Extraction of molybdenum from aqueous solutions of wolframates

 

(57) Abstract:

The invention relates to a process for recovering molybdenum from aqueous solutions of tungstate and can be used in ferrous and nonferrous metallurgy, as well as treatment of industrial and domestic wastewater. The method of extraction of molybdenum from concentrated aqueous solutions of tungstate comprises preparing an acidic solution introduction in the original solution of hydrogen peroxide and acids, the extraction of molybdenum and the subsequent deposition of the raffinate tungsten acid. Preparation of the solution before the extraction is carried out by introducing first, hydrogen peroxide, and then hydrochloric acid, and extraction was carried out with a solution of trialkylamine and isooctyl alcohol in kerosene. The method is cheap and effective, reduces the consumption of reagents. 10 table.

The method of extraction of molybdenum from aqueous solutions of tungstate refers to the extraction of substances extraction and selective precipitation from aqueous solution and can be used in ferrous and nonferrous metallurgy, as well as treatment of industrial and domestic wastewater.

A known method of purification of aqueous solutions of wolframite by precipitation of poorly soluble trisulde molybdenum, based on R the I Universities. Non-ferrous metallurgy. 1979. 3. S. 97-103].

The disadvantages of the method are the hydrogen sulphide in the deposition of trisulde molybdenum, which requires the cost of disposal of gases, the need to heat the solution, this method does not provide deep cleaning.

The closest technical solution is the method of extraction of molybdenum from concentrated aqueous solutions of tungstate, comprising preparing an acidic solution introduction in the original solution of hydrogen peroxide and acids, the extraction of molybdenum and the subsequent deposition of the raffinate tungsten acid [US 4275039, CL 01 G 39/00 from 23.06.1981].

The disadvantages of this method are the high consumption of reagents, and the use of expensive and hard-to-reach extractants.

Object of the invention is the extraction of molybdenum from concentrated aqueous solutions of tungstate using inexpensive and readily available extractant, and reducing consumption of Realengo.

The technical result, which can be obtained by carrying out the invention, lies in the efficiency and effectiveness of the process of removing molybdenum from concentrated aqueous solutions of tungstate extraction, "ptx2">

This technical result is achieved by the fact that in the known method for extracting molybdenum from concentrated aqueous solutions of tungstate, comprising preparing an acidic solution introduction in the original solution of hydrogen peroxide and acids, the extraction of molybdenum and the subsequent deposition of the raffinate tungsten acid, the preparation of the solution before the extraction is carried out by introducing first, hydrogen peroxide, and then hydrochloric acid, and extraction was carried out with a solution of trialkylamine and isooctyl alcohol in kerosene.

The essence of the method is illustrated in table. 6-10, in which are given the results of the extraction of molybdenum from concentrated aqueous solutions of tungstate extraction solution trialkylamine and isooctyl alcohol in kerosene and subsequent sedimentation of the raffinate tungsten acid.

Examples of specific implementation method.

Example 1 (table. 6).

The original solution volume 70 cm3with the content 120 g/DM3W(VI) and 1.2 g/DM3Mo(VI) (weight ratio of Mo(VI) W(VI)=1:100), was prepared by dissolving salts of Na2WO42H2O and PA2Moo42H2O in distilled water. To the resulting solution were added first 36% peroxide solution n solution was extracted with molybdenum at pH 0 and the volume of extractant 35 cm3(composition of the extractant, wt.%: trialkylamine - 8, isooctyl alcohol - 15, kerosene - else), from the raffinate besieged tungsten acid at pH 0. The content of W(VI) and Mo(VI) in the original solution, raffinate and a clarified water phase after deposition of tungsten acid was determined by the weight and photocolorimetric methods on the photocolorimeter brand KLF-3. The content of components in the extract was determined but the difference between the concentrations of the components in the initial solution and in the raffinate. The pH value of the solution was measured by pH-meter pH-121.

The results of extraction are presented in table. 6, in which are given extraction time , min, concentration of ions of molybdenum and tungsten in the raffinate, mg/DM3the distribution coefficient D, as the ratio of the concentrations of the components in the extract and the raffinate, the separation factor , as the ratio of the distribution coefficients of molybdenum and tungsten, extract, wt.%

From the data table. 6 we can draw the following conclusions:

1. Within 30 min of extraction of the molybdenum content is reduced from 1,204 to 0,224 g/DM3further, the molybdenum content slightly increases to 2 hours of extraction is 0,260 g/DM3.

2. Within 2 hours extraction nigerianotre decreases from 0.89 to 0.23 percent.

4. The best indicators of extraction obtained within 30 min of extraction and make up: DMo=8,75; = 11,36; Mo/(Mo+W)=0,23%.

5. Increasing the number of operations of extraction, it is possible to achieve the required degree of purification of tungsten from molybdenum impurities.

After 2 hours of extraction, the extract was separated from the raffinate in the last besieged tungsten acid. In the deposition process of tungsten acid purification from molybdenum continues (see table 1).

The speed of lightening tungsten acid when it is precipitation of the raffinate is characterized by the indicators in table 2.

Thus for a time less than one day deposited 97% tungsten acid, in the future is uplotnenie draft: two days after the sediment is compacted by 8.8% compared with the sediment obtained through the day deposition.

The precipitate is well filtered and washed.

Example 2 (table. 7).

Extraction of molybdenum from the aqueous solution of tungstate was carried out analogously to example 1 with the only difference that the process was carried out using a smaller amount of peroxide in a molar ratio of N2ABOUT2:(W+Mo)=1:1.

