Method for separating cobalt and manganese in cobalt and manganese wastes

A technology for separating cobalt and separating waste liquid is applied in the direction of improving process efficiency, which can solve the problems of cobalt and manganese entrainment, many extraction stages, and inability to separate cobalt and manganese, and achieves improved purity, simple process, and avoidance of cobalt recovery. rate reduction effect

Active Publication Date: 2018-04-13
JIANGSU UNIV OF TECH
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0005] The separation of cobalt and manganese by organic solvent extraction generally uses D2EHPA, but the direct use of D2EHPA to separate cobalt and manganese from a solution with high manganese and low cobalt requires a large amount of extractant, and there are many extraction stages, and there is also the entrainment of cobalt and manganese after extraction. , cannot achieve complete separation of cobalt and manganese

Method used

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  • Method for separating cobalt and manganese in cobalt and manganese wastes

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Embodiment 1

[0027] The cobalt-manganese waste treated in this embodiment is waste cobalt-manganese waste liquid produced in the production of PTA, wherein the content of cobalt is 29.55g / L, and the content of manganese is 67.66g / L. A kind of sulfidation precipitation-modified D2EHPA extraction combined technology of this embodiment separates cobalt and manganese in waste PTA cobalt-manganese catalyst, including the following steps:

[0028] (1), take 30g CoSO 4 ·7H 2 O salt was dissolved in 150ml deionized water and 150ml D2EHPA (V D2EHPA :V 煤油 =4) mixing, adjusting the pH to 4, and filtering to obtain Co-D2EHPA after the reaction;

[0029] (2) Take 50ml of cobalt-manganese waste liquid, adjust the pH value to less than 3.5 with sulfuric acid, heat in a water bath at 90°C for 30 minutes, and filter with suction to remove organic matter and iron ions in the waste liquid. The measured cobalt content in the waste liquid is 29.55g / L, and the manganese content is 67.66g / L. If there are ir...

Embodiment 2

[0035] The cobalt and manganese in the cobalt and manganese of a kind of sulfidation precipitation of this embodiment-modified D2EHPA extraction combined technology separation waste PTA cobalt-manganese catalyst are different from embodiment 1 in that:

[0036] The acid added in step 6) is sulfuric acid, and the pH of the control solution is 2.

[0037] The number of extraction stages in step 6) is 6, O / A: 1:3.

[0038] The recovery rate of cobalt in this experiment was 93%, and the separation ratio of cobalt and manganese reached 8000:1.

Embodiment 3

[0040] The cobalt and manganese in the cobalt and manganese of a kind of sulfidation precipitation of this embodiment-modified D2EHPA extraction combined technology separation waste PTA cobalt-manganese catalyst are different from embodiment 1 in that:

[0041] The sulfide used in step 2) and step 3) is sodium hydrosulfide, and the concentration of sodium hydrosulfide is 0.5mol / L.

[0042] The acid added in step 6) is sulfuric acid, and the pH of the control solution is 3.

[0043] The number of extraction stages in step 6) is 7, O / A: 1:2.

[0044] The recovery rate of cobalt in this experiment was 90%, and the separation ratio of cobalt and manganese reached 8000:1.

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Abstract

The invention discloses a method for separating cobalt and manganese in a waste cobalt-manganese catalyst by a vulcanization precipitation and modified D2EHPA extraction combined technology. The method comprises the following steps: 1, Co-D2EHPA is prepared; 2, the pH value of wastes is controlled to be less than or equal to 3.5; 3, impurities are removed; 4, a sulfide salt solution is prepared; 5, the sulfide salt solution is added into waste liquid, after adding is completed, the reaction liquid reacts for 0.5-3 hours, and after the reaction is ended, filtering is carried out obtain a cobaltsulfide precipitate and a manganese-containing solution respectively; and 6, a reducing agent is added into the manganese-containing solution to react, suction filtration is conducted after ending, precipitate is washed and dried after suction filtration to obtain a manganese precipitate, and the manganese recovery is completed. The obtained cobalt sulfide precipitates through filtration are dissolved by acid, modified Co-D2EHPA is added into the solution, and multi-stage extraction and reverse extraction is carried out, so that the obtained solution contains only cobalt.

Description

technical field [0001] The invention relates to a method for separating and recovering cobalt and manganese waste. Background technique [0002] Purified terephthalic acid (PTA) is an important organic raw material. The oxidation residues discharged during the production process mainly include p-xylene, terephthalic acid, isophthalic acid and phthalic acid and other organic substances and waste cobalt. manganese catalyst. Recycling the spent cobalt-manganese catalysts has important social and economic benefits. [0003] The waste cobalt-manganese catalyst has the characteristics of high manganese content and low cobalt content, and the commonly used cobalt-manganese separation method is generally not suitable for this kind of waste cobalt-manganese catalyst. [0004] Chinese patent document CN 105349789A (application number 201510839428.X) discloses a method for separating and recovering cobalt and manganese in high-manganese and low-cobalt waste materials with ammonia-sod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B23/00C22B47/00
CPCC22B7/006C22B23/0461C22B47/0009Y02P10/20
Inventor 刘维桥郑成邹超潘君丽周全法
Owner JIANGSU UNIV OF TECH
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