Method for separating tetravalent cerium or tetravalent cerium and fluorine

A cation and anion technology, applied in the field of separation of tetravalent cerium or tetravalent cerium and fluorine, can solve the problems of high production cost and serious environmental pollution, achieve less acid and alkali consumption, reduce environmental pollution, and achieve good separation effect

Inactive Publication Date: 2012-04-11
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] This method uses an acidic phosphine extractant to extract and separate tetravalent cerium from a mixed rare earth sulfate solution. However, the acidity of the extraction is high, and a large amount of acid and alkali consumption is required. Not only the production cost is relatively high, but also the environmental pollution is more serious.

Method used

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  • Method for separating tetravalent cerium or tetravalent cerium and fluorine
  • Method for separating tetravalent cerium or tetravalent cerium and fluorine
  • Method for separating tetravalent cerium or tetravalent cerium and fluorine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] In the reactor, add 6.39g of sodium metal and 125mL of distilled isopropanol to react at room temperature. After 3 hours of reaction, a solution of sodium isopropoxide is obtained, and continue to add 500mL of distilled, dissolved in 112.36g of methyl alcohol. The isopropanol solution of trioctylammonium chloride was reacted. After stirring at 50°C for 4 hours, the centrifuge was used to centrifuge the obtained isopropanol solution at a speed of 8000r / min for 10min. After collecting the filtrate by filtration, pour it into the filtrate Add 500mL of deionized water and shake for 30min to obtain a methyl trioctyl ammonium hydroxide ([A336][OH]) solution.

[0069] Take 1 mL of the obtained [A336][OH] solution, use bromothymol blue as an indicator, and titrate with hydrochloric acid with a concentration of 0.132 mol / L to obtain a concentration of [A336][OH] of 0.121 mol / L.

Embodiment 2

[0071] In the reactor, add 172mL of the [A336][OH] solution prepared in Example 1 and 6.25g of P507, reflux and stir at 50°C for 12h, put the stirred solution to stand and separate phases, take the upper phase at 80°C, 20mbar Contained isopropanol and water are spinned out at the bottom to obtain the mono-2-ethylhexylphosphonic acid ionic liquid ([A336][P507]) of methyl trioctyl ammonium 2-ethylhexyl ester, and its proton nuclear magnetic resonance spectrum and nuclear magnetic resonance The spectrogram data of the carbon spectrum are as follows:

[0072] 1 H NMR: 0.822-0.847(t, J=8.4Hz, 3H), 0.851-0.872(t, J=8.4Hz, 3H), 0.875-0.894(t, J=6.6Hz, 9H), 1.264(s, 30H ), 1.287-1.298(m, 6H), 1.330-1.408(m, 12H), 1.419-1.454(m, 2H), 1.466-1.515(m, 2H), 1.539-1.583(m, 1H), 1.609-1.677 (m, 6H), 1.710-1.779(m, 1H), 2.699(s, 2H), 3.322(s, 3H), 3.404-3.432(t, J=8.4Hz, 6H), 3.672-3.705(m, 2H );

[0073] 13C NMR: 65.87, 61.00(3C), 48.82, 40.55, 34.80, 33.75, 31.65, 31.49(2C), 30.0(2C), ...

Embodiment 3

[0075] In the reactor, add 177mL of the [A336][OH] solution prepared in Example 1 and 8.01g of P204, reflux and stir at 50°C for 12h, leave the stirred solution to separate phases, take the upper phase at 80°C, 20mbar Contained isopropanol and water are spinned out at the bottom to obtain methyl trioctyl ammonium di(2-ethylhexyl) phosphonic acid ionic liquid ([A336][P204]), the data of its proton nuclear magnetic resonance spectrum and carbon nuclear magnetic resonance spectrum They are as follows:

[0076] 1 H NMR: 0.854-0.870 (m, 6H), 0.876-0.894 (m, 9H), 1.265-1.274 (m, 30H), 1.282-1.296 (m, 6H), 1.308-1.358 (m, 12H), 1.370- 1.411(m, 4H), 1.424-1.470(m, 1H), 1.500-1.530(m, 1H), 1.613-1.677(m, 6H), 3.294(s, 3H), 3.375-3.403(t, J=7.8Hz , 6H), 3.711-3.745(m, 4H);

[0077] 13 C NMR: 10.66(2C), 13.70, 13.74, 13.80, 22.11(3C), 22.28(3C), 22.33(3C), 22.87(3C), 23.06(3C), 26.09(2C), 28.77, 28.81(2C) , 28.91 (2C), 28.95, 29.12, 29.16, 29.85, 31.38, 31.54, 40.14, 48.59, 60.93, 6...

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Abstract

The invention provides a method for separating tetravalent cerium. The method comprises the following steps: a) providing feed liquor, wherein the feed liquor contains tetravalent cerium ions, trivalent rare earth ions and sulphuric acid and the concentration of sulphuric acid in the feed liquor is 0.06mol / L-0.5mol / L; b) extracting the feed liquor in the step a) with a mixed solution of ionic liquid and a diluent to obtain extract liquor and raffinate, wherein the cations of the ionic liquid are quaternary ammonium cations and the anions of the ionic liquid are anions obtained by deprotonating an acidic phosphine extractant; and c) performing back extraction on the extract liquor obtained in the step b) by using dilute sulphuric acid as the back-extractant to obtain back extraction liquor containing tetravalent cerium. The invention also provides a method for separating tetravalent cerium and fluorine. The method for separating tetravalent cerium and fluorine, provided by the invention, has lower extraction acidity and back-extractant acidity, thus the consumptions of acid and base can be reduced, the production cost can be saved and the environmental pollution can be reduced.

Description

technical field [0001] The invention relates to the technical field of rare earth separation, in particular to a method for separating tetravalent cerium or tetravalent cerium and fluorine. Background technique [0002] Cerium in rare earth elements is widely used, such as polishing powder, phosphor, colorant and catalyst. Cerium-containing compounds are generally obtained by smelting cerium-containing minerals such as bastnaesite and monazite. However, the smelted products contain not only cerium, but also other elements such as lanthanum, praseodymium, and neodymium. Therefore, it is of great practical significance to separate cerium from other elements. [0003] The usual way to separate cerium from other elements is to oxidize trivalent cerium in cerium-containing minerals or other cerium-containing mixtures to tetravalent cerium, then add acid solution for leaching or washing, and then remove the tetravalent cerium in acid leaching solution or acid washing solution. E...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/38C22B59/00
CPCY02P10/20
Inventor 陈继张冬丽邓岳锋
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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