Preparation method of rare earth fluoride

A technology of rare earth fluorides and rare earth elements, applied in the direction of rare earth metal fluorides, rare earth metal halides, etc., can solve the problems of complex steps, human hazards, and difficulty in hydrogen fluoride tail gas treatment, and achieve high purity and low water and oxygen content in products Effect

Pending Publication Date: 2020-07-10
GRIREM ADVANCED MATERIALS CO LTD
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Problems solved by technology

[0004] There are two common dry processes, one is obtained by the reaction of hydrogen fluoride and rare earth oxides, but the hydrogen fluoride tail gas produced by this method is more difficult to treat
If the exhaust gas is not treated cleanly, it will cause danger to people
Another dry process is to use ammonium bifluoride to react with rare earth oxides. This method is a solid-solid reaction. On the one hand, there will be problems of incomplete reaction. On the other hand, there will be deamination and dehydration treatment, and the steps are more complicated.

Method used

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  • Preparation method of rare earth fluoride

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preparation example Construction

[0023] Such as figure 1 As shown, the steps of the method for preparing rare earth fluorides include: step S101 to step 105:

[0024] Step S101, dissolving the salt containing rare earth elements in a hydroxy ether solvent.

[0025] Among them, the salt containing rare earth elements is rare earth chloride salt, rare earth nitrate or rare earth sulfate.

[0026] Optionally, the salt containing rare earth elements is DyCl 3 , NdCl 3 、LaCl 3 or La(NO 3 ) 3 one or more of.

[0027] Specifically, the structural formula of the hydroxy ether solvent is:

[0028]

[0029] Wherein, R1 is any one of hydrogen, methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl and tert-butyl; R2 is hydrogen, methyl, ethyl, n-propyl , isopropyl, n-butyl, isobutyl and tert-butyl; 1≤n≤10, and n is a positive integer.

[0030] In an optional embodiment, the hydroxy ether solvent is ethylene glycol or 2-hydroxypropyl methyl ether.

[0031] Step S102, ultrasonically treating the hydroxy ether ...

Embodiment 1

[0048] 36g of NdCl 3Dissolve in 500mL ethylene glycol, and sonicate it for 10min to obtain a homogeneous solution. Add 25 mL of 1-ethyl-3-methylimidazolium tetrafluoroborate dropwise into the homogeneous solution, stir with a glass rod during the dropwise addition, and stir for 10 minutes after the addition to obtain a suspension. The suspension was suction-filtered to obtain 30 g of a precipitate, which was washed with water and ethanol respectively, and then vacuum-dried at 60° C. for 24 hours to obtain 25 g of a reaction product.

[0049] figure 2 is the XRD pattern of the reaction product.

[0050] Such as figure 2 Shown, where the black line is NdF 3 XRD pattern, the gray line is the XRD pattern of the reaction product. After comparison, the precipitate is NdF 3 . It can be seen that the method of the present application is used to prepare rare earth fluorides, and the yield is relatively high. The oxygen content of the reaction product was analyzed by an oxygen...

Embodiment 2

[0052] 49g of LaCl 3 Dissolve in 700 mL 2-hydroxypropyl methyl ether, and sonicate it for 5 min to obtain a homogeneous solution. Add 45mL of 1-butyl-3-methylimidazolium hexafluorophosphate dropwise into the homogeneous solution, and stir with magnetic force during the dropwise addition. After complete addition, stirring for 10 minutes resulted in a suspension. The suspension was suction-filtered to obtain 35 g of a precipitate, which was washed with water and ethanol respectively, and then vacuum-dried at 100° C. for 18 hours to obtain 28 g of a reaction product.

[0053] By performing X-ray diffraction on the reaction product, the XRD pattern of the reaction product is obtained, which proves that the reaction product is LaF 3 . The oxygen content of the reaction product was analyzed by an oxygen and nitrogen analyzer, and the oxygen content was 60 ppm. Illustrate adopting the method that the embodiment of the present invention provides to prepare LaF 3 , the oxygen cont...

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Abstract

The invention discloses a preparation method of rare earth fluoride. The preparation method comprises the following steps: dissolving salt containing rare earth elements into a hydroxyl ether solvent;carrying out ultrasonic treatment for 3-15 minutes to obtain a uniform solution; adding liquid containing fluorine ions into the uniform solution and uniformly mixing to obtain turbid liquid containing rare earth fluoride; extracting precipitate in the turbid liquid; and vacuum-drying the precipitate at the temperature of 60-100 DEG C for 1 h or longer to obtain rare earth fluoride, wherein the water oxygen content of the rare earth fluoride is smaller than 100ppm. According to the preparation method of the rare earth fluoride provided by the embodiment of the invention, the salt containing rare earth elements is dissolved in the hydroxyl ether solvent, the viscosity of the hydroxyl ether solvent is relatively high, the rare earth fluoride is prepared in a high-viscosity environment, thereaction environment is liquid, the reaction selectivity is relatively high, and the reaction is complete. Moreover, the whole process is carried out in liquid, hydrogen fluoride is not needed, no tail gas is generated, and the reaction process is energy-saving and environment-friendly. No water is contained in the whole reaction process, and the water oxygen content of the product is low.

Description

technical field [0001] The invention relates to the field of rare earth elements, in particular to a preparation method of rare earth fluorides. Background technique [0002] There are two existing techniques for preparing rare earth fluorides: wet method and dry method. [0003] The wet process is obtained by reacting rare earth hydroxide aqueous solution or rare earth chloride aqueous solution with hydrofluoric acid. Due to the reaction between aqueous solutions, the rare earth fluoride prepared by this process is easy to form compounds such as crystal water, resulting in the prepared rare earth Fluoride impurities have high water and oxygen content; if rare earth oxides are used as raw materials, an acid-dissolving step is added, which is easy to introduce additional impurities, high water and oxygen content, and the process is long and the amount of wastewater treated is large. Rare earth fluorides usually obtained by wet process have oxygen content above 3000ppm and hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/265
Inventor 苗睿瑛张小伟庞思明陈德宏杨宏博杨秉政吴道高朱琼
Owner GRIREM ADVANCED MATERIALS CO LTD
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