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Method for recovering ruthenium in activated carbon supported ruthenium catalyst

A technology of ruthenium catalyst and recovery method, which is applied in the direction of improving process efficiency, etc., can solve the problems of high price and low domestic production, and achieve the effects of low cost, high product recovery rate and simple operation

Active Publication Date: 2010-02-03
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the catalyst uses the noble metal ruthenium (Ru) as an active component, its price is expensive, and the domestic output is very small. Therefore, whether the ruthenium in the ruthenium catalyst can be recycled becomes a key factor for whether the ruthenium-based ammonia synthesis catalyst can realize industrialization and application. one of the keys

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Activated carbon-supported ruthenium catalyst (without additives) 10g was placed in a muffle furnace and calcined at 700°C for 6 hours to obtain 0.8504g of a gray-black mixture. Mix the gray-black mixture with 2 g of NaOH and NaNO in a mass ratio of 1:1 3 The solid mixture was packed in a crucible, placed in a muffle furnace at 250°C for 0.5 hours, alkali-fused at 630°C for 3 hours, and cooled. Transfer the cooled alkali melt (sodium perruthenate) to a 500mL beaker, add 100mL of deionized water at a temperature of 60°C to 95°C to dissolve, and the solution turns red. Use a Buchner funnel to filter out the water-insoluble matter, wash the insoluble matter with a small amount of deionized water at 50°C to 80°C, combine the washing liquid with the obtained red filtrate, and add an appropriate amount of ethanol dropwise, stir, and the red perruthenate That is, it turns into black ruthenium hydroxide precipitate. Wash with hot deionized water at 50°C to 80°C, and suction f...

Embodiment 2

[0048] Activated carbon-supported ruthenium catalyst (containing Ba, K and Mg additives) 15g, soaked in 75mL of hot water at a temperature of 50°C to 90°C for 3 hours, filtered to obtain the filtrate and filter residue, and then used 75mL of the filter residue at a temperature of 50°C to Soak in hot water at 80°C for 3 hours, and then filter to obtain filtrate and filter residue. Combine the filtrate obtained by two times of filtration, and drop in HNO with a concentration of about 20% 3 The pH value of the filtrate was adjusted to 6, and the water was evaporated to dryness to obtain 3.0531gKNO 3 , K recovery rate is 91.1%;

[0049] The obtained filter residue was soaked in 150 mL of 8% by mass hydrochloric acid solution at room temperature for 24 hours, and filtered to obtain a filtrate and a filter residue. Add appropriate amount of sulfuric acid to the filtrate to make BaSO 4 The precipitation is complete, and BaSO is obtained by filtering, washing and drying. 4 0.6477...

Embodiment 3

[0055] Repeat Example 2, but stir and dissolve the obtained ruthenium hydroxide precipitate with 36% hydrochloric acid at 80°C to 100°C to obtain RuCl 3 Aqueous solution, transfer this solution to a three-necked distillation flask, in a vacuum of about 4×10 4 Distilled under reduced pressure to dryness under the condition of Pa to obtain β-RuCl containing 37.5% ruthenium 3 .xH 2 O crystals were 1.7569 g, and the recovery rate of ruthenium was 91.1%.

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Abstract

The invention relates to a method for recovering an activated carbon supported ruthenium catalyst, which comprises the steps of: performing high-temperature roasting on an activated carbon supported ruthenium catalyst in which an alkali metal or alkaline-earth metal compound additive is not contained or is removed; performing high-temperature alkaline fusion on a roasted product; dissolving an alkaline fusion product in hot water with a temperature of between 60 and 95 DEG C to obtain a K2RuO4 or Na2RuO4 solution, adding ethanol or an alkaline solution into the K2RuO4 or Na2RuO4 solution to obtain a Ru(OH)4 precipitate; and drying the precipitate, or dissolving the precipitate by using strong acid, or using H2 to reduce the precipitate to obtain different ruthenium products. The method hasthe advantages that precious metal ruthenium can be efficiently recovered, the operation process of the recovery is safe, alkali metal and alkaline-earth metal additives can be synchronously recovered, and the form of the recovered product can be selected. The method has reliable technology, simple operation, low cost and no pollution.

Description

technical field [0001] The invention relates to a method for recovering ruthenium in a ruthenium catalyst supported by activated carbon of a noble metal catalyst. Background technique [0002] Activated carbon-supported ruthenium catalysts are widely used in the catalytic hydrogenation of petrochemicals, fine chemicals and other fields, especially since the successful development of activated carbon-supported ruthenium ammonia synthesis catalysts by British BP Company and American Kellogg Company in 1992, because the catalyst can be used in Efficient synthesis of ammonia under lower reaction temperature, pressure and other conditions is considered to be the second generation of ammonia synthesis catalysts after iron-based ammonia synthesis catalysts. However, because the catalyst uses the noble metal ruthenium (Ru) as an active component, its price is expensive, and the domestic output is very small. Therefore, whether the ruthenium in the ruthenium catalyst can be recycled ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B11/00
CPCY02P10/20
Inventor 王榕谢峰孔繁华张天釜张春光魏可镁俞秀金林建新倪军林炳裕
Owner PETROCHINA CO LTD
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