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INVENTION
Patent of the Russian Federation RU2094075
METHOD OF EXTRACTING LITHIUM FROM ITS ALUMINUM-CONTAINING MATERIALS
The name of the inventor: Samoilov Yu.M .; Isupov V.P.
Name of patent holder: Institute of Solid State Chemistry and Mineral Raw Material Processing, SB RAS; Samoilov Yuri Mikhailovich; Isupov Vitaly Petrovich
Address for correspondence:
Date of commencement of the patent: 1995.07.25
Usage: refers to the hydrometallurgy of rare metals, in particular to methods for extracting lithium from solutions of aluminum chloride obtained as a result of hydrochloric acid treatment of waste aluminum-lithium alloys, lithium aluminates of various compositions. SUMMARY OF THE INVENTION: The method comprises extraction with tributyl phosphate followed by stripping, extraction being conducted from aluminum chloride solutions resulting from hydrochloric acid dissolution of aluminum containing materials, using a mixture of iron-containing TBP (Fe = 20-30 g / l) with 5-10% carboxylic acid Acid, and stripping is carried out 4-6 N. Solution of hydrochloric acid.
DESCRIPTION OF THE INVENTION
The invention relates to the hydrometallurgy of rare metals, in particular to methods for extracting lithium from solutions of aluminum chloride, obtained as a result of hydrochloric acid treatment of wastes of aluminum-lithium alloys, lithium aluminates of various composition, chemical etching sludge of lithium aluminum alloys,
A method for extracting lithium from solutions of aluminum chloride with a helix and ketones is known, followed by a reextraction with water.
Disadvantages of the known method are small lithium distribution coefficients (D Li <0.1, extraction of lithium in one step of 10%), high losses of used extractants due to their solubility in the aqueous phase, and high fire hazard of organic extractants.
The purpose of the invention is to increase the efficiency of the lithium recovery process from solutions of aluminum chloride using an extractant slightly soluble in the aqueous phase and fireproof.
The goal is achieved by the extraction of lithium of their chloride-containing aqueous phase by tributyl phosphate (TBP) containing HFeCl 4 (Fe 0 20 30 g / l), with the addition of carboxylic acid (5-10 vol.), And lithium reextraction is carried out with a solution of hydrochloric acid with Concentration of HCl > 4 mol / l.
In Table. 1 shows the extraction data from the chloride-containing solution of the composition, g / l: LI 1.3; Al 64.0 depending on the composition of the extractant. As you can see from Table. 1, when extracting pure TBP (line 1), a small extraction value (E li %) is observed. Using pentanol (line 17, prototype condition) lithium recovery and low 5% Addition of carboxylic acid (HR) to TBP leads to a slight increase in E Li from 5.7 to 15.2% (lines 2-5). The introduction of an iron-containing chloride complex (HfeCl 4 ) 0 in TBP causes a sharp increase in E Li to a value of 95% (examples 6-10). The optimum concentration of iron in the organic phase should be 20-30 g / l. At a concentration of less than 20 g / L, lithium extraction is small, and at C Fe > 30 g / l, the viscosity of the organic phase increases, which leads to an increase in the phase separation time, and also to an increase in iron distribution in raffinate (example 10).
Since for the effective recovery of lithium, neutralization of the aqueous phase (ie HCl), for example, with ammonia, is necessary, in order to prevent the formation of a precipitate of iron hydroxide (in this case non-dispersible emulsions are formed), an acidic extractant additive, caprylic acid (HR ). The optimum HR content in the organic phase is 5-10%. At C HR <5%, the possibility of emulsification due to the formation of solid iron hydroxide particles remains, and at C HR > 10% the active concentration of TBP in the mixture decreases, which leads to a decrease in lithium recovery (examples 11 - 13). Based on this, the optimal composition of the organic phase for lithium extraction from solutions of aluminum chloride TPB (Fe 0 20 30 g / l) HR (5 - 10%).
To remove lithium from the organic phase of the optimal composition, hydrochloric acid solutions are used (Table 2). As you can see from Table. 2, an effective lithium reextraction is observed at O: B 1: 1 in the whole range of the change in the concentration of hydrochloric acid (examples 1 6). But to retain iron in the organic phase, it is necessary to use hydrochloric acid with a concentration of at least 4 N. (Example 6). At O: B 5: 1, in order to obtain a more concentrated lithium reextract, the optimal concentration of hydrochloric acid in the reextractant is 4 6 N. With C HCl <4 N, Iron begins to pass into the aqueous phase (for example, 9), and for C HCl > 6 N. In the lithium reextract there will be a large excess of hydrochloric acid and the associated high consumption of neutralizing reagents before obtaining lithium compounds from the re-extractor.
Example 1 . The extraction was carried out with a chloride solution containing, g / l: Li 6.5; Al 68. Extraction was carried out with an organic phase of TBP (30 g / l Fe 0 ) + 10% caprylic acid at an O: B ratio of 2.5: 1. After shaking for 10 minutes, an extract containing 2.4 g / L Li (extraction percentage 91.5) is obtained. After re-extraction of lithium 4N. Solution of hydrochloric acid at O: B 5: 1, a reextract containing 10 g / L Li (a percentage of lithium 83 reextraction) was obtained.
Example 2 . The chloride solution of the composition is taken for extraction, g / l: Li 1.3; Al 64. Extraction is carried out with an organic phase, as in Example 1, with an O: B ratio of 1: 3. An organic phase containing 3.2 g / L Li (a percentage of lithium extraction 82) was obtained. After re-extraction of lithium 6N. Hcl at O: B 3: 1, a reextract containing 8 g / L lithium (86% reextraction degree) was obtained.
Example 3 . A chloride solution containing 7 g / L Li and 70 g / l Al is taken for extraction. Extraction is carried out with an organic phase, as in Example 1, with an O: B ratio of 2: 1. A lithium re-extract containing 3 g / l (86% recovery of lithium) and a raffinate in which 0.5 g / L of Li remained remains. After the second stage of extraction with the fresh organic phase, the concentration of lithium in the raffinate is reduced to 0.1 g / l, the total recovery of lithium in two steps is 98.5%
Thus, the method according to the invention makes it possible to efficiently recover lithium from solutions of aluminum chloride. At the same time, the extractant, which is very inexpensive in the water phase and is fireproof, is used.
CLAIM
A method for recovering lithium from aluminum-containing materials by extraction with tributyl phosphate followed by stripping, characterized in that the extraction is carried out from solutions of aluminum chloride obtained by hydrochloric acid dissolution of aluminum-containing materials, using a mixture of iron-containing TBF (Fe 20 30 g / l) with 5 10% Carboxylic acid, and the stripping is carried out at 4 6N. Solution of hydrochloric acid.
print version
Date of publication 16.03.2007gg
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