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RE salt preparing process and apparatus

A technology of rare earth salts and rare earths, applied in the fields of rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of storage, huge reaction equipment, fluctuations in the crystallization process of rare earth salts, increase product quality, etc., and reduce the process Steps and times of solid-liquid separation, eliminate the reaction time of dissolution, and ensure the effect of the wastewater treatment process

Active Publication Date: 2006-10-18
CHINA NORTHERN RARE EARTH (GROUP) HIGH TECH CO LTD
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0003] In the existing precipitation process, with the addition of the precipitant, the precipitation conditions at different stages are changing, causing changes in the formation of rare earth salts, and as the concentration of the rare earth solution decreases, the addition rate of the precipitant increases or the overall addition is excessive, and finally Causes fluctuations in the crystallization process of rare earth salts, resulting in inconsistent product quality
As far as multiple batches are concerned, due to the inability to achieve consistent operations, there are also differences between batches, which increases the fluctuation of product quality
[0004] Using the existing technology to make rare earth salts usually adopts direct mixing and batch operation, and the formation process takes a long time. Rare earth salts are easy to form peritectic, adsorption and other auxiliary processes, resulting in difficult product quality control, large quality fluctuations, and poor consistency.
In addition, the adoption of intermittent operation process will inevitably lead to increased storage and transshipment volume before and after the process, huge storage and reaction equipment, and a large overall investment
In the precipitation (transformation) process, a large amount of corresponding non-rare earth salt solution is formed, and the concentration is low and it is not easy to recycle.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0026] Example 1: Process steps of continuous precipitation method for producing mixed rare earth carbonate with rare earth sulfate solution:

[0027] (1) Prepare the mixed solution of rare earth sulfate with a concentration of 0.04-O.3 mol / l, and at the same time prepare the precipitation agent ammonium bicarbonate at a concentration of 1-1.5 mol / l;

[0028] (2) Pass the prepared rare earth sulfate and rare earth mixed solution through the raw material inlet 9 and the ammonium bicarbonate solution through the reagent inlet 18 according to the mass flow ratio: RE0:NH 4 HCO 3 =1:1.3-1.7 into the mixing method submerged chamber 7, the temperature is 15-45℃, the rotation speed is 350-750 rpm, the vortex stirring paddle 6 is used to suck the above-mentioned raw materials and reagents into the cylinder 4 by the inclined stirring paddle 3 and The baffle 5 completes the mixing process, mixing for 3-12 minutes;

[0029] (3) The mixed rare earth carbonate produced by the reaction enters th...

Embodiment 2

[0031] Example 2: Process steps of continuous precipitation method for producing cerium carbonate with cerium nitrate solution:

[0032] (1) Prepare the cerium nitrate solution to a concentration of 0.1-1 mol / l, while preparing the precipitation agent ammonium bicarbonate to a concentration of 1-3.5 mol / l;

[0033] (2) Pass the cerium nitrate solution prepared above through the raw material feed port 9, and the ammonium bicarbonate solution through the reagent feed port 8 according to the mass flow ratio: REO:NH 4 HCO 3 =1:1.3-1.7 into the mixing method submerged chamber 7, the temperature is 25-50℃, the rotation speed is 255-600 rpm, the vortex stirring paddle 6 is used to suck the above-mentioned raw materials and reagents into the cylinder 4 by the inclined stirring paddle 3 and The baffle 5 completes the mixing process, mixing for 5-12 minutes;

[0034] (3) The mixed rare earth carbonate produced by the reaction enters the clarifier through the discharge port 1 of the mixer fo...

Embodiment 3

[0036] Example 3: Process steps of continuous precipitation method for producing rare earth oxalate using cerium chloride solution:

[0037] (1) Prepare the rare earth cerium chloride solution to a concentration of 0.04-O.6 mol / l, and at the same time prepare the precipitation agent oxalic acid to a concentration of 0.7-1.1 mol / l;

[0038] (2) Pass the prepared cerium chloride solution through the raw material feed port 9, and the oxalic acid solution through the reagent feed port 8 according to the mass flow ratio: REO:H 2 C 2 O 4 =1:1.1-1.6 into the mixing submerged chamber 7, the temperature is 15-75°C, the rotation speed is 180-325 rpm, the vortex stirring paddle 6 is used to suck the above-mentioned raw materials and reagents into the cylinder 4 by the inclined stirring paddle 3 and The baffle 5 completes the mixing process, mixing for 10-15 minutes;

[0039] (3) The cerium oxalate generated by the reaction enters the clarifier through the discharge port 1 of the mixer for se...

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Abstract

The present invention belongs to the field of non-ferrous metallurgy technology, and is especially RE salt preparing process and apparatus. The RE salt preparing process includes the following steps: compounding RE salt solution of 0.04-1.2 mol / l concentration and precipitant solution of 0.1-3.5 mol / l concentration; mixing the RE salt solution and precipitant solution in the mass flow rate between REO and precipitant of 1 to 1.1-1.7 at 15-60 deg.c temperature and 150-890 rpm rotation speed for 3-30 min; precipitating in a clarificator; injecting with one mud pump into a plate-frame press to obtain RE salt precipitate. The apparatus includes one barrel with material feeding port and precipitant feeding port in the bottom, eddy flow stirring rake, mixing sub chamber in the center and porous mist discharging plate in the upper part. The present invention realizes continuous production by means of the fast precipitation and solid-liquid separation.

Description

1. Technical Field [0001] The invention belongs to a non-ferrous metallurgical process, and relates to a preparation method and implementation device of rare earth salts. 2. Background technology [0002] The current production methods of rare earth salts (single element or mixed elements) mainly include the following two methods: (1) After the rare earth solution is formulated, the solid precipitation (conversion) agent is directly added to form the rare earth salt; (2) the rare earth solution After preparation, the precipitation (conversion) agent solution is directly added to form rare earth salts. [0003] In the existing precipitation process, with the addition of the precipitating agent, the precipitation conditions at different stages are changing, causing changes in the formation of rare earth salts. As the concentration of the rare earth solution decreases, the addition rate of the precipitating agent increases or the overall addition amount is excessive. This causes flu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
Inventor 赵治华王静李冬桑晓云
Owner CHINA NORTHERN RARE EARTH (GROUP) HIGH TECH CO LTD
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