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Extractant for yttrium extraction separation and extraction separation method thereof

A separation method and extraction agent technology, which is applied in the field of rare earth extraction and separation, can solve the problems of organic phase concentration decrease, extraction agent emulsification, loss, etc., and achieve the effect of improving stripping rate, good separation effect and stable performance

Active Publication Date: 2015-09-30
XIAMEN INST OF RARE EARTH MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Long-term industrial application has exposed the disadvantages of naphthenic acid process as follows: ① Naphthenic acid is a by-product of the petroleum industry, and its composition is extremely unstable; ② The pKa value of naphthenic acid is relatively high, which is 7.57, and it works at a higher pH. It is very easy to form solid naphthenate with iron (III), thorium (IV), titanium (IV), zirconium (IV) and other high-priced impurity elements, resulting in serious emulsification and loss of extractant; ③ naphthenic acid and phase The slow reaction of the improver isooctyl alcohol leads to a continuous decline in saponification value, which requires regular replenishment of fresh extractant or even replacement, resulting in a large amount of waste organic phase [Li Deqian, Chemical Problems in Rare Earth Hydrometallurgy Industry, Progress in Chemistry 7(3), 209- 213, (1995)]
Chinese invention patent 99118261.8 discloses a liquid-liquid extraction process for separating high-purity yttrium, using secondary octylphenoxy substituted acetic acid (code name CA12) and monobasic phosphorus (phosphine) acid or its monothio derivatives (such as P204, P507, Cyanex 272, Cyanex302, etc.) as an extractant to separate the yttrium element, which solves the emulsification problem of the naphthenic acid system, but the above-mentioned method still has the problem of a decrease in the concentration of the organic phase

Method used

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  • Extractant for yttrium extraction separation and extraction separation method thereof
  • Extractant for yttrium extraction separation and extraction separation method thereof
  • Extractant for yttrium extraction separation and extraction separation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Synthesis of [N4,4,4,4][CA12]

[0044]In a 125ml separating funnel, add 0.006 mole of tetrabutylamine bromide (denoted as [N4,4,4,4]Br) to 40ml of methanol, and then add 75ml of strong basic anion exchange resin to obtain Tetrabutylamine (denoted as [N4444]OH) solution. Add 0.006 mole of 2-octylphenoxy substituted acetic acid (code name CA12) to this solution, and stir the resulting mixture at room temperature for 6 h until the solution becomes neutral, then use a rotary evaporator to spin out methanol and water at 70°C , the product was dried in a vacuum oven at 70°C for 12h to obtain viscous liquid [N4,4,4,4][CA12]. The yield reaches 95%.

Embodiment 2

[0046] Synthesis of [P6,6,6,14][CA12]

[0047] In a 250ml separating funnel, add 0.012 moles of tetradecyltrihexylphosphonium chloride (recorded as [P6,6,6,14]Br, code name CYPHOS IL 101) into 80ml of methanol, and then add 150ml of strong alkaline Anion exchange resin, prepared tetradecyltrihexylphosphonium hydroxide (recorded as [P6,6,6,14]OH) solution. Add 0.012 moles of sec-octylphenoxy substituted acetic acid (code name CA12) to this solution, and stir the resulting mixture at room temperature for 6 h until the solution becomes neutral, then use a rotary evaporator to spin out methanol and water at 70°C , the product was dried in a vacuum oven at 70°C for 12h to obtain a viscous liquid [P6,6,6,14][CA12]. The yield reached 94%.

Embodiment 3

[0049] Preparation of organic phase: [P6,6,6,14][CA12] synthesized in Example 2 is mixed with toluene to form an organic phase, and the concentration of [P6,6,6,14][CA12] is 0.10 mol / liter .

[0050] Prepare the raw material solution: take the solutions of yttrium, holmium, erbium, thulium, ytterbium and lutetium respectively, add dilute hydrochloric acid, and prepare a raw material solution containing yttrium with a single rare earth concentration of 0.06 mol / liter, wherein NaCl is 0.5 mol / liter, pH is 3.2, and the total concentration is 0.36 mol / L.

[0051] 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 is completed, calculate the extraction rate E, distribution ratio D and separation coefficient β. The extraction rate E and distribution ratio D are shown in Table 1, and the separation coefficient β is shown in Table 1. figure 1 . After 15 cyc...

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Abstract

The invention relates to an extractant for yttrium extraction separation and an extraction separation method thereof. The cation of the extractant is quaternary phosphine or quaternary ammonia group, and the anion is sec-octylphenoxy substituted acetate. The extractant is simple in components; and the prepared organic phase has stable performance and can be recycled, and the concentration is not obviously lowered. The organic phase formed by mixing the extractant and diluter can be used for efficiently extracting an yttrium-containing rare-earth solution. Due to the particular phase transition action of the ionic liquid, the back extraction agent can enter the organic phase more easily, thereby greatly enhancing the back extraction rate.

Description

technical field [0001] The invention relates to the field of rare earth extraction and separation, in particular to an extraction agent for extraction and separation of yttrium and an extraction and separation method thereof. Background technique [0002] Yttrium oxide is one of the matrix materials of fluorescent, microwave, laser, precision ceramics and other materials, and is widely used. But due to the ionic radius of yttrium Erbium falling on the lanthanide sequence Nearby, the chemical properties of yttrium are also very similar to those of lanthanides, especially heavy lanthanides, and it is difficult to separate them from each other. [0003] In the prior art, the separation of yttrium mainly adopts the extraction and separation method using naphthenic acid (code name NA) as the main extractant. Long-term industrial application has exposed the disadvantages of naphthenic acid process as follows: ① Naphthenic acid is a by-product of the petroleum industry, and it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/26C22B59/00
CPCY02P10/20
Inventor 孙晓琦王艳良董亚敏
Owner XIAMEN INST OF RARE EARTH MATERIALS
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