A nickel-cobalt synergistic extractant and its method for extracting and separating nickel-cobalt from impurities

An extractant, nickel-cobalt technology, applied in the field of metal extractant, nickel-cobalt synergistic extractant, can solve the problems of poor selectivity and achieve the effects of short phase separation time, clear oil-water interface, and good solubility

Active Publication Date: 2019-09-27
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the defects in the DA acid extractant used in the extraction, separation and recovery of nickel and cobalt in the prior art, the purpose of the present invention is to provide a synergistic extractant comprising pyridyl phosphoramide compound and dialkylnaphthalene sulfonic acid, which can Nickel-cobalt has a strong selective coordination effect, which can be used for the extraction and separation of nickel-cobalt and other metal impurities, and overcomes the defect of poor selectivity of single dialkylnaphthalene sulfonic acid in the nickel-cobalt extraction process

Method used

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  • A nickel-cobalt synergistic extractant and its method for extracting and separating nickel-cobalt from impurities
  • A nickel-cobalt synergistic extractant and its method for extracting and separating nickel-cobalt from impurities
  • A nickel-cobalt synergistic extractant and its method for extracting and separating nickel-cobalt from impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Synthesis of intermediate product p-pyridinecarboxaldehyde 2-ethylhexyleneamine

[0055] In a 250ml round bottom flask, dissolve pyridine-4-carbaldehyde (21.38g, 0.2mol), 2-ethylhexylamine (25.90g, 0.2mol) and 1.0g p-toluenesulfonic acid in absolute ethanol (150mL) , Stirring and refluxing in 80℃ oil bath for 8h, TLC tracking and detecting until the reaction is complete, adding 1.54g anhydrous K 2 CO 3 , Continue the reaction for 30 minutes, cool to room temperature, concentrate under reduced pressure, wash with water, and extract three times with 100 ml of ethyl acetate. Collect the organic phase, dry with anhydrous magnesium sulfate, filter, remove the organic solvent by vacuum rotary evaporation, and dry in vacuum. Yield: 41.24g. The yield was 94.50%.

Embodiment 2

[0057] Synthesis of extractant α-phosphoramidate (abbreviated as EHPMPD)

[0058] In a 500ml round-bottomed flask, the product obtained in the previous step (182.85g, 0.84mol), diethyl phosphite (162.77g, 0.84mol) were reacted in an oil bath at 80°C without solvent for 5h, followed by TLC to check whether the reaction was complete , Cooled to room temperature, transferred to a 1000ml separatory funnel, acid washed 3 times, alkaline washed 3 times, washed with water to neutral, extracted with ethyl acetate, dried with anhydrous magnesium sulfate, filtered, combined the organic phases, vacuum rotary evaporated to remove acetic acid The ethyl ester was dried under vacuum overnight to obtain a wine-red liquid. Yield: 326.56g. The yield was 94.52%. The structure is characterized as follows: IR (KBr) ν / cm-1: 3417, 3026, 2930, 1596, 1561, 1463, 1382, 1246, 1025, 898, 575; 1H NMR (500MHz, CDCl3) δ 8.59 (d, J =5.4Hz, 2H), 7.38 (d, J = 4.1 Hz, 2H), 4.14 (dd, J = 14.3, 7.1 Hz, 1H), 4.06–...

Embodiment 3

[0060] Aqueous material liquid: simulated material liquid, the material liquid contains Ni 1.187g / L, Co 1.163g / L, Mg 1.309g / L, Mn1.204g / L, Ca 0.463g / L, pH 5.81;

[0061] Organic phase: Use sulfonated kerosene as the diluent, and the extraction agent is the single extractant EHPMPD, and the concentration is set to: 0.10, 0.15, 0.20, 0.25mol / L.

[0062] Extraction: The above-mentioned organic phase and the feed liquid are compared (O / A) 2:1, the mixing time is 5 min, the shaking frequency is 200 r / min, and the extraction is performed at room temperature. The experimental results are shown in Table 1 below.

[0063] It can be seen from Table 1 that the single extractant EHPMPD has very poor ability to extract nickel, cobalt, magnesium, manganese and calcium, and there is almost no extraction effect.

[0064] Table 1 Extraction effect of single extractant EHPMPD

[0065]

[0066]

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Abstract

The invention discloses a nickel-cobalt synergistic extractant and a method for extracting and separating nickel-cobalt from impurities. The synergistic extractant includes pyridyl phosphoramide compound and dialkylnaphthalene sulfonic acid; The aqueous solution containing nickel ions and / or cobalt ions and impurity metal ions is extracted, and the extracted organic phase is back-extracted to obtain a solution containing nickel ions and / or cobalt ions from which impurity metal ions are removed; the synergistic extractant can realize Separation of nickel and cobalt and effective separation of nickel and cobalt from impurity metal ions (such as magnesium, manganese, calcium, etc.), and has the advantages of high selectivity and fast phase separation.

Description

Technical field [0001] The invention relates to a metal extractant, in particular to a nickel-cobalt synergistic extractant composed of a pyridyl phosphoramide compound and dialkylnaphthalene sulfonic acid, and also relates to a synergistic extractant in nickel and cobalt and magnesium, calcium, manganese, etc. The application of impurity extraction separation and purification belongs to the field of hydrometallurgy. Background technique [0002] At present, the cobalt and nickel scraps in secondary resources can be divided into five categories according to industry classification, namely: stainless steel alloy scraps, cobalt-containing nickel catalyst scraps, permanent magnetic metal scraps, waste batteries, and scraps of defective corners. Among them, the waste with the highest content of cobalt and nickel is used batteries. The random disposal of used batteries not only causes environmental pollution to the ecosystem, but also wastes scarce metal resources. Therefore, the se...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/40C22B23/00
CPCC22B23/0453C22B3/409
Inventor 曹佐英何冬梅张贵清李青刚曾理关文娟
Owner CENT SOUTH UNIV
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