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Series of micro/nano-rare earth materials and preparation method thereof

A nano-rare earth and rare earth material technology, which is applied in the fields of oxidized rare earth materials, basic rare earth carbonate materials and their preparation, micro/nano rare earth materials and their preparation, oxalic acid rare earth materials, hydroxide rare earth materials, and carbonate rare earth materials. Solve the problems of difficult large-scale production, expensive equipment, slow diffusion speed, etc., and achieve the effects of large-scale production, controllable grain size, and reduced growth rate

Inactive Publication Date: 2018-09-28
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the common co-precipitation method is used in the production of rare earth materials in my country. This method has an obvious disadvantage: the rare earth salt solution and the precipitant solution are reacted by ordinary stirring in the reactor, and the reactants The contact area between them is small, the diffusion rate is slow, and there is a concentration gradient that leads to uneven reaction
During the reaction process, the precipitation formed in the early stage of the reaction is covered by new precipitation particles as the seed crystals of the later precipitation. The coexistence of new and old precipitation particles directly leads to the uneven particle size distribution of the material, which makes the particle size of the rare earth material synthesized The size and dispersion properties are greatly affected, and the existence of particles of different sizes also makes it difficult for the crystal size of the prepared rare earth material to reach the nanometer level, which greatly affects the performance and application fields of the material
[0004] In recent years, many researchers have tried hydrothermal method, solvothermal method, microemulsion method and sol-gel method to prepare rare earth nanomaterials and made good progress, but these methods are complicated to operate, expensive equipment, and harsh reaction conditions. Low output and high cost make it difficult to apply to large-scale production. Therefore, it is imminent to explore a preparation method that can accurately control the particle size and particle size distribution of rare earth nanomaterials and is suitable for industrial production.

Method used

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  • Series of micro/nano-rare earth materials and preparation method thereof
  • Series of micro/nano-rare earth materials and preparation method thereof
  • Series of micro/nano-rare earth materials and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0030] A. Weigh 37.3g of cerium chloride and dissolve it in 1L of deionized water to prepare a 0.1mol / L cerium chloride solution for use.

[0031] B. Weigh 12.0 g of sodium hydroxide and dissolve it in 1 L of deionized water to prepare a sodium hydroxide solution with a concentration of 0.3 mol / L for use.

[0032] C. Add the solution in step A and step B to the nucleation reactor simultaneously with the same flow rate (100ml / min), control the rotating speed of the nucleation reactor to be 3000 rpm, and form the precipitated slurry from the outlet of the nucleation reactor flow out.

[0033] D. The slurry obtained from the reaction was placed in a crystallization kettle and crystallized at 80° C. for 5 hours, then filtered and washed, and then dried at 60° C. for 12 hours. Cerium hydroxide can be obtained, the chemical formula is Ce(OH) 3 .

[0034] figure 1 It is the scanning electron microscope picture of the prepared sample, and it can be seen from the picture that the p...

Embodiment 2

[0036] A. Weigh 37.1g of lanthanum chloride and dissolve it in 500mL of deionized water to prepare a 0.2mol / L lanthanum chloride solution for use.

[0037] B. Weigh 12.0g of sodium hydroxide and dissolve it in 500mL of deionized water to prepare a sodium hydroxide solution with a concentration of 0.6mol / L, which is ready for use.

[0038] C. Add the solution in step A and step B to the nucleation reactor simultaneously with the same flow rate (100ml / min), control the rotating speed of the nucleation reactor to be 3000 rpm, and form the precipitated slurry from the outlet of the nucleation reactor flow out.

[0039] D. The slurry obtained from the reaction was placed in a crystallization kettle for crystallization at 80° C. for 5 hours, filtered and washed, and then dried at 60° C. for 12 hours. Lanthanum hydroxide can be obtained, the chemical formula is La(OH) 3 .

[0040] figure 2 is a scanning electron microscope image of the prepared sample, from which it can be seen ...

Embodiment 3

[0042] A. Weigh 37.3g of cerium chloride and dissolve it in 1L of deionized water to prepare a 0.1mol / L cerium chloride solution for use.

[0043] B. Weigh 12.0 g of sodium hydroxide and dissolve it in 1 L of deionized water to prepare a sodium hydroxide solution with a concentration of 0.3 mol / L, which is ready for use.

[0044]C. Add the solution in step A and step B to the nucleation reactor simultaneously with the same flow rate (100ml / min), control the rotating speed of the nucleation reactor to be 3000 rpm, and the precipitated slurry formed from the outlet of the nucleation reactor flow out.

[0045] D. The slurry obtained from the reaction was placed in a crystallization kettle and crystallized at 80° C. for 5 hours, then filtered and washed, and then dried at 60° C. for 12 hours.

[0046] E. Put the product obtained in step D into a muffle furnace for roasting, keep it warm at 450°C for 3 hours and then lower it to room temperature naturally to obtain cerium oxide, t...

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Abstract

The invention discloses a series of micro / nano-rare earth materials and a preparation method thereof. The method prepares a large amount of a series of rare earth micro / nano-materials with high dispersion, uniform particle size distribution and controllable sizes. The rare earth micro / nano-material comprises one or more of an oxidized rare earth material, a hydroxide rare earth material, a rare earth carbonate material, a rare earth oxalate material and a rare earth subcarbonate material. The preparation method comprises preparing a rare earth salt or a mixed solution of a rare earth salt andadditives, fast mixing the rare earth salt or the mixed solution and a precipitant solution in a nucleating reactor for a reaction, placing the slurry in a crystallization tank, carrying out crystallization, carrying out washing for solid and liquid separation to obtain products, and calcining the products to obtain a rare earth oxide material. The particle sizes of the product can be controlled in a range of 20-2000nm. The preparation method is easy to operate, has high efficiency and is used for large-scale production. The rare earth micro / nano-material can be used in the fields of catalysis, polishing, luminescence and magnetism.

Description

technical field [0001] The invention belongs to the technical field of rare earth material preparation, in particular to a series of micro / nano rare earth materials and preparation methods thereof, in particular to oxidized rare earth materials, hydroxide rare earth materials, carbonate rare earth materials, oxalic acid rare earth materials, basic rare earth carbonate materials and the like Preparation. Background technique [0002] my country is the country with the largest rare earth reserves in the world. Rare earth micro / nano materials have shown very good performance in the fields of light, electricity, force, heat, magnetism, and catalysis. The application fields of rare earth materials have penetrated into various industries in society. , and play a more prominent role in the field of national defense science and technology. However, at present, most of the rare earth products in our country are based on primary processing, the product grades are not high, and the tec...

Claims

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Application Information

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IPC IPC(8): C01F17/00C07C51/41C07C55/07B82Y40/00
CPCB82Y40/00C01F17/206C01F17/247C01P2002/72C01P2004/03C01P2004/04C01P2004/61C01P2004/62C01P2004/64C07C51/412C07C55/07
Inventor 孔祥贵段昊泓雷晓东
Owner BEIJING UNIV OF CHEM TECH
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