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Preparation method of hollow palladium catalyst microspheres

A palladium catalyst and a catalyst technology are applied in the field of preparation of hollow palladium catalyst microspheres, can solve problems such as easy deactivation of the catalyst, and achieve the effects of improving the encapsulation effect, the service life and the good catalytic effect.

Active Publication Date: 2021-06-11
浙江工业大学上虞研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the problems in the prior art, the present invention provides a method for preparing hollow palladium catalyst microspheres, which solves the problem that existing catalysts are easily deactivated, and utilizes the mesoporous structure of the silicon-oxygen layer to effectively prevent macromolecules from entering. At the same time, it does not affect the contact between hydrogen molecules and palladium particles, achieving a good catalytic effect and improving the service life of the catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method of hollow palladium catalyst microspheres, comprising the following steps:

[0019] Step 1, add ethyl cellulose into 1L ether and stir to form a solution, then add ammonium carbonate and continue stirring at constant temperature for 30min, and granulate to form granules; the concentration of the ethyl cellulose in the ether is 40g / L, stirring The speed is 1000r / min, the amount of ammonium carbonate added is 200% of the mass of ethyl cellulose, the temperature of constant temperature stirring is 30°C, the stirring speed is 500r / min, and the temperature of the granulation is 50°C;

[0020] Step 2, adding ethyl silicate to 1 L of anhydrous ether and stirring at low temperature to form a silicon ether solution, then evenly spraying on the surface of the particles, and drying at a constant temperature to form a first film; The concentration is 20g / L, the temperature of low temperature stirring is 5℃, and the stirring speed is 1000r / min; the spray volume ...

Embodiment 2

[0025] A preparation method of hollow palladium catalyst microspheres, comprising the following steps:

[0026] Step 1, add ethyl cellulose into 1L ether and stir to form a solution, then add ammonium carbonate and continue stirring at constant temperature for 60min, and granulate to form particles; the concentration of the ethyl cellulose in the ether is 70g / L, and stirring The speed is 2000r / min, the added amount of the ammonium carbonate is 600% of the mass of ethyl cellulose, the temperature of constant temperature stirring is 40°C, the stirring speed is 1000r / min, and the temperature of the granulation is 40°C;

[0027] Step 2, adding ethyl silicate to 1 L of anhydrous ether and stirring at low temperature to form a silicon ether solution, then evenly spraying on the surface of the particles, and drying at a constant temperature to form a first film; The concentration is 50g / L, the temperature of low temperature stirring is 10℃, and the stirring speed is 2000r / min; the sp...

Embodiment 3

[0032] A preparation method of hollow palladium catalyst microspheres, comprising the following steps:

[0033] Step 1, add ethyl cellulose into 1L ether and stir to form a solution, then add ammonium carbonate and continue stirring at constant temperature for 50min, and granulate to form granules; the concentration of the ethyl cellulose in the ether is 60g / L, stirring The speed is 1500r / min, the amount of ammonium carbonate added is 400% of the mass of ethyl cellulose, the temperature of constant temperature stirring is 35°C, the stirring speed is 800r / min, and the temperature of the granulation is 45°C;

[0034] Step 2, adding ethyl silicate to 1 L of anhydrous ether and stirring at low temperature to form a silicon ether solution, then evenly spraying on the surface of the particles, and drying at a constant temperature to form a first film; The concentration is 40g / L, the temperature of low temperature stirring is 8°C, and the stirring speed is 1500r / min; the spray volume...

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Abstract

The invention discloses a preparation method of hollow palladium catalyst microspheres, wherein the preparation method comprises the steps: adding ethyl cellulose into diethyl ether, uniformly stirring to form a dissolving solution, then adding ammonium carbonate, continuously stirring at a constant temperature for 30-60 min, and granulating to form particles; adding ethyl silicate into absolute diethyl ether, stirring at low temperature to form silyl ether liquid, then uniformly spraying the silyl ether liquid on the surfaces of particles, and drying at constant temperature to form a first surface film; adding ethyl silicate and palladium acetate into diethyl ether, uniformly stirring to form a mixed solution, then uniformly spraying the mixed solution on the first surface film, and drying at constant temperature to obtain a second surface film; uniformly spraying the silyl ether liquid on the second surface film, and drying at constant temperature to obtain a third surface film; and then putting the particles with the third surface film into a reaction kettle, standing for 2-5 hours to obtain a prefabricated catalyst, and carrying out reduction reaction to obtain the hollow palladium catalyst. The mesoporous structure of a silica layer can effectively prevent macromolecules from entering, contact between hydrogen molecules and palladium particles is not affected, and a good catalytic effect is achieved.

Description

technical field [0001] The invention belongs to the field of hydrogenation catalysis, and in particular relates to a preparation method of hollow palladium catalyst microspheres. Background technique [0002] The active metal components of the hydrogenation catalyst are in the oxidized state before use, and the active metal of the oxidized state catalyst needs to be activated before it has high catalytic activity. With the long-term operation of the catalyst, the deactivation of the hydrogenation catalyst exists. The current hydrogenation catalysts are mainly noble metal hydrogenation catalysts, which utilize the activity of the precious metal surface to achieve the hydrogenation effect. However, in the actual use process, the raw materials of the hydrogenation reaction are easily formed surface adhesion, resulting in the deactivation of the catalyst. SUMMARY OF THE INVENTION [0003] In view of the problems in the prior art, the present invention provides a method for pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J37/02B01J37/08B01J37/18B01J35/08B01J35/02B01J35/10C07C209/36C07C211/52B01J35/00
CPCB01J23/44B01J37/0215B01J37/082B01J37/0018B01J37/18C07C209/36B01J35/40B01J35/51B01J35/60C07C211/52
Inventor 许萌方标柯军梁
Owner 浙江工业大学上虞研究院有限公司
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