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Method for preparing micron gadolinium oxide with center particle size of 20-60 micrometers

A technology of center particle size and gadolinium oxide, which is applied in chemical instruments and methods, rare earth metal oxides/hydroxides, inorganic chemistry, etc., can solve the problems of high content of non-rare earth impurities, difficulty in seed crystal preparation, and difficult control of precipitation process and other problems, to achieve the effect of simple process and good reproducibility

Active Publication Date: 2016-11-09
FUJIAN CHANGJIANG GOLDEN DRAGON RARE EARTH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ammonium bicarbonate or ammonium salt will produce a large amount of ammonia nitrogen wastewater, which will bring great difficulties to the wastewater standard; sodium carbonate precipitation will have high content of non-rare earth impurities (sodium, iron, chloride, etc.), which cannot meet the requirements of high-grade gadolinium oxide products. Control requirements for non-rare earth impurities
The method of adding seed crystals at the same time, first of all, to obtain better seeds, but the preparation of seed crystals is difficult, and the precipitation process is not easy to control

Method used

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  • Method for preparing micron gadolinium oxide with center particle size of 20-60 micrometers
  • Method for preparing micron gadolinium oxide with center particle size of 20-60 micrometers
  • Method for preparing micron gadolinium oxide with center particle size of 20-60 micrometers

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Experimental program
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Effect test

Embodiment 1

[0015] Add 500ml pure water or deionized water in advance in the precipitation reactor, adjust acidity to be 0.5mol / L, temperature is 50 ℃, stir, and gadolinium chloride (concentration 0.63mol / L, feed liquid acidity 3.5mol / L) and Oxalic acid (concentration 120g / L) according to the stoichiometric ratio n(GdCl 3 ) / n(H 2 C 2 o 4 )=1 / 1.50, the feed liquid advances into the reactor for 30s, and the oxalic acid enters later, the flow rate of the gadolinium chloride solution is kept at 20mL / min, the flow rate of the precipitant oxalic acid solution is 21.0ml / l, after the precipitation is completed, the temperature is raised to 100°C, kept for 10h, and controlled The acidity of mother liquor is 6.8mol / L. Filter, wash 8 times, and keep warm at 950°C for 3 hours. Detect electron microscope, particle size, non-rare earth impurities (Fe, Si, Ca, Cl, Na) content in the following table, and refer to figure 1 and figure 2 .

[0016]

Embodiment 2

[0018] Add 500ml of pure water or deionized water in advance in the precipitation reactor, adjust the acidity to be 1mol / L, the temperature is 50 ℃, stir, mix gadolinium chloride (concentration 0.52mol / L, acidity 4.2mol / L) and oxalic acid (concentration 120g / L) according to the stoichiometric ratio n(GdCl 3 ) / n(H 2 C 2 o 4 )=1 / 1.52, the feed liquid advances into the reactor for 30s, and the oxalic acid enters later, the flow rate of the gadolinium chloride solution is kept at 15mL / min, the flow rate of the precipitant oxalic acid solution is 12.5ml / L, after the precipitation is completed, the temperature is raised to 100°C, kept for 6h, and controlled The acidity of the mother liquor is 7.1mol / L. Filter, wash 8 times, and keep warm at 950°C for 3 hours. Detect electron microscope, particle size, non-rare earth impurities (Fe, Si, Ca, Cl, Na) content in the following table, and refer to image 3 and Figure 4 .

[0019]

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Abstract

The invention relates to a method for preparing micron gadolinium oxide with center particle size of 20-60 micrometers. The method comprises the following steps: adding acidic water in a reactor, gradually adding chlorinated gadolinium material liquid with adjusted acidity and oxalic acid in a reactor by employing a concurrent flow mode according to the stoichiometric ratio, controlling the reaction temperature at 50-80 DEG C, heating the material to 100 DEG C after the reaction is complete, insulating the material for 6-10 hours, controlling the mother liquor terminal point acidity at 5-8 mol / L, filtering the material and washing, and calcinaing the material for 3 hours at the temperature of 850-950 DEG C to obtain the large granular gadolinium oxide powder with D50:20-60 [mu]m. The method has the advantages of simple process, good reappearance, no environmental protection pressure, and little non-rare earth impurities (Fe, Si, Ca, Cl, Na) content in the product, requirements of different grades of gadolinium oxide for granularity control can be satisfied, and the method has industrial value.

Description

technical field [0001] The invention relates to a preparation method of gadolinium oxide with a central particle diameter of 20-60 microns. Background technique [0002] Gadolinium oxide is widely used in catalysis, ceramics, glass industry, solid oxide fuel cells, luminescent materials, polishing materials and nuclear materials and other fields. Large particle gadolinium oxide is often used in the electrolysis of metal gadolinium. Large particle size, good particle size distribution, high bulk density and good fluidity can prevent splashing during electrolysis. Gadolinium oxide can also be used as a main component in solid fuel cells. With the development of science and technology, manufacturers have higher requirements on the physical properties of gadolinium oxide. Less reported. Most of the currently disclosed large-grain rare earth oxide powder preparation technologies use ammonium bicarbonate and sodium carbonate as precipitants, and sometimes other substances such ...

Claims

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Application Information

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IPC IPC(8): C01F17/00
CPCC01F17/206C01P2004/03C01P2004/61
Inventor 朱世清周晓宏喻小珍傅志勤曾辉辉
Owner FUJIAN CHANGJIANG GOLDEN DRAGON RARE EARTH CO LTD