Single-stage continuous carbon nano tube preparation device and method

A technology of carbon nanotubes and catalysts, which is applied in the field of single-stage continuous preparation of carbon nanotubes, and can solve the problems of blocked reactors, easy agglomeration of carbon nanotubes, and low utilization of catalysts.

Active Publication Date: 2018-11-02
SHANDONG DAZHAN NANO MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The fixed fluidized bed process has simple equipment and flexible operation, and is only suitable for catalyst screening and the preparation of a small amount of carbon nanotubes; a fluidized fluidized bed can process a large amount of catalysts, and the yield of carbon nanotubes is also good, but the conversion rate of feed gas is low and the cost is high ; Floating fluidized beds are suitable for catalytic systems that are easy to gasify and decompose, and have high limitations; moving fluidized beds have problems with temperature gradients and moving speeds
In addition, for traditional fluidized beds, catalyst density and particle size have a great influence on reaction efficiency
If the density of the catalyst is low, the density of the prepared carbon nanotubes is small, and it is easy to be blown out of the reactor, and the residence time is short, resulting in low utilization of the catalyst
On the contrary, if the residence time in the reactor is increased, the carbon nanotubes will easily agglomerate, block the reactor, and easily cause fluidization difficulties in the production process, etc.

Method used

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  • Single-stage continuous carbon nano tube preparation device and method
  • Single-stage continuous carbon nano tube preparation device and method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0143] based on figure 1 In the shown reaction device, the carbon source is propylene, the catalyst is an iron-based catalyst, and the total iron content is 29.12%.

[0144] Nitrogen was introduced from the mixed gas inlet for 20 minutes before the reaction, N 2 The flow rate is 8.0m / s, and the temperature of the main reactor is raised to 650°C under the protection of nitrogen. The catalyst feeding port starts to feed continuously and stably 60g / h, and the mixed gas of propylene: nitrogen 1:2 is passed into the reactor from the mixed gas inlet, and the gas flow rate is 1.2m / s, forming a fluidized state; the main reactor is annular The air curtain at the variable diameter and the bottom is opened for pulse purge, the exhaust lock valve is open, and the continuous production is 3 hours, producing 9.25kg of carbon nanotubes. The SEM picture of carbon nanotubes is as follows image 3 shown.

[0145] The parameters and properties of the obtained carbon nanotube products are as f...

Embodiment 2

[0148] based on figure 1 In the preparation device shown, the carbon source is propane, the catalyst is a nickel-based catalyst, the total nickel content is 9.15%, and the iron content is 31%.

[0149] Nitrogen was passed through the mixed gas inlet for 30 minutes before the reaction, N 2 The flow rate is 8.0m / s, and the temperature of the main reactor is raised to 730°C under the protection of nitrogen. The catalyst feeding port starts to feed 30g / h continuously, and the mixed gas of propane: nitrogen 1:2.5 is passed into the reactor from the mixed gas inlet, and the gas flow rate is 0.9m / s, forming a fluidized state; the main reactor is annular The air curtain at the variable diameter and the bottom is opened for pulse purge, the exhaust lock valve is open, and the continuous production is 2 hours, the production of carbon nanotubes is 3.51kg. The SEM picture of carbon nanotubes is as follows Figure 4 shown.

[0150] The parameters and properties of the obtained carbon n...

Embodiment 3

[0153] based on figure 1 In the preparation device shown, the carbon source is ethylene, and red cobalt catalyst is used, and the total cobalt content is 36.39%.

[0154] Nitrogen was passed through the mixed gas inlet for 60 minutes before the reaction, N 2 The flow rate is 8.0m / s, and the temperature of the main reactor is raised to 690°C under the protection of nitrogen. The catalyst feeding port starts to feed continuously and stably 50g / h, and the mixed gas of ethylene: nitrogen of 1:3 is passed into the reactor from the mixed gas inlet, and the gas flow rate is 0.8m / s, forming a fluidized state; the main reactor is annular The air curtain at the variable diameter and the bottom is opened for pulse purge, the exhaust lock valve is open, and the continuous production is 3 hours, producing 4.57kg of carbon nanotubes. The SEM picture of carbon nanotubes is as follows Figure 5 shown.

[0155] The parameters and properties of the obtained carbon nanotube product are as fol...

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Abstract

The invention provides a single-stage continuous carbon nano tube preparation device and the device is based on a fluidized bed reactor. The fluidized bed reactor comprises an annular variable-diameter area, a raw material gas inlet, a catalyst feeding opening, a protection gas inlet and a pulse gas controller, wherein the position of the annular variable-diameter area is arranged from the 1/4 position of the bottom of the fluidized bed reactor to the top of the fluidized bed reactor, the pulse gas controller is arranged at the arc top of the annular variable-diameter area, the catalyst feeding opening is arranged at the top of the fluidized bed reactor, and the raw material gas inlet and the protection gas inlet are arranged at the bottom of the fluidized bed reactor. The device is further provided with a product outlet and a tail gas outlet. The device has the advantages of simple structure, low cost, easiness in operation, high raw material utilization rate, ability of effectively controlling the problem of carbon deposit on an inner wall of a main reactor, ability of preparing high-purity carbon nano tubes and suitability for industrialized large-scale production.

Description

technical field [0001] The invention relates to a device and method for single-stage continuous preparation of carbon nanotubes. The device for continuously preparing carbon nanotubes of the present invention adopts a single-stage fluidized bed, has a simple structure, is easy to operate, can continuously and stably produce carbon nanotubes under normal pressure or high pressure, and has the advantages of improving the utilization rate of catalysts and raw materials and increasing carbon The advantages of the purity of nanotube products can save costs and are suitable for large-scale industrial production. Background technique [0002] As a one-dimensional nanomaterial, carbon nanotubes have excellent physical and mechanical properties. They are mainly coaxial circular tubes with several to dozens of layers composed of carbon atoms arranged in a hexagonal shape. It has a very large aspect ratio, the diameter is usually between 1-100nm, and the length is several microns to h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/164
CPCC01P2004/03C01P2004/04C01P2004/13C01P2006/80C01P2004/64C01P2006/12C01P2004/51B01J8/12B01J8/18C01B32/05C01B32/164D01F9/00B01J2219/185B01J2219/1946B01J8/1809B01J8/40B01J8/005B01J8/1881B01J23/745B01J23/75B01J23/755B01J2208/00548C01B2202/06
Inventor 李岩耿磊吕振华李龙利鲍中村
Owner SHANDONG DAZHAN NANO MATERIALS
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