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Preparation method of sulfur-tolerant palladium-base catalyst

A catalyst and a palladium-based technology are applied in the field of preparation of sulfur-resistant palladium-based catalysts, which can solve the problems of low sulfur-resistant stability of the catalyst, complicated preparation methods, inconvenient operation, etc., and achieve shortened preparation time, simple technological process, and easy operation. handy effect

Inactive Publication Date: 2012-02-15
CHINA UNIV OF MINING & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The above supported catalyst Pd / γ-Al 2 o 3 The preparation method is complex, time-consuming, high energy consumption, high preparation cost, low sulfur resistance stability of the catalyst, inconvenient operation, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Prepare a concentration of 0.02 mol L -1 Ce(NO 3 ) 3 .6H 2 O (cerium nitrate) and Zr (NO 3 ) 4 ·5H 2 O (zirconium nitrate) aqueous solution, with Ce(NO 3 ) 3 .6H 2 O and Zr(NO 3 ) 4·5H 2 O mixed solution, Ce(NO 3 ) 3 .6H 2 O and Zr(NO 3 ) 4 ·5H 2 O is analytically pure with a purity of more than 99.5;

[0023] (2) Weigh γ-Al with a particle size of 0.6~0.9 mm 2 o 3 (activated alumina) carrier material 5 g, add it to 20ml step (1) to obtain Ce(NO 3 ) 3 .6H 2 O and Zr(NO 3 ) 4 ·5H 2 O mixed aqueous solution, dilute to 150 ml;

[0024] (3) Dilute the solution at 30 o Stir at C to make γ-Al 2 o 3 After the carrier material was impregnated for 2 h, at 60 o Evaporate to dryness at C to obtain impregnated γ-Al 2 o 3 Carrier material; the γ-Al 2 o 3 The nitrogen adsorption specific surface area of ​​the support material is 275 m 2 .g -1 Above, γ-Al 2 o 3 More than 90% of the pore diameter of the carrier is concentrated within 10 nm, and...

Embodiment 2

[0032] (1) Prepare a concentration of 0.02 mol L -1 Ce(NO 3 ) 3 .6H 2 O and Zr(NO 3 ) 4 ·5H 2 O aqueous solution with Ce(NO 3 ) 3 .6H 2 O and Zr(NO 3 ) 4 ·5H 2 O mixed solution; Ce(NO 3 ) 3 .6H 2 O and Zr(NO 3 ) 4 ·5H 2 O is analytically pure with a purity of more than 99.5;

[0033] (2) Accurately weigh γ-Al with a particle size of 0.6-0.9 mm 2 o 3 5 g of carrier material, add it to 20 ml step (1) to get Ce(NO 3 ) 3 .6H 2 O and Zr(NO 3 ) 4 ·5H 2 O mixed aqueous solution, dilute to 150 ml;

[0034] (3) Dilute the solution at 50 o Stir and impregnate at C for 2 h, 80 o Evaporate to dryness at C to obtain impregnated γ-Al 2 o 3 Carrier material; the γ-Al 2 o 3 The nitrogen adsorption specific surface area of ​​the support material is 275 m 2 .g -1 Above, γ-Al 2 o 3 More than 90% of the pore diameter of the carrier is concentrated within 10 nm, and the main peak appears between 4.4-5.0 nm, γ-Al 2 o 3 The surface acid content of the carrier i...

Embodiment 3

[0042] (1) Prepare a concentration of 0.02 mol L -1 Cerium nitrate and calcium nitrate aqueous solution, the molar ratio is 1:2 ratio configuration cerium nitrate and calcium nitrate mixed solution, both cerium nitrate and zirconium nitrate are analytically pure with a purity of more than 99.5;

[0043] (2) Accurately weigh γ-Al with a particle size of 0.6-0.9 mm 2 o 3 Add 5 g of carrier material to 20 ml of the mixed aqueous solution of cerium nitrate and calcium nitrate obtained in step (1), and dilute to 150 ml;

[0044] (3) Dilute the solution at 70 o After stirring and impregnating at C for 2 h, at 90 o Evaporate to dryness at C to obtain impregnated γ-Al 2 o 3 Carrier material; the γ-Al 2 o 3 The nitrogen adsorption specific surface area of ​​the support material is 275 m 2 .g -1 Above, γ-Al 2 o 3 More than 90% of the pore diameter of the carrier is concentrated within 10 nm, and the main peak appears between 4.4-5.0 nm, γ-Al 2 o 3 The surface acid content ...

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Abstract

The invention relates to a preparation method of a sulfur-tolerant palladium-base catalyst, belonging to the field of preparation of supported catalysts. The method comprises the following steps: mixing a gamma-Al2O3 carrier, of which the granularity is 0.6-0.9mm, with a cerous nitrate-zirconium nitrate water solution by an isometric impregnation method, impregnating at constant temperature while stirring, drying by distillation, sectionally roasting with microwaves to prepare the CeO2-ZrO2 / gamma-Al2O3 catalyst carrier; and mixing the CeO2-ZrO2 / gamma-Al2O3 catalyst carrier and a PdCl2 solution, impregnating at constant temperature while stirring, drying by distillation, and roasting with microwaves to obtain the Pd-CeO2-ZrO2 / gamma-Al2O3 catalyst. When being used for synthesizing dimethyl ether by a coal-base synthetic gas one-step method, the sulfur-tolerant Pd-CeO2-ZrO2 / gamma-Al2O3 catalyst has higher CO conversion rate and higher selectivity for the product dimethyl ether; and the invention obviously enhances the sulfur-tolerant stability and anti-carbon performance of the catalyst, optimizes the catalyst preparation technique, is simple to operate, and has the advantages of short time consumption, small energy consumption and good repetitiveness.

Description

technical field [0001] The invention relates to a preparation method of a sulfur-resistant palladium-based catalyst, in particular to a preparation method of a sulfur-resistant palladium-based catalyst under microwave roasting conditions, and belongs to the field of preparation of supported catalysts. Background technique [0002] In the past 10 years, the average annual growth rate of China's oil consumption has reached more than 10%. However, the annual growth rate of domestic self-extracted oil supply is only 1.7%. This contradiction between supply and demand has made China's dependence on foreign oil reach more than 50%. According to the analysis of authoritative departments, if a country's energy dependence exceeds 50%, there will be an energy crisis. Therefore, from the perspective of national security and energy strategy, the research and development of coal conversion and the production of various downstream products to replace petroleum raw materials and petroleum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/63
Inventor 孟献梁褚睿智魏贤勇宗志敏刘亚非张中彩
Owner CHINA UNIV OF MINING & TECH
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