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A kind of preparation method of highly selective palladium catalyst

A palladium catalyst and high-selectivity technology, which is applied in chemical instruments and methods, physical/chemical process catalysts, inorganic chemistry, etc., to achieve the effects of simple process operation, improved adsorption capacity, and high purity

Inactive Publication Date: 2017-12-29
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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  • A kind of preparation method of highly selective palladium catalyst
  • A kind of preparation method of highly selective palladium catalyst
  • A kind of preparation method of highly selective palladium catalyst

Examples

Experimental program
Comparison scheme
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 is a preparation method of a highly selective palladium catalyst. The steps are as follows: (1) Fully stir and dissolve 2-ethylanthraquinone in isopropanol at room temperature, and add 2-ethylanthraquinone to the above solution. The mass ratio of aluminum isopropoxide to aluminum isopropoxide is 1: (28.57~100) Add aluminum isopropoxide, heat and stir to fully dissolve, then add a mixture of acetic acid and water dropwise to the above solution, and stir thoroughly at room temperature for hydrolysis; (2 ) Aging the above hydrolyzate for 20 hours at 80°C, after separation, washing, drying, and roasting in sequence to obtain γ-Al2O3 powder; (3) Impregnating the above γ-Al2O3 powder with an equal volume of sodium tetrachloropalladate solution, and then The high-efficiency supported palladium catalyst is obtained by washing, drying and roasting in sequence. The invention has the advantages of novel method, simple operation, and controllable texture properties such as product specific surface area and pore size. The prepared 2-ethylanthraquinone-regulated catalyst has excellent selectivity and activity for the 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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Patent Type & Authority Patents(China)
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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