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Preparation method of high-selectivity palladium catalyst

A palladium catalyst, high-selectivity technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., to achieve high purity, large specific surface area, improved activity and selectivity sexual effect

Inactive Publication Date: 2016-05-04
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as far as we know, molecular imprinting technology has not been used for the preparation of H by the anthraquinone method 2 o 2 A report on the preparation process of the catalyst in the hydrogenation process

Method used

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  • Preparation method of high-selectivity palladium catalyst
  • Preparation method of high-selectivity palladium catalyst
  • Preparation method of high-selectivity palladium catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0028] First, 0.048 g of 2-ethylanthraquinone (4 wt %) was dissolved in 45 mL of isopropanol with sufficient stirring at room temperature. Next, 4.8 g of aluminum isopropoxide was added, stirred at 72° C., and fully dissolved. Then, a mixed solution prepared by 1.27mL of water and 0.67mL of acetic acid (molar ratio water: acetic acid=6:1) was added dropwise thereto, and fully stirred at room temperature for 0.5h to obtain a sol, which was put into an oven and heated at 80 Aging at constant temperature for 20 hours at ℃, the gel obtained after aging was centrifuged and washed 3 times with isopropanol; finally, γ-Al 2 o 3 .

[0029] Take the above 1.2g γ-Al 2 o 3 , impregnated with an equal volume of aqueous solution prepared by 0.0060g palladium chloride and 0.0040g sodium chloride at 60°C for 2h, washed with distilled water, and suction filtered until there was no Cl in the filtrate - , and then dried in an oven at 120°C for 2h, further calcined at 450°C for 4h, and final...

Embodiment 2

[0032] First, 0.168 g of 2-ethylanthraquinone (14 wt %) was thoroughly stirred and dissolved in 45 mL of isopropanol at room temperature. Next, 4.8 g of aluminum isopropoxide was added, stirred at 72° C., and fully dissolved. Then, a mixed solution prepared by 0.85mL of water and 0.67mL of acetic acid (molar ratio water: acetic acid=4:1) was added dropwise thereto, and fully stirred at room temperature for 1.5h to obtain a sol, which was put into an oven and heated at 80 Aging at constant temperature for 20 hours at ℃, centrifuging and washing the gel obtained after aging for 3 times with isopropanol; finally, vacuum drying at 80℃ for 6 hours and roasting at 700℃ for 3 hours to obtain γ-Al 2 o 3 .

[0033] Take the above 1.2g γ-Al 2 o 3 , impregnated with an equal volume of aqueous solution prepared by 0.0040g palladium chloride and 0.0026g sodium chloride at 60°C for 2h, washed with distilled water, and suction filtered until there was no Cl in the filtrate - , and then ...

Embodiment 3

[0036] First, 0.108 g of 2-ethylanthraquinone (9 wt %) was thoroughly stirred and dissolved in 45 mL of isopropanol at room temperature. Next, 4.8 g of aluminum isopropoxide was added, stirred at 72° C., and fully dissolved. Then, a mixed solution prepared by 2.12 mL of water and 0.67 mL of acetic acid (molar ratio water: acetic acid = 10:1) was added dropwise thereto, and stirred thoroughly at room temperature for 3 hours to obtain a sol, which was put into an oven and heated at 80° C. After aging at constant temperature for 20 hours, the aged gel was centrifuged and washed 3 times with isopropanol; finally, it was vacuum-dried at 80°C for 9 hours and calcined at 400°C for 5 hours to obtain γ-Al 2 o 3 .

[0037] Take the above 1.2g γ-Al 2 o 3 , impregnated with an equal volume of aqueous solution prepared by 0.0020g palladium chloride and 0.0013g sodium chloride at 60°C for 2h, washed with distilled water, and suction filtered until there was no Cl in the filtrate - , an...

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Abstract

The invention provides a preparation method of a high-selectivity palladium catalyst, which comprises the following steps of: (1) dissolving 2-ethyl anthraquinone in isopropanol at room temperature by sufficiently stirring, adding aluminum isopropoxide to the solution according to the mass ratio of 2-ethyl anthraquinone to aluminum isopropoxide being 1:(28.57-100), heating, sufficiently stirring for dissolving, dripping mixed liquid of acetic acid and water, and sufficiently stirring at room temperature for hydrolysis; (2) aging a hydrolysis product at 80 DEG C for 20h, separating, washing, drying and calcining to obtain gamma-Al2O3 powder; and (3) isometrically immersing the gamma-Al2O3 powder with sodium tetrachloropalladate solution, washing, drying and calcining to obtain the efficient loaded palladium catalyst. The preparation method has the advantages of novelty, simple operation, controllable specific area, pore diameter and other structure properties of the product and the like; and the prepared 2-ethyl anthraquinone regulated and controlled catalyst has good selectivity and activity on anthraquinone hydrogenation reaction.

Description

technical field [0001] The invention belongs to the field of preparation and catalytic application of mesoporous alumina, in particular to an anthraquinone method for producing H 2 o 2 Highly selective palladium catalyst for hydrogenation process and method for its preparation. Background technique [0002] h 2 o 2 It is an excellent green chemical raw material, widely used in papermaking, food, environmental protection and pharmaceutical industries. Its production methods are constantly being innovated. The direct synthesis of hydrogen and oxygen has attracted much attention, but most of them are in the laboratory stage, while the anthraquinone method is the current industrial production of H 2 o 2 mainstream route. At present, palladium catalyst fixed bed anthraquinone method is widely used in China to produce H 2 o 2 , the hydrogenation process is a key step in the anthraquinone process, which mainly uses the catalyst of mesoporous active alumina supported noble m...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J35/10C01B15/023
CPCC01B15/023B01J21/04B01J23/44B01J35/615B01J35/635B01J35/633B01J35/647
Inventor 蔡卫权卓俊琳方继敏
Owner WUHAN UNIV OF TECH
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