Method of extraction of rich components from production solutions for processing of black-shale ores. RU patent 2493279.

IPC classes for russian patent Method of extraction of rich components from production solutions for processing of black-shale ores. RU patent 2493279. (RU 2493279):

C22B60/02 - Obtaining thorium, uranium or other actinides

C22B59 - Obtaining rare earth metals

C22B34/34 - Obtaining molybdenum

C22B34/22 - Obtaining vanadium

C22B3/24 - by adsorption on solid substances, e.g. by extraction with solid resins

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Method of producing scandium-bearing concentrate from red mud / 2484164
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Method of extracting rare-earth metals from aqueous solutions / 2484163
Proposed method comprises extraction of rare-earth metal cations by organic phase including extragent solution in inert diluter. Naphthenic acid is used as said extragent. Kerosene is used as inert diluter. Extraction is conducted in three stages at relationship between organic and aqueous phases O:A=1·(9-11) at every stage. Note here that, at first stage, europium cations (III) are extracted at content of naphthenic acid in kerosene of 10-13 vol. % and aqueous solution pH 5.0-5.1. At second stage, samarium cations (III) are extracted at content of naphthenic acid in kerosene of 13-16 vol. % and aqueous solution pH 4.6-4.7. At third stage cerium and lanthanum cations (III) are extracted at the same content of extragent and pH 5.0-5.1.

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

The invention relates to the field of hydrometallurgy, namely, to methods of extraction of rare and radioactive elements.

There is a method of concentration of uranium from dilute solutions, in which the sorption of uranium anion exchange washing anion from impurities, anion uranium by contact with the part of the uranium , desorption uranium acid-salt solutions and the precipitation of commodity uranium peroxide of hydrogen (patent RU №2404126, IPC C01G 43/00, publ. 20.11.2010).

The disadvantage is the inability of selective separation of uranium from anionic impurities, the reduction in the intensity of the sorption process.

There is a method of selective extraction of uranium from ore, in which the ore is subjected to after grinding leaching to produce pulp at pH 4.2-2.2 and later when pH 4.6-2.0 leaching process is combined with countercurrent sorption of uranium, maintaining the necessary value of the temperature and pH on the course of pulp. As an oxidizer use manganese compounds, desorption uranium saturated resin implement those solutions of (patent RU №2094512 MPK6 22 60/02, publ. 27.10.1997).

The disadvantage is the lack of selective separation of uranium from anionic impurities, and the introduction of an oxidant compounds with manganese not keep vanadium degree of oxidation (+IV) and achieve selective extraction of valuable components (uranium and molybdenum).

Know how to extract uranium, molybdenum and vanadium from ores, which includes crushing and leaching of valuable components of mineral acid and subsequent sorption extraction of dissolved uranium, molybdenum and vanadium from the pulp. Prior to leaching crushed ore in the form of an aqueous slurry oxidized by processing base resin in the OH form at pH 8.5-11.6, redox potential (ORP) -50 to +150 mV @ 30-80°C and leaching and sorption extraction of lead by adding its oxidized pulp sulphuric acid to pH 1.5-3.5 and anion in its sulfate form (patent RU №2211253, IPC 22 60/02, publ. 27.08.2003).

However, this method can't oxidize compounds of rare metals in the lower degrees of black shale anion exchanger in the OH form.

The technical result of the invention is selective sorption preconcentration and separation of uranium and molybdenum from vanadium and vanadium from rare earth elements and rare earth elements from iron and aluminum, increasing intensification of the sorption process, reduction of technological schemes and the use of environmentally friendly oxidants.

The technical result is achieved by the way of extraction of precious components of productive solutions processing of ores of black schist, including sorption of valuable components countercurrent ionitami at controlled pH of solutions, and redox potential Eh, sorption was carried out stages of several ionitami of productive solutions containing uranium molybdenum, vanadium and rare-earth elements, in the first stage by sorption on ion-exchange resin extract uranium and molybdenum, at the second stage by sorption on ion-exchange resin extracted vanadium in the presence of hydrogen peroxide at Eh 750-800 mV, pH 1,8-2,0 and at a temperature of 60 C and lead sorption of vanadium to the complete destruction of hydrogen peroxide and to lowering Eh below 400 mV, after which the nurseries sorption send cation at pH 2.0 to 2.5 and Eh 300-350 MB for extraction of rare earth elements.

