Method of extracting uranium from mother liquors

FIELD: chemistry.

SUBSTANCE: invention relates to method of uranium extraction from mother liquors. Method includes obtaining resin, modified by aminophosphonic groups, and obtaining mother liquor, which contains from 25 to 278 g/l of sulphate and uranium. After that, mother liquor is passed through resin, modified by aminophosphonic groups, in acid form to separate uranium from mother liquor. Then, elution of uranium from resin is realised.

EFFECT: possibility of sorption extraction of uranium from solutions, which contain high concentrations of sulfate.

7 cl, 1 tbl, 3 ex

 

The present invention relates to a new, more eco friendly way of extracting uranium from acidic uterine leach liquors containing high levels of chloride, using resin-modified aminophosphonate groups.

Many of the minerals found in the surface layers in very small quantities, which makes it difficult to extract. However, in most cases, these minerals are extremely valuable, thereby justified the cost of retrieving them. One of these minerals is uranium. However, many other valuable minerals such as copper, Nickel, molybdenum, rhenium, silver, selenium, vanadium, thorium, gold, rare earth metals and the like, are also present in small quantities in the near-surface layers separately or quite often associated with uranium. Therefore, the extraction of these minerals was largely due to the same problems that arise in the extraction of uranium, and to extract such minerals can be used similar technologies, which are used to extract uranium regardless of the presence of these valuable minerals separately from uranium or a related condition. Thus, the methods of extraction of uranium are suitable for all such minerals.

Uranium vstreche is camping in many of the near-surface sediments, such as granite and granite deposits, pegmatites and pegmatitic dikes and veins, and sedimentary rocks, such as Sandstone, unconsolidated Sands, limestone and tpona very small number of near-surface sediments contain high concentrations of uranium. For example, most containing uranium deposits contain from about 0.1 to 1 wt.% uranium in the form U3O8as is known in the art. Some ores contain more than 1% uranium, so fat, containing less than about 0.1% uranium, are considered so poor that at present the extraction of uranium from them is not economically feasible, except when the simultaneous extraction of uranium and other valuable minerals such as vanadium, gold, etc.

Describes several ways of extracting uranium from containing uranium materials. One well-known method involves roasting of the ore, usually in the presence of sustaining combustion gas, such as air or oxygen, and the uranium is extracted from the resulting ash. However, the present invention relates to the extraction of uranium, representing a commercial value, using aqueous solutions for leaching. There are two well-known method of leaching (or wet processing method for extracting uranium, depends largely on the availability and size when poverhnostnogo deposits. If the deposits containing uranium available for development using standard equipment for extraction and is large enough to justify the standard formulation from an economic point of view, the ore is mined, crushed to increase the area of contact between particles of uranium in the ore and leach solution, usually up to a particle size of approximately less than 14 mesh, but in some cases, such as the development of limestone, nominally less than 325 mesh, and enter into contact with the aqueous leach solution for a time sufficient for the maximum extraction of uranium. On the other hand, if the deposits containing uranium unavailable or too little to justify the standard formulation, the aqueous leach solution is injected into the surface layer of at least one injection well, through deposition, provide contact containing uranium deposition in a period of time sufficient to extract uranium, and at least one production well get a leach solution containing uranium, which is usually denoted by the term "uterine" the leach solution (PLS). The last option is the leaching of subsurface formations in situ, which includes the present invention.

Most of the article is Hartig aqueous leach liquors are either aqueous acid solutions, such as sulphuric acid solutions, or aqueous alkaline solutions, such as solutions of sodium carbonate and/or sodium bicarbonate.

Usually quite effective for the extraction of uranium are aqueous acidic solutions. However, aqueous acid solutions basically cannot be used to extract uranium from the ore, or in-situ from sediments containing high concentrations kislotoprovody waste rock, such as limestone. Although some amount of hexavalent uranium is included in the composition of ores and near-surface sediments, the valency of the main quantity of natural uranium in the main is less than 6. For example, uranium minerals are commonly found in the form of uraninite, natural uranium oxide in various oxidation States, such as UO2UO3UO·U2About3and in mixed oxidation States U3O8(UO2, 2UO3), most of which is resin uranium ore containing from about 55 to 75% uranium as UO2and approximately 30% of the uranium in the form UO3. Other forms of uranium minerals include coffinet, carnotite, hydrated Vanadate of uranium and potassium (K2(UO2)2(VO4)2·3H2O, and urbanity, which are mixed phosphates, uranium, copper or calcium, for example, uranium tar General formula Cao·2UO3·P2O ·8H2O. Hence, to extract the uranium from the near-surface layers aqueous acidic leach liquors is necessary to oxidize the uranium with a lower valence to the soluble hexavalent state.

