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Process for preparing superfine, high-purity praseodymium oxide by using Pr-Nd riched materials

A technology of enrichment and praseodymium oxide, which is applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problem of low extraction rate and separation efficiency of rare earth, poor crystallization and precipitation of praseodymium oxalate, and difficult to reach product use Requirements and other issues to achieve the effect of improving product quality, reducing investment in equipment and reagents, and improving the production environment

Inactive Publication Date: 2007-08-29
常州市西南化工研究所 +2
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AI Technical Summary

Problems solved by technology

The main problems existing in these separation and preparation methods at present are: (1), extraction and separation rate and efficiency are low: the equipment used in the extraction and separation method at present is mixing and settling tank, centrifugal extractor equipment etc., rare earth extraction rate and separation efficiency are low, extraction time long, which leads to an increase in production costs, and it is difficult to increase production capacity
Improving the extraction and separation speed and separation efficiency of rare earth has been a problem that has been difficult to solve for a long time in the extraction and separation process of praseodymium-neodymium fractionation, and it is also an urgent problem to be solved; Adding oxalic acid as a precipitating agent to generate praseodymium oxalate crystals and precipitation is the crystallization and precipitation method of rare earth elements commonly used in industrial production
Oxalic acid is used as a precipitant, the production cost is high, and oxalic acid is highly toxic and pollutes the environment
It is difficult for the rare earth element praseodymium to form crystalline carbonate. Usually, the prepared praseodymium carbonate is an amorphous flocculent precipitate with a large volume, which contains a large amount of water and impurities. It is difficult to wash and filter, and the product quality is poor and the loss of rare earth is large. , production is difficult
(3), poor product quality: the praseodymium oxalate product obtained by the traditional crystallization precipitation method commonly used at present, the quality of the praseodymium oxide product prepared through solid-liquid separation, drying, and burning is unstable, and it is generally difficult to obtain Pr 6 o 11 The content is as high as 99.99% purity, especially the particle size of the product is large, and the particle size distribution is uneven, it is difficult to meet the requirements of the product used in the high-tech field

Method used

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  • Process for preparing superfine, high-purity praseodymium oxide by using Pr-Nd riched materials
  • Process for preparing superfine, high-purity praseodymium oxide by using Pr-Nd riched materials

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Main equipment: extraction kettle with probe-type ultrasonic generator, crystallization kettle with probe-type ultrasonic generator.

[0026] Main raw materials: praseodymium-neodymium Pr-Nd enrichment, HNO 3 , TBP extractant, kerosene, NH 4 HCO 3 .

[0027] As shown in Figure 1 and Figure 2, a kind of praseodymium-neodymium Pr-Nd concentrate prepares the method for ultrafine high-purity praseodymium oxide, is to be raw material with praseodymium-neodymium Pr-Nd enrichment, and described method step is as follows:

[0028] (1) Mixing ingredients: Mix ingredients of praseodymium-neodymium Pr-Nd concentrate, nitric acid, and water, remove insoluble impurities through solid-liquid separation, and obtain praseodymium-neodymium Pr-Nd enrichment material liquid, rare earth in the feed liquid The concentration is 0.1-2.3mol / L;

[0029] (2) Ultrasonic fractionation extraction: In an extraction kettle with a probe-type ultrasonic generating device, add praseodymium-neodymium...

Embodiment 2

[0037] Main equipment: extraction tank with vibrator-type ultrasonic generator, crystallization tank with vibrator-type ultrasonic generator.

[0038] Main raw materials: praseodymium-neodymium Pr-Nd enrichment, HNO 3 , TBP extractant, sulfonated kerosene, (NH 4 ) 2 CO 3 .

[0039] As shown in Figure 1 and Figure 3, a kind of praseodymium-neodymium Pr-Nd concentrate prepares the method for ultra-fine high-purity praseodymium oxide, is to take praseodymium-neodymium Pr-Nd enrichment as raw material, and described method step is as follows:

[0040] (1) Mixing ingredients: Mix ingredients of praseodymium-neodymium Pr-Nd concentrate, nitric acid, and water, remove insoluble impurities through solid-liquid separation, and obtain praseodymium-neodymium Pr-Nd enrichment material liquid, rare earth in the feed liquid The concentration is 0.1-2.3mol / L;

[0041](2) Ultrasonic fractionation extraction: In the extraction tank with vibrator-type ultrasonic generating device, add pras...

Embodiment 3

[0049] Main equipment: extraction tube with vibrating plate ultrasonic generating device, crystallization tube with vibrating plate ultrasonic generating device.

[0050] Main raw materials: praseodymium-neodymium Pr-Nd enrichment, HNO 3 , TBP extractant, No. 200 gasoline, NH 4 HCO 3 .

[0051] As shown in Fig. 1 and Fig. 5, a kind of praseodymium-neodymium Pr-Nd concentrate prepares the method for superfine high-purity praseodymium oxide, is to take praseodymium-neodymium Pr-Nd enrichment as raw material, and described method step is as follows:

[0052] (1) Mixing ingredients: Mix ingredients of praseodymium-neodymium Pr-Nd concentrate, nitric acid, and water, remove insoluble impurities through solid-liquid separation, and obtain praseodymium-neodymium Pr-Nd enrichment material liquid, rare earth in the feed liquid The concentration is 0.1-2.3mol / L;

[0053] (2) Ultrasonic fractionation extraction: In the extraction tube with a vibrating plate type ultrasonic generating...

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Abstract

The invention relates to a method to make praseodymium oxide that includes the following steps: mixing raw material, taking ultrasonic fractional extraction to gain enriched liquid containing Pr(NO3)3, taking ultrasonic to gain refined liquid of Pr(NO3)3, taking adsorption and trash extraction, taking solid-liquid separation, taking ultrasonic crystal deposition to gain Pr2(CO3)3 crystal deposit, taking solid-liquid separation, drying and burning to gain the superfine high purity praseodymium oxide product that has content over 99.99%, and the particle diameter is 0.01-10.0um. The advantages of the invention are that it improves leaching and extracting speed, and the particle diameter is small, and particle size distribution equal.

Description

technical field [0001] The invention relates to a method for preparing praseodymium oxide, in particular to a method for preparing ultrafine high-purity praseodymium oxide by using praseodymium-neodymium Pr-Nd enrichment as a raw material, belonging to the field of hydrometallurgy. Background technique [0002] Ultra-fine high-purity praseodymium oxide (Pr 6 o 11 ) products refer to praseodymium oxide products with a praseodymia content of ≥99.99% and a particle size of ≤10.0 μm. Ultra-fine high-purity praseodymium oxide is used in pigments, optical filters, magnets and other materials, and is expanding to other fields, especially in intelligence devices, such as computers, mobile phones, etc., and the rare earths required for magnets, capacitors, etc. The quantity and purity requirements of oxides are also constantly increasing. Ultra-fine high-purity praseodymium oxide can meet the requirements of high-grade products and is an important light rare earth oxide product, wh...

Claims

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Application Information

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IPC IPC(8): C01F17/00C22B3/00
CPCY02P10/20
Inventor 许文林王雅琼魏晓廷朱金玉魏巍赵红坤刘斌
Owner 常州市西南化工研究所
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