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Nano-carbon fiber preparation method and equipment

A technology of nano-carbon fiber and carbon source gas, which is applied in the direction of nano-carbon, nanotechnology, chemical instruments and methods, etc., can solve the problems of uneconomical, high yield and output, etc., to promote industrialization and increase yield Effect

Active Publication Date: 2013-09-04
BTR NEW MATERIAL GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In the preparation of catalysts in the prior art and the preparation of carbon fibers with the obtained catalysts, no matter in the horizontal or vertical deposition method, due to the limitation of the reaction chamber, the yield and output cannot be very high. In order to realize industrialization, the only way to make the reaction chamber Very large, so that the carbon source and the catalyst fully react and deposit, but it is uneconomical

Method used

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  • Nano-carbon fiber preparation method and equipment
  • Nano-carbon fiber preparation method and equipment
  • Nano-carbon fiber preparation method and equipment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1, co-precipitation method prepares catalyst, prepares nanometer carbon fiber,

[0045] Dissolve 4.36kg Co(NO 3 ) 2 ·6H 2 O, dissolve 1.84kgMn(NO 3 ) 2 4H 2 O, two solutions were prepared. The two solutions were mixed at room temperature and stirred uniformly to obtain a mixed solution. Contain 4.10kg Mg(NO in the mixed solution and 3.5L water solvent 3 ) 2 ·6H 2 The solutions of O were mixed and stirred uniformly to obtain solution A. 7.30kg(NH 4 ) 2 CO 3 Dissolve in 22.5L deionized water, stir evenly to obtain solution B. Under stirring at 2500 rpm, the solutions A and B were added dropwise to 20 L of deionized water, and the pH of the solution was kept at 7 during the dropwise addition. After the dropwise addition was completed, stir for 5 minutes and then filter. The obtained solid was dried in the air at 120° C., then calcined in the air at 600° C. for 4 hours, then pulverized, and passed through a 200-mesh sieve to obtain a catalyst for ca...

Embodiment 2

[0046] Embodiment 2, co-precipitation method prepares catalyst, prepares nanometer carbon fiber,

[0047] 4.36kg Co(NO 3 ) 2 ·6H 2 O, 1.84kg Mn(NO 3 ) 2 4H 2 O and 0.25kg (NH 4 ) 6 Mo 7 o 24 4H 2 O was dissolved in 20L of deionized water, and 4.10kg of Mg(NO 3 ) 2 ·6H 2 O, stir until the solution is transparent and uniform to obtain solution A. 7.30kg(NH 4 ) 2 CO 3 Dissolve in 22.5L deionized water, stir until the solution is uniform, and obtain solution B. Under stirring at 2500 rpm, the solutions A and B were added dropwise to 20 L of deionized water, and the pH of the solution was kept at 7 during the dropwise addition. After the dropwise addition was completed and stirred for 5 minutes, it was filtered, and the obtained solid was dried in the air at 120°C, then calcined in the air at 600°C for 4 hours, then pulverized, and passed through a 200-mesh sieve to obtain a catalyst for carbon fiber preparation. The above catalyst is introduced into the heating z...

Embodiment 3

[0048] Embodiment 3, liquid catalyst, prepare carbon nanofiber,

[0049] Dissolve 0.83kg of ferrocene and 0.155kg of thiophene in 14kg of benzene to prepare a liquid catalyst. The above-mentioned liquid catalyst is introduced into the heating zone with a temperature of 1100°C in the reaction chamber by peristaltic injection and spraying, and the flow rate is 15mL / s.M 3 , the carbon source gas in gas 1 is methane, the carrier gas is nitrogen-hydrogen mixed gas containing 20% ​​hydrogen, the volume ratio of carbon source gas and carrier gas is 2:1, and the flow rate is 10mL / s.M 3 , gas 2 is nitrogen, the flow rate is 10mL / s.M 3 , The reaction time is 20min. Put the carbon nanofibers generated by the above reaction in nitrogen, the flow rate is 10mL / s.M 3 , direct heat treatment at 2500°C for 24h, and naturally cool down to room temperature in the furnace to obtain carbon nanofibers. The electrical performance test results and yields are shown in Table 1.

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Abstract

The invention discloses a nano-carbon fiber preparation method and equipment, which aims to improve yield of carbon fibers. The preparation method includes heating the inside of a vertically arranged tubular reaction cavity, filling gas 1 and catalyst from the upper side of a furnace, feeding gas 2 from the lower side of the furnace, and obtaining nano-carbon fibers. The gas 1 is gas of a carbon source and carrier gas, and the gas 2 is nitrogen or hydrogen. The preparation equipment is the vertical tubular sealed reaction cavity, a first gas inlet pipe and a catalyst inlet pipe are arranged on the upper portion of the reaction cavity, a second gas inlet pipe is disposed on the lower portion of the reaction cavity, and a heating resistance wire is arranged on the periphery of the reaction cavity. Compared with the prior art, the preparation method adopts the vertically arranged tubular sealed reaction cavity, a mode that the gases are vertically guided into the cavity from different directions is adopted, the carbon source and the catalyst are sufficiently reacted and deposited under the action of fluid, yield of gas-phase deposited carbon fibers is improved under the condition that the reaction cavity is not large, and industrialization of nano-carbon fiber production is promoted.

Description

technical field [0001] The invention relates to a method and equipment for preparing carbon nanofibers, in particular to a method and equipment for preparing carbon nanofibers that can be used as conductive agents for lithium-ion batteries. Background technique [0002] The key to the preparation of carbon fibers by vapor deposition is the way of carbon source deposition, which has a very important relationship with the yield and diameter distribution of carbon fibers. Regarding the preparation of carbon fibers in the gas phase, various studies have been carried out since the second half of the 1980s, and various schemes involving catalysts have been proposed, including catalyst preparation methods such as sol-gel and co-precipitation. In terms of deposition methods, horizontal and vertical deposition methods are also proposed. [0003] For example, Patent Document 1: Japanese Patent Publication No. 2003-205239 discloses a metal containing fibril-forming catalyst properties...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/889C01B31/02B82Y40/00C01B32/15
Inventor 粱奇梅佳时浩吕雪孔东亮
Owner BTR NEW MATERIAL GRP CO LTD