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Method for recovering ruthenium catalyst carried by active carbon

A technology of ruthenium catalyst and recovery method, which is applied in chemical recovery, chemical instruments and methods, catalyst regeneration/reactivation, etc., to achieve the effects of improving economic and ecological benefits, reducing the consumption of heavy metal resources, and simple operation

Inactive Publication Date: 2006-12-06
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there is no recovery method for the ruthenium-based ammonia synthesis catalyst supported by activated carbon at home and abroad, and the present invention fills this gap

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 24.0 g of spent ruthenium catalyst (containing Ba and K promoters) supported on activated carbon was soaked in 10% hydrochloric acid solution by mass percentage for 12 hours, and filtered to obtain filtrate and filter residue. Add appropriate amount of dilute sulfuric acid to the filtrate to make BaSO 4 The precipitation is complete, and BaSO is obtained by filtration and drying. 4 2.1423g, the Ba recovery rate is 87.8%; the remaining filtrate is evaporated to dryness to obtain KCl 4.8485g, and the K recovery rate is 77.7%.

[0036] Ruthenium recovery: the filter residue was calcined in a muffle furnace at 800°C for 10 hours to obtain 0.9882 g of a gray-black mixture. Mix the gray-black mixture with 2 g of KOH and KNO at a mass ratio of 1:1 3 The solid mixture was packed in a crucible and placed in a muffle furnace for alkali fusion at 650°C for 1 hour. After the alkali melt is cooled, it is washed with cold water to neutrality, and then filtered to obtain a filter ...

Embodiment 2

[0039] Activated carbon-supported ruthenium catalyst (containing Ba promoter) 20g was soaked with 10% dilute hydrochloric acid solution for 16 hours, and filtered to obtain filtrate and filter residue. Add appropriate amount of dilute sulfuric acid to the filtrate to make BaSO 4 The precipitation is complete, and BaSO is obtained by filtration and drying. 4 2.1737g, Ba recovery rate is 89.8%. Other operations are the same as the ruthenium recovery step in Example 1. The recovery rate of ruthenium was 93.05%.

Embodiment 3

[0041] Activated carbon-supported ruthenium catalyst (containing K promoter) 20g was soaked in 10% dilute hydrochloric acid solution by mass percentage for 6 hours, and filtered to obtain filtrate and filter residue. The filtrate was dried to obtain KCl4.5737g, and the K recovery rate was 81.8%. Other operations are the same as the ruthenium recovery step in Example 1. The recovery rate of ruthenium was 95.55%.

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Abstract

A recovering process for the activated carbon carried Ru catalyst not containing the compound of alkali metal or alkali-earth metal includes such steps as calcining at 600-1000 deg.C for 2-20 hr to obtain gray mixture, mixing it with KOH and KNO3, holding the temp at 300-950 deg.C for 105 hr, cooling, dissolving in hot water at 50-90 deg.C to obtain K2RuO4 solution, adding sodium hypochlorite and concentrated sulfuric acid, distilling to generate RuO4 gas, absorbing it by strong acid solution, and distilling to obtain Ru salt.

Description

(1) Technical field [0001] The invention relates to the field of recovery of precious metal catalysts, in particular to the recovery of activated carbon-supported ruthenium catalysts. (2) Background technology [0002] Since the successful development of ruthenium-based ammonia synthesis catalyst by British BP Company and American Kellogg Company in 1992, in-depth research and development of ruthenium-based ammonia synthesis catalyst has been carried out at home and abroad. Compared with iron-based catalysts, the main advantage of ruthenium-based ammonia synthesis catalysts is their high activity, which can catalyze ammonia synthesis reactions at lower temperatures and pressures. Therefore, the ruthenium-based ammonia synthesis catalyst is considered to be the second-generation ammonia synthesis catalyst after the iron-based ammonia synthesis catalyst. Activated carbon-supported ruthenium catalysts are also widely used in catalytic hydrogenation in petrochemical, fine chemi...

Claims

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Application Information

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IPC IPC(8): B01J38/68B01J38/64B01J38/02C01G55/00C22B11/00
CPCY02P20/584
Inventor 刘化章岑亚青韩文峰朱虹杨丽仙李烽潘红志陆磷姜文海
Owner ZHEJIANG UNIV OF TECH
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