CN105600767B - The preparation method and device of carbon nanotube sponge - Google Patents
The preparation method and device of carbon nanotube sponge Download PDFInfo
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- CN105600767B CN105600767B CN201511004895.7A CN201511004895A CN105600767B CN 105600767 B CN105600767 B CN 105600767B CN 201511004895 A CN201511004895 A CN 201511004895A CN 105600767 B CN105600767 B CN 105600767B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C01B2202/32—Specific surface area
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Abstract
The preparation method of carbon nanotube sponge includes the following steps: a, nickel oxide is placed in weight percentage to impregnate 1~10 hour in 10~50% citric acid solution, after 200~900 DEG C 0.2~1 hour dry, obtains nickel oxide C catalyst；B, nickel oxide C catalyst made from step a is placed in reacting furnace; it is passed through nitrogen or inert gas into reacting furnace from carrier gas tank again; and the temperature in reacting furnace is risen to 500~900 DEG C by temperature controller under nitrogen or inert gas shielding; then make 0.05~0.5:1 of flow-rate ratio of the hydrogen being passed through in reacting furnace and propylene by adjusting the flowmeter of hydrogen gas tank and propylene tank respectively; after reaction 0.5~2 hour; cooled to room temperature to get arrive carbon nanotube sponge.The present invention also provides the devices for realizing carbon nanotube sponge preparation method.The dispersibility of carbon nanotube sponge produced by the present invention is better than conventional carbon nanotube, and yield is high, suitable for mass production.The present invention also have the characteristics that preparation process and device be simple and convenient to operate, reaction condition it is mild.
Description
[technical field]
The present invention relates to the preparations of carbon nanotube, high and suitable for mass production more particularly to a kind of simple process, yield
Carbon nanotube sponge preparation method and device.
[background technique]
Carbon nanotube has high ratio modulus, and high specific strength is highly conductive to wait excellent properties, can be used as catalyst and catalyst carries
Body, lithium ion battery, microelectronic component, absorbing material, super capacitor material, high-efficiency adsorbent, release agent, structure strengthening material
Material etc. receives extensive research and concern in recent years.However, carbon nanotube obtained is microstructure under normal circumstances,
It is macroscopically being powdered or graininess, bad dispersibility, it usually needs using mechanical damage grinding distribution or destroy carbon Guan Wei
The method of structure grafted functional group, not only preparation process is complicated for this, but also the performance for making carbon nanotube itself can not be played
Come, the application of carbon nanotube is caused to be restricted.
Currently, carbon nano-tube macroscopic body is other than having powdered or graininess, macroscopic form there are also carbon nanotube long filament,
Carbon nano-tube film, carbon nano pipe array and carbon nanotube sponge.Wherein, carbon nanotube sponge is due to high specific surface area
With porosity, compared with low-density, preferable macroscopic property and electric conductivity and good dispersion, reinforced composite material, greasy dirt absorption,
The fields such as microelectronic component have a good application prospect.However, the method for existing preparation carbon nanotube sponge mainly has matrix
Method, floating catalyst system and chemical vapour deposition technique, there are complex process, severe reaction conditions and the not high problem of yield, system
Carbon nanotube sponge weight with the use of the weight ratio of catalyst is up to 40~60, be not suitable for batch production.Therefore, such as
What simplifies the preparation process of carbon nanotube sponge, the yield of raising carbon nanotube sponge just becomes a kind of objective demand.
[summary of the invention]
Present invention seek to address that the above problem, and provide that a kind of preparation process is simple, yield is high, suitable for mass production, and
The preparation method of the good carbon nanotube sponge of carbon nanotube sponge dispersion performance obtained.
The present invention also provides a kind of devices for realizing the carbon nanotube sponge preparation method.
To achieve the purpose of the present invention, the present invention provides a kind of preparation method of carbon nanotube sponge, this method includes
Following steps:
A, nickel oxide is placed in the citric acid solution that weight percentage is 10~50% and is impregnated 1~10 hour, through 200
~900 DEG C after drying 0.2~1 hour, obtain nickel oxide C catalyst；
B, nickel oxide C catalyst made from step a is placed in reacting furnace, then is passed through nitrogen into reacting furnace from carrier gas tank
Gas or inert gas, and the temperature in reacting furnace is risen to 500~900 by temperature controller under nitrogen or inert gas shielding
DEG C, then make the flow-rate ratio of the hydrogen being passed through in reacting furnace and propylene by adjusting the flowmeter of hydrogen gas tank and propylene tank respectively
0.05~0.5:1, reaction 0.5~2 hour after, cooled to room temperature to get arrive carbon nanotube sponge.
