CN114538418A - Carbon nano tube fluidization production process - Google Patents
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Abstract
The invention relates to the technical field of carbon nano-material preparation, and particularly discloses a carbon nano-tube fluidization production process. The carbon nano tube fluidization production process comprises the following steps: introducing a mixed gas containing carbon source gas and protective gas into a fluidized bed reactor filled with a catalyst to react to generate carbon nano tubes; and introducing pulse gas and/or sound waves at intervals in the reaction process. The invention breaks up secondary aggregates among the aggregates of the oligowalled array carbon nano tubes by using pulse gas and/or sound waves with an interval of 2-5 min, and keeps the oligowalled tubes in a good fluidized growth state in the middle and later growth stages by using the characteristic of fluidization hysteresis, thereby realizing the continuous and stable fluidized growth of the oligowalled array carbon nano tubes.
Description
Technical Field
The invention relates to the technical field of carbon nano-material preparation, in particular to a carbon nano-tube fluidization production process.
Background
With the development of lithium ion batteries towards high nickel, silicon carbon and high rate, a conductive agent with more excellent conductivity needs to be adopted, so that lower addition amount and lower internal resistance in the lithium battery are realized. As the wall number of the carbon nano-tube of the oligowall array is only 3-6, the carbon nano-tube has better conductivity compared with the multi-wall carbon nano-tube (the wall number is more than 10) which is currently applied in large-scale commercial application. But the packing density of the carbon nano-tube is low (about 0.01 g/cm) due to the oligowall array3) Making it difficult to perform continuous batch growth through a fluidized bed.
The carbon nano tube growing by the current fluidized bed process requires that the powder has better flowing characteristics, the powder is in a fluidized state in the growing process by controlling the flow of the gas, and the gas is ensured to be fully contacted with a catalytic center in the powder, so that the good growth of the carbon nano tube is realized. But the powder density of the oligowall array carbon nano tube powder in the middle and later growth stages is low (less than or equal to 0.02 g/cm)3) And the interactions between clusters formed by the oligowalled arrays are large, resulting in volatile fluidization in the middle and later stages of growth. After the carbon nano tube loses fluidization, on one hand, if the raw materials are continuously introduced for growth, the impurity carbon of the obtained product is increased, and the product performance is reduced; on the other hand, defluidized carbon nanotube agglomerates are more easily attached to the surface of the reactor, the adhesion force of the carbon nanotube agglomerates and the reactor is increased by the impure carbon generated by the side reaction, finally coking carbon is formed on the wall of the reactor, the coked reactor continuously adsorbs new carbon nanotubes and is coked again, the performance of the product is reduced due to continuous vicious circle, the production capacity of the reactor is continuously reduced, the coking layer needs to be cooled and cleaned, and the utilization rate of equipment is reduced. Although increasing the gas velocity can reduce the probability of the carbon nanotubes agglomerating and losing fluidization, the too high gas velocity inevitably leads to a reduction in the residence time of the carbon source gas in the reaction due to the shortened contact time of the raw material with the catalyst, a reduction in the conversion rate of the carbon source, and an increase in the production cost.
Disclosure of Invention
In order to solve the problems of product quality reduction, small quantity of batches for continuous preparation and production efficiency reduction caused by volatile fluidization of the oligo-wall array carbon nano tubes in the middle and later stages of growth, pulse gas and/or sound waves are adopted to break up secondary aggregates formed by carbon nano tube aggregates in the middle and later stages of reaction, continuous batch growth of the oligo-wall array carbon nano tubes is realized at lower operating gas velocity, and the fluctuation range of powder performance among each batch is ensured to be within +/-7%.
Specifically, the invention relates to the following technical scheme:
a carbon nano tube fluidization production process comprises the following steps: introducing a mixed gas containing carbon source gas and protective gas into a fluidized bed reactor filled with a catalyst to react to generate carbon nano tubes; introducing pulse gas and/or sound waves at intervals in the reaction process; the interval time of the pulse gas and/or the sound wave is 2 min-5 min.