Combinations of acids and oxidizing agents described in the prior art, include nitric acid, hydrochloric acid or sulfuric acid, especially sulfuric acid, in combination with air, oxygen, sodium chlorate, permangante potassium, hydrogen peroxide, perchlorate and magnesium dioxide as oxidizing agents. However, the present invention proposes the use of solutions of sulphuric acid for leaching containing the appropriate oxidants and other additives, such as catalysts.

There are two main standard method of extracting uranium from mother solutions for leaching (PLS). One method of removing the solvent, is to use a nonaqueous solvent for the selective extraction of uranium from PLS.

The second method includes ionoobmennoi technology. Usually use strongly - and weakly basic anionoobmennika resin. The method using ion exchange has become the most preferred method for the extraction of uranium in different regions of the world due to its environmental benefits and security. There is no need the diamonds in the use of volatile toxic solvents in contrast to the retrieval method using a solution, contains chemically hazardous reagents.

In addition, it was found that in the environment containing relatively high concentrations of sulfate, i.e. more than 25 g/l, based on the composition of PLS is the contamination of the ion exchange resin. Such contamination reduces the capacity of the resin. In the patent US 4599221 described the use of resin modified aminophosphonate groups, for the extraction of uranium from phosphoric acid; however, there is a need to develop a method of extracting uranium from acidic leach liquors in environments containing high concentrations of sulfate. The extraction of uranium from phosphoric kilty differs from acid leaching, as in the solution for acid leaching are competing ions, such as sulfate, which can contaminate any environment for leaching. In the method using phosphoric acid ions such olustur. Additionally, the levels of uranium extracted by the method using phosphoric acid are relatively low, i.e. less than 300 ppm million When using the acid leach liquors ability of uranium to contact the resin should greatly increase because the levels of uranium in acid leach liquors can be up to 2000 mg/ml (or frequent./million). It is known that h is about the same concentration of uranium in the PLS, the working capacity in the acid solution to leach significantly exceeds the working capacity in the solution of phosphoric acid. Thus, specialists in the art generally do not use a method of extraction of metals from phosphoric acid for leaching of the acid solution.

The present invention offers a solution to the problems in the art by obtaining resin modified aminophosphonate groups, which can be used to extract uranium without pollution in environments containing sulphates more than 25 g/L.

In the present invention proposes a method of extracting uranium from the mother liquor, which comprises the following stages:

i) obtaining a resin-modified aminophosphonate groups,

ii) obtaining a mother liquor containing sulfate and uranium,

iii) passing the mother liquor through the resin, modified aminophosphonate groups to separate uranium from the mother liquor, and

iv) elution of uranium,

moreover, the sulfate content is from 25 to 280 g/l

The term "resin, modified aminophosphonate groups"used in this context, refers to a resin containing aminophosphonate group, or a resin containing aminocyclopropane group.

According to the present invention, the resin is a styrene polymer resin, in which the active aminophosphonate groups attached to the polymer matrix is. The term "styrene polymer" refers to a copolymer of a vinyl monomer or mixture of vinyl monomers containing styrene and/or at least one crosslinking agent, while the total mass content of styrene and a cross-linking agent is at least 50 wt.% calculated on the total weight of the monomers. The content of crosslinking agent is from 4 to 10 wt.%.

Crosslinking agent is a monomer containing at least two polymerizable double bond carbon-carbon bonds, including, for example, divinecaroline compounds, the compounds of di - and tri(meth)acrylate, and compounds divinely esters. Preferably the binder agent(s) is divinecaroline binding agent, such as divinylbenzene.

The polymer can form a gel-like or macroporous (macrostate) structure. The term "gel-like" resin refers to a resin, which is obtained from a copolymer with very low porosity (from 0 to 0.1 cm3/g), low average pore size (from 0 to 17 Å) and low specific surface according to the method of brunauer-Emmett-teller (BET, from 0 to 10 m2/g). The term "macroporous (MP)" resin used in relation to the resin, which is obtained from srednevoljskogo copolymer with a higher specific surface area compared to the gel-like resin. Total porosity MP resin is from 0.1 to 0.7 cm 3/g, an average pore size from 17 to 500 Å and a specific surface area by BET method of 10 to 200 m2/gsmol is corresponding ionic form, preferably in an acid form. The resin of the present invention may be in the sodium form.

