Procedure for extraction of uranium and molybdenum from carbonate salt uranium-molybdenum water solutions

FIELD: metallurgy.

SUBSTANCE: procedure consists in extracting uranium by means of liquid extraction of organic phase of synergy mixture on base of di(2-ethylhexyl)phosphorous acid containing tributylphosphate (TBP) or tributylphosphate together with trialkylamine (TAA) or heteroradical phosphynoxide of composition of oxide of isoamyldioktylphosphyne in organic thinner. Also, while mixing, there is performed simultaneous gradual neutralisation of mixture of phases with mineral acid till there are established balanced values of pH of water phase in interval 5.6-6.6.

EFFECT: increased efficiency of extraction of uranium and molybdenum from carbonate solutions.

3 dwg, 3 tbl, 3 ex

 

Carbonate uranium-molybdenum-containing solutions are formed when carbonate leaching of uranium-molybdenum ores, concentrates, waste, and when sorption processing carbonate solutions or slurries using highly basic anion exchange resin and subsequent regeneration of carbonate-salt solutions (carbonate, chloride, carbonate, sulfate, etc. solutions).

Direct separation and extraction of uranium and molybdenum from carbonate uranium-molybdenum-containing solutions industrial extractants neutral or acidic organophosphorus compounds (for example, tributyl phosphate and/or di(2-ethylhexyl)phosphoric acid) is not possible, as in carbonate solutions of uranium is in the form of a strong negatively charged complexes (urbanistically-ions), and molybdenum in the form of anionic molybdate ions. This finding is consistent with the statement in the monograph B.V. Gromov, "Introduction to chemical technology of uranium". M: Atomizdat, 1978, s:

"It should be noted disadvantages inherent in the extraction, which include the inability to apply extraction for processing slurries from carbonate solutions".

Extraction processing of carbonate uranium-molybdenum solutions are possible when the deoxidation carbonate solutions, which formed in the acidic environment of proishodit the destruction of urbanistically ions with the formation of positively charged uranyl ion UO 22+and polymer urbilateria ions and molybdate anions become ions molybdenite of Moo22+and other positive ions. Due to the formation of positive ions of uranium (VI) and molybdenum (VI), it becomes possible liquid-liquid extraction of various types of extractants and, in particular, energetyki mixtures of extractants based D2EGFK. But the purification of uranium from molybdenum solvent extraction does not provide.

The description of this method in the open literature not found.

Using carbonate-chloride solution containing 6,24 g/l of uranium and 2,78 g/l of molybdenum, the authors experiment was carried out by deoxidation of this carbonate solution until the excess acidity of 12.4 g/l sulfuric acid. From the resulting uranium-molybdenum solution, extraction was performed with a solution of 0,15M D2EGFK + 0,15M TBP if A:B=1:2. After carrying out the solvent extraction raffinate contained (g/l): uranium 1,66, molybdenum 2,45. The distribution coefficients of uranium and molybdenum respectively 5,51 and 0.27. Thus, uranium and molybdenum are redistributed between the aqueous and organic phases without separation of metals. Taking into account the correlation of the phases of the uranium concentration in the organic phase was 9,16 g/l, molybdenum 0.66 g/L. the impurity Content of molybdenum in relation to the uranium in the organic phase was 0,66/9,16·100%=7,21%. According to Ciampino international airport is popular With ASTM 967 limit the content of molybdenum in uranium chemical concentrate should not exceed 0.3%. That is, after conventional liquid extraction, the content of molybdenum in relation to the uranium it exceeds the allowable content of uranium in 24 times.

A prototype of the proposed method can serve as a method of separating uranium and molybdenum, developed by French researchers for processing uranium-molybdenum ores Tag in Niger (Thiry J., Issa A. Recent process development at the SOMAIRE Uranium Mill. URANIUM 2000. Int. Sym.on the Process Metallurgy of Uranium, str-237). The method is based on the precipitation of uranium of alkali carbonate uranium-molybdenum solution. For the preparation of carbonate uranium-molybdenum solution should 2,4 kg of sodium carbonate/ kg of uranium. The concentration of alkali 150-200 g/l, flow rate on the deposition of uranium 1.2 kg/kg of uranium. The average content of molybdenum in relation to uranium in the sediment is 21%. To reduce the content of molybdenum in uranium concentrate it is treated with alkali and spend it more pereosazhdeniya. It should be noted the high consumption of reagents for carrying out this method.

The technical result of the present invention is to increase the efficiency of separation of uranium and molybdenum from carbonate solutions.

The technical result is achieved by the fact that the separation of uranium and molybdenum from the carbonate salt uranium-molybdenum aqueous solutions is carried out by extraction from a solution of liquid uranium is the extraction of uranium by organic phase sinergetnoy mixture on the basis of di(2-ethylhexyl)phosphoric acid, containing tributyl phosphate (TBP) or tributyl phosphate together with triallylamine (TAA) or phosphine oxide rasoredeleniy composition solidiarity oxide (FMR) in an organic diluent while gradually neutralization phase mixture of mineral acid under stirring to establish equilibrium pH values of the aqueous phase constituting the interval of 5.6 and 6.6.

