Rare earth precipitation device and rare earth precipitation method

A precipitation device and rare earth technology, applied in the direction of improving process efficiency, can solve problems such as unstable crystal quality of rare earth, achieve uniform pH distribution in liquid phase, improve operating environment, and improve use efficiency.

CN109022767APending Publication Date: 2018-12-18CHINA ENFI ENGINEERING CORPORATION
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2018-12-18

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Abstract

The invention provides a rare earth precipitation device and a rare earth precipitation method. The rare earth sedimentation device comprises a precipitation container, a feeder, a stirrer and a sealing cover; the precipitation container is provided with a body and a containing cavity defined by the body; the feeder is used for supplying rare earth liquid and a precipitating agent to the containing cavity of the precipitation container; the stirrer is provided with a stirring paddle, and the stirring paddle is arranged in the containing cavity; and the sealing cover is detachably arranged at the top of the body to seal the containing cavity. According to the rare earth precipitation device and the rare earth precipitation method, through the arrangement of the sealing cover, the pressure in a reaction space is increased, the forward implementation of a precipitation reaction is strengthened, the formation of crystallites is promoted, meanwhile, the growth rate of precipitated crystalsis decreased, precipitated samples are relatively small in particle size and low in crystallization rate, and fewer impurities are contained in the precipitated samples; then closed operation can improve the operating environment, the precipitating agent and the rare earth liquid participate in the reaction in a relatively stable ratio, and the use efficiency of the precipitating agent is improved; and finally, the closed operation can increase the stirring strength, liquid-phase pH distribution is uniform, and crystal particle size growth is promoted to be more uniform.
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Description

technical field

[0001] The invention relates to the field of rare earth production, in particular to a rare earth precipitation device and a rare earth precipitation method. Background technique

[0002] After the rare earth ore goes through the leaching and extraction steps in the later stage of the production process, the rare earth feed liquid needs to be purified by precipitation. In the precipitation process, there are positive sequence feeding, co-feeding and reverse sequence feeding. Different feeding methods have effects on the crystal form, crystal size and distribution of the precipitate. Adding the rare earth precipitant to the rare earth feed liquid in the forward sequence feeding or adding the rare earth feed liquid to the rare earth precipitant in the reverse sequence feeding will affect the precipitation quality of rare earth precipitated crystals due to the high concentration of a certain reactant in the local area, and then affect the subsequent filtration ...

Examples

Embodiment 1

[0062] use figure 1 The rare earth precipitation device shown performs the following process.

[0063] Rare earth solution (concrete composition is shown in table 1) and rare earth precipitating agent (concentration is the ammoniacal liquor of 12wt%) by feeder respectively by the rate of 10mL / min and 9mL / min into the settling tank, rare earth precipitating agent in The injection surface at the bottom of the precipitation container and the injection surface of the rare earth solution at the bottom of the precipitation container overlap by 70-95%. The precipitation temperature is set at 50°C, and the temperature is regulated by a temperature controller; after the precipitation is completed, continue to keep warm for 30 minutes. During the precipitation process, the sedimentation tank is sealed with an air condensation hood, and the pressure controller is used to adjust the pressure of the closed environment to 0.1MPa. During the precipitation process, the pH value of the materi...

Embodiment 2

[0071] Rare earth solution (concrete composition as shown in table 1) and rare earth precipitant (concentration is the ammonium aqueous solution of 14wt%) are squeezed in the precipitation tank by the speed of 10mL / min and 9mL / min respectively by feeder, and precipitation temperature is set Set at 90°C, and use the temperature controller to adjust the temperature to adjust the precipitation; after the precipitation is completed, continue to keep warm for 30 minutes. During the precipitation process, the sedimentation tank is sealed with an air condensation hood, and the pressure of the closed environment is adjusted to 0.15MPa by a pressure controller. During the precipitation process, the pH value of the material is monitored by a pH meter, and the pH value is controlled between 7 and 8. During the precipitation process, the motor drives the stirring paddle to rotate, and the clockwise and counterclockwise rotation speeds are 20 to 300 rpm. The chemical composition of the pre...

Embodiment 3

[0077] The difference from Example 1 is that the precipitation temperature is set at 60°C. The rare earth precipitation agent is oxalic acid with a concentration of 0.25-0.35 mol / L. The chemical composition of the precipitated samples analyzed by XRF is shown in Table 7. The particle size analysis method is the same as above, and the particle size distribution information is shown in Table 6.

[0078] Table 6

[0079] Median diameter (D50): 14.01μm