In step b, the nitrogen or inert gas are carrier gas, and the hydrogen is growth promoter, and the propylene is carbon source.
The inert gas is argon gas.
In step b, the weight of obtained carbon nanotube sponge and the weight ratio of reacting furnace internal oxidition nickel C catalyst are
100~150.
The present invention also provides a kind of device for realizing the carbon nanotube sponge preparation method, the device be equipped with reacting furnace and
For controlling the temperature controller of reaction in-furnace temperature, the probe of the temperature controller is contacted with the inner wall of reacting furnace, the reacting furnace
Air inlet is connected separately with carrier gas tank, propylene tank and hydrogen gas tank, in the carrier gas tank, propylene tank and hydrogen gas tank and reacting furnace air inlet
The flowmeter of control flow is respectively provided between mouthful.
The air inlet of the reacting furnace is connected with four-way union, and the carrier gas tank, propylene tank and hydrogen gas tank pass through respectively
The connection of the air inlet of four-way union and reacting furnace.
The reacting furnace is tube furnace.
Contribution of the invention is, efficiently solves existing carbon nanotube bad dispersibility, complex process and low output
Problem.The present invention is by the way that using nitrogen or inert gas as carrier gas, propylene is carbon source, and hydrogen is growth promoter, and nickel oxide carbon is
Catalyst is obtained with carbon nanotube sponge existing for spongy state.The dispersibility of carbon nanotube sponge produced by the present invention is better than normal
The carbon nanotube of rule, it is not easy to reunite, and the weight of carbon nanotube obtained and the weight ratio using catalyst are 100~150, are produced
Amount is high, suitable for mass production.The present invention also have the characteristics that preparation process and device be simple and convenient to operate, reaction condition it is mild.
[Detailed description of the invention]
Fig. 1 is reaction unit structural schematic diagram of the invention.
Fig. 2 is the image of carbon nanotube sponge of the invention.
Fig. 3 is the scanning electron microscope diagram of carbon nanotube sponge of the invention.
[specific embodiment]
The following example is that of the invention is explained further and being supplemented, and is not limited in any way to the present invention.
Refering to fig. 1, the preparation facilities of carbon nanotube sponge of the invention be equipped with reacting furnace 10, temperature controller 20, carrier gas tank 30,
Propylene tank 40, hydrogen gas tank 50 and flowmeter 60.Wherein, the reacting furnace 10 in the present invention is tube furnace, and catalyst is loaded on tube furnace
It is interior.Temperature controller 20 is equipped on reacting furnace 10, the probe of the temperature controller 20 is contacted with the inner wall of reacting furnace 10, for monitoring and controlling
Temperature in reacting furnace 10 processed.Four-way union, carrier gas tank 30, propylene tank 40 and hydrogen are connected in the air inlet of reacting furnace 10
Tank 50 is connect by four-way union with the air inlet of reacting furnace 10 respectively, wherein carrier gas tank 30 is provided with nitrogen or indifferent gas
Body, the inert gas are argon gas；It is provided with propylene in propylene tank 40, is provided with hydrogen in hydrogen gas tank 50.In reacting furnace 10 and carry
Be respectively equipped with flowmeter 60 between gas tank 30, propylene tank 40 and hydrogen gas tank 50, the flowmeter 60 be respectively used to control carrier gas tank 30,
The flow that propylene tank 40 and hydrogen gas tank 50 export.
Embodiment 1
2 kilograms of citric acids are dissolved in 8 kilograms of water and form citric acid solution, then nickel oxide is placed in citric acid solution
It impregnates 5 hours, after 500 DEG C 0.8 hour dry, obtains nickel oxide C catalyst, be then catalyzed 10 milligrams of nickel oxide carbon
Agent is placed in tube furnace 10, opens nitrogen tank valve, is made full of nitrogen in reacting furnace 10, under the protection of nitrogen, starts temperature control
Device 20 simultaneously controls reacting furnace 10 temperature is risen to 700 DEG C, then opens valve and the adjusting of propylene tank 40 and hydrogen gas tank 50 respectively
Propylene tank 40 and the flowmeter of hydrogen gas tank 50 60 make the flow-rate ratio 0.2:1 of hydrogen and propylene close propylene after reaction 1 hour
The valve of tank 40, hydrogen gas tank 50 and nitrogen gas tank, and temperature controller 20 is closed, make 10 cooled to room temperature of reacting furnace, obtains 1.5 grams
Product.By product macrostructure manufactured in the present embodiment as shown in Fig. 2, it is spongelike structure, the form of product such as Fig. 3 institute
Show, detected through scanning electron microscope, which is carbon nano tube structure, this illustrates that the product is carbon nanotube sponge.
