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Method for preparing cerium trifluoride using neutral phosphoras (phosphine) extraction system

A cerium trifluoride, neutral phosphorus technology, applied in chemical instruments and methods, liquid solution solvent extraction, inorganic chemistry and other directions, can solve the problems of single type of extractant and narrow range of extractant, and achieve uniform product particle size distribution, The effect of reducing pollution

Inactive Publication Date: 2007-02-14
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The type of extractant used in the method is single, does not involve other neutral phosphorus (phosphine) extractants except Cyanex923, and the range of extractants to choose from is relatively narrow

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Take 300ml Cyanex923, 100ml TBP, 600ml n-heptane, mix well, and prepare the extraction composition;

[0027] (2) Take the nitric acid leaching solution of bastnaesite through oxidative roasting as feed liquid, wherein [REO] is 100g / L, [CeO ] is 1g / L, and the acidity of feed liquid is adjusted to be 0.2mol / L, adding high Potassium manganate, make the potassium permanganate concentration in the feed liquid be 0.1g / L, add boric acid, make the boric acid concentration in the feed liquid be 0.1g / L;

[0028] (3) Use a 30ml separatory funnel as a reactor to carry out 5-stage countercurrent extraction, and the flow ratio of the extraction composition to the feed liquid is 1:5;

[0029] (4) Then carry out 2 stages of countercurrent back extraction, the back extraction liquid is the H2O2 aqueous solution with volume percentage concentration of 0.1%, the flow ratio of the extraction composition and the back extraction liquid is 1: 5, and the obtained back extraction mixture is...

Embodiment 2

[0032] (1) Take 200ml Cyanex923, 50ml P350, and 750ml n-hexane, mix them evenly, and prepare the extraction composition;

[0033] (2) Take the sulfuric acid leaching solution of bastnaesite through oxidative roasting as feed liquid, wherein [REO] is 120g / L, [CeO ] is 60g / L, and the acidity of feed liquid is adjusted to be 1.3mol / L, adding high Potassium manganate, make the potassium permanganate concentration in the feed liquid be 1.8g / L, add boric acid, make the boric acid concentration in the feed liquid be 5.0g / L;

[0034](3) Use a 30ml separatory funnel as a reactor to carry out 5-stage countercurrent extraction, and the flow ratio of the extraction composition to the feed liquid is 5:3;

[0035] (4) Optionally: then carry out 4-stage countercurrent washing, the washing solution is 0.5mol / L H2SO4 and 1g / L H3BO3 mixed aqueous solution, the flow ratio of the extraction composition and the washing solution is 1:10;

[0036] (5) Then carry out 2 stages of countercurrent back ...

Embodiment 3

[0039] (1) Take 300ml of Cyanex923, 10ml of PBBP, and 690ml of n-octane, mix them evenly, and prepare an extraction composition;

[0040] (2) Take the sulfuric acid leaching solution of bastnaesite through oxidative roasting as feed liquid, wherein [REO] is 40g / L, and [CeO ] is 30g / L, and the acidity of feed liquid is adjusted to be 3.0mol / L, adding high Potassium manganate, make potassium permanganate concentration in the feed liquid be 5.0g / L, add boric acid, make the boric acid concentration in the feed liquid be 5.0g / L;

[0041] (3) Use a 30ml separatory funnel as a reactor to carry out 6-stage countercurrent extraction, and the flow ratio of the extraction composition to the feed liquid is 2:1;

[0042] (4) Optional: then carry out 6-stage countercurrent washing, the washing solution is 0.1mol / L H2SO4 and 0.1g / L H3BO3 mixed aqueous solution, the flow ratio of the extraction composition and the washing solution is 2:3;

[0043] (5) Then carry out 2 stages of countercurren...

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Abstract

The process of preparing cerium trifluoride micro powder with neutral phosphorus extracting system adopts the material solution of RE sulfuric acid and / or nitric acid solution containing Ce(IV) and F and with acidity of 0.2-6.0 mol / L; extractant comprising Cyanex923 and one or several of TBP, P350, PBBP, DEHEHP, ODOP, Cyanex921, Cyanex925, Cyanex471 and TOEDPO in arbitrary proportion; diluting solvent of n-hexane, n-heptane, octane, noane, decane or sulfonated kerosene to constitute extracting composition together with the extractant; and the back extracting solution of hydrogen peroxide, hydrazine hydrate, hydroxylamine hydrochloride or their mixture with sulfuric acid and / or nitric acid. The extracted composition is washed and back extracted to obtain the cerium trifluoride micro powder with purity of 90-99.9999 % and granularity of 1-4000 nm.

Description

technical field [0001] The invention relates to a method for preparing cerium trifluoride micropowder, in particular to a method for preparing CeF3 micropowder from rare earth sulfuric acid or nitric acid or a mixed acid solution of sulfuric acid and nitric acid containing cerium (IV) and fluorine by using a neutral phosphorus (phosphine) extraction system. Background technique [0002] CeF3 is an important raw material for the production of single rare earth metal cerium by metallothermic reduction, and it has important applications in high-energy physics, nuclear medicine, solid lubricants, and optoelectronic devices. At present, the common synthesis methods of CeF3 include HF (NH4HF2) precipitation-vacuum dehydration method, HF (NH4HF2) fluorination method, and NH4HCO3 conversion preparation method. In industrial production, HF precipitation-vacuum dehydration method is often used, that is, HF is directly passed into CeCl3 solution to precipitate CeF3, and then washed, dr...

Claims

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Application Information

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IPC IPC(8): C01F17/00B01D11/04
Inventor 李德谦国富强李红飞张志峰孟淑兰张绘
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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