CN106395794B - A kind of coupling fluidized bed carbon nanotube efficient continuous preparation method - Google Patents
A kind of coupling fluidized bed carbon nanotube efficient continuous preparation method Download PDFInfo
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- CN106395794B CN106395794B CN201610784804.4A CN201610784804A CN106395794B CN 106395794 B CN106395794 B CN 106395794B CN 201610784804 A CN201610784804 A CN 201610784804A CN 106395794 B CN106395794 B CN 106395794B
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Abstract
The present invention relates to be related to technical field of material, more particularly to a kind of coupling fluidized bed carbon nanotube efficient continuous preparation method, the preparation method comprises the following steps: catalyst reduction activated reactor is placed in carbon nanotube reactor, the reduction activation of catalyst is completed by the cracked gas waste heat generated in carbon nanotube growth process, catalyst is continuously introduced into fluidized bed carbonization reactor again, carbon nano tube growth reaction carries out in the intermediate circular fluidized-bed reactor with circulation, obtained carbon nanotube agglomerate bulky grain is collected by lower part fluidized bed collector, the carbon nanotube of collection is continuously and uniformly removed from fluidized bed carbonization reactor later, up to product, catalyst reduction activation and carburizing reagent are coupled in one by the present invention, the reduction activation of catalyst is completed in carbonisation, save operation Time improves the efficiency of entire reaction unit, and catalyst is avoided to be crushed as caused by the charging of air pulse spray regime.
Description
Technical field
The present invention relates to technical field of material, and in particular to a kind of coupling fluidized bed carbon nanotube high-efficiency and continuous preparation
Method.
Background technique
Carbon nanotube is considered as a kind of new function material and structural material haveing excellent performance, and becomes and grinds in the latest 20 years
The hot spot studied carefully.Up to the present, preparation carbon nanotube is there are many method, but most important method only there are three types of, i.e., arc process,
Laser ablation method and gas phase chemical deposition.Chemical vapor deposition method be using nano-level iron, silver etc. as catalyst, lower carbon number hydrocarbons,
Hydrocarbon or carbon monoxide are unstripped gas, and the method for catalytic cracking reaction growth carbon nanotube occurs at high temperature.The party
The produced carbon nano pipe purity of method is high, specification is controllable, and is easy to industrial amplification, it is considered to be most have development prospect prepares carbon
The method of nanotube.
The premise that carbon nanomaterial is used widely is the development and continuous maturation of inexpensive batch techniques, at present in carbon
Nanotube production aspect mostly uses chemical vapor deposition method, uses fluidized-bed reactor to be produced, but in carbon nanotube system
Before standby, also need to carry out reduction activation to its catalyst.But catalytic amount required for prepared by every batch of carbon nanotube is few, and restores
Activation condition is special, needs to carry out in another individual reactor, process is cumbersome, complicated, can not achieve real meaning
Serialization preparation in justice.In addition, being easily caused during the good catalyst of reduction activation is shifted toward carbonization reactor conveying
Catalyst granules is crushed, therefore can change the growth morphology and speed of carbon pipe.The operating time of carbon nanotube production every batch of
It is long, entire reaction unit it is inefficient.Meanwhile fluidized-bed reactor because temperature distributing characteristic and hydrocarbon gas Pintsch process it is anti-
The endothermic character answered can not achieve the high yield production of carbon nanotube.Therefore, it is necessary to provide a kind of new high efficiency continuously system
Preparation Method, to overcome drawbacks described above.
