Active carbon supported ruthenium-based ammonia synthetic catalyst and preparation thereof

A technology of catalyst and activated carbon, which is applied in the field of ruthenium-based ammonia synthesis catalyst and its preparation, and achieves the effects of simple equipment, strong catalytic activity and high preparation efficiency

Inactive Publication Date: 2008-12-17
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no literature report on the preparation of ruthenium se...

Method used

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  • Active carbon supported ruthenium-based ammonia synthetic catalyst and preparation thereof
  • Active carbon supported ruthenium-based ammonia synthetic catalyst and preparation thereof
  • Active carbon supported ruthenium-based ammonia synthetic catalyst and preparation thereof

Examples

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preparation example Construction

[0012] Adopt the preparation step of citrate ruthenium chloride mixed impregnation method to be:

[0013] 1) Mix and dissolve ruthenium chloride citrate in water, the mass ratio of citric acid and ruthenium chloride in the mixed solution is 1:0.5~15, and the mass fraction of citric acid in the mixed solution is 1%~30% , the mass fraction of ruthenium is 1.5%~2.5%, the equal volume of mixed solution is impregnated with activated carbon; Taking the weight of activated carbon carrier as a benchmark, the content of ruthenium in the catalyst is 3.5~8% of the weight of activated carbon carrier;

[0014] 2) heat-treating the impregnated activated carbon, the heat-treatment temperature being 100-250°C;

[0015] 3) Reduction: Reducing the heat-treated activated carbon, using hydrogen-nitrogen mixed gas as the reducing gas, wherein the hydrogen is the reducing medium, the reduction temperature is 450°C, and the reduction time is 6 hours;

[0016] 4) Auxiliary loading: impregnating the ...

Embodiment 1

[0035]Get 0.22g ruthenium trichloride and 0.08g citric acid to mix and be dissolved in water (based on gac carrier weight, ruthenium and citric acid content are 4% of gac carrier weight), after citric acid and ruthenium chloride equal volume impregnation gac Dry the activated carbon under an infrared lamp, and then reduce it with a mixed gas with a volume ratio of hydrogen and nitrogen of 3:1 at 450 ° C. The reduced activated carbon is first loaded with the auxiliary agent Ba in equal volume, and then loaded with K, barium and potassium in equal volume. The weight content is respectively 4% and 12% of the weight of activated carbon carrier, and the precursors of barium and potassium are barium nitrate and potassium hydroxide respectively. The mass fraction of barium in the barium-containing solution is 0.5%-4%, and the mass fraction of potassium in the potassium-containing solution is 1%-8%.

[0036] Above also can be dissolved in water respectively with 0.22g ruthenium trichl...

Embodiment 2

[0039] Catalyst activity evaluation was carried out in a high-pressure activity testing device. The reactor is a fixed bed with an inner diameter of 14mm. The catalyst particles are 12-16 meshes, the bulk volume is 2ml, and the catalyst is packed in the isothermal zone of the reactor. The reaction gas is a mixture of nitrogen and hydrogen, and the ratio of hydrogen to nitrogen is 3:1. Catalyst activity is expressed by the volume percentage of ammonia in the reactor outlet gas.

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Abstract

The invention provides an active carbon-supported ruthenium ammonia synthesis catalyst and a preparation method thereof. The catalyst takes active carbon as a carrier and takes ruthenium as an active component; the components of the catalyst are (CA+Ru)-Ba-K/AC and CA-Ru-Ba-K/AC, wherein, CA represents citric acid and AC represents the active carbon; in preparation of the catalyst, the citric acid is selected to carry out the pretreatment of the active carbon and ruthenium chloride; one or more of barium nitrate, potassium hydroxide or potassium nitrate is or are selected as an assistant; the equivalent-volumetric impregnation method is adopted in the preparation method for preparing the catalyst. Compared with the sol-gel method or the oxidation method in the prior art, the invention adopts the citric acid method and has the advantages of simple technique, high preparation efficiency, little energy consumption, cheap raw material and less material consumption, thus being beneficial to greatly lowering the production cost. The devices required by the invention are simple, are easy to be operated, do not need to change the original devices and are easy to realize mass production. The catalyst prepared by the invention has good performance and strong catalytic activity.

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 and a preparation method thereof Background technique [0002] Ammonia synthesis catalyst is the most important catalyst in ammonia synthesis industry. In the 1980s and 1990s, people have studied the application of various oxides in ruthenium-based ammonia synthesis catalysts. Some early literatures introduced the research results of this part: the main precursor of ruthenium catalysts is Ru 3 (CO) 12 , RuCl 3 ,Ru(acac) 2 ,RuNO(NO 3 ) 3 , RuCl 3 etc., but the high input of noble metals in ruthenium catalyst hinders its wide application. The cost performance of various ruthenium precursors is significantly different, and the low-priced precursors have high cost performance. In general, ruthenium catalysts use Ru 3 (CO) 12 Or other chlorine-free precursors instead of ruthenium chlo...

Claims

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Application Information

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IPC IPC(8): B01J31/04C01C1/04
CPCY02P20/52
Inventor 魏可镁倪军王榕林建新俞秀金林炳裕
Owner FUZHOU UNIV
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