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A kind of pyridyl phosphoramide compound and its preparation method and application as nickel-cobalt extractant

A pyridyl phosphoramide and compound technology, which is applied in the field of pyridyl phosphoramide compounds, can solve the problems of poor selectivity and difficulty in applying nickel-cobalt extraction and separation, and achieves the effects of enhanced selectivity, favorable for large-scale production and mild reaction conditions

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

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Problems solved by technology

[0004] Aiming at the defects in the prior art that P204 has too strong ability to chelate metal ions, poor selectivity, and is difficult to be applied to the extraction and separation of nickel and cobalt, the purpose of the present invention is to provide a pyridine compound containing pyridyl, amino and phosphate groups at the same time. Phosphoramide compound, its use with P204 can significantly enhance the selective chelation of P204 to nickel and cobalt, and can be used for the extraction and separation of nickel and cobalt from other metal impurities

Method used

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  • A kind of pyridyl phosphoramide compound and its preparation method and application as nickel-cobalt extractant
  • A kind of pyridyl phosphoramide compound and its preparation method and application as nickel-cobalt extractant
  • A kind of pyridyl phosphoramide compound and its preparation method and application as nickel-cobalt extractant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Synthesis of intermediate product p-pyridine formaldehyde acetal 2-ethylhexylamine

[0047] In a 250 ml round bottom flask, pyridine-4-carbaldehyde (21.38 g, 0.2 mol), 2-ethylhexylamine (25.90 g, 0.2 mol) and 1.0 g of p-toluenesulfonic acid were dissolved in absolute ethanol (150 mL) , stirred and refluxed in an oil bath at 80°C for 8h, tracked and detected by TLC until the reaction was complete, and added 1.54g of anhydrous K 2 CO 3 , continue to react for 30min, cooled to room temperature, concentrated under reduced pressure, washed with water, extracted three times with 100ml ethyl acetate, collected the organic phase, dried over anhydrous magnesium sulfate, filtered, removed the organic solvent by rotary evaporation in vacuum, and dried in vacuum. Yield: 41.24 g. Yield 94.50%.

Embodiment 2

[0049] Synthesis of extractant α-phosphoramidate (abbreviated as EHPYEP)

[0050] In a 500ml round bottom flask, the product obtained in the previous step (43.66g, 0.2mol) and diethyl phosphite (27.65g, 0.2mol) were reacted in an oil bath at 80°C for 5h without solvent, followed by TLC to detect whether the reaction was complete , cooled to room temperature, transferred to a 500ml separatory funnel, washed with acid 3 times, washed with alkali 3 times, washed with water until neutral, extracted with ethyl acetate, dried over anhydrous magnesium sulfate, filtered, combined organic phases, vacuum rotary evaporation to remove acetic acid Ethyl ester was dried in vacuo overnight to obtain wine red liquid. Yield: 68.63 g. Yield 96.34%. The structure is characterized as follows: IR(KBr)ν / cm -1 : 3417, 3026, 2928, 1596, 1561, 1463, 1387, 1245, 1027, 968, 876, 792, 575; 1 H NMR (500MHz, CDCl 3 )δ H : 8.57(d, J=4.0Hz, 2H), 7.37(dd, J=9.3, 7.5Hz, 2H), 4.14–3.93(m, 5H), 2.35(s, 2H)...

Embodiment 3

[0052] Water phase feed liquid: simulated feed liquid, feed liquid containing Ni 1.187g / L, Co 1.163g / L, Mg 1.309g / L, Mn1.204g / L, pH 5.81;

[0053] Organic phase: use sulfonated kerosene as diluent, extractant is single extractant EHPYEP, concentration setting: 0.10, 0.15, 0.20, 0.,25mol / L.

[0054] Extraction: The ratio between the organic phase and the feed liquid (O / A) was 2:1, the mixing time was 5 minutes, the oscillation frequency was 200r / min, and the extraction was carried out at room temperature. The experimental results are shown in Table 1 below.

[0055] It can be seen from Table 1 that the single extractant EHPYEP has poor ability to extract nickel, cobalt, magnesium and manganese, and almost has no extraction effect.

[0056] The extraction effect of table 1 single extractant EHPYEP

[0057] EHPYEP Concentration 0.10M 0.15M 0.20M 0.25M Ni extraction rate 1.85％ 1.86％ 2.53％ 2.87％ Extraction rate of Co 1.32％ 1.45％ 1.21％ 1.83％ Ext...

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Abstract

The invention discloses a pyridinylphosphoramide compound and its preparation method and its application as a nickel-cobalt extractant. Pyridine-4-formaldehyde and alkyl primary ammonia are subjected to an amaldehyde condensation reaction to generate a Schiff base intermediate. Addition reaction between Schiff base intermediate and dialkyl phosphite to obtain pyridyl phosphoramide compound. The preparation method has the advantages of environmental protection, mild conditions, simple process, short process, etc.; the synthesized pyridyl phosphoramide compound is combined with P204 as a nickel-cobalt synergistic extractant for the extraction and separation of cations containing nickel, cobalt, and magnesium manganese. It has the characteristics of high extraction capacity, short phase separation time, excellent extraction and stripping performance, etc., and has a good industrial application prospect.

Description

technical field [0001] The present invention relates to a pyridyl phosphoramide compound and its preparation and use, in particular to a pyridyl phosphoramide compound containing a pyridine ring, a phosphite group and an amino group, and a pyridyl phosphoramide compound combined with P204 as a nickel-cobalt The application of the synergistic extractant in the extraction, separation and purification of impurity metals such as nickel and cobalt, magnesium and manganese belongs to the field of hydrometallurgy. Background technique [0002] Nickel-cobalt is an important strategic metal in my country and has a wide range of uses in the fields of industry, national economy and life. With the increasing depletion of high-grade high-quality nickel and cobalt ore resources, the improvement of environmental protection requirements, and the need for resource recycling, from low-grade nickel oxide ore (such as laterite nickel ore) and nickel-cobalt secondary resources (such as nickel-co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/58C22B3/40C22B23/00
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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