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Method for preparing super-fine high-purity neodymia oxide by using Pr-Nd enriched material

A technology of enrichment and neodymium 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 neodymium 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: 2009-12-02
常州市西南化工研究所 +2
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problems existing in these separation and preparation methods are: (1), extraction and separation rate and low efficiency: the equipment used in the extraction and separation method is mixing and settling tank, centrifugal extractor equipment, etc., and the existing process generally passes through 70-100 grade The entire extraction process can only be completed, and some even have to pass through hundreds of levels to complete the entire extraction process. The rare earth extraction rate and separation efficiency are low, and the extraction time is long, which leads to an increase in production costs and difficulty in improving production capacity; (2), The precipitation effect of neodymium oxalate crystals is not good: adding oxalic acid to the refined neodymium nitrate solution as a precipitant to form neodymium oxalate crystals and precipitation is the crystallization 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 neodymium to form crystalline carbonate. Usually, the obtained neodymium 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 to carry out; (3), poor product quality: the neodymium oxalate product that adopts the traditional crystallization precipitation method that generally adopts at present obtains, the quality of the neodymium oxide product prepared through solid-liquid separation, drying, burning is unstable, Generally difficult to obtain Nd 2 o 3 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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  • Method for preparing super-fine high-purity neodymia oxide by using Pr-Nd enriched material
  • Method for preparing super-fine high-purity neodymia oxide by using Pr-Nd enriched material
  • Method for preparing super-fine high-purity neodymia oxide by using Pr-Nd enriched material

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] like figure 1 and figure 2 As shown, a method for preparing ultrafine high-purity neodymium oxide from a praseodymium-neodymium Pr-Nd enrichment is to use the praseodymium-neodymium Pr-Nd enrichment as a raw material, and the steps of the method are as follows:

[0028] (1) Mixing batching: carry out mixing batching with praseodymium-neodymium Pr-Nd, nitric acid, water, through solid-liquid separation, remove insoluble impurity, obtain praseodymium-neodymium Pr-Nd enrichment material liquid, the concentration of rare earth in the feed liquid 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 Pr-N...

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] like figure 1 and image 3 As shown, a method for preparing ultrafine high-purity neodymium oxide from a praseodymium-neodymium Pr-Nd enrichment is to use the praseodymium-neodymium Pr-Nd enrichment as a raw material, and the steps of the method are as follows:

[0040] (1) Mixing batching: carry out mixing batching with praseodymium-neodymium Pr-Nd, nitric acid, water, through solid-liquid separation, remove insoluble impurity, obtain praseodymium-neodymium Pr-Nd enrichment material liquid, the concentration of rare earth in the feed liquid is 0.1-2.3mol / L;

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

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] like figure 1 and Figure 5 As shown, a method for preparing ultrafine high-purity neodymium oxide from a praseodymium-neodymium Pr-Nd enrichment is to use the praseodymium-neodymium Pr-Nd enrichment as a raw material, and the steps of the method are as follows:

[0052] (1) Mixing batching: carry out mixing batching with praseodymium-neodymium Pr-Nd, nitric acid, water, through solid-liquid separation, remove insoluble impurity, obtain praseodymium-neodymium Pr-Nd enrichment material liquid, the concentration of rare earth in the feed liquid 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 neodymium oxide that includes the following steps: mixing raw material, taking ultrasonic fractional extraction to gain enriched liquid containing Nd(NO3)3, taking ultrasonic to gain refined liquid of Nd(NO3)3, taking adsorption and trash extraction, taking solid-liquid separation, taking ultrasonic crystal deposition to gain Nd2(CO3)3 crystal deposit, taking solid-liquid separation, drying and burning to gain the superfine high purity neodymium 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 neodymium oxide, in particular to a method for preparing superfine high-purity neodymium 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 neodymium oxide (Nd 2 o 3 ) products refer to neodymium oxide products with neodymium oxide content ≥ 99.99% and particle size ≤ 10.0 μm. Ultra-fine high-purity neodymium oxide has been well applied in rare earth permanent magnets, lasers, glass, ceramics and superconductors, and can meet the needs of high-grade products. It is an important light rare earth oxide product. At present, my country's preparation of ultra-fine high-purity Nd 2 o 3 The main raw materials are the following four kinds: (1) rare earth sulfate [RE 2 (SO 4 ) 3 ], which is composed of rare earth concentrates in Baotou, Inner Mongolia (REO≥50%, Nd 2 o 3 17%) processed RE ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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
Owner 常州市西南化工研究所
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