Procedure for processing uranium ore

FIELD: metallurgy.

SUBSTANCE: silicate uranium ore is crushed and crumbled; further, it is leached with sulphuric acid with addition of nitric acid as oxidant. Uranium is extracted and refined from impurities using mixture of extragents. Also as mixture of extragents there is used synergetic mixture containing di(2-ethyl-hexyl)phosphoric acid - 0.05-0.075 mole/l, tri-alkyl-amine - 0.05-0.075 mole/l in hydrocarbon dissolver at ratio of volumes of organic and water phases VO-VW= 1-3÷6. Upon extraction organic phase saturated with uranium is washed with solution of sulphuric acid. Further, uranium is re-extracted with solution of coal-ammonia salts producing crystals of ammonia-uranyl-tri-carbonate and is filtered. Produced crystals are tempered to production of protoxide-oxide of uranium.

EFFECT: output of finished product in form of protoxide-oxide of uranium of high quality.

2 tbl, 2 dwg, 3 ex

 

The invention relates to the field of processing of uranium raw material and can be used in the hydrometallurgical processing of uranium ores, in particular for the complex processing of ores Elkon plateau of the Elkon uranium ore district.

There is a method of uranium ore processing, including crushing, ore grinding, leaching with sulfuric acid with the addition of sodium chlorate as an oxidant. Pulp after leaching is classification, countercurrent decantation with the addition of the flocculant and the uranium solution, after clarification on the filters is directed to the extraction. Extraction is carried out with 2.5%solution "Alamine 336 in kerosene with the addition of 2.5% of sodelovala alcohol. Reextraction uranium lead NaCl. This is followed by ammonium precipitation, thickening, filtering and special leaching from chlorine ion. Dried and Packed product contains more than 80% U3O8[Gromov B.V. Introduction to uranium. M: mhti them. Mendeleev, 1972, p.123-125].

The disadvantages of this method of uranium extraction in the extraction step tertiary amine should include the necessity of equimolar supplements of high molecular weight alcohols to prevent the formation of the third phase, the application only in the area of concentration of sulfuric acid of 10-30 g/l, the negative effects of the nitrate ions on the extraction of uranium.

Also the method for extracting uranium from solutions after leaching extraction solution D2EGFK in kerosene (Dapex process). As sinergetnoy additive and modifier in the solution add TBP. Before the extraction of iron in the solution is reduced to divalent to prevent its extraction together with uranium. Uranium is extracted from the organic phase by reextracting 10%soda solution. Then reextract is acidified with sulfuric acid and precipitated uranium ammonia [Ritchie G.M., Ashbrook AV Extraction. Principles and applications in metallurgy. Edited by Laskarina B.N., M.: metallurgy, 1983, s-257].

The disadvantages of this method are the low selectivity of the extraction of uranium and the need for a restore operation iron to Fe2+.

The closest analogue for the intended purpose and essential features is the patent RU 2239668 C2 (IPC SW 60/02, 20.04.2004), in which is disclosed a method of processing of uranium ores, including crushing and grinding ore, sulfuric acid leaching, sorption extraction of uranium ion exchange resins, solvent extraction uranium extraction from decorate with the cleanup of uranium from impurities, using as a solvent a mixture of extractants, reextraction uranium solution ammonium salts of obtaining crystals ammoniyuraniltrikarbonata (AUTKA), filter the s and annealing of the obtained crystals AUTKA to obtain a mixed oxide of uranium.

The disadvantages of this method of uranium extraction are as follows:

the presence of additional operations - processing rich mixture of extractants concentrated uranium solutions for Considine, the frequency of operation of obtaining concentrated uranium solutions, technological scheme additional concentration of uranium sorption extraction ion exchange resins.

The technical result of the proposed method is:

- getting the finished product in the form of nitrous oxide uranium high quality that meets the national requirements for THE 95.1981-2009 nitrous oxide (U3O8);

- the application of the proposed mixture of extractants increases the effectiveness of the technology to extract uranium as a whole;

- reduced consumption of reagents;

- reducing the cost of production by eliminating the operation of sorption.

The technical result is achieved by the method of processing of uranium ores, including crushing and grinding ore, sulfuric acid leaching, extraction extraction purification of uranium from impurities using as a solvent a mixture of extractants, reextraction uranium solution ammonium salts of obtaining crystals ammoniyuraniltrikarbonata (AUTKA), filtration and calcination of the obtained crystals to obtain sakisaka uranium. Leach is subjected to silicate uranium ore with the addition of nitric acid as an oxidant and as an extractant used sinergetnuyu mixture containing di(2-ethylhexyl) phosphoric acid 0,05÷0,075 mol/l, trialkylamine 0,05÷0,075 mol/l and tributyl phosphate 0,05÷0,075 mol/l in a hydrocarbon diluent with respect to the volumes of the phases Vo÷Vin=1-3÷6, after the extraction of rich uranium organic phase is washed with a solution of sulphuric acid.

Example 1.

