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Method for preparing narrow-distributed ultra-fine yttrium oxide by sodium carbonate precipitation

A technology of sodium carbonate and yttrium carbonate, which is applied in chemical instruments and methods, rare earth metal oxides/hydroxides, inorganic chemistry, etc., can solve the problems of low concentration of reactants, narrow organic unity, and difficulty in scale, and achieve eradication Effects of ammonia nitrogen pollution, promotion of upgrading and easy industrialization

Active Publication Date: 2018-11-30
GANZHOU ZHANHAI IND & TRADING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the ammonium bicarbonate precipitation method commonly used in industry produces a large amount of ammonia nitrogen wastewater, and the concentration is dilute, so it is difficult to treat it up to the standard
Therefore, some enterprises use sodium carbonate, sodium bicarbonate and other precipitants instead. The unit consumption of sodium bicarbonate precipitation is high (6 mol sodium bicarbonate is required to precipitate 2 mol of yttrium), while the consumption of sodium carbonate to precipitate yttrium is low (only 3 mol is required to precipitate 2 mol of yttrium) Sodium carbonate), but the above-mentioned direct precipitation methods such as sodium carbonate and sodium bicarbonate all have the common problem that the direct addition of the precipitant will easily make the concentration of the local precipitant too high, resulting in uneven supersaturation, and it is difficult to achieve fine powder particle size and Organic unity with narrow distribution range, unable to controlly produce ultrafine yttrium oxide powder
In addition, the researchers used the homogeneous precipitation method to solve the problem. This method ensures that the precipitant is uniformly and slowly precipitated in the entire solution through chemical reactions, so that the supersaturation can be controlled within an appropriate range to achieve the goal of controlling the particle growth rate. The purpose is to obtain ultrafine particles with uniform particle size, compactness and high purity, but the disadvantages of this method are that the concentration of reactants is low, the yield is also low, and it is difficult to scale up; and the most commonly used precipitants are urea and hexamethylene tetra Amines, the inevitable introduction of ammonia nitrogen wastewater, limited industrial application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add bottom water to the reaction kettle, control the bottom water without the stirring blade, then add 0.1mol / L yttrium chloride feed solution and 0.2mol / L sodium carbonate solution in parallel to react, control the yttrium chloride feed liquid and sodium carbonate The feeding position of the solution is below the liquid level, and is distributed on opposite sides at the same time. The feeding rate of the yttrium chloride feed liquid is controlled to be 2.0mL / min, and the reaction temperature is 80 o C, the pH of the reaction process is 6.0, and the stirring speed is 350r / min. When the addition of yttrium chloride feed liquid is 300mL, the reaction is stopped, and the yttrium carbonate seed crystals obtained at this time have good crystallization properties. Filter and wash to obtain the filter cake, mix the above filter cake with water, control the slurry to pass through the stirring paddle blade, and then add 0.5mol / L yttrium chloride feed solution and 1.0mol / L sodium ...

Embodiment 2

[0038] Add the bottom water in the reactor, control the bottom water without the stirring paddle blade, then add 0.05mol / L yttrium chloride feed liquid and 0.05mol / L sodium carbonate solution in parallel to react, control the yttrium chloride feed liquid feed rate as 1.5mL / min, the reaction temperature is 80 o C, the pH of the reaction process is 5.8, and the stirring speed is 400r / min. When the addition of yttrium chloride feed liquid is 300mL, the reaction is stopped, and the yttrium carbonate seed crystals obtained at this time have good crystallization properties. Filter and wash to obtain the filter cake, mix the above filter cake with water, control the slurry to pass through the stirring paddle blade, and then add 0.2mol / L yttrium chloride feed solution and 0.3mol / L sodium carbonate solution in parallel to carry out precipitation reaction, control chlorine The feeding rate of yttrium feed solution is 3.0mL / min, and the precipitation temperature is 70 o C. The pH of the...

Embodiment 3

[0040] Add bottom water to the reaction kettle, control the bottom water without the stirring blade, then add 0.08mol / L yttrium chloride feed solution and 0.15mol / L sodium carbonate solution in parallel to react, control the yttrium chloride feed liquid and sodium carbonate The feeding position of the solution is below the liquid level, and is distributed on opposite sides at the same time. The feeding rate of the yttrium chloride feed liquid is controlled to be 1.0mL / min, and the reaction temperature is 75 o C, the pH of the reaction process is 5.8, and the stirring speed is 300r / min. When the addition of yttrium chloride feed solution is 300mL, the reaction is stopped, and the yttrium carbonate seed crystals obtained at this time have good crystallization properties. Filter and wash to obtain the filter cake, mix the above filter cake with water, control the slurry to pass through the paddle blade, and then add 0.5mol / L yttrium chloride feed solution and 0.8mol / L sodium carbo...

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PUM

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Abstract

The invention discloses a method for preparing narrow-distributed ultra-fine yttrium oxide by sodium carbonate precipitation. The method utilizes sodium carbonate as a precipitating agent and yttriumchloride as a material liquid and a parallel feeding method, strictly controls the conditions in seed crystal preparation, precipitation aging and staged roasting, especially controls the temperate and pH in the seed crystal preparation and precipitation aging and the temperature in the staged roasting, and prepares the narrow-distributed yttrium oxide powder with the primary particle sizes of less than or equal to 100nm, the secondary particle size D50 of less than or equal to 4 micrometers and (D90-D10) / (2D50) of less than 1.0. The method has the advantages of low cost, easy industrialization and removal of ammonia nitrogen pollution, can transform the advantages of China's plutonium resources into economic advantages and plays an important role in promoting the upgrading of the China'srare earth industry.

Description

technical field [0001] The invention relates to the field of rare earth hydrometallurgy, in particular to a method for preparing narrowly distributed ultrafine yttrium oxide by precipitation of sodium carbonate. Background technique [0002] Yttrium oxide is an important rare earth compound and a key basic raw material for the preparation of rare earth luminescent materials, crystal materials, ceramic materials, catalytic materials and other high-tech materials. With the continuous expansion of its application fields, the relationship between the full manifestation of the intrinsic properties of yttrium element and the material performance indicators has become more and more obvious. In the field of high-tech materials, the quality requirements for rare earth yttrium oxide powder have changed from simple chemical composition and purity requirements to crystal form, A change in the direction of taking into account the control of physical properties such as particle size and d...

Claims

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Application Information

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IPC IPC(8): C01F17/00B82Y30/00
CPCB82Y30/00C01F17/206C01P2004/61C01P2004/64
Inventor 肖燕飞高国华徐志峰饶明璐赖安邦
Owner GANZHOU ZHANHAI IND & TRADING
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