Method for preparing rare earth fluoride by using fluorinated ionic liquid

A technology of rare earth fluoride and fluoride ions, which is applied in the preparation/treatment of rare earth metal compounds, rare earth metal halides, rare earth metal fluorides, etc., can solve the problems of energy consumption environment, fluorine gas generation, disadvantages, etc., and achieve reaction Effects of mild conditions and improved purity

Active Publication Date: 2022-02-22
XIAMEN INST OF RARE EARTH MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These three methods are relatively mature, but the current research shows that the preparation of most rare earth fluorides needs to be carried out under higher temperatur...

Method used

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  • Method for preparing rare earth fluoride by using fluorinated ionic liquid
  • Method for preparing rare earth fluoride by using fluorinated ionic liquid
  • Method for preparing rare earth fluoride by using fluorinated ionic liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Refer figure 1 Using fluorinated ionic liquid [Bmim] [PF 6 ] Direct preparation of rare earth fluoride NdF 3 The method comprising the steps of:

[0033] (1) Weigh 1.12mmol Nd 2 O 3 6mL solid powder and fluorinated ionic liquid [Bmim] [PF 6 ] In 20mL Teflon liner, after a Teflon-lined stainless steel reaction kettle placed;

[0034] (2) A stainless steel autoclave, an oven, heat the reaction solvent, the reaction temperature was controlled 180 ℃, reaction time 48h, the use of ionic liquids will heat the solid ion Nd 2 O 3 Into a solid at a high temperature and pressure NdF 3 ; Until completion of the reaction, the reaction product was removed by centrifugation, 8000 rpm for controlling the rotational speed centrifugation, the centrifugation time 5min, solid-liquid separation;

[0035] (3) The precipitate was washed three times with anhydrous ethanol, to remove residual ionic liquid;

[0036] (4) After completion of washing the precipitate was dried at 80 ℃ for 12h, to obtai...

Embodiment 2

[0039] Using fluorinated ionic liquid [BMIM] [PF 6 ] Directly prepare fluorinated rare earth LAF 3 Method, including the steps of:

[0040] (1) Weigh 0.56mmol LA 2 O 3 Solid powder and 6 mL fluorinated ionic liquid [BMIM] [PF 6 The polytetrafluoroethylene liner is placed in a stainless steel reaction kettle in a 20 ml polytetrafluorine liner.

[0041] (2) Put the stainless steel reactor into the oven, heat reaction, the temperature of the reaction temperature is 160 ° C, the reaction time is 96h, and the solid La 2 O 3 Convert to solid LAF under high temperature high pressure 3 At the end of the reaction, the reaction product was centrifuged, and the centrifugation speed was 6000 rpm, centrifugation time was 10 min, and solid-liquid separation was achieved.

[0042] (3) Wash the precipitate three times with anhydrous ethanol, remove the residual ionic liquid;

[0043] (4) After the washing is completed, the precipitate is dried under 80 ° C for 18 h, which can get LAF. 3 Powder.

...

Embodiment 3

[0046] Using fluorinated ionic liquid [BMIM] [PF 6 ] Directly prepare fluorinated rare earth CEF 3 Method, including the steps of:

[0047] (1) Weigh 1.12mmol CE 2 O 3 Solid powder and 9 ml of fluorinated ionic liquid [BMIM] [PF 6 The polytetrafluoroethylene liner is placed in a stainless steel reaction kettle in a 20 ml polytetrafluorine liner.

[0048] (2) Put the stainless steel reactor into the oven, heat reaction, the temperature of the reaction temperature is 200 ° C, the reaction time is 24 h, and the solid CE 2 O 3 Convert to solid CEF under high temperature high pressure 3 At the end of the reaction, the reaction product was centrifuged, and the centrifugation speed was 10000 rpm, centrifugation time was 3 min, and solid-liquid separation was achieved.

[0049] (3) Wash the precipitate 4 times with anhydrous ethanol, remove the residual ionic liquid;

[0050] (4) After the washing is completed, the precipitate is dried under 90 ° C for 12 h, which can be obtained from CEF...

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Abstract

The invention discloses a method for preparing rare earth fluoride by using fluorinated ionic liquid. The rare earth fluoride is represented by a chemical formula REF3, wherein RE is selected from at least one of La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Y and Sc. A fluorinated ionic liquid and rare earth oxides are used as raw materials, the rare earth oxides are directly converted into rare earth fluoride through a solvothermal method, and the reaction can be carried out under a relatively low-temperature condition, so that a certain danger caused by fluorine gas generated at a high temperature is avoided; and meanwhile, the preparation method of the rare earth fluoride provided by the invention is mild in reaction condition, and the rare earth fluoride can be obtained without adding any surfactant, catalyst or template, so that the purity and the yield of the rare earth fluoride are greatly improved. The oxygen content of the rare earth fluoride prepared through the method is lower than 100 ppm, and the rare earth fluoride can be widely used for preparing rare earth fluoride single crystals, low-oxygen metal gadolinium and fluorescent matrix materials.

Description

Technical field [0001] The present invention belongs to the special physical properties of rare earth fluoride powder materials and their preparation, and in particular relates to a method of using a fluorinated rare earth fluorinated ionic liquids prepared. Background technique [0002] Rare earth compound 4f electron shell has a unique structure, which shell electron transition generated electrical, optical and chemical properties, can provide a suitable and effective crystal field ion emission center, light emission promoting excite the luminescent center ions, rare earth compounds are widely used in optical, optoelectronic, diagnostics, biomarker, catalysis. Compared with the group systems, rare earth fluoride (i.e., rare earth fluoride) having a lower vibrational energy, wide bandgap, high refractive index and a minimum excited state quenching of rare earth ions, rare earth fluoride-based light emitting materials such as the most promising photochromic nonlinear optical mate...

Claims

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Application Information

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IPC IPC(8): C01F17/265C01F17/10
CPCC01F17/265C01F17/10C01P2002/72C01P2006/80
Inventor 薛丽燕杨帆谢美英邵志恒赵志钢
Owner XIAMEN INST OF RARE EARTH MATERIALS
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