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A carbon nanotube, purification device technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve problems such as reducing production costs, acid mist and waste acid are not recycled, etc. The effect of reducing production costs, avoiding excessive heating temperature, and reducing washing time
Inactive Publication Date: 2014-12-03
WUXI DONGHENGNEWENERGYTECHNOLOGYCO LTD
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[0004] The present invention aims at the problem that neither acid mist nor waste acid has been recycled in the above-mentioned existing purification process, and provides a purification device and method for carbon nanotubes with small diameters, which can effectively recycle and utilize the carbon nanotubes generated during the purification process. acid mist and waste acid, reducing production costs
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Embodiment 1
[0042] The iron catalyst is prepared by a sol-gel method, ethylene is used as a reaction gas, and the cracking temperature is 700°C. The metal content in the prepared small diameter carbon nanotube is about 4%, and the diameter of the carbon nanotube is less than 20nm. A catalyst that does not contain rare earth elements and has no heavy pollution to the environment is prepared by using the sol-gel method, and small-diameter carbon nanotubes with high yield and high conductivity are prepared by using the catalyst.
[0043] A hydrofluoric acid solution with a mass concentration of 5% was prepared to react with the carbon nanotubes, the weight ratio of the solution to the carbon nanotubes was 10:1, the reaction temperature was 80° C., and the reaction time was 20 hours.
[0044] The acid mist generated during the heating process of the reactor is cooled through the horizontal tube heat exchanger in the pure water pool, the cooling temperature is 10-20°C, and the acid liquid obtai...
Embodiment 2
[0050] The iron catalyst is prepared by a sol-gel method, ethylene is used as a reaction gas, the cracking temperature is 700 DEG C, the metal content in the prepared carbon nanotube is about 4%, and the diameter of the carbon nanotube is less than 20nm.
[0051] A hydrochloric acid solution with a mass concentration of 24% was prepared to react with the carbon nanotubes, the weight ratio of the solution to the carbon nanotubes was 10:1, the reaction temperature was 80° C., and the reaction time was 20 hours.
[0052] The acid mist generated during the heating process of the reactor is cooled through the horizontal tube heat exchanger in the purified water pool, the cooling temperature is 10-20°C, and the acid liquid obtained after cooling is introduced into the secondary acid storage tank.
[0053] The carbon nanotube solution after the reaction is press-filtered by a filter press, and the waste acid solution filtered out by the press-filter is purified by a diffusion dialyzer...
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Abstract
The invention relates to a small-tube-diameter carbon nano-tube purification device and a small-tube-diameter carbon nano-tube purification method. The small-tube-diameter carbon nano-tube purification device comprises a reaction kettle, a heat exchanger, a secondary acid storage tank, a diffusion dialysis device and a pressure filter. The small-tube-diameter carbon nano-tube purification method comprises the following steps: adding acid liquid and small-tube-diameter carbon nano-tube raw material powder into the reaction kettle to react, introducing a small-tube-diameter carbon nano-tube solution obtained after reaction into the pressure filter for pressure filtration, performing water-washing and drying on a small-tube-diameter carbon nano-tube in the pressure filter to obtain a small-tube-diameter carbon nano-tube finished product, introducing waste acid liquid filtered by virtue of pressure filtration into the diffusion dialysis device for purification, and introducing the purified acid liquid into the secondary acid storage tank; introducing acid mist generated in the reaction kettle into the heat exchanger for cooling, and introducing the cooled acid liquid into the secondary acid storage tank; performing concentration adjustment on the acid liquid in the secondary acid storage tank and then introducing the acid liquid into the reaction kettle. According to the small-tube-diameter carbon nano-tube purification device and method disclosed by the invention, the acid mist generated in a purification process is cooled and recycled, and the waste acid liquid generated in a production process is purified and recycled, so that the environment pollution caused by the acid mist and the waste acid liquid can be reduced, and the production cost can be reduced.
Description
technical field [0001] The invention relates to a purification process of small-diameter carbon nanotubes, in particular to a purification device and method for small-diameter carbon nanotubes. Background technique [0002] The preparation techniques of carbon nanotubes mainly include: arc discharge method, laser etching method, chemical vapor deposition method, solid phase pyrolysis method, flame synthesis method, glow discharge method and polymerization reaction synthesis method. Among them, chemical vapor deposition (CVD) is the most widely used method. This method is to let gaseous alkanes pass through a template attached with catalyst particles, and decompose gaseous hydrocarbons to form carbon nanotubes under the condition of 600-1200°C. An outstanding advantage of this method is that the residual reactants are gases, which can leave the reaction system to obtain carbon nanotubes with high purity, and the temperature does not need to be very high, which relatively save...
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