Ruthenium system ammonia synthesis catalyst using graphitization activated carbon as carrier and preparation method of catalyst

An activated carbon and graphitization technology is applied in the field of ruthenium-based ammonia synthesis catalyst and its preparation, which can solve the problems of easy methanation and poor thermal stability of the catalyst, and achieve the effects of good stability, no decrease in activity and high ammonia synthesis activity.

Active Publication Date: 2014-10-08
FUZHOU UNIV ASSET MANAGEMENT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a kind of ruthenium series ammonia synthesis catalyst and preparation method thereof with graphitized activated carbon as the carrier, for solving the problem that the catalyst prepared by common preparation method is easy to methanate and has poor thermal stability, and prepares high Active and highly stable ruthenium-based ammonia synthesis catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Get 10 grams of graphitized activated carbon after the hole expansion and further heat treatment under hydrogen atmosphere. 10%, after the loading is completed, use 10wt% potassium hydroxide as a precipitant to precipitate ruthenium chloride. After the ruthenium chloride is completely precipitated, wash with deionized water to remove chloride ions, and then load barium nitrate additives. The content of barium is 10%. The loading process adopts equal volume impregnation and infrared lamp drying. A series of ammonia synthesis catalysts with different ratios of barium to ruthenium can be prepared by changing the atmosphere and treatment time of the carrier treatment, as well as changing the amount of ruthenium and barium in the catalyst. At a hydrogen-nitrogen ratio of 3:1, 400 ℃, 10000 h -1 , under the condition of 10MPa, the initial activity of the catalyst is 18.9%, 500 ℃, 10000 h -1 , After 10MPa heat resistance for 150 hours, the activity of the catalyst is 20.5%. ...

Embodiment 2

[0023] Repeat Example 1, except that the graphitized activated carbon heat treatment atmosphere after hole expansion is nitrogen, and the treatment temperature is 1200 ° C. A series of ammonia synthesis catalysts with different ratios of barium to ruthenium can be prepared by changing the atmosphere and treatment time of the carrier treatment, as well as changing the amount of ruthenium and barium in the catalyst. At a hydrogen-nitrogen ratio of 3:1, 400 ℃, 10000 h -1 , under the condition of 10MPa, the initial activity of the catalyst is 19.1%, 500 ℃, 10000 h -1 , After 10MPa heat resistance for 150 hours, the activity of the catalyst is 20.2%.

Embodiment 3

[0025] Repeat Example 1, except that the heat treatment atmosphere of graphitized activated carbon after hole expansion is ammonia gas, and the treatment temperature is 1200°C. A series of ammonia synthesis catalysts with different ratios of barium to ruthenium can be prepared by changing the atmosphere and treatment time of the carrier treatment, as well as changing the amount of ruthenium and barium in the catalyst. At a hydrogen-nitrogen ratio of 3:1, 400 ℃, 10000 h -1 , under the condition of 10MPa, the initial activity of the catalyst is 18.7%, 500 ℃, 10000 h -1 , After 10MPa heat resistance for 150 hours, the activity of the catalyst is 21.2%.

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Abstract

The invention discloses a ruthenium system ammonia synthesis catalyst using a graphitization activated carbon as a carrier and a preparation method of the catalyst. The ruthenium system ammonia synthesis catalyst is as shown in Ru-X-K/AC, wherein Ru represents that a precursor is a water-soluble chloride-free ruthenium complex or ruthenium chloride; X represents a metal adjuvant and is one or more of nitrate, acetate, carbonate, metallic oxide and hydroxide of rare-earth metal or alkaline-earth metal; AC represents a graphitization activated carbon carrier, and K represents a kalium adjuvant, namely potassium hydroxide, potassium nitrate, potassium acetate and potassium carbonate; the graphitization activated carbon which has the advantages of high specific surface area, high graphitization and low oxygen content is utilized as the carrier, and the ammonia synthesis catalyst is prepared through steps such as secondary graphitization of graphitization activated carbon, preparation of precursor and preparation of catalyst. The ruthenium system ammonia synthesis catalyst has the advantages that the graphitization activated carbon has large specific surface area and pore volume, enough place is provided for metal segregation, the graphitization degree is high, the oxygen content is low, the methanation resisting capacity of the catalyst is strong, and the stability is good.

Description

technical field [0001] The invention belongs to the technical field of ammonia synthesis catalyst preparation, and more specifically relates to a ruthenium-based ammonia synthesis catalyst with graphitized activated carbon as a carrier and a preparation method thereof. Background technique [0002] In the field of ammonia synthesis catalysts, ruthenium-based ammonia synthesis catalysts based on activated carbon or graphitized activated carbon as a carrier have high initial activity, but this type of catalyst is prone to methanation reaction and has poor thermal stability. The performance of the catalyst will be affected by long-term use. Influence. Early documents and patents aimed to improve the stability of ruthenium-based ammonia synthesis catalysts mainly by increasing the degree of graphitization of the carrier. However, if the degree of graphitization of the carrier is too high, it is difficult to expand the pores of the graphitized carrier. It is not conducive to the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/58C01C1/04
CPCY02P20/52
Inventor 魏可镁倪军林建新林炳裕
Owner FUZHOU UNIV ASSET MANAGEMENT CO LTD
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