The authors have established the conditions of extraction separation of uranium and molybdenum in the extraction processing of the uranium-molybdenum-containing solutions, especially at high content of molybdenum in relation to uranium, reaching 50% or more. Developed by the authors, the method is also suitable for extraction separation of uranium and molybdenum at a lower relative content of molybdenum.

A distinctive feature of the proposed method is the combination of solvent extraction with a gradual neutralization of the mineral acid (sulfuric or other), formed by stirring the mixture of phases to establish the equilibrium pH of the aqueous phase. Below are examples of extraction separation of carbonate uranium-molybdenum solutions of the proposed method with a relatively high content of molybdenum.

Example 1. Carbonate-chloride uranium-molybdenum desorbed regeneration of highly basic anion exchange resin contained (g/l): ur the 6,24, molybdenum 2,78, sodium chloride 90, carbonate, and sodium bicarbonate 20. As extractant used sinergetnuyu mixture of 0,15M di(2-ethylhexyl)phosphoric acid (D2EGFK) with 0,15M tributyl phosphate (TBP) in a hydrocarbon diluent. The developed method was carried out under mechanical stirring carbonate uranium-molybdenum solution and the extractant, the above composition, when the volume ratio of the phases Of:1:2. Sequential neutralization stir the mixture was carried out with concentrated sulfuric acid for 5-15 minutes After carrying out the above process and separation of the phases was determined the content of uranium and molybdenum. The results of the experiment are presented in table 1 and figure 1.

6,91
Table 1
The dependence of the distribution of uranium and molybdenum from the equilibrium pH of the aqueous phase during the extraction solution 0,15M D2EGFK 0,15M TBP and the gradual neutralization of carbonate-chloride uranium-molybdenum solution containing 6,24 g/l of uranium and 2,78 g/l of molybdenum at A:B=1:2. The contact time of the phases 10 min
pH equalthe 5.45of 5.896,20to 6.57
The uranium concentration in the raffinate, g/l0,9850,01220,00770,0480,792
Cu uranium10,71021161825713,8
Mo org, mg/l6,06,09,01833

The data in table 1 indicate effective extraction separation of uranium and molybdenum in the range of pH of 5.9 to 6.3. The maximum distribution coefficient of uranium at pH of 6.2 is 1600, and the distribution coefficient of the molybdenum - 0,0032. Thus, there is almost quantitative transition of uranium in the organic phase at this pH value, and the molybdenum remains in the raffinate. If we compare these data with the data of the prototype, in the proposed method, the distribution coefficients of uranium and molybdenum in hundreds of times higher than the distribution coefficients of uranium and cleaning it from molybdenum compared with the prototype of the proposed method.

From the organic phase, the uranium can be extragonadal known way way the processing solution of carbonate-ammonium bicarbonate (15-18%) obtaining crystals of uranyltricarbonate ammonium (AUTKA) with their subsequent annealing after filtration and washing. Using ion-exchange adsorption or solvent extraction of the raffinate can get paramolybdate ammonium.

According to table 1 was constructed by the graph of the logarithm of the distribution coefficient of uranium from the equilibrium pH of the aqueous phase.

Given curve in figure 1 passes through a maximum at pH of 6.20. By extraction separation of uranium and molybdenum the proposed method, the relative content of molybdenum in uranium decreased from 44.5% in the initial solution to 0,072% in the extract given the volume ratio of the phases, i.e. almost 620). The concentration of molybdenum in the raffinate is reduced to 6-9 mg/l, that is 270 times in comparison with the prototype.

Example 2. Using the developed method was validated extraction separation of uranium and molybdenum in relation to the processing of carbonate-sulphate uranium-molybdenum solution obtained by regeneration of highly basic anion exchange resin. Carbonate-sulphate solution contained(g/l): uranium 3,99, molybdenum 1,90, carbonate and bicarbonate 23,5, sulfate ions 60, the pH value of 8.6. As extractant was used synergene mix: 0,15M D2EGFK with 0,10 M TBP in the hydrocarbon solvent, the ratio of phase A:B=1:2.

Extraction separation of uranium and molybdenum were conducted in the same manner as described in example 1. The results split the uranium and molybdenum by extraction with a gradual neutralization of the sulfuric acid solution are given in table 2 and figure 2.

td align="center"> Mo org, mg/l
Table 2
The dependence of the distribution of uranium and molybdenum from the equilibrium pH of the aqueous phase during the extraction solution 0,15M D2EGFK 0,10M TBP if A:B=1:2, and the gradual neutralization of sulfuric acid carbonate-sulphate solution containing 3,99 g/l of uranium and 1,90 g/l of molybdenum. The contact time of the phases 10 min
pH equalof 5.295,63to 5.935,966,236,566,62for 6.81
The uranium concentration in the raffinate, g/l0,1550,00350,00300,00320,00340,00320,00450,0061
Cu uranium49,5227826572490215424901771128,8
9,84,4of 5.45,29,07,48,810,8

Due to the lower concentrations of uranium in carbonate-sulphate solution and, respectively, low saturation of the organic phase with uranium, its content in the refined in some cases corresponded to the threshold photocolorimetric determination in the aqueous phase.

