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Preparation method of high-purity yttrium oxide

A high-purity, yttrium oxide technology, applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problems of waste of resources, low purity, damage to the environment, etc., to save acid and alkali consumption, and save rare earth Effects of conservation of resources and recycling

Active Publication Date: 2013-12-25
中稀(宜兴)稀土新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As known in the industry, the purity of yttrium oxide is not only related to the brightness of the luminescent material, but also related to the service life of the product. However, the purity of yttrium oxide in the prior art is relatively low, about 99.99%, so that its purity can reach The preparation method of ≥99.9995%, that is, the preparation method with a purity of five nines, has not been reported so far
[0006] At present, there are many manufacturers producing yttrium oxide in my country, and the method used is generally extraction and separation. In the extraction and separation process, in order to ensure the yield as much as possible, the amount of acid and alkali consumed is relatively large, so the raffinate in the extraction process contains The discharge of acid wastewater is relatively large
In order to avoid damage to the environment, the raffinate acid-containing waste water is usually neutralized with alkali and then discharged up to the standard, resulting in the following technical problems: first, the cost of waste water treatment is high; cause waste of resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028]A) Pretreatment, the rare earth chloride solution containing Ho, Er, Tm, Yb, Lu and Y enrichment and tertiary amine, which is customarily called N235, tri(octyl-decyl)alkyl tertiary amine, in a volume ratio of 1 : 3 drop into a container with a stirring device and stir for 60min at a speed of 150rpm at the rotating speed of the stirring device to obtain a pretreated rare earth chloride solution, wherein: the rare earth chloride solution is preferably purchased from a commercial channel, such as Purchase and use the trade mark that is produced and sold by China Inner Mongolia Baotou Pioneer Rare Earth Co., Ltd. to be XFA-D-2 rare earth chloride solution, and the mass percent content of yttrium in this rare earth chloride solution is 70%, and the mass percent concentration of hydrochloric acid 0.007%;

[0029] B) Pre-balance, put the first extractant and the pre-treated rare earth chloride solution obtained in step A) into a container with a stirring device, and add the al...

Embodiment 2

[0036] Only change the volume ratio of the rare earth chloride solution in step A) to the tri(octyl-decyl)alkyl tertiary amine to 1:1, change the rotating speed of the stirring device, that is, the stirring speed to 80rpm, and the stirring time to 120min, Change the mass percentage of yttrium in the rare earth chloride solution to 60%, change the mass percentage concentration of hydrochloric acid to 0.01%; change the pH value in step B) to 5, and change the pretreated rare earth chloride solution, The volume ratio of the first extraction agent and the alkaline regulator is changed to 1: 1: 0.15, the mass percentage concentration of the alkaline regulator is changed to 32%, the time and the rotating speed of the continuous stirring are changed to 120min and 80rpm respectively, The dropping time of liquid caustic soda is changed into 120min, and the volume ratio of naphthenic acid, additive and diluent is changed into 1:1:2.5; The molar concentration of the yttrium-rich material ...

Embodiment 3

[0038] Only change the volume ratio of the rare earth chloride solution in step A) to the tri(octyl-decyl)alkyl tertiary amine to 1:2, change the rotating speed of the stirring device, that is, the stirring speed to 115rpm, and change the stirring time to 90min. Change the mass percentage of yttrium in the rare earth chloride solution to 70%, change the mass percentage concentration of hydrochloric acid to 0.085%; change the pH value in step B) to 4.5, and change the pretreated rare earth chloride solution, The volume ratio of the first extraction agent and the basic conditioner is changed to 1: 2: 0.1, the mass percentage concentration of the basic conditioner is changed to 31%, the time and the rotating speed of the continuous stirring are changed to 90min and 125rpm respectively, The dropping time of liquid caustic soda is changed into 90min, and the volume ratio of naphthenic acid, additive and diluent is changed into 1: 0.85: 2.65; The molar concentration of the yttrium-ri...

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Abstract

The invention relates to a preparation method of high-purity yttrium oxide, belonging to the field of rare earth separation technologies. The preparation method comprises the following steps: putting a rare earth chloride solution containing Ho, Er, Tm, Yb, Lu and Y enrichments and tertiary amine into a vessel with a stirring device, and stirring; putting a first extraction agent and the pre-treated rare earth chloride solution into a vessel with a stirring device, and standing until phase splitting, thus obtaining a pre-equilibration solution; adding pure water into the pre-equilibration solution, evenly stirring to obtain an yttrium-enriched material, and controlling the mol concentration of the yttrium-enriched material; taking the yttrium-enriched material as a raw material, and performing continuous extraction separation by using a second extraction agent and adding a washing solution, a reverse extraction solution and liquid alkali, thus obtaining a crude yttrium chloride solution; taking the crude yttrium chloride solution as a raw material, performing successive extraction separation by using a third extraction agent and adding a washing solution and a reverse extraction solution, thus obtaining a high-purity yttrium chloride solution; introducing the high-purity yttrium chloride solution into a precipitation tank; and introducing solid yttrium oxalate into a roller type tunnel kiln, and firing to obtain the finished product. The preparation method embodies cyclic utilization of waste water and environment protection.

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 yttrium oxide. Background technique [0002] Yttrium oxide (yttrium oxide) belongs to rare earth oxides, the chemical formula or molecular formula is: Y 2 o 3 ; Molecular weight: 225.81; Density: 5.01g / ㎝ 2 ; Melting point: 2410℃; Properties: white slightly yellow powder; Physical and chemical properties: insoluble in water and alkali but soluble in acid. [0003] As an important functional material, yttrium oxide is used in aviation, aerospace, atomic energy, high-performance ceramics, microwave magnetic materials, optical glass, high-brightness phosphors for large-screen TVs, picture tubes, LEDs, infrared lenses and even military weapons such as infrared guidance. Missile windows and fairings and other areas. [0004] The technical information on the preparation methods of yttrium oxide can be seen in the publish...

Claims

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Application Information

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IPC IPC(8): C01F17/00C22B3/10C22B3/26C22B3/44C22B59/00
CPCY02P10/20
Inventor 查国平钱建龙
Owner 中稀(宜兴)稀土新材料有限公司
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