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A kind of composite oxide supported ruthenium ammonia synthesis catalyst and preparation method thereof

A technology of composite oxides and catalysts, applied in the direction of metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problem of low specific surface area of ​​catalyst carrier and restriction of catalyst ammonia synthesis activity and other problems, to achieve good industrial application prospects, low-temperature and low-pressure ammonia synthesis activity improvement, and simple equipment

Inactive Publication Date: 2016-01-20
FUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, their preparation process needs to be realized at high temperature, which leads to a low specific surface area of ​​the catalyst carrier, which restricts the further improvement of the ammonia synthesis activity of the catalyst.

Method used

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  • A kind of composite oxide supported ruthenium ammonia synthesis catalyst and preparation method thereof
  • A kind of composite oxide supported ruthenium ammonia synthesis catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1 (comparative example)

[0035] Mg(NO 3 ) 2 ·6H 2 O: A mixture of citric acid: ethylene glycol with a molar ratio of 1:2:4 was dissolved in an appropriate amount of distilled water to obtain a colorless clear viscous liquid. The solution was slowly heated in a water bath at 80°C for 4h to evaporate excess water, and then heated at a constant temperature of 90°C for 12h to promote the gelation of the mixture. Finally, the obtained gel was calcined at 300°C for 1 h to obtain the precursor, and then calcined at 750°C for 3 h to obtain the MgO support material. The active component ruthenium was impregnated into the carrier by equal volume impregnation method, and then reduced with absolute ethanol. The mass fraction of the active component Ru in the carrier was 4%, and the catalyst Ru / MgO was obtained. The catalyst is at 3MPa and the space velocity is 10000h -1 The activity of the catalyst is measured under the following conditions, and the activity of the...

Embodiment 2

[0036] Embodiment 2 (comparative example)

[0037] Zr(NO 3 ) 4 . 5H 2 O: Ba(NO 3 ) 2 : A mixture of citric acid: ethylene glycol molar ratio of 1:1:2:4 was dissolved in an appropriate amount of distilled water to obtain a colorless clear viscous liquid. The solution was slowly heated in a water bath at 80°C for 4h to evaporate excess water, and then heated at a constant temperature of 90°C for 12h to promote the gelation of the mixture. Finally, the obtained gel was calcined at 300 °C for 1 h to obtain the precursor, and then calcined at 750 °C for 3 h to obtain BaZrO 3 carrier material. The active component ruthenium is impregnated into the carrier by the equal volume impregnation method, and then reduced with absolute ethanol. The mass fraction of the active component Ru in the carrier is 4%, and the obtained catalyst is Ru / BaZrO 3 . The catalyst is at 3MPa and the space velocity is 10000h -1 The activity of the catalyst is measured under the following conditions, ...

Embodiment 3

[0039] Prepare 1:1 mixed oxide carrier by ultrasonic mixing method: weigh 19.3g of Mg(NO 3 ) 2 . 6H 2 O is put into a beaker, and an appropriate amount of distilled water is added to obtain a colorless and clear solution of magnesium nitrate, and the concentration of the substance is 1mol / L (NH 4 ) 2 CO 3 The solution was slowly added to the above magnesium nitrate solution, stirred at 40°C for 0.5h, after fully reacting, aged in the mother liquor for 1h, and weighed 3g of the BaZrO prepared in Example 2 3 Put the solid powder into the mortar and grind it, then add it to the above milky white suspension, and apply ultrasonic action for 40 minutes to make it evenly dispersed. After standing, aging, and centrifugal separation, the product after ultrasonic action is placed in an oven Dry at 90°C for 12 hours to obtain a bulk mixed carrier precursor. Finally, the obtained mixed carrier precursor was calcined at 300°C for 1 h to obtain the precursor, and then calcined at 750°...

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Abstract

The invention discloses a composite oxide-supported ruthenium ammonia synthesis catalyst and a preparation method thereof, belonging to the technical field of fertilizer catalysts. The ruthenium-based ammonia synthesis catalyst uses metal ruthenium as an active component, MgO and perovskite BaZrO3 composite oxide as a carrier, and the mass ratio of MgO and BaZrO3 in the composite oxide is 1:5-5:1, and the activity is The component uses K2RuO4 as the precursor, and is directly impregnated into the carrier material, and the loading amount is 2%-10% of the carrier weight in terms of Ru. The preparation method of the invention is simple, the equipment is simple, no auxiliary agent is needed, and the prepared catalyst has good low-temperature and low-pressure activity and high stability.

Description

technical field [0001] The present invention relates to a composite oxide supported ruthenium ammonia synthesis catalyst, in particular to a kind of metal ruthenium as an active component, MgO and perovskite BaZrO 3 A highly active ammonia synthesis catalyst with a composite oxide as a carrier and a preparation method thereof. The invention belongs to the technical field of fertilizer catalysts and is applied to the synthesis of ammonia from the mixed gas of hydrogen and nitrogen. Background technique [0002] The second-generation Ru-based catalysts following the iron catalysts have higher ammonia synthesis activity under mild conditions, and are an important direction in the research of ammonia synthesis catalysts. Among them, the ruthenium-based ammonia synthesis catalyst supported by graphitized activated carbon materials has achieved industrial application in the 1990s. Chinese patents CN101362080A and CN101053834A disclose an ammonia synthesis catalyst with ruthenium...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/58
Inventor 林建新马运翠齐衍超倪军林炳裕江莉龙魏可镁
Owner FUZHOU UNIV
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