4) after second group of column plate (21) turns back to level attitude, first group of column plate (20) begins turning, and the catalyzer on catalyzer on the 1st block of column plate (13) and the 3rd block of column plate (15) is fallen respectively on the 2nd block of column plate (14), the 4th block of column plate (16);
(5) the above step that circulates, when catalyzer leaves last piece column plate (8), catalyzer falls into thick products export (4) together with carbon nanotubes grown thereon.
9, preparation carbon nanotube technology as claimed in claim 8 is characterized in that: catalyzer is closed lower flashboard (12) when falling into catalyzer quantitative slot (2), open upper flashboard (11), after catalyzer falls into catalyzer quantitative slot (2), close upper flashboard (11), open lower flashboard (12).
10, preparation carbon nanotube technology as claimed in claim 8, it is characterized in that: comprise also that in step (3), (4) and/or (5) (8) first groups of column plates of column plate (20) and second group of column plate (21) are driven the motion that moves forward and backward of the level of doing respectively by corresponding connection mechanism (9), in fallback procedures, the material on the column plate (8) is stopped by scraper (10) to be fallen on next column plate (8).
11, continuous preparation carbon nanotube technology according to claim 8, it is characterized in that: the working temperature of tower reactor is in 400～1300 ℃ of scopes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 02113678 CN1284726C (en) | 2002-04-29 | 2002-04-29 | Reaction unit and process of continuous preparation of carbon nano-tube |
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| CN 02113678 CN1284726C (en) | 2002-04-29 | 2002-04-29 | Reaction unit and process of continuous preparation of carbon nano-tube |
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| CN1454838A CN1454838A (en) | 2003-11-12 |
| CN1284726C true CN1284726C (en) | 2006-11-15 |
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| CN103101902B (en) * | 2013-01-28 | 2014-10-29 | 深圳青铜剑电力电子科技有限公司 | Preparation equipment of nano material |
| CN106276846B (en) * | 2016-07-15 | 2018-02-23 | 华北电力大学 | A kind of system and method for preparing CNT |
| CN114699784B (en) * | 2022-04-15 | 2023-04-28 | 河南中托力合化学有限公司 | Rectifying tower for separating n-heptadecane by utilizing liquid paraffin |
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