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Method for purifying tantalum powder

A technology of tantalum powder and alkali metal, which is applied in the field of purifying tantalum powder from a mixture containing tantalum powder, alkali metal and alkali metal halide, which can solve the problem of high content of K and Na in tantalum powder, reduced yield of tantalum powder, and difficulty in cleaning Eliminate other problems, achieve the effect of high purity of raw powder, high yield of tantalum powder, and low leakage current

Active Publication Date: 2014-05-28
NINGXIA ORIENT TANTALUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this prior art process has the following problems: on the one hand, the generated potassium tantalate is easily soluble in water, so that part of the tantalum enters the waste liquid, and the yield of tantalum powder is reduced; on the other hand, the generated potassium metatantalate and tantalum Sodium tantalate / sodium metatantalate is difficult to dissolve in water and is not easy to wash off, resulting in high K and Na content in tantalum powder
However, this method has many disadvantages

Method used

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  • Method for purifying tantalum powder
  • Method for purifying tantalum powder

Examples

Experimental program
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Effect test

Embodiment 1

[0041] First, a mixture containing tantalum powder, alkali metal and alkali metal halide is provided by the following method: 100kg of sodium chloride (NaCl) is charged into the reaction vessel, heated to 900°C, and 100kg of potassium fluorotantalate ( K 2 TaF 7 ), then add about 30kg of liquid metal sodium, keep warm at 900°C for 2 hours, cool to room temperature to obtain a mixture of tantalum powder, alkali metal and alkali metal halide in the form of condensed block, take out the condensed block from the reaction vessel, Break into small pieces less than 20mm, and divide into two evenly.

[0042] Then, add the hydrochloric acid aqueous solution that 3 / 4 tank pH value is 4.0 in the filter washing tank, add the first small piece in the filter washing tank and wash, guarantee that the aqueous solution liquid level is higher than the reaction material surface more than 10cm in the washing process; In the first 1 hour of washing, use pH test paper to detect the pH value of th...

Embodiment 2

[0051] First, the mixture containing tantalum powder, alkali metal and alkali metal halide is provided by the following method: put a mixture of 100kg potassium chloride (KCl) and 100kg potassium fluoride (KF) in a reaction vessel, heat to 900°C, and then Add 100kg potassium fluorotantalate (K 2 TaF 7 ), then add about 30kg of liquid metal sodium, keep it warm at 900°C for 1 hour, and after cooling to room temperature, take out the reaction product from the reaction vessel, that is, a mixture of tantalum powder, alkali metal and alkali metal halide in the form of condensed block, and crush it into small pieces smaller than 20mm, and divide the crushed material into two parts equally.

[0052] Then, add 3 / 4 tank of hydrochloric acid aqueous solution with a pH value of 4.0 to the filter washing tank with stirring paddle, turn on the stirring paddle, and the rotating speed of the stirring paddle is 10 rpm; add the first small piece into the filtering tank for washing , in the f...

Embodiment 3

[0061] First, the mixture containing tantalum powder, alkali metal and alkali metal halide is provided by the following method: put a mixture of 150kg potassium chloride (KCl) and 150kg potassium fluoride (KF) in a reaction vessel, heat to 880°C, and then In the reaction vessel, add 30kg potassium fluorotantalate (K 2 TaF 7 ), then add about 10kg of liquid metal sodium, keep it warm at 880°C for 0.5 hours, and after cooling to room temperature, take out the reaction product, that is, the condensed block, from the reaction vessel, break it into small pieces smaller than 20mm, and divide the broken material into two share.

[0062] Then, add 3 / 4 tank of hydrochloric acid aqueous solution with a pH value of 4.0 in the filter washing tank, add the first small pieces into the filter washing tank for washing, and ensure that the aqueous solution has no reaction materials during the washing process; in the first 1 hour of washing In the washing tank, check the pH value of the aqueo...

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Abstract

The invention relates to a method for purifying tantalum powder. The method comprises the following step of washing a mixture containing tantalum powder, alkali metal and alkali halide by using an aqueous solution of acidic electrolyte and further comprises the following specific steps of: providing the mixture comprising the tantalum powder, the alkali metal and the alkali metal halide; putting the mixture comprising the tantalum powder, the alkali metal and the alkali metal halide into a filtering and washing tank containing the aqueous solution of the acidic electrolyte, washing out impurities, such as alkali metal halides as well as K, Na and oxides thereof by using the aqueous solution of the acidic electrolyte, monitoring pH of the aqueous solution at the same time, and filtering to obtain a first filter cake till no mixture particle of alkali metal salts can be seen by naked eyes and pH value of the aqueous solution is unchanged; putting the first filter cake to a deionized-water-containing stirring and washing tank, carrying out stirring and washing, and then filtering to obtain a second filter cake; putting the second filter cake to a pickling bath and pickling for 2-4 hours, and then filtering to obtain a third filter cake, wherein the pickling bath contains 10wt% of aqueous mixture solution prepared from hydrochloric acid, nitric acid, hydrofluoric acid and hydrogen peroxide; and drying the third filter cake to obtain raw tantalum powder.

Description

technical field [0001] The invention relates to a method for purifying tantalum powder, in particular to a method for purifying tantalum powder from a mixture containing tantalum powder, alkali metal and alkali metal halide. Background technique [0002] Tantalum is a rare metal, mainly used in the electronics industry, chemical equipment, metal cutting, aerospace and other industries. In recent years, the consumption of tantalum has grown rapidly, but resources are scarce. Therefore, it is a development trend of the tantalum industry to effectively utilize tantalum resources and reduce the waste of tantalum. [0003] In the electronics industry, the main use of tantalum powder is to manufacture electrolytic capacitors. The development trend of tantalum electrolytic capacitors is to require high capacitance, low leakage current and low equivalent series resistance (low loss for the anode). Tantalum powder, the main material of tantalum electrolytic capacitor anode, requires...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B34/24C22B9/02B22F1/00
CPCY02P10/20
Inventor 林辅坤马跃忠王春翔王治道雒国清张学清杨生芳冒海红习旭东王宁张洪刚景镇远高淑琴任萍
Owner NINGXIA ORIENT TANTALUM IND
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