Method of extraction of rare-earth elements from technological and productive solutions

FIELD: metallurgy.

SUBSTANCE: method for extracting rare-earth elements from the technological and productive solutions containing iron (III) and aluminium, with a pH-0.5÷2.5, includes the sorption of rare-earth elements with strong-acid cation resin. As the strong-acid cation resin the microporous strong-acid cation resin is used based on hypercrosslinked polystyrene having a size of micropores 1-2 nm.

EFFECT: higher efficiency of the process due to greater sorption capacity of the said strong-acid cation resin, high kinetics of sorption and selectivity, improvement of the subsequent quality of eluates and simplification of the process of their further processing.

5 tbl, 5 ex

 

The invention relates to hydrometallurgy rare metals, in particular to the extraction of rare earth elements (REE) by integrated processing of technological and productive solutions, and can be used in the technology of production of concentrates REE.

In connection with the recovery of rare earth industry in Russia is an actual task associated extraction of rare earth elements (REE) in ferrous, non-ferrous and rare metal industry, as well as involvement in the processing of non-traditional raw materials. The characteristics of the data sources are typically low content of REE and complex chemical composition. In this regard, many waste industry technology concentration and extraction of REE are useless and unproductive. In addition, the choice of method of REE extraction is often associated with the impossibility of changing the chemical composition of process intermediates in closed technologies.

Sorption extraction of REE seems to be the most appropriate at the stage of initial concentration. A serious problem with sorption recovery of REE from the technological and productive solutions with pH 0,5÷2,5 is the presence of large amounts of iron(III) and Al, because it is known that such an environment is non-selective for the separation of iron(III) and Al (for the most interfering impurities) from REE, as at the stage of sorption, and at the stage of desorption [Bolshakov K.A. Chemistry and technology of rare and scattered elements. Part 2 - M.: Higher school. 1976. - 360 C.]. In practice, the task of extracting REE of these solutions solved by hydrolytic precipitation of iron(III) and Al alkaline agents [Mursalimova M., Stroeva EV Determination of equilibrium parameters of ion sorption of yttrium and lanthanum of mineralized solutions and iron-containing slurries on carboxylic cation exchanger KB-4 gel type. // Vestnik OSU, No. 5, 2006, pp.86-90]. The disadvantages of this method include large losses REE (20÷25%) due to co-precipitation with hydroxides of iron(III) and Al, the use of strong solutions of precipitators, large consumption, education trudnoobrabatyvaemyh wastewater.

Another way is advance recovery solution with a pH of 0.5÷2.5 the most disturbing impurities of iron(III) to iron(II) iron shavings, urea, sodium sulfite, etc., When such an organization process, the selection of sorption systems with significant coefficients of the separation of iron(II) and REE is much wider [A.S. 2070595. The method of extraction of cerium / Shevchuk Ivan Alekseevich, Simon Tamara Nikolaevna, Rockoon Antonina Nikolaevna // Publ. 20.12.1996]. The disadvantage of this method is the change of the chemical composition of process solutions with a high consumption of reagents-restore is she.

At the same time, in many industries, the maintenance of high concentrations of dissolved iron(III) is dictated by technological necessity, because its presence promotes leaching (oxidizing) the ability of the solutions [Eaatem. Physico-chemical Geotechnology exploration for uranium and gold in the Kyzylkum region. - M.: Moscow state mining University. 1999. - 331 S.]. Therefore, development of a method for the selective extraction of REE from solutions with pH 0.5÷2.5, containing iron(III) and Al without changing the chemical composition of the solutions, is an extremely important task.

The known method [Smirnov DI, Molchanov T.V., Divers LI, Peganov, VA Sorption extraction of rare earth elements, yttrium and aluminium from red mud. // Non-ferrous metals. - 2002. No. 8. - P.64-69], in which the recovery of REE from the technological solution of pH 0.5÷2.5 is carried out by adsorption on the gel sulfonic cation exchanger KU-2. Obtained after deposition of rough concentrate contains, %: REE - 1; iron - 2,0-2,2; aluminum - 15-18; water - 82. This is followed by a stage with resultant deposition rates in order to bring the draft of REM concentrate to commercial products 30-40%.