Extraction uranium extraction was performed from a solution of the following composition, g/l: U 1,56; Fe3+6,0; H2SO420,0; NO-35,0. By the method of successive contacting the organic phase with an aqueous solution in a separating funnels were determined by saturation of uranium extractant after 3-8 contacts when the ratio of the phases O:b=1:1. As extractants had the following mixture of extractants in kerosene: 0.05 mol/l TAA+0.05 mol/l D2EGFK+0.05 mol/l of TBP; 0,075 mol/l TAA+0,075 mol/l D2EGFK+0,075 mol/l of TBP. Experimental data are given in table 1.

The data show that the saturation of equimolar mixtures of the composition of 0.05 mol/l TAA+0.05 mol/l D2EGFK+0.05 mol/l of TBP and 0,075 mol/l TAA+0,075 mol/l D2EGFK+0,075 mol/l of TBP in similar conditions was 5.2 g/l and of 7.95 g/l, respectively. When the first contacts triple energenie mixture well shaken out a bit as is ESA. But in subsequent contacts, closer to saturation, an exclusion of iron uranium.

Example 2.

In the next series of experiments shows the effect of nitrate ions on the extraction of mixtures of extractants of the following composition: 0,075 mol/l TAA+0,075 mol/l D2EGFK+0,075 mol/l of TBP. Studies were performed on solutions of the following composition, g/l: U 1,56; Fe3+6,0; H2SO420,0; NO-3- 0; 3,33; 5; 7. The results of the experiment are presented in figures 1,2.

Changing the value of the saturation uranium with increasing nitrate concentrations from 3.3 g/l to 7 g/l practically does not occur. Moreover, we observed a slight increase in the slope of the curve at the initial part of the isotherm when the concentration of the nitrate ion. This fact is very important for the practical application of the proposed mixture of extractants in technology, since, as noted above, in domestic practice on stage leaching use of nitric acid as an oxidizer.

Example 3.

Studies were performed on the clarified solution obtained after autoclave leaching of ore.

Sulphate leachate leachate obtained after crushing and grinding ore, sulfuric acid pressure leaching, with addition as the oxidant nitric acid, filtering, and clarifying had the following composition, g/l: X 1,5; V 0,33; Fe 5,1; Si 0,056; Al 1,31; Mg 4,19; Ca ,47; H2SO430,6. Extraction the extraction of uranium were sinergetnoy mixture composition of 0.075 mol/l D2EGFK+0,075 mol/l TAA+0,075 mol/l of TBP in a hydrocarbon diluent with respect to the volumes of the phases Vo:Vin=1-5,5 reverse current for a 4-speed extraction. The time of contact was 3 minutes vanadium in these conditions is not extracted, and the iron concentration in a saturated solvent is less than 30 mg/L.

After extraction the extraction of uranium enriched uranium in the organic phase is washed with a solution of sulfuric acid (15 g/l) at the ratio of volumes of the phases Vo:Vin=5:1, to remove coextrusion impurities. While the iron content in the extract was reduced to 5-8 mg/l After washing the organic phase was conducted the solid-phase reextraction uranium solution ammonium salt concentration of 150 g/l

Crystals AUTKA washed with a solution of ammonium salt (150 g/l), filtered, and progulivali to nitrous oxide of uranium. The content of impurities in relation to uranium are shown in table 2.

From the data in table 2 shows that the obtained by this method, the oxide-uranium oxide corresponds to the impurity content of nitrous oxide of uranium on THE 95. 1981-89.

Table 1
Extraction isotherm ur is on and iron extractants of different composition.
№ p/pThe extraction mixtureThe U concentration in the raffinate, g/lThe U concentration in the organic phase, g/lThe concentration of Fe in the organic phase, mg/l
10.05 M D2EGFK+0,05M TAA+0,05M TBP0,0461,52442,94
20,112,98433,84
30,3064,248of 5.53
40,894,9281,46
51,365,1381,31
61,475,218-
10,075 M D2EGFK+0,75M TAA+0,M TBP0,01991,5560,0
2 0,04423,07679,47
30,1034,54372,36
40,1995,91436,1
50,4727,0126,7
60,987,6021,89
71,33to 7.84-
81,467,950,73
10,2M TAA+0,2M DC0,02281,5375,01
20,2362,8612,0
31,72,7211,5

Table 2
Mass fraction of impurities in uranium content, %.
UK+NaPVFeMoSiBCuNiAlMnThEuSmCd
Oxide of uranium THAT 95.1981-8984,00,020,030,010,030,0090,0082,5*10-50,00060,000040,0100,0060,005is 0.00020,000050,00005
Sample84,40,0020,010,007 0,0030,00050,0003<1·10-50,000050,00004<0,0010,000070,00050,000020,00004<1·10-5

The method of processing of uranium ores, including crushing and grinding ore, sulphuric acid leaching, extraction extraction purification of uranium from impurities using a mixture of extractants, reextraction uranium solution ammonium salts of obtaining crystals ammoniyuraniltrikarbonata, filtration and calcination of the obtained crystals to obtain a mixed oxide of uranium, characterized in that the leaching is subjected to silicate uranium ore with the addition of nitric acid as an oxidant and as a mixture of extractants used sinergetnuyu mixture containing di(2-ethylhexyl)phosphoric acid 0,05÷0,075 mol/l, trialkylamine 0,05÷0,075 mol/l and tributyl phosphate 0,05÷0,075 mol/l in a hydrocarbon diluent at a ratio of volumes of organic and aqueous phases, is equal to Vabout÷Vin=1-3÷6, after extraction extract rich in uranium in the organic phase is washed with a solution of sulfuric acid.



