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High performance supported Pd catalyst for 2-ethyl anthraquinone hydrogenation and preparation method thereof

A high-performance technology of ethylanthraquinone, applied in the field of high-performance supported Pd-catalyst for hydrogenation of 2-ethylanthraquinone and its preparation

Inactive Publication Date: 2016-10-12
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But so far, there are few reports on the simultaneous addition of Fe and Ba modified alumina supports to improve the activity and stability of anthraquinone hydrogenation to prepare hydrogen peroxide hydrogenation catalysts.

Method used

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  • High performance supported Pd catalyst for 2-ethyl anthraquinone hydrogenation and preparation method thereof
  • High performance supported Pd catalyst for 2-ethyl anthraquinone hydrogenation and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 1. γ-Al 2 o 3 Preparation of vector

[0015] Weigh 5.5g of sodium metaaluminate and dissolve it in 60mL of deionized water, adjust the pH to 7 with concentrated hydrochloric acid, put it in a water bath at 80°C for 8h, wash the precipitate with deionized water until neutral, separate it and dry it in vacuum at 70°C for 8h The aluminum hydroxide precursor was obtained, and then calcined in a muffle furnace under a static air atmosphere at 650 °C for 4 hours to obtain γ-Al 2 o 3 carrier.

[0016] 2. Loading of Pd-

[0017] Take 1.0g of the γ-Al prepared above 2 o 3 carrier, with PdCl 2 The solution was impregnated in equal volume at 60°C for 2h (the loading capacity of Pd- was 0.3wt%), and then washed three times with 0.1mol / L NaOH solution (1h interval between each time), and then washed with deionized water until neutral, and then Normal drying at 120°C for 4h, and finally calcining in a muffle furnace at 550°C under a static air atmosphere for 4h to prepare cat...

Embodiment 2

[0021] 1. γ-Al 2 o 3 Preparation of vector

[0022] Weigh 1.0g of P123 and dissolve it in 60mL of deionized water. After the dissolution is complete, add 5.5g of sodium metaaluminate until it is completely dissolved, adjust its pH to 8 with concentrated hydrochloric acid, bathe in water at 80°C for 6 hours, and wash the precipitate with deionized water to Neutral, washed once with ethanol, separated and dried in vacuum at 80°C for 10h to obtain the aluminum hydroxide precursor, and then roasted in a muffle furnace for 4h under a static air atmosphere at 550°C to obtain γ-Al 2 o 3 carrier.

[0023] 2. Loading of Pd

[0024] Take 1.0g of the γ-Al prepared above 2 o 3 carrier, with PdCl 2 The solution was impregnated in equal volume at 60°C for 2h (the loading capacity of Pd- was 0.3wt%), and then washed three times with 0.1mol / L NaOH solution (1h interval between each time), and then washed with deionized water until neutral, and then Normal drying at 120°C for 4h, and f...

Embodiment 3

[0026] 1. γ-Al 2 o3 Preparation of vector

[0027] Weigh 1.0g of P123 and dissolve it in 60mL of deionized water. After the dissolution is complete, add 5.5g of sodium metaaluminate until it is completely dissolved, adjust its pH to 8 with concentrated hydrochloric acid, bathe in water at 70°C for 8 hours, and wash the precipitate with deionized water until Neutral, then washed once with ethanol, separated and dried in vacuum at 80 °C for 10 h to obtain the precursor of aluminum hydroxide, and used Fe(NO 3 ) 3 9H 2 O was co-impregnated with equal volume of the above-mentioned vacuum-dried product at 60°C for 2h (the loading of Fe- was 1wt%), and further vacuum-dried the impregnated product in a vacuum drying oven, and then in a static air atmosphere at 600°C in a muffle furnace. Under roasting for 4h, the carrier can be prepared.

[0028] 2. Loading of Pd

[0029] Take 1.0g of the γ-Al prepared above 2 o 3 carrier, with PdCl 2 The solution was impregnated in equal volu...

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Abstract

The invention relates to a high performance supported Pd catalyst for 2-ethyl anthraquinone hydrogenation and a preparation method thereof. The method includes: adopting cheap and easily available sodium metaaluminate as a precursor salt for preparation of a catalyst carrier, taking a Pluronic triblock copolymer P123 as the template agent, preparing a hydroxide precipitate by sol-gel method under an alkaline condition, then carrying out separation, vacuum drying, equivolumetric co-impregnation of Ba- and Fe- precursor salts, vacuum drying and roasting in order, thus obtaining Ba-Fe / gamma-Al2O3; further conducting equivolumetric co-impregnation of a Pd- precursor salt, ordinary drying and roasting, thus obtaining a Pd-Ba-Fe / gamma-Al2O3 catalyst. The prepared catalyst has high activity, high selectivity and high stability, and the hydrogenation efficiency is up to 9-10g H2O2 / L working fluid.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a high-performance supported Pd-catalyst for hydrogenation of 2-ethylanthraquinone and a preparation method thereof. Background technique [0002] At present, the methods used in the world to produce hydrogen peroxide include electrolysis, isopropanol oxidation and anthraquinone method. Among them, the electrolysis method consumes a lot of electricity, which leads to high production costs, is not conducive to large-scale industrial production, and is being gradually eliminated; the isopropanol oxidation method will produce a large amount of acetone, and the generated hydrogen peroxide is difficult to separate and purify; and anthraquinone The preparation method of hydrogen peroxide has low energy consumption, low cost and large production capacity, and has become the main method for producing hydrogen peroxide. The commonly used catalysts for the preparatio...

Claims

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Application Information

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IPC IPC(8): B01J23/89C01B15/023
Inventor 张春燕雷昊江燕蔡卫权
Owner WUHAN UNIV OF TECH
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