The method of extraction and preconcentration of thorium from technological solutions

 

The invention relates to hydrometallurgy and can be used for selective extraction of thorium from solutions containing other metals. The technical result is achieved by the use of the invention is to increase the degree of extraction of thorium from scandium-containing solutions, increase the degree of purification of scandium from thorium and reducing the deadweight loss of scandium with thorium is radioactive residues form and precipitation. The method of extraction and preconcentration of thorium from technological solutions includes sorption of thorium at pH 2.8 to 3.5 and a temperature of 60-95oWith porous sulfacetamide with subsequent washing of the cation and desorption of thorium carbonate-bearing solution. In the initial solution before adsorption pre-injected magnesium chloride in the amount of 10-100 mgEQ Mg2+1 mgEQ ions Th4+in the original solution, washing the cation exchange resin after sorption, first with water, then the solution of MgCl2with a concentration of 50-150 g/DM3the filtrate after sorption unite with Promode, the combined solution successively enter first the potassium Iodate, then barium chloride and sodium sulfate, the slurry is filtered, radioactive iodata and trace metals. Thorium the eluate is treated with mineral acid, for example hcl, to a pH of 0.5 to 2.0, heated to 80-100oC, maintained at an elevated temperature for 0.5-2 h, the injected alkaline reagent, for example a solution of sodium hydroxide and/or ammonia to a pH of 5-8, formed pulp defend and filtered, the precipitate of hydroxide and gidroksicarbonata thorium is separated from the mother liquor, together with a radioactive Iodate-sulfate cecom and sent for recycling or disposed of in store special waste (HSO). In addition, magnesium chloride is introduced into the initial solution in an amount to provide its content in the solution before adsorption of 50-150 g/DM3. For the introduction of the original solution of magnesium chloride use natural and/or synthetic bischofite, and/or carnallite, and/or products and/or waste from processing of carnallite raw materials, selected from the range: carnallite dust first stage of dehydration of carnallite, sludge carnallite chlorinators. In addition, KIO3impose a solution with a concentration of 10-50 g/DM3in the amount of 10-100 cm31 DM3solution. It is advisable l2and Na2SO4enter in the form of solutions with a concentration of 50-150 g/DM3in the amount of 1.2 to 1.5 mol to hydrometallurgy and can be used for selective extraction of thorium from solutions containing other metals. The invention can be used, in particular, the technology for production of scandium oxide from various raw materials for selective extraction and preconcentration of thorium from scandium-containing solutions.

The method for extracting thorium from solutions, such as the sorption of thorium ions from chloride-hydrochloric acid solutions followed by desorption of thorium (see the Extract thorium from waste chlorination process loparite concentrates//radiochemistry, 1986, 4. C. 486-489). The disadvantage of this method is the lack of selectivity of the process for extracting thorium from solutions containing scandium: in this case, simultaneously with the adsorbed thorium also scandium. This disadvantage have other known methods of extraction of thorium (and.with. 1420972 USSR publ. BIPM 19, 2000, S. 602; and.with. 1485606 USSR publ. BAPM 2, 2000, S. 593), lies in the sorption of thorium from solutions aminoheterocycles the ampholytes.

Known analogues closest to the proposed invention as intended, the totality of symptoms and the achieved result is a well-known method for extracting thorium from solutions containing scandium (and.with. 703929 the USSR with the priority. from 05.10.1977. Publ. B 41, 1983. S. 256; see also: news In the prototype is the following: the original solution, containing thorium and scandium with a pH of 2.8 to 3.5 is passed through the sorption column with porous sulfonic cation exchanger in the Na form; sorption is carried out at 60-90oWith the emergence of" thorium in the filtrate, after which the cation exchange resin in the column was washed with 2-3 volumes of water, NaCl solution (desorption scandium) and then carry out desorption of thorium 1-3 N. a solution of Na2CO3. Compared to other previously known methods, the method according to the prototype allows to selectively extract thorium from scandium-containing solutions. The disadvantage of this method is unsatisfactory separation of scandium and thorium, and relatively low dynamic exchange capacity of thorium - i.e. the capacity to "overshoot" of thorium in the filtrate.

The claimed invention is directed to solution of the problem consisting in increasing the efficiency of the process by increasing the degree of separation of scandium and thorium; improving the performance of the process by increasing THE on thorium.

Technical result achieved in this case, is to increase the degree of extraction of thorium from scandium-containing solutions, increase the degree of purification of scandium from thorium and reducing the deadweight loss of scandium with thorium is radioactive residues form and precipitation. Inch the dynamic capacity for thorium and increased sorption load thorium, i.e. the increase in productivity, reduction of losses of scandium with thorium radioactive precipitation.

