Method for preparing potassium fluotantalate

A technology of potassium fluorotantalate and hydrofluoric acid, which is applied in the field of metallurgy, can solve the problems of high recovery process cost, high ammonia nitrogen content in the discharge, and large hydrofluoric acid consumption, so as to reduce production costs, reduce consumption, and eliminate pollution. Effect

Active Publication Date: 2014-09-03
ZHUZHOU HARD ALLOY GRP CO LTD
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  • Abstract
  • Description
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Problems solved by technology

[0005] The purpose of the present invention is to overcome the defects of the prior art such as high consumption of hydrofluoric acid, serious environmental pollution, high cost of mother liquor recovery process after crystallization of potassium fluorotantalate, low effect,

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  • Method for preparing potassium fluotantalate

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Effect test

Embodiment 1

[0028] (1) The raw material is tantalum capacitor waste with tantalum content: 80% (mass), and Nb less than 1%. The weight is 500 grams. Add 400 grams of hydrofluoric acid, 150 grams of sulfuric acid, and 500 grams of mother liquor. Stir in the decomposition tank and carry out After 8 hours of decomposition, 1.05L of decomposition solution was obtained;

[0029] (2) Add 3.1 kg of mother liquor, 0.21 kg of fluosilicic acid, and 0.10 kg of sulfuric acid to the decomposition liquid for low-acid preparation. The total acidity is 3.5 mol / L, and the sulfuric acid is 1 mol / L, and then filter out potassium fluorosilicate precipitation. Obtain 183.3 grams of industrial potassium fluorosilicate and acid adjusting solution;

[0030] (3) Perform 10-stage extraction of the acid-adjusting solution, the extraction agent is 2-octanol, 8-stage pickling, and 12-stage back extraction with deionized water to obtain 7.31L of tantalum solution;

[0031] (4) After heating the tantalum solution to 9...

Embodiment 2

[0035] The raw material is tantalum capacitor waste with tantalum content: 90%, Nb less than 1%, the weight is 500 grams, then add 750 grams of hydrofluoric acid, 400 grams of sulfuric acid, 1000 grams of mother liquor, stir, and decompose for 24 hours to obtain 2.15L of decomposition liquid Add 6 kg of mother liquor, 1.4 kg of fluosilicic acid, and 0.63 kg of sulfuric acid, and carry out low-acid deployment. The total acidity reaches 4.5 mol / L, and the sulfuric acid reaches 1.5 mol / L, and then filters out potassium fluosilicate precipitation to obtain industrial fluosilicate Potassium 210 grams and acid-adjusting solution; the acid-adjusting solution is subjected to 10-stage extraction, the extraction agent is 2-octanol, 8-stage pickling, and 12-stage back extraction with deionized water to obtain 8.1L of tantalum solution; after the tantalum solution is heated to 90°C , and then add reagent hydrofluoric acid 0.81L, potassium chloride 430 grams, carry out conversion, then wate...

Embodiment 3

[0037] The raw material is tantalum content: 10%, Nb is less than 1%, the by-product of preparing tantalum powder by sodium reduction after water washing, the weight is 1000 grams, then add 800 grams of hydrofluoric acid, 300 grams of sulfuric acid, 1000 grams of mother liquor, stir, carry out Decompose in 8 hours to obtain 2.1L of decomposition liquid; add 4.5 kg of mother liquor, 0.93 kg of fluosilicic acid, and 0.3 kg of sulfuric acid to make low-acid preparation, the total acidity reaches 3.5 mol / L, sulfuric acid reaches 1.1 mol / L, and then filters out fluosilicic acid Potassium precipitation to obtain 140 grams of industrial potassium fluorosilicate and acid-adjusting solution; the acid-adjusting solution was subjected to 10-stage extraction, the extractant was 2-octanol, 8-stage pickling, and 12-stage back extraction with deionized water to obtain tantalum solution 2.0L After the tantalum solution is heated to 90°C, add 0.1L of reagent hydrofluoric acid and 98 grams of po...

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Abstract

The invention relates to a preparation method of potassium fluotantalate. In the method, potassium fluotantalate is prepared by a mother liquid internal-circulation process instead of the crystallized mother liquid in recycling treatment of a liquid ammonia neutralizing process; the mother liquid instead of water is sufficiently decomposed with hydrofluoric acid and sulfuric acid; then fluorosilicic acid, sulfuric acid and mother liquid are added for low-acid blending and low-acid extraction; potassium fluotantalate is obtained through transformation and cooling crystallization. According to the method provided by the invention, the use of liquid ammonia is abandoned, and the pollution of ammonia nitrogen is reduced from the source; compared with the traditional process, the discharge of wastewater and the dosage of hydrofluoric acid are greatly reduced, the recycling of industrial potassium fluorosilicate from the mother liquid is realized, and the recycling rate of potassium fluotantalate is as high as 98%.

Description

[0001] technical field [0002] The invention belongs to the technical field of metallurgy, and in particular relates to a method for preparing potassium fluorotantalate from tantalum-containing raw materials (including recycled tantalum materials). Background technique [0003] At present, the production process of potassium fluorotantalate mainly adopts the decomposition of tantalum-niobium ore, adding sulfuric acid to adjust the acidity, extraction, pickling, and stripping to obtain tantalum solution, adding hydrofluoric acid and potassium chloride for conversion, and then cooling and crystallizing to obtain potassium fluorotantalate . The process consumes a lot of hydrofluoric acid, and about 10% of the hydrofluoric acid is discharged in the form of waste gas, which becomes the main source of gas pollution; the mother liquor after crystallization of the intermediate product produced by this process is mainly neutralized by liquid nitrogen at this stage The recycling pro...

Claims

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Application Information

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IPC IPC(8): C01G35/00
Inventor 何平李韧
Owner ZHUZHOU HARD ALLOY GRP CO LTD
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