Procedure for extraction of nickel from solutions and for purification from impurities

FIELD: metallurgy.

SUBSTANCE: procedure for extraction of nickel from solutions and purification from impurities: Cr3+, Fe3+, Al3+, Cu2+, Zn2+, Co2+, Fe2+, Mn2+, Ca2+, Mg2+ consists in bringing pH of solutions to values 4.0-6.5, in sorption of nickel at pH=4.0-6.5 from solutions or pulps on sub-acid cationites, in desorption of nickel from saturated cationites with solution of sulphuric or hydrochloric acid with production of solution of nickel strippant. Before desorption saturated cationite is treated with solution of nickel purified from impurities, also with portion of solution of strippant with concentration of nickel higher, than its concentration in source solution or pulp coming to sorption at a value of pH less, than pH of solution or pulp in the process of sorption. Ratio of CNI:ΣCimpurity in solution of strippant changes from 7:1 to 500:1.

EFFECT: more deep purification of solution of nickel strippant from impurities.

4 tbl

 

The invention relates to hydrometallurgy, and in particular to methods of extraction of Nickel from aqueous solutions and purification from impurities using ion-exchange resins.

The method for extracting Nickel from slurries of the oxidative leaching of pyrrhotite concentrates using weak acid carboxylic cation exchangers, including cationic chelate type calcium form: SG-1, KB-4, KM-2S, ANKB-35 (see Ova and Nijubashimae. The use of sorption technologies for processing slurries from the autoclave oxidative leaching of pyrrhotite concentrates Tsvet, No. 1, 1985). The liquid phase of the slurries had a complex chemical composition containing, along with Nickel, cobalt impurities, copper, zinc, iron, aluminum, manganese, magnesium and calcium commensurate with Nickel concentrations. To increase the capacity of ion exchangers for non-ferrous here recommended between cycles of sorption process saturated cation exchange resin with an alkaline reagent, in particular lime, with additional sorption and subsequent desorption of non-ferrous metals with a solution of sulfuric acid to obtain a solution decorate. It is further recommended that additional deeper cleaning solution decorate Nickel from iron, cobalt, copper and zinc by chemical deposition. The Nickel concentration in the liquid phase of the pulp was 4-5 g/is, in the solution of decorate - 30-50 g/l

Described in a similar way to the extraction and refining of Nickel during sorption processing allows only partially clear solution decorate from the impurities of iron, aluminum, calcium and magnesium, and does not allow to separate Nickel from cobalt and other base metals.

There is also known a method of cleaning and extraction of Nickel and cobalt from solutions from the leaching of pyrite Ogarkov using weak acid carboxylic cation exchanger KB-P in sodium or calcium form (see Lseskin, Way and other Extraction and sorption in non-ferrous metallurgy. M, metallurgy, 1968. VNIItsvetmet. Sat. No. 12). Initial solutions contained: Ni2+, Fe3+, Al3+, Cu2+, Zn2+With2+, Fe2+, Mn2+Ca2+, Mg2+. They were treated with soda ash or lime and oxygen for oxidation of Fe2+and precipitation of Fe3+and other impurities in the form of hydrates at pH 5.0-5.5. Next were the sorption of non-ferrous metals directly from hydrate slurries in counter-current mode with the Department of ion-exchange resin from the pulp on the net, desorption was performed 4 N. HCl. Then a solution of decorate processed extraction for the separation of non-ferrous metals.

Described in a similar way to the extraction and refining of Nickel during sorption processing allows only partial purge process is decorate from iron impurities, aluminum, calcium and magnesium, and does not allow to separate Nickel from cobalt and other base metals.

The present invention is to develop a method for extracting Nickel from acidic solutions and a deeper purification using ion-exchange resins, weak acid cation exchangers, including cationic chelate type.

The problem is solved in that the saturated at pH 4.0 to 6.5 from solutions or slurries of the complex structure of the cation exchanger before desorption is treated with a solution of Nickel, free from impurities, with the concentration of Nickel is greater than its concentration in the initial solution or pulp entering the sorption at pH values less than pH value of the solution or slurry in the process of sorption.