 

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FIELD: metallurgy.

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FIELD: metallurgy.

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FIELD: chemistry.

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7 cl, 8 ex, 2 tbl

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9 cl, 3 tbl, 1 ex

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7 cl, 6 tbl, 6 ex

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17 cl, 1 dwg, 7 tbl, 5 ex

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2 tbl

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1 ex

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3 cl, 7 tbl, 1 dwg, 2 ex

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4 cl, 1 tbl, 4 ex

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6 dwg, 3 ex

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6 cl, 1 tbl, 17 ex

FIELD: chemistry.

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5 tbl, 7 ex

FIELD: metallurgy.

SUBSTANCE: invention can be implemented in method of extraction and concentrating rhenium (VII) from acid sulphate, chloride and nitrate solutions. The method consists in extraction of rhenium from acid solutions and its successive re-extraction with water solution of ammonia. As extracting agent mixture of hexabutyltriamide and trialkylphosphineoxide in kerosene is used. Reagents are taken at molar ratio 1.0 : (0.2-5.0) correspondingly.

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6 tbl, 6 ex

FIELD: metallurgy.

SUBSTANCE: invention can be implemented for extraction, purification and concentration of vanadium, for example at processing re-circulated mother solutions of production V2O5 and acid solutions of leaching ashes after black oil burning. The method of extracting vanadium from weak-acid mediums consists in extracting with nitrogen containing extracting agent, in the capacity of which N-(2-hydroxy-5-nonylbenzyl)-ββ-dihydroxyethylamine (NBEA) is used in organic diluter. After extraction re-extraction of vanadium is performed with ammonia solution.

EFFECT: upgraded degree of vanadium extracting from weak-acid solutions.

1 tbl, 5 ex

FIELD: metallurgy.

SUBSTANCE: invention relates to hydrometallurgy, particularly it relates to method of joint separation of platinum metal (PM). Method includes several stages: first stage is implemented for leaching of initial material, containing PM and impurity element. The second stage is implemented for removing of impurity elements from alkaline solution from leaching by solvent extraction, the third stage - for removing of palladium from raffinate. The fourth stage is implemented for removing from raffinate of impurity element cations by extraction by dissolvent. The fifth stage is implemented for extraction from the raffinate of platinum by hydrolysis, the sixth stage - for extraction from ruthenium settling by leaching and the seventh stage - for extraction of iridium by solvent extraction with receiving of desorbed alkaline solution, containing iridium, and raffinate containing rhodium.

EFFECT: effective removing of impurity elements, with each of separated PM allows grade enough for that it could serve in the capacity of commercial product.

18 cl, 14 tbl, 1 ex, 3 dwg

FIELD: metallurgy.

SUBSTANCE: invention concerns method of gallium extraction from aluminate mud. Method includes electrodialysis, in which solution for recapture containing gallium is subjected to electrodialysis for gallium concentration and acid extraction, stage of iron removal, when gallium is removed from concentrated solution, and stage of ultrafiltration, when iron-free gallium solution is neutralized. Received suspension of gallium hydroxide is subjected to ultrafiltration for suspension concentration. Then it is implemented stage of resolution, when concentrated suspension of gallium hydroxide is dissolved in alkaline solution, and electrolysis stage, when alkaline electrolytic solution of gallium received on stage of resolution is subjected to electrolysis for metallic gallium extraction.

EFFECT: providing of ability to reuse acid excluding waste acid generation commercially, increasing of gallium concentration in alkaline electrolytic solution of gallium, thereby increasing current efficiency on the electrolysis stage, and decreasing of spent solution quantity.

5 cl, 1 dwg, 2 tbl, 1 ex

FIELD: metallurgy of rare and dispersed metals, chemical technology.

SUBSTANCE: invention relates to a method for extraction separation of tantalum and niobium. Method involves extraction separation of tantalum from niobium with organic solvent. As an organic solvent method involves using a mixture of methyl isobutyl ketone taken in the amount 40-80 vol.% with aliphatic (C7-C9)-alcohol taken in the amount 20-60 vol.%. At the extraction process tantalum transfers into organic phase and niobium - into aqueous phase. Then organic and aqueous phases are separated. Invention provides enhancing the extraction degree of tantalum into organic phase and to enhance the separation degree of tantalum and niobium in extraction.

EFFECT: improved separating method.

5 tbl, 5 ex

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