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Composite oxide supported ruthenium-based ammonia synthesis catalyst and its preparation method

A technology for synthesizing composite oxides and ammonia, applied in the field of carrier, can solve the problem of low activity, and achieve the effect of high catalytic activity and good application prospect.

Inactive Publication Date: 2007-10-17
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the ruthenium-based ammonia synthesis catalysts supported by oxides generally have the problem of low activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The metered magnesium salt Mg(NO 3 ) 2 With alkaline earth metal barium salt Ba(NO 3 ) 2 The aqueous solution is mixed evenly, the ratio of the amount of magnesium to barium is 4:1, the concentration of magnesium salt is 2.3mol / L, the concentration of barium salt is 1.5mol / Lmol / L, and excessive NH 3 ·H 2 O, while applying ultrasound. The frequency of ultrasonic action is 25KHz, the power is 300W, and the time is 60min. After the ultrasonically applied product was left to stand and aged for 28 hours, the upper layer was poured out to clear the night, and after suction filtration, it was dried in an oven at 110°C for 24 hours, and then calcined in a muffle furnace at 400-500°C for 5 hours. Then use Ru with a content of 2wt% of the composite oxide in terms of Ru 3 (CO) 12 THF solution (concentration 0.035mol / L) was impregnated for 18 hours, dried in an oven at 110°C for 24 hours, then vacuumed at 350-650°C and then reduced by hydrogen for 5 hours. After cooling, the...

Embodiment 2

[0020] Repeat the process of embodiment 1, just do not apply ultrasonic effect, adopt Ru(Cl) 3 (Concentration: 0.15 mol / L) is used as the precursor of the active component Ru, and the dosage is adjusted so that the loading amount of Ru is 4wt%, and the reduction does not need to be vacuumized, and the reduction can be carried out by directly passing hydrogen gas. Prepared catalyst Ru / Ba-MgO at 10MPa, 475°C, 20000h -1 Next, its outlet ammonia concentration is 7.08%.

Embodiment 3

[0022] Repeat the process of Example 1, just change the power of ultrasonic action to 60W, and the Ru loading capacity that makes is 2wt% catalyst Ru / Ba-MgO at 10MPa, 425 ℃, 10000h -1 Next, its outlet ammonia concentration is 14.73%.

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PUM

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Abstract

The invention provides a ruthenium catalyst for ammonia synthesis with high activity which has composite oxide as a carrier, and a preparation method thereof. The ruthenium catalysts for ammonia synthesis comprises composite oxide as the carrier, metal Ru as an active component, wherein the capacity is 1-12 wt.% of the active carbon weight calculated based on Ru. The composite oxide is formed by magnesium and one or two or more than two nonferrous metal of: 1) alkaline earth but not magnesium; 2) alkali metals; 3) rare earth metal, wherein the ratio of magnesium and the nonferrous metal based on the amount of substance is 0.2-25:1. The catalyst of the invention has higher catalytic activity and better application prospects compared with the existing ruthenium catalyst for ammonia synthesis which has oxide as a carrier.

Description

(1) Technical field [0001] The invention relates to a composite oxide-supported ruthenium-based ammonia synthesis catalyst and a preparation method thereof, in particular to a catalyst which uses noble metal ruthenium as an active component, and uses magnesium and one of alkaline earth metals, alkali metals, and rare earth metals other than magnesium. Or a composite oxide of more than one non-ferrous metal as a carrier, a highly active ammonia synthesis catalyst that does not need additives or uses alkali metals and / or rare earth metals as additives, and a preparation method thereof. (2) Background technology [0002] The ruthenium-based ammonia synthesis catalyst has the characteristics of high activity at low temperature and low pressure, and is known as the second-generation ammonia synthesis catalyst after the molten iron catalyst. Among them, the ruthenium-based ammonia synthesis catalyst supported by activated carbon has been industrialized, but there are problems such...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/58C01C1/02
CPCY02P20/52
Inventor 霍超刘化章晏刚
Owner ZHEJIANG UNIV OF TECH
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