The method of extraction and separation of derivatives of tungsten and cobalt

 

(57) Abstract:

The method of extraction and separation of derivatives of tungsten and cobalt relates to the field of hydrometallurgy of non-ferrous and rare metals, in particular to the separation and recovery of the product in the solid phase of the sediment and in the aqueous phase of the filtrate. The method can be used for the extraction of tungsten and cobalt from waste wolframkarbid hard alloys in the form of scrap, as well as powdered and pulverized waste. To do this, make processing of the feedstock solution of oxidizing agent in an alkaline medium, followed by their separation through distribution in the solution (the filtrate) and the solid precipitate. Moreover serves for processing the feedstock with any particle size, the extract produced by the oxidation of tungsten and cobalt with sodium hypochlorite in an alkaline medium, and the separation of tungsten acid in the form of a solid residue and a solution of cobalt salts produced by the introduction of the mixture into a solution heated hydrochloric acid followed by filtration. In this case, the processing solution of the oxidizing agent in alkaline medium is carried out at 20-50oWith, and the separation at a temperature of hydrochloric acid 50-100oC. avoids the energy, resource and what kind of scheme and make applicable to any waste in the form of dust, powder, scrap, or mixtures of these fractions. 1 C.p. f-crystals, 1 Il.

The method of extraction and separation of derivatives of tungsten and cobalt relates to the field of hydrometallurgy of non-ferrous and rare metals, in particular to the separation and recovery of the product in the solid phase of the sediment and in the aqueous phase of the filtrate. The method can be used for the extraction of tungsten and cobalt from waste wolframkarbid hard alloys in the form of scrap, as well as powdered and pulverized waste.

Known hydrometallurgical, pyrometallurgical and mixed methods of extraction and separation of tungsten and cobalt from waste wolframkarbid hard alloys:

oxidation firing pulverized waste wolframkarbid hard alloys with pre-treatment with sulfuric or hydrochloric acid and leaching of calcine at normal pressure or in autoclaves (1,2);

- oxidation decomposition of pulverized waste with a mixture of hydrochloric and nitric acid at elevated temperature (3);

- fusion of dusty and powdery wastes with soda and subsequent leaching of compounds of tungsten with water (3).

Known hypochlorination precipitate of cobalt hydroxide fine, poorly filtered, which are difficult to separate. Therefore, prior to the dissolution and separation of cobalt hydrochloric acid or sulfuric acid solution. This method is effective only in about powdered and pulverized waste, as the acidic dissolution/oxidation of cobalt, which in waste typically contains 8-15%, is only on the surface of the pieces and must be preceded by the grinding of bulk material in powder or dust, which leads to energy, time and material costs.

The closest to this technical solution is the method of extracting tungsten and cobalt from the carbide waste, including processing of raw materials with sodium hypochlorite in an alkaline medium and the subsequent separation of the derivatives of tungsten and cobalt(4).

The technical result of the proposed method of extraction and separation of derivatives of tungsten and cobalt is the creation of a cheap, simple, universal technological scheme effective waste management in any degree of dispersion: powdered, pulverized, and also in the form of carbide valframbert scrap.

The technical result to the bottom of the raw material with sodium hypochlorite in an alkaline medium and the subsequent separation of the derivatives of tungsten and cobalt, when this processing is subjected to raw materials with any particle size, and the division lead by introducing obtained after processing the mixture heated hydrochloric acid to obtain tungstic acid in the form of a solid residue and a solution of cobalt salts; the processing is carried out at 20-50oWith, and the separation at a temperature of hydrochloric acid 50-100oC.

Processing waste any degree of dispersion avoids the energy, resource and time costs associated with their crushing or separation into fractions, that is, to unify the technological scheme and make applicable to any waste in the form of dust, powder, scrap, or mixtures of these fractions. Other methods of extraction and separation of the grinding pieces of scrap is necessary because the process of dissolution of cobalt is only on the surface of the pieces.

