Alkaline process for preparing europium oxide in fluorescence level

A technology for preparing fluorescent grade, europium oxide, applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problems of large investment and complicated operation, and achieve the effect of remarkable economic benefit, good effect and low production cost.

Inactive Publication Date: 2004-06-02
包头钢铁公司稀土研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the rare earth impurities can generally be removed after the alkalinity method is adopted, and the non-rare earth impurities are not only unable to be removed, but a large amount of non-rare earth impurities are also introduced due to the reduction of zinc powder
The reduction extraction method is suitable for large-scale enterprise production due to its large investment and complicated operation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The chloride solution containing 60% of europium oxide obtained from the three outlets of samarium, europium and gadolinium, through Zn powder reduction-alkalinity method, the alkali cake obtained is dissolved with hydrochloric acid, and the concentration of europium chloride solution is adjusted to be 0.3mol / L, and the pH value is 4. The temperature is 18°C, add 13mmol M2S (M + =Na + or NH 4 + , made into a dilute solution with a concentration of less than 1mmol / L), fully stirred, and the pH after the reaction was controlled to be 5-6. After the supernatant was checked for no precipitation, filtered, the filtrate was heated to 60°C, and the pH was adjusted to 1-1.5 , carry out oxalate precipitation, filter, wash with water, burn, and prepare fluorescent grade europium oxide.

[0015] Its non-rare earth impurity content is as follows:

[0016] CaO 4.8ppm, Fe 2 o 3 1.1ppm, ZnO 4.5ppm, PbO<1ppm, CuO<1ppm, CoO<1ppm, NiO<1ppm.

Embodiment 2

[0018] The chloride solution containing 60% of europium oxide obtained from the three outlets of samarium, europium and gadolinium, through Zn powder reduction-alkalinity method, the alkali cake obtained is dissolved with hydrochloric acid, and the concentration of europium chloride solution is adjusted to be 0.4mol / L, and the pH value is 3. The temperature is 22°C, add 18mmolM to each liter of europium chloride solution 2 S, the temperature of oxalate precipitation is 75°C, and fluorescent grade europium oxide is prepared.

[0019] Its non-rare earth impurity content is as follows:

[0020] CaO 4.5ppm, Fe 2 o 3 0.65ppm, ZnO 4.1ppm, PbO<1ppm, CuO<1ppm, CoO<1ppm, NiO<1ppm.

Embodiment 3

[0022] The process is the same as in Example 1. The crude europium containing 80% europium oxide is obtained from the samarium europium gadolinium enrichment through the europium sulfate method, dissolved with nitric acid, and after the Zn powder reduction-alkalinity method, the alkali cake is dissolved with nitric acid to adjust The concentration of europium nitrate solution is 0.4mol / L, the pH value is 2, and the temperature is 25°C. Add 26mmolM to each liter of europium nitrate solution 2 S, oxalate precipitation was carried out at 65°C to prepare fluorescent grade europium oxide.

[0023] Its non-rare earth impurity content is as follows:

[0024] CaO 4.9ppm, Fe 2 o 3 0.76ppm, ZnO 4.7ppm, PbO<1ppm, CuO<1ppm, CoO<1ppm, NiO<1ppm.

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Abstract

The present invention is one wet chemical separation process and can produce product of fluorescence level through eliminating non-rare earth impurity in europium chloride or europium nitrate solution. The europium chloride or europium nitrate solution with the rare earth impurity eliminated through alkaline process is further processed through addition of inorganic sulfide solution, once oxalate precipitation and once burning to prepare europium oxide in fluorescence level. The process has low cost, simple operation and stable product quality.

Description

1. Technical field: [0001] The invention belongs to a wet chemical separation process, which uses an inorganic sulfide and oxalate precipitation separation alkalinity method to remove non-rare earth impurities in europium (III) solution after rare earth impurities, and prepares fluorescent grade europium oxide. 2. Background technology: [0002] At present, the domestic preparation of fluorescent grade europium oxide mainly adopts alkalinity method and reduction extraction method. The alkalinity method is suitable for the production of small and medium-sized rare earth enterprises because of its low investment and simple operation. However, the rare earth impurities can generally be removed after the alkalinity method is adopted, and the non-rare earth impurities are not only unable to be removed, but a large amount of non-rare earth impurities are also introduced due to the reduction of zinc powder. The reduction extraction method is suitable for large-scale production due...

Claims

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Application Information

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IPC IPC(8): C01F17/00
Inventor 李梅满拥军叶祖光冷忠义
Owner 包头钢铁公司稀土研究院
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