Summary of the invention
The present invention provides a kind of coupling fluidized bed carbon nanotube efficient continuous preparation method, the preparation method will be catalyzed
Agent reduction activation and carburizing reagent are coupled in one, and the reduction activation of catalyst is completed in carbonisation, save the operating time,
The efficiency for improving entire reaction unit avoids catalyst from being crushed as caused by the charging of air pulse spray regime.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of coupling fluidized bed carbon nanotube efficient continuous preparation method, comprising the following steps: will be good by heating conduction
Metal material made of catalyst reduction activated reactor be placed in carbon nanotube reactor, by carbon nanotube growth process
The cracked gas waste heat of middle generation completes the reduction activation of catalyst, then the catalyst of reduction activation is continuously introduced into fluidized bed carbon
Change in reactor, the fluidized bed carbonization reactor is received by top settling section, intermediate circular fluidized-bed reactor, lower part fluidized bed
Storage three parts constitute, carbon nano tube growth reaction in the biggish intermediate circular fluidized-bed reactor with circulation of internal diameter into
Row, obtained carbon nanotube agglomerate bulky grain is collected by lower part fluidized bed collector, later by the carbon nanometer of collection
Pipe is continuously and uniformly removed from fluidized bed carbonization reactor to get product.
Preferably, the catalyst is continuously and uniformly sent anti-to catalyst reduction activation by way of screw conveyer
It answers in device, the temperature of control catalyst reduction activated reactor is 350~650 DEG C, and the mixed gas for being passed through hydrogen and carrier gas arrives
In the reactor, hydrogen and the volume ratio of carrier gas are 1:0.5~2.0, the air speed of reduction activation reaction in the mixed gas
For 1~15h-1, linear gas velocity is 0.05~2.0m/s, and the carrier gas is nitrogen or argon gas.
Preferably, the bottom sides of the catalyst reduction activated reactor are provided with the board-like sealing valve pneumatically opened,
It is periodically turned on by phased manner, by applying an air pulse at top, with same mass flowrate by the catalysis of reduction activation
Agent is transmitted in fluidized bed carbonization reactor.
Preferably, the temperature of the intermediate circular fluidized-bed reactor is 550~750 DEG C, respectively in intermediate ring when reaction
The mixed gas for flowing the inner cylinder distributor of fluidized bed, being passed through carbon-source gas and carrier gas in annular space distributor, in the mixed gas
The volume ratio of carbon-source gas and mixed gas is 1:0.5~2.0, and the carrier gas is the mixed gas of nitrogen and argon gas；Inner cylinder point
In cloth device or annular space distributor, reaction velocity is 0.6~1.5h-1, the linear speed of mixed gas is 0.5~1.5m/s, is higher than
Catalyst and the short grained minimum fluidization velocity of carbon nanotube, lower than the minimum fluidization velocity of carbon nanotube agglomerate bulky grain.
Preferably, the carbon-source gas is the following lower carbon number hydrocarbons of five carbon.
Preferably, in the carbon nano tube growth reaction process, carbon nanotube agglomerate bulky grain is constantly from centre
It screens out and in the multiple dimensioned particle stream of circular fluidized-bed reactor, continuously enter in the fluidized bed collector of lower part, using inertia
Gas nitrogen or argon gas are fluidizing agent, and control linear speed is 0.1~0.5m/s, so that carbon nanotube is in loosening state, then pass through
Screw conveyer mode or air pulse spray regime remove carbon nanotube from reactor.
Preferably, the inner/outer tube radius ratio of the intermediate circulation fluidized bed is 0.3~0.8, and inner cylinder ratio of height to diameter is 4~9, interior
Outer cylinder linear gas velocity ratio is 2~4.
Preferably, the catalyst reduction activated reactor can also be top half by the good metal material of heating conduction
Material is made, and lower half portion is made of the powder of stainless steel agglomerated material with filtration, is produced using carbon nanotube preparation process
The cracking gas of the raw hydrogen for containing 20~50% carries out the reduction activation of catalyst as reducing agent.
Preferably, the catalyst is single-phase transition metal or its alloy, or contains the single-phase transition metal or its conjunction
The organic compound of gold.