The results of extraction separation of uranium and molybdenum method developed by us testify to its high efficiency. Despite the relatively low saturation of the organic phase uranium, coextracted molybdenum does not exceed 10 mg/l, i.e. the ratio of molybdenum to Uranus in the extract is less than 0,13% compared with the ratio in the initial solution was 43.6%. Thus, the relative content of molybdenum in uranium in the extract by the proposed method decreased 350 times compared to their ratio in the initial solution.

The graphical dependence of the logarithm of the distribution coefficients of uranium from the equilibrium pH of the aqueous phase, are presented in figure 2 and is based on the results of table 2 indicates an increase in the range of pH from 5.6 to 6.6 compared with Bo is the narrow range of pH (5,9-6,3) in example 1, probably due to the lower saturation of the organic phase with uranium.

Example 3. Determined by the efficiency of separation of uranium and molybdenum developed by way of the carbonate-chloride solution of the same composition as in example 1, but as the extractant used a triple mixture of extractants composition: 0, 15M D2EGFK + 0,15M TBP + 0,07M TAA in a hydrocarbon diluent. The results of extraction separation are given in table 3 and figure 3.

Table 3
The dependence of the distribution of uranium and molybdenum from the equilibrium pH of the aqueous phase during extraction separation of uranium and molybdenum from carbonate-chloride solution using triple sinergetnoy mixture of extractants composition: 0,15M D2EGFK + 0.15 M TBP + 0,07M TAA, the ratio of phase A:B=1:2
redrawnthe 5.455,906,38to 6.58of 6.686,97
The uranium concentration in the raffinate, g/l1,840,3990,1960,6031,66 3,47
Cu uranium4,8829,762,819,05,631,65
Mo org, mg/l20,122,223,825,85,14,8

It should be noted that according to table 1 and table 3, the distribution coefficient of uranium using ternary mixture is significantly lower than when using the double mixture of 0,15M D2EGFK 0,15M TBP, and their maximum values are, respectively, 10-90 and 1500-2000.

Figure 3 shows the dependence of the logarithm of the distribution coefficient of uranium from the equilibrium pH of the solution. The original solution contained: 6,33 g/l of uranium, 2.85 g/l of molybdenum, 90 g/l of sodium chloride, 4 g/l of sodium carbonate, 15 g/l sodium bicarbonate. Synergene mixture of extractants (mol/l): D2EGFK 0,15, TBP 0,15, TAA 0,07. According to figure 3, the interval of the optimal separation of uranium and molybdenum slightly shifted to higher pH values. It was also noted higher coextraction of molybdenum and uranium (up to 25, 8 mg/l, compared with 6.0-9.0 mg/l when using dual sinergetnoy mix).

The data given in the example is x 2 and 3, confirm the efficiency of extraction separation of uranium and molybdenum proposed method in comparison with the prototype.

As a double sinergetnoy mixture was also tested 0,10M D2EGFK and 0,03M FAURE (effective neutral organophosphorus compounds of the phosphine oxide rasoredeleniy composition solidiarity oxide) and positive results were obtained by extraction separation of uranium and molybdenum from carbonate-salt uranium-molybdenum-containing solutions.

Method of separating uranium and molybdenum from the carbonate salt uranium-molybdenum aqueous solutions, including extraction from a solution of uranium, characterized in that the extraction of uranium perform liquid extraction of uranium by organic phase sinergetnoy mixture on the basis of di(2-ethylhexyl)phosphoric acid containing tributyl phosphate (TBP) or tributyl phosphate together with triallylamine (TAA) or phosphine oxide rasoredeleniy composition solidiarity oxide (FMR), in an organic diluent while gradually neutralization phase mixture of mineral acid under stirring to establish equilibrium pH values of the aqueous phase constituting the interval of 5.6 and 6.6.



 

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FIELD: chemistry.

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FIELD: chemistry.

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2 cl, 3 tbl, 2 ex

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FIELD: metallurgy.

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FIELD: technological processes.

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FIELD: metallurgy.

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FIELD: metallurgy.

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EFFECT: improved properties of finished product.

1 ex

FIELD: metallurgy.

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FIELD: metallurgy.

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EFFECT: improvement and reliability enhancement of metallurgical products (sheet products, foil paper, wire, storage plates).

2 tbl, 1 ex

FIELD: metallurgy.

SUBSTANCE: composition consists of one or more ortho-hydroxy-aryl-aldoxymes and/or one or more ortho-hydroxy-aryl-ketoxymes. Also it additionally contains one or more modifiers of selectivity consisting of phosphine and/or phosphonic acids, their salts and complex ethers and one or more modifiers of equilibrium. Molar ratio of modifier of selectivity to ortho-hydroxy-aryl-aldoxime is approximately from 0.001 to 0.05.

EFFECT: ensuring controlled, correspondingly desired coefficients of metal distribution.

21 cl, 10 tbl, 10 ex

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