Preparation method of non-metallic element doped nano zero-valent nickel loaded carbon fiber composite material

A technology of fiber composite materials and non-metallic elements, applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve problems such as complex operations, achieve good flexibility, large specific surface area, and inhibit oxidation Effect

Active Publication Date: 2018-09-04
HEFEI UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, it is necessary to switch carrier gases of different compositions during the preparation process, which makes the operation complicated

Method used

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  • Preparation method of non-metallic element doped nano zero-valent nickel loaded carbon fiber composite material
  • Preparation method of non-metallic element doped nano zero-valent nickel loaded carbon fiber composite material
  • Preparation method of non-metallic element doped nano zero-valent nickel loaded carbon fiber composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Pretreatment of carbon fiber cloth

[0034] Arrange 0.13g of carbon fibers in ethanol solution to ultrasonically remove surface impurities, then place them in nitric acid solution with a mass concentration of 32%, soak them at room temperature for 3 hours, wash them with water until they are neutral, and then dry them to obtain the modified carbon fibers modified by nitric acid. Activated carbon fiber cloth;

[0035] (2) Zero-valent nickel (Ni 0 ) loading of nanoparticles

[0036] The activated carbon fibers modified by nitric acid were arranged in a layer containing 2.3769g (10mmol) NiCl 2 ·6H 2 O(AR) and 1g polyvinylpyrrolidone in 20mL N,N-dimethylformamide (AR) solution, stirred for 200min, then transferred to a muffle furnace, pre-oxidized at 350°C for 2 hours to obtain a composite material precursor;

[0037] Weigh 1g (12mmol) of dicyandiamide in a quartz boat, spread the obtained precursor on the upper layer of dicyandiamide, and then transfer the whole to...

Embodiment 2

[0043] The preparation method of this embodiment is the same as that of Example 1, except that the calcining and pyrolysis process in step (2) is as follows: first, the temperature is raised to 400°C at 5°C / min, and the temperature is kept at a constant temperature for 2 hours; 800°C, constant temperature for 2 hours. After the reaction is finished, cool to room temperature to obtain nitrogen-doped nanometer zero-valent nickel (Ni 0 )Carbon fiber composite material.

[0044] The mass of the composite material prepared in this embodiment is ~0.134g, and the doping rate of nitrogen is ~4%.

Embodiment 3

[0046] The preparation method of this embodiment is the same as that of Example 1, except that the calcining and pyrolysis process in step (2) is as follows: first, the temperature is raised to 400°C at 5°C / min, and the temperature is kept at a constant temperature for 2 hours; 900°C, constant temperature for 2 hours. After the reaction is finished, cool to room temperature to obtain nitrogen-doped nanometer zero-valent nickel (Ni 0 )Carbon fiber composite material.

[0047] The mass of the composite material prepared in this example is ~0.133g, and the doping rate of nitrogen is ~4%.

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Abstract

The invention discloses a preparation method of a non-metallic element doped nano zero-valent nickel loaded carbon fiber composite material. The method includes the steps of: firstly impregnating nitric acid modified activated carbon fiber in a N, N-dimethylformamide solution containing nickel ions for pre-oxidation to obtain a precursor; then transferring the obtained precursor and an inorganic non-metallic salt into a tubular furnace together, and conducting calcination and pyrolysis under inert gas protection to obtain the target product. According to the invention, the nitric acid modifiedcarbon fiber surface has a lot of highly dispersed active centers, and provides favorable conditions for dispersion, growth and nucleation of metal particles; the in-situ controlled synthesis effectively avoids the agglomeration and oxidation of zero-valent nickel and the loss of active centers in the reaction process; and the composite material prepared by the method provided by the invention has excellent properties, and can be used for purification of volatile organic gases, catalytic hydrogenation, magnetic materials, supercapacitors and other fields.

Description

technical field [0001] The invention belongs to the technical field of carbon fiber materials, and in particular relates to a non-metallic element doped loaded nanometer zero-valent nickel (Ni 0 ) Preparation method of carbon fiber composite material. Background technique [0002] Zero-valent nickel (Ni 0 ) has broad application prospects in many fields such as catalysis, magnetic materials, optoelectronics, magnetic fluids, and information storage due to its unique properties such as low valence, small size, and many surface active sites. Zero-valent nickel (Ni 0 ) The common preparation methods include sol-gel method, hydrothermal method, chemical reduction method and vapor phase deposition method, etc. These commonly used preparation methods are simple in equipment and easy to operate, but the zero-valent nickel (Ni 0 ) is prone to agglomeration, cannot exist stably in the air, and is easily oxidized into nickel oxide. [0003] In order to overcome zero-valent nickel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/06B01J37/02B01J37/08B01J37/16
CPCB01J27/24B01J35/006B01J35/06B01J37/0207B01J37/082B01J37/16
Inventor 姚运金傅少同张婕余茂静冯乙巳高梦雪胡熠
Owner HEFEI UNIV OF TECH
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