Supported nickel catalyst for production of hydrogen peroxide through anthraquinone hydrogenation method, and preparation method thereof

A nickel catalyst, supported technology, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the high cost of hydrogen peroxide production, unfavorable operation, hydrogen consumption And other issues

Inactive Publication Date: 2014-05-07
HIGH TECH RES INST NANJING UNIV LIANYUNGANG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, using palladium as a catalyst, the hydrogenation of the benzene ring in anthraquinone is carried out at the beginning of the reaction. Although the generation of a small amount of tetrahydroanthraquinone has no effect on the yield of hydrogen peroxide, and it is possible to increase the reaction rate, but with As the reaction progresses, more and more tetrahydroanthraquinones accumulate, making the viscosity of the working fluid thicker, which is unfavorable for operation and causes unnecessary consumption of hydrogen
In addition, the high price of the palladium catalyst also makes the production cost of hydrogen peroxide produced by this method higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: take by weighing 29.7g Ni (NO 3 ) 2. 6H 2 O, 27.4gAl(NO 3 ) 3. 9H 2 O and 19.2gMg(NO 3 ) 2. 6H 2 O, dissolved in water to make 100ml solution; another 22.9gNa 2 CO 3 Dissolve in water to form a 100ml solution. Add the above two solutions dropwise to 200ml of distilled water (80°C water bath) under stirring to form a green precipitate, wash the precipitate with distilled water, then wash once with absolute ethanol, add 100ml of absolute ethanol, evaporate to dryness at 80°C, and place in an oven Dry at 120°C to obtain a green supported nickel catalyst precursor. The resulting nickel catalyst precursor was first placed in N 2 Baked at 200°C for 4h under atmosphere, then switched to H 2 atmosphere, and reduced at 400°C for 2 hours to obtain a supported metal nickel catalyst. The measured surface area is 435m 2 / g, the average pore diameter is 9.2nm, and the pore volume is 1.0cm 3 / g, active metal nickel surface area 44m 2 / g.

Embodiment 2

[0020] Embodiment 2: take by weighing 39.6g Ni (NO 3 ) 2. 6H 2 O and 7.35gAl(NO 3 ) 3. 9H 2 O was dissolved in water to make 100ml solution; another 23.6gNa 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 60°C) under stirring to form a green precipitate, wash the precipitate with distilled water, and wash once with acetone, then add 100ml of n-amyl alcohol, evaporate to dryness at 80°C, and place in an oven at 120°C ℃ drying to obtain a green supported nickel catalyst precursor. The resulting nickel catalyst precursor was first placed in N 2 Calcined at 400°C for 4h under atmosphere, then switched to H 2 atmosphere, and reduced at 400°C for 2 hours to obtain a supported metal nickel catalyst. The measured surface area is 380m 2 / g, the average pore diameter is 15nm, and the pore volume is 1.4cm 3 / g, active metal nickel surface area 68m 2 / g.

Embodiment 3

[0021] Embodiment 3: take by weighing 34.7g Ni (NO 3 ) 2. 6H 2 O and 7.35gAl(NO 3 ) 3. 9H 2 O was dissolved in water to make 100ml solution; another 23.6gNa 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 60°C) under stirring to form a green precipitate, wash the precipitate with distilled water, and wash once with acetone, then add 100ml of n-amyl alcohol, evaporate to dryness at 80°C, and place in an oven at 120°C ℃ drying to obtain a green supported nickel catalyst precursor. The resulting nickel catalyst precursor was first placed in N 2 Calcined at 400°C for 4h under atmosphere, then switched to H 2 atmosphere, and reduced at 400°C for 2 hours to obtain a supported metal nickel catalyst. Measure its surface area to be 260m 2 / g, the average pore diameter is 29nm, and the pore volume is 1.9cm 3 / g, active metal nickel surface area 54m 2 / g.

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Abstract

The invention discloses a preparation method of a supported nickel catalyst. The method comprises the following steps: making a mixed solution containing soluble nickel salt and aluminium nitrate or a mixed solution containing soluble nickel salt, magnesium nitrate, and aluminium nitrate react with a precipitant so as to obtain a green precipitate, washing the precipitate with distilled water, then carrying out a supercritical drying treatment or an azeotropic distillation drying treatment so as to obtain a precursor of the supported nickel catalyst; calcining the precursor for 2 to 5 hours in the atmosphere of N2 and at a temperature of 200 to 600 DEG C; and then switching to an atmosphere of H2 to carry out reduction reactions for 2 to 4 hours at a temperature of 300 to 550 DEG C so as to obtain the supported high active nickel catalyst. The supported nickel catalyst has a specific surface area of 250 to 450 m<2> / g, an average pore diameter of 9 to 30 nm, and a pore volume of 1.0 to 1.9 cm<3> / g. The surface area of the active metal nickel loaded on the catalyst is 40 to 70 m<2> / g. The supported nickel catalyst is applied to the hydrogen peroxide production through an anthraquinone hydrogenation method.

Description

technical field [0001] The invention relates to a preparation method of a supported metal nickel catalyst, which is used for hydrogenation of anthraquinone to prepare hydrogen peroxide. Background technique [0002] Hydrogen peroxide is an important inorganic chemical product, which is widely used in papermaking, chemical industry, food, environmental protection and other fields. The final product decomposed during the use of hydrogen peroxide is mainly water, which will not produce secondary pollutants. It is an environmentally friendly oxidant, and the oxidation process using hydrogen peroxide as the oxidant has the characteristics of mild reaction conditions and high selectivity. With the continuous development of the green chemical process, the application of hydrogen peroxide as a green oxidant will become more and more extensive. For example, new clean production processes such as cyclohexanone, caprolactam, hydroquinone, and propylene oxide all use hydrogen peroxide a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755C01B15/023
Inventor 沈俭一赵长艳申卫卫李明时黄玉安宋金文
Owner HIGH TECH RES INST NANJING UNIV LIANYUNGANG
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