Method for preparing ultra-thin highly-pure lanthanum oxide by beneficiated lanthanum

A technology of enrichment and lanthanum oxide, applied in the direction of improving process efficiency, can solve the problems of high toxicity of oxalic acid, difficulty in improving production capacity, and increase in production cost.

Inactive Publication Date: 2007-08-08
CHANGZHOU HUANAN CHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main problem that these preparation methods exist at present is: (1), extraction separation rate and efficiency are low: the equipment that extraction separation method uses at present is mixed settling tank, centrifugal extractor etc., carry out multistage extraction, if improve the purity of product, just The number of stages must be increased, and the existing extraction stages are many, and generally the entire extraction process can only be completed through 70-100 stages; and 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 difficult production capacity. Improve; (2), lanthanum oxalate crystal precipitation effect is not good: adding oxalic acid in the refined lanthanum nitrate solution is the precipitating agent to generate lanthanum oxalate crystal precipitation and is the crystallization precipitation method of the rare earth element generally adopted at present
The disadvantage of using oxalic acid as

Method used

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  • Method for preparing ultra-thin highly-pure lanthanum oxide by beneficiated lanthanum
  • Method for preparing ultra-thin highly-pure lanthanum oxide by beneficiated lanthanum

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Main equipment: extraction kettle with probe-type ultrasonic generator, crystallization kettle with probe-type ultrasonic generator.

[0025] Main raw materials: Lanthanum concentrate, HNO 3 , TBP extractant, kerosene, NH 4 HCO 3 .

[0026] As shown in Figures 1 and 2, a method for preparing ultrafine high-purity lanthanum oxide from a lanthanum enrichment is to use the lanthanum enrichment as a raw material, and the steps of the method are as follows:

[0027] (1) Mixing ingredients: mixing lanthanum-enriched material, nitric acid, and water, and removing insoluble impurities through solid-liquid separation to obtain lanthanum-enriched material liquid, the concentration of rare earth in the material liquid is 0.1-2.3mol / L;

[0028] (2) Ultrasonic fractionation extraction: In the extraction kettle with a probe-type ultrasonic generator, add lanthanum-enriched material liquid, extraction liquid, and back-extraction liquid. The volume ratio of the three material ingred...

Embodiment 2

[0035] Main equipment: extraction tank with vibrator-type ultrasonic generator, crystallization tank with vibrator-type ultrasonic generator.

[0036] Main raw materials: Lanthanum concentrate, HNO 3 , TBP extractant, sulfonated kerosene, (NH 4 ) 2 CO 3 .

[0037] As shown in Figures 1 and 3, a method for preparing ultrafine high-purity lanthanum oxide from a lanthanum enrichment is to use the lanthanum enrichment as a raw material, and the steps of the method are as follows:

[0038] (1) Mixing ingredients: mixing lanthanum-enriched material, nitric acid, and water, and removing insoluble impurities through solid-liquid separation to obtain lanthanum-enriched material liquid, the concentration of rare earth in the material liquid is 0.1-2.3mol / L;

[0039] (2) Ultrasonic fractionation extraction: In the extraction tank with a vibrator-type ultrasonic generator, add lanthanum-enriched material liquid, extraction liquid, and back-extraction liquid. The volume ratio of the th...

Embodiment 3

[0046] Main equipment: Main equipment: extraction tube with vibrating plate ultrasonic generating device, crystallization tube with vibrating plate ultrasonic generating device.

[0047] Main raw materials: Lanthanum concentrate, HNO 3 , TBP extractant, No. 200 gasoline, NH 4 HCO 3 .

[0048] As shown in Figures 1 and 5, a method for preparing ultrafine high-purity lanthanum oxide from a lanthanum enrichment uses the lanthanum enrichment as a raw material, and the steps of the method are as follows:

[0049] (1) Mixing ingredients: mixing lanthanum-enriched material, nitric acid, and water, and removing insoluble impurities through solid-liquid separation to obtain lanthanum-enriched material liquid, the concentration of rare earth in the material liquid is 0.1-2.3mol / L;

[0050] (2) Ultrasonic fractionation extraction: In the extraction tube with a vibrating plate ultrasonic generator, add lanthanum-enriched material liquid, extraction liquid, and stripping liquid. The volum...

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Abstract

The invention discloses a making method of lanthanum oxide, which comprises the following steps: (1) blending raw material to form enriched lanthanum slurry; (2) fractionating and extracting through ultrasound; obtaining La (NO3) 3 solution and promethium-neodymium enriched liquid; (3) adsorbing impurity; (4) separating solid from liquid; obtaining fined liquid of purified La(NO3)3; (5) crystallizing; sedimenting La2(CO3)3; (6) proceeding solid-liquid separation; (7) drying; sintering; obtaining La2O3 with content not less than 99.99% and grain size at 0.01-10.0um.

Description

technical field [0001] The invention relates to a method for preparing lanthanum oxide, in particular to a method for preparing ultrafine high-purity lanthanum oxide by using lanthanum enrichment as a raw material, which belongs to the field of hydrometallurgy. Background technique [0002] Ultra-fine high-purity lanthanum oxide (La 2 o 3 ) products refer to lanthanum oxide products with lanthanum oxide content ≥ 99.99% and particle size ≤ 10.0 μm. At present, ultrafine high-purity lanthanum oxide (La 2 o 3 ) The method used in the preparation of the product is generally based on lanthanum enrichment as raw material, using HNO 3 Dissolve to make lanthanum nitrate solution, and then use P350 etc. as extraction agent for extraction and separation to obtain refined lanthanum nitrate solution. Lanthanum nitrate solution uses oxalic acid as precipitant to form lanthanum oxalate crystals and precipitate out. After drying and burning, lanthanum oxalate can be obtained Ultra-fi...

Claims

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Application Information

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IPC IPC(8): C22B3/00C22B3/06C22B3/22C22B3/44
CPCY02P10/20
Inventor 许文林王雅琼魏晓廷朱金玉魏巍张月
Owner CHANGZHOU HUANAN CHEM
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