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Preparation method of terbium oxide with D50 being 2-3 microns

A technology of terbium oxide and terbium chloride, which is applied in chemical instruments and methods, rare earth metal oxides/hydroxides, inorganic chemistry, etc., can solve the problems of uneven particle size distribution and difficult particle control of terbium oxide, and achieve good results. Chemical properties and electronic properties, meeting environmental protection requirements, simple preparation process

Active Publication Date: 2018-11-23
CHANGZHOU GEOQUIN NANO NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the technical defects of uneven terbium oxide particle size distribution and difficult particle control in the existing terbium oxide preparation technology, and provide a method for preparing terbium oxide with a D50:2-3 μm

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] This specific embodiment adopts the following technical scheme to prepare terbium oxide powder: first weigh the refined oxalic acid (also known as oxalic acid dihydrate, molecular formula is C) with two crystal waters. 2 h 2 o 4 .2(H 2 0), molecular weight is 126.06, hereinafter the same) 12.8kg, puts into the oxalic acid solution that preparation concentration is 0.2mol / L in the retort, and retort selects ceramic reaction interlayer tank for use; Add the Polyethylene Glycol 20000 of 0.4kg, stir 0.5 hour Finally, drip concentration is 214L of terbium chloride aqueous solution of 0.2mol / L, add dropwise at a speed of 5L / min, leave standstill after the dropwise addition finishes and stir for 15min, add ice water circulation aging in the interlayer of ceramic reaction interlayer tank After 1 hour, the material mixture is obtained, and the temperature of the material in the reaction kettle is controlled to 0-5° C. by ice water circulation during the aging process. Then di...

Embodiment 2

[0018] This specific embodiment adopts the following technical scheme to prepare terbium oxide powder: first weigh 24kg of refined oxalic acid with two crystal waters, put it into a reaction tank to prepare an oxalic acid solution with a concentration of 0.4mol / L, and the reaction tank is a ceramic reaction interlayer tank Add the Polyethylene Glycol 20000 of 1.05kg, after stirring for 0.5 hours, dropwise concentration is 200L of terbium chloride solution of 0.4mol / L, add dropwise at a speed of 5L / min, leave standstill after the dropwise addition finishes and stir for 15min, After adding ice water to the interlayer of the ceramic reaction interlayer tank and aging for 4 hours, the material mixture is obtained. During the aging process, the temperature of the material in the reaction kettle is controlled to 0-5° C. by ice water circulation. Then discharge the material mixture into the suction filter barrel, drain the liquid in the material mixture, and then add pure water for wa...

Embodiment 3

[0020] This specific embodiment adopts the following technical scheme to prepare terbium oxide powder: first weigh 48kg of refined oxalic acid with two crystal waters, put it into a reaction tank to prepare an oxalic acid solution with a concentration of 0.3mol / L, and the reaction tank is equipped with a disk Tube ceramic reaction kettle; add 1.6kg of polyethylene glycol 1000, stir for 0.5 hours, then add dropwise 357L of terbium chloride aqueous solution with a concentration of 0.3mol / L, add dropwise at a speed of 4L / min, and stir after the dropwise addition After standing still for 25 minutes, ice water was added to the coil of the ceramic reactor and aged for 5 hours to obtain a material mixture. During the aging process, the temperature of the material in the reactor was controlled to 0-5°C by ice water circulation. Then discharge the material mixture into the suction filter barrel, drain the liquid in the material mixture, and then add pure water for washing. The temperatu...

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Abstract

The invention discloses a preparation method of terbium oxide with D50 being 2-3 microns. The preparation method concretely comprises the following steps of firstly, preparing an oxalic acid solution,adding polyethylene glycol 20000 with a set mass ratio, performing stirring until uniform dispersion, then slowly dropwise adding a terbium chloride solution with the concentration being 0.20.4mol / Lwhile performing stirring, performing ageing for 4-5 hours at 0-5 DEG C, then performing suction filtration and washing with the washing temperature being larger than 95 DEG C, performing dry filtering after washing to obtain precipitates, and searing the precipitates for 3-5 houses at 850-900 DEG C to prepare the terbium oxide with D50 being 2-3 microns. The prepared terbium oxide with a specificparticle size range can further improve some defects of some lithium iron phosphate materials and thus effectively improves the specific capacity, the cycling stability, the discharge rate and the like of a battery; and the terbium oxide with the particle size expresses better chemical performance and electronic performance in doping and improvement of lithium battery cathode materials.

Description

technical field [0001] The invention belongs to the technical field of rare earth compound ultrafine powder preparation, and in particular relates to a preparation method of terbium oxide with D50: 2-3 μm. Background technique [0002] As a functional material, terbium oxide is used to make metal terbium, magneto-optical glass, fluorescent powder, magneto-optic storage materials, chemical additives, etc., and can also be used to prepare functional ceramics. However, due to the scarcity and preciousness of terbium oxide, its application fields are limited. With the development of some industries, many excellent properties of terbium oxide have emerged. For example, in the lithium battery industry, the positive electrode material determines the performance of lithium batteries. At present, a new type of lithium iron phosphate material has attracted more and more attention, and the addition of terbium oxide has improved some defects of some lithium iron phosphate materials. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
CPCC01P2004/62C01P2006/80C01F17/206
Inventor 王鹭
Owner CHANGZHOU GEOQUIN NANO NEW MATERIALS
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