The technical result is achieved in that in the method of extraction of thorium from technological solutions, including sorption of thorium at pH 2.8 to 3.5 and a temperature of 60-95oWith porous sulfonic cation exchanger with subsequent washing of the cation and desorption of thorium carbonate-bearing solutions, what's new is that in the original solution before adsorption pre-injected magnesium chloride in the amount of Mg2+mEq per 1 mEq ions Th4+in the original solution, the cation exchanger after sorption washed first with water, then the solution of MgCl2with a concentration of 50-150 g/DM3prambody combined with the filtrate after sorption sequentially injected solution (10-50 g/DM3) of potassium Iodate in the amount of 10-100 cm31 DM3the solution then is injected solutions (50-150 g/DM3) barium chloride and sodium sulfate in the amount of 1.2 to 1.5 mol of Na2SO41 mol l2radioactive Iodate-sulfate cake is separated from the decontaminated solution, which is directed to the recovery and recycling of rare and trace metals (Sc), thorium the eluate is treated with mineral acid, now, enter an alkaline reagent, for example a solution of sodium hydroxide and/or ammonia to a pH of 5-8, formed pulp defend and filtered, the precipitate of hydroxide and gidroksicarbonata thorium is separated from the mother liquor, together with a radioactive Iodate-sulfate cecom and sent for disposal in store special waste. In addition, magnesium chloride is introduced into the initial solution in an amount to provide its content in the solution before adsorption. In addition, with the introduction of magnesium chloride in the original solution before adsorption of thorium use natural and/or synthetic bischofite, and/or carnallite, and/or products and/or waste carnallite processing of raw materials, selected from the range: carnallite dust first stage of dehydration of carnallite, sludge carnallite chlorinators.

Under other equal conditions, the proposed method is characterized by new techniques of performing actions and the new order of execution of actions, the use of certain substances, without which it is impossible the implementation of the method, the new modes and parameters of the process, ensures the achievement of the technical result in the implementation of the claimed invention.

Check the patentability of the claimed from the first image.

The analysis of the prior art indicates that in book, journal and patent literature contains no information about selective extraction of thorium from technological solutions containing scandium by sorption from solutions at pH 2.8 to 3.5, in which a sorption pre-enter MgCl2in the amount of 10-100 mg-EQ 1 mEq Th, a washing of the cation exchanger after the sorption of lead solution MgCl2with a concentration of 50-150 g/DM3the filtrate after sorption unite with Promode, the combined solution consistently give CRO3, Na2SO4, l2radioactive Iodate-sulphate precipitate separated from the solution, which is directed to the extraction of rare metals, such as Sc, thorium carbonate eluate is treated with Hcl to a pH of 0.5 to 2.0, heated to 80-100oC, incubated for 0.5-2 hours, injected alkaline reagent to a pH of 5-8, pulp defend, filtered, radioactive precipitate separated from the solution, together with cecom and sent to GSO.

Therefore, the claimed invention meets the condition of "novelty". It should be stressed that the technical result according to the claimed invention is achieved only when all the above conditions and process parameters. what given the dynamic viscosity of the thorium and does not allow to increase the efficiency of the extraction of thorium from solutions containing scandium. In particular, when used for the sorption of thorium phosphate ion (instead of the sulfonic cation) and when all other conditions (pH, temperature, concentration of MgCl2and so on) technical result not only achieved, but generally selective extraction of thorium from scandium-containing solutions is not happening. On the other hand, when introduced into the initial solution of MgCl2in amounts that differ from the optimal (more or less 50-150 g/DM3) the effect of increasing THE on thorium disappears. Important is also the question of the fate of the solutions of thorium eluates. In the known methods there are no technical solutions for recycling and disposal.

Thus, the analysis of the totality of the features of the claimed invention and achieved this result indicates that between them there is a causal relationship, which is expressed in the fact that the implementation process in the above conditions provides problem solving and achievement of the technical result. For violations of the above modes of process, sequence, etc. of the above technical result is not achieved.

If this is derived from published data on the chemistry and technology of thorium and its compounds.

Information supporting the implementation of the present invention to provide the above technical result, and comparing the effectiveness of known (the prototype) and the proposed technical solutions described in the examples.

Example 1.

A comparison of the efficiency of extraction of thorium from solutions of known and proposed methods.

By a known method: through the sorption column with 2 g of porous sulfonic cation exchanger KU-23 in Na-form flow solution with pH 3.0, containing 2.4 g/l scandium and 4.4 g/l thorium to "overshoot" of thorium in the filtrate (DOE"). Sorption is carried out at 80oC. After adsorption cation exchange resin in the column was washed with water and carry out desorption: scandium - 2 N. a solution of sodium chloride; thorium - 3 N. solution of ammonium carbonate.

In the proposed method: in the original solution containing 2.7 g/l scandium and 3.7 g/l thorium, enter 100 g/l of magnesium chloride MgCl2(33 mEq per 1 mEq Th). This solution (pH 3.0) pass at 80oWith through the sorption column with 2 g of macroporous sulfonic cation exchanger before the "breakthrough" of thorium in the filtrate (DOE). After sorption, cation exchange resin in the column was washed with water and carry out desorption: scandium - solution of magnesium chloride (100 g/DM3and, then, thorium - 3 nemy method provides compared to the prototype increasing sorption loading on the cation exchange resin in 1.5 times and, therefore, increasing the productivity of the process by introducing in the original solution of magnesium chloride and increases the volume of solution passing to "overshoot" thorium ions in the filtrate and to increase the sorption capacity of the cation on thorium.