The invention consists in the following. The capacity of the weak acid cation exchange resin according to any of Jonah, when sorption from solutions of complex composition ceteris paribus depends on the ion concentration in the solution, the pH of the solution in the phase resin and ion affinity to the functional group of the cation, or position it in a range of selectivity. The affinity of those or other ions to the functional groups of weak acid cation exchangers, including cationic chelate type is defined as a property of the ion, and a property of the functional groups, and in General is subject to the following range selectivity:

N+ >Cr3+>Fe3+>Al3+>Cu2+>Ni2+>Zn2+>With2+>Fe2+>Mn2+>CA2+>Mg2+>Na+(see kN. Cebelia and other Resins in non-ferrous metallurgy, M., metallurgy, 1975.). Given the selectivity series is not very different with respect to different weak acid to the cation. And these differences are not in this case fundamental. Of the number of selectivity follows that if lead sorption in continuous countercurrent decantation of the solution or slurry and cation exchange resin (to achieve equilibrium concentration of Nickel on the pitch at its original size in solution), then the resin will be mainly absorb Nickel ions and Cr3+>Fe3+>Al3+>Cu2+. Ions as Zn2+>With2+>Fe2+>Mn2+>CA2+>Mg2+>Na+will be only partially absorbed and displaced from the phase of the resin in the tail nurseries sorption. If saturated in equilibrium cation exchange resin treated with a solution of Nickel, purified from the above impurity concentration of Nickel is greater than its concentration in the initial solution supplied to the sorption, the equilibrium will change. In this case, part of the impurities viesnica of phase resin (more to the right of the Nickel in a row, at least to the left of the Nickel in the series), and the capacity is of Oranta Nickel will increase. And the higher the concentration of Nickel is used for such processing, the more the cation exchanger, and hence the subsequent solution decorate Nickel will be cleansed of impurities.

For weak acid cation exchange resin containing carboxylic, phosphonic or other functional groups that strongly binds hydrogen ions (H+) and weakly dissociable in an acidic environment, is of great importance and the value of pH of the solution in the phase resin. The lower the pH value, the more difficult sorption for all ions of a given selectivity series (more to the right of the Nickel in a row, at least to the left of the Nickel in a row).

If saturated in equilibrium cation exchange resin treated with a solution of Nickel, purified from the above impurity concentration of Nickel is greater than its concentration in the initial solution supplied to the sorption at pH values less than pH value of the solution or slurry in the process of sorption, the equilibrium in the phase resin will change even more. And the more the cation exchanger, and therefore the subsequent solution decorate Nickel will be cleansed of impurities.

In the analog, it is shown that the test cation KB-P in the range pH 4.0-9.0 the greatest selectivity for non-ferrous metals obtained at pH values between 5.5 and 6.5 (see Lseskin, Way and the other EXT the action and sorption in non-ferrous metallurgy, M, metallurgy, 1968. VNIItsvetmet. Sat. No. 12). However, proceeding from the above as applied to the purification of Nickel, it is better to sorption in the pH value, as can smaller - in the range of 4.0 to 6.5. It is likely that the capacity of Nickel in this case will decrease, but the relative capacity of impurities will decrease even more. When bringing the pH of the initial solution the main criteria should be the pH value of the precipitation of hydrates oxides ions of impurities, the concentration of impurities in the initial solution and of the requirements for the purity of the Nickel solution decorate. For example, the almost complete precipitation of the hydroxide of Fe3+is achieved at pH 4.0, hydrate Al3+- at pH of 5.2, hydrates Cr3+and Cu2+- at pH 6,7-6,8, hydrates Zn2+, Ni2+With2+and Fe2+- at pH 8.0 and 9.7 (see kN. Yu. Handbook of analytical chemistry. M, Chemistry, 1971). Therefore it is better to bring the pH of the initial solution to the minimum values (in the range of 4.0 to 6.5), though not complete, but the maximum possible precipitation of impurities, standing on the far left of the selectivity of Nickel. Thus in the process of sorption significantly reduced the capacity of the resin for the removal of impurities, standing to the right of the Nickel in the series. For example, lead sorption at pH 4.5 to 5.0, when fully precipitated Fe3+and Al3+mostly Cr3+and Cu2+. This conclusion is due to the fact that the note is C the right of Nickel have similar with Nickel, or large pH precipitation of hydrates and to clear them from the solution of Nickel hydrolysis is not possible. Clean Nickel residue admixtures, standing on the far left of the selectivity can be further handling solution decorate alkaline reagent to pH deposition of their hydrates. If the concentration of impurities to the right of the Nickel in a row in the source solution is not large, the sorption can be maintained and at a pH of 6.5 - to get the maximum capacity of the resin for Nickel.

