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Ultrafine lanthanum oxide and preparation method thereof

A technology of lanthanum oxide and lanthanum salt, which is applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problems that large particles cannot meet the requirements, and achieve the prevention of re-agglomeration, short standing time, and prevention of particle size change big effect

Inactive Publication Date: 2015-11-25
CHANGZHOU GEOQUIN NANO NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in some specific magnetic material fields, small particles of lanthanum oxide are required, and large particles cannot meet the requirements, and uniform particle size distribution is required

Method used

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  • Ultrafine lanthanum oxide and preparation method thereof
  • Ultrafine lanthanum oxide and preparation method thereof
  • Ultrafine lanthanum oxide and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0030] The lanthanum chloride solution is obtained from the rare earth ore separated by the extraction tank, and adjusted to a concentration of 1.0mol / l, pH:1. Take 2g of sodium dodecylbenzenesulfonate as an anionic surfactant and add it to pure water at 50°C, and keep stirring until the sodium dodecylbenzenesulfonate is completely dissolved to obtain an aqueous solution containing sodium dodecylbenzenesulfonate Get lanthanum chloride solution 614ml, add above-mentioned aqueous solution in the lanthanum chloride solution, and stir. Take 200 g of oxalic acid and dilute to obtain 3.17 L of oxalic acid solution with a solution concentration of 0.5 mol / L. While the oxalic acid solution is constantly stirring, quickly add the lanthanum chloride solution containing sodium dodecylbenzenesulfonate, stir and age for 1.5 hours, then suction filter and wash until the pH value of the washing solution is 7, and remove the precipitate Dry at 120°C for 1 hour, then burn at 1000°C, the heati...

Embodiment 2

[0032] Dissolve lanthanum carbonate in nitric acid to obtain lanthanum nitrate solution, adjust to a concentration of 0.8mol / l, pH: 1.5. Take 2.3g of sodium dodecylbenzenesulfonate as an anionic surfactant and add it to pure water at 65°C and keep stirring until the sodium dodecylbenzenesulfonate is completely dissolved to obtain an aqueous solution containing sodium dodecylbenzenesulfonate Get lanthanum nitrate solution 1150ml, add above-mentioned aqueous solution in the lanthanum chloride solution, and stir. Take 270 g of oxalic acid and dilute to obtain 3.57 L of oxalic acid solution with a concentration of 0.6 mol / L. While the oxalic acid solution is constantly stirring, quickly add the lanthanum nitrate solution containing sodium dodecylbenzenesulfonate, stir and age for 1 hour, then carry out suction filtration and washing until the pH of the washing solution is 7, and put the precipitate in Dry at 90°C, and then burn at 900°C. During burning, the heating time is 4 hour...

Embodiment 3

[0034] Dissolve lanthanum oxide in 18.6mol / L concentrated sulfuric acid to obtain lanthanum sulfate solution, adjust to 0.5mol / L, pH:1. Take 1g of sodium lauryl sulfate and stir it as an anionic surfactant, add it into pure water at 80°C, and keep stirring until the sodium lauryl sulfate is completely dissolved to obtain an aqueous solution containing sodium lauryl sulfate; take lanthanum sulfate solution 1230ml, the above aqueous solution was added to the lanthanum sulfate solution, and stirred. Take 150g of oxalic acid and dilute to obtain 1488ml of solution. When the oxalic acid solution is continuously stirred, quickly add it to the lanthanum sulfate solution containing sodium lauryl sulfate, and stir and age for 0.5 hours, filter and wash to pH: 7, and dry the precipitate at 100°C Dry for 2 hours, then burn at 800°C. During burning, the heating time is 3.5 hours, and the holding time is 2 hours. After burning, grind and sieve to obtain ultrafine lanthanum oxide. The D50...

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Abstract

The invention belongs to the field of preparation of rare earth materials, and especially relates to an ultrafine lanthanum oxide and a preparation method thereof. The preparation method of the ultrafine lanthanum oxide comprises the following steps: 1, preparing a lanthanum salt solution A; 2, preparing an anionic surfactant solution B, and adding the solution B to the solution A to obtain a solution C; 3, preparing an oxalic acid solution, pouring the oxalic acid solution into a reaction container, adding the solution C to the oxalic acid solution in a dropwise manner while continuously stirring, and reacting the solution C with the oxalic acid solution to generate lanthanum oxalate precipitate; and 4, carrying out pumping filtration on the generated precipitate, washing with water, drying, calcining to obtain crude lanthanum oxide, crushing the crude lanthanum oxide, and sieving to obtain the ultrafine lanthanum oxide with uniformly distributed granularity. The preparation method of the ultrafine lanthanum oxide is simple, allows rare earth lanthanum oxide with small granularity and uniform particle distribution to be directly obtained through an oxalate precipitation technology, and can avoid particle fragmentation caused by a physical technology, and the ultrafine lanthanum oxide can be directly used in magnetic materials.

Description

technical field [0001] The invention belongs to the field of preparation of rare earth materials, and in particular relates to an ultrafine lanthanum oxide and a preparation method thereof. Background technique [0002] Rare earth lanthanum oxide has a wide range of applications, and it plays an important role in glass, ceramics, electronics and other fields. With the continuous development of science and technology, the rare earth lanthanum oxide produced is required to have a specific physical and chemical form. At present, the market demand for products with controllable particle size has increased significantly. [0003] In many applications, there are strict requirements on the particle size and particle size distribution of rare earth lanthanum oxide powder. For example, when lanthanum oxide is used in the glass industry, in order to increase the refractive index, reduce dispersion, and improve the chemical corrosion resistance of the glass, it is generally required ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
Inventor 杨应亚龚晔王鹭
Owner CHANGZHOU GEOQUIN NANO NEW MATERIALS
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