Method for preparing high-purity terbium oxide

A terbium oxide, high-purity technology, applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problems of high cost, many influencing factors, many steps, etc., to reduce preparation costs, reduce process steps, and process short step effect

Active Publication Date: 2015-01-21
CHINALCO RARE EARTH CHANGSHU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of this method is that there are many steps. It takes three or three steps only for extraction and separation, and each step needs to use acid and alkali to saponify and back-extract, and there are many steps. The precious terbium element is pressed in each process equipment. The quantity will increase, so the cost of the whole process is also high
It can be seen that although a single pure terbium oxide can be obtained directly through extraction and separation, the process is too complicated, and the more steps in the process, the more factors affecting the final high-purity terbium oxide
[0007] In view of this, the problem of how to find a reasonable balance between simplifying the process and shortening the process steps and obtaining high-purity terbium oxide has long puzzled the industry, and it is expected to be resolved, but in the patent and non-patent literature disclosed so far There is no technical enlightenment that can be used for reference. For this reason, the applicant has made persistent and beneficial explorations, and finally found a solution to the problem, and formed the technical solution that will be introduced below

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A) Prepare the mixed rare earth chloride solution, and put the mixed rare earth oxide obtained from the commercial channels, 30% hydrochloric acid with a mass percentage concentration of 30%, and pure water, ie deionized water, into a stirring device and heating at a weight ratio of 1:2:2 The container of the device is stirred in a heated stirred tank to dissolve the mixed rare earth oxide, and the mixed rare earth chloride solution is obtained after filtration. In this step, the stirring speed of the stirring device is controlled to 150rpm, the stirring time is controlled to 8h, and the heating device The heating temperature is controlled to 70°C, and the mixed rare earth oxide is preferably an ionic mixed rare earth oxide from southern China;

[0025] B) Prepare the separation material, add the mixed rare earth chloride solution obtained in step A) into a container with a stirring device such as a stirred tank for continuous stirring, and add dropwise to a mass percentage...

Embodiment 2

[0031] Only change the weight ratio of mixed rare earth oxide, hydrochloric acid and deionized water in step A) to 1:3:1.5, the mass percentage concentration of hydrochloric acid to 27%, the stirring speed to 120rpm, and the stirring time to 10h , The heating temperature is changed to 60℃; the mass percentage concentration of liquid caustic soda in step B) is changed to 32%, the pH value is changed to 3.5, the dripping time of liquid caustic soda is changed to 1h, and the stirring speed is changed to 150rpm, Change the stirring time to 1h and the molar concentration of the separated material to 1.755 mol; change the volume ratio of the separated material, the first extractant, the liquid caustic soda and the counter liquid in step C) to 1:6.5:0.8: 1. Change the mass percentage concentration of liquid caustic soda to 17%, and change the mass percentage concentration of the reverse liquid that is the hydrochloric acid solution to 17%, change the stirring speed of the stirring devi...

Embodiment 3

[0033] Only change the weight ratio of mixed rare earth oxide, hydrochloric acid and deionized water in step A) to 1:2.5:1.8, the mass percentage concentration of hydrochloric acid to 28.5%, the stirring speed to 80rpm, and the stirring time to 12h , The heating temperature is changed to 80℃; the mass percentage concentration of liquid caustic soda in step B) is changed to 31%, the pH value is changed to 3, the dripping time of liquid caustic soda is changed to 1.5h, and the stirring speed is changed to 120rpm , Change the stirring time to 2h, and the molar concentration of the separated material to 1.7mol; change the volume ratio of the separated material, the first extractant, the liquid caustic soda and the anti-liquid in step C) to 1:6:0.65 : 0.8, change the mass percentage concentration of liquid caustic soda to 18%, and change the mass percentage concentration of the reverse liquid, that is, the hydrochloric acid solution, to 16%, change the stirring speed of the stirring ...

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Abstract

The invention discloses a method for preparing high-purity terbium oxide, belonging to the technical field of rare-earth separation. The method comprises the following steps of feeding mixed rare-earth oxide, hydrochloric acid and pure water into a container with a stirring device and a heating device, stirring, and filtering so as to obtain a mixed rare-earth chloride solution; adding the mixed rare-earth chloride into another container with a stirring device, and continuously stirring so as to obtain a separated material; by taking the separated material as a raw material, continuously extracting and separating by using a first extraction agent, a caustic soda liquid and a returning fluid so as to obtain a rich terbium chloride solution; by taking the rich terbium chloride solution as another raw material, adding a second extraction agent and the returning fluid, further extracting and separating so as to obtain a high-purity terbium chloride solution; introducing the high-purity terbium chloride solution into a settling pond, and filtering so as to obtain solid oxalate terbium; and introducing the solid oxalate terbium into a roller table type tunnel kiln for firing, controlling the firing temperature and the firing time, discharging from the roller table type tunnel kiln so as to obtain high-purity terbium oxide, wherein the purity of the terbium oxide is 99.9%. The first-pass yield is high, and the preparation cost is low.

Description

Technical field [0001] The invention belongs to the technical field of rare earth separation, and specifically relates to a preparation method of high-purity terbium oxide. Background technique [0002] Terbium Oxide (Terbium Oxide) is a rare earth oxide, chemical formula: Tb 4 O 7 , Molecular weight 747.70; density: 7.3g / cm 3 ; Melting point: 2340℃; Properties: brown powder; Physicochemical properties: insoluble in water and alkali but soluble in acid. [0003] As a main functional material, terbium oxide is used to make metal terbium, magneto-optical glass, phosphor, magneto-optical storage materials, chemical additives, etc. [0004] Terbium is a medium and heavy rare earth among the fifteen rare earth elements, and its content in the earth's crust is very low, only 1.1ppm. Even in the high yttrium ion type heavy rare earth ore containing the highest terbium, the content of terbium only accounts for the total rare earths 1.1-1.2% of The content of terbium in the general yttrium-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
Inventor 钱建平钱建龙
Owner CHINALCO RARE EARTH CHANGSHU
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