Preparation method of high-dispersity supported nano metal catalyst

A nano metal and catalyst technology is applied in the field of preparation of highly dispersed supported nano precious metal catalysts, which can solve the problems of inability to control the size and morphology of metal particles, and it is difficult to obtain highly dispersed and long-life catalysts.

Active Publication Date: 2012-07-11
贵州鑫醇科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This patent also uses liquid phase reduction, but before the reduction, it is necessary to add alkali to adjust the pH value. During the reduction process, no structure-directing reagent and protective agent are added, and the size and shape of the metal particles cannot be controlled. Only a wide size distribution (40–80nm) is obtained. ) metal pellets; this patent still does not have ultrasonic dispersion and roasting steps, it is difficult to obtain a catalyst with high dispersion and long life

Method used

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  • Preparation method of high-dispersity supported nano metal catalyst
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  • Preparation method of high-dispersity supported nano metal catalyst

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Embodiment 1

[0039] Embodiment 1: Preparation of 2% Pd / Al 2 o 3 nanocatalyst

[0040] Weigh 1g of alumina and impregnate it into 5mL of 37.6mmol / L Pd(NO 3 ) 2- In the aqueous solution, stir for 3 hours, ultrasonically disperse in a 40°C water bath with 250W energy for 4 hours, dry at 110°C for 4 hours, bake at 350°C for 4 hours, add 0.070g ascorbic acid, 0.353g KBr, 0.444g PVP, and reduce at 100°C for 30 minutes, washed three times with water and ethanol, and dried under vacuum at 60°C for 10 hours. TEM photo see figure 1 , it can be seen from the figure that Pd is evenly dispersed on the surface of the carrier, and the particles are mainly spherical, with a small amount of irregular polyhedron, and the average size is 4–5 nm. High-resolution transmission electron microscope photos see figure 2 , it can be seen from the figure that the main exposed crystal plane of Pd is (111) plane.

Embodiment 2

[0041] Embodiment 2: Preparation of 1% Pd / Al 2 o 3 nanocatalyst

[0042] Weigh 1g of alumina and impregnate it into 2.5mL of 37.6mmol / L Pd(NO 3 ) 2- Add 2.5mL ethanol to the aqueous solution, stir for 3 hours, ultrasonically disperse in a 40°C water bath with 250W energy for 4 hours, dry at 110°C for 4 hours, and roast at 350°C for 4 hours, add 0.105g citric acid, 0.353g KBr, 0.523 g P123, reduced at 90°C for 15 hours, then added 0.018g of ascorbic acid to continue the reduction at 90°C for 30 minutes, washed with water and ethanol three times, and dried in vacuum at 60°C for 10 hours. TEM photo see image 3 , it can be seen from the figure that Pd is evenly dispersed on the surface of the carrier, and the particles are mainly spherical, with a small amount of irregular polyhedrons, and the average size is 4–6 nm. High-resolution transmission electron microscope photos see Figure 4 , it can be seen from the figure that the main exposed crystal plane of Pd is (111) plane...

Embodiment 3

[0043] Embodiment 3: Preparation of 0.5% Pd / Al 2 o 3 nanocatalyst

[0044] Weigh 1g of alumina and impregnate it into 1.25mL of 37.6mmol / L Pd(OAc) 2- Add 4 mL of acetone to the acetone solution, stir for 3 hours, ultrasonically disperse in a 35°C water bath with 200W energy for 4 hours, dry at 110°C for 4 hours, and roast at 400°C for 2 hours, add 1mL of 0.4mol / L potassium borohydride solution, 0.353 g KBr, 0.444g PVP, reduced at 100°C for 30 minutes, washed with water and ethanol three times, and dried under vacuum at 60°C for 10 hours. TEM photo see Figure 5 , it can be seen from the figure that Pd is evenly dispersed on the surface of the carrier, and the particles are mainly spherical, with a small amount of irregular polyhedron, and the average size is 3–5 nm.

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Abstract

The invention discloses a preparation method of a high-dispersity supported nano metal catalyst, particularly a preparation method of a supported nano noble metal catalyst, belonging to the technical field of catalyst preparation. The preparation method comprises the following steps: 1) impregnating a support into a metal precursor solution, and uniformly stirring; 2) carrying out ultrasonic dispersion under heating conditions; 3) drying, and roasting; 4) carrying out alkali-free liquid-phase controllable reduction; and 5) carrying out vacuum drying. By utilizing the actions of stirring and ultrasonic dispersion, the metal precursor is evenly adsorbed to the surface of the support, thereby implementing high dispersity of the active component; the roasting is utilized to enhance the interactions between the metal and the support; and the alkali-free liquid-phase controllable reduction is utilized to synthesize the nano metal catalyst of which the dimension is 2-10nm, the shape is spherical, cubic or polyhedral and the bare crystal face is (111), (100) or (110), thereby implementing the controllable preparation of the high-dispersity supported nano metal catalyst.

Description

[0001] technical field [0002] The invention relates to a preparation method of a highly dispersed and supported nanometer metal catalyst, in particular to a preparation method of a highly dispersed and supported nanometer precious metal catalyst. [0003] technical background [0004] Supported metal catalysts, especially supported noble metal catalysts, play an extremely important role in petroleum, chemical, pharmaceutical, pesticide, food, environmental protection, energy, electronics and other fields due to their irreplaceable catalytic activity and selectivity. Hydroreduction, oxidative dehydrogenation, catalytic reforming, hydrocracking, hydrodesulfurization, reductive amination, telomerization, coupling, disproportionation, ring expansion, cyclization, carbonylation, formylation, Noble metals are excellent catalysts in reactions such as dechlorination and asymmetric synthesis. In the field of environmental protection, precious metal catalysts are widely used in au...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J23/42B01J23/52B01J23/46B01J35/08
Inventor 徐忠宁郭国聪王明盛姚元根
Owner 贵州鑫醇科技发展有限公司
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