The invention can break up the secondary aggregate formed by the carbon nano tube aggregate by introducing pulse gas and/or sound waves into the reaction system at intervals, so that the carbon nano tube and the catalyst are kept in a fluidized state, and the loss of fluidization is avoided, thereby realizing the continuous fluidized production of the carbon nano tube.
The secondary aggregates of the carbon nano tube aggregates are scattered by introducing pulse gas and/or sound waves, the interval time needs to be controlled within 2-5 min, if the interval is less than 2min, the retention time of the carbon source gas in the main reaction section of the fluidized bed reactor is too short, the conversion rate is reduced, and the yield of a single batch of products is also reduced; if the time interval is longer than 5min, secondary agglomerates with strong interaction between the carbon nanotube agglomerates are difficult to break up by the pulse gas and/or the sound wave, and defluidization still occurs. The reason why the secondary aggregate formed by the interaction between the carbon nanotube aggregates can be broken up by the gas pulse or the sound wave within the proper time interval is that the interaction force between the carbon nanotube aggregates is small within the proper time interval, the flowing characteristic of the powder can be enhanced by increasing the airflow or applying the sound wave, the formed secondary aggregate can be decomposed spontaneously, and the better flowing characteristic can be maintained within a shorter time due to the 'fluidization hysteresis' phenomenon of the carbon nanotube, so that the possibility of the secondary aggregation of the carbon nanotube aggregates is obviously reduced, and the carbon nanotube can be kept in a good fluidization growth state.
In some embodiments of the invention, the pulsed gas and/or sound waves are introduced at intervals after the reaction has occurred for 20 min. The cracking reaction is in the middle and later stages of the growth of the carbon nano tube after 20min, the carbon nano tube agglomeration phenomenon is easy to occur in the middle and later stages, and the secondary agglomerates formed by the carbon nano tube agglomeration can be scattered by introducing pulse gas and/or sound waves.
In some embodiments of the invention, the pulse gas and/or the sound wave is introduced for a time period of 5s to 20 s.
In some embodiments of the invention, the gas velocity of the mixture is between 0.03m/s and 0.15 m/s. The production process of the present invention can realize the continuous batch growth of carbon nanotube at relatively low operation gas speed.
In some embodiments of the present invention, the pulse gas is introduced by: and increasing the flow of the protective gas on the basis of the mixed gas. After the pulse gas is introduced, the gas velocity of the mixed gas is more than or equal to 0.2m/s, and preferably 0.2m/s to 0.30 m/s.
In some examples of the invention, the acoustic wave comprises an ultrasonic wave.
In some examples of the invention, when the sound wave is introduced at intervals, the intensity of the sound wave is more than or equal to 100dB, and preferably 100-500 dB.
In some embodiments of the invention, the gas mixture further comprises hydrogen. In the mixed gas, the volume ratio of the carbon source gas, the protective gas and the hydrogen is 1: 0.5-2: 0.00001 to 0.00005.
In some examples of the invention, the various gas flows in the mixture are: 500L/min-800L/min of carbon source gas, 500L/min-800L/min of protective gas and 5 mL/min-50 mL/min of hydrogen. Preferably, the carbon source gas is 600L/min-700L/min, the protective gas is 600L/min-700L/min, and the hydrogen gas is 10 mL/min-20 mL/min.
In some embodiments of the present invention, when the pulse gas is introduced, a protective gas with a flow rate of 2000L/min to 6000L/min, preferably 2500L/min to 5000L/min may be additionally introduced on the basis of the mixed gas.
In some embodiments of the present invention, the present invention does not specifically limit the parameters of reaction temperature, catalyst type, catalyst loading, etc., and these parameters can be determined according to the production methods commonly used in the art and can be reasonably adjusted according to actual needs. As an example, the temperature of the reaction is 600 ℃ to 800 ℃; the catalyst takes at least one of Fe, Co, Ni, Mo and Mn as an active component and takes oxide of at least one of Al, Mg, Si and La as a carrier; the ratio of the loading amount of the catalyst to the flow of the carbon source gas is 1 kg: 500L/min-800L/min.
