Methods of selective extraction of metal components

 

The invention relates to the extraction and selective extraction of metal components, such as uranium, thorium, scandium and zirconium, from the source material, which includes these components. The method is especially suitable for extraction and extract metal from the ore sludge from the production of tantalum and niobium containing fluoride compounds metal components. The method involves the dissolution of tantalum and niobium components, separation of insoluble material and processing with sulfuric acid to remove the fluoride component in the form of gaseous hydrogen fluoride. Received sulfatizing material subjected to leaching. 4 C. and 11 C.p. f-crystals, 2 ill., table 1.

The invention relates to methods of selective extraction and extraction of metal from metal-containing materials. This method is especially suitable for extraction and retrieval of radioactive metal from the material containing tantalum and niobium, for example from ores, ore sludge and slag.

The production of many representing the industrial value of the metals or metal compounds from ores involves the operation in the cation contained in the ore metal components to metal components soluble in aqueous systems, to allow separation of metal components by the methods of selective extraction or etc.

In the usual process ore concentrates containing tantalum and niobium, usually decompose hydrofluoric acid (HF) or mixtures of hydrofluoric and sulfuric acid (HF/H2SO4). After that, the formed heptapteridae compounds of tantalum and niobium purified by solvent extraction and sephirot.

In particular, in the conventional process of production of tantalum pentoxide (Ta2O5) fraction of tantalum obtained from the decomposition of the ore, is desorbed into the aqueous phase, and patikis tantalum precipitated with ammonia and extracted with filtration method. Similarly, you can get patikis niobium.

Industrial schema extraction and separation of tantalum and niobium components of the enriched ore or slag tin production is described in detail in U.S. patents 2767047, 2953453, 2962372, 3117833, 3300297, 3658511, 3712939, 4164417 and 5023059. General description of other schemes ore processes can be found in the "Extractive metallurgy of niobium, tantalum and vanadium" in International review of metallurgy ("International Metals Review"), 1984, T. 29, 26, S. 405-444, published by the Society of Metallurgy (London), as well as in Eimer, the above-described methods remain the ore sludge with elevated levels of metal components that were not extracted or separated in the process. In particular, the ore sludge from industrial processes typically have elevated levels of radioactive metal components. There is therefore a need in the way of separation and extraction of radioactive metal from ore slurries for possible sales, as well as to obtain residue, which can be recycled and delete as non-radioactive waste. The proposed method allows to obtain these and other positive results.

Summary of the invention According to one of the objects of the invention, a method of selective extraction of metal components, including zirconium, uranium, thorium, or scandium, from a source material containing metal fluoride components, tantalum or niobium metal components and one or more able to transfer to a soluble state metal selected from zirconium, uranium, thorium, or scandium components, including: the implementation of the reaction of the source material with a solution ENISA least part of the tantalum or niobium metal components from the source material, the separation of insoluble material, the separation and removal of fluoride components of undissolved material by implementing the response undissolved material with mineral acid containing sulfuric acid, over a period of time and at a temperature and pressure sufficient for separation of gaseous hydrogen fluoride and education sulfatizing material, leaching sulfatizing material for dissolving at least part of the contained metal components and formation of an aqueous solution containing the dissolved metal components and a solid phase at least partially depleted of dissolved metal components, and selective extraction of dissolved metal component from the specified water solution.

The source of metal-containing material may be a natural ore, ore tailings, or waste containing precious metal components. This method is especially suitable for the extraction of metal from ore slimes production of tantalum and niobium.

According to another object of the invention proposes a method of extracting metal from the source m and radioactive metal components, separating and removing fluoride components from the source material, the leaching of the material obtained by translation in a solution of uranium, zirconium, thorium and/or scandium, filtration to obtain solids, leaching solids solution of ethylenediaminetetraacetate for removal of radium, thorium and/or uranium in solution and the formation of non-radioactive solid residue and precipitation from the filtrate of radium, thorium and/or uranium.

Further, the invention is illustrated by examples of its implementation with reference to the attached diagrams, in which: Fig. 1 is a block diagram of the sequence of operations in an embodiment of the method according to the invention, and Fig.2 is an exemplary process diagram for the implementation of options for performing the method according to the invention.

According to the invention proposes a method of selective extraction of uranium, zirconium, thorium and/or scandium from materials such as ore slurries, in particular, of the sulfate liquor from the leaching obtained from ore slimes. The proposed method is especially suitable for processing ore slurries containing fluorinated metal components, for example, to process the ore sludge from the production of tantalum and niobium, which to date is of the metallic constituents of the ore slimes containing fluorinated metal components due to the presence of fluorine and insolubility fluoride compounds. In a preferred embodiment of the proposed method fluoride components are removed from the ore slurry, the remaining ore tailings leached to dissolve the contained metal components, after which the dissolved metal components are selectively extracted from the leachate from the leachate.

In the future, the proposed method is described in more detail with reference to its implementation, in which the starting material is an ore slurry. It is clear that the proposed method can also be successfully used to extract metal components and other metal-containing source materials, non-ore slimes, so you should not consider this description as limiting the scope of the claims of the present invention.

In Fig. 1 schematically illustrates a possible variant of the proposed method. In the first stage of the original ore slurries, such as sludge from the production of tantalum and niobium, leached with acid. If the source material contains tantalum and niobium metal sostavlyaetsya separation, to separate the remaining solid ore residue from the aqueous solution after leaching. This solution can be subjected to further processing for the extraction of tantalum and niobium metal components.

The remaining solids ore slurry from the acid leaching in the second stage is subjected to reaction with acids, preferably in a rotary kiln at elevated temperatures to convert the metallic components in the ore slurry in sulfate compounds. The gas released during sulfatization, you can skip through the condenser and remove as HF (if the original ore tailings contain fluorinated metal components). Sulfatirovanne solids ore slurry is subjected to leaching with water and filtered to separate the aqueous solution from the remaining residues leaching. Residues from leaching (solids) can be subjected to further processing to extract metal components and/or for subsequent removal. The resulting aqueous solution is treated further in order separation and extraction of metal components containing zirconium, uranium, thorium and scandium.

Part of the aqueous solution obtained from the E. desorption Zr, U, Th and Sc) will contain the remaining elements of the original sulfatizing ore slurry, which were dissolved during water leaching, including, for example, Fe, Al, TA and Nb. You can use solvent extraction to remove tantalum, niobium and other metal components. Following the raffinate after removal of tantalum, niobium and/or other pre-installed metal components, can be treated with lime to precipitate the remaining metals in the form of hydroxides for removal.

These techniques will be described in more detail in the following paragraphs, in which the following terminology is used to trace the path of the source material through the process: the original ore slurry --> or remaining undissolved ore slurry (nerastvorimaya part of the original ore slurry after it has been processed to remove tantalum and niobium components) --> the resulting ore slurry (after processing to remove fluorides of metals) --> the remaining solids ore slurry.

Removal of tantalum and niobium components Tantalum and niobium components can be removed from the original ore slimes, such as fluorinated ore slimes promiscuous mineral acid for a time and at a temperature and pressure sufficient for the formation of a tantalum/niobium concentrate in the solution and the remaining ore slurry, and
separation of the remaining (non-dissolved) ore slurry from the associated solution from leaching.

In addition, the solution of tantalum/niobium concentrate can be processed further to extract tantalum and niobium. In particular, the solution of tantalum/niobium concentrate, separated after the initial reaction of the ore slurry with the mineral acid can be processed further to extract tantalum and niobium by further increasing the concentration of the solution by the method of solvent extraction and further processing of the solution in the form of the process of production of tantalum and niobium.

Mineral acids suitable for use with the original ore slurry for the formation of a tantalum/niobium concentrate in the solution include sulfuric acid and mixtures of sulfuric acid with another mineral acid, such as hydrofluoric acid. The initial reaction of the ore slurry with a solution of mineral acid can be conducted at atmospheric pressure and a temperature of 80-100oC. the Solids preferably leached acid at a concentration of 9-30 wt.% acid in plants the AI in General lead in the filtrate (solution, formed by acid leaching of the original ore tailings), a significant proportion, for example up to 70 wt.% or more of tantalum and niobium present in the ore tails before this treatment. Tantalum and niobium can be concentrated by the method of solvent extraction and concentrate to treat as part of the production of tantalum and niobium.

The remaining undissolved ore slimes (undissolved part of the original ore slimes after processing to remove the TA and Nb components) can be separated and/or dried by any known method.

Removal of fluorides
Fluoride compounds can be removed from the remaining ore slimes in the following way, providing
the reaction of the remaining ore slimes with a mineral acid or a mixture of mineral acid containing sulfuric acid, preferably concentrated sulfuric acid for a time and at a temperature and pressure sufficient to release gaseous hydrogen fluoride and education sulfated ore slimes. The resulting gaseous hydrogen fluoride can be extracted by the known methods.

The formation of sulfated ore slimes and the release of gaseous hydrogen fluoride which substances can usually be leaching, using 576-794 g (1.25-1.75 lb) of concentrated sulfuric acid at 453 g (1 lb) solids. Preferably, technological methods of sulfatization include adding 576 g (1.25 lb) of concentrated sulfuric acid at 453 g (1 lb) of the original solids and heating the mixture to 250oFor release of gaseous hydrogen fluoride. Released during the formation of sulfated solids gaseous hydrogen fluoride can condense and collect in the form of a solution of known methods.

Leaching received ore slimes (after treatment to remove fluoride compounds)
After removal of fluoride compounds obtained sulfatirovanne ore slurries subjected to leaching with water for the formation of an aqueous solution containing dissolved metal components. An aqueous solution of metal components, including one or more elements from the group of uranium, zirconium, scandium and/or thorium, can be obtained from the sulfated ore slurries containing such metal components, in the following way, providing
reaction (leaching) of sulfated ore slurry with water for a time and at a temperature and pressure EA to separate the remaining solids ore slimes from aqueous solution. You can then selectively extracted from an aqueous solution of dissolved metal components, for example, as will be described below.

The operation of the reaction of sulfated ore tailings with water, known as "leaching", can be conducted at atmospheric pressure and a temperature of at least 25oC to about 100oWith, preferably in the range of 60-90oC. the Solids preferably leached when the concentration of 5-50 wt.%, preferably at 10-25 wt.%, in the water. More preferably sulfatirovanne solid sludge is leached at a rate of 40% solids in water, and then filtered to education downloadable solution for subsequent solvent extraction and extraction of uranium, zirconium, scandium, and thorium.

Generally, leaching, preferably with stirring to obtain a homogeneous solution, for 30-1080 min (0.5-18 h) is sufficient for the formation of an aqueous solution of metal components, including uranium, zirconium, thorium and/or scandium.

Filtering the aqueous solution can be performed by any known method. Suitable methods include, without limitation, the filtering on the conveyor f is selected. While the filtrate is an aqueous solution containing metal constituents, including uranium, zirconium, thorium and/or scandium.

The remaining solids ore slurry after filtering can be leaching solution DA for removal of radium, thorium and uranium, and then filter. The filtered solids will contain non-radioactive residues, which can be buried. The solution of the filtrate can be treated with barium chloride, and then with sulfuric acid to produce barium sulfate with a crystal lattice containing the substituted atoms of radium. Any remnants of thorium and uranium can be displayed in the sediment in the same way. Precipitated radioactive concentrate containing radium, may be suitable for use in medicine.

Selective extraction of dissolved metal components
Dissolved metal components in aqueous solution formed by leaching, can be selectively extracted from aqueous solution and to extract, as will be described below. In a preferred embodiment of the proposed method the aqueous solution is subjected to cationic and anionic extraction in two separate process streams. Electoral excercise and uranium selectively sequentially separated from the aqueous solution, containing zirconium and uranium, in the following way, providing
ensuring contacting the aqueous solution with an organic medium, which contains not miscible with an aqueous solution of a diluent and extractant and, preferably, also contains a modifier, to form an organic phase containing zirconium and uranium, and the aqueous phase of the raffinate depleted in zirconium and uranium
separating the organic phase from the raffinate phase,
desorption of zirconium from the organic phase by contacting the organic phase with desorbent zirconium, resulting in a phase of zirconium, preferably the aqueous phase of Zirconia containing zirconium from the organic phase, and the resulting organic phase containing uranium diluent and extractant, and
desorption of uranium from the resulting organic phase by contacting the resulting organic phase with desorbent uranium, resulting in a phase uranium, preferably, the aqueous phase uranium containing uranium from the resulting organic phase, and the final organic phase containing the diluent and extractant.

If Zirconia is a solid phase, a water phase, containing desorbent circus

The extractants suitable for formation of an organic phase containing at least a portion of Zirconia and at least part of the uranium from aqueous solution extractants are able to selectively extract the zirconium and uranium. They include, but are not limited to, organic amines, in particular non-aqueous insoluble alkanolamine long-chain, preferably tertiary alkanolamine long chain, such as ALAMINE 336 (manufactured and supplied by Henkel Corporation, Illinois).

The choice of solvent depends, in part, on the used extractant. Suitable solvents are solvents that are compatible with organic environments and do not form a gel or become viscous so that they are hard to pump after loading of organic liquids. In particular, suitable diluents for use with organic aminovymi the extractants can be, but is not limited to, diluents with low aromatic content, including diluent SX-12 (Phillips 66 Co., Oklahoma), kerosene, thinner EXXAL 100 (Exxon Chemical Co., Houston, Texas) and thinner on the basis of alkanes With9and above, preferably9-C20.

The term "modify what ielem, for example, by increasing the separation between the organic phase and the raffinate, not forming the emulsion. The choice of modifier will partly depend on the extractant and diluent used in the organic environment. Suitable modifiers for use with organic aminoven extractant and aliphatic diluent can be, but not limited to, normally branched tridecylamine alcohol.

Organic medium preferably contains
5-15 wt.%, preferably 10 wt.%, the extractant from the organic environment,
0-3 weight. %, preferably 1-3 wt. % modifier from the organic environment, and
72-92% wt. diluent from the organic environment.

Preferred organic medium contains 5 to 15 wt.%, preferably 10 weight. % from organic environment alkanolamine ALAMINE 336 as extractant, 1-3 wt.%, preferably 3 wt.%, from the organic environment tridecylalcohol alcohol as a modifier, and the rest is thinner.

Suitable desorbent zirconium for the education of the aqueous phase of Zirconia containing zirconium from the organic phase, include mineral acids such as hydrochloric acid (Hcl), sulfuric acid (H2SO4) and nitric acid (NGO3). Predpochtitelney and temperature during the time of contact, enough to go zirconium in the aqueous phase. In a preferred embodiment of the proposed method the aqueous phase of Zirconia and the resulting organic phase are essentially not miscible, and therefore can easily be split, for example, by the method of decanting.

Suitable desorbent uranium for the formation of the aqueous phase uranium containing uranium can be salt solutions (brines), the solutions of carbonates, hydroxide solutions of ammonia (NH4OH), acid solutions with both molarity above 3M for such acids as hydrochloric (Hcl), sulfuric (H2SO4), etc. are Suitable salt solution contains a mineral salt and water and may also contain mineral acid. Suitable mineral salts are sodium chloride and potassium chloride. Suitable mineral acids are sulfuric acid (H2SO4) and hydrochloric acid (Hcl). The preferred salt solution (brine) contains sodium chloride at a concentration of 1 mol/l and sulfuric acid at a concentration of 0.1-1.0 mol/L. Suitable carbonate solution consists of carbonate and water. Suitable carbonates include alkali carbonates such as sodium carbonate, ammonium carbonate and potassium carbonate. The preferred solution of the second phase at ambient temperature in a period of time sufficient for the transition of uranium in the aqueous phase. In a preferred embodiment of the proposed method the aqueous phase uranium and the resulting organic phase are hardly miscible and therefore can easily be separated, for example, by the method of decanting.

The final organic phase remaining after extraction of zirconium and uranium, may be returned to the process for reuse.

From the above description it is clear that the raffinate comprises metal components, which were not extracted in the organic phase by contact with an organic environment. Therefore, the raffinate will contain dissolved metal components leached from the ore slimes, including thorium and scandium. Thorium and scandium can be selectively extracted from the raffinate described below.

According to a variant implementation of the invention, thorium and scandium selectively and sequentially sephirot from aqueous solution containing thorium and scandium, such as the raffinate from operations extraction of zirconium and uranium, by the way, according to which
provide contacting the aqueous solution with an organic environment, which includes not miscible with the aqueous solution of razbaby thorium and scandium, and the aqueous phase of the raffinate depleted thorium and scandium,
sephirot the organic phase from the raffinate phase,
extracted thorium from the organic phase, preferably by desorption of thorium from the organic phase by contacting the organic phase with desorbent thorium, resulting in a phase thorium, preferably aqueous phase thorium containing thorium, and the resulting organic phase containing scandium, diluent and extractant, and
extracted scandium from the organic phase depleted thorium, preferably by desorption of scandium from the resulting organic phase when contacting the resulting organic phase with desorbent scandium, resulting in a phase of scandium, preferably the aqueous phase of the scandium containing scandium, and the final organic phase containing the diluent and extractant.

If thorium is a solid phase, also formed aqueous phase containing desorbent thorium. Similarly, if scandium is a solid phase, also formed aqueous phase containing desorbent scandium.

The extractants suitable for the formation of the organic phase, containing at least part of the thorium and at least a portion of the scandium from the performance communications extractants include di-2-ethylhexylamine acid (D-2EGFK); tributyl phosphate (TBP), phosphinic acid RSA (manufactured and supplied by Daihachi Chemical, Japan), phosphinic acid IONQUEST 801 (manufactured and supplied by the company Albright & Wilson Associates, Richmond, Virginia), and mixtures thereof.

The choice of solvent depends, in part, on the used extractant. Suitable solvents are solvents that are compatible with organic environments and do not form a gel or not becoming so viscous that they are hard to pump after loading of organic liquids. In particular, suitable diluents for use with organic extractants thorium and scandium may be, but is not limited to, insoluble aliphatic diluents long-chain (C9-C16), kerosene and thinner SX-12.

The term "modifier" refers to a composition which when added to the organic environment enhances the extraction solvent, for example, by increasing the separation between the organic phase and the raffinate. The choice of modifier will partly depend on the extractant and diluent used in the organic environment. Suitable modifiers for use with organic extractants thorium and scandium and Alif is zilavy alcohol.

Organic medium preferably contains
5-15 wt.% the extractant from the organic environment,
0-6 wt.% modifier from the organic environment, and
79-89% wt. diluent from the organic environment.

Preferred organic medium contains
5-15 wt.%, preferably 5 wt.%, Dr. 2EGFK from the organic environment,
1-5 wt.%, preferably 5 wt.%, tributyl phosphate from organic environment,
0.1-1 wt.%, preferably 1 wt.%, tridecylalcohol alcohol from the organic environment and
79-93,9 wt.% aliphatic solvent from the organic environment.

Suitable desorbent thorium for the formation of the aqueous phase of thorium containing thorium from the organic phase, include mineral acids such as sulfuric acid (H2SO4), hydrochloric acid (Hcl) and nitric acid (NGO3). The preferred desorbent thorium for the formation of the aqueous phase thorium is a solution containing 250 g/l of sulfuric acid in water. Desorption of thorium can be conducted at atmospheric pressure and temperature for a time sufficient for the extraction of thorium in aqueous phase. In a preferred embodiment of the proposed method the aqueous phase of thorium and the resulting organic phase are essentially immiscible, and therefore they can who are aqueous solutions of caustic soda (aqueous solutions of hydroxides). Suitable caustics are caustic soda and sodium carbonate. The preferred aqueous solution of caustic soda for use as desorbent is 3 molar (M) sodium hydroxide solution. Desorption of scandium can be conducted at atmospheric pressure and temperature with contacting for a time sufficient for the transition of scandium in the phase of scandium, which in many variants of the proposed method is a solid substance containing scandium. In a preferred embodiment of the proposed method, the phase of scandium and the resulting organic phase are practically immiscible, and therefore they are easy to share.

The final organic phase remaining after extraction of zirconium and uranium, preferably is returned to the process for reuse.

The raffinate formed during the extraction of thorium and scandium, contains metal components, which were not extracted in the organic phase. Thus, the raffinate will contain the remaining dissolved metal components leached from the ore slurry and can be used to obtain a concentrate of the remaining metal components. In General, the raffinate may contain elements of the source is for example an amine, for the extraction of tantalum and niobium from the raffinate formed during the extraction of thorium and scandium. The remaining solution can be treated with lime to precipitate the metals in the form of hydroxides for removal.

Zirconium, uranium, thorium and scandium extracted in the proposed method, it is possible to extract in purified form of methods, which include sediment containing this metal component, separating the precipitate and calcining to obtain a metal oxide. Below are specific ways for each metal component.

Purified zirconium oxide (ZrO2) can be obtained by the method, according to which
carry out the reaction between the aqueous phase Zirconia and the main solution is to form a precursor of zirconium oxide,
separate the predecessor from the resulting solution and
convert the precipitate of the purified precursor oxide of zirconium.

Preferred basic solution is a solution of hydroxide, preferably ammonium hydroxide, ensuring the formation of a precipitate of zirconium hydroxide, which can be cleaned by annealing at temperatures above 100oWith, preferably 120-400oC.

Purified uranium oxide (UO2can procuratoria predecessor oxide of uranium,
separate the predecessor from the resulting solution and
convert the precipitate precursor of the purified uranium oxide.

Preferred basic solution is a solution of hydroxide, preferably ammonium hydroxide, forming a precipitate of ammonium diuranate, which can be cleaned by annealing at temperatures above 100oWith, preferably 120-400oC.

Purified fluoride thorium (ThF4) can be obtained by the method, according to which
carry out the reaction between the aqueous phase thorium and acid solution for education predecessor fluoride thorium,
separate the predecessor of fluoride thorium from the resulting solution, for example, filtration method, and
convert the precipitate predecessor in purified fluoride thorium.

Preferred acidic solution is a solution of hydrofluoric acid, forming a precipitate fluoride thorium, which can be separated and cleaned by the methods of filtration and drying.

In one embodiment of the proposed method, the phase of scandium is in the form of solid hydroxide scandium. Purified oxide of scandium can be obtained by the method lies in the fact that
calcined scandium hydroxide to obtain the oxide of scandium.

If scandium is water F. the phase of scandium with acid solution for formation of the precursor, containing scandium, separate predecessor from the resulting solution and
convert predecessor in purified scandium.

From the preceding description it is clear that the variant of the proposed method can be described as a method of extracting one or more predefined metal components selected from the group comprising zirconium, uranium, thorium and scandium, namely, that
carry out the reaction between the source of the ore slurry and a solution of mineral acid for a time and at a temperature and pressure sufficient to transfer tantalum and niobium in solution and the formation of a solution containing tantalum and niobium, and the remaining ore slurry,
separated and dried the remaining ore slurry,
carry out the reaction between the remaining ore slurry and mineral acid for a time and at a temperature and pressure sufficient to release gaseous hydrogen fluoride and education sulfated ore tailings,
carry out reaction (leaching) between sulfatation ore slurry and water for a time and at a temperature and pressure sufficient for the formation of an aqueous solution containing at least one from Zara is whether the components) of an aqueous solution of metal components. Removing a predetermined metal component of the aqueous solution can implement the described methods. Preferably, the extraction and desorption was carried out sequentially, starting with the loading and separation of zirconium and uranium, with subsequent loading and separation of thorium and scandium, in order to minimize the impact of one or more of these metal components to the extraction of other metal component. Consistent implementation of the extraction and desorption particularly preferably, if there is reason to believe that an aqueous solution containing more than one metal component from the group consisting of zirconium, uranium, thorium and scandium.

An embodiment of the proposed method, since the ore slurry, in which the predefined metal components include zirconium, uranium, thorium and scandium, can be described as the way in which
carry out the reaction between the source of the ore with a solution of mineral acid for a time and at a temperature and pressure sufficient to transfer tantalum and niobium in solution and the formation of a solution containing tantalum and niobium, and the remaining ore slimes,
separated and dried ostavi the e time and at a temperature and pressure sufficient to release gaseous hydrogen fluoride and education sulfated ore tailings,
carry out reaction (leaching) between sulfatirovanne ore slimes and water for a time and at a temperature and pressure sufficient to generate an aqueous solution of metal components,
filtered aqueous solution to separate the remaining solids ore slimes from aqueous solution,
provide contacting the aqueous solution with an organic environment, which includes not miscible with an aqueous solution of a diluent and extractant, and preferably also containing a modifier, to form an organic phase containing zirconium and uranium, and the aqueous phase of the raffinate depleted in zirconium and uranium
separate the organic phase from the raffinate phase, is desorbed zirconium from the organic phase by contacting the organic phase with desorbent zirconium, resulting in a phase of zirconium, preferably the aqueous phase of Zirconia containing zirconium from the organic phase, and the resulting organic phase containing uranium diluent and extractant, and was stripped uranium obtained from the resulting organic phase by Kohn is preferably the aqueous phase uranium, containing uranium from the resulting organic phase, and the final organic phase containing the diluent and extractant,
provide contacting the raffinate with other organic environment, which includes not miscible with raffinate solvent and extractant, and preferably also containing a modifier, to form an organic phase containing thorium and scandium, and the other phase of the raffinate depleted thorium and scandium,
separate the organic phase from the raffinate phase,
desorbed thorium from the organic phase by contacting the organic phase with desorbent thorium, resulting in a phase thorium, preferably aqueous phase thorium containing thorium from the organic phase, and the other resulting organic phase containing scandium, diluent and extractant, and
desorbed scandium from another resulting organic phase by contacting the resulting organic phase with desorbent scandium, resulting in a phase of scandium, preferably the aqueous phase of the scandium containing scandium from the resulting organic phase, and the other end of the organic phase containing the diluent and extractant.

In further describes some of the activities and benefits of the proposed method of extraction of metal components, including zirconium, uranium, thorium and scandium, from ore slurries was performed in laboratory conditions. In Fig.2 is a flow diagram of this method.

As the original ore slimes for this method took the ore sludge from the production of tantalum and niobium. Ore slurries were videlacele at a concentration of 20% solids on a dry basis, at the rate of 3 g of concentrated sulfuric acid per gram of ore slurry at 80oC for 1 h under stirring in a beaker 40 with a capacity of 4000 ml, shown in Fig.2. Aqueous liquor was separated from the remaining solids by using a Buchner funnel. Then the remaining solids was combined with concentrated sulfuric acid (36 normal) at a concentration of 1.25 g of acid per gram of dry residue and kept at a temperature of 250oC for three hours in a graphite crucible 42 with a capacity of 1000 ml to sulfatization acid leached ore residue. In the process of sulfatization formed hydrofluoric acid in gaseous form and it was removed by passing gas through the condenser 44.

Then sulfatirovanne solids were combined with water in the vessel 46 with a capacity of 1000 ml at a concentration of 40% solids and videris delali filtration method using a filter funnel 48.

The extraction of zirconium, uranium, scandium and thorium were carried out using two consecutive contour extraction solvent. On the reaction line for the extraction of zirconium and uranium used 8 pairs of interconnected vessels (mixer-settlers) 50 (a and b) 64 (a and b) located at different heights, to the organic solution from the top of each vessel to drain down from the top of the vessel through the remaining seven vessels to the bottom of the vessels. A pair of vessels were grouped into three groups: 3 pairs 3 pairs 2 pairs. The loading of uranium and zirconium in organic phase produced in the upper three pairs of 50 vessels (a and b) - 54 (a and b). The desorption reaction of zirconium were in the middle of the three pairs of 56 vessels (a and b) - 60 (a and b) in the middle of the line. The reaction desorption of uranium were in the other two lower pairs of vessels 62 (a and b) and 64 (a and b).

On the reaction line for the extraction of scandium and thorium used 7 pairs of receptacles 66 (a and b) 78 (a and b) located at different heights, to the organic solution from the top of each vessel to drain down from the top of the vessel through the remaining six vessels to the bottom of the vessels. A couple of tanks were grouped into three groups: 3 pairs 2 pairs 2 pairs. Download scandium and thorium in orgnic two pairs of receptacles 72 (a and b) - 74 (a and b) in the middle of the line. The desorption reaction of scandium were in the other two lower pairs of 76 vessels (a and b) and 78 (a and b).

Vessel-faucet And in each pair was a chemical beaker 200 ml, and the vessel In chemical beaker 500 ml

An aqueous solution (the filtrate from leaching) from the reservoir 46 to the leaching water was applied to the vessel 54A. The organic solution containing 10 wt.% alkanolamine ALAMINE 336 in the diluent, was filed in the vessel 50A for contacting the organic solution with an aqueous solution to obtain an organic phase containing uranium and zirconium metal components.

The organic phase containing zirconium and uranium, ran down to the second group of three vessels, where the solution was desirerable Zirconia. Desorption conducted by the method of contacting the organic phase containing zirconium and uranium, with a solution of 10% hydrochloric acid. Hydrochloric acid was applied to the vessel 60A and pumped down to contact with the organic phase. Aqueous solution from the desorption containing zirconium were taken from the bottom of the vessel V.

The remaining organic phase containing uranium was coming down in the remaining pairs of vessels, in particular in the vessel A, for desorption of uranium. Desorption of uranium Astor from desorption, containing uranium were taken from the bottom of the vessel V. Remaining after desorption of uranium in the organic phase is returned to the upper vessel V.

The raffinate obtained from the loading of uranium and zirconium, taken from the bottom of the vessel 50V and added to the second reaction line for the extraction of scandium and thorium. An aqueous solution containing zirconium and uranium, was filed in the vessel 70 and pumped up for contact with organic boot environment scandium and thorium. Organic boot environment was represented by a solution of D-2EGFK, TBP, TDA in the solvent, and it was added to the vessel 66A for contact with the aqueous solution for the extraction of scandium and thorium.

The organic phase containing scandium and thorium, the drain from the vessel 70 V in the vessel 72A, the first vessel to the second group of pairs of vessels. Thorium was desirerable from the solution by adding 250 g/l of sulfuric acid in the vessel A and pumping sulphuric acid up to contact with the organic phase. The solution from the desorption of thorium containing thorium was pumped from the bottom of the vessel 72A.

