Method of processing chemical concentrate of natural uranium

FIELD: chemistry.

SUBSTANCE: method involves leaching in order to dissolve uranium when the concentrate reacts with nitric acid solution to obtain pulp from the concentrate. Uranium is then extracted from the pulp using tributyl phosphate in a hydrocarbon solvent. The extract is washed and uranium is re-extracted. Extraction is carried out from freshly prepared pulp which is obtained through direct-flow reaction at temperature 20-65C of a stream of a suspension of the concentrate in water which is prepared beforehand and a stream of nitric acid solution with flow rate ratio which ensures nitric acid concentration in the pulp of 25-120 g/l. The period from the beginning of leaching to the beginning of extraction is not more than 10 minutes.

EFFECT: protection of extraction from formation of non-demixing emulsions, providing given purity of uranium from ballast impurities and obtaining raffinates which can be removed into underground collector sand layers.

2 tbl, 1 ex

 

The invention relates to methods for processing chemical concentrates, natural uranium (NUC) and can be used in the technology of extraction processing NUC with a high silicon content, with the aim of obtaining nuclear-friendly materials, suitable for the production of uranium hexafluoride for enrichment.

Known methods of processing NUC, in which the uranium is leached with solutions of nitric acid, and extraction of uranium tributyl phosphate in a hydrocarbon diluent direct the slurry containing the insoluble residue of hydrated oxides of iron and other impurities in the uranyl nitrate solution. The extraction of the pulp is carried out, for example, by the method (Cherrington, Arule. Production technology of uranium. - M.: gosatomizdat, 1961, s-162 [1]) or by method (Cherrington, Arule. Production technology of uranium. - M.: gosatomizdat, 1961, s-182 [2]).

Positive extraction of the pulp is the elimination of time-consuming separation of the suspension (solid and liquid phases) in order to obtain a solution of uranyl nitrate.

When processing NUC with a high content of silicon slurry contains, apart from the undissolved residue concentrate (mostly in the form of hydrated compounds of iron and some other metals), silicic acid, prone to polymerization and forming gels. The disadvantage of e is straccia from the pulp, containing and insoluble residues and silicon as silicic acid, is the fact that the particles of insoluble residues concentrate, especially in the presence of gels of silicic acid, contribute to the stabilization of emulsions, which are formed by the interaction of the extractant with uranyl nitrate solution, it leads to the termination of the separation of emulsions, the formation of so-called jellyfish, violation of the extraction process.

This disadvantage is inherent in both the above ways. In addition, get a refined, containing gels of silicic acid, which makes it impossible for them underground burial in sand reservoirs due to low speed filtering and caused by this circumstance clogging of the reservoir.

In both methods the extraction of direct pulp obtained by a few hours of interaction between acid and concentrate.

In the method [1] leaching NUC spend 60%nitric acid for 3 hours at a temperature of 82C, the result is a pulp with a uranium content of 20010 g/l of nitric acid 3,00,2 mol/l, which is sent on the extraction.

In the method [2] in the processing of NUC with a high content of silicon leaching spend 40%nitric acid at a temperature 93-104C for 4 hours. In the finished pulp uranium contains 350-450 g/l, free nitrogen is Oh acid 0.8 to 1.8 mol/L. The slurry is directed to the extraction of 30%tributyl phosphate in an organic diluent. The method chosen for the prototype.

Object of the invention is the processing of slurries NUC with a high content of silicon without forming nerasseivayushchee aqueous-organic emulsion on the extraction of uranium with obtaining refined, which may be buried in the underground sand reservoirs, providing a required degree of purification of uranium from impurities.

The set task is solved by the fact that in the method of chemical processing of natural uranium concentrate with a high content of silicon, including the dissolution of uranium leaching by the interaction of concentrate with a solution of nitric acid to obtain pulp from concentrate, extraction of uranium from the pulp by tributyl phosphate in a hydrocarbon diluent, washing of the extract and reextraction uranium extraction is carried out on freshly prepared slurry, which is obtained flow interaction at a temperature of 2065C pre-cooked flow of a suspension concentrate in the water and flow solution of nitric acid at a ratio of expenditure flows, providing the concentration of nitric acid in the pulp 25120 g/l, at the same time from the beginning of the leaching prior to the extraction does not exceed 10 minutes.

