Preparation method of high-purity potassium fluorotantalate

A technology of pure potassium fluorotantalate and potassium fluorotantalate, which is applied in chemical instruments and methods, tantalum compounds, inorganic chemistry, etc., can solve the problem of how to remove impurities such as potassium fluorotantalate and the limited extraction effect of niobium and other impurities. question

Active Publication Date: 2018-11-30
NINGXIA ORIENT TANTALUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The current process also adopts single crystallization, and some impurity elements such as silicon and niobium are easy to form crystals and crystallize together with potassium fluorotantalate. Chinese patent application number 02801094.9 reports a high-purity potassium fluorotantalate crystal or high-purity The manufacturing method of potassium fluoroniobate crysta

Method used

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  • Preparation method of high-purity potassium fluorotantalate
  • Preparation method of high-purity potassium fluorotantalate
  • Preparation method of high-purity potassium fluorotantalate

Examples

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Effect test

Embodiment 1

[0038] Grind 1000kg of tantalum-niobium ore (30% of tantalum oxide and 20% of niobium oxide) to 200 mesh, add it to 1700L of hydrofluoric acid with a concentration of 55% by mass, and then add 400L of sulfuric acid with a concentration of 92% by mass, and keep it warm break down.

[0039] Enter the ore extraction tank, use MIBK solution to extract tantalum and niobium, make fluorotantalic acid and fluoroniobic acid enter into MIBK, and then use 3.7mol / L sulfuric acid to countercurrent extract in the pickling tank, after extraction, the tantalum and niobium The organic solvent enters the anti-niobium extraction tank, and the sulfuric acid solution with an acidity of 0.75mol / L is used for countercurrent extraction with the organic solvent containing tantalum and niobium. The fluoroniobic acid solution enters the sulfuric acid solution, and the fluorotantalic acid remains in the organic solvent. in solvent.

[0040] The organic solvent containing fluorotantalic acid was put into...

Embodiment 2

[0047] Grinding 1000kg of tantalum-niobium ore (30% of tantalum oxide and 20% of niobium oxide) to below 200 mesh, adding to 1700L of hydrofluoric acid with a mass concentration of 55%, and then adding 400L of sulfuric acid with a mass concentration of 92%, Insulation decomposition.

[0048] Enter the ore extraction tank, use 2-octanol solution to extract tantalum and niobium, fluorotantalic acid and fluoroniobic acid enter the 2-octanol, use 4.2mol / L sulfuric acid to extract countercurrently in the pickling tank, the organic material containing tantalum and niobium The solvent enters the anti-niobium-extracting tantalum tank, and a sulfuric acid solution with an acidity of 0.7 mol / L is used for countercurrent extraction with an organic solvent containing tantalum and niobium.

[0049] Put the fluoroniobic acid solution into the sulfuric acid solution, and the fluorotantalic acid remains in the organic solvent, and the organic solvent containing fluorotantalic acid enters the ...

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Abstract

The invention relates to a preparation method of high-purity potassium fluorotantalate. The preparation method is characterized by comprising the following steps: (1) decomposition: adding tantalum-niobium mineral into hydrofluoric acid and sulfuric acid for decomposition; (2) mineral-pulp extraction: utilizing an MIBK (Methyl Isobutyl Ketone) solvent or sec-octyl alcohol solvent to carry out backflow extraction and extracting fluorine-niobium acid and fluorine-tantalum acid into the solvent; (3) acid pickling: adopting sulfuric-acid solution to be contacted with the solvent obtained after extraction of step (2) in a backflow manner; (4) tantalum extraction by back extraction of niobium: utilizing the sulfuric-acid solution and the obtained solvent to carry out backflow extraction in an extraction groove, extracting the fluorine-niobium acid into an aqueous phase and forming fluorine-niobium acid aqueous solution; (5) back extraction of tantalum: placing the remaining organic solutionin another extraction groove, utilizing pure water to carry out back extraction on fluorine-tantalum acid organic solution into the pure water and forming fluorine-tantalum acid aqueous solution; (6)synthesis; (7) cooling and crystallization. The method for preparing high-purity potassium fluorotantalate by a method of sectional back extraction and sectional crystallization has the beneficial effect that impurities in the potassium fluorotantalate can be effectively removed.

Description

technical field [0001] The invention relates to a preparation method of high-purity potassium fluorotantalate. Background technique [0002] In the current tantalum-niobium metallurgy, the classic preparation process of potassium fluorotantalate has been formed. It is to use ore to add hydrofluoric acid to decompose tantalum and niobium into fluorotantalic acid or fluorotantalic acid, use MIBK or 2-octanol solution to extract fluoroniobic acid or fluorotantalic acid in the aqueous solution, and use low acidity sulfuric acid to further remove the loaded tantalum and niobium For impurities in the organic matter, use a sulfuric acid solution with a hydrogen ion concentration of 1.2-1.6 mol / L to back-extract the organic solution loaded with tantalum and niobium, and the fluoroniobic acid enters the acid solution. To achieve the purpose of separation from tantalum fluoride in organic solution. The organic solution containing fluorotantalic acid enters the anti-tantalum process,...

Claims

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Application Information

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IPC IPC(8): C01G35/00
CPCC01G35/006C01P2006/80
Inventor 鲁东焦红忠郑培生张伟宁颉维平闫青虎聂全兴
Owner NINGXIA ORIENT TANTALUM IND
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