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Preparation method for high-purity niobium oxide

A niobium oxide, high-purity technology, applied in chemical instruments and methods, inorganic chemistry, niobium compounds, etc., can solve the problems of waste, long production process, high raw material requirements, etc., to improve production efficiency, reduce solvent extraction times, and save labor and the effect of raw materials

Active Publication Date: 2015-12-09
NINGXIA ORIENT TANTALUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Repeated solvent extraction leads to a long production process and high requirements for raw materials, resulting in a large waste of labor and raw materials

Method used

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  • Preparation method for high-purity niobium oxide
  • Preparation method for high-purity niobium oxide
  • Preparation method for high-purity niobium oxide

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Embodiment 1

[0013] The tantalum-niobium ore is analyzed, the content is 15% of tantalum oxide, 38% of niobium oxide, 2% of phosphorus pentoxide, 1.5% of arsenic pentoxide, 0.5% of antimony pentoxide, and 1 ton of the above ore is crushed to 200 mesh , added to 1.7 tons of 55% HF, reacted for 8 hours, added 300L of 92% concentrated sulfuric acid, and finally adjusted. In the pulp extraction section, use MIBK (methyl isobutyl ketone) to countercurrently extract tantalum and niobium in the solution; in the pickling section, use 4mol / L sulfuric acid solution to remove impurities; in the anti-niobium section, use 1.7mol / L Sulfuric acid, countercurrent extraction, after extraction, a solution containing fluorotantalic acid is generated. The measured content of niobium oxide in the solution is 120g / L, take 1000L of the solution, heat it to 80 degrees Celsius, then add 200 kg of potassium chloride, heat for 20 minutes, cool and crystallize, separate the mother liquor, add pure water to the contai...

Embodiment 2

[0015] Analyze the tantalum-niobium ore, the content is 20% of tantalum oxide, 21% of niobium oxide, 0.6% of phosphorus pentoxide, 1.5% of diarsenic pentoxide, 0.5% of antimony pentoxide, 1 ton of above ore, crushed to 200 mesh , added to 1.8 tons of 55% HF, reacted for 8 hours, added 300L of 92% concentrated sulfuric acid, and finally adjusted. In the pulp extraction section, use MIBK (methyl isobutyl ketone) to countercurrently extract tantalum and niobium in the solution; in the pickling section, use 4mol / L sulfuric acid solution to remove impurities; in the anti-niobium section, use 1.7mol / L Sulfuric acid, countercurrent extraction, after extraction, a solution containing fluoroniobic acid is generated. The measured content of niobium oxide in the solution is 100g / L, take 1000L of the solution, heat it to 90 degrees Celsius, then add 180 kg of potassium chloride, heat for 20 minutes, cool and crystallize, separate the mother liquor, add pure water to the container for wash...

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Abstract

A preparation method for high-purity niobium oxide is disclosed and comprises: crushing tantalum niobium ore to 200 mesh, adding into a hydrofluoric acid solution, adding a proper amount of an acid, extracting the tantalum niobium solution by MIBK (methyl isobutyl ketone) to generate a supported organic solution, washing by a sulfuric acid solution, performing washing back extraction to form a fluoroniobic acid solution, adding KCl or KF, and performing filtering and washing, so as to obtain potassium fluoxyniobate crystal; and dissolving the potassium fluoroniobiate crystal in pure water, adding a hydrofluoric acid solution and a sulfuric acid solution, performing back extraction on the MIBK or 2-octanol solution containing fluoroniobic acid by utilizing pure water and enabling fluoroniobic acid enter pure water, and performing ammonia gas neutralization, filtering, washing, drying and roasting, so as to prepare high-purity niobium oxide. The method combines solvent extraction and crystallization, is capable of effectively removing phosphorus, arsenic, antimony and other impurities, and improves the production efficiency.

Description

technical field [0001] The invention belongs to the field of metal chemical smelting, in particular to a preparation method of high-purity niobium oxide. Background technique [0002] High-purity niobium oxide (99.99%) is an important functional material in the high-tech new material industry. It is mainly used in the preparation of lithium niobate ferroelectric crystals, high refractive index optical glass, and niobium oxide sputtering targets. The preparation method of high-purity niobium oxide is mainly solvent extraction method. By selecting suitable raw materials, hydrofluoric acid, sulfuric acid decomposition, and multiple solvent extractions, a high-purity fluoroniobic acid solution is prepared, and then precipitated by ammonia gas, washed, Drying and roasting prepare high-purity niobium oxide. This method needs to select suitable raw materials, and there is no way to process raw materials with high impurities such as phosphorus, arsenic, and antimony. Moreover, in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G33/00
CPCC01G33/00C01P2006/80
Inventor 鲁东马应利陈宗强郑陪生郭涛
Owner NINGXIA ORIENT TANTALUM IND