The invention has the benefit that catalyst reduction activation and carburizing reagent are coupled in one by the present invention, wherein urging
The normal flow fluidized bed reactor of agent reduction activation part is placed in carbon nano tube growth reactor head settling section, by means of
The waste heat of the cracked gas of carbon nano tube growth reaction process completes the reduction activation of catalyst in carbonisation, saves behaviour
Make the time, improve the efficiency of entire reaction unit, catalyst is avoided to be crushed as caused by the charging of air pulse spray regime.Carbon
Nanotube growing process carries out in the biggish intermediate circular fluidized-bed reactor with circulation of internal diameter, reinforces gas-solid contact effect
Rate avoids the problem that conversion zone Temperature Distribution caused by carbon pipe fast-growth and reactant concentration are unevenly distributed；Operating linear velocity
Control is being higher than catalyst and the short grained minimum fluidization velocity of carbon nanotube, and most lower than carbon nanotube agglomerate bulky grain
Small fluidizing velocity, so that this part carbon nanotube agglomerate bulky grain be made to sieve from the multiple dimensioned particle stream of carbon nanotube reactor
It branches away, continuously into lower part fluidized bed collector, and uses inert gas for fluidizing agent, be at loosening state,
Convenient for removing from reactor, serialization preparation is really realized.
Detailed description of the invention
Fig. 1 is the implementation diagram of the embodiment of the present invention 1；
Fig. 2 is the implementation diagram of the embodiment of the present invention 2.
Specific embodiment
Further illustrate technical solution of the invention combined with specific embodiments below, embodiment is not to be construed as pair
The limitation of technical solution.
Embodiment 1:
A kind of coupling fluidized bed carbon nanotube efficient continuous preparation method is present embodiments provided, process is as shown in Figure 1, tool
Steps are as follows for body:
Catalyst 1 101 is continuously and uniformly sent to by the good metal material of heating conduction by way of screw conveyer
In manufactured catalyst reduction activated reactor 102, the temperature of catalyst reduction activated reactor 102 is controlled at 350~650 DEG C
Between, it is passed through in the mixed gas 2 to catalyst reduction activated reactor 102 of hydrogen and nitrogen or argon gas, hydrogen in mixed gas
The volume ratio of gas and nitrogen or argon gas is 1:0.5~2.0, and holding reduction activation reaction velocity is 1~15h-1, linear gas velocity is
0.05~2.0m/s.
The board-like sealing valve 103 pneumatically opened is provided in the bottom sides of catalyst reduction activated reactor 102, therebetween
It periodically turns on to disconnected property, by applying an air pulse 3 at top, urging for reduction activation will be completed with same mass flowrate
Agent is transmitted in fluidized bed carbonization reactor 104.Wherein fluidized bed carbonization reactor 104 is by top settling section 1041, centre
Circular fluidized-bed reactor 1042,1043 three parts of lower part fluidized bed collector are constituted, and catalyst reduction activated reactor 102 is put
It sets in carbon nanotube reactor 104, specifically in the top settling section 1041 on 104 top of carbon nanotube reactor.
The temperature of intermediate circular fluidized-bed reactor 1042 is controlled between 550~750 DEG C, is fluidized respectively in intermediate circulation
Inner cylinder distributor 10421, the annular space distributor 10422 of bed reactor are passed through the mixed of five carbon lower carbon number hydrocarbons below and nitrogen or argon gas
Gas 4 is closed, the volume ratio of five carbon lower carbon number hydrocarbons below and nitrogen or argon gas is 1:0.5~2.0 in mixed gas gas 4, in
Between circular fluidized-bed reactor 1042 inner cylinder distributor 10421 or annular space distributor 10422 in, the linear speed of mixed gas 4
Control is higher than catalyst and the short grained minimum fluidization velocity of carbon nanotube between 0.5~1.5m/s, is lower than carbon nanotube
The minimum fluidization velocity of aggregation bulky grain, inner cylinder distributor 10421 or the control of 10422 air speed of annular space distributor 0.6~
1.5h-1Between.
