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Method for reclaiming ruthenium from ruthenium-containing waste liquid

A technology for waste liquid and concentrated liquid, applied in the field of ruthenium recovery, can solve the problems of inability to recover metal ruthenium and low recovery rate, and achieve the effects of low cost, high recovery rate and high efficiency

Active Publication Date: 2022-04-15
铜陵欣诺科新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the existing recovery methods for metal ruthenium in ruthenium-containing catalysts, most of them are for solid ruthenium-containing wastes, which are recovered by high-temperature calcination, but this recovery method cannot recover from such as deactivated p-cymene dichloride ruthenium dichloride Metal ruthenium is recovered from the waste liquid of ruthenium-containing homogeneous catalysts such as polymer catalysts
Another method is to recover metal ruthenium by reducing and recovering first, and then oxidizing and purifying, but the recovery rate of this method is low

Method used

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Effect test

Embodiment 1

[0041] A kind of method of present embodiment reclaims ruthenium from waste liquid containing ruthenium, and the steps are as follows:

[0042] (1) Concentrating 1L of deactivated (p-cymene) ruthenium chloride catalyst by evaporation under reduced pressure, adjusting the weight percent content of ruthenium to 1.2% (wherein, the molar weight of ruthenium is calculated as 0.076mol);

[0043] (2) Add 120 grams of sodium nitrite (1.74 mol) to the concentrated solution of step (1) for preliminary oxidation, heat to 90° C. and stir for 8 hours, then add sodium hydroxide to adjust the pH value of the reaction system to 8;

[0044] (3) Add 100mL perchloric acid (1.76mol) dropwise to the reaction solution after pH adjustment in step (2) to carry out secondary oxidation to obtain ruthenium tetroxide gas; absorb the ruthenium tetroxide gas with concentrated nitric acid to obtain 100mL Ruthenium nitrate solution; the calculation rate of ruthenium recovery is 92%.

Embodiment 2

[0046] A kind of method of present embodiment reclaims ruthenium from waste liquid containing ruthenium, and the steps are as follows:

[0047] (1) Concentrating 1L of deactivated (p-cymene) ruthenium chloride catalyst by evaporation under reduced pressure, adjusting the weight percent content of ruthenium to 1.2% (wherein, the molar weight of ruthenium is calculated as 0.076mol);

[0048] (2) Add 100 grams of potassium nitrite (1.17 mol) to the concentrated solution of step (1) for preliminary oxidation, heat to 90°C and stir for 8 hours, then add sodium hydroxide to adjust the pH value of the reaction system to 9;

[0049] (3) Add 150mL perchloric acid (2.64mol) dropwise to the reaction solution after pH adjustment in step (2) to carry out secondary oxidation to obtain ruthenium tetroxide gas; absorb ruthenium tetroxide gas with concentrated nitric acid to obtain 120mL Ruthenium nitrate solution; the calculation rate of ruthenium recovery is 95%.

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Abstract

The invention relates to a method for recovering ruthenium from waste liquid containing ruthenium. The method comprises the following steps: concentrating the ruthenium-containing waste liquid to prepare a concentrated liquid; the weight percentage of ruthenium in the concentrated liquid is not less than 1%; adding nitrite to the concentrated liquid for primary oxidation to prepare the first reaction liquid; adding perchloric acid to the first reaction liquid for secondary oxidation to prepare ruthenium tetroxide. The method can recover metal ruthenium from ruthenium-containing waste liquid, has high recovery rate, simple operation, low cost and high efficiency.

Description

technical field [0001] The invention relates to the technical field of metal recovery, in particular to a method for recovering ruthenium from ruthenium-containing waste liquid. Background technique [0002] Among the platinum group metals, metal ruthenium has been widely used in the field of organic synthesis due to its low price, special electrochemical properties and excellent catalytic performance. Ruthenium can accept the special spatial structure formed by many different kinds of complexes, so it can be applied in the field of chemical catalysis. [0003] p-Cymene dichloride ruthenium dimer (CAS: 52462-29-0) is a new homogeneous catalyst for platinum group metals, which has the advantages of wide range of substrates and high chiral selectivity, and is also an effective catalyst for alkylation. An important class of catalysts that need to be used in reactions such as hydrogenation reactions, hydrogenation reactions, and oxidation reactions. However, at present, the re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B11/00C22B7/00C01G55/00
CPCC22B11/00C22B7/009C01G55/004Y02P10/20
Inventor 刘相禹蓝仁峰
Owner 铜陵欣诺科新材料有限公司
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