Preparation and purification method of coal-based carbon nanotubes

A purification method and technology of carbon nanotubes, applied in the direction of carbon nanotubes, chemical instruments and methods, nano-carbon, etc., can solve the problems of high environmental risk, uneconomical, harsh conditions, etc., to achieve perfect technology and purification process, reduce coal Base template, effect of improving purity

Active Publication Date: 2019-12-13
TAIYUAN UNIV OF TECH
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  • Description
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Problems solved by technology

However, the use of halogen-containing compounds is problematic due to the inconvenience of halogen gas disposal, environmental risks and high input costs
[0006] Although there are currently some reported methods that can also obtain high-purity single-walled carbon nanotubes, the raw materials used are often samples with relatively low impurity content, which is not economical. In addition, the method of ultra-high temperature calcination under high vacuum conditions is used The conditions for obtaining high-purity single-walled nanotubes are very harsh, and it is difficult to achieve and popularize; moreover, most methods are not suitable for the purification of a large number of samples (single processing volume > 200mg), and with the continuous application of carbon nanotubes Expansion, the demand for high-purity tubes is growing rapidly, so it is urgent to establish a purification process with mild conditions suitable for industrial mass production

Method used

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  • Preparation and purification method of coal-based carbon nanotubes
  • Preparation and purification method of coal-based carbon nanotubes
  • Preparation and purification method of coal-based carbon nanotubes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: step 1, a bituminous coal is crushed and screened to a particle size range of 0.01-1 mm, and 5 parts of mixed potassium iodide and potassium chloride are added in 100 parts of coal after crushing and screening Catalyst, the mass fraction ratio of potassium iodide and potassium chloride catalyst is 1:0.01, after the catalyst and coal are fully mixed evenly, the mixture is evenly spread in the reactor;

[0029] Step 2, feed the generating gas A of equimolar methane and carbon monoxide in the reactor of step 1, the space velocity of generating gas A is 10000h -1 , when the microwave heating power is 1-30KW and the microwave wavelength is 121.704mm, the coal material is heated intermittently to 800-1050°C with a total heating cycle of 0.5 h, and the interval between two heatings is 10 min. For 5 minutes, a small amount of coal-based carbon nanotubes are obtained on the coal surface;

[0030] Step 3: When the temperature of the coal-based carbon nanotubes prod...

Embodiment 2

[0034] Embodiment 2: Step 1, a bituminous coal is crushed and screened to a particle size range of 0.5-1 mm, and 10 parts by mass of mixed potassium chloride and potassium iodide are added to 100 parts of coal after crushing and screened Catalyst, the mass fraction ratio of potassium chloride and potassium iodide catalyst is 1:0.5, after the catalyst and coal are fully mixed evenly, the mixture is evenly spread in the reactor;

[0035]Step 2, feed the generating gas A of equimolar methane and carbon monoxide in the reactor of step 1, the space velocity of generating gas A is 10000h -1 , when the microwave heating power is 1-30KW and the microwave wavelength is 121.704mm, the coal is heated intermittently to 1050°C with a total heating cycle of 6 hours, the interval between two heatings is 30 minutes, and the intermittent single heating time is 10 minutes , a small amount of coal-based carbon nanotubes were obtained on the coal surface;

[0036] Step 3: When the temperature of...

Embodiment 3

[0040] Embodiment 3: step 1, a bituminous coal is crushed and screened to a particle size range of 0.01-0.5 mm, and 7.5 parts by mass of mixed potassium chloride and potassium iodide are added to 100 parts of coal after crushing and screened Catalyst, the mass fraction ratio of potassium chloride and potassium iodide catalyst is 1:0.25, after the catalyst and coal are fully mixed evenly, the mixture is evenly spread in the reactor;

[0041] Step 2, feed the generating gas A of equimolar methane and carbon monoxide into the reactor of step 1, and the space velocity of generating gas A is 5000 h -1 , when the microwave heating power is 1-30KW and the microwave wavelength is 121.704mm, the coal is heated intermittently to 1050°C with a total heating cycle of 0.5 h, the interval between two heatings is 10 minutes, and the intermittent single heating time is 10 minutes , a small amount of coal-based carbon nanotubes were obtained on the coal surface;

[0042] Step 3: When the temp...

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Abstract

The invention belongs to the technical field of preparation of carbon nanotubes, and provides a preparation and purification method of a coal-based carbon nanotubes. The method comprises the followingsteps: taking coal as a base, mixing potassium chloride and potassium iodide to obtain a catalyst, uniformly mixing the coal and the catalyst, paving an obtained mixture in a reactor, introducing generated gas A, and performing microwave heating to obtain coal-based carbon nanotubes on the surface of the coal; cooling the coal-based carbon nanotubes to 400 DEG C, introducing purified gas B for purification, and when the temperature of the coal-based carbon nanotubes is higher than 550 DEG C, stopping introducing the purified gas B and introducing nitrogen for cooling to 400 DEG C; repeating the process used for generating and purifying the coal-based carbon nanotubes, and repairing and prolonging the carbon nanotubes until the mass fraction of the coal is below 30%; and washing with an acid, washing with distilled water, and heating at 60-90 DEG C to remove water, thereby obtaining the pure coal-based carbon nanotubes. According to the preparation and purification method, a large number of coal-based carbon nanotubes are prepared on taking coal as the base, so that coal-based templates are reduced, and the purity of the coal-based carbon nanotubes is improved as much as possible.The technology and the purification process for preparing the carbon nanotubes from the coal base are perfected, so that the coal-based carbon nanotubes has more economic advantages and product advantages.

Description

technical field [0001] The invention belongs to the technical field of preparation of carbon nanotubes, in particular to a method for preparing and purifying coal-based carbon nanotubes, in particular to a method for reducing the quality of coal for synthesizing carbon nanotubes with coal as the base, and increasing carbon nanotubes Tube length and number of craft. Background technique [0002] Carbon nanotubes are widely used because of their unique one-dimensional structure in terms of mechanics, electricity, heat, and adsorption. However, the high price of carbon nanotubes severely limits their large-scale application market. The development of technologies for mass-preparing low-cost carbon nanotubes has become one of the most challenging directions in the field of carbon nanomaterials. [0003] Coal-based carbon nanotubes refer to carbon nanotubes containing coal-based materials produced on the basis of coal. Both ZL201810309097.2 and ZL 201810590741.8 are processes fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/162C01B32/17
CPCC01B32/162C01B32/17C01B2202/34C01B2202/30
Inventor 王影吕学枚张天开刘俊罗云焕李国强赵钰琼朱沛宇
Owner TAIYUAN UNIV OF TECH
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