A kind of supported lacquer original nickel catalyst and preparation method thereof

A catalyst and lacquer raw nickel technology, applied in the field of integral lacquer raw nickel catalyst and its preparation, can solve the problems of complicated reaction process control, short reaction residence time, etc., and achieve the effects of optimizing the reaction process, improving the catalytic reaction efficiency and uniform distribution

Inactive Publication Date: 2017-05-10
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN1245163A discloses an improved method for hydrogenation of dinitrotoluene, which enables dinitrotoluene to be hydrogenated continuously, substantially solvent-free, and adiabatically to toluene by incorporating a monolithic catalyst into the plug flow reactor system Diamine, but the reaction residence time is short and the reaction process control is complex

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  • A kind of supported lacquer original nickel catalyst and preparation method thereof

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Effect test

Embodiment 1

[0028] (1) Φ6×10cm, the hole density is 260cpsi, the bulk density is 0.6g / cm 3 The ceramic carrier was immersed in a silica sol with a solid content of 30% at 55°C and stirred continuously. After 2 minutes, it was slowly taken out and purged with air, dried at 110°C for 1 hour, and then baked in a muffle furnace at 300°C for 3 hours to obtain a coating. carrier;

[0029] (2) The coated carrier is put into a vacuum chamber, and then the vacuum chamber is filled with Zn(CH 3 ) 2 , After 1min, vacuumize to 130Pa. After scanning the surface of the carrier with a frequency-doubled ultraviolet continuous argon ion laser (λ=250nm, P=3.000mw) for 4min, fill the vacuum chamber with 7% Zn(CH 3 ) 2 , irradiate with defocused pulsed excimer ArF laser (λ=195nm, 12mJ / pulse, 10ns) for 60s, and load Zn on the carrier coating;

[0030] (3) Configure 300ml of 0.5mol / L nickel chloride solution, immerse the Zn-loaded carrier in step (2) into the prepared solution and react for 1h under stirr...

Embodiment 2

[0033] (1) Φ6×10cm, the hole density is 260cpsi, the bulk density is 0.6g / cm 3 The ceramic carrier was immersed in silica gel with a solid content of 30% at 55°C and stirred continuously. After 3 minutes, it was slowly taken out and purged with air, dried at 110°C for 1 hour, and then baked in a muffle furnace at 500°C for 1 hour to obtain a coated carrier. ;

[0034](2) The coated carrier is put into a vacuum chamber, and then the vacuum chamber is filled with Zn(CH 3 ) 2 , After 3min, vacuumize to 140Pa. After scanning the surface of the carrier with a frequency-doubled ultraviolet continuous argon ion laser (λ=255nm, P=2.500mw) for 6min, fill the vacuum chamber with 9% Zn(CH 3 ) 2 , with a defocused pulsed excimer ArF laser (λ=192nm, 10mJ / pulse, 10ns) irradiated for 70s, Zn is loaded on the carrier coating;

[0035] (3) Configure 300ml of 0.75mol / L nickel chloride solution, immerse the Zn-loaded carrier in step (2) into the prepared solution and react for 1h under stir...

Embodiment 3

[0038] (1) Φ6×10cm, the hole density is 260cpsi, the bulk density is 0.6g / cm 3 The ceramic carrier was immersed in silica gel with a solid content of 30% at 55°C and stirred continuously. After 2 minutes, it was slowly taken out and purged with air, dried at 110°C for 1 hour, and then baked in a muffle furnace at 400°C for 2 hours to obtain a coated carrier. ;

[0039] (2) The coated carrier is put into a vacuum chamber, and then the vacuum chamber is filled with Zn(CH 3 ) 2 , After 1min, vacuumize to 135Pa. After scanning the surface of the carrier with a frequency-doubled ultraviolet continuous argon ion laser (λ=257nm, P=2.000mw) for 7min, fill the vacuum chamber with 12% Zn(CH 3 ) 2 , with a defocused pulsed excimer ArF laser (λ=195nm, 11mJ / pulse, 8ns) irradiated for 70s to load Zn on the carrier coating;

[0040] (3) Configure 300ml of 1mol / L nickel chloride solution, immerse the Zn-loaded carrier in step (2) in the prepared solution and react for 2h under stirring i...

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Abstract

A supported urushibara nickel catalyst is characterized in that the catalyst adopts ceramic as a supporter, SiO2 as a coat and metallic zinc and nickel as active components, the mass of the coat SiO2 is 10-20wt% of the mass of the coat supported supporter, the support amount of the active component Zn is 2-5wt% of the mass of the coat supported supporter, and the support amount of the active component Ni is 3-8wt% of the mass of the coat supported supporter. The catalyst is suitable for bubble reactors, and has the advantages of simple separation, high mechanical strength and large specific surface area.

Description

technical field [0001] The invention belongs to a catalyst and a preparation method thereof, in particular to an integral lacquer original nickel catalyst and a preparation method thereof. Background technique [0002] Toluene diamine is an important organic chemical raw material, which is often used to synthesize toluene diisocyanate (TDI). At present, the catalysts used to catalyze the hydrogenation of dinitrotoluene to synthesize toluenediamine in industry are mainly supported noble metal catalysts and skeleton nickel catalysts. The supported noble metals are expensive and prone to carbon deposition and deactivation, and skeleton nickel catalysts are prone to spontaneous combustion and environmental pollution. serious problem. [0003] Urushihara nickel catalyst was replaced by reduced Zn powder in 1952 by the scientist Urushihara. 2+ It is elemental Ni, which is prepared by lye activation. The lacquer original nickel catalyst has a simple preparation process, is not e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755
Inventor 李忠郝志强于智慧
Owner TAIYUAN UNIV OF TECH
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