The essence of the method consists in the extraction to produce and the fresh pulp, that is, a slurry, after which obtain, without delay, send to the extractor.

The method is as follows.

Way processed silicon-containing concentrates, natural uranium, including the ammoniyuraniltrikarbonata, uranium peroxide, octoxyglycerin, uranium trioxide.

Processed NUC "yellowcake". Yellowcake is a salt - ammoniyuraniltrikarbonata. Yellowcake contains 3642 wt.% U and other elements such as silicon, iron and aluminum. The content in the "yellow cake" ballast impurities is:

(wt.%): Si (0,470,71); SiO2- (1,01,52); Fe - (0,581,0); Al - (0,541,0);

(wt.% to U): Si - (1,31,7); SiO2- (2,83,6); Fe - (1,62,4); Al - (1,52,4).

Example.

In the experiments of series 1, 2 and 3 refined yellowcake, containing, wt.%: U - 40,0; Si - 0,60; Fe - 0,79; Al - 0,70. In terms of wt.% to U: Si - 1,49; Fe - 1,98; Al - 1,74.

In the experiments of series 1 and 2 first preparing a suspension of "yellow cake" in the water, this powdered concentrate was mixed with a given quantity of water at a ratio of T:W mass of concentrate to water volume (t/m3) 1:(0,540,60). Translation of "yellow cake" in aqueous suspension significantly accelerates the subsequent dissolution of the concentrate in acid.

Then the flow of the suspension was introduced into an interaction with a flow of 40%aqueous solution of nitric acid (7.9 mol/l) by filing a thread in thermostatic when the ass is authorized temperature (between 2065C) flow reactor. The ratio of expenditure flows were selected so that after the dissolution of uranium residual concentration of nitric acid in the pulp at the outlet of the reactor (or, equivalently, at the entrance to the extractor) would be equal to 25120 g/l, and the concentration of uranyl nitrate in the pulp in terms of uranium would be equal to 200300 g/l Pulp contained insoluble residues of hydrated metal compounds. The duration of the dissolution of uranium at 65C does not exceed 5 minutes at 20C - 10 minutes (about the end of the dissolution of uranium testified cessation of gassing).

From once-through reactor, the flow of the reaction mixture in the form of a freshly prepared slurry was moving in the extractor first stage of extraction. From the beginning of the leaching prior to the extraction took place no more than 10 minutes.

In the experiments of series 3 "yellow cake" (not a suspension, and in solid powdered form, as in the prototype) was mixed with a solution of nitric acid. Leaching with getting uranyl nitrate solution and an insoluble residue was carried out at a temperature of 65C, it was completed in 15-20 minutes. The pulp through 3 hours after the start of the leaching of the concentrate was applied for extraction. The extraction was performed on the same stage and under the same conditions as in the experiments of series 1 and 2.

Table 1 shows the conditions of the dissolution of "yellow cake" and the compositions of the slurries obtained in the experiments of series 1-3.

In all the experiments of series 1-3 extraction cascade consisted of four blocks of mixer-settlers: extraction (5 steps), flushing (2 steps), Stripping (6 steps) regeneration and recycling of the extractant (2 steps). Extraction of uranium spent 30%tributyl phosphate in a hydrocarbon diluent. When this extract was supported by [U]=100105 g/l, were refined with [U] < 0.1 g/L. Then carried out reextraction uranium.

In the process of extraction processing was monitored by accumulation of interfacial structures on the boundary of phases in the extraction unit and analyzed the content of impurities in the reextractors uranium.