From the data table. 7 we can draw the following conclusions:

1. Within 45 minichello increases to 2 hours of extraction is 0,310 g/inch

2. Within 2 hours of extraction, the content of tungsten in solution is reduced by 15.7%.

3. In the extraction process, the mass ratio of Mo:(Mo+W) in the solution decreases from 0,86 to 0.35%.

4. The best indicators of extraction obtained for 45 min extraction and make up: DMo=4,71; = 13,85; Mo/(Mo+W)=0,30%.

5. Increasing the number of operations of extraction, it is possible to achieve the required degree of purification of tungsten from molybdenum impurities.

After 2 hours of extraction, the extract was separated from the raffinate in the last besieged tungsten acid. In the deposition process of tungsten acid purification from molybdenum continues (see table 3).

The precipitate is well filtered and washed.

Compared with example 1 was slightly lower all parameters extraction and subsequent precipitation of tungstic acid.

Example 3 (table. 8).

Extraction of molybdenum from the aqueous solution of tungstate was carried out analogously to example 1 with the only difference that the process was carried out with the use of more peroxide at a molar ratio of N2ABOUT2:(W+Mo)=2.5 To 1.

From the data table. 8 you can make the following conclusions:

1. Within 30 min of extraction is maintained is of 15 min extraction, the content of tungsten is reduced by 30.7%.

3. In the extraction process, the mass ratio of Mo:(Mo+W) in the solution decreases from 0,86 to 0.58%.

The precipitate is well filtered and washed.

Compared with example 1 dramatically increases the rate of formation of tungstic acid in the raffinate, the precipitate formed after 30 min of extraction. Within 15 min parameters extraction similar to those presented in example 1.

Example 4 (table. 9).

Extraction of molybdenum from the aqueous solution of tungstate was carried out analogously to example 1 with the only difference that the process was carried out at higher concentrations of molybdenum (VI), a component of 5.0 g/DM3(the weight ratio of Mo(VI) W(VI)=1:24).

From the data table. 9 we can draw the following conclusions:

1. Within 15 min of extraction of the molybdenum content is reduced from 3950 to 2270 g/DM3.

2. Within 15 min of extraction of tungsten content is reduced by 19.4%.

3. In the process of extraction for 15 min mass ratio of Mo:(Mo+W) in the solution decreases with 3,27 to 2.58%.

4. There exists an optimal extraction time (15 min) at which the maximum separation performance.

After 30 min of extraction, the extract was separated from the raffinate in the last besieged in Jerusalem. 4).

In less than 3 hours obtained the best results for cleaning sludge from molybdenum when removing tungsten precipitates more than 95%.

The speed of lightening tungsten acid when it is precipitation of the raffinate is characterized by the following indicators (see table 5).

In less than 1,5-3,0 h is deposited over 95% tungsten acid, in the future, the amount of loose sediment increases slightly.

The precipitate is well filtered and washed.

Compared with example 1 of the best indicators of extraction and precipitation obtained at the initial moment of time.

Example 5 (table. 10).

Extraction of molybdenum from the aqueous solution of tungstate was carried out analogously to example 1 with the only difference that the process was carried out without the use of peroxide.

From the data table. 10 it follows that the extraction of molybdenum and tungsten minor, separation of these components is almost not happening.

After two hours of extraction, the raffinate was separated from the extract.

The raffinate was a turbid colloidal solution from which, within two hours the precipitate does not fall out.

The process is inefficient.

Experimental data the slots, containing not more than 0, 04% molybdenum when removing tungsten acid in a single operation in the processes of extraction and deposition of at least 70%.

Extraction with peroxide and subsequent precipitation of tungstic acid from the raffinate contributes to obtaining a precipitate tungstic acid with low impurity content of molybdenum, while the deposition rate of tungsten acid is great.

The precipitate tungstic acid after washing you can use to obtain the anhydride or parabolicamara ammonium in the usual way.

The clarified aqueous phase obtained after deposition of tungsten acid, is a 1 M solution of hydrochloric acid containing a small amount of peroxide. This solution can be used in technological processes at wastewater from organic components in the oxidation of gaseous components, for oxidation of metal ions (Fe2+Cu2+and so on) and for other purposes.

The extract can be processed in the usual way.

In combination with the optimal number of operations of extraction cycles and precipitation of tungstic acid on the proposed technology can perform a deep cleaning of voltra is determined by the stoichiometry of the reaction kompleksowe in the extract phase, the deposition rate of tungsten acid, temperature, initial concentration of the components of the solution, ionic strength of the solution, the molar ratio of ions of molybdenum and tungsten in solution, the pH value of the solution and other factors.

Way better than a higher concentration of tungsten ions and lower the concentration of ions of molybdenum in the original cleaning solution. The proposed method can be used in the decomposition Selimovic concentrates acids.

Compared with the prototype of the proposed method is more versatile, reduces the amount of extractant and other reagents, reduces the number of stages, allows to obtain a dense, well-filtered, the precipitate tungstic acid with the required degree of purification from the impurity of molybdenum, and the precipitated acid may be used to obtain anhydride or parabolicamara in the usual way.

The method of extraction of molybdenum from concentrated aqueous solutions of tungstate, comprising preparing an acidic solution introduction in the original solution of hydrogen peroxide and acids, the extraction of molybdenum and the subsequent deposition of the raffinate tungsten acid, characterized in that the preparation of the solution will move solution trialkylamine and isooctyl alcohol in kerosene.

 

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