For the sample experiments we used the solution from the leaching tests silicate Nickel ore with a solution of sulfuric acid in the laboratory. The original solution from the leaching of silicate Nickel ore had the following composition, g/l: Ni2+- 1,740, With2+- 0,064, Cr3+- 0,031, Fe3+- 5,341, Al3+- 0,865, Cu2+- 0,040, Zn2+- 0,035, Fe2+- 0,080, Mn2+- 0,585, CA2+- 0,323, Mg2+- 8,572 (pH 2.0). Samples of the solution were treated with chalk and reach values in the range pH 4.0 to 6.5. As sorbents were tested weak acid cation exchangers of the following brands: S-106, S-930, firm Pluralit (Purolite); Lewatit TP-207, firm LANXESS (Lanxess) and SN-23, firms Resinex (Resinex). All tested resin showed essentially similar results to demonstrate which will present data on the use of cation exchange resin Lewatit TP-207.

Dissolve the above composition was treated under stirring finely ground chalk (caso 3), resulting hepahydrate pulp with a pH of 4.5. Sorption on ion exchange resin in the H+form was carried out in a continuous countercurrent decantation 4xstages of sorption under stirring at each step for 1 hour. Then the sample resin was separated from the pulp in the sieve and was introduced to the next stage of sorption and uterine pulp is contacted with the next portion of the resin. Just contact time was 4 hours, the ratio of the volume of pulp and resin in each stage is 18:1. At each stage of sorption is pH 4.5 was supported by additional dosage of chalk. Thus obtained, saturated with Nickel resin was thoroughly washed on a sieve with distilled water from the pulp and the pore solution and was used in experiments on desorption with pre-treatment and without it.

Sample saturated resin 60 ml was loaded in a vertically mounted glass column, as the transport of moisture was also used distilled water. As desorbent was used a solution of sulfuric acid 100 g/l with a ratio of solution volume to 1 volume of resin (Vp-pa/Vresinin all experiments is 1.5:1. The feed solution desorbent in each experiment was carried out by a peristaltic pump for 2xhours filtering solutions from the bottom up.

In known ways is at (experiment 1) was carried out desorption of Nickel. The proposed method was carried out series of experiments with pre-treatment of the resin with a solution of pure Nickel with different concentration and pH value. Supply of pure solution of Nickel when the processing was carried out also from the bottom up with a ratio of Vp-pa/Vresin=0,7:1 for 1 hour. This ratio corresponded to the pore volume of the resin, found empirically, and predetermined minimum overshoot of Nickel in the mother liquor. For treatment was prepared solution of pure Nickel sulfate 30 g/l brand NS-1 (GOST 2665-85). A solution of pure Nickel sulfate had the following composition, g/l: Ni2+- 30,010, With2+at 0.020, Cr3+is 0.001, Fe3+- 0,0005, Al3+is 0.001, Cu2+- 0,001, Zn2+is 0.001, Fe2+- UTS., Mn2+- 0,001, CA2+- 0,003, Mg2+- 0,002 (pH 4.5). This solution is brought to the required values for the concentrations of Nickel (dilution) and pH values (sulfuric acid). After treatment in each experiment was conducted desorption mode, similar to that of experiment 1 without processing.

In the first series of experiments on the proposed method (experiments 2, 3, 4) Nickel concentration in pure solution when processing was 10, 20 and 30 g/l (more than 1,740 g/l in the initial solution supplied to the sorption), and a pH value of 4.5 was the same in all three experiments as in the sorption process. The results are presented in table 1. How is C 1, in experiment 1 by a known method, the ratio of the concentrations of Nickel and the sum of the concentrations of impurities in the solution of decorate amounted to, CNiimpurities=7:1. In experiments 2, 3, 4 in the proposed method, it increased from 22:1 to 51:1, indicating a significant cleaning solution decorate Nickel impurities. The concentration of Nickel in decorate increased from 21 g/l to 25-35 g/l

In the second series of experiments on the proposed method (experiments 5, 6, 7) Nickel concentration in pure solution was the same and amounted to 20 g/l (more than 1,740 g/l in the initial solution supplied to the sorption), and the pH value is 3.5; the 3.0 and 2.5 (less than 4.5 in the original solution). The results are presented in table 2. The data indicate that with decreasing pH of the solution during processing of pure resin with a solution of Nickel from 4.5 to 2.5, the ratio of CNiimpuritiesincreased from 40:1 to 486-500:1, what happened was much deeper cleaning solution decorate Nickel impurities. The specific consumption of pure Nickel was 14 g per 1 l of resin or about 30% of the total extracted Nickel.