The proposed method includes interactions in adsorption column in counter base resin complex salt composition solutions, and interaction is the variable interval values, redox potential (Eh) and pH environment in which the recoverable metals are in a dissolved condition.

The source of the solution, an applicant sorption redistribution, shown in table 1

Table 1 pH 1,2

Eh mV 350-450

Salinity 220-280 g/l

Components

H 2 SO 4 VO 2+ UO 2 2+ MoO 2 2+ REE 3+ PO 4 3- Fe 3+ Al 3+

Content, g/l

15 3,5 0,15 0,20 0,30 2,5 8-12 12-15

The composition of ionic forms of elements in the solution does not allow to choose one property and on its basis to create a technology of complex extraction and separation. To resolve this issue, you must apply a number of combined approaches of chemistry. It is known that the behavior of multivalent ions of elements in solutions depends on the ionic capacity, defined as the ratio of charge to the ionic radius. On Fig. grouped properties of rare metals depending on the ionic capacity. Metals with an ionic potential less than 3-cations (with 8-electron configuration in the outer shell). Metals with extremely high ionic potential - more than 10, form a stable complex anions with covalent bonds: (PO 4 ) 3- , (VO 4 ) 3 - UO 2 2+ , MoO 2 2+ . At ion potential 3-10 are metal ions with amphoteric properties. In addition, it is known that the Eh and pH affect ionic forms and kinetics of their mutual transition.

The essence of the method of extraction of valuable components from the pregnant solution processing ores extraction of uranium, molybdenum, vanadium and rare-earth elements is that at the first stage of sorption oxidation of uranium and molybdenum spend iron (+III) and vanadium (+IV), and the second stage of sorption oxidation of vanadium (+IV) conduct peroxide of hydrogen sorption of rare-earth elements is carried out after the destruction of peroxide.

Concentration and selective extraction of uranium and molybdenum anion, a floating counterflow solution, lead and under conditions which Eh support iron (Fe 2+ ) within 350-400 mW (Fe 3+ /Fe 2+ =20:1) and pH 1.0 to 1.5, vanadium with sufficient reliability held in solution in the form of a pair of V 4+ /V 3+ , which prevents the emergence of 5 V+ .

The emergence of vanadium in the maximum degree of oxidation call two unwanted process, on the one hand, the transition of vanadium on anionit together with uranium and molybdenum (in breach of selectivity of the process), and on the other hand, the precipitation of sparingly soluble complex salts of iron and vanadium. With a decrease Eh less than 350 mB decreases the intensity of sorption extraction and increase Eh more than 400 mB and a pH of more than 1.6 leads to the precipitation of sparingly soluble salts.

Selective separation of vanadium from rare earth elements is achieved through the introduction of peroxide of hydrogen (H 2 O 2 ), which plays a role as an oxidant and reducing agent. When the concentration of H 2 O 2 1.0-1.5 g/l or redox potential Eh 750-800 mV and pH of 1.8-2.0 vanadium is extracted from the solution to the content of 0.008 g/HP In the process of sorption of vanadium at a temperature of 60 C is the destruction of peroxide of vanadium hydrogen peroxide is removed and in the solution decreases Eh to less than 400 MB.

Example of the method.

Take a productive solution, the composition of which is given in table 1., spend sorption column filled with anion exchanger AM-p of 10 ml at pH 1.2 and Eh 400 mV in a dynamic environment, and passed the 1 liter of solution. Liquor sorption control on the content of uranium (U) and molybdenum (Mo). The sorption finish when the content of the liquor U no more than 4 mg/l and Mo 8 mg/L. Resin contains U 14.5 kg/t and Mo 17.5 kg/T.

Next liquor sorption containing 3.5 g/l V 2 O 5 , process solution to the CON to pH 1.9 and peroxide of hydrogen (H 2 O 2 ) at the rate of 1.0 g/l to Eh 750 mV. The solution is passed through a new portion of the anion to the residual content of V 2 O 5 the liquor is not more than 0.01 g/L. the Process of sorption carried out at a temperature 60 C to the complete destruction of H 2 O 2, and a decrease Eh less than 400 MB. Queen sorption passed through the cation exchanger cu-2 at pH 2.0 to 2.2 and Eh 300-350 MB for extraction of rare earth elements (REE). Removing Σ REE is about 90%.

