Synergic extraction agent for heavy rare earth elements and extraction separation method of synergic extraction agent

The technology of a heavy rare earth element and a separation method, which is applied in the field of rare earth extraction and separation, can solve the problems of saponification of an organic phase, difficulty in back extraction, etc., and achieve the effects of improving extraction capacity, increasing extraction capacity, and improving back extraction rate.

Inactive Publication Date: 2015-08-26
XIAMEN INST OF RARE EARTH MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Invention patent CN 201310043075 discloses an extractant for separating heavy rare earth elements, which is prepared by fully mixing two acidic phosphine extractants, C272 and P507, at a volume ratio of 1:0.5 to 1:2, and then diluted with kerosene. Solved the problem of difficult stripping of thulium, ytterbium and lutetium elements, but the organic phase still needs to be saponified

Method used

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  • Synergic extraction agent for heavy rare earth elements and extraction separation method of synergic extraction agent
  • Synergic extraction agent for heavy rare earth elements and extraction separation method of synergic extraction agent
  • Synergic extraction agent for heavy rare earth elements and extraction separation method of synergic extraction agent

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Experimental program
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Effect test

Embodiment 1～2

[0057] Synthesis of [P6,6,6,14][P507] and [P6,6,6,14][C272]

[0058] In a 125ml separating funnel, add 0.008mol of tetradecyltrihexylphosphonium chloride (referred to as [P6,6,6,14]Cl) to 60ml of methanol, and then add 75ml of anion exchange resin to obtain hydroxide Tetradecyltrihexylphosphonium (denoted as [P6,6,6,14]OH) solution. Add 0.008mol 2-ethylhexylphosphonic acid-mono-2-ethylhexyl ester (code P507) or bis(2,4,4-trimethylpentyl) to [P6,6,6,14]OH solution base) phosphinic acid (code C272), the resulting mixture was stirred at room temperature for 6h until the solution became neutral, methanol and water were spin-out at 70°C with a rotary evaporator, and the product was dried in a vacuum oven at 70°C After 12h, viscous liquid [P6,6,6,14][P507] or [P6,6,6,14][C272] was obtained. The yields all reached 95%.

Embodiment 3～4

[0060] Synthesis of [N4444][P507] and [N4444][C272]

[0061] In a 125ml separatory funnel, add 0.006mol tetrabutylamine bromide (denoted as [N4444]Br) to 40ml methanol, then add 75ml () anion exchange resin to obtain tetrabutylamine hydroxide (denoted as [N4444]OH) solution. Add 0.006mol P507 or C272 to this solution, and stir the resulting mixture at room temperature for 6h until the solution becomes neutral. Use a rotary evaporator to spin out methanol and water at 70°C, and dry the product in a vacuum oven at 70°C After 12h, viscous liquid [N4444][P507] or [N4444][C272] was obtained. The yields all reached 96%.

Embodiment 5～9

[0063] Preparation of organic phase: [P6,6,6,14][P507] was synthesized according to the method in Example 1, and [P6,6,6,14][C272] was purchased from Cytec Corporation of Canada. [P6,6,6,14][P507] and [P6,6,6,14][C272] of different compositions were mixed with toluene to form 5 ml of organic phase with concentrations of 0.0208 and 0.0052, 0.0156 and 0.0104, respectively , 0.013 and 0.013, 0.0104 and 0.0156, 0.0052 and 0.0208mol / L.

[0064] Preparation of raw material solution: Take 0.0030mol / L Lu(III) solution and add dilute hydrochloric acid to make Lu(III) concentration 4.5×10 -4 mol / L raw material solution, NaCl=0.5 mol / liter, pH=2.09.

[0065] The organic phase and the raw material solution are mixed at a volume ratio of 1:1, and extracted at room temperature, and the extraction stage is 1 stage. After the extraction was completed, the co-extraction coefficient R was calculated. Such as figure 1 As shown, the distribution ratio of the ionic liquid mixture after mixing ...

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Abstract

The invention relates to a synergic extraction agent for heavy rare earth elements and an extraction separation method of the synergic extraction agent. The synergic extraction agent comprises a component (a) and a component (b). The synergic extraction agent and thinner are mixed to form an organic phase to extract a heavy rear earth solution. In the extraction process, due to the fact that the two ionic-liquid-based extraction agents have a quite strong synergic extraction effect on heavy rare earth, the extraction capacity for heavy rare earth is obviously improved. Due to the fact that ionic liquid has a special phase shifting effect, a re-extraction agent more easily enters the organic phase, and the re-extraction rate is greatly increased. Multiple times of circulating saponification are not needed for the ionic liquid, and no ammonia-nitrogen waste water is generated in the extraction process.

Description

technical field [0001] The invention relates to the field of rare earth extraction and separation, in particular to a synergistic extraction agent for heavy rare earth elements and an extraction and separation method thereof. Background technique [0002] With the development of science and technology, the demand for rare earth materials related to heavy rare earths is increasing. For example, scintillation crystals used in positron tomographic scanners (PET) rely heavily on lutetium. Due to the extremely similar properties between heavy rare earth elements, separation is particularly difficult. [0003] In the prior art, the separation of heavy rare earths mainly adopts the extraction and separation method using 2-ethylhexylphosphonic acid-mono-2-ethylhexyl ester (code name P507) as the main extractant. The P507 extraction system has the following problems that need to be solved: ① P507 has a small separation coefficient for some rare earth elements; ② the concentration o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B59/00C22B3/40
CPCY02P10/20
Inventor 孙晓琦王艳良赵泽原
Owner XIAMEN INST OF RARE EARTH MATERIALS
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