In some embodiments of the present invention, before introducing the mixed gas of the carbon source gas and the shielding gas into the fluidized bed reactor containing the catalyst, the shielding gas is introduced into the fluidized bed reactor in advance to reduce the oxygen content in the fluidized bed reactor to less than 0.5%, and then the catalyst is added.
In some embodiments of the invention, the reaction is carried out continuously in batches, each batch having a reaction time of from 30min to 100min, preferably from 50min to 60 min. And after the reaction of each batch reaches the required time, stopping introducing the carbon source gas, blowing the materials in the fluidized bed reactor into a storage bin, and cooling the materials in a protective atmosphere.
In some examples of the invention, the batch is ≧ 100, preferably ≧ 150.
In some examples of the present invention, the specific surface area of each batch of produced carbon nanotubes is 520m or more2Per g, preferably 550m2/g～600m2/g。
In some examples of the invention, the yield of carbon nanotubes produced per batch does not exceed 10% of the average.
In some embodiments of the invention, the yield of carbon nanotubes produced per batch is 20kg/kg catalyst, preferably 22kg/kg catalyst.
In some embodiments of the present invention, the utilization rate of the carbon source in the carbon nanotube fluidized production process is greater than or equal to 60%.
In some examples of the invention, the carbon nanotubes are oligowall array carbon nanotubes. The carbon nanotube with the oligowall array is a carbon nanotube with the wall number of 3-6.
Compared with the prior art, the invention has the following beneficial effects:
due to the wall arrayThe carbon nanotube grows to a certain degree, and the bulk density is low (less than or equal to 0.02 g/cm)3) The interaction among the carbon nano tube agglomerates is increased, secondary agglomeration is easy to occur among the agglomerates, so that fluidization loss is caused, on one hand, the quality fluctuation of products is large, a reactor is coked, and on the other hand, the equipment is frequently stopped and cleaned. The invention breaks up secondary aggregates among the aggregates of the oligowalled array carbon nano tubes by using pulse airflow or ultrasonic waves with the interval of 2-5 min, and keeps the oligowalled tubes in a good fluidized growth state in the middle and later growth stages by using the characteristic of fluidization hysteresis, thereby realizing the continuous and stable fluidized growth of the oligowalled array carbon nano tubes.
Drawings
FIG. 1 is an SEM image of the carbon nanotubes of the oligowall array of example 1 at different magnifications.
Detailed Description
The invention provides a carbon nano tube fluidization production process, which is characterized in that after a carbon nano tube grows for 20min, the gas velocity is controlled to ensure that the gas velocity of a main reaction section is between 0.03m/s and 0.15m/s, pulse gas and/or sound waves are introduced at intervals of 2min to 5min and last for 5s to 20s, and secondary aggregates of carbon nano tube aggregates are scattered. When pulse gas is introduced, the gas velocity of the main reaction section needs to reach 0.2-0.30 m/s; when the sound wave is transmitted, the intensity of the sound wave is more than or equal to 100 dB.
The technical solution of the present invention is further described below with reference to specific examples. The starting materials used in the following examples, unless otherwise specified, are available from conventional commercial sources; the processes used, unless otherwise specified, are conventional in the art.
Example 1
Step 1: setting the temperature of the reactor to 650 ℃, introducing inert gas to reduce the oxygen content in the reactor to be below 0.5%, and adding 1000g of FeCoNiAlMg catalyst;
step 2: nitrogen (700L/min), ethylene (700L/min) and hydrogen (20mL/min) were fed in at a gas velocity of 0.06m/s in the main reaction zone. After 20min of ethylene feed, an additional nitrogen flow of 2800L/min was added at 2min intervals for a period of about 5 s. Ethylene was turned off after 50min of feeding ethylene, the material was blown into a silo and cooled under nitrogen atmosphere.