At the same time increases about 3 times the separation of scandium and thorium at the stage of sorption.

Example 2.

In the original chloride solution with pH 3.0, containing 5.0 g/DM3thorium and 4.0 g/DM3scandium has introduced 100 g/DM3MgCl2in an amount to provide the optimal ratio of Mg2+/Th4+equal to 24.4 mEq/mEq. Then this solution was passed at 805oWith heated through sorption column of macroporous sulfonic cation exchanger KU-23 in salt form. Sorption was carried out before "breakthrough" before the advent of thorium in the filtrate. Under these conditions, the thorium was selectively sorbirovtsa a sulfonic cation exchanger, and scandium were superseded in the filtrate. A small amount of scandium, remaining in the intergranular space and phase of the cation - after the "breakthrough" of Th4+were removed by serial washing first with water (2 volume relative to the volume of resin-cation), then the solution of MgCl2with a concentration of 100 g/DMub> in the amount of 30 cm31 DM3then l2and PA2SO4(in the form of a solution with a concentration of 150 g/DM3and Na2SO4(in the amount of 1.3 mol of Na2SO41 mol l2). The resulting slurry was filtered, radioactive sludge containing thorium and daughter products of disintegration (Ra-228, Ra-224), was separated from the mother - deactivated scandium-containing solution, and then the residue was combined with hydrate-hydroxocobalamin the precipitate obtained after processing of thorium of the eluate (150 g/DM3Na2CO3), which was treated with concentrated model HC1 to pH 10,2, was heated to 955oC, kept at this temperature for 1 hour, then treated with a solution of NaOH (100 g/DM3) to a pH of 6.0. Eye-catching sediment oxyhydrates and hydroxocobalamin thorium was separated from the solution by filtration, combined with Iodate sulfate precipitate and buried in the cemetery ("HSA" store special waste).

Example 3.

Spend sorption extraction of thorium from solutions of example 1 (according to the proposed method, but the concentration of magnesium chloride in the conducted experiments is 20, 50, 150, 200 g/DM3. Results op the consequently, and improving the performance of the process) is provided by the introduction to the original solution of magnesium chloride in the amount of 50-150 g MgCl2/DM3.

Thus, the implementation of the developed technical solutions provides high selectivity (selectivity) extract Th of the scandium-containing solutions, allows to improve the performance of the process in 1.5 times.

Claims

1. The method of extraction and preconcentration of thorium from technological solutions, including sorption of thorium at pH 2.8 to 3.5 and a temperature of 60-95oWith porous sulfacetamide with subsequent washing of the cation and desorption of thorium carbonate-bearing solution, characterized in that in the original solution before adsorption pre-injected magnesium chloride in the amount of 10-100 mgEQ Mg2+1 mgEQ ions Th4+in the original solution, washing the cation exchange resin after the sorption of lead first with water, then with a solution of magnesium chloride with a concentration of 50-150 g/DM3the filtrate after sorption unite with Promode, the combined solution successively enter first the potassium Iodate, then barium chloride and sodium sulfate, the slurry is filtered, rage and recycling of rare and scattered metals, thorium the eluate is treated with mineral acid such as hcl, to a pH of 0.5 to 2.0, heated to 80-100oC, maintained at an elevated temperature for 0.5-2 h, the injected alkaline reagent, for example a solution of sodium hydroxide and/or ammonia to a pH of 5-8, formed pulp defend and filtered, the precipitate of hydroxide and gidroksicarbonata thorium is separated from the mother liquor, together with a radioactive Iodate-sulfate cecom and sent for recycling or disposed of in store special waste.

2. The method according to p. 1, characterized in that the magnesium chloride is introduced into the initial solution in an amount to provide its content in the solution before adsorption of 50-150 g/DM3.

3. The method according to p. 1, characterized in that the introduction in the original solution of magnesium chloride use natural and/or synthetic bischofite, and/or carnallite, and/or products and/or waste from processing of carnallite raw materials, selected from the range: carnallite dust first stage of dehydration of carnallite, sludge carnallite chlorinators.

4. The method according to p. 1, characterized in that the potassium Iodate is injected in the form of a solution with a concentration of 10-50 g/DM1in the amount of 10-100 cm31 DM3solution.

5. The method according to p. 1, wherein the 1,5 mol of sodium sulfate per 1 mol of barium chloride.

 

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SUBSTANCE: invention relates to sorption-mediated recovery of molybdenum from solutions containing heavy metal cations. Method of invention comprises providing solution to be treated, sorption of molybdenum(VI) on anionite at pH < 7. Sorption is conducted from solutions with anionites AM-2b and AMP at solution pH below pH of hydrolytic precipitation of heavy metal cations but higher than pH of formation of molybdenum cations (pH ~ 1).

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9 dwg, 3 tbl, 4 ex

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