Process for preparing Fe-series catalyst used to synthesize nano carbon tubes

A catalyst and synthetic carbon technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of small scale, low efficiency, wall thickness, uneven pipe diameter, etc., and achieve small diameter , thin wall and low cost

Inactive Publication Date: 2002-10-30
TSINGHUA UNIV
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Problems solved by technology

The nanocatalysts reported so far are limited by particle size and dispersion, and most of them can only be used to prepare ordinary carbon nanotubes with a diameter greater than 10nm, and the wall thickness and diameter are uneven, often accompanied by impurities such as amorphous carbon. , the winding phenomenon is also very prominent (Y.D.Li, J.L.Chen, L.Chang, et.al. Feitknecht Compound Used as the Precursor of the Catalyst for the Catalytic Growth of Fibers from Methane, Studies in Surface Science and Catalysis, 1998, 118(1- 4): 321-329; V.Ivanov, A.Fonseca, J.B.Nagy, et.al.Catalytic Production and Purification of Nanotubules Having Fullerens-scale Diameters.Catalytic Production and Purification of Nanotubules, 1995, 132(8): 1727-1737 .); although there are reports of straight tubes or single-walled tubes, they are all made by physical methods, with relatively large diameter (>10 μm), small scale, and low efficiency (Xie Sishen, Pan Zhengwei, Ultra-long aligned carbon nanotube array Preparation, Physics, 1999, 28(1): 1-3; H.Zhang, k.Chen, Y.He, et.al.Formation and Raman Spectroscopy of SingleWall Carbon Nanotubes Synthesized by co 2 Continuous Laser Vaporization, Journal of Physics and Chemistry of Solids, 2001, 62(11): 2007-2010.)
The work of using highly dispersed ultrafine nanocatalysts to prepare large-scale uniform, thin-walled, and basically unentangled carbon nanotubes has not been reported yet

Method used

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  • Process for preparing Fe-series catalyst used to synthesize nano carbon tubes
  • Process for preparing Fe-series catalyst used to synthesize nano carbon tubes
  • Process for preparing Fe-series catalyst used to synthesize nano carbon tubes

Examples

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Embodiment 1

[0034] Prepare 5% (w / v) NiCl 2 Solution 100ml, 5% (w / v) NH 4 HCO 3 Solution 100ml, 1%(w / v(NaPO 3 ) 650ml. (NaPO 3 ) 6 The solution is added to NH 4 HCO 3 In solution, (NaPO 3 ) 6 The solution addition rate is 10ml / min. NiCl 2 After the solution is heated to 80℃, the temperature is kept constant, and then NH is gradually added under stirring. 4 HCO 3 With (NaPO 3 ) 6 The solution is added at a rate of 5ml / min. After the addition is complete, the temperature and stirring are continued for 2 hours, and then the reaction is stopped. The resulting suspension was placed in an autoclave at 150°C for hydrothermal modification for 2 hours, then cooled, filtered, washed with deionized water and ethanol 3 times, and dried at 105°C for 4 hours in an air atmosphere. The dried intermediate precipitate was placed in a muffle furnace and calcined at 800°C for 1 hour to obtain a nanocrystalline nickel catalyst with a particle size of 10nm and a specific surface area of ​​150m 2 / g, the main compos...

Embodiment 2

[0037] Prepare 20% (w / v) Fe(NO 3 ) 3 Solution 100ml, 20%(w / v)(NH 4 ) 2 CO 3 Solution 100ml, 5% (w / v) Na 2 SiO 3 50ml. Add CH at room temperature and stirring (800rpm) 3 CH 2 OH solution is added (NH 4 ) 2 CO 3 Solution, CH 3 CH 2 The OH solution addition rate is 10ml / min. Fe(NO 3 ) 3 The solution was heated to 25°C and then kept at a constant temperature, and then gradually added (NH 4 ) 2 CO 2 With CH 3 CH 2 The OH mixed solution, the solution adding rate is 20ml / min. After the addition is complete, the temperature and stirring are continued for 2 hours, and then the reaction is stopped. The resulting suspension was placed in an autoclave at 105°C for hydrothermal modification for 1 hour, then cooled, filtered, washed with deionized water and ethanol 3 times, and dried at 105°C for 4 hours in an air atmosphere. The dried intermediate precipitate was placed in a muffle furnace and calcined at 400°C for 2 hours to obtain a nanocrystalline iron catalyst with a particle size of 3nm a...

Embodiment 3

[0040] Prepare 10% (w / v) FeCl 3 Solution 100ml, 20% (w / v) Na 2 CO 3 100ml solution, 2%(w / v)CH 3 CH 2 OH 50 ml. Add C at room temperature and stirring (800rpm) 18 H 19 SO 3 Na solution add Na 2 CO 3 Solution, C 18 H 19 SO 3 The Na solution addition rate is 10ml / min. FeCl 3 The solution was heated to 40℃ and then kept at a constant temperature, and then gradually added (NH 4 ) 2 CO 3 With C 18 H 19 SO 3 For the mixed solution of Na, the adding rate of the solution is 5ml / min. After the addition is complete, the temperature and stirring are continued for 2 hours, and then the reaction is stopped. The resulting suspension was placed in an autoclave at 120°C for hydrothermal modification for 4 hours, then cooled, filtered, washed with deionized water and ethanol 3 times, and dried at 105°C for 4 hours in an air atmosphere. The dried intermediate precipitate was placed in a muffle furnace and calcined at 300°C for 5 hours to obtain a nanocrystalline iron catalyst with a particle size of...

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Abstract

A process for preparing Fe-series catalyst used to synthesize nano carbon tubes by gas-phase catalytic deposition method includes such steps as liquid-phase codeposition reaction of inorganic Fe saltand carbonate at 25-85 deg.C under existance of water-soluble disperser, hydrothermal modification of suspension at 105-150 deg.c, filtering and washing deposit, and calcining at 300-800 deg.C to obtain the high-dispersity catalyst. The nano carbon tubes prepared with said catalyst features thin wall, fine diameter (3-10 nm) and high uniformity.

Description

Technical field [0001] The invention relates to a method for preparing a catalyst, in particular to a method for preparing an iron-based catalyst for the synthesis of carbon nanotubes by a catalytic chemical vapor deposition method, and belongs to the technical field of inorganic chemical technology. Background technique [0002] Nano powder refers to a powder material with a particle size of 1-100 nm. The special structure of nanomaterials makes it have surface effects, volume effects, quantum size effects, and macro-quantum tunneling effects, etc., so it has a series of novel physical and chemical properties, and has great application value in many fields including the chemical industry. For example, there are a large number of interfaces in nanomaterials. These interfaces provide short-range diffusion pathways for atoms. Therefore, nanomaterials have high activity and diffusivity, and have significant effects on chemical reactions, creep, superplasticity and other properties. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/74B01J37/03C01B31/02
Inventor 向兰邓祥义魏飞罗国华李志飞
Owner TSINGHUA UNIV
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