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Process for preparing carbon nano fiber knitting macro-particles containing high active nickel catalyst

A carbon nanofiber, nickel catalyst technology, applied in the field of catalysis, can solve the problems of macroscopic carbon particles that do not meet industrial requirements, particle strength damage, low catalyst activity, etc.

Inactive Publication Date: 2004-04-28
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] [Catal Rev-Sci Eng 42 (2000) 481] from the Netherlands [Catal Rev-Sci Eng 42 (2000) 481], due to the low activity of the catalyst used, it is necessary to increase the density of the active components of the catalyst particles and limit the carbon growth space. The overall crushing strength of carbon nanofiber aggregate particles of about 100 microns is equivalent to that of general industrial catalysts, but the original catalyst in the aggregate accounts for about 10wt%, which must be removed before use, which will cause great damage to the particle strength
Russia's Kuvshinov etc. [Carbon 37 (1999) 1239] also prepared aggregated particles of about 1mm size, but only reported their abrasion strength, so far, the important indicator of whether it can be industrially applied-single particle mechanical strength There is no public report yet, that is to say, macroscopic carbon particles that meet industrial requirements have not been obtained

Method used

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  • Process for preparing carbon nano fiber knitting macro-particles containing high active nickel catalyst
  • Process for preparing carbon nano fiber knitting macro-particles containing high active nickel catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take Ni 2+ 、Cu 2+ 、Al 3+ Mix about 300ml of nitrate solution, the molar ratio is: Ni: Cu: Al = 75: 2: 23, the total concentration of metal ions is 1M; the temperature is raised to 55°C in a constant temperature water bath, and the concentration of 1M Na 2 CO 3 The solution is about 220ml; after fully reacting, filter the above reaction solution; wash the filtered precipitate with 65°C deionized water for 5 times; dry the washed precipitate at 120°C for 5 hours; grind the dried precipitate and sieve Obtain particles with a size of 10 mesh; calcinate the above particles at 450°C for 10h to obtain Ni-Cu / Al with a molar ratio of Ni:Cu:Al=75:2:23 2 o 3 Catalyst: Take 100mg of the above-mentioned catalyst particles and place them in a horizontal tubular reactor with an inner diameter of 38mm. The catalyst is first reduced with hydrogen at 750°C for 4h, and then cooled down to 500°C under the protection of nitrogen, and the volume ratio of feeding is 2:1 The mixed gas of ...

Embodiment 2

[0023] Take Ni 2+ 、Cu 2+ 、Al 3+ Mix about 300ml of nitrate solution, the molar ratio is: Ni:Cu:Al=75:15:10, the total concentration of metal ions is 1M; the temperature is raised to 60°C in a constant temperature water bath, and the concentration of 1M Na 2 CO 3 The solution is about 170ml; after fully reacting, filter the above reaction solution; wash the filtered precipitate with 60°C deionized water for 3 times; dry the washed precipitate at 120°C for 5 hours; grind the dried precipitate and sieve Obtain particles with a size of 20-40 mesh; calcinate the above particles at 450°C for 10h to obtain Ni-Cu / Al with a molar ratio of Ni:Cu:Al=75:15:10 2 o 3 Catalyst: Take 100mg of the above-mentioned catalyst particles and place them in a horizontal tubular reactor with an inner diameter of 38mm. The catalyst is first reduced with hydrogen at 700°C for 2h, then cooled down to 600°C under the protection of nitrogen, and then pure methane is introduced to react. It was 68ml / min...

Embodiment 3

[0025] Take Ni 2+ 、Cu 2+ 、Al 3+ Mix about 300ml of nitrate solution, the molar ratio is: Ni:Cu:Al=75:30:45, the total concentration of metal ions is 0.5M; the temperature is raised to 65°C in a constant temperature water bath, and the concentration of 1M Na 2 CO 3 The solution is about 260ml; after fully reacting, filter the above reaction solution; wash the filtered precipitate with 55°C deionized water for 7 times; dry the washed precipitate at 120°C for 5 hours; grind the dried precipitate and sieve Obtain particles with a size of 10-20 mesh; calcinate the above particles at 450°C for 10h to obtain Ni-Cu / Al with a molar ratio of Ni:Cu:Al=75:30:45 2 o 3 Catalyst: Take 250 mg of the above-mentioned catalyst particles and place them in a horizontal tubular reactor with an inner diameter of 38 mm. The catalyst is first reduced with hydrogen at 750 ° C for 4 hours, then cooled to 700 ° C under the protection of nitrogen, and then pure methane gas is introduced to react. The...

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Abstract

The present invention discloses a preparation process of woven nano carbon fiber macro particle containing high activity nickel catalyst for industrial application. The preparation process includes the following steps: preparing nitrate solution with Ni, Cu and Al ions of 0.4-1 M concentration; heating the solution to 55-65 deg.c and dropping 1 M concentration Na2CO3 solution; filtering and washing the precipitate with deionized water in 55-65 deg.c for 2-8 times; drying the precipitate at 120 deg.c for 5 hr; crushing the precipitate, incinerating at 350-550 deg.c and reduction in reactor; introducing methane for reaction at 450-750 deg.c. The particle thus obtained has high mechanical strength, high conducting capacity and excellent antioxidant ability.

Description

technical field [0001] The invention relates to the field of catalysis, and more specifically relates to a preparation method of carbon nanofiber weaving macroscopic porous particles. Background technique [0002] In the field of catalysis, traditional activated carbon is widely used as the carrier of noble metal catalysts (Pt, Pd and Rh, etc.) in the production of dyes, pigments and pharmaceutical intermediates. The loaded precious metal is lost with the material, resulting in great waste. [0003] Carbon nanofibers and nanotubes are new carbon materials with good mechanical strength, high degree of graphitization, excellent electrical conductivity and oxidation resistance, and overcome the shortcomings of activated carbon as a carrier. High activity or high selectivity. In addition, it has a good adsorption effect on some gases, such as NO, CO and organic substances, such as alcohols, hydrocarbons and phenols. These carbon materials are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J37/03B01J37/16
Inventor 陈久岭李永丹
Owner TIANJIN UNIV
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