Process of directly preparing rare-earth compound from extraction separation load organic phase

A technology of rare earth compounds and organic phases, which is applied in the field of rare earth compound preparation, rare earth hydrometallurgy and the preparation of rare earth compounds, can solve the problems of medium and heavy rare earth stripping difficulties, large acid consumption, particle agglomeration, etc. The effect of removing organic phase saponification process, reducing mutual adsorption, and uniform particle size distribution

Inactive Publication Date: 2009-12-16
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of the present invention is to provide a process for directly preparing rare earth compounds by extracting and separating the loaded organic phase, which saves the rare earth stripping in the loaded organic and consumes a large amount of acid, solves the difficulty of medium and heavy rare earth stripping, and the residual acid in the stripping liquid is high. For the problem of large acid consumption, if the organic phase after precipitation of rare earth contains sodium or ammonia ions, it can be directly returned for rare earth extraction and separation, saving the saponification process of the organic phase and saving a large amount of alkali required for the saponification of the organic phase; The problem of particle agglomeration and uneven particle size distribution in the preparation process of rare earth materials can obtain evenly distributed rare earth compound materials, which meets the requirements of the continuously developing rare earth material applications

Method used

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  • Process of directly preparing rare-earth compound from extraction separation load organic phase

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Effect test

Embodiment 1

[0032] LaCePrNd rare earth chloride solution (acidity is 0.00001mol / L, rare earth content is 1.5mol / L REO), containing NH 4+ The P507 extraction agent concentration is 1.5mol / L (diluent is kerosene) and acidity is that the hydrochloric acid washing liquid of 5.0mol / L is added in the 70-stage extraction tank and carries out Ce / Pr cascade fractionation extraction separation; Part of the organic phase of praseodymium and neodymium is continuously drawn into the settling tank, and a theoretical amount of 130% ammonium bicarbonate (concentration is 0.1wt%) solution is added, stirred for 1 hour at a temperature of 40° C., and the precipitated slurry is obtained by suction filtration. The rare earth filter cake is washed with kerosene and ethanol, dried by azeotropic distillation, and calcined at 900°C for 3 hours to obtain praseodymium and neodymium oxide powder. The particle size test results are shown in Table 1. Contains NH 4+ The P507 organic phase is directly returned to the ...

Embodiment 2

[0034] LaCePrNd sulfuric acid rare earth solution (acidity is 0.0001mol / L, rare earth content is 0.1mol / L REO), containing Na + The P204 (40%vol) and P507 (60%) mixed extractant (diluent is kerosene) concentration is that 1.5mol / L, acidity are that the hydrochloric acid wash of 5.5mol / L is added in 70 grades of extraction tanks respectively and carries out Ce / Pr cascade fractional distillation extraction and separation; at 65 grades, part of the organic phase loaded with cerium is continuously drawn into the settling tank, and a theoretical amount of 120% sodium carbonate (concentration is 30wt%) solution is added, and stirred for 2 hours at a temperature of 20°C. The precipitated slurry was suction filtered to obtain a rare earth carbonate filter cake, washed with kerosene, and dried in vacuum to obtain praseodymium and neodymium carbonate powder. The particle size test results are shown in Table 1. Contains Na + After standing and stratifying, the mixed extractant is direc...

Embodiment 3

[0036] LaCe rare earth chloride solution (acidity is 0.001mol / L, rare earth content is 1.4mol / L REO), containing Na + The P204 extraction agent concentration is 1.3mol / L (diluent is kerosene) and acidity is that the hydrochloric acid washing solution of 5.5mol / L is added respectively in the 60-stage extraction tank and carries out La / Ce cascade fractionation extraction separation; Part of the organic phase of cerium is continuously drawn into the settling tank, and a mixed solution of sodium carbonate and oxalic acid (the molar ratio is 1:1, and the average concentration is 15wt%) is added in a theoretical amount of 100%, and stirred for 1 hour at a temperature of 65°C. After precipitation, The slurry was suction filtered to obtain a rare earth carbonate filter cake, washed with ethanol, and dried by azeotropic distillation to obtain cerium carbonate powder. The particle size test results are shown in Table 1. Contains Na + The P204 organic phase is directly returned to the e...

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Abstract

The invention provides a process of directly preparing a rare-earth compound from an extraction separation load organic phase. The process comprises following steps: carrying out a mixed precipitation reaction between a precipitator solution and the load organic phase which is obtained from extraction separation and contains rare-earth; post-treating the filter cake obtained by filtering slurry liquid so as to obtain the rare-earth compound with good dispersity and uniform particle size distribution; and returning the organic phase to the extraction separation working procedure for recycling use. The process of extracting and separating rare-earth omits the rare-earth stripping step, saves a great amount of acid needed by the rare-earth in a stripping load organic phase and solves the problems of stripping difficulty of medium-heavy rare-earth, high spent acid of a stripping solution, and the like. The invention uses the precipitator to precipitate the rare-earth from the organic phase, and the whole precipitation reaction is carried out on an oil-water interface to effectively control the grain size. Meanwhile, a trace organic phase is attached to grain surfaces and is used as a surface active agent to reduce the mutual adsorption action of grains for deflocculation. The invention can obtain products with good dispersity and uniform grain size distribution, thereby being a new method for preparing a high-quality rare-earth compound material. The invention has simple process, is easy to realize the industrialized production and has low production cost.

Description

technical field [0001] The invention relates to a preparation method of rare earth compounds and a new process for extracting and separating rare earths from rare earth feed liquid, and belongs to the field of rare earth hydrometallurgy and the preparation of rare earth compounds. Background technique [0002] The special electronic configuration of rare earth elements makes them have special optical, electrical and magnetic properties, and is known as a treasure house of new materials. Rare earth and its compound powders are not only a new material, but also can be used as raw materials for new materials. They have important applications in luminescent materials, magnetic materials, hydrogen storage materials, high-temperature superconducting materials, etc. There have been many reports on the preparation and performance of rare earth compound powders, and there are many preparation methods, such as hydrolysis, alkoxide, thermal decomposition, explosion, homogeneous precipi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00C22B3/32C22B3/38
CPCY02P10/20
Inventor 黄小卫龙志奇韩业斌张顺利崔大立彭新林
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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