And step 3: carrying out continuous batch growth according to the steps 1 and 2, and counting the yield and the specific surface area of each batch (static multipoint BET method) until the yield of the single batch of carbon nano tubes is reduced by more than 10 percent of the average value or the specific surface area of the powder is reduced to 520m2The ratio of the carbon atoms to the carbon atoms is less than g.
The test results are shown in Table 1.
Meanwhile, the SEM image of the obtained product is shown in figure 1, and figure 1 shows that the obtained product has a nanotube array structure, and the number of walls is 3-6, which indicates that the oligowalled array carbon nanotube is successfully obtained.
Example 2
Step 1: setting the temperature of the reactor to 650 ℃, introducing inert gas to reduce the oxygen content in the reactor to be below 0.5%, and adding 1000g of FeCoNiAlMg catalyst;
step 2: nitrogen (700L/min), ethylene (700L/min) and hydrogen (20mL/min) were fed in at a gas velocity of 0.06m/s in the main reaction zone. After 20min of ethylene introduction, nitrogen was additionally introduced at intervals of 5min at a flow rate of 4600L/min for a duration of about 15 s. Ethylene was turned off after 50min of feeding ethylene, the material was blown into a silo and cooled under nitrogen atmosphere.
And step 3: carrying out continuous batch growth according to the steps 1 and 2, and counting the yield and the specific surface area of each batch (static multipoint BET method) until the yield of the single batch of carbon nano tubes is reduced by more than 10 percent of the average value or the specific surface area of the powder is reduced to 520m2The ratio of the carbon atoms to the carbon atoms is less than g.
The test results are shown in Table 1.
Example 3
Step 1: setting the temperature of the reactor to 650 ℃, introducing inert gas to reduce the oxygen content in the reactor to be below 0.5%, and adding 1000g of FeCoNiAlMg catalyst;
step 2: nitrogen (700L/min), ethylene (700L/min) and hydrogen (20mL/min) were fed in at a gas velocity of 0.06m/s in the main reaction zone. After ethylene is introduced for 20min, sound waves are introduced at intervals of 3min, the intensity of the sound waves is 150dB, and the duration is about 10 s. Ethylene was turned off after 50min of feeding ethylene, the material was blown into a silo and cooled under nitrogen atmosphere.
And step 3: according to the steps 1 and 2Growing in batches, and counting the yield and the specific surface area of each batch (static multipoint BET method) until the yield of the single batch of the carbon nano tubes is reduced by more than 10 percent of the average value or the specific surface area of the powder is reduced to 520m2The ratio of the carbon atoms to the carbon atoms is less than g.
The test results are shown in Table 1.
Comparative example 1
This comparative example differs from example 1 in that: the time interval of the pulse gas is reduced to below 2min, specifically 1.5 min.
Step 1: setting the temperature of the reactor to 650 ℃, introducing inert gas to reduce the oxygen content in the reactor to be below 0.5%, and adding 1000g of FeCoNiAlMg catalyst;
step 2: nitrogen (700L/min), ethylene (700L/min) and hydrogen (20mL/min) were fed in at a gas velocity of 0.06m/s in the main reaction zone. After 20min of ethylene feed, an additional nitrogen flow of 2800L/min was added at 1.5min intervals for a period of about 5 s. Ethylene was turned off after 50min of feeding ethylene, the material was blown into a silo and cooled under nitrogen atmosphere.
And step 3: carrying out continuous batch growth according to the steps 1 and 2, and counting the yield and the specific surface area of each batch (static multipoint BET method) until the yield of the single batch of carbon nano tubes is reduced by more than 10 percent of the average value or the specific surface area of the powder is reduced to 520m2The ratio of the carbon atoms to the carbon atoms is below g.
The test results are shown in Table 1.
Comparative example 2
This comparative example differs from example 1 in that: the time interval of the pulse gas is increased to more than 5min, specifically 6 min.
