Ruthenium catalyst for synthesis ammonia and preparation method thereof

A ruthenium catalyst and a technology for synthesizing ammonia, applied in catalyst activation/preparation, ammonia preparation/separation, chemical instruments and methods, etc.

Inactive Publication Date: 2019-08-09
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the shortcomings of the existing rare earth oxide-supported ruthenium catalysts, the present invention provides a ruthenium-based catalyst for ammonia synthesis and a preparation method thereof to obtain a high-performance ruthenium catalyst

Method used

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  • Ruthenium catalyst for synthesis ammonia and preparation method thereof
  • Ruthenium catalyst for synthesis ammonia and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) Dissolve 6.46 g of lanthanum nitrate and 6.48 g of cerium nitrate in 10 mL of water to form an aqueous solution; then add 70 mL of 25% ammonia water to the aqueous solution and stir for 1 hour to form a precipitate. After the obtained precipitate was dried, the temperature was raised to 700 °C at 1 °C / min under an oxygen atmosphere, and calcined for 5 hours to obtain CeO with a La:Ce molar ratio of 1:1. 2 -La 2 o 3 composite oxides.

[0023] 2) The ruthenium nitrosyl nitrate was dried at 80 °C for 3 h and then dissolved into a methanol solution with a volume concentration of 75% to obtain a ruthenium precursor alcohol solution;

[0024] 3) The ruthenium precursor alcohol solution obtained in step 2) was impregnated into the lanthanum-cerium composite support prepared in step 1) at 30 °C for 1 h.

[0025] 4) Dry the sample prepared in step 3) at 100 °C for 0.5 h, and then reduce it with pure hydrogen at 400 °C for 2 h to obtain the ruthenium-based ammonia synthesis...

Embodiment 2

[0027] 1) Dissolve 4.16 g of lanthanum nitrate and 9.73 g of cerium nitrate in 10 mL of water to form an aqueous solution; then add 50 mL of potassium hydroxide solution (5mol / L) to the aqueous solution and stir for 1 hour to form a precipitate. After the obtained precipitate was dried, the temperature was raised to 600 °C at 10 °C / min under an oxygen atmosphere, and calcined for 4 hours to obtain CeO with a La:Ce molar ratio of 3:7. 2 -La 2 o 3 composite oxides.

[0028] 2) After drying ruthenium carbonyl at 60 °C for 6 h, it was dissolved in a methanol solution with a volume concentration of 60% to obtain a ruthenium precursor alcohol solution;

[0029] 3) The ruthenium precursor alcohol solution obtained in step 2) was impregnated into the lanthanum-cerium composite support prepared in step 1) at 30 °C for 2 h.

[0030] 4) Dry the sample prepared in step 3) at 150 °C for 1 h, and then 2 -Ar mixed gas was reduced at 550 °C for 4 h to obtain the ruthenium-based ammonia sy...

Embodiment 3

[0032] 1) Dissolve 5.54 g of lanthanum nitrate and 8.34 g of cerium nitrate in 10 mL of water to form an aqueous solution, then add 85 mL of 3 mol / L urea solution to the aqueous solution and stir for 0.5 hours to form a precipitate. After the obtained precipitate was dried, the temperature was raised to 500 °C at 5 °C / min under an oxygen atmosphere, and calcined for 4 hours to obtain CeO with a La:Ce molar ratio of 2:3. 2 -La 2 o 3 composite oxides.

[0033] 2) After drying ruthenium carbonyl at 80 °C for 3 h, it was dissolved in absolute ethanol solution to obtain ruthenium precursor alcohol solution;

[0034] 3) The ruthenium precursor alcohol solution obtained in step 2) was impregnated into the lanthanum-cerium composite support prepared in step 1) at 25 °C for 0.5 h.

[0035] 4) The sample prepared in step 3) was dried at 90 °C for 1 h, and then washed with 10% H 2-Ar mixed gas was reduced at 550 °C for 3 h to obtain the ruthenium-based ammonia synthesis catalyst, and...

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Abstract

The invention discloses a ruthenium catalyst for synthesis ammonia and a preparation method thereof, and relates to a synthesis ammonia ruthenium base catalyst adopting a CeO2-La2O3 composite oxide asa carrier and adopting ruthenium as an active component and a preparation method thereof. The catalyst is applicable to a synthesis ammonia reaction adopting nitrogen and hydrogen as raw materials. The preparation method of the catalyst comprises the steps that cerous nitrate and lanthanum nitrate are adopted as raw materials, a precipitant is added to obtain precipitates through a co-precipitation method, and then calcination is performed to prepare the CeO2-La2O3 composite oxide; after a chloride-free ruthenium compound is dried, the compound is dissolved into an alcoholic solution to obtain a ruthenium precursor alcoholic solution; the ruthenium precursor alcoholic solution is introduced into the composite oxide for dipping; after drying reduction, the ruthenium base synthesis ammoniacatalyst is obtained. Compared with existing cerium oxide and La-Ce mixed oxide loaded ruthenium base ammonia synthesis catalysts, the catalyst has the high ammonia synthesis activity, and the good application prospect.

Description

technical field [0001] The invention belongs to the technical field of fertilizer catalysts, and in particular relates to a ruthenium catalyst for ammonia synthesis and a preparation method thereof. Background technique [0002] Synthetic ammonia is an industry with large output and high energy consumption. The Haber-Bosch method currently used for industrial ammonia synthesis must produce ammonia under harsh conditions of high temperature (400–500 °C) and high pressure (15–30 MPa), making the ammonia synthesis industry a high energy-consuming and capital-intensive industry. Therefore, the development of new catalysts for efficient synthesis of ammonia under mild conditions (low temperature and low pressure) is the key to energy conservation and emission reduction in the ammonia synthesis industry. Developing new catalysts with low temperature and high activity, lowering the reaction temperature, increasing the equilibrium conversion rate and single-pass conversion rate of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/63B01J37/03B01J37/02B01J37/18C01C1/04
CPCB01J23/002B01J23/63B01J37/0201B01J37/031B01J37/18C01C1/0411Y02P20/52
Inventor 林炳裕李春艳倪军林建新江莉龙
Owner FUZHOU UNIV
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