Device and process method for continuously producing carbon nanotubes

A technology of carbon nanotubes and process methods, applied in the field of nanomaterials, can solve problems such as the inability to guarantee continuous production of carbon nanotubes, difficulty in controlling the fluidization state and stability of mass and heat transfer, and improve the flexibility of operation High performance, improved utilization, and compact structure

Active Publication Date: 2013-08-28
GUANGZHOU BAIYUN CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the existing technologies only use a separate fluidized bed for reaction to prepare carbon nanotubes, and have not really realized continuous production, and cannot adjust the process conditions in a wide range, and it is difficult to control the fluidization state and mass transfer. Thermal stability, so continuous production of high-quality carbon nanotubes cannot be guaranteed

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  • Device and process method for continuously producing carbon nanotubes

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Experimental program
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Embodiment 1

[0031] The process method for continuous production of carbon nanotubes in this embodiment, wherein the preparation process of the catalyst is as follows: dissolve cobalt nitrate and nickel nitrate in water according to the molar ratio of 0.6:1, after stirring evenly, add oxidizing agent 5 times the mass of the metal salt The aluminum gel is mixed evenly, dried at 120°C for 2 hours, put into a muffle furnace and calcined at 600°C for 3 hours, ground, and sieved with 200 meshes before use.

[0032] based on figure 1 As shown in the production device, the process steps of the continuous production of carbon nanotubes in this embodiment are as follows:

[0033] a. Addition of catalyst

[0034] Put the catalyst prepared above into the feeder 1, vacuum up to 600mmHg and feed nitrogen, and check the oxygen concentration. If the oxygen concentration is less than 100PPM, the system is safe.

[0035] b. Reduction catalyst

[0036] Add the catalyst into the fluidized bed of the reduc...

Embodiment 2

[0043] The process method of continuous production of carbon nanotubes in this embodiment differs from Embodiment 1 in that:

[0044] (1) In the preparation process of the catalyst, nickel nitrate is used as the metal salt; the carrier is magnesium oxide, and its dosage is twice the mass of the metal salt; the calcination temperature is 500°C.

[0045] (2) In step b, N 2 :H 2 The volume ratio=0.4:1, and the reduction time is 30min.

[0046] (3) In step c, the reaction temperature is 900°C, the carbon source gas is methane, N 2 :H 2 :CH 4 The volume ratio=0.3:0.5:1, the space velocity of the reaction process is 10000 hours ～1 , the gas superficial flow velocity is 0.5m / s, and the reaction residence time is 60min.

[0047] The parameters and properties of the obtained carbon nanotube product are as follows: purity>88%, outer diameter 15-30nm, length 10-30μm, specific surface area>120m 2 / g, black, bulk density 0.14g / cm 3 .

Embodiment 3

[0049] The process method of continuous production of carbon nanotubes in this embodiment differs from Embodiment 1 in that:

[0050] (1) In the preparation process of the catalyst, cobalt nitrate and iron nitrate are used, cobalt nitrate: iron nitrate molar ratio=1:4; the consumption of carrier alumina gel is 3 times of the metal salt quality; the calcination temperature is 500°C.

[0051] (2) In step b, the reaction temperature is 450° C., and the reduction time is 180 min.

[0052] (3) In step c, the reaction temperature is 700°C, the carbon source gas is propane, N 2 :H 2 : C 3 h 6 The volume ratio=0.5:1:1, the space velocity of the reaction process is 5000 hours ～1 , The reaction residence time is 70min.

[0053] The parameters and properties of the obtained carbon nanotube products are as follows: purity>92%, outer diameter 10-35nm, length 15-30μm, specific surface area>130m 2 / g, black, bulk density 0.14g / cm 3 .

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Abstract

The invention discloses a device for continuously producing carbon nanotubes, which consists of a feeder, a reduction reactor, a synthesis reactor and a product collector which are connected in series in turn, wherein the reduction reactor is a fluidized bed reactor; and the synthesis reactor is a spouted bed reactor. The invention also discloses a process method for continuously producing carbonnanotubes based on the device. The catalyst reduction and deposition preparation of the carbon nanotubes are respectively realized by the fluidized bed and the spouted bed, so that the process conditions can be regulated in a wider range, the fluidized state of agglomerated nanoparticles in the beds is ensured, and the high-quality carbon nanotubes are continuously produced.

Description

technical field [0001] The invention relates to the technical field of nanometer materials, in particular to a production device and a process method of carbon nanotubes. Background technique [0002] Carbon nanotubes have a typical layered hollow structure, and there is a certain angle between the layers that constitute carbon nanotubes. The tube body of carbon nanotubes is a quasi-circular tube structure, and most of them are composed of pentagonal cross-sections. The tube body of carbon nanotubes is a coaxial circular tube consisting of several to dozens of layers of hexagonal carbon ring microstructure units, with a fixed distance between layers, about 0.34nm, and a diameter of generally 2- 20nm; the end cap part is a polygonal structure composed of pentagonal carbon rings, or a polygonal cone-shaped multi-walled structure, which is a one-dimensional quantum material with a special structure. Due to their unique structure, the study of carbon nanotubes has great theoret...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/02B82Y40/00
Inventor 张利利邱浩孟刘光华龙飞陈建军缪明松欧阳喜仁
Owner GUANGZHOU BAIYUN CHEM IND
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