From the second series of experiments it is possible to conclude that if part of the solution decorate Nickel, refined, display, and use in circulation for processing a saturated resin, Nickel phase resin, and hence the entire solution decorate Nickel will be bol is e to deeply cleanse away impurities without additional consumption of pure Nickel. Therefore, in experiment 8 the sample is saturated resin was processed us part of the solution decorate from experience 6 diluted to 20 g/l and brought to pH 3.0. Comparative results of the experiment 8 and experiments 1,6 presented in table 3. As follows from table 3, in comparison with the experience of 6, where the treatment was carried out with a solution of pure Nickel, in experiment 8 with the processing of the reverse part of the solution decorate the ratio of CNiimpuritiesslightly decreased from 500:1 to 462:1, but remained significantly higher than in the known method, where the ratio of CNiimpuritieswas 7:1.

Thus, if saturated with Nickel at pH 4.0 to 6.5 from solutions or slurries of complex mixture of weak acid cation exchanger before desorption process with a solution of Nickel, free from impurities, with the concentration of Nickel is greater than its concentration in the initial solution or pulp entering the sorption at pH values less than pH value of the solution or slurry in the process of sorption, extracted in a solution of decorate Nickel more deeply cleansed of impurities and the problem should be resolved.

Table 1
Parameters and valuesThe known methodExperience, №
Experience No. 1234
The Ni concentration, g/l:
- in the original solution by sorption1,741,741,741,74
- in a clean solution when processing-102030
PH value:
- in the original solution by sorption-4,54,54,5
- in a pure solution of Ni when processing-4,54,54,5
UD. the load when the supply of clean the solution of Ni during processing, VR-RA/Vresin-0,70,70,7
The concentration of sulfuric acid in desorbers solution, g/l100100100100
The output solution of decorate, VR-RA/Vresin1,51,51,51,5
The output of the recovered Nickel, g on 1 l of resin30,7837,8245,0652,51
UD. consumption of pure Nickel:
- g on 1 l of resin-7,014,021,0
- % the extracted Nickel-183140
The composition of the solution of decorate,g/l:
Nito 20.5225,2130,0435,01
Co0,7450,2550,1200,094
Fe3+0,0110,0100,0110,011
Al0,2800,2680,257is 0.260
Cu0,0270,0230,0250,022
Cr0,0340,0330,0340,030
Zn0,0350,0200,0150,010
Fe2+to 0.0600,020 0,0100,010
Mn0,657of) 0.1570,107is 0.102
Mg0,8870,0880,0580,055
Ca0,3660,1660,1120.104 g
The ratio of CNiimpurities7:122:140:151:1

Table 2
Parameters and valuesThe known methodThe proposed method
Experience, №
Experience No. 13567
The Ni concentration, g/l:
- in the original solution by sorption1,741,741,741,741,74
- in a clean solution when processing20202020
PH value:
- in the original solution by sorption-4,54,54,54,5
- in a pure solution of Ni when processing-4,53,53,02,5
UD. load cleaner solution Ni during processing, VR-RA/Vresin-0,70,70,70,7/td>
The concentration of sulfuric acid in desorbers solution, g/l100100100100100
The output solution of decorate, VR-RA/Vresin1,51,51,51,51,5
The output of the recovered Nickel, g on 1 l of resin30,7845,0645,1245,0240,10
UD. consumption of pure Nickel:
- g on 1 l of resin-14,014,014,014,0
- % the extracted Nickel-31313135
The composition of the solution of decorate, g/l:
Nito 20.5230,0430,0830,0126,73
Co0,7450,1200,0550,0220,029
Fe3+0,0110,0110,0090,0050,001
Al0,2800,2570,0260,0010,001
Cu0,0270,0250,0130,0020,002
Cr0,0340,0340,0230,0040,003
Zn0,0350,0150,0020,0010,001
Fe2+to 0.0600,0100,0020,0010,001
Mn0,6570,1070,0170,0040,002
Mg0,8870,0580,0280,0080,005
Ca0,3660,1120,0160,0120,010
The ratio of CNi:ΣCimpurities7:140:1157:1500:1486:1

