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Method for preparing high-purity terbium oxide

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

Active Publication Date: 2014-01-01
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, put the mixed rare earth oxide obtained from commercial channels, hydrochloric acid with a mass percentage concentration of 30%, and pure water (deionized water) in a weight ratio of 1:2:2 into a stirring device and heating The container of the device is stirred in a heating and stirring tank, so as to dissolve the mixed rare earth oxide, and obtain a mixed rare earth chloride solution after filtration. In this step, the stirring speed of the stirring device is controlled to be 150rpm, and the stirring time is controlled to be 8h. The heating temperature is controlled at 70°C, and the mixed rare earth oxide is preferably an ionic mixed rare earth oxide in southern my country;

[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 stirring tank for continuous stirring, and add it dropwise in a state of continuous stirring w...

Embodiment 2

[0031] Only change the weight ratio of mixed rare earth oxides, hydrochloric acid and deionized water in step A) to 1:3:1.5, change the mass percentage concentration of hydrochloric acid to 27%, change the stirring speed to 120rpm, and change the stirring time to 10h , the heating temperature is changed to 60°C; the mass percentage concentration of the liquid caustic soda in step B) is changed to 32%, the pH value is changed to 3.5, the dripping time of the liquid caustic soda is changed to 1h, and the stirring speed is changed to 150rpm, Change the stirring time to 1h, and change the molar concentration of the separation material to 1.755mol; change the volume ratio of the separation material, the first extraction agent, liquid caustic soda and the reverse 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%...

Embodiment 3

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

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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 in particular relates to a preparation method of high-purity terbium oxide. Background technique [0002] Terbium oxide (Terbium Oxide) belongs to rare earth oxides, chemical formula: Tb 4 o 7 , molecular weight 747.70; density: 7.3g / cm 3 ; Melting point: 2340℃; Properties: brown powder; Physical and chemical 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 powder, magneto-optic storage materials, chemical additives, etc. [0004] Terbium is a medium-to-heavy rare earth element among the fifteen rare earth elements, and its content in the earth's crust is very low, only 1.1ppm. 1.1-1.2% of the total. The content of terbium in general medium-yttrium and europium-rich materials is 0.6-0.8%. As for the content of terbium in northern my country, whi...

Claims

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Application Information

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