Preparation method of carbon nanotube metal symbiotic material

A technology of carbon nanotubes and metals, which is applied in the field of preparation of carbon nanotube metal symbiotic materials, can solve problems such as difficult control, uneven metal particle size, difficult control of metal loading, etc., to achieve uniformity and good catalytic performance Effect

Pending Publication Date: 2019-06-25
SHAANXI YANCHANG PETROLEUM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the currently published carbon nanotube-supported metal-based catalysts, metals or metal oxides are mainly distributed on the surface of carbon nanotubes, and there are problems such as the loading amount of metals is difficult to control and the size of metal particles is uneven and difficult to control.

Method used

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  • Preparation method of carbon nanotube metal symbiotic material
  • Preparation method of carbon nanotube metal symbiotic material

Examples

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Effect test

Embodiment 1

[0025] A preparation method of carbon nanotube cobalt symbiotic material includes the following steps:

[0026] (1) Add 1.40 g Co(NO 3 ) 2 ·6H 2 O and 1.00g Al passed through a 150 mesh sieve 2 O 3 The carrier was mixed, added with deionized water, immersed in ultrasonic treatment for 4h, filtered, and the obtained filter residue was washed 3 times with deionized water, then dried, and calcined at 500°C for 4h to obtain a cobalt-based catalyst; in the cobalt-based catalyst, The content of cobalt is based on the mass of cobalt trioxide, accounting for 28.57% of the mass of the cobalt-based catalyst;

[0027] (2) Put the cobalt-based catalyst in the reactor, and then pass in the inert gas nitrogen to replace the air and then pass in the reducing gas hydrogen for 50 minutes. The hydrogen space velocity is 10000mL / g / h, heated to 600℃, and the reduction is stopped. Then pass the carbon source methane, the space velocity is controlled at 20000 mL / g / h, the reaction is 2h, the inert gas ni...

Embodiment 2

[0029] A preparation method of carbon nanotube iron symbiotic material, including the following steps:

[0030] (1) Add 3.54 g Fe(NO 3 ) 3 ·9H 2 O and 1.00g SiO passed through 200 mesh sieve 2 The carrier was mixed, added with deionized water, immersed in ultrasonic treatment for 3h, filtered, and the obtained filter residue was washed with deionized water 3 times, then dried, and calcined at 450°C for 5h to obtain an iron-based catalyst; in the iron-based catalyst, The iron content is based on the mass of ferric oxide, accounting for 41.18% of the mass of the iron-based catalyst;

[0031] (2) Put the iron-based catalyst in the reactor, and then pass in the inert gas argon to replace the air, and then pass in the reducing gas methane for 10 minutes. The reducing gas methane has a space velocity of 30,000 mL / g / h, and then heat to 700°C , Continue to pass in methane, control the space velocity at 15000 mL / g / h, react for 4 hours, pass in the inert gas argon again, and drop to room tem...

Embodiment 3

[0033] A preparation method of carbon nanotube nickel symbiotic material, including the following steps:

[0034] (1) Add 8.95g Ni(NO 3 ) 2 ·6H 2 O and 1.50g of ZSM-5 carrier passed through a 100-mesh sieve were mixed, added with deionized water, immersed in ultrasonic treatment for 2h, filtered, and the obtained filter residue was washed with deionized water for 3 times, then dried and calcined at 480℃ for 4h. Obtain a nickel-based catalyst; in the nickel-based catalyst, the content of nickel is based on the mass of nickel oxide, accounting for 60.52% of the mass of the nickel-based catalyst;

[0035] (2) Put the nickel-based catalyst in the reactor, and pass the inert gas helium to replace the air and then pass the reducing gas methane for 20 minutes, the reducing gas methane space velocity is 15000mL / g / h, and then heating to 750℃ , Stop feeding the reducing gas methane, and then feed the carbon source ethane, the space velocity is controlled at 15000 mL / g / h, the reaction is 1.5h...

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Abstract

The invention discloses a preparation method of a carbon nanotube metal symbiotic material. The preparation method comprises the following steps: (1) after a metal source and a carrier are mixed, deionized water is added, impregnation is carried out for 2-4 h under ultrasonic treatment, filtering is carried out, obtained filter residue is washed for three times through deionized water, then dryingand calcination are carried out, a metal-based catalyst is obtained, or the metal source is directly calcinated, and the metal-based catalyst is obtained; and (2) the metal-based catalyst is placed into a reactor, inert gas is introduced firstly for replacement, then reducing gas is introduced, the reducing gas stops being introduced till heating is conducted to 500-800 DEG C, then a carbon source is introduced, reacting is carried out for 1-5 h, the inert gas is introduced again, the temperature is decreased to be the room temperature under the atmosphere of the inert gas, and then the carbon nanotube metal symbiotic material is obtained. According to the preparation method, a carbon nanotube grows on metal particles, uniformity of the tube diameter of the carbon nanotube and the metal particles can be ensured, the diameter of the finally prepared material is about 500 nm, and good catalytic performance is achieved.

Description

Technical field [0001] The invention belongs to the technical field of carbon nanotubes, and specifically relates to a method for preparing a carbon nanotube metal symbiotic material. Background technique [0002] Carbon materials, including activated carbon, carbon nanofibers, and carbon nanotubes, are a kind of excellent catalyst carriers with large specific surface area and high thermal stability. Because the surface is inert and has no interaction with active components, activated carbon is currently the most widely used carbon material carrier. However, the natural carbon source used for the production of activated carbon contains impurities such as heavy metals and sulfur. As a result, activated carbon needs to be removed in advance when used as a carrier. The heavy metal and sulfur impurities in the removal process are complicated, the conditions are harsh, and the cost is high. As a new type of nanomaterial, carbon nanotubes have high structural regularity, high mechanic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/745B01J23/75B01J23/755B01J35/02B82Y30/00B82Y40/00C01B32/16
Inventor 张伟刘俊霞王军峰闫鹏杨东元张新庄
Owner SHAANXI YANCHANG PETROLEUM GRP
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