Table 3
Parameters and values The known methodThe proposed methodThe proposed method
Experience No. 1Experience, No. 6Experience, no 8
The Ni concentration, g/l:
- in the original solution by sorption1,741,741,74
- in a clean solution when processing-2020
PH value:
- in the original solution in the process of sorption-4,54,5
- in a pure solution of Ni when processing-3,03,0
UD. load cleaner solution Ni during processing, VR-RA/Vresin-0,70,7
The concentration of sulfuric acid in desorbers solution, g/l100100100
The output solution of decorate, VR-RA/Vresin1,51,51,5
The output of the recovered Nickel, g on 1 l of resin30,7845,0245,0
UD. consumption of pure Nickel:
- g on 1 l of resin-14,0-
- % the extracted Nickel-31-
The composition of the solution, g/l:desorbeddesorbeddesorbed
Nito 20.5230,0130,0
Co0,7450,0220,24
Fe3+0,0110,0050,004
Al0,2800,0010,001
Cu0,0270,0020,002
Cr0,0340,0040,005
Zn0,0350,0010,001
Fe2+to 0.0600,0010,001
Mn0,6570,0040,005
Mg0,8870,0080,010
Ca0,3660,0120,015
The ratio of CNiimpurities7:1500:1462:1

Woytach with hydrochloric acid as desorbent was used a solution of hydrochloric acid 100 g/l under the same parameters, as in the experiments with sulphuric: the ratio of volume of solution per volume of resin (VR-RA/Vresinin all experiments is 1.5:1. The feed solution desorbent in each experiment was carried out by a peristaltic pump for 2xhours filtering solutions from the bottom up. By a known method (experiment 9) was carried out desorption of Nickel. The proposed method was carried out series of experiments with pre-treatment of the resin with a solution of pure chloride of Nickel with different concentration and pH value. Supply of pure solution of Nickel chloride in the processing was carried out also from the bottom up with a ratio of VR-RA/Vresin=0,7:1 for 1 hour. For treatment was prepared solution of pure Nickel chloride 30 g/l qualification "chemically pure". The clean solution of Nickel chloride had the following composition, g/l: Ni2+- 30,170, With2+- 0,005, Cr3+is 0.001, Fe3+- 0,0005, Al3+is 0.001, Cu2+- 0,001, Zn2+is 0.001, Fe2+- UTS, Mn2+- 0,001, CA2+- 0,001, Mg2+- 0,001 (pH 4.5). The most optimal in the processing, as well as in experiments with Nickel sulfate, was a solution of Nickel chloride with a concentration of 20 g/l of Nickel and at pH 3.0. After processing was carried out desorption of Nickel, the results are shown in experiment 10. In the experience of 11 part of the solution dealbata of Nickel chloride from the experience of 10 was diluted to 20 g/l of Nickel and brought to pH 3.. Followed by processing fresh portions of saturated resin and subsequent desorption solution of hydrochloric acid. Performance experiments are shown in table 4.

Table 4
Parameters and valuesThe known methodThe proposed methodThe proposed method
Experience No. 9Experience, No. 10Experience, No. 11
The Ni concentration, g/l:
- in the original solution by sorption1,741,741,74
- in a clean solution when processing-2020
PH value:
in Ref. the solution in the process of sorption-4,54,5
- in pure chloride solution Ni when processing-3,03,0
UD. load cleaner solution Ni during processing, Vp-pa/Vresin-0,70,7
The concentration of hydrochloric acid in desorbers solution, g/l100100100
The output solution of decorate, Vp-pa/Vresin1,51,51,5
The output of the recovered Nickel, g on 1 l of resin30,8045,0545,01
UD. consumption of pure Nickel:
- g on 1 l of resin-14,0-
- % the extracted Nickel-31-
The composition of the solution decor the ATA, g/l:desorbeddesorbeddesorbed
Ni20,5530,0230,0
Co0,7480,0120,018
Fe3+0,0100,0050,006
Al0,2850,0030,004
Cu0,0250,0070,004
Cr0,0370,0010,005
Zn0,0380,0010,001
Fe2+0,0400,0010,001
Mn0,6570,0040,005
Mg,877 0,0100,011
Ca0,3560,0140,005
The ratio of CNiimpurities6,7:1517:1461:1

