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Active carbon loading ruthenium ammonia synthesis catalyst and preparation method thereof

A technology of activated carbon and catalyst, which is applied in the field of new ammonia synthesis catalyst and its preparation, can solve the problems of slow reaction speed, incomplete salt, loss of ruthenium, etc., and achieve the effect of improving stability, reducing loss and stable performance

Inactive Publication Date: 2009-02-11
福州开发区科盛催化材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN1385238A uses hydrazine hydrate instead of hydrogen for reduction, but the treatment of ammonia-containing waste liquid after reduction is very troublesome
However, since from Ru 3+ Precipitate to get Ru(OH) 3 The reaction speed is slow, and it takes 2 to 30 hours at room temperature to 100°C, and soluble Ru 3+ It is difficult for the salt to deposit completely and uniformly on the surface of the carrier, resulting in uneven distribution of ruthenium content on the activated carbon carrier, and the preparation process is easy to cause part of the ruthenium loss, so it is difficult to ensure the quality consistency of catalysts prepared in different batches, and at the same time, the precipitation time is relatively long. Q greatly affects the production efficiency of the catalyst

Method used

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  • Active carbon loading ruthenium ammonia synthesis catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Take 500 grams of BET specific surface area is 1050m 2 / g of coconut shell charcoal, placed in a washing tower and washed with flowing pure water until the pH value = 7; the activated carbon taken out was dried in a drying oven at 120°C for 4 hours, and then placed in a high-temperature oven under the protection of an inert gas Treat at 1800-1900°C for 2 hours, after the temperature is lowered to room temperature, take it out and place it in a hole-enlarging furnace, and feed it with oxygen, CO 2 The mixed gas composed of nitrogen, nitrogen and water vapor is treated at 380-460°C for 16 hours and then cooled to room temperature for use.

[0044] Get the ruthenium trichloride aqueous solution 200ml that ruthenium concentration is 2.5% (w / w), add concentration and be 30% H 2 o 2 25ml of the solution, stir well at room temperature ~ 95°C and let it stand still, then the Ru in the solution +3 converted to Ru +4 .

[0045] Get 100g of the above-mentioned activated carbo...

Embodiment 2

[0047] The process of Example 1 was repeated except that the impregnation order of each material was different. That is, the treated activated carbon support was first impregnated with RuCl 4 solution and precipitated with KOH solution, washed with deionized water and dried, impregnated with 100ml of oxalic acid solution with a concentration of 12%, dried at 60-120°C with an infrared lamp, impregnated with Ba(NO 3 ) 2 The aqueous solution is based on the weight of the carbon carrier, and the Ba content of the carrier is controlled to be about 4wt%. It is dried at 60-120°C with an infrared lamp or an oven, and the obtained sample is impregnated with a KOH solution at room temperature. The amount of KOH is the same as in Example 1. The sample Drying at 60-120° C. with an infrared lamp can obtain the activated carbon-supported ruthenium-based ammonia synthesis catalyst.

Embodiment 3

[0049] The procedure of Example 2 was repeated, except that oxalic acid was not used.

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Abstract

The invention discloses an active carbon-loaded ruthenium ammonia-synthesis catalyst and a preparation method thereof, pertaining to catalysts for fertilizers. The active carbon-loaded ruthenium ammonia-synthesis catalyst takes active carbon as a carrier, metal ruthenium as an active ingredient, and alkali metal and alkaline-earth metal as auxiliary agents, the active ingredient, namely, ruthenium, is loaded on the carrier, that is, the active carbon, in the form of Ru(OH)4 or RuO2.2H2O, and the load is calculated by Ru, with the weight of the active ingredient being 2 percent to 9 percent of the weight of the active carbon; the alkaline-earth metal is loaded on the carrier (the active carbon) in the form of a nitrate or an oxalate, and the loaded quantity is calculated by the alkaline-earth metal, with the mass ratio between the alkaline-earth metal and the ruthenium being 0.3-5:1 and the amount-of-substance ration between the alkali metal and the ruthenium being 2-10. The method is quick and simple for operation, and the prepared catalyst has stable performance and high activity and is applicable to industrial production.

Description

technical field [0001] The invention relates to a novel ammonia synthesis catalyst using hydrogen and nitrogen to synthesize ammonia in the ammonia synthesis industry in the field of chemical fertilizers and a preparation method thereof, in particular to an activated carbon-supported ruthenium-based ammonia synthesis catalyst and a preparation method thereof. Background technique [0002] The ruthenium-based ammonia synthesis catalyst supported by activated carbon is usually prepared by impregnation method, and the active components and cocatalysts are impregnated step by step. Usually the active components are reduced by hydrogen (such as Chinese patents CN1621148A, CN1270081A, etc.). Chinese patent CN1385238A uses hydrazine hydrate instead of hydrogen for reduction, but the treatment of ammonia-containing waste liquid after reduction is very troublesome. Chinese patent CN101053834A discloses that the RuCl 3 Take Ru(OH) 3 The preparation technology of the supported ruthe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/02B01J21/18C01C1/04
CPCY02P20/52
Inventor 王榕魏可镁林建新俞秀金倪军林炳裕瞿胜谢峰莫崇望
Owner 福州开发区科盛催化材料有限公司
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