The resin used for treatment of acid uterine leach solution (PLS). PLS according to the present invention includes uranium and sulfate. Uranium is mainly present primarily in the form U3O8, although there may be other well-known forms and uranium isotopes. The term "uranium"used in this context, refers to all forms and uranium isotopes. Uranium is present in the composition of PLS in the amount of from 25 to 2000 mg/l, preferably from 50 to 1500 mg/l and even more preferably from 60 to 1000 mg/L. of Sulfate ion and the sulfate complex, together denoted by the term "sulfate", present in the composition of PLS in the amount of from 25 to 280 g/l, preferably from 35 to 220 g/l and more preferably from 40 to 180 g/L. PLS according to the present invention optionally may contain other components. These components include, but are not limited to, iron, sulfuric acid, sodium, calcium, potassium, chloride, copper, phosphorus and aluminum. The pH PLS is in the acid range is from About to 4, preferably from 0 to 3, more preferably from 0 to 2, and most predpochtitelno from 0 to 1.8. Also PLS can be obtained by any standard method, including, but not limited to, in situ leaching, heap leaching, leaching, leaching from the pulp using ion-exchange resin and removing in situ.

The uranium is separated from the PLS by passing through PLS resin, a modified aminophosphonate groups. To separate uranium from PLS you can use any standard technology. These methods include, but are not limited to, the stationary layer, direct-flow or counterflow pseudovirions layer, leaching from the pulp using ion-exchange resins (RIP). The method is a batch or continuous process. Typically, the flow rate in the column or in the system with the Packed resin is from 0.5 to 50 volumes of resin/h

Uranium from the PLS is associated with resin-modified aminophosphonate groups, are retained on the resin and then elute from the resin. In the present invention using standard methods of elution. Preferably the resin with an associated uranium is treated with a solution of ammonia or ammonium hydroxide. Then for the elution of uranium resin washed with sodium carbonate solution. The uranium is removed from solution using standard methods of separation, such as, for example, deposition. It is established that it is possible to extract at least 10% of the uranium, nodamage is in the original PLS. At pH PLS in the range from 0 to 4, you can extract up to 25% of the uranium, preferably up to 10%. The number of extracted uranium can be from 5 to 25%, preferably from 10 to 25% and more preferably from 15 to 25%.

For the extraction of uranium from PLS with a high content of sulfate in addition to the ion exchange method can be used extraction solvent. Usually for extraction using solvents with Quaternary amino group. The advantage of the present invention is to enable the solvent molecule aminophosphonates or aminocyclohexanol group instead of functional Quaternary amino group. You can use the standard methods of exactIy solvent.

Examples

In this work, we used the following laboratory equipment:

a glass column with a shirt (height 30 cm, diameter 2-3 cm, equipped with a sintered glass filter No. 1), peristaltically nanoos with flexible hoses, graduated cylinder 10, 100, plastic flask for sample volumes of 25 ml, stopwatch, equipment, suitable for the analysis of uranium (i.e., for analysis with inductive coupled plasma (ICP)), standard laboratory glassware.

Used resin

Resin AMBERSEPTM940U registered trademark of Rohm and Haas Company, Dow Chemical Company. Resin in the sodium form with a polystyrene matrix, made of divinylbenzene containing aminophosphonate functional group.

Note

Before conducting the experiments, the resin was transferred into the corresponding ionic form (i.e., in the acid form).

Examples

Solution

Solution 1: Solution containing 500 mg/l uranium (U), 25 g/l of sulfate, 0 g/l chloride, 2 g/l iron (as Fe3+), incubated with the sample resin AMBERSEPTM940U within 8 hours

Solution 2: Solution containing 500 mg/l uranium (U), 195 g/l sulfate, 20 g/l chloride, 2 g/l iron (as Fe3+), incubated with the sample resin AMBERSEPTM940U within 8 hours

Solution 3: Solution containing 500 mg/l uranium (U), 278 g/l sulfate, 0 g/l chloride, 2 g/l iron (as Fe3+), incubated with the sample resin AMBERSEPTM940U at a flow rate of 2.5 volumes of resin/h

Experiments

All experiments were performed at 25°C. 500 ml were incubated with 10 ml of resin AMBERSEPTM940U. In order to avoid any external perturbations used a constant ratio resin/solution 1:50. To determine the effect on the capacity of the incubation mixtures was carried out at different pH values (i.e. 0, 1, 1,8, 2,5, 3). After shaking for 8 h were measured residual uranium content in the supernatant and the capacity of the resin. Results

pH
01 1,82,53
Capacity (g/l)Solution 141,037,429,034,838,0
Solution 236,224,219,423,027,8
Solution 324,8of 21.916,716,221,1

The increase in pH increases the capacity of the resin in the ratio of uranium. At pH 0 solution with a concentration of 195 g/l capacity is 36.2 g/l (U).

