Carbon material coated nickel nanoparticle catalyst as well as preparation method and application thereof

A technology of nickel nanoparticles and carbon materials, used in catalyst protection, cyanide reaction preparation, amino compound preparation, etc., can solve the problem of metal utilization, carbon coating degree, which has not been reported, cannot be applied to acidic environment systems, and hydrogen chloride has no effect on equipment. Corrosion and other problems, to achieve the effect of green and efficient preparation method, easy operation, and improved catalytic activity

Pending Publication Date: 2021-12-31
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Tang et al [RSC Advances, 2017, 7(3):1531-1539] take terephthalic acid as coordination, nickel nitrate as nickel source, N,N-dimethylformamide as solvent, and react in an autoclave Prepare Ni-MOF precursor, and further prepare carbon-coated nickel catalyst through high-temperature nickel carbide source. This material also shows good selectivity in the hydrogenation reaction of aromatic nitro compounds such as p-chloronitrobenzene, but The thicker carbon layer leads to poor activity, and there are obvious pores that can be entered by reactant molecules, and metal nickel can be completely leached in an acidic environment
Although the above materials have shown good activity and selectivity in the reaction of halonitrobenzene to haloaniline, they cannot be applied to acidic environment systems, and it is easy to dechlorinate p-chloroaniline during the reaction process, reducing the risk of product quality. The hydrogen chloride produced at the same time will seriously corrode the equipment
In addition, the metal utilization rate and carbon coating degree of metal nickel prepared into carbon-coated catalysts have not been reported.

Method used

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  • Carbon material coated nickel nanoparticle catalyst as well as preparation method and application thereof
  • Carbon material coated nickel nanoparticle catalyst as well as preparation method and application thereof
  • Carbon material coated nickel nanoparticle catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] Weigh a certain amount of nickel nitrate hexahydrate and 4-pyridinecarboxylic acid and dissolve in a certain amount of absolute ethanol, the molar ratio of nickel to organic ligand is 1:2; the mass ratio of nickel to alcohol solution is 1:100. Heat at 25°C After stirring for 6 hours, add 1.0 mol / L sodium hydroxide aqueous solution dropwise to the mixed solution, adjust the pH of the solution to 4.0, and keep for 1 hour; add dropwise 98% triethanolamine solution, adjust the pH to 6.5, and keep for 2 hours; Add 25-28% ammonia water dropwise, adjust the pH to 8.5, and keep it for 2 hours. The resulting slurry is sealed and placed on a vibration table. The vibration program is set as follows: 1) Vibration frequency 10Hz, banner vibration for 2 minutes; 2) Vibration frequency 30Hz, banner vibration for 5 minutes; 3) Vibration frequency 40Hz, banner vibration for 1 minute; 4) The operation procedure 1)-3) is a vibration cycle; the entire crystallization, precipitation and agi...

Embodiment 16

[0118] Example 16 investigated the performance of different nickel nanoparticle catalysts prepared in Examples 1-15 and Comparative Examples 1-16 in catalytic hydrogenation synthesis of haloanilines.

[0119] In a 50ml stainless steel reaction kettle, add 25ml methanol, 1.0g p-chloronitrobenzene, 0.05g carbon material coated nickel nanoparticle catalyst prepared by different embodiments or comparative examples, close the reaction kettle, and replace the air in the reaction kettle with hydrogen for 10 The second time, the temperature was raised to 100°C, the hydrogen pressure was 1.0 MPa, stirring was started, and the stirring rate was 1800 r / min, and the reaction was carried out for 40 minutes. Stop the reaction, and after the temperature drops to room temperature, take the supernatant of the reaction solution, filter the catalyst, and analyze the filtrate by gas chromatography. The experimental results are shown in Table 3:

[0120] Table 3 Performance of different carbon ma...

Embodiment 17

[0124] Example 17 investigated the reaction performance of the carbon material-coated nickel nanoparticle catalyst prepared in Example 2 for the hydrogenation of different halogenated nitrobenzenes to prepare halogenated anilines.

[0125] In a 50ml stainless steel reactor, add 25ml of methanol, 1.0g of different halogenated nitrobenzenes, 0.05g of the carbon material coated nickel nanoparticle catalyst prepared in Example 2, close the reactor, and replace the air in the reactor with hydrogen for 10 times , the temperature was raised to 100° C., the hydrogen pressure was 1.0 MPa, stirring was started at a stirring rate of 1800 r / min, and the reaction was carried out for 1 h. Stop the reaction, and after the temperature drops to room temperature, take the supernatant of the reaction solution, filter the catalyst, and analyze the filtrate by gas chromatography. The experimental results are shown in Table 4:

[0126] Table 4 Reaction performance of nickel nanoparticle catalysts ...

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Abstract

The invention discloses a carbon material coated nickel nanoparticle catalyst as well as a preparation method and application thereof. The carbon material coated nickel nanoparticle catalyst is prepared according to the following steps of: (1) weighing and pouring nickel salt and an organic ligand into an alcohol solvent for dissolving, and stirring at 0-50 DEG C for 3-24 hours to obtain a mixed solution; (2) dropwise adding alkali liquor into the mixed solution in batches, and adjusting the pH value of the solution in three stages; (3) sealing the slurry obtained in the step (2), placing the sealed slurry on a vibration platform, crystallizing, precipitating, aging, filtering, washing, and carrying out vacuum drying to obtain a metal organic framework precursor; and (4) roasting the precursor to obtain the carbon material coated nickel nanoparticle catalyst. The invention provides an application of the catalyst in the catalytic hydrogenation synthesis of halogenated aniline from halogenated nitrobenzene. According to the preparation method disclosed by the invention, the morphology of the precursor is effectively controlled on the basis of improving the metal utilization rate, so that the catalyst with a specific micro-structure is obtained, and the product selectivity can be effectively improved.

Description

technical field [0001] The invention belongs to the field of catalyst preparation technology and application, and relates to a carbon material-coated nickel nanoparticle catalyst and a preparation method and application thereof. Background technique [0002] Nickel nanoparticles have great application value in catalysis, lithium batteries, sensors and other fields. As a catalyst, nanoscale nickel particles have better catalytic activity than bulk or flake, but due to the high surface energy, nanoscale nickel particles are easy to agglomerate and limit its advantages. When exposed to the air, the metal nanoparticles are easily oxidized into metal oxides, and a layer of carbon material wrapped around the metal nanoparticles can prevent the metal nanoparticles from being oxidized. In addition to the characteristics of non-toxicity, high thermal stability and low price, the carbon layer-coated metal structure also has the characteristics of graphene. Its rich internal pore stru...

Claims

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Application Information

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IPC IPC(8): B01J21/18B01J23/755B01J33/00B01J35/00B01J35/02C07C209/36C07C211/52C07C213/02C07C217/90C07C221/00C07C225/34C07C227/04C07C229/60C07C303/22C07C309/46
CPCB01J23/755B01J21/18B01J33/00C07C209/365C07C227/04C07C303/22C07C213/02C07C221/00B01J35/394B01J35/396B01J35/393B01J35/40C07C211/52C07C229/60C07C309/46C07C217/90C07C225/34
Inventor 卢春山杨园园李小年张群峰丰枫
Owner ZHEJIANG UNIV OF TECH
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