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Process for preparing grain-size-adjustable rare earth fluoride micro-powder in neutral phosphorus (phosphine) extraction system

A technology of rare earth fluoride and neutral phosphorus, applied in the direction of improving process efficiency, etc., to achieve the effects of good monodispersity, low cost and simple process

Inactive Publication Date: 2008-07-30
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the research on rare earth fluorides at home and abroad mainly focuses on the single crystal growth and scintillator properties of rare earth fluorides (Kiyoshi Shimamura et al., Journal of Crystal Growth, 2004, 264, 208; Encarnacio′n et al., Nuclear Instruments and Methods in Physics Research A, 2005, 537, 139), luminescent properties of rare earth fluorides (J.W.Stouwdam et al., Nano Lett, 2002, 7, 733), CeF 3 Tribological behavior of nanoparticles (Wu Zhishen et al., Rare Earth, 2001, 5, 1), CeF 3 Nanoparticle synthesis and characterization (Sunqing Qiu et al., Powder Technology, 2000, 113, 9; Eiden-Assmann et al., Materials Research Bulletin, 2004, 39, 21) and other aspects of research, Chinese patent ZL 2004 10010618.2 discloses a preparation of high The method of pure cerium trifluoride powder, there is no report on the particle size control method of rare earth fluoride powder

Method used

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  • Process for preparing grain-size-adjustable rare earth fluoride micro-powder in neutral phosphorus (phosphine) extraction system
  • Process for preparing grain-size-adjustable rare earth fluoride micro-powder in neutral phosphorus (phosphine) extraction system
  • Process for preparing grain-size-adjustable rare earth fluoride micro-powder in neutral phosphorus (phosphine) extraction system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Take 300ml of Cyanex923 and 700ml of n-heptane, mix them evenly, and prepare the extraction composition;

[0032] (2) The ceric sulfate solution obtained by dissolving cerium dioxide with sulfuric acid is used as the feed liquid, and the feed liquids with different ceric sulfate concentrations are configured so that the ceric sulfate concentrations are respectively 0.005, 0.01, 0.02, 0.03, 0.05, 0.10, 0.15mol / L, add HF, make the concentration ratio of F(I) and Ce(IV) in the feed liquid be 3, adjust the feed liquid acidity to be 0.5mol / L;

[0033] (3) Ce(IV) and F(I) in the feed liquid of step (2) different ceric sulfate concentrations are extracted respectively with the extraction composition in step (1), and the ratio of the extraction composition and the feed liquid is 1 : 1, the extraction equilibrium time is 0.5h;

[0034] (4) Then carry out back extraction respectively, with 2%H 2 o 2 The mixed solution with 0.5% Triton X-100 (volume ratio) is the back extr...

Embodiment 2

[0039] (1) Take 50ml, 100ml, 200ml, 300ml, 400ml, 500ml, and 600ml of Cyanex923 respectively, and use n-hexane as the dilution solvent to prepare 1000ml of Cyanex923 with volume percentage concentrations of 5, 10, 20, 30, 40, 50, and 60%. - n-hexane extraction composition;

[0040] (2) Take the sulfuric acid leaching solution of bastnaesite through oxidative roasting as the feed liquid, adjust the acidity of the feed liquid to be 3.0mol / L, add potassium permanganate, and make the concentration of potassium permanganate in the feed liquid be 5.0g / L , add boric acid, make the concentration of boric acid 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) Then perform 6-stage countercurrent washing, the washing liquid is 0.5mol / LH 2 SO 4 and 1g / LH 3 BO 3 The mixed aqueous solution, the flow ratio of the extr...

Embodiment 3

[0049] (1) Take 400ml of Cyanex923 and 600ml of octane, mix them evenly, and prepare the extraction composition;

[0050] (2) The samarium nitrate solution obtained by dissolving samarium oxide with nitric acid is a feed liquid, the concentration of samarium nitrate in the feed liquid is adjusted to 0.04mol / L, and the acidity is adjusted to 1.0mol / L;

[0051] (3) Extracting Sm(III) in the feed liquid of step (2) with the extraction composition in step (1), the ratio of the extraction composition to the feed liquid is 3:1, and the extraction equilibrium time is 24h;

[0052] (4) Then carry out stripping separately, with 0.5mol / L HNO 3 , 0.15mol / LHF and volume percent concentration are respectively 0.01, 0.03, 0.05, 0.08, 0.1, 0.3, 0.5, 1.0, 2.0% Triton X-100 mixed solution is stripping solution stripping from the extraction composition, the extraction combination The ratio of the product to the stripping solution is 2:1, and the obtained stripping mixture is filtered separatel...

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Abstract

The invention discloses a micro-powder grain size modulating method in the preparing course of rare earth fluoride extracted by neutral phosphor, which is characterized by the following: adopting neutral phosphor as extract; controlling the grain size within 1-4000nm; reducing pollution greatly; fitting for phototronics, tribology and high-energy physics domain due to different property of rare earth fluoride with different grain sizes.

Description

technical field [0001] The invention relates to a method for preparing rare earth fluoride micro-powder to regulate particle size through a neutral phosphorus (phosphine) extraction system, and belongs to the technical field of inorganic chemical industry. Background technique [0002] Rare earth fluorides are important raw materials for producing single rare earth metals by metallothermic reduction, and they have important applications in high energy physics, nuclear medicine, magneto-optical storage, solid lubricants, and optoelectronic devices. The preparation of existing rare earth fluorides, common 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. In industrial production, HF precipitation-vacuum dehydration method is often used, that is, in CeCl 3 Directly pass HF into the solution to precipitate CeF 3 , and then processed by washing, drying and va...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/40C22B3/06
CPCY02P10/20
Inventor 李德谦国富强李红飞张志峰孟淑兰
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES