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INVENTION
Patent of the Russian Federation RU2227170
METHOD OF RELIEF EXTRACTION
The name of the inventor:
The name of the patent holder: State Unitary Enterprise "All-Russian Scientific Research Institute of Chemical Technology"
Address for correspondence: 115230, Moscow, Kashirskoye sh., 33, State Unitary Enterprise "VNIIKhT", information-patent department
Date of commencement of the patent: 2002.10.16
The invention relates to hydrometallurgy. The method includes sorption of rhenium by a granular polymer, desorption of rhenium with an ammonia solution to obtain concentrated rinse solutions. As the sorbent, an extraction polymer (EP) consisting of granular super-cross-linked polystyrene and an extractant is used. As an extractant, a trialkylamine of the general formula R 3 N, where R is an alkyl radical (C 8 -C 10 ), is used. Impregnation of the granules of the hypercrosslinked polystyrene is carried out using a 0.1-40% trialkylamine solution of general formula 3 N, where R is alkyl radicals (C 8 -C 10 ) in an organic diluent. The method allows to provide a high degree of extraction of rhenium from poor solutions, to shorten the time and to reduce the cost of the hardware scheme.
DESCRIPTION OF THE INVENTION
The invention relates to hydrometallurgy and can be used to extract rhenium from solutions.
Methods are known for the extraction of rhenium by sorption using strongly [1] and weakly basic [2] ion-exchange resins.
A disadvantage of these recovery methods is the low selectivity in the extraction of rhenium from industrial solutions containing in addition to rhenium (from 0.05 to 0.2 g / l) to 25 g / l molybdenum and other impurities. In order to efficiently separate Re and Mo, strict control over the pH of the solutions to be processed and the use of concentrated acids in the technology are required, as well as the slow kinetics of mass transfer of ReO -4 ions in sorbents, reaching several hours. The industrial use of the above ion exchange resins is constrained by the high cost and large volumes of ion exchange resins required to create industrial rhenium recovery plants from solutions with a Re content <10 mg / l.
The closest to the proposed in terms of technical essence is the method for extracting rhenium on a granular polymer [3], in which an anionite of AN-21 porous modification containing 16% divnibenzene as a cross-linking agent and 0.8-1.0 weight parts is used for the sorption of rhenium . Isooctanol as a pore-former. In this rhenium extraction process, the sodium desorbate of the following composition: 435-760 Re; 110-140 SO2-4; 700-800 Cl - , acidified to pH 4 with hydrochloric acid, was directed to ion exchange columns. Sorption was carried out before the rhenium breakthrough in the filtrate 230-250 mg / l, the elution of rhenium from the saturated resin was carried out with a warmed ammonia solution of 2.6-2.7 N at a temperature of 40 
FROM.
The disadvantages of this method of extracting rhenium include the mandatory acidification of hydrochloric acid solutions before sorption, which dramatically increases production costs for large volumes of processed solutions. The minimum elution time is 5-6 hours, and the entire technological cycle of the rhenium extraction technology on the ion-exchange resin AN-21 is 25-30 hours, which makes the whole technological process of obtaining rhenium-containing salts considerably hindered. And for the complete elution of rhenium from the resin, 10 specific volumes of eluate are required.
The technical result of the invention is that the time of sorption and desorption in comparison with the same parameters of the known sorbents of rhenium ASBR-1, AN-21 (n), VP-14KR is significantly reduced, which dramatically reduces and reduces the cost of hardware scheme and technology for processing poor rhenium-containing Solutions (with concentration 
10 mg / l rhenium).
The technical result is achieved by using granules of super-cross-linked polystyrene impregnated in a 0.1-40% solution of a trialkylamine of the general formula (II) in a method for extracting rhenium from solutions, including sorption of rhenium by a granular polymer, rhenium desorption with an ammonia solution to obtain concentrated solutions. R 3 N, where R is C 8 -C 10 alkyl radicals, in an organic solvent.
The minimum and maximum amount of the extractant (from 0.1 to 40%) is chosen on the basis that less than 0.1% the extractive capacity of the multicomponent polymer decreases dramatically. At extractant concentrations above 40%, during extraction of rhenium, the loss of the extractant from the polymer matrix sharply increases.
The extracting polymer (EP) proposed for the recovery of rhenium has an increased resistance to abrasion (it exceeds the strength of currently used ion exchange resins made on the basis of divinylbenzene DVB and vinylpyridine (Table 2)).
The entrainment of the extractant from the EP granules for 10 cycles was not observed. At the same time, the capacity of rhenium in the proposed sorbent did not change (Table 1).
The invention was carried out as follows
Example. Rhenium extraction was carried out from solutions containing 10.23 mg / dm 3 rhenium and 110 g / dm 3 sulfuric acid, under static conditions. In a beaker with a stirrer, 1 g of a granular extracting polymer (EP) with a pellet diameter of 0.4 mm, with different concentrations of TAA (see Table), and 0.5 dm 3 rhenium-containing solution was placed. The rate of mass transfer in the extraction of rhenium from sulfuric acid solutions is much higher than currently used AMP, AN-21 (n), VP-14KR sorbents and does not exceed 120 minutes (Table 3). Analyzes for the content of rhenium were carried out according to the standard method by the colorimetric method.
The regeneration of rhenium from saturated EP, AMP, VP-14KR was carried out with a solution containing 10% ammonia and conducted in one stage. The rhenium-saturated polymer was mixed with 20 ml of the regenerating solution in a beaker with a mechanical stirrer for 15, 30, 70 and 90 minutes (Table 4). At the same time, part of the solution was taken for analysis. The extracting polymer was filtered off, washed with distilled water at a ratio of T: H = 1: 10, and regenerated with 10% ammonia at a ratio of T: F = 1: 20.
From the results given in Table 4, it follows that the use of the claimed method of extracting rhenium from solutions will allow:
- ensure a high degree of extraction of rhenium from poor solutions;
- reduce the time of the entire technological cycle of sorption - rhenium regeneration up to 2 hours;
- because of low EP losses in cycles, to reduce the prime cost of the technology of rhenium extraction from solutions several times due to reduction of the amount of used sorbent EP required for the whole technological cycle;
- It is economically feasible to extract rhenium from solutions of underground leaching (PV), heap leaching (KB), volcanic origin, etc. with rhenium content <1 mg / dm . 1. V.I. Bibikova, A.V. Peredereev et al. Kinetics of ion exchange of rhenium and molybdenum on resin AM./ In Sb. "Rhenium. Chemistry, technology, analysis. " - Moscow: Nauka, 1976, p.54-60. 2. A.G. Kholmogorov et al. Extraction of rhenium from sulfuric acid solutions and its separation from molybdenum on anion exchangers of various types - Ibid., P.63-66. 3. K.B. Lebedev et al. Industrial tests and introduction of anionite AN-21 porous modification for the extraction of rhenium. // Non-ferrous metals, No. 2, 1976, p.79-83.
A process for the recovery of rhenium from solutions, including sorption of rhenium by a granular polymer, desorption of rhenium with an ammonia solution to produce concentrated solutions of rhenium, characterized in that the granulars of the hypercrosslinked polystyrene impregnated in a 0.1-40% trialkylamine solution of the general formula R 3 N , Where R is an alkyl radical of C 8 -C 10 in an organic solvent. print version
USED BOOKS
CLAIM
Date of publication 15.03.2007гг
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