The main disadvantages of this method are the low sorption capacity of the cation by the sum of the REE, and hence the complex subsequent operation of bringing the draft REE concentrate to commodity productivety disadvantages lead to the need for additional equipment reactors for dissolution of hydrates, filters for filtering a large number of intermediates, as well as to additional consumption rather expensive reagent alkali leaching of aluminum. In addition, the degree of REE extraction this method is sufficiently low output is 60%.

The closest in technical essence and the achieved result is a method (prototype) of REE extraction in the presence of iron(III) and Al from solutions with pH 0.5÷2.5, which for REE extraction uses sulfonic cation macroporous structure with the content of divinylbenzene from 8 to 12% [Ehitajate, Antoniow. Inch. 1963, 8, №9, 2189]. Such sulfonic cation is obtained by copolymerization of monomers (styrene and divinylbenzene in the presence of inert additives, and then removed from the structure of the polymer. However, a significant drawback sulfonic cation macroporous structures are relatively low magnitude of their sorption capacity due to the fact that the process of copolymerization with divinylbenzene not always ensures a uniform distribution of cross-linking in a polymer mesh. This leads to the formation of cavities in the volume of the macroporous sulfonic cation, is not available for sorbed ions, and hence to a decrease of the sorption capacity.

In addition, swollen in water macroporous and largely the spruce the sulfonic cation change in volume upon contact with concentrated solutions of electrolytes. The volume change layer sulfonic cation exchanger reduces the efficiency of the separation process and shortens the life of the sulfonic cation exchanger.

Satisfying the above requirements are microporous sulfonic cation-based supersewn polystyrene. The process of forming supersewn polystyrene grid is fundamentally different from the synthesis of traditional copolymers of styrene and divinylbenzene. Supersewn polystyrene receive not the copolymerization of styrene and divinylbenzene, as by stitching dissolved or highly swollen chains of polystyrene large number of hard-bridges-struts. This leads to the fact that all supersewn the polystyrene virtually disappear small cavity characteristic of the gel porous copolymer of styrene with a radius of 0.1÷0.5 nm, and appear larger cavity having a size distribution of 1÷2 nm micropores. The result is a porous structure with a very large inner surface of more than 1000 m2/, the Size of the macropores in the macroporous sulfonic cation varies from 50 to 1000 nm, depending on the content of divinylbenzene.

The size of the micropores is commensurate with the size of hydrated ions simple mineral electrolytes, which makes the main effect in the separation process, reducing the ability more hydrated (and thus having greatly the th size) ion iron(III) and Al in solutions with pH 0.5÷2.5, because of the sieve effect, to penetrate into the volume of the microporous sulfonic cation exchanger to its functional groups.

A characteristic feature of the microporous sulfonic cation exchanger based on supersewn polystyrene is that it does not change in volume when water is replaced by concentrated solutions of electrolytes due to the fact that the three-dimensional grid supersewn polystyrene has a very rigid frame.

The present invention is to create a more efficient sorption method for REE extraction from solutions of pH 0.5÷2.5, containing iron(III) and Al.

This object is achieved according to the method which consists in sorption extraction sums REE microporous sulfonic cation exchanger based on supersewn polystyrene.

Example 1

Sorption was carried out in static conditions of HCl, H2SO4, HNO3(pH 0.5; 1; 1.5; 2; 2.5), containing 1000 mg/DM3Rare earth elements (lanthanum). Weighed samples sulfonic cation (0.5 g) was contacted with stirring with 50 cm3the above solution for 5 days. The solutions were analyzed by atomic emission method with inductively coupled plasma. Sobiraemosti and the degree of extraction was determined as the difference of the initial and final concentrations of ions in solution.

From table 1 it follows, is the microporous sulfonation extracts lanthanum effectively, both gel and macroporous sulfonic cation, selected from solutions of pH range.

