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Method of preparing high purity cerium trifluoride micro powder

A technology of cerium trifluoride and micropowder, which is applied in chemical instruments and methods, fluoride preparation, inorganic chemistry, etc., and can solve problems such as changes in organic phase components, complicated treatment processes, and non-recyclable organic phases.

Inactive Publication Date: 2004-12-22
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

There are two disadvantages in this process: the surfactant dissolves in the organic phase, resulting in a change in the composition of the organic phase, the organic phase cannot be recycled, and the excess surfactant is difficult to recover; the reactant must be a pure substance, and the production cost is high
However, the process is based on CeO 2 Recovering cerium and fluorine in the feed liquid in the form of NaF and NaF requires two back extractions, the unit consumption of acid and alkali is relatively large, and the treatment process is complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] The feed liquid comes from the sulfuric acid leaching liquid of bastnaesite oxidation roasting, the acidity of the feed liquid is adjusted to 0.1mol / L, and potassium permanganate is added to make the concentration of potassium permanganate in the feed liquid 0.1g / L. Add boric acid, make the concentration of boric acid in the feed liquid be 0.1g / L. Take 300ml of Cyanex923 and 700ml of n-heptane, mix well, and prepare the extraction composition. A 30ml separatory funnel was used as a reactor to carry out 5-stage countercurrent extraction, and the flow ratio of the organic phase to the feed liquid was 1:5. Then carry out 2-stage counter-current stripping, stripping liquid is 0.1% H 2 o 2 Aqueous solution, the flow ratio of organic phase and stripping liquid is 1:10. Filter the resulting back-extraction product to obtain CeF 3 Nano powder, the average particle size is 70nm, CeO 2 / REO = 99.92%. Then, three stages of countercurrent washing are carried out, the washing ...

Embodiment 2

[0059] The feed liquid from Example 1 was adjusted to have an acidity of 1.5 mol / L, and potassium permanganate was added to make the concentration of potassium permanganate in the feed liquid 2.0 g / L. Add boric acid, make the concentration of boric acid in the feed liquid be 5.0g / L. Take 200ml of Cyanex923 and 800ml of octane, mix well, and prepare the extraction composition. A 30ml separating funnel was used as a reactor to carry out 5-stage countercurrent extraction, and the flow ratio of the organic phase to the feed liquid was 3:2. Then carry out 4 stages of countercurrent washing, the washing liquid is 0.5mol / L H 2 SO 4 and 1g / LH 3 BO 3 The mixed aqueous solution, the flow ratio of the organic phase to the washing liquid is 1:10. Then carry out 2-stage countercurrent back extraction, the back extraction solution is 10.0% H 2 o 2 Aqueous solution, the flow ratio of organic phase and stripping liquid is 1:10. Filter the resulting back-extraction product to obtain Ce...

Embodiment 3

[0061] The feed liquid from Example 1 was adjusted to have an acidity of 3.0 mol / L, and potassium permanganate was added to make the concentration of potassium permanganate in the feed liquid 5.0 g / L. Add boric acid, make the concentration of boric acid in the feed liquid be 5.0g / L. Take 300ml of Cyanex923 and 700ml of n-hexane, mix them evenly, and prepare the extraction composition. A 30ml separating funnel was used as a reactor to carry out 6-stage countercurrent extraction, and the flow ratio of the organic phase to the feed liquid was 2:1. Then carry out 6 stages of countercurrent washing, the washing liquid is 0.5mol / L H 2 SO 4 and 1g / LH 3 BO 3 The mixed aqueous solution, the flow ratio of the organic phase to the washing liquid is 2:3. Then carry out 2-stage countercurrent back extraction, the back extraction solution is 10.0% hydrazine hydrate aqueous solution, the flow ratio of the organic phase and the back extraction solution is 2:1. Filter the resulting back-...

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Abstract

A process for preparing the superfine particles of high-purity cerium trifluoride includes proportionally mixing Cyanex 923 with diluent chosen from hexane, pentane, octane, etc to obtain composite extractant, extracting the Ce and F contained RE sulfate solution, washing and back extracting by strip liquid chosen from hydrogen peroxide, hydrazine hydrate, hydroxyamine hydrochloride, etc. Its purity is 99.9-99.999%.

Description

technical field [0001] The present invention relates to the preparation of CeF 3 The method, more specifically, the present invention relates to prepare high-purity CeF from the rare earth sulfuric acid solution containing cerium (IV), fluorine 3 micronized method. Background technique [0002] CeF 3 It is an important raw material for the preparation of single rare earth metal cerium by metallothermal reduction method. At the same time, due to its Faraday effect, CeF 3 Crystals can be made into laser communication modulators and single-pass light valves. Nanoscale CeF 3 It is a good solid lubricant and can also be used as a grease and lubricating oil additive. [0003] CeF commonly used in industry 3 Synthetic methods include HF(NH 4 HF 2 ) precipitation-vacuum dehydration method, HF (NH 4 HF 2 ) fluorination method, NH 4 HCO 3 Transformation preparation method, the current production mostly adopts HF precipitation-vacuum dehydration method, that is, in CeCl 3 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B9/08C01F17/00
CPCY02P10/20
Inventor 李德谦李红飞国富强张志峰
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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