The results obtained indicate that the resin AMBERSEPTM940U is highly effective for the extraction of uranium in the presence of high sulfate concentrations.

It should be noted that the lower the pH, the higher working capacity. This property allows to use the sample resin AMBERSEPTM940U to extract uranium at high sulfate concentrations. The effectiveness of the resin (i.e. its working capacity) can be improved with decreasing pH.

E. SIA

The resin with the associated uranium (obtained as described in the experiment using a solution of 2 at pH 0) was treated with 2 volumes (resin) 1 BC (1 mol/l) solution of ammonium hydroxide. Then the resin was washed 1 BC (1 mol/l) solution of sodium carbonate.

The whole is contained in the resin uranium eluted 7 volumes (resin) solution of sodium carbonate.

1. The method of extracting uranium from the mother liquor, which comprises the following stages:
i) obtaining a resin-modified aminophosphonate groups,
ii) obtaining a mother liquor containing sulfate and uranium
iii) passing the mother liquor through the resin, modified aminophosphonate groups in acid form to separate uranium from the mother liquor, and
iv) elution of uranium
where the content of the sulfate is from 25 to 278 g/l

2. The method according to claim 1, where the pH-value of the mother liquor is from 0 to 4.

3. The method according to claim 1, where the mother liquor contains from 25 to 2000 mg/l of uranium.

4. The method according to claim 1, where the mother liquor contains from 35 to 220 mg/l of sulfate.

5. The method according to claim 1, where the resin, modified aminophosphonate groups, is in the sodium form.

6. The method according to claim 2, allowing to extract 10-25% of the uranium from the mother liquor.

7. The method according to claim 2, allows you to retrieve up to 25% of the uranium from the mother liquor.



 

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EFFECT: simple method with high recovery of molybdate or tungstate from solutions.

19 cl, 2 tbl, 10 ex

FIELD: metallurgy.

SUBSTANCE: method includes sorption of rich components from production solutions by ion-exchange material counterflow under controlled pH of environment and oxidation-reduction potential Eh. Sorption is performed by ion-exchange materials in stages from production solutions containing uranium, molybdenum, vanadium and rare earth elements. At the first stage uranium and molybdenum are extracted by anion-exchange material sorption. At the second stage vanadium is extracted by anion-exchange material sorption with hydrogen dioxide available at Eh of 750-800 mV, pH of 1.8-2.0 and temperature of 60°C, at that vanadium sorption is performed till complete destruction of hydrogen dioxide and till Eh is below 400 mV. Then barren solutions are transferred to cationite at pH of 2.0-2.5 and Eh of 300-350 mV for extraction of rare earth elements.

EFFECT: sorption concentration and selective separation of uranium and molybdenum from vanadium, and vanadium from rare earth elements, and rare earth elements from iron and aluminium, intensification of sorption process, reduction of flow diagram and possibility of environmentally sound oxidants use.

1 dwg, 4 tbl, 1 ex

FIELD: metallurgy.

SUBSTANCE: gold-bearing pulp from alluvial and ores is prepared, absorbent based on liquid hydrocarbons is used. Density of this absorbent is lower than density of the pulp. Then pulp contacts absorbent, during this process free gold transfers from pulp to absorbent. Free gold is extracted from absorbent by absorbent filtration in filter press. Volumetric contact of pulp with absorbent is performed due to pulp filtration in downward direction through at least one layer of absorbent, at that used absorbent has oxidation-reduction potential (Eh) not less than +1400 mV and is characterised by adhesion value to free gold not less than 40 Pa. Process efficiency of production plant for filtration-absorption extraction of gold from gold-bearing pulp is 800-1000 m3/day.

EFFECT: improving extraction efficiency of free gold of small, thin, pulverescent and disperse classes from alluvial and ores.

16 cl, 1 dwg, 5 tbl, 5 ex

FIELD: hydrometallurgy.

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

EFFECT: increased process selectivity and reduced number of stages in preparation of pure molybdenum.

9 dwg, 3 tbl, 4 ex

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