Example 2

Sorption was carried out in static conditions of the sulfuric acid solution (pH 1.5)containing 1000 mg/DM3Rare earth elements (lanthanum). Weighed samples sulfonic cation (0.5 g) was contacted with stirring with 50 cm3the above solution for 0.2; 1; 2; 4; 8 hours. The solutions were analyzed by atomic emission method with inductively coupled plasma. Sobiraemosti and the degree of extraction was determined as the difference of the initial and final concentrations of ions in solution.

Table 2
The ion exchanger% the capacity of the maximum
0.5 hours1 hour2 hours4 hours8 hours
Gel sulfonation1840506680
Macroporous sulfonation457091 95100
Microporous sulfonation71939698100

From table 2 it follows that the kinetics of extraction of lanthanum microporous sulfonic cation exchanger is much higher than the sorption kinetics of lanthanum on the gel and macroporous sulfonic cation selected from solutions of pH range.

Example 3

Sorption was carried out in static conditions of the sulfuric acid solution (pH 1.5)containing 1000 mg/DM3Rare earth elements (lanthanum). Weighed samples sulfonic cation (0.5 g) was contacted with stirring with 50 cm3the above solution at a temperature of 20; 40; 60; 80°C for 3 hours. The solutions were analyzed by atomic emission method with inductively coupled plasma. Sobiraemosti and the degree of extraction was determined as the difference of the initial and final concentrations of ions in solution.

Table 3
The ion exchangerThe degree of extraction, %
20°C40°C60°C80°C
Gel sulfonation55576063
Macroporous sulfonation92939495
Microporous sulfonation9798100100

From table 3 it follows that the temperature of the sorption of lanthanum sulfonic cation has no significant impact on the degree of extraction from acidic solutions.

Example 4

Sorption was carried out in static conditions of the sulfuric acid solution (pH 0.5; 1; 1.5; 2; 2.5)containing 50 mg/DM3lanthanum, 1000 mg/DM3iron(III) and 1000 mg/DM3aluminum. Weighed samples sulfonic cation (0.5 g) was contacted with stirring with 50 cm3the above solution at a temperature of 20°C for 5 days. The solutions were analyzed by atomic emission method with inductively coupled plasma. Sobiraemosti and the degree of extraction was determined as the difference of the initial and final concentrations of ions in solution.

From table 4 it follows that microprecipitation has a significantly greater capacity for rare earth elements (lanthanum) in the presence of 20-fold excess of iron(III) and Al and a lower capacity for these elements in comparison with gel and macroporous sulfonic cation during sorption from solutions of the selected pH range.

Example 5

Sorption was carried out in static conditions from sulfuric acid solutions (pH 1.5)containing 50 mg/DM3lanthanum, or containing 50 mg/DM3cerium, or containing 50 mg/DM3dysprosium, or containing 50 mg/DM3lutetium, or containing 50 mg/DM3the sum of the REE. Weighed samples sulfonic cation (0.5 g) was contacted with stirring with 50 cm3the above solution at a temperature of 20°C for 5 days. The solutions were analyzed by atomic emission method with inductively coupled plasma. Sobiraemosti and the degree of extraction was determined as the difference of the initial and final concentrations of ions in solution.

Table 5
The ion exchangerThe degree of extraction, %
LaCEDyLuΣ
Microporous cation5557555756

Thus, the technical result of the proposed method is zlecenia REE from solutions with pH 0.5÷2.5 is determined by the high efficiency of this method due to the greater sorption capacity of microporous sulfonic cation exchanger by REE in the presence of iron(III) and aluminium, high sorption kinetics and selectivity, which leads to the subsequent improvement of the quality of the eluates and facilitate their further processing.

The method for extracting rare earth elements from the technological and productive solutions containing iron (III) and aluminium, with a pH 0,5÷2,5, including sorption of rare earth elements sulfonic cation exchanger, characterized in that as a sulfonic cation exchanger using microporous sulfonation based supersewn polystyrene, having a size of micropores of 1-2 nm.



 

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