The results of sorption extraction of metals are given in tables 2, 3, 4

Table 2

The results of sorption extraction and separation of uranium and molybdenum from vanadium.

Parameter

Liquor sorption

Content by ion-exchange resin

Eh, MB pH U Mo

V 2 O 5 , g/l

Fe Al, g/l REE, g/l

CC * , g/l

The Ratio Of Fe 3+ /Fe 2+ , g/l

U Mo mg/l WPI-e, % mg/l WPI-e, %

Fe 3+ , g/l

Fe 2+ , g/l

kg/t % kg/t % 350 1,2 15,0 90,0 26,0 89,6 3,5 5,2 0,5 9,2 0,31 141 10,4 13,5 90 17,4 87 400 1,2 4,0 97,4 24,0 90,4 3,5 5,3 0,28 9,1 0,25 150 18,9 14,6 97,3 17,6 88 450 1,2 2,0 98,7 21,0 91,6 3,5 5,3 0,25 9,0 0,26 140 21,0 14,8 98,6 17,9 89,5 400 1,0 12,0 92,0 25,0 90,6 3,5 5,2 0,20 9,1 0,25 143 26,0 13,8 92,0 17,5 87,5 400 1,25 3,0 98,0 21,0 91,6 3,5 5,2 0,22 9,0 0,24 155 23,6 14,7 98,0 17,9 89,5 400 1,5 1,0 99,3 18,0 92,8 3,5 5,2 0,23 9,2 0,23 150 22,6 14,9 99,3 18,2 91

*CC - salt content

Table 3

The results of sorption extraction and separation of vanadium from rare earth elements (REE)

Source solution

Liquor sorption

Content by ion-exchange resin

Parameter

H 2 O 2 , g/l

V REE, g/l Fe Al, g/l P, g/l

CC * , g/l

V 2 O 5 Eh, MB pH mg/l WPI-e, %

Fe 3+ , g/l

Fe 2+ , g/l

kg/t % 700 1,8 1,0 0,009 97,3 0,22 5,3 0,001 9,1 2,41 140 to 349.1 99,7 750 1,8 1,5 0,006 98,1 0,21 5,3 0,002 9,0 2,34 150 349,4 99,8 800 1,8 2,0 0,005 99,0 0,22 5,3 - 9,0 2,42 142 349,5 99,85 750 1,6 2,0 0,008 97,3 0,22 5,3 0,001 9,1 2,45 138 349,2 99,7 750 1,8 2,0 0,006 98,1 0,22 5,3 - 9,2 2,35 139 349,4 99,82 750 2,0 2,0 0,005 99,0 0,22 5,3 - 9,0 2,28 138 349,5 99,85

CC* - salt content

Table 4

The results of sorption extraction and separation of rare earth elements

Eh, MB pH

Liquor sorption

Content by ion-exchange resin

REE Fe

H 2 O 2 , g/l

REE mg/l WPI-e, %

Fe 3+ , g/l

Fe 2+ , g/l

kg/t % 300 2,0 18 92.0 5,1 0,21 - 20,2 92.0 350 2,0 22 90.0 5,0 0,18 - 19,8 90.0 400 2,0 26 88.0 5,0 0,20 - 19,4 88.0

Method of extraction of valuable components from productive solutions processing of ores of black schist, including sorption of valuable components countercurrent ionitami at controlled pH and redox potential Eh, sorption was carried out stages of several ionitami of productive solutions containing uranium, molybdenum, vanadium and rare-earth elements, in the first stage by sorption on ion-exchange resin extract uranium and molybdenum, at the second stage by sorption on ion-exchange resin extracted vanadium in the presence of hydrogen peroxide at Eh 750-800 mV, pH 1,8-2,0 and at a temperature of 60 C, and sorption vanadium lead to the complete destruction of peroxide of hydrogen and to lowering Eh below 400 mV, after which the nurseries sorption send cation at pH 2.0 to 2.5 and Eh 300-350 MB for extraction of rare earth elements.