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Preparation method of supported nickel catalyst

A nickel catalyst, supported technology, applied in catalyst activation/preparation, physical/chemical process catalyst, hydrogenation hydrocarbon production, etc., can solve the problems of long time, high product price, high equipment requirements, etc.

Inactive Publication Date: 2010-06-16
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under critical conditions, the gas-liquid interface disappears, and the surface tension no longer exists. Supercritical drying technology can effectively eliminate surface tension and prepare materials with high surface area and large pore volume, but the time required for supercritical drying is relatively long, and the equipment is The requirements are relatively high, and the price of the resulting product is also relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 29.7g Ni(NO 3 ) 2 .6H 2 Dissolve O in water to make a 100ml solution; take another 18.9g Na 2 SiO 3 .9H 2 O and 11.7 g Na 2 CO 3 Dissolve in water to form a 100ml solution. Add the above two solutions dropwise to 200ml of distilled water (60°C water bath) under stirring to form a green precipitate, wash the precipitate with distilled water and add it to the autoclave, then add 100ml of absolute ethanol as a supercritical solvent, and pass N 2 Purge for 30 minutes, remove the air in the system, seal the supercritical drying device, raise the temperature of the autoclave to 260 ° C, and the pressure in the autoclave reaches about 7.0 MPa, keep this state for 1 hour and release the pressure to normal pressure, then use N 2 Purge for 2 hours and cool to room temperature. Open the sealing cap to obtain the green supported nickel catalyst precursor. The obtained nickel catalyst precursor was calcined at 300° C. for 4 hours in a nitrogen atmosphere, then switche...

Embodiment 2

[0024] Weigh 34.7g Ni(NO 3 ) 2 .6H 2 O and 3.4g Al(NO 3 ) 3 .9H 2 O, dissolved in water to make 100ml solution; another 11.8g Na 2 SiO 3 .9H 2 O and 16.1 g Na 2 CO 3 Dissolve in water to form a 100ml solution. Add the above two solutions dropwise to 200ml of distilled water (water bath at 80°C) under stirring to form a green precipitate, wash the precipitate with distilled water, wash with ethanol once, add 100ml of absolute ethanol, evaporate to dryness at 80°C, and place in an oven at 120°C ℃ drying to obtain a green supported nickel catalyst precursor. The obtained nickel catalyst precursor was calcined at 200° C. for 4 hours in a nitrogen atmosphere, then switched to a hydrogen atmosphere, heated to 400° C., and reduced for 2 hours to obtain a supported metal nickel catalyst. The measured surface area is 480m 2 / g, average pore diameter 9.2nm, pore volume 1.5cm 3 / g, the surface area of ​​metallic nickel is 58m 2 / g-catalyst.

Embodiment 3

[0028] Weigh 24.8g Ni(NO 3 ) 2 .6H 2 O and 18.4g Al(NO 3 ) 3 .9H 2 Dissolve O in water to make a 100ml solution; take another 11.8g Na 2 SiO 3 .9H 2 O and 40.6 g Na 2 CO 3 Dissolve in water to form a 100ml solution. Add the two solutions dropwise to 200ml of distilled water (40°C water bath) under stirring to form a green precipitate, wash the precipitate with distilled water, then wash once with ethanol, add 100ml of n-butanol, evaporate to dryness at 80°C, and place in an oven at 120°C drying to obtain a green supported nickel catalyst precursor. The obtained nickel catalyst precursor was calcined at 400° C. for 4 hours in a nitrogen atmosphere, then switched to a hydrogen atmosphere, and reduced for 2 hours to obtain a supported metal nickel catalyst. The measured surface area is 530m 2 / g, average pore diameter 16.4nm, pore volume 1.8cm 3 / g, the surface area of ​​metallic nickel is 50m 2 / g-catalyst.

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Abstract

The invention discloses a preparation method of a supported nickel catalyst, which comprises the following steps of: reacting soluble nickel salt solution and a precipitator to obtain a green precipitate, wherein the precipitator is mixed solution of sodium silicate and sodium carbonate, the Na<+> concentration is 0.1-1 mol / L, the amount of the sodium silicate is calculated according to the content of SiO2 in a carrier, and the amount of the sodium carbonate is 10-30 percent more than that of nickel nitrate based on a stoichiometric ratio; washing the precipitate by distilled water and carrying out supercritical drying or azeotropic distillation drying to obtain a supported nickel catalyst precursor; roasting the supported nickel catalyst precursor for 2-5 hours under N2 atmosphere at 200-600 DEG C, changing the N2 atmosphere into H2 atmosphere, and reducing the supported nickel catalyst precursor for 2-4 hours under H2 atmosphere at 300-550 DEG C to obtain the supported nickel catalyst with the surface area of high active metal nickel. The surface area of the obtained catalyst is 250-450m<2> / g, the average aperture is 4-16nm, and the pore volume is 1.0 -1.9cm<3> / g. The surface area of the active metal nickel of the obtained catalyst is 40-70m<2> / g. The catalyst prepared by using the method can be used for catalyzing hydrogenation of a benzene ring.

Description

Technical field: [0001] The invention relates to a preparation method of a supported metal nickel catalyst, which can be used for aromatic ring hydrogenation reaction. Background technique: [0002] Nickel catalysts are widely used in industrial catalytic reactions, such as hydrogenation of compounds, hydrogen production by reforming hydrocarbons, and reductive amination of alcohols. Typical hydrogenation reactions include hydrogenation of olefins to saturated hydrocarbons, hydrogenation of aromatic rings, hydrogenation of nitriles to amines, etc. Raney nickel and supported nickel catalysts are commonly used hydrogenation catalysts. At present, Raney nickel is widely used in industrial hydrogenation reactions. However, Raney nickel catalysts have problems such as poor catalytic performance, environmental pollution, and difficulty in recycling spent catalysts. Now they are gradually replaced by supported nickel catalysts. [0003] In the hydrogenation reaction, the nature, ...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J37/08C07B35/02C07C13/18C07C5/10C07C35/08C07C29/19
Inventor 沈俭一薛明伟胡胜华陈慧
Owner NANJING UNIV
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