Embodiment 2
1 kilogram of citric acid is dissolved in 9 kilograms of water and forms citric acid solution, then nickel oxide is placed in citric acid solution
It impregnates 3 hours, after 200 DEG C 1 hour dry, nickel oxide C catalyst is obtained, then by 15 milligrams of nickel oxide C catalyst
It is placed in tube furnace 10, opens nitrogen tank valve, make full of nitrogen in reacting furnace 10, under the protection of nitrogen, start temperature controller
It 20 and controls reacting furnace 10 temperature is risen to 500 DEG C, then open the valve of propylene tank 40 and hydrogen gas tank 50 respectively and adjust third
Alkene tank 40 and the flowmeter of hydrogen gas tank 50 60 make the flow-rate ratio 0.5:1 of hydrogen and propylene close propylene after reaction 0.5 hour
The valve of tank 40, hydrogen gas tank 50 and nitrogen gas tank, and temperature controller 20 is closed, make 10 cooled to room temperature of reacting furnace, is detected, obtained
To 2 grams of carbon nanotube sponges.
Embodiment 3
5 kilograms of citric acids are dissolved in 5 kilograms of water and form citric acid solution, then nickel oxide is placed in citric acid solution
It impregnates 10 hours, after 900 DEG C 0.2 hour dry, obtains nickel oxide C catalyst, be then catalyzed 5 milligrams of nickel oxide carbon
Agent is placed in tube furnace 10, opens argon gas tank valve, is made full of argon gas in reacting furnace 10, under the protection of argon gas, starts temperature control
Device 20 simultaneously controls reacting furnace 10 temperature is risen to 900 DEG C, then opens valve and the adjusting of propylene tank 40 and hydrogen gas tank 50 respectively
Propylene tank 40 and the flowmeter of hydrogen gas tank 50 60 make the flow-rate ratio 0.05:1 of hydrogen and propylene close third after reaction 2 hours
The valve of alkene tank 40, hydrogen gas tank 50 and argon tanks, and temperature controller 20 is closed, make 10 cooled to room temperature of reacting furnace, through detecting,
Obtain 0.7 gram of carbon nanotube sponge.
Embodiment 4
3 kilograms of citric acids are dissolved in 7 kilograms of water and form citric acid solution, then nickel oxide is placed in citric acid solution
It impregnates 1 hour, after 400 DEG C 0.5 hour dry, obtains nickel oxide C catalyst, be then catalyzed 12 milligrams of nickel oxide carbon
Agent is placed in tube furnace 10, opens nitrogen tank valve, is made full of nitrogen in reacting furnace 10, under the protection of nitrogen, starts temperature control
Device 20 simultaneously controls reacting furnace 10 temperature is risen to 600 DEG C, then opens valve and the adjusting of propylene tank 40 and hydrogen gas tank 50 respectively
Propylene tank 40 and the flowmeter of hydrogen gas tank 50 60 make the flow-rate ratio 0.1:1 of hydrogen and propylene close third after reaction 0.8 hour
The valve of alkene tank 40, hydrogen gas tank 50 and nitrogen gas tank, and temperature controller 20 is closed, make 10 cooled to room temperature of reacting furnace, through detecting,
Obtain 1.2 grams of carbon nanotube sponges.
Embodiment 5
4 kilograms of citric acids are dissolved in 6 kilograms of water and form citric acid solution, then nickel oxide is placed in citric acid solution
It impregnates 8 hours, after 700 DEG C 0.4 hour dry, nickel oxide C catalyst is obtained, then by 8 milligrams of nickel oxide C catalyst
It is placed in tube furnace 10, opens nitrogen tank valve, make full of nitrogen in reacting furnace 10, under the protection of nitrogen, start temperature controller
It 20 and controls reacting furnace 10 temperature is risen to 800 DEG C, then open the valve of propylene tank 40 and hydrogen gas tank 50 respectively and adjust third
Alkene tank 40 and the flowmeter of hydrogen gas tank 50 60 make the flow-rate ratio 0.3:1 of hydrogen and propylene close propylene after reaction 1.5 hours
The valve of tank 40, hydrogen gas tank 50 and carrier gas tank 30, and temperature controller 20 is closed, make 10 cooled to room temperature of reacting furnace, through detecting,
Obtain 1 gram of carbon nanotube sponge.