In the experiments of series 1 and 2 on the phase boundaries in settling chambers mixer-settlers accumulation of interfacial structures ("jellyfish") occurred. The extract was transparent with no visible traces of sediment. Particles of insoluble residues, while in the aqueous phase, already in the first extraction stage was enlarged, as it occurs in the presence of a coagulant, and followed with the aqueous phase.

In addition, it was not observed the formation of gels of silicic acid in the aqueous phase at all levels of extraction; filtration rate clarified by sedimentation refined (separation from insoluble residues held by decantation) through the layer of sand filter is not changed within one month from the moment of the receipt and was comparable to the rate of water filtration. This makes it possible underground burial clarified refined in sand reservoirs.

In the experiments of series 3 on the phase boundaries in settling chambers mixer-settlers extraction unit immediately after the filing of pulp extraction began the accumulation of interfacial structures ("jellyfish"), which led after a tenfold exchange solutions in the extraction unit to the termination of the separation of emulsions and stop the cascade. The extract obtained to stop the cascade, was muddy with traces of sediment.

The gel of silicic acid contained in the raffinate, after clarification of the raffinate by sedimentation followed by decantation, scored a sand filter, which made it impossible for underground disposal of raffinate.

Table 1 shows the following. In experiments 1.1, 1.2, 2.1, 2.2 silicon content in the water phase of the slurries used for extraction corresponds to the percentage of silicon to Uranus in NUC, equal 1,49%. In experiments 2.32.5 silicon content in the aqueous phase of the pulp is reduced compared with the percentage of silicon to Uranus, equal 1,49% in NUC, with reduction of the nitric acid and the residual concentration of nitric acid in the pulp. This is followed, as shown by the analysis of rainfall, isolated from refined, the advent of silicon precipitation in the experiments 2.32.5. The volume of settled sediments in the refined increased ,about 2 % in experiment 2.3 [HNO 3] in the pulp and 47.0 g/l to 11.3% vol. in the experience of 2.5 [HNO3] in the pulp of 25.1 g/l Revealed a pattern of increasing amounts of solid waste, and lower consumption of nitric acid - allows you to choose the economically optimal consumption expensive nitric acid (subject to the proposed interval residual nitric acid in the pulp supplied to the extraction) and the number of the obtained solid waste disposed.

Thus, the process of extraction from the fresh pulp does not prevent any undissolved residues or silicon; this allows to carry out time-consuming operation separation of solid and liquid phases.

The reextractors uranium in the experiments of series 1 and 2 had the same composition, in experiments 3 series reextractors differed in the content of certain impurities. The content of impurities in the reextractors are shown in table 2.

As can be seen from table 2, the inventive method (experiments series 1 and 2) provides the necessary cleanup of uranium from impurities, namely as one stripped off reextractors meet the requirements of technical conditions With ASTM 788-03 on a solution or crystals of uranyl nitrate nuclear purity. In experiments 3 received reextract the uranium content of impurities in excess of normalized values set With ASTM 788-03 (exceeding the amount of trace elements that do not form volatile fluorides, and rumney).

Thus, the inventive method allows the extraction of the pulp obtained from concentrates with a high content of silicon, without the inherent extraction from such slurries disadvantages, i.e. to protect the extraction from education nerasseivayushchee emulsions, to provide the specified clearance of uranium from impurities and to obtain a refined, which can be removed in an underground sand reservoirs.

The method of chemical processing of natural uranium concentrate with a high content of silicon, including leaching to dissolve the uranium in the interaction of the concentrate with a solution of nitric acid to obtain pulp from concentrate, extraction of uranium from the pulp by tributyl phosphate in a hydrocarbon diluent, washing of the extract and reextraction uranium, characterized in that the extraction is carried out on freshly prepared slurry, which is obtained flow interaction at a temperature of 2065C pre-cooked flow of a suspension concentrate in the water and flow solution of nitric acid at a ratio of expenditure flows, providing the concentration of nitric acid in the pulp 25-120 g/l, while from the beginning of the leaching to the beginning of extraction does not exceed 10 minutes



 

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