The operation input into the solution and precipitated in fine sediment, poorly filterable cobalt hydroxide heated hydrochloric acid solution eliminates the prior dissolution of cobalt and remove it from the sphere of reaction (PP.3Iand 4Iand to use the mixture directly to obtain legkorazmyvaemykh fractions derived tungsten is aemula (II) methods.

The essence of the proposed method (II), schematically represented in the drawing, is as follows.

In the first stage of the process waste solid alloys with different sizes of particles are oxidized with sodium hypochlorite in an alkaline environment (p. II.1) at a temperature of 20-50oC. produce a solution of sodium tungstate, unreacted hypochlorite, sodium hydroxide, free chlorine and precipitate cobalt hydroxide. The resulting solution and the precipitate is not shared, as usual, and add heated to 50-110oWith hydrochloric acid (ii. II.2). Get a mixture of legkorazmyvaemykh fractions. In the sediment falls tungsten acid, and the solution in the form of chloride shifting the entire cobalt. The precipitate is separated on a filter (p. II.3), washed (p. II.4) and goes on ammonia treatment, and from the filtrate with a solution of oxalic acid is precipitated cobalt oxalate. Tungsten acid after the ammonia purification is made red-hot and in the form of tungsten trioxide is reduced by hydrogen or carbon to metallic tungsten. The cobalt oxalate is made red-hot until the oxide of cobalt, which hydrogen is recovered in pure cobalt.

Example.

To 100 kg of carbide scrap - clove exhaust roller bits, alloy VK-8, enamel is of sodium chlorite and at periodic bubbling and a temperature of 20-50oWith weathered system 20-25 hours then turned on the mixer, heated the mixture to 50-110oWith and poured 200-250 kg of hydrochloric acid, heated to 50-110oC. Stirring is continued for 40-60 minutes After the system has withstood several hours for a complete sludge, after which the mixture is dropped on a filter, washed and dried. Received 1100-1200 kg of a solution containing cobalt chloride, about 1.5% (17-18 kg, calculated on the anhydrous salt) and 60-80 kg of tungstic acid. Tungsten acid was introduced coarse legkopolirujushchiesja fraction with a sodium content of about 0,005% and chlorides of 0.001%. Cobalt obtained by reduction with hydrogen after deposition and annealing oxalic acid cobalt, contained traces of sodium and chlorine.

The implementation of the reaction at a lower temperature of hydrochloric acid leads to the formation of the monohydrate tungsten acid and "white" modification, fine and truefilter. The temperature of the reaction leads to intensive evaporation of hydrochloric acid and intensive corrosion of the equipment.

Comparing the above two technological schemes on the drawing gives reason to believe that the proposed scheme II is more economical scheme I, because the technology of the Ohm's hard alloys is very energy intensive and heavily wears the grinding units).

Sources of information

1. Yurkevich Y. N.,.Yanshin, S. I. "Development of technology for processing of pulverized waste from sharpening carbide tools. The report of the all-Union scientific research Institute of solid alloys, 1967.

2. Matusevich W. And.. Sviridovskiy P. M. "the Development and use of technologies of production of tungsten trioxide and nitric oxide cobalt-rich pulverized waste". The report of the all-Union scientific research Institute of solid alloys. 1953.

3. Reznichenko Century A. "the metallurgy of tungsten, molybdenum and niobium". 1967, S. 43, S. 91.

4. Zelikman A. N. and other Tungsten, M., metallurgy, 1978, S. 89, 4th paragraph.

1. The method of extracting tungsten and cobalt from the carbide waste, including processing of raw materials with sodium hypochlorite in an alkaline medium and the subsequent separation of the derivatives of tungsten and cobalt, characterized in that the treatment machine raw material with any particle size, and the division lead by introducing obtained after processing the mixture heated hydrochloric acid to obtain tungstic acid in the form of a solid residue and a solution of cobalt salts.

2. The method according to p. 1, characterized in that the processing carried out at 20-50oWith, and the separation at a temperature of hydrochloric acid 50-100oC.

 

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