The inner/outer tube radius ratio of the intermediate circular fluidized-bed reactor 1042 of fluidized bed carbonization reactor 104 is r/R=0.3
~0.8, inner cylinder ratio of height to diameter is h/r=4~9, and inner/outer tube gas line Transmission Ratio Control is between 2~4.With carburizing reagent into
Row, carbon nanotube agglomerate bulky grain are constantly screened out from the multiple dimensioned particle stream of intermediate circular fluidized-bed reactor 1042
Come, continuously enters in lower part fluidized bed collector 1043, as the collector of carbon nanotube agglomerate bulky grain, using inertia
Gas nitrogen or argon gas are fluidizing agent 5, enter 1043 bottom of lower part fluidized bed collector by distributor 10431, use is lazy
Property gas nitrogen or argon gas be fluidizing agent, control linear speed be 0.1~0.5m/s, be at loosening state, passed by screw rod
Mode or air pulse spray regime 105 is sent to remove product 6 to get product from lower part fluidized bed collector 1043.This implementation
Example can be achieved to talk the serialization preparation of nanotube, and wherein carburizing reagent cracking gas 7 is arranged at the top of fluidized bed carbonization reactor 104
Out.
Embodiment 2
Coupling fluidized bed carbon nanotube efficient continuous preparation method is present embodiments provided, process is as shown in Fig. 2, specific step
It is rapid as follows:
This method is made of catalyst reduction activation and carburizing reagent two parts, wherein catalyst reduction activated reactor
101 be normal flow fluidized bed reactor, and 101 top half 1011 of catalyst reduction activated reactor is by the good metal of heating conduction
Material is made, and lower half portion 1012 is made of the powder of stainless steel agglomerated material for capableing of filtration.Fluidized bed carburizing reagent
Device 104 is made of three parts, including top settling section 1041, intermediate circular fluidized-bed reactor 1042, lower part fluidized bed are collected
Device 1043.Wherein catalyst reduction activated reactor 101 is placed in carbon nanotube reactor 104, specifically anti-in carbon nanotube
In the top settling section 1041 for answering 104 top of device.
It is heavy at the top of bed carbonization reactor by means of changing in carbon nano tube growth reaction process in carbon nanotube preparation process
The hydrogen in the cracked gas waste heat and cracking gas of section 1041 is dropped, catalyst reduction activation process is completed.In preparation process, it will urge
Agent 1 102 is continuously and uniformly sent into catalyst reduction activated reactor 101 by way of screw conveyer, catalyst reduction
For the control of activated reactor temperature at 350~650 DEG C, the cracking gas of carburizing reagent passes through catalyst reduction activated reactor 101
The powder of stainless steel sintering filter plate of lower half portion 1012 fluidizes catalyst 1, contacts with catalyst, carries out catalyst
Reduction activation, maintains 5~20min of reduction activation process, and linear gas velocity control is 0.05~2.0m/s.
In the bottom sides of catalyst reduction activated reactor 101, the board-like sealing valve 103 pneumatically opened, discontinuity are set
Ground periodically turns on, and by applying an air pulse 2 at top, is transmitted to the catalyst of reduction activation with same mass flowrate
In fluidized bed carbonization reactor 104.The temperature for maintaining intermediate circular fluidized-bed reactor 1042 is 550~750 DEG C, respectively in ring
Stream fluidized bed inner cylinder distributor 10421, annular space distributor 10422 be passed through five carbon of carbon-source gas lower carbon number hydrocarbons below and nitrogen or
The mixed gas 4 of argon gas, the volume ratio of five carbon lower carbon number hydrocarbons below and nitrogen or argon gas is 1:0.5~2.0 in mixed gas 4,
In the inner cylinder distributor 10421 or annular space distributor 10422 of intermediate circular fluidized-bed reactor 1042, mixed gas 4
Linear speed controls between 0.5~1.5m/s, is higher than catalyst and the short grained minimum fluidization velocity of carbon nanotube, and receives lower than carbon
The minimum fluidization velocity of mitron aggregation bulky grain, inner cylinder distributor 10421 or the control of 10422 air speed of annular space distributor exist
Between 0.6~1.5h.
