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Method for recovering ruthenium from benzene hydrogenation prepared cyclohexene catalyst

A catalyst and cyclohexene technology, applied in the field of ruthenium recovery, can solve problems such as multi-organic waste water, and achieve the effects of simple operation, low production cost, and improved raw material utilization rate

Inactive Publication Date: 2018-08-14
LUXI CATALYST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] CN 104787811 A patent discloses a method for recovering ruthenium and zirconium in the catalyst for hydrogenation of benzene to cyclohexene. The method uses ethanol and hydrazine to reduce the materials after alkali fusion, and uses organic solvents in the process to produce more organic wastewater

Method used

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Examples

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Effect test

Embodiment 1

[0033] 1) Weigh 100g of the spent catalyst, add 1mol / L hydrochloric acid, stir and react at 40°C for 1h, filter, wash until the solution is neutral, put the filter cake in an oven for drying, and recover the filtrate and washing liquid by conventional methods zinc. 2) Grind the filter cake obtained in step 1), add 26g of potassium nitrate and 6g of potassium hydroxide, mix well, place in a muffle furnace, and roast at 600°C for 2h. 3) dissolving the molten material with hot water, filtering and washing to obtain a potassium ruthenate solution. 4) Add sulfuric acid to the potassium ruthenate solution, adjust the pH to 3, and add sodium hypochlorite dropwise until no golden yellow gas is generated in the solution. 5) The generated ruthenium tetroxide enters the four-stage 1:1 hydrochloric acid absorption solution through the buffer device for absorption to obtain a reddish-brown ruthenium trichloride hydrochloric acid solution, and the tail gas is passed into 15% sodium hydroxi...

Embodiment 2

[0035] 1) Weigh 100g of the spent catalyst, add 1mol / L sulfuric acid, stir and react at 40°C for 1h, filter, wash until the solution is neutral, put the filter cake in an oven for drying, and recover the filtrate and washing liquid by conventional methods zinc. 2) Grind the filter cake obtained in step 1), add 26g of sodium nitrate and 6g of sodium hydroxide, mix well, place in a muffle furnace, and roast at 600°C for 2h. 3) dissolving the molten material with hot water, filtering and washing to obtain a potassium ruthenate solution. 4) Add sulfuric acid to the potassium ruthenate solution, adjust the pH to 3, and add sodium hypochlorite dropwise until no golden yellow gas is generated in the solution. 5) The generated ruthenium tetroxide enters the four-stage 1:1 hydrochloric acid absorption solution through the buffer device for absorption to obtain a reddish-brown ruthenium trichloride hydrochloric acid solution, and the tail gas is passed into 15% sodium hydroxide solutio...

Embodiment 3

[0037] 1) Weigh 100g of the spent catalyst, add 1mol / L sulfuric acid, stir and react at 40°C for 1h, filter, wash until the solution is neutral, put the filter cake in an oven for drying, and recover the filtrate and washing liquid by conventional methods zinc. 2) Grind the filter cake obtained in step 1), add 26 g of sodium nitrate and 6 g of sodium hydroxide, mix well, place in a muffle furnace, and roast at 600° C. for 2 h. 3) dissolving the molten material with hot water, filtering and washing to obtain a potassium ruthenate solution. 4) Add sulfuric acid to the potassium ruthenate solution, adjust the pH to 3, and dropwise add the sodium chlorate solution until no golden yellow gas is generated in the solution. 5) The generated ruthenium tetroxide enters the four-stage 1:1 hydrochloric acid absorption solution through the buffer device for absorption to obtain a reddish-brown ruthenium trichloride hydrochloric acid solution, and the tail gas is passed into 15% sodium hyd...

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Abstract

The invention discloses a method for recovering ruthenium from a benzene hydrogenation prepared cyclohexene catalyst. The method comprises the following steps that alkali fusion treatment is carried out on the catalyst by adopting a conventional method, and thermal dissolution by adopting water is carried out; then an oxidizing agent is added to carry out distillation reaction, and the generated ruthenium tetroxide gas is absorbed by an acidic solution; and the absorption liquid is subjected to concentrated and drying to obtain a ruthenium trichloride product. According to the method, the distillation reaction liquid is returned and used for the alkali fusion heat treatment step without wastewater discharge; and excessive chlorine generated in the distillation reaction is recovered by adopting a dilute alkali liquid, and the generated hypochlorite is returned and used for distillation reaction, so that the utilization rate of raw materials is improved.

Description

technical field [0001] The invention relates to a method for recovering ruthenium in a catalyst for preparing cyclohexene from benzene hydrogenation, and belongs to the technical field of recovering precious metals from catalysts. Background technique [0002] Ruthenium trichloride is one of the most important compounds of ruthenium. It can react with many reagents to form a variety of complexes. It is also the starting material for the preparation of many ruthenium complexes. It can also be used as the polymerization, isomerization, As a catalyst for hydrogenation and other reactions, ruthenium trichloride can also be used for the determination of sulfite, the manufacture of chlororuthenate, and as an electrode coating material, etc. my country's ruthenium resources are scarce, and most of them depend on imports. Ruthenium is a non-renewable resource. How to recover and recycle it from spent catalysts is of great significance for sustainable development, resource conservat...

Claims

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Application Information

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IPC IPC(8): C22B7/00C22B11/00
CPCC22B7/007C22B11/048Y02P10/20
Inventor 曹全福郭喜文胡大春张照飞
Owner LUXI CATALYST
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