The remaining organic phase containing scandium, passed down in the third group of steam vessels for the desorption of scandium. Used desorbent scandium (trehballny caustic soda) was added to the vessel 78A, peracchia W. The remaining organic phase, leaving the vessel V returned to the vessel 70 V.

The raffinate obtained when loading scandium and thorium, without zirconium, uranium, thorium and scandium, were taken from the bottom of the vessel V.

From the organic phase, the aqueous solution or solid phase at different points in the process, these figures 1-19, enclosed in a circle, Fig.2, samples were taken and analyzed their composition. Analyses were performed using the methods of neutron activation analysis (NAA), inductively coupled plasma (ICP) and/or atomic absorption (AA), standard equipment on well-known technologies. The results are presented below (see table).

These results show that the proposed method can be successfully applied for the extraction and recovery of valuable metal from ore slurries, in particular for the extraction and retrieval of radioactive metal from ore slurries containing tantalum and niobium.

It should be understood that the above described embodiments of the invention are given to illustrate and not limit the scope of the invention.


Claims

1. The method of selective extraction of metal components, including zirconium, uranium, is objawy metal components and one or more able to transfer to a soluble state metal components, selected from zirconium, uranium, thorium, or scandium components, including: the implementation of the reaction of the source material with a solution of mineral acid for a period of time and at a temperature and pressure sufficient to dissolve at least part of the tantalum or niobium metal components from the source material, separation of insoluble material, the separation and removal of fluoride components of undissolved material by implementing the response undissolved material with mineral acid containing sulfuric acid, over a period of time and at a temperature and pressure sufficient for separation of gaseous hydrogen fluoride and education sulfatizing material, leaching sulfatizing material for dissolving at least part of the contained metal components and formation of an aqueous solution containing the dissolved metal components and a solid phase at least partially depleted of dissolved metal components, and selective extraction of dissolved metal component from the specified water solution.

2. The method according to p. 1, on the go, or scandium, able to transfer to a soluble state metal components.

3. The method according to p. 2, characterized in that stage leaching undissolved material for dissolving the metal components contained in the undissolved material, and the formation of a water solution containing dissolved metal components, includes the implementation phase reaction sulfatizing material with water for a time and at a temperature and pressure sufficient for the formation of an aqueous solution containing dissolved metal components, filtering the aqueous solution for separation of the remaining solids material from the aqueous solution.

4. The method according to p. 3, characterized in that the aqueous solution contains zirconium and uranium, and phase extraction of dissolved metal component of the aqueous solution includes the extraction of zirconium and uranium metal components, including provision phase of contacting the aqueous solution with an organic medium containing the diluent, is not miscible with the aqueous solution and the extractant to obtain the organic phase containing zirconium and uranium, and the aqueous raffinate phase, separating the organic phase from the phase Rafi is I, the resulting aqueous phase containing zirconium and an organic phase containing uranium and desorption of uranium from the organic phase by contacting it with desorbent uranium, resulting in an aqueous phase containing uranium, and the final organic phase containing the diluent and extractant.

5. The method according to p. 4, characterized in that the aqueous solution contains uranium, zirconium, thorium and scandium, and the method includes the additional extraction of thorium and scandium metal components of the raffinate phase, formed by contacting an aqueous solution with an organic environment, through the stages of extraction raffinate phase with the other organic medium comprising a diluent, is not miscible with the aqueous solution and the extractant to obtain the organic phase containing thorium and scandium, and other aqueous raffinate phase, separating the organic phase from the other phase of the raffinate, desorption of thorium from the organic phase by contacting the organic phase with desorbent thorium, resulting in an aqueous phase containing thorium, and the organic phase containing scandium, and desorption of scandium from the resulting organic phase by contacting phase, containing desorbent scandium, and the final organic phase.

6. The method according to p. 4, characterized in that the organic medium further comprises a modifier.

7. The method according to p. 5, wherein the other organic environment further comprises a modifier.

8. The method of selective extraction of metal components, including zirconium, uranium, thorium and scandium, from a source material containing the above metal components, as well as tantalum and niobium, providing for the implementation phase of the reaction between the source material and the solution of mineral acid for a time and at a temperature and pressure sufficient for the conclusion of tantalum and niobium in solution and the formation of the solution containing the tantalum and niobium, and material, separation of the remaining material, the implementation of the reaction between the remaining material and mineral acid for a time and at a temperature and pressure sufficient for separation of gaseous hydrogen fluoride and education sulfatizing material, leaching water sulfatizing material for a time and at a temperature and pressure sufficient to generate an aqueous solution of metal components, otfit is the formation of an aqueous solution with an organic medium, including the diluent, is not miscible with the aqueous solution and the extractant, and preferably also containing a modifier, to obtain an organic phase containing zirconium and uranium, and the aqueous phase of the raffinate depleted in zirconium and uranium separation of the organic phase from the raffinate phase, desorption of zirconium from the organic phase by contacting the organic phase with desorbent zirconium, resulting in an aqueous phase of Zirconia containing zirconium from the organic phase and organic phase containing uranium diluent and extractant, and desorption of uranium from the organic phase by contacting it with desorbent uranium, the resulting aqueous phase uranium containing uranium from the organic phase, and the final organic phase containing the diluent and an extractant contacting the raffinate phase with the other organic medium comprising a diluent, is not miscible with the raffinate phase and the extractant, and preferably also containing a modifier to obtain an organic phase containing thorium and scandium, and the other phase of the raffinate depleted thorium and scandium, separation of the organic phase from the other phase of the raffinate, desorption of thorium from the organic phase by Kohn is th thorium from the organic phase, and another organic phase containing scandium, diluent and extractant, and desorption of scandium from the resulting organic phase by contacting it with desorbent scandium, resulting in a phase scandium containing scandium from the organic phase, the aqueous phase containing desorbent scandium, and the other end of the organic phase containing the diluent and extractant.