The inner/outer tube radius ratio of the intermediate circular fluidized-bed reactor 1042 of fluidized bed carbonization reactor 104 is r/R=0.3
~0.8, inner cylinder ratio of height to diameter is h/r=4~9, and inner/outer tube gas line Transmission Ratio Control is between 2~4.With carburizing reagent into
Row, carbon nanotube agglomerate bulky grain are constantly screened out from the multiple dimensioned particle stream of intermediate circular fluidized-bed reactor 1042
Come, continuously enters in lower part fluidized bed collector 1043, as the collector of carbon nanotube agglomerate bulky grain, using inertia
Gas nitrogen or argon gas are fluidizing agent 5, enter 1043 bottoms by distributor 10431, and control linear speed is 0.1~0.5m/s,
It is at loosening state, is moved product 6 from collector 1043 by screw conveyer mode or air pulse spray regime 105
Out, serialization preparation is realized.Wherein carburizing reagent cracking gas 7 is discharged at the top of reduction activation fluidized bed 101.
The above are the descriptions to the embodiment of the present invention to keep this field special by the foregoing description of the disclosed embodiments
Industry technical staff can be realized or using the present invention.Various modifications to these embodiments carry out those skilled in the art
Saying will be apparent, and the general principles defined herein can be the case where not departing from the spirit or scope of the present invention
Under, it realizes in other embodiments.Therefore, the present invention will not be limited to the embodiments shown herein, but to accord with
Close the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. a kind of coupling fluidized bed carbon nanotube efficient continuous preparation method, which comprises the following steps: will be by thermally conductive
Catalyst reduction activated reactor made of metal material of good performance is placed in carbon nanotube reactor, by carbon nanotube
The cracked gas waste heat generated in growth course completes the reduction activation of catalyst, then the catalyst of reduction activation is continuously introduced into
In fluidized bed carbonization reactor, the fluidized bed carbonization reactor is by top settling section, intermediate circular fluidized-bed reactor, lower part
Fluidized bed collector three parts are constituted, and carbon nano tube growth is reacted in the biggish intermediate circulation fluidized-bed reaction with circulation of internal diameter
It is carried out in device, obtained carbon nanotube agglomerate bulky grain is collected by lower part fluidized bed collector, later by collection
Carbon nanotube is continuously and uniformly removed from fluidized bed carbonization reactor to get product.
2. coupling fluidized bed carbon nanotube efficient continuous preparation method according to claim 1, which is characterized in that described to urge
Agent is continuously and uniformly sent by way of screw conveyer into catalyst reduction activated reactor, control catalyst reduction activation
The temperature of reactor is 350 ~ 650 DEG C, is passed through in the mixed gas to the reactor of hydrogen and carrier gas, in the mixed gas
Hydrogen and the volume ratio of carrier gas are 1:0.5 ~ 2.0, and the air speed of reduction activation reaction is 1 ~ 15h -1, linear gas velocity is 0.05 ~ 2.0
M/s, the carrier gas are nitrogen or argon gas.
3. coupling fluidized bed carbon nanotube efficient continuous preparation method according to claim 1, which is characterized in that described to urge
The bottom sides of agent reduction activation reactor are provided with the board-like sealing valve pneumatically opened, and periodically turn on by phased manner, lead to
It crosses and applies an air pulse at top, the catalyst of reduction activation is transmitted to by fluidized bed carburizing reagent with same mass flowrate
In device.
4. coupling fluidized bed carbon nanotube efficient continuous preparation method according to claim 1, which is characterized in that in described
Between the temperature of circular fluidized-bed reactor be 550 ~ 750 DEG C, respectively in inner cylinder distributor, the ring of intermediate circulation fluidized bed when reaction
The mixed gas of carbon-source gas and carrier gas is passed through in gap distributor, the volume of carbon-source gas and mixed gas in the mixed gas
Than for 1:0.5 ~ 2.0, the carrier gas is the mixed gas of nitrogen and argon gas；In inner cylinder distributor or annular space distributor, reaction
Air speed is 0.6 ~ 1.5h-1, the linear speed of mixed gas is 0.5 ~ 1.5m/s, is higher than catalyst and the short grained minimum of carbon nanotube
Fluidizing velocity, lower than the minimum fluidization velocity of carbon nanotube agglomerate bulky grain.
