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Ruthenium-based ammonia synthesis catalyst and its preparation method

A technology for ammonia synthesis and catalyst, applied in the field of new high-efficiency ammonia synthesis catalyst and its preparation, can solve the problems of high cost, high toxicity, complicated operation, etc., and achieve the effects of easy operation, favorable industrial production, and low preparation cost

Inactive Publication Date: 2007-10-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the disadvantages of complex operation, high cost, and high toxicity in the preparation of hydrogen reduction or hydrazine hydrate reduction process by ruthenium-based ammonia synthesis catalysts in the prior art, the present invention provides a catalyst that does not require hydrogen or hydrazine hydrate reduction steps, has high catalyst activity, and is suitable for Industrial application of ruthenium-based ammonia synthesis catalyst and preparation method thereof

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 3g of activated carbon and place it in hydrogen for 12 hours at 800°C, then use 30% HNO 3 30ml of the solution was refluxed in a water bath at 90°C for 8h, washed with deionized water until neutral, dried at 110°C for 4h, and degassed for 2h;

[0026] Take Ba(NO 3 ) 2 Add 5mL deionized water to 0.2284g to make a solution, add the above activated carbon, soak for 12h, dry at 110°C for 4h, and degas for 2h;

[0027] Immerse with 5 mL of ruthenium trichloride aqueous solution with a concentration of 0.0621 g / mL for 12 hours, and use a volume concentration of 2.5% NH 3 ·H 2 O 15mL was precipitated at 50°C for 12 hours, washed with deionized water, and washed with AgNO 3 The solution did not detect Cl - After washing, dry in an oven at 110°C for 8 hours, then pump for 5 hours.

[0028] Finally impregnate KNO with alkali metal salt concentration 0.2266g / mL 3 4.8mL of aqueous solution, impregnated at 50°C for 10h, dried at room temperature to 150°C for 10h, and the...

Embodiment 2

[0030] Repeat Example 1, except that the NH 3 ·H 2 O solution was changed to NaHCO at pH 8 3 solution. NaHCO 3 The mass concentration of the solution is 5%.

Embodiment 3

[0032] Repeat Example 1, just add NH 3 ·H 2 The O solution was changed to KOH with a pH of 12, and the solution mass concentration was 0.06%.

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PUM

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Abstract

The invention provides a ruthenium catalyst for ammonia synthesis and a preparation method thereof. The ruthenium catalysts for ammonia synthesis comprise active carbon as a carrier, metal ruthenium as active component, and alkali metal and alkaline-earth metal as cocatalyst. The active component ruthenium is loaded on the active carbon carrier in a Ru(OH)3 manner, wherein the capacity is 0.5-10 wt.% of the active carbon weight calculated based on Ru, and ratio of the alkaline-earth metal and Ru based on the amount of substance is 0.2-10:1. The catalyst of the invention has high noble metal dispersion degree, simple process and device, convenience for operation, short preparing time and high activity of the produced catalyst, thus facilitating for industrial production, in which reaction of the noble metal precursorcan be achieved without hydrogen or other reducing solution and the subsequent preparation step will not influence the distribution of the noble metal.

Description

(1) Technical field [0001] The invention relates to a catalyst with noble metal as active component and its preparation method, especially a novel high-efficiency ammonia synthesis catalyst with ruthenium as active component, alkali metal and alkaline earth metal as cocatalyst, activated carbon as carrier and its preparation method. (2) Background technology [0002] The ruthenium-based ammonia synthesis catalyst supported by activated carbon is usually prepared by the impregnation method, the active component and the cocatalyst are impregnated step by step, and the active component is reduced by hydrogen. For example, the catalyst preparation routes described in Chinese patents such as CN1270081A, CN1162219C and CN1481933 are to impregnate the carbon carrier and cocatalyst with a ruthenium-containing compound solution, and reduce the ruthenium-containing compound precursor to metal Ru with hydrogen. The patents of DE2748972, GB2034194 and other ruthenium-based ammonia synth...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J37/02C01C1/02
CPCY02P20/52
Inventor 韩文锋刘化章朱虹岑亚青柴海芳
Owner CHINA PETROLEUM & CHEM CORP
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