Extraction separation method for heavy rare earth elements

A technology of heavy rare earth elements and a separation method, which is applied in the field of extraction and separation of heavy rare earth elements, can solve the problems of high concentration of heavy rare earth elements stripping acid, difficulty in obtaining high-purity heavy rare earth products, and small separation coefficient of rare earth elements, etc. Good interface phenomenon, saving acid and alkali consumption, high selectivity

Inactive Publication Date: 2014-12-10
XIAMEN INST OF RARE EARTH MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The following problems need to be solved in the P507 extraction system: ① P507 has a small separation coefficient for some rare earth elements, such as Gd / Eu, Er / Y, Lu / Yb, etc.; The low stripping rate of Lu makes it difficult to obtain high-purity heavy rare earth products. In order to make the product qualified, the number of extraction stages can only be greatly increased

Method used

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  • Extraction separation method for heavy rare earth elements
  • Extraction separation method for heavy rare earth elements
  • Extraction separation method for heavy rare earth elements

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Synthesis of ionic liquid-based extractant: take 0.6 mole of methyltri-n-hexylammonium bromide [N1666][Br], dissolve it in 1L of methanol, add a strong basic anion exchange resin, exchange bromide ions into hydroxide ions, and obtain hydrogen Methyltri-n-hexylammonium oxide [N1666][OH]. Add 0.6 moles of 2,4,4-trimethylpentylphosphonic acid-mono-2,4,4-trimethylpentyl ester (code P572) dropwise into the generated [N1666][OH] to complete deprotonation to obtain ionic liquid-based extractant [N1666][P572].

[0059] Preparation of organic phase: Mix [N1666][P572] with sulfonated kerosene to form an organic phase. The volume ratio of ionic liquid-based extractant to sulfonated kerosene in the organic phase is 0.1:0.9.

[0060] Preparation of raw material solution: take Tm-Yb-Lu enrichment, add dilute hydrochloric acid, and prepare raw material solution, its composition is ΣREO=0.02 mol / liter, NaCl=0.5 mol / liter, pH=2.2, Tm:Yb:Lu = 10:80:10.

[0061] Single-stage extraction...

Embodiment 2～8

[0071] Preparation of loaded organic phase: Mix [N1666][P572] prepared in Example 1 with sulfonated kerosene to form an organic phase. The volume ratio of ionic liquid-based extractant to sulfonated kerosene in the organic phase is 0.02:0.98. with LuCl 3 Extraction was performed with a loading of 0.53 g / L in the organic phase.

[0072] Preparation of back-extraction solution: prepare a series of hydrochloric acid as back-extraction solution with concentrations of 0.05, 0.1, 0.125, 0.15, 0.2, 0.25 and 0.3 mol / liter.

[0073] Single-stage stripping: Mix the loaded organic phase with a volume ratio of 1:1 and the stripping liquid, and strip at room temperature, and the stripping stage is 1 stage. After the extraction was completed, the stripping rate was calculated. The result is as figure 1 as shown, figure 1 It is the stripping result diagram provided by Examples 2-8 of the present invention. Depend on figure 1 It can be seen that the ionic liquid-based extractant is easy...

Embodiment 9-12

[0075] Synthesis of ionic liquid-based extractant: Take 0.6 mole of tetrabutylammonium bromide [N4444][Cl], dissolve it in 0.4 liter of ethanol, add dropwise 305 milliliters of 2 moles of potassium hydroxide-ethanol solution per liter, stir for 0.5 hours and then filter Precipitation of potassium chloride gave tetrabutylammonium hydroxide [N4444][OH]. Mix [N4444][OH] with 2,3,4-trimethylpentylphosphonic acid-mono-2,3,4-trimethylpentyl ester (code P573) to complete deprotonation to obtain ionic liquid Base extractant [N4444] [P573].

[0076] Prepare the organic phase: mix [N4444][P573] with sulfonated kerosene to form the organic phase, and the molar concentration of the ionic liquid-based extractant in the organic phase is 0.03 moles per liter.

[0077] Preparation of raw material solution: take GdCl separately 3 , TbCl 3 , DyCl 3 , HoCl 3 , ErCl 3 0.0045 moles per liter, adjust pH 2.2.

[0078] Single-stage extraction: The organic phase and the raw material solution ar...

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Abstract

The invention provides an extraction separation method for heavy rare earth elements. The extraction separation method comprises the following steps: mixing rare earth concentrates with inorganic acid to obtain a raw material liquid; using an organic phase comprising an extraction agent and a thinning agent to extract rare earth elements in the raw material liquid, wherein the extraction agent is a difunctional ionic liquid extraction agent, and the difunctional ionic liquid extraction agent comprises one deprotonated acid phosphine negative ion of quaternary ammonium positive ions and quaternary phosphonium positive ions. According to the method provided by the invention, in the extraction process, due to the fact that the quaternary ammonium positive ions or the quaternary phosphonium positive ions in the difunctional ionic liquid extraction agent are distributed in an organic phase and a water phase, the competitive effect of ionic liquid positive ions and rare earth ions is strengthened, and the extraction separation coefficient of heavy rare earth is improved. Moreover, in the subsequent extraction process, due to specific phase transfer effect of ions, a stripping agent is easier to enter the organic phase, and the reextraction rate is greatly improved.

Description

technical field [0001] The invention relates to the technical field of extraction, in particular to an extraction and separation method of heavy rare earth elements. Background technique [0002] Rare earth elements refer to the lanthanide elements with atomic number 57-71 and yttrium with atomic number 39. Today, rare earth elements are widely used in luminescent materials, electronic communications, magnetic materials, metallurgy, ceramics and other fields. According to the atomic electron layer structure and physical and chemical properties of rare earth elements, as well as their symbiosis in minerals and different ionic radii that can produce different properties, the seventeen rare earth elements are usually divided into two groups: light rare earths and heavy rare earths. [0003] Heavy rare earths are called "super industrial monosodium glutamate", mainly including gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium. Since the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/38C22B3/40C22B59/00
CPCY02P10/20
Inventor 孙晓琦王艳良郭向广
Owner XIAMEN INST OF RARE EARTH MATERIALS
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