5. coupling fluidized bed carbon nanotube efficient continuous preparation method according to claim 4, which is characterized in that the carbon
Source gas is the following lower carbon number hydrocarbons of five carbon.
6. coupling fluidized bed carbon nanotube efficient continuous preparation method according to claim 1, which is characterized in that described
In carbon nano tube growth reaction process, carbon nanotube agglomerate bulky grain is constantly from more rulers of intermediate circular fluidized-bed reactor
It screens out to come in degree particle stream, continuously enter in the fluidized bed collector of lower part, inert nitrogen gas or argon gas is used to be situated between for fluidisation
Matter, control linear speed are 0.1 ~ 0.5m/s, so that carbon nanotube is in loosening state, then spray by screw conveyer mode or air pulse
It penetrates mode and removes carbon nanotube from reactor.
7. coupling fluidized bed carbon nanotube efficient continuous preparation method according to claim 1, which is characterized in that in described
Between circulation fluidized bed inner/outer tube radius ratio be 0.3 ~ 0.8, inner cylinder ratio of height to diameter be 4 ~ 9, inner/outer tube linear gas velocity ratio be 2 ~ 4.
8. coupling fluidized bed carbon nanotube efficient continuous preparation method according to claim 1, which is characterized in that described to urge
Agent reduction activation reactor is made of top half of the good metal material of heating conduction, and lower half portion is by having filtering to make
Powder of stainless steel agglomerated material is made, and utilizes the cracking gas for the hydrogen for containing 20 ~ 50% that carbon nanotube preparation process generates
The reduction activation of catalyst is carried out as reducing agent.
9. coupling fluidized bed carbon nanotube efficient continuous preparation method according to claim 1-8, feature exist
In the catalyst is single-phase transition metal or its alloy, or the organic compound containing the single-phase transition metal or its alloy
Object.
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| CN114538418B (en) * | 2021-12-31 | 2023-05-23 | 佛山市格瑞芬新能源有限公司 | Fluidization production process of carbon nano tube |
| CN114394588A (en) * | 2022-02-09 | 2022-04-26 | 武汉先见科技有限公司 | Method for continuously producing graphene by fluidized bed |
| CN115321524B (en) * | 2022-07-15 | 2023-10-20 | 深圳烯湾科技有限公司 | Process for preparing carbon nano tube by carbon nano tube and fluidized bed |
| CN115285976B (en) * | 2022-07-15 | 2023-08-22 | 深圳烯湾科技有限公司 | Carbon nano tube and fluidized bed preparation process for carbon nano tube |
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| CN1327943A (en) * | 2001-05-25 | 2001-12-26 | 清华大学 | Process and reactor for continuously preparing nm carbon tubes with fluidized bed |
| CN101049927A (en) * | 2007-04-18 | 2007-10-10 | 清华大学 | Method for producing Nano carbon tubes continuously and equipment |
| CN102120570A (en) * | 2011-01-22 | 2011-07-13 | 广州市白云化工实业有限公司 | Device and process method for continuously producing carbon nanotubes |
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|---|---|---|---|---|
| CN1327943A (en) * | 2001-05-25 | 2001-12-26 | 清华大学 | Process and reactor for continuously preparing nm carbon tubes with fluidized bed |
| CN101049927A (en) * | 2007-04-18 | 2007-10-10 | 清华大学 | Method for producing Nano carbon tubes continuously and equipment |
| CN102120570A (en) * | 2011-01-22 | 2011-07-13 | 广州市白云化工实业有限公司 | Device and process method for continuously producing carbon nanotubes |
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