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INVENTION
Russian Federation Patent RU2081831
Method of extracting scandium from solutions of aluminum chloride
Name of the inventor: Samoilov YM .; Isupov VP
The name of the patentee: Institute of Solid State Chemistry and Mineral Processing, SB RAS; Yury Samoilov; Isupov Vitaly
Address for correspondence:
Starting date of the patent: 1993.11.29
Use of: extracting rare metals and alkaline extraction. The inventive method: scandium aluminum chloride solution is treated with a mixture of TBP containing 20 - 30 g / l Fe O 5 - 10 vol.%. carboxylic acid. Re-extracted with a mixture of scandium 3N 3N HCl and H 2 SO 4. In the presence of lithium in the starting solution is carried out at the beginning of its stripping with 6N HCl, then reextracted scandium.
DESCRIPTION OF THE INVENTION
The invention relates to the hydrometallurgy of rare metals, particularly to methods for the extraction of scandium and lithium from aluminum chloride solutions.
The method for extracting scandium from tributyl aluminum chloride solutions [1], followed by re-extraction of scandium solutions of hydrochloric acid.
The disadvantages of this method are smaller distribution coefficients scandium (D Sc January 3 C Al 60 with 70 g / l, scandium extraction 50 to 60%), and inability to extract and other valuable lithium component as D Li 0,1 0,3 (2).
The task of the invention improving the efficiency of extraction of scandium with the simultaneous release of lithium from solutions of aluminum chloride, which simplifies the process and provides greater completeness in the processing of rare metal raw materials.
This object is achieved in that the extraction of scandium and lithium from a chlorine-containing aqueous phase is carried out with tributyl phosphate containing HFeCl 4(Fe O 30 g / l), supplemented with the carboxylic acid (10 vol.) And metal stripping is performed separately: first reextracted lithium on June 8 n. hydrochloric acid solution, then with 3N scandium. HCl or a mixture with sulfuric acid.
Table 1 shows data on the extraction of scandium and lithium chlorinated solution composition, r-x Sc 0.13, Li 1.3, 64.0 Al, depending on the composition of the extractant. As can be seen from Table. 1, in the extraction of pure TBP (line 1, a prototype of the conditions) are observed low values of the degree of extraction (the E,), lithium and scandium.
Addition of carboxylic acid (HR) to TBP results in a slight increase in E Li from 5,7% to 15,2% E Sc when this is in the range 34 - 65.9% (row 2 of 5). Introduction to TBP ferrous chloride complex (HFeCl 4)O causes a sharp increase in E Li to a value of 95% E Sc and at the same time increased (Examples 6 10). The optimum concentration of iron in the organic phase should be 20 30 g / l. At concentrations less than 20 g / l low extraction of scandium and lithium, and for C Fe> 30 g / L increases the viscosity of the organic phase, which increases the delamination phase time. Adding the carboxylic acid to the rail TBP (Fe O 30 g / l) E Sc increases to a value of 90% E Li while still quite high (line 11, 15). On this basis, the optimum composition of the organic phase for the extraction of scandium and lithium from aluminum chloride solutions: TBP (Fe O 30 g / l) + HR (May 10%).
For scandium and lithium stripping of the organic phase from the optimum composition used solutions of hydrochloric acid and sulfuric acid mixture (Table 2). If there is a quantitative lithium reextraction for the entire range of the concentration of hydrochloric acid or sulfuric acid mixture. For scandium at -5 C HCl 3 n. and the phase volume ratio O: B = 1: 1 distribution of its coefficients are 0.2 0.3 and at a higher C HCl, D Sc increases sharply to a value of 116, which indicates the impossibility of re-extraction solutions of hydrochloric acid at a concentration of 5, 5 8.5 n. (Row 4 8 Table 2). When O: B equal to 5: 1, and n C HCl 4-6. back-extraction of scandium and small. To improve reekstragiruemosti scandium Mixtures HCl and H 2 SO 4, and the distribution ratio of scandium least 0.1 is observed for the mixture 3 normal acid (Example 15, Tab. 2), in this case iron reextract shift a few tenths g / l and stripping scandium degree is 91.5% based on the data table. 2 implementation of the split back-extraction of lithium and scandium as follows: first, the lithium is stripped June 8 n. hydrochloric acid solution, and thus there is a purification organic phase from aluminum impurities as quantitatively, scandium remains in the extract. Next reextracted scandium 3N. HCl 3N. H 2 SO 4 and it is isolated by known methods from the strip liquor and the organic phase is regenerated in the direct process for the extraction head.
Example 1. On taken chloride extraction solution containing in g / l: Li 1.31, 0.13 Sc, Al -64. Organic phase extraction is carried out: TBP (30 g / L Fe) + 10% caprylic acid at a ratio of O: B 1:20. After stirring for 10 min the extract is obtained containing 1.58 g / l Sc, 2.7 g / L of Li and 2 g / l Al (Sc extraction percentage 61% 10% Li). After washing the extract from lithium aluminum 6N HCl solution, the organic phase is obtained containing 1.52 g / l Sc and 0.28 g / L Li (transferred to the aqueous phase and 3.8% Sc> 90% Li). With further stripping scandium 3N HCl 3N H 2 SO 4 at O: B 1: 1 reextract obtained containing 1.5 g / l of Sc, and 0.22 g / L Li.
Example 2. Conditions of extraction solution composition as in Example 1, except for the value O: B, which is 1: 3. The organic phase is obtained containing 3.2 g / L of Li and 0.243 g / l Sc (extraction of 82 percent Li, Sc 62). After re-extraction of lithium (and cleaning of Al) 6N. HCl at O: B 3: 1 is obtained Li-reextract composition 8 g / L Li, 5 g / l Al and 0.06 g / l of Sc and an organic phase containing 0.222 g / l Sc and 0.2 g / l Li . The resulting reextraction mixture HCl - H 2 SO 4 at O: B of 5: 1 reextract obtained containing 0.6 g / l Sc (D Sc 0,17) and 0.5 g / L of Li.
Thus, the process of extracting scandium chloride solutions and lithium may be carried out as follows: co-extraction of scandium and lithium at O: B 1: 2 1: 3 and a separate re-extraction of lithium, followed by scandium.
Thus, the use of the proposed method allows to efficiently remove the scandium and lithium, and from solutions of chlorides using the same extractant, which simplifies the process and provides greater complexity in the processing of rare metal raw materials.
USED BOOKS
1. Korovin SS Glubokov YM Petrov KI et al. The interaction of metal chlorides with organophosphorus compounds. Proc. Chemistry of extraction processes. M. Science, 1972, p. 162,171.
2. LV Favorskaja Presnetsova VA Weinberger GN Extraction of scandium and tributyl iron from chloride solutions. Proc. Chemistry of extraction processes. M. Science, 1972, p. 178,181.
CLAIM
1. A method of extracting scandium from the solution of aluminum chloride, followed by extraction with tributyl phosphate reextraction, wherein the extraction mixture are tributyl phosphate, iron (Fe 0 20 30 g / l) 5 10 vol. carboxylic acid, and stripping of 3N. Or a mixture of HCl 3N. And 3N HCl. H 2 SO 4.
2. The method of claim. 1, characterized in that in the case of lithium present in the initial solution, it is carried out a pre-stripping 6N. HCl.
print version
Publication date 15.03.2007gg
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