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Method for separating and recovering valuable components from rare earth praseodymium-neodymium fused salt electrolysis waste

A technology of molten salt electrolysis and recovery method, which is applied in the direction of improving process efficiency, etc., can solve the problems of long process flow and high processing cost, and achieve the effects of simple process, high yield and reduced roasting process

Active Publication Date: 2015-07-29
YIYANG HONGYUAN RARE EARTH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this process avoids the pollution of the waste gas produced by the process to the environment, the result of calcification and roasting leads to the introduction of calcium element into the system. The content of CaO in the acid solution solution exceeds 10g / L, and the method of extraction has to be used to remove Rare earth decalcification, long process, high processing cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A method for separating valuable components in electrolytic waste of rare earth praseodymium and neodymium molten salt, which includes the following steps:

[0025] ⑴ Raw material processing: use the waste material produced by the molten salt electrolysis method to produce rare earth praseodymium and neodymium metal as the raw material, and crush the raw material to obtain powder;

[0026] In this example, a rare earth molten salt electrolysis waste from a rare earth factory in Hunan is used as an example to further illustrate the present invention. The total rare earth and main impurity content analysis results of the electrolyte waste are shown in Table 1 (unit: ﹪):

[0027] Table 1 Analysis results of electrolytic waste

[0028] TREOFe 2 O 3 SiO 2 CaO Al 2 O 3 80.650.490.021.140.50

[0029] In order to facilitate the leaching of soluble oxides, especially non-rare earth impurities, in the slurry, in step (1) of the present invention, the particle size of the powder is 32...

Embodiment 2

[0055] In order to facilitate the leaching of acid-soluble impurities and oxide slag in the slurry into the solution, in step (3) of the method for separating valuable components in the rare earth neodymium praseodymium molten salt electrolysis waste, the slurry is first heated to 60℃~80℃, then continue to stir and react for 2h~4h.

[0056] In order to facilitate the leaching of acid-soluble impurities and oxide slag in the slurry into the solution, in step 3 of the method for recovering valuable components in the rare earth neodymium praseodymium molten salt electrolysis waste, the slurry is first heated to 60℃~80℃, then continue to stir and react for 2h~4h.

[0057] After the addition of acid was stopped in this example, the slurry was heated to 60° C., and the stirring reaction was continued for 2 hours, the pH value was almost unchanged, and the filter residue containing neodymium praseodymium fluoride and the filtrate containing neodymium praseodymium chloride were obtained by...

Embodiment 3

[0068] In this example, take 1 kg of powder into a beaker, add 2 kg of pure water and mix well, add 2 mol / L hydrochloric acid while stirring at room temperature, and stop adding acid until the final pH value remains at 1.0 to 1.5, and the slurry is heated to 60 ℃, continue to stir and react for 2h, the pH value is almost unchanged; filter residue and filtrate are obtained by filtration.

[0069] The filter residue was washed with water to neutrality, and dried at 70°C to obtain 534.9 g of neodymium praseodymium fluoride. The composition analysis results are shown in Table 6 (unit: ﹪):

[0070] Table 6: Analysis results of praseodymium and neodymium fluoride in Example 3

[0071] TREOFe 2 O 3 SiO 2 CaO Al 2 O 3 82.500.060.050.070.05

[0072] Obtain 3.21L of filtrate containing neodymium praseodymium chloride with a concentration (TREO) of 110.5g / L. After heating the filtrate to 75℃, add saturated oxalic acid solution to crystallize and precipitate, filter to obtain neodymium pra...

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Abstract

The invention discloses a separating and recovering method for separating valuable components in rare earth praseodymium-neodymium fused salt electrolysis waste into a liquid phase (praseodymium-neodymium chloride) and a solid phase (praseodymium-neodymium fluoride) by adopting leaching by low-concentration hydrochloric acid. The method is characterized by comprising steps of raw materials processing, beating and leaching to obtain filter residues containing praseodymium-neodymium fluoride and filtrate containing praseodymium-neodymium chloride; the filter residues containing praseodymium-neodymium fluoride are washed to neutral and dried at the temperature of 60-80 DEG C to obtain praseodymium-neodymium fluoride; the filtrate containing praseodymium-neodymium chloride is subjected to crystallization and precipitation with an oxalic acid method to obtain praseodymium-neodymium oxalate, and the obtained praseodymium-neodymium oxalate is burnt at the temperature of 950 DEGC and degraded to obtain praseodymium-neodymium oxide. By means of the characteristic that rare earth fluoride does not react with hydrochloric acid, the low-concentration hydrochloric acid is used for leaching soluble impurities and oxides, a rare earth fluoride structure is not required to be damaged with high-temperature strong acid or strong base, and the valuable components are recycled; compared with the traditional concentrated sulfuric acid roasting method or strong base roasting method, the method omits a roasting process, a follow-up feed liquid is not required to be subjected to an extraction process, so that the method has the characteristics of simple process, short process flow, low cost, high yield and environment-friendliness, and the fluorine element is recycled efficiently.

Description

Technical field [0001] The invention relates to a method for separating and recovering valuable components in rare earth waste residue, in particular to a method for separating and recovering valuable components in rare earth praseodymium fused salt electrolysis waste, in particular to a method for leaching with low concentration hydrochloric acid Extraction, separation and recovery of valuable components in the rare earth neodymium praseodymium molten salt electrolysis waste into liquid phase (neodymium praseodymium chloride) and solid phase (neodymium praseodymium fluoride). Background technique [0002] Because of their special electronic structure, rare earth elements have the characteristics of 4f orbitals that are not full of electrons and lanthanide shrinkage, and they have optical, electrical, magnetic and thermal effects that other elements do not have. They are called "the treasure house of new materials". It is widely used in industries such as permanent magnets, metal...

Claims

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Application Information

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IPC IPC(8): C22B7/00
CPCY02P10/20
Inventor 肖勇陈月华许鸽鸣朱焱任萍崔小震
Owner YIYANG HONGYUAN RARE EARTH
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