The method of extraction of Nickel from solutions and cleaning impurities: Cr3+, Fe3+, Al3+, Cu2+, Zn2+With2+, Fe2+, Mn2+, CA2+, Mg2+and other elements, including bringing the pH of the solution to values of 4.0 to 6.5, the sorption of Nickel at pH 4.0 to 6.5 from solutions or slurries in weak acid cation exchangers, the desorption of Nickel from a saturated cation exchange resin with a solution of sulfuric or hydrochloric acid to obtain a solution decorate Nickel, characterized in that before desorption saturated cation exchange resin is treated with a solution of Nickel, free from impurities, including part of the solution decorate with Nickel concentration greater than the concentration in the original solution or slurry entering the sorption at pH values less than pH of the solution or slurry in the process of sorption.



 

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1 ex

FIELD: metallurgy.

SUBSTANCE: procedure for purification of zinc sulphate solution from impurities consists in hydrolytic purification with preliminary iron oxidisation in two stages: first with diluted solution of hydrogen peroxide at temperature 20-55°C and consumption 0.95-1.1 of stoichiometric required amount, then with manganese dioxide contained in electrolytic slime of zinc production.

EFFECT: complete or partial avoiding expenditures for costly oxidant - manganese ore and reduced contents of foreign impurities in zinc sulphate solution.

2 ex

FIELD: metallurgy.

SUBSTANCE: invention relates to metallurgy of noble metals, in particular, to method of processing nitration hydroxides in refinery of platinum metals containing chalcogenides, tin, arsenium and platinum group metals, gold and silver. Proposed method comprises leaching of hydroxides and extracting basic metal compounds from the solution. Hydroxide leaching is carried out for 1-2 h by alkali solution with concentration of 140-180 g/l with l:S ratio varying from 3:1 to 4:1, temperature 80-90°C, and introducing hydrazine hydrate into pulp to reach OVP of minus 400-600 mV relative to reference silver-chloride electrode. Then, alkaline solution is separated from insoluble residue that concentrates platinum metals. Now, extraction of basic metals is carried out in processing alkaline solution by sulfuric acid to pH=4-5 to produce hydroxide precipitate of tin, arsenium, selenium and tellurium, and by filtration, or processing of alkaline solution by sulfuric acid to pH 0.5-1.0 along with adding iron powder to OVP varying from 0 to minus 100 mV, and filtration of obtained cementates obtained on the basis of selenium and tellurium, and processing the solution by alkali to pH = 4-5 with deposition of tin and arsenium hydroxides. Invention allows extracting up to 85% of Se and Te into target products, 90% of Sn and As into secondary hydroxides at minimum transition (less than 1%) into PMH.

EFFECT: over 99% of platinum metals left in refinery cycle, reduced processing cycle.

4 tbl

FIELD: metallurgy.

SUBSTANCE: procedure consists in concentrating refractory ore with successive concentrate fine crumbling to release gold with extracting solution and in mixing fine crumbled concentrate with wastes or by-products of concentrating to facilitate filtering said concentrate mixed with said wastes of concentrating. Here is also disclosed the installation for implementation of the said procedure.

EFFECT: increased rate of processing of refractory mineral ore avoiding harmful effect to environment.

14 cl, 4 dwg, 1 ex

FIELD: chemistry.

SUBSTANCE: electrosorption carbon material is the cathode and is carbon fibric on which there is a layer a conducting polymer - poly-3,4-ethylenedioxythiophene or polyaniline which can chemically reduce ions of noble metals Ag, Au and Pd to metal state. Before passing the aqueous solution to the electrosorption carbon material, a negative potential between -0.5 and -0.3 V is applied relative a silver chloride electrode. Reduction takes place upon contact of the electrosorption carbon material with the aqueous solution in flow mode while feeding the solution at a rate of 10-20 ml per minute per square centimetre of the electrosorption carbon material. Concentration of the extracted metal in the solution is measured and the reduction process is repeated many times.

EFFECT: invention increases efficiency of extracting noble metals, shortens duration of the process of their separation and simplifies and lowers the cost of the extraction process.

