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Synthesis of novel efficient extractant oxamide for light rear earth element and extraction separation method

An extractant and light rare earth technology, which is applied in the field of oxamide extractant for separating light rare earth, can solve the problems of unsatisfactory separation effect, unstable properties, easy emulsification, etc.

Inactive Publication Date: 2018-06-15
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the raw material of naphthenic acid is easy to obtain and the cost of use is low, the composition is complex, and the property is unstable and easy to emulsify during long-term use, so the separation effect is not ideal

Method used

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  • Synthesis of novel efficient extractant oxamide for light rear earth element and extraction separation method
  • Synthesis of novel efficient extractant oxamide for light rear earth element and extraction separation method

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0006] Example 1.N, the preparation of N-dihexyl oxalic acid (HA6)

[0007] 10ml of monoethyl oxalyl chloride was dissolved in 30ml of dichloromethane, and 30ml of a dichloromethane solution of di-n-butylamine (15ml) and triethylamine (20ml) was added dropwise in an ice-water bath. After 1 hour, spin the reaction solution to dryness, add 20ml of ethanol, 20ml of 0.2M sodium hydroxide aqueous solution, reflux for 5 hours, add hydrochloric acid to acidify, evaporate most of the solvent, then add 50ml of dichloromethane, wash with water three times, separate the phases with anhydrous The organic phase was dried over sodium sulfate, concentrated and purified by silica gel chromatography (dichloromethane as eluent) to obtain a light brown viscous liquid with a purity of 92% and a yield of 76%.

[0008] 1H NMR (CDCl3 / TMS) δ / ppm: 1.20 (s, 1H), 3.32-1.25 (m, 12H), 0.85 (m, 6H).

example 2

[0009] Example 2.N, the preparation of N-diisooctyl oxalic acid (HA8)

[0010] 10ml of monoethyl oxalyl chloride was dissolved in 30ml of dichloromethane, and 30ml of a dichloromethane solution of diisooctylamine (20ml) and triethylamine (20ml) was added dropwise in an ice-water bath. After 1 hour, spin the reaction solution to dryness, add 20ml of ethanol, 20ml of 0.2M sodium hydroxide aqueous solution, reflux for 5 hours, add hydrochloric acid to acidify, evaporate most of the solvent, then add 50ml of dichloromethane, wash with water three times, separate the phases with anhydrous The organic phase was dried over sodium sulfate, concentrated and purified by silica gel chromatography (dichloromethane as eluent) to obtain a light brown viscous liquid with a purity of 90% and a yield of 75%.

[0011] 1 HNMR (CDCl 3 / TMS) δ / ppm: 3.06-3.56 (m, 4H), 1.63 (d, 2H), 1.24 (s, 16H), 0.87 (t, 12H)

example 3

[0012] Example 3.HA6, HA8 compare the extraction performance of light rare earth

[0013] Extraction process: prepare a 0.005M single rare earth hydrochloric acid solution; dissolve the extractant in the diluent to prepare a 0.06M solution; ±1℃)

[0014] Shake in a water-bath shaker for 60 minutes until the extraction is balanced; after phase separation, measure the concentration of rare earth ions in the water phase, and then calculate the content of rare earth in the organic loading phase through material balance, so as to obtain the extraction rate. The results are shown in Table 1.

[0015] Table 1. Extraction studies of light rare earths with dialkyl oxamide extractants.

[0016]

[0017] Remarks: 1. Distribution ratio: the ratio of the concentration of metal ions in the organic phase to the concentration of metal ions in the aqueous phase at extraction equilibrium;

[0018] 2. The separation coefficient β represents the ratio of the distribution ratio of two differe...

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Abstract

The invention relates to synthesis of a novel efficient extractant oxamide for a light rear earth element and an extraction separation method. The extraction separation method is applied in extractionand separation of light rear earth elements. The extractant has excellent extraction performance on light rear earth elements, the separation coefficient of adjacent rear earth elements in toluene can be up to 3.2, and the half-extraction pH1 / 2 in n-heptane can decrease to 1.2. In addition, the extractant is simple to synthesize and can be obtained through two conventional reaction steps, synthesis conditions are mild and industrial production is convenient, and therefore the extractant is a potential extractant for light rear earth elements.

Description

technical field [0001] The invention discloses a novel extractant used in hydrometallurgy and its extraction method, in particular an oxamide extractant for separating light rare earth. Background technique [0002] Rare earths have excellent magnetic, optical and electrical properties due to their unique electronic layer structure, and are widely used in more than 10 fields such as metallurgical machinery, petrochemical industry, electronic information, energy and environmental protection, national defense and military industry, and high-tech materials. However, due to the close chemical properties of rare earth elements, the separation of rare earth elements has always been one of the most challenging issues in the rare earth industry. [0003] Carboxylic acid extractants are a very important category of rare earth extractants, and are currently mainly used to separate yttrium from other rare earths. Naphthenic acid is a representative of this type of extractant. Although...

Claims

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Application Information

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IPC IPC(8): C22B3/32C22B59/00C07C231/02C07C231/14C07C233/56
CPCC07C231/02C07C231/14C07C233/56C22B59/00C22B3/32Y02P10/20
Inventor 郭创龙支永刚
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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