A kind of preparation method of supporting type palladium-alumina catalyst

A catalyst, alumina technology, applied in the direction of physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, catalyst carrier, etc. Utilization, catalyst promotion effect is not optimal and other problems, to achieve good catalytic life, production process safety, improve activity and selectivity

Active Publication Date: 2019-11-29
福建省福大百阳化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patent uses a single promoter like the previous example, and the catalytic effect on the catalyst is not optimal, and its average pore radius of 10-14nm is not conducive to the inner surface of the catalyst for the gas-liquid-solid three-phase catalytic reaction. Fully utilize and affect the improvement of catalyst activity and selectivity

Method used

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  • A kind of preparation method of supporting type palladium-alumina catalyst

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preparation example Construction

[0020] Specifically, the preparation method of the supported palladium-alumina catalyst provided by the invention includes:

[0021] preparing an aluminum sol with an Al / Cl mass ratio of 1.0 to 1.5 and an Al content of 9 to 16 wt %;

[0022] Mixing the alkaline earth metal oxide precursor salt solution, the hexamethylenetetramine solution and the aluminum sol to form a premix solution, and keeping the temperature of the premix solution at 5-10°C;

[0023] The premixed solution is granulated by the oil column forming method to obtain aluminum rubber balls;

[0024] After the aluminum rubber balls are aged and washed, they are dried at 100-120°C for 4 hours, 200-300°C for 2-3 hours, 550°C for 3-4 hours, 960-1000°C for 3-4 hours, and cooled Obtain alumina carrier;

[0025] impregnating the alumina carrier with a precursor salt solution of an alkali metal oxide and then drying;

[0026] The dried alumina carrier is impregnated with metal palladium precursor solution, washed wit...

Embodiment 1

[0043] Take by weighing 60g purity ≥ 99.0wt% metal aluminum powder and 240g deionized water add in the 1000ml three-necked flask that has glass stirrer, thermometer, reflux condenser, by aluminum chloride weight ratio Al / Cl=1.4 / 1, (w / w) to the there-necked flask to add concentration of 15wt% hydrochloric acid, the stirring speed is controlled at 1000 rev / min, and the hydrogen generated in the reaction process is exported through the upper opening of the condensing tube. In the initial stage of the reaction between metal aluminum powder and hydrochloric acid, the temperature is rapidly raised to 50°C by external heating, and then the heating is stopped, and then the temperature of the reaction system is maintained at 95-100°C due to the heat release of the aluminum hydrolysis reaction. When the temperature cannot be maintained by the heat of reaction at the later stage of the reaction, the temperature of the system is maintained in the above range by external heating. After th...

Embodiment 2

[0053] Repeat the process of embodiment 1, difference is:

[0054] Change the precursor salt of alkaline earth metal oxide to Mg(NO 3 ) 2 . That is, when adding the precursor salt solution of the alkaline earth metal oxide to the aluminum sol, the Mg(NO 3 ) 2The aqueous solution was added to the aluminum sol and stirred evenly. Based on the weight of the alumina carrier, the loading amount of MgO on the carrier is about 2wt%.

[0055] Change the precursor salt of alkali metal oxide to NaHCO 3 . That is, with 30ml of NaHCO with a concentration of 0.05163mol / L 3 The aqueous solution impregnated 30 g of the macroporous spherical alumina carrier prepared above. Based on the weight of the alumina carrier, the Na on the carrier 2 The O loading is about 0.16wt%.

[0056] Change the metal palladium precursor solution to H 2 PdCl 4 solution. That is, pour 70ml of H with a concentration of 0.00958mol / L and a temperature of room temperature 2 PdCl 4 solution for impregnati...

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Abstract

The invention relates to a preparation method of a loaded type palladium-alumina catalyst, wherein the preparation method includes the steps: mixing a precursor salt solution of an alkaline earth metal oxide, a hexamethylenetetramine solution and an aluminum sol to prepare a premixed liquid; granulating the premixed liquid through an oil-column shaping method to obtain aluminum gel balls; aging and washing the aluminum gel balls, drying for 4 hours at the temperature of 100-120 DEG C, treating for 2-3 hours at the temperature of 200-300 DEG C, treating for 3-4 hours at the temperature of 550 DEG C, and treating for 3-4 hours at the temperature of 960-1000 DEG C, to obtain an alumina carrier; impregnating the alumina carrier with a precursor salt solution of an alkali metal oxide, and then drying; and impregnating the dried alumina carrier with a metal palladium precursor solution, washing with water, drying, and roasting for 3-5 hours at the temperature of 450-550 DEG C in an air atmosphere, to obtain the loaded type palladium-alumina catalyst. The prepared loaded type palladium-alumina catalyst has higher catalytic activity and selectivity in the premise of ensuring good catalytic life.

Description

technical field [0001] The invention relates to a method for preparing a metal catalyst, in particular to a method for preparing a palladium-alumina catalyst used in the production of hydrogen peroxide by a fixed-bed anthraquinone method. Background technique [0002] Anthraquinone method is currently the world's largest production of H 2 o 2 the most widely used method. Palladium on alumina or other platinum group metal catalysts are the most commonly used hydrogenation catalysts for this process. In order to continuously improve the performance of catalysts and use expensive platinum group metals more reasonably, people have done a lot of research work on the impregnation process of platinum group metals (such as palladium) and the relationship between the structure of the carrier and the performance of the catalyst for a long time. , selectivity and longevity have been discussed a lot. [0003] Anthraquinone hydrogenation reaction is a catalytic reaction involving gas...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44B01J21/04B01J35/10B01J32/00B01J35/08
CPCB01J21/04B01J23/44B01J35/08B01J35/1014B01J35/1061
Inventor 王榕
Owner 福建省福大百阳化工科技有限公司
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