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Preparation method of spherical micron-size gamma-aluminium oxide carrier for preparing hydrogen peroxide by anthraquinone hydrogenation

An aluminum oxide, quasi-spherical technology, applied in the preparation of organic compounds, quinone preparation, chemical instruments and methods, etc., can solve problems such as complicated steps, and achieve the effects of low preparation cost, high specific surface area, and high hydrogenation efficiency

Inactive Publication Date: 2018-07-27
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method needs to prepare carbon black first, and then carry out hydrothermal treatment, and the steps are a bit cumbersome.

Method used

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  • Preparation method of spherical micron-size gamma-aluminium oxide carrier for preparing hydrogen peroxide by anthraquinone hydrogenation
  • Preparation method of spherical micron-size gamma-aluminium oxide carrier for preparing hydrogen peroxide by anthraquinone hydrogenation
  • Preparation method of spherical micron-size gamma-aluminium oxide carrier for preparing hydrogen peroxide by anthraquinone hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) 0.036mol anhydrous glucose and 0.018mol Al(NO 3 ) 3 9H 2 O was dispersed in 90 mL of deionized water (the molar ratio of the two was 2:1), ultrasonicated for 10 min (ultrasonic power 100 W), 10 mL of 0.2 mol / L urea solution was added as a precipitant, stirred for 30 min, and hydrothermally heated at 180 °C 8h, filter the obtained black product, and alternately wash it with deionized water and absolute ethanol until the filtrate is clear, and dry it in a blast drying oven at 80°C for 8h to obtain fine and fluffy colloidal carbon / AlOOH composite material powder body. The powder was calcined in an air atmosphere at 550°C for 3h (heating rate 2°C / min) to obtain γ-Al 2 o 3 Powder.

[0036] (2) With the above γ-Al 2 o 3 The powder is used as a carrier, and the auxiliary component Ni is loaded by an equal-volume impregnation method, and 0.0594g Ni (NO 3 ) 2 ·6H 2 O is dissolved in 0.6g carrier corresponding to the saturated water absorption, and the obtained solu...

Embodiment 2

[0041] (1) 0.072mol anhydrous glucose and 0.018mol Al(NO 3 ) 3 9H 2 O was dispersed in 90 mL of deionized water (the molar ratio of the two was 4:1), ultrasonicated for 10 min (ultrasonic power 100 W), and 10 mL of 0.2 mol / L urea solution was added as a precipitant, stirred for 30 min, and hydrothermally heated at 180 °C 8h, filter the obtained black product, and alternately wash the filtrate with deionized water and absolute ethanol until the filtrate is clear, and dry it in a blast drying oven at 80°C for 8h to obtain a fine and fluffy colloidal carbon / AlOOH composite material powder . The powder was calcined in an air atmosphere at 550°C for 3h (heating rate 2°C / min) to obtain γ-Al 2 o 3 carrier.

[0042] (2) With the above γ-Al 2 o 3 The powder is the carrier, and the auxiliary component Fe is loaded by the equal-volume impregnation method, and 0.1298g Fe (NO 3 ) 3 9H 2 O is dissolved in 0.6g carrier corresponding to the saturated water absorption, and the obtain...

Embodiment 3

[0047] (1) 0.144mol anhydrous glucose and 0.018mol Al(NO 3 ) 3 9H 2 O was dispersed in 90 mL of deionized water (the molar ratio of the two was 8:1), ultrasonicated for 10 min (ultrasonic power 100 W), and 10 mL of 0.2 mol / L urea solution was added as a precipitant, stirred for 30 min, and hydrothermally heated at 180 °C 8h, filter the obtained black product, and alternately wash the filtrate with deionized water and absolute ethanol until the filtrate is clear, and dry it in a blast drying oven at 80°C for 8h to obtain fine and fluffy colloidal carbon / AlOOH composite powder . The powder was calcined in an air atmosphere at 550°C for 3h (heating rate 2°C / min) to obtain γ-Al 2 o 3 carrier.

[0048] (2) With the above γ-Al 2 o 3 The powder is used as a carrier, and the auxiliary component Zn is loaded by an equal volume impregnation method, and 0.1373g Zn (NO 3 ) 2 ·6H 2 O is dissolved in 0.6g carrier corresponding to the saturated water absorption, and the obtained so...

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Abstract

The invention relates to a preparation method of spherical micron-size gamma-aluminium oxide carrier for preparing hydrogen peroxide by anthraquinone hydrogenation. The preparation method comprises the following steps: dispersing anhydrous glucose and Al(NO3)3.9H2O into deionized water, carrying out ultrasonic treatment for 10min, adding a urea water solution, heating the mixed solution at 180 DEGC for 8 hours, alternately washing the hydrothermal product with deionized water and ethanol until the filtrate is clear; drying the filter cake in a blower drying oven at 80 DEG C for 8 hours to obtain a colloid carbon / AlOOH complex, and carrying out calcination in an air atmosphere of 550 DEG C for 3 hours to obtain spherical micron-size gamma-Al2O3 powder, taking the powder as a carrier, supporting an active component Pd- by adopting a incipient wetness method, then carrying out washing, drying and calcination to obtain a Pd / gamma-Al2O3 catalyst, wherein before the Pd- is supported, auxiliary agents such as Ni-, Fe- and Zn- can also be supported by adopting the same incipient wetness method of the Pd-. The Pd / gamma-Al2O3 catalyst exhibits high hydrogenation efficiency in an anthraquinone hydrogenation reaction, and the hydrogenation efficiency can reach 11.30g H2O2 per liter of a working fluid.

Description

technical field [0001] The present invention relates to mesoporous Al 2 o 3 The preparation method of microsphere and its application in the preparation of anthraquinone method to produce H 2 o 2 The application in palladium catalyst belongs to the field of preparation of catalyst carrier and catalyst, and provides a kind of hydrogenation of anthraquinone to produce H 2 o 2 Use spherical micron grade γ-Al 2 o 3 The preparation method of the carrier. Background technique [0002] h 2 o 2 The synthesis methods of the compound include acid hydrolysis peroxide method, electrolysis method, isopropanol method, anthraquinone method and direct synthesis method of hydrogen and oxygen. At present, palladium catalyst fixed bed anthraquinone method is widely used in China to produce H 2 o 2 , the anthraquinone method mainly includes three processes such as hydrogenation, oxidation and extraction. The hydrogenation process is the control process of the entire production proces...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J23/60B01J35/10B01J37/03B01J37/08B01J37/02C07C50/18C07C46/00
CPCC07C46/00B01J23/60B01J23/8906B01J23/892B01J37/0201B01J37/031B01J37/082B01J37/088B01J35/613B01J35/633B01J35/647C07C50/18
Inventor 蔡卫权王昕杨志超
Owner WUHAN UNIV OF TECH
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