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A kind of production method of fine-grained low-chloride rare earth carbonate

A rare earth carbonate and production method technology, applied in the fields of rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of polluting the environment, affecting the recovery rate of rare earth, etc., achieve the effect of less washing water and realize continuous production

Active Publication Date: 2017-03-01
NAT ENG RES CENT OF RARE EARTH METALLURGY & FUNCTION MATERIALS
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Problems solved by technology

[0003] The Chinese patent "Ultrasonic-assisted oxalate precipitation to produce low-chloride fine-grained high-purity rare earth compounds" (CN102978399A) invented a method of using oxalic acid and its salts to directly precipitate rare earths to produce low-chloride fine-grained rare earth compounds, but the price of oxalic acid is high Toxicity will pollute the environment, and the solubility of oxalate will affect the recovery rate of rare earths; Chinese patent "Production method of high bulk density fine particle low chloride rare earth carbonates and oxides" (CN 103708525A) is based on the phase between rare earth carbonates Transformation characteristics, using alkali solution to treat rare earth carbonate to prepare fine-grained low chloride basic rare earth carbonate method, the chloride content is above 160ppm

Method used

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  • A kind of production method of fine-grained low-chloride rare earth carbonate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take 200 mL of pure water and place it in the precipitation reaction device. At the same time, add 5 g of lanthanum carbonate to the pure water as a seed crystal, heat the solution in the reaction device to a constant temperature of 50 °C, and add lanthanum chloride material with a concentration of 40 g / L Both the ammonium bicarbonate solution and the ammonium bicarbonate solution with a concentration of 80 g / L were simultaneously fed in parallel at a feeding rate of 6 mL / min. After stirring the reaction system for 20 min, the valve at the bottom of the reaction device was opened to allow the suspension to Discharge at a discharge rate of 12 mL / min, filter, and wash with normal temperature water until the filtrate does not become turbid in contact with the silver nitrate solution, and the obtained solid is a fine-grained low-chloride lanthanum carbonate product. The total amount of rare earth in the lanthanum carbonate product is 50.31%, the chloride radical contained in...

Embodiment 2

[0030] Take 200 mL of pure water and place it in the precipitation reaction device, add 5 g of cerium carbonate as a seed crystal to the pure water at the same time, heat the solution temperature in the reaction device to a constant temperature of 60 °C, and transfer the cerium chloride material with a concentration of 60 g / L The ammonium bicarbonate solution and the ammonium bicarbonate solution with a concentration of 80 g / L were fed in parallel flow at the feeding speed of 5 mL / min and 3 mL / min respectively. After stirring the reaction system for 30 min, the valve at the bottom of the reaction device was opened. The suspension was discharged at a discharge rate of 8 mL / min, filtered, and washed with normal temperature water until the filtrate contacted with the silver nitrate solution did not produce turbidity, and the obtained solid was a fine-grained low-chloride cerium carbonate product. The total amount of rare earth in the cerium carbonate product is 51.12%, the chlorid...

Embodiment 3

[0032] Take 200 mL of pure water and place it in the precipitation reaction device. At the same time, add 5 g of yttrium carbonate to the pure water as a seed crystal, heat the solution in the reaction device to a constant temperature of 60 °C, and transfer the yttrium chloride material with a concentration of 60 g / L to The ammonium bicarbonate solution and the ammonium bicarbonate solution with a concentration of 100 g / L were simultaneously fed in a co-current manner at a feeding rate of 6 mL / min and 3 mL / min, respectively. After stirring the reaction system for 30 min, the valve at the bottom of the reaction device was opened. The suspension was discharged at a discharge rate of 9 mL / min, filtered, and washed with normal temperature water until the filtrate contacted with the silver nitrate solution did not produce turbidity, and the obtained solid was fine-grained and low-impurity yttrium carbonate product. The total amount of rare earths in the yttrium carbonate product is ...

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Abstract

The invention relates to a production method and device of fine-grained low-chloride rare earth carbonate. The production method is mainly characterized in that rare earth chloride and a carbonate solution are added in a concurrent flow feeding way on a designed special precipitation reaction device, the spatial separation of a reaction zone and a crystallization zone is realized by controlling the feeding speed and discharging speed and controlling the aging time of rare earth carbonate, and thus the double purposes of directly obtaining a fine-grained low-chloride rare earth carbonate product from a hydrochloric acid medium by precipitation and realizing continuous production are achieved. By adopting the production method and device provided by the invention, the fine-grained rare earth carbonate product with the chloride content of less than 50ppm can be directly obtained from the hydrochloric acid medium by using cheap ammonium bicarbonate, the precipitation reaction device has a simple structure, and the continuous production can be realized.

Description

technical field [0001] The invention relates to a production method of fine-grained low-chloride rare earth carbonate, which belongs to the field of rare earth hydrometallurgy and rare earth materials. Background technique [0002] Rare earth carbonate is used as a precursor for the preparation of rare earth phosphors, rare earth polishing powders, rare earth permanent magnet materials, hydrogen storage materials and structural materials, and various quality indicators are the main factors affecting its physical and chemical properties. In addition to the basic requirements for the chemical composition of rare earth products, many rare earth application companies have also put forward new and higher requirements. For example: In recent years, the price instability of rare earth products has forced rare earth application enterprises to reduce the amount of rare earth as much as possible to achieve the purpose of saving costs. The amount of rare earth can be reduced by further...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
CPCC01F17/36C01P2004/61
Inventor 田皓许延辉周建鹏赵文怡马升峰张旭霞王英杰
Owner NAT ENG RES CENT OF RARE EARTH METALLURGY & FUNCTION MATERIALS
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