Take this, for the present invention by the way that using nitrogen or inert gas as carrier gas, propylene is carbon source, hydrogen is growth promoter, oxygen
Changing nickel carbon is that catalyst is obtained with carbon nanotube sponge existing for spongy state.The dispersibility of carbon nanotube sponge of the invention is excellent
It is not easy to reunite in conventional carbon nanotube, and the weight of carbon nanotube obtained and using catalyst weight ratio be 100~
150, yield is high, suitable for mass production.Also there is the present invention preparation process and device to be simple and convenient to operate, reaction condition is mild
The features such as.
Although being disclosed by above embodiments to the present invention, scope of protection of the present invention is not limited thereto,
Under conditions of without departing from present inventive concept, deformation, the replacement etc. done to above each ingredient will fall into right of the invention
In claimed range.
Claims (4)
1. a kind of preparation method of carbon nanotube sponge, which is characterized in that this method comprises the following steps:
A, nickel oxide is placed in the citric acid solution that weight percentage is 10~50% and is impregnated 1~10 hour, through 200~
900 DEG C after drying 0.2~1 hour, obtain nickel oxide C catalyst；
B, nickel oxide C catalyst made from step a is placed in reacting furnace (10), then from carrier gas tank (30) to reacting furnace (10)
It is inside passed through nitrogen or inert gas, and passes through temperature controller (20) for the temperature in reacting furnace (10) under nitrogen or inert gas shielding
Degree rises to 500~900 DEG C, then makes to be passed through with the flowmeter (60) of propylene tank (40) by adjusting hydrogen gas tank (50) respectively and react
The flow-rate ratio of hydrogen and propylene in furnace (10) is 0.05~0.5:1, after reaction 0.5~2 hour, cooled to room temperature, i.e.,
Carbon nanotube sponge is obtained, the nitrogen or inert gas are carrier gas, and the hydrogen is growth promoter, and the propylene is carbon
Source.
2. the preparation method of carbon nanotube sponge as described in claim 1, which is characterized in that the inert gas is argon gas.
3. the preparation method of carbon nanotube sponge as described in claim 1, which is characterized in that in step b, obtained carbon is received
The weight of mitron sponge and the weight ratio of reacting furnace (10) internal oxidition nickel C catalyst are 100~150.
4. a kind of device for realizing carbon nanotube sponge preparation method described in claim 1, which is characterized in that the device is equipped with
Reacting furnace (10) and temperature controller (20) for controlling reacting furnace (10) interior temperature, the probe and reacting furnace of the temperature controller (20)
(10) inner wall contact, the reacting furnace (10) is tube furnace, and the air inlet of the reacting furnace (10) is connected separately with carrier gas tank
(30), the air inlet of propylene tank (40) and hydrogen gas tank (50), the reacting furnace (10) is connected with four-way union, the carrier gas tank
(30), propylene tank (40) and hydrogen gas tank (50) are connect by four-way union with the air inlet of reacting furnace (10) respectively, described
Control flow is respectively provided between carrier gas tank (30), propylene tank (40) and hydrogen gas tank (50) and reacting furnace (10) air inlet
Flowmeter (60).
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| CN108251063B (en) * | 2016-12-28 | 2021-05-11 | 有研工程技术研究院有限公司 | High-performance composite phase-change material and preparation method thereof |
| CN107814379A (en) * | 2017-11-22 | 2018-03-20 | 哈尔滨工业大学 | A kind of method that low defect graphene ribbon sponge is prepared using CNT sponge |
| CN107758647A (en) * | 2017-11-22 | 2018-03-06 | 哈尔滨工业大学 | A kind of preparation method of low defect graphene ribbon sponge composite |
| CN107804838A (en) * | 2017-11-22 | 2018-03-16 | 哈尔滨工业大学 | A kind of preparation method of low defect graphene ribbon sponge ultracapacitor |
| CN107986261B (en) * | 2018-01-09 | 2021-01-05 | 郑州大学 | Device and method for preparing oversized carbon nanotube three-dimensional porous block |
| CN116535239A (en) * | 2023-05-10 | 2023-08-04 | 广东比沃新能源有限公司 | Preparation method of carbon-loaded nano honeycomb ceramic and reactor equipment for carbon loading |
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| CN103449405A (en) * | 2013-08-29 | 2013-12-18 | 中国科学院金属研究所 | Method for selectively growing metal-enriched single-wall carbon nanotube by using floating catalyst method |
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| CN103922310B (en) * | 2014-04-09 | 2016-01-13 | 中国科学院金属研究所 | The method of low-temperature gaseous phase magnanimity growing high-quality, straight carbon nanotubes and device |
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