9. The method of selective extraction of metal components, including zirconium, uranium, thorium and scandium, from sulfatizing source material containing the above metal components providing the stage of leaching water source sulfatizing material over time and temperature and pressure conditions sufficient for the formation of an aqueous solution of metal components, filtering the aqueous solution for separation of the remaining solids material from the aqueous solution, contacting the aqueous solution with an organic medium comprising a diluent, is not miscible with the aqueous solution, the solvent, and preferably also containing a modifier, to obtain an organic phase containing zirconium and uranium, and the aqueous raffinate phase, depleted zirconium and uranium, organicheskoi phase with desorbent zirconium, the resulting aqueous phase of Zirconia containing zirconium from the organic phase and organic phase containing uranium diluent and extractant, and desorption of uranium from the organic phase by contacting it with desorbent uranium, resulting in an aqueous phase uranium containing uranium from the organic phase and the final organic phase containing the diluent and an extractant contacting the raffinate with other organic medium comprising a diluent, is not miscible with raffinate, extractant, and preferably also containing a modifier, to obtain an organic phase containing thorium and scandium, and the other phase of the raffinate, depleted thorium and scandium, separation of the organic phase from the raffinate phase, desorption of thorium from the organic phase by contacting the organic phase with desorbent thorium, resulting in an aqueous phase thorium containing thorium from the organic phase, and another organic phase containing scandium, diluent and extractant, and desorption of scandium from another organic phase by contacting it with desorbent scandium, resulting in a phase scandium containing scandium from the organic phase, aqueous phase, codisposal eject metal components from the source material, containing zirconium, uranium, thorium, scandium, uranium, tantalum and/or niobium, with the division of non-radioactive and radioactive metal components, separating and removing fluoride components from the source material, the leaching of the material obtained by translation in a solution of uranium, zirconium, thorium and/or scandium, filtration to obtain solids, leaching solids solution of ethylenediaminetetraacetate for removal of radium, thorium and/or uranium in solution and the formation of non-radioactive solid residue and precipitation from the filtrate of radium, thorium and/or uranium.

11. The method according to p. 10, characterized in that it further carry out selective extraction of the dissolved metal from the aqueous solution.

12. The method according to p. 11, wherein the selective extraction of dissolved metal constituents from the aqueous solution includes a stage of contacting the aqueous solution with an organic environment, not miscible with the aqueous solution, to obtain a first organic phase comprising a part of the metal component, and the first aqueous raffinate phase containing the other part of the metallic components, separating the first organic fancesco phase with the first reextraction, resulting in a first aqueous phase comprising a part of the metal components, and the resulting organic phase comprising the other part of the metallic components, and Stripping the resulting organic phase by contacting the resulting organic phase with a second reextraction, resulting in a second aqueous phase containing part of the metal components, and the first organic phase, suitable for recirculatory.

13. The method according to p. 12, wherein the selective extraction of dissolved metal from the aqueous solution additionally provides a stage of contacting the first aqueous raffinate phase from the second organic environment, not mixed with the first aqueous raffinate phase, to obtain a second organic phase comprising part of the metal component, and the second aqueous raffinate phase containing the other part of the metallic components, separating the second organic phase from the second aqueous raffinate phase, Stripping the second organic phase by contacting the second organic phase with the third reextraction, resulting in a third aqueous phase, comprising part of the metal to which extractio second resultant organic phase by contacting the second resultant organic phase with the fourth reextraction, resulting in a fourth aqueous phase, containing part of the metal component, and a second organic phase, suitable for recirculatory.

14. The method according to p. 12, characterized in that the first organic phase contains zirconium and uranium, the first restraint extragere zirconium from the first organic phase, resulting in a first aqueous phase contains zirconium, and the resulting organic phase contains uranium, and the second restraint extragere uranium from the resulting organic phase for the formation of an aqueous phase containing uranium, and the first organic phase, suitable for recirculatory.

15. The method according to p. 13, wherein the second organic phase contains thorium and scandium, the third restraint extragere thorium from the third organic phase, resulting in a third aqueous phase contains thorium, and the second resultant organic phase contains scandium, and the fourth restraint extragere scandium from the second resultant organic phase for the formation of a water phase containing scandium, and a second organic phase, suitable for recirculatory, and niobium concentrate by solvent extraction, and the concentrate is processed for p is

 

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