4 cl, 3 ex, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to chemical engineering of inorganic substances and can be used in cases when there is need to produce a nickel concentrate. The method of processing oxidised nickel ore involves mixing the ore with ammonium chloride, heating the obtained mixture and water leaching to obtain a solution. The ammonium chloride is mixed with the material in ratio of 100-150 mol % of the stoichiometric quantity. The mixture is then heated to temperature 200-315°C and kept at that temperature until release of ammonia, water and hydrogen chloride stops. After water leaching, ammonia water is used to precipitate iron and aluminium at pH 6, nickel and cobalt at pH 8-8.5 and manganese, magnesium and calcium at pH above 8.5.

EFFECT: design of industrial processing oxidised nickel ore to obtain a nicke-cobalt concentrate.

1 dwg, 2 ex

FIELD: technological processes.

SUBSTANCE: invention is related to production of highly pure tungsten for spattering targets. Method includes cleaning of ammonium paratungstate from admixtures by ammonia sulfide and further treatment of solution anion-exchange resin AM-p. Then thermal decomposition of ammonium paratungstate is executed at the temperature of 600-800°C to produce tungsten trioxide, as well as cleaning of tungsten trioxide by zone sublimation at the temperature of 900-950°C in continuous flow of oxygen. After sublimation, heterogeneous recovery of tungsten trioxide is carried out by hydrogen at the temperature of 700-750°C to produce tungsten powder, as well as tungsten powder pressing to produce bar. Then electronic vacuum zone recrystallisation of bar is carried out to produce crystals of highly pure tungsten, as well as electronic vacuum melting in flat crystalliser with melting of flat bar from each side to the whole depth at least twice. Device is also suggested for zonal sublimation of tungsten trioxide.

EFFECT: sharp increase in purity of tungsten intended for thin-film metallisation by magnetron spattering of targets.

2 cl, 2 dwg, 1 ex

FIELD: technological processes.

SUBSTANCE: invention is related to production of highly pure molybdenum for spattering targets. Method includes cleaning of ammonium paramolybdate in the form of solution from admixtures with ion exchange in neutral and alkalescent mediums on hydrated tin oxide and on weakly-basic anion-exchange resin AN-106. Then thermal decomposition of ammonium paramolybdate is executed at the temperature of 600-800°C to produce molybdenum oxide, as well as cleaning of molybdenum oxide by zone sublimation at the temperature of 750-800°C in continuous flow of oxygen. After cleaning, heterogeneous recovery of molybdenum oxide is carried out by hydrogen at the temperature of 700-750°C to produce molybdenum powder, as well as its pressing to produce bar. Then electronic vacuum zone recrystallisation of pressed bars is carried out to produce crystals of highly pure molybdenum, as well as electronic vacuum melting in flat crystalliser with melting of flat bars of highly pure molybdenum from each side to the whole depth at least twice. Device is also suggested for cleaning of molybdenum oxide by zonal sublimation.

EFFECT: sharp increase in purity of molybdenum intended for thin-film metallisation by magnetron spattering of targets, since purity of molybdenum to a large degree defines electrophysical parametres of applied thin layers.

2 cl, 2 dwg, 1 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of reclaiming cyanide from aqueous solutions, particularly recycled water which contains thiocyanates CNS-. The method involves electrochemical oxidation of thiocyanates. Before electrochemical oxidation, recycled water, which contains from 2 to 20 g/l thiocyanates, is acidified to pH=2-3. Electrochemical oxidation is carried out at current density of not less than 750 A/m2 for 2 to 3 hours while simultaneously letting in air into the solution. The formed hydrogen cyanide is trapped in an absorption vessel with its output ranging from 70 to 80%.

EFFECT: reduced content of thiocyanates in recycled water with simultaneous reclamation of cyanide.

3 dwg, 1 ex

FIELD: metallurgy.

SUBSTANCE: procedure consists in leaching with solution of sulphuric acid and in receiving productive solution. Productive solutions are received by heap or underground leaching with solution of sulphuric acid. During process periods of ore leaching and concentration are alternated, while concentration of sulphuric acid in leaching solution is maintained under a differential mode with change of higher concentration of 50-250 g/l in a period of ore leaching to a lowered one - 1-10 g/l in periods of mode of ore buddling. Further, impurities of iron, aluminium, magnesium and silicon are removed from productive solutions; nickel is extracted into concentrate and re-circulated solutions are returned to leaching after strengthening with sulphuric acids.

EFFECT: reduced specific consumption of sulphuric acid for specified extraction of nickel.

3 cl, 2 tbl, 6 ex

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