High dispersed loaded nano-metal Ni catalyst and preparation method thereof

A nano-metal and supported technology is applied in the field of preparation of highly dispersed supported nano-metal Ni catalysts, which can solve the problems of large particle size, collapse of laminates, small specific surface area, etc., and achieve good catalytic performance and improved dispersibility. Effect

Inactive Publication Date: 2011-05-25
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, as a kind of nano-sized particles, LDHs particles are easy to agglomerate, and after high-temperature roasting, the laminates will collapse, and the product nanoparticles will be sintere...

Method used

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  • High dispersed loaded nano-metal Ni catalyst and preparation method thereof
  • High dispersed loaded nano-metal Ni catalyst and preparation method thereof
  • High dispersed loaded nano-metal Ni catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 1 g of carbon nanotubes with a diameter of 40-60 nm and a length of 5-10 μm into 200 ml of acetone and mix them in a four-neck flask, then add 10 ml of acrylic acid, and ultrasonicate at room temperature for 30 minutes under nitrogen protection; then add 0.5 g of azobisiso Butyronitrile was reacted at 55°C for 8h; after cooling to room temperature, suction filtration was repeated, washed with water until neutral, and vacuum-dried at 60°C for 12h to obtain polyacrylic acid surface-functionalized carbon nanotubes for future use.

[0022] A. Weigh 4.3620g of Ni(NO 3 ) 2 ·6H 2 O and 1.8757g of Al(NO 3 ) 3 9H 2 O was dissolved in 50ml deionized water to prepare Ni(NO 3 ) 2 and Al(NO 3 ) 3 mixed salt solution, where Ni(NO 3 ) 2 The concentration is 0.3mol / L, Al(NO 3 ) 3 The concentration is 0.1mol / L; Weigh 2.5600g of NaOH and 2.1198g of NaOH 2 CO 3Dissolve in 100ml deionized water to prepare NaOH and Na 2 CO 3 Mixed alkaline solution, wherein the concentra...

Embodiment 2

[0027] A. with embodiment 1;

[0028] B. Add the mixed salt solution of 1.0000g of carbon nanotubes and 0.9087g of L-cysteine ​​and 50ml of step A after the method described in Example 1 into the reaction vessel, wherein the bridging agent L-cysteine Amino acid and Ni(NO 3 ) 2 The molar ratio of the substances is 1.0:2, ultrasonically disperse for 30min, then take 100ml of the above mixed alkali solution and add it dropwise into the reaction vessel, adjust the pH of the solution to 10.0, until the mixed alkali solution is added dropwise, then ultrasonically disperse for 30min, and crystallize The temperature is controlled at 60°C, the crystallization time is 6h, and the whole reaction is carried out under N 2 under atmosphere. After the reaction is completed, cool to room temperature, wash the filter cake with deionized water until neutral, and dry it in an oven at 60°C for 12 hours to obtain a NiAl-layered double metal hydroxide / carbon nanotube composite;

[0029] C. Plac...

Embodiment 3

[0032] A. with embodiment 1;

[0033] B. Add 0.5000g of carbon nanotubes treated according to the method described in Example 1 and 1.8174g of L-cysteine ​​and 50ml of step A mixed salt solution into the reaction vessel, wherein the bridging agent L-cysteine Acid and Ni(NO 3 ) 2 The molar ratio of the substances is 1.0:1, ultrasonically disperse for 40min, then take 100ml of the above mixed alkali solution and add it dropwise into the reaction vessel, adjust the pH of the solution to 11.0, until the mixed alkali solution is added dropwise, then ultrasonically disperse for 40min, and crystallize The temperature is controlled at 80°C, the crystallization time is 12h, and the whole reaction is carried out under N 2 under atmosphere. After the reaction is completed, cool to room temperature, wash the filter cake with deionized water until neutral, and dry it in an oven at 80°C for 18 hours to obtain a NiAl-layered double metal hydroxide / carbon nanotube composite;

[0034] C. P...

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Abstract

The invention provides a high dispersed loaded nano-metal Ni catalyst and a preparation method thereof, and belongs to the technical field of preparation of metal nano-particles. The bridging role of L-cysteine is utilized, the co-precipitation method is adopted for firstly preparing a NiAl-layered double-metal hydroxide/polyacrylic acid surface functional carbon nano-tube complex precursor, and then the high dispersed Ni metal catalyst loaded by carbon nano-tubes is further obtained by reducing the precursor through hydrogen. The loaded nano-metal Ni catalyst is formed by uniformly loading the mixture of Ni nano-particles and amorphous Al2O3 on the surface of the carbon nano-tubes, wherein the weight percentage content of the Ni is 3-30%, the weight percentage content of the amorphous Al2O3 is 1-10%, and the weight percentage content of the carbon nano-tubes is 60-95%; and the particle size distribution of the Ni nano-particles is 6-12nm. The catalyst is applied in hydrogenation reaction of o-chloronitrobenzene and can enable the o-chloronitrobenzene to perform selective hydrogenation for further generating o-chloroaniline, thereby showing good catalytic hydrogenation performance.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a preparation method of a highly dispersed and supported nanometer metal Ni catalyst. The catalyst is used for the selective catalytic hydrogenation of o-chloronitrobenzene. technical background [0002] O-chloroaniline is widely used as an intermediate in the production of pesticides, pharmaceuticals, dyes, and cosmetics. However, in the selective catalytic hydrogenation of o-chloronitrobenzene, it is often accompanied by side reactions of hydrodechlorination, which seriously affects the selectivity of the reaction and causes unnecessary waste of raw materials. Studies have shown that in order to increase the yield of p-chloronitrobenzene, many supported metal single-substance catalysts are used for selective hydrogenation, and they can convert o-chloronitrobenzene into o-chloroaniline very well. For example, Chen et al. found that the conversion rate and selectiv...

Claims

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Application Information

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IPC IPC(8): B01J23/755B82Y30/00B82Y40/00C07C211/52C07C209/36
Inventor 李峰王佳
Owner BEIJING UNIV OF CHEM TECH
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