Step 1: setting the temperature of the reactor to 650 ℃, introducing inert gas to reduce the oxygen content in the reactor to be below 0.5%, and adding 1000g of FeCoNiAlMg catalyst;
step 2: nitrogen (700L/min), ethylene (700L/min) and hydrogen (20mL/min) were introduced at a gas velocity of 0.06m/s in the main reaction zone. After 20min of ethylene feed, nitrogen was additionally fed at intervals of 6min at a rate of 4400L/min for a period of about 15 s. After 50min of ethylene was fed in, the ethylene was turned off, and the material was blown into a silo and cooled in a nitrogen atmosphere.
And step 3: according to the steps 1 and 1Step 2, carrying out continuous batch growth, and counting the yield and the specific surface area of each batch (static multipoint BET method) until the yield of the single batch of the carbon nano tubes is reduced by more than 10 percent of the average value or the specific surface area of the powder is reduced to 520m2The ratio of the carbon atoms to the carbon atoms is below g.
The test results are shown in Table 1.
TABLE 1 continuous batch fluidized growth of carbon nanotubes
As can be seen from Table 1, in the examples 1 to 3, the pulse gas inlet or the sound wave is added in the middle and later growth stages, more than 150 batches of continuous growth oligowall pipes are realized, the average utilization rate of the carbon source is more than or equal to 60 percent, and the yield and the specific surface area fluctuation of each batch are within 7 percent. In comparative example 1, the pulse gas supply interval achieved continuous growth of approximately 200 batches, but the yield per batch was lower by 17% or more and the carbon source conversion rate was only 49.6%. In comparative example 2, the interval between the pulse gas injections was too long, the secondary agglomerates of carbon tube agglomerates were difficult to break up by increasing the gas flow, the fluidization state in the middle and later stages of growth deteriorated, the number of continuous batches for stable fluidized growth decreased sharply, and the yield and performance fluctuation of the continuous batches increased.
The results show that the secondary aggregate of the carbon tube aggregate is broken up by adopting the method of pulse airflow or sound wave, the fluidization state of the oligowall array carbon nano tube in the middle and later growth periods can be effectively improved, and more than 150 batches of continuous and stable fluidization growth can be realized.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A carbon nano tube fluidization production process is characterized in that: the method comprises the following steps: introducing a mixed gas containing carbon source gas and protective gas into a fluidized bed reactor filled with a catalyst to react to generate carbon nano tubes; introducing pulse gas and/or sound waves at intervals in the reaction process; the interval time of the pulse gas and/or the sound wave is 2 min-5 min.
2. The carbon nanotube fluidization production process according to claim 1, wherein: and introducing the pulse gas and/or the sound wave at intervals after the reaction occurs for 20 min.
3. The carbon nanotube fluidization production process according to claim 1, wherein: the duration of each time of pulse gas and/or sound wave introduction is 5 s-20 s.
4. The carbon nanotube fluidization production process according to claim 1, wherein: the gas velocity of the mixed gas is between 0.03m/s and 0.15 m/s.
5. The carbon nanotube fluidization production process according to claim 4, wherein: the introduction mode of the pulse gas is as follows: and increasing the flow of the protective gas on the basis of the mixed gas.
6. The carbon nanotube fluidization production process according to claim 5, wherein: after the pulse gas is introduced, the gas velocity of the mixed gas is more than or equal to 0.2 m/s.
7. The carbon nanotube fluidization production process according to claim 1, wherein: when the sound wave is introduced at intervals, the intensity of the sound wave is more than or equal to 100 dB.
8. The carbon nanotube fluidization production process according to claim 1, wherein: the reaction is continuously carried out in batches, and the reaction time of each batch is 30-100 min.
9. The carbon nanotube fluidized production process according to claim 8, wherein: the batch is more than or equal to 100.
10. The carbon nanotube fluidization production process according to any one of claims 1 to 9, wherein: the carbon nano tube is an oligowall array carbon nano tube.
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