Method of producing scandium oxide

IPC classes for russian patent Method of producing scandium oxide (RU 2478725):

C22B59 - Obtaining rare earth metals

C22B3/06 - in inorganic acid solutions

C01F17 - Compounds of the rare-earth metals, i.e. scandium, yttrium, lanthanum, or the group of the lanthanides

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FIELD: metallurgy.

SUBSTANCE: proposed method comprises dissolving scandium-bearing concentrate in sulfuric acid, removing acid-insoluble residue, and precipitating scandium in the presence of ammonium compounds. Then, precipitate is filtered, flushed, dried and calcined to obtain scandium oxide precipitate. With acid-insoluble residue removed, sulfuric acid concentration in filtrate is increased to 540-600 g/dm³, ammonium chloride is added to solution in amount of 26.7-53.5 g/dm³ at 50-70°C and held for one hour at mixing. Produced precipitate is flushed by ethanol at volume ratio of 1-10-11.

EFFECT: simplified process, higher purity scandium oxide.

3 ex

The invention relates to ferrous metallurgy, namely the recovery of scandium oxide from poor scandium concentrate obtained after processing by the carbonate leaching of red mud waste production in the processing of bauxite to alumina.

A known method of producing scandium oxide (patent RU 2069181, IPC C01F 17/00, 1996), including the dissolution of scandium-containing concentrate in mineral acid to bring the acid concentration in the solution to 260-400 g/DM³the sludge separation of scandium sulfate from the solution, washing and dissolution in water and precipitation from a solution of soluble compounds of scandium by processing, for example, oxalic acid, washing, drying and calcination to obtain commercial scandium oxide (99%).

The disadvantage of this method is a significant percentage of the total losses of scandium (up 11%), which are caused in particular by the fact that when washing the precipitate of sulphate of scandium sulfuric acid concentration used for deposition of scandium-containing concentrate, the solubility of scandium in it quite high, which leads to its effects.

Closest to the proposed technical solution is the method of producing oxide of scandium (patent RU 2257348, IPC C01F 17/00, 2005)(prototype), the essence of which is expressed by the following set of essential to recognize the s: the dissolution of the scandium-containing solution in mineral (salt, sulfuric, nitric) acid; clear scandium solution from impurities by processing solutions solfataras inorganic compound and then with barium chloride; processing the purified scandium solution of alkaline reagents, in particular NH₄OH, obtaining low-solubility compounds of scandium: oxyhydrate or hydrooxicarbonate scandium; filtering the slurry to separate scandium precipitate from solution; sludge treatment with formic acid; separating the precipitate formate scandium from the mother liquor; washing the precipitate with formic acid, drying and calcining the precipitate to obtain commercial scandium oxide 99.99%purity.

The disadvantages of this method include its multi-stage, in particular to remove impurities at the first stage in scandium solution is injected sulfadimidine inorganic compounds and barium chloride, and then spend additional sludge treatment oxyhydrate scandium formic acid.

Thus, the authors goal was to develop a simple method to produce scandium oxide of high purity with a minimum total loss of scandium.

The problem is solved in the proposed method of producing oxide of scandium, including the dissolution of scandium-containing concentrate sulfuric acid, removing the acid-insoluble precipitate, the transfer of scandium in about the of Adak in the presence of ammonium compounds, filtering, washing, drying and calcination of the resulting sludge, characterized in that after removal of the acid-insoluble precipitate the sulfuric acid concentration in the filtrate is brought to 540-600 g/DM³as ammonium compounds using ammonium chloride, is introduced into the solution in the amount 26,7-53,5 g/DM³at a temperature of 50-70°C, followed by exposure for 1 to 2 hours under stirring, and washing the obtained precipitate is carried out with ethyl alcohol based volume ratio 1 - 10÷11.

At the present time of patent and technical literature is not a method of obtaining oxide of scandium by dissolving scandium-containing concentrate sulfuric acid in the presence of ammonium chloride, is introduced into the solution in a certain amount and under certain conditions, obtained by washing the precipitate with ethyl alcohol in a certain volume ratios.

Experimentally, the authors found that when the pH of the solution 540-600 g/DM³H₂SO₄achieved saturation solubility of scandium and the introduction of a reagent containing both ions Cl^-andcreate the conditions causing almost complete precipitation of scandium with simultaneous separation from many metals impurities. At a low content of scandium is in the original concentrate (1-2,5 g/DM ³) when transforming a scandium in the sediment reached a low residual content of scandium in solution, which reduces the loss of scandium and increases the yield of the final product. This eliminates the need for the preliminary stages of concentration and getting richer concentrate on scandium (for example, by the method prototype content of scandium in the original concentrate is 38 wt.%). It was established experimentally that significant values are terms of the introduction of chloride of ammonium sulfate in the solution obtained by dissolution of the scandium-containing concentrate in sulfuric acid and then bringing the pH of the solution to 540-600 g/DM³. So, with the introduction of ammonium chloride less than 26.7 g/DM³an increase in losses of scandium with a solution, with the introduction of more of 53.5 g/DM³not observed a noticeable increase in recovery of scandium in the sediment. Lowering the temperature below 50°C leads to incomplete precipitation of the compounds of scandium in the sediment; the increase in temperature above 70°C is impractical as it does not affect the output of scandium. Reducing the exposure time of the solution with the reagent less than 1 hour also does not provide sufficient recovery of scandium from the solution. The increase in time more than 2 hours is also impractical, as it does not affect the output of scandium. Significant t what is the use for washing the obtained precipitate of ethyl alcohol. Thus, the magnification ratio is more than 1:11 unreasonably increases the flow rate of the reagent, does not improve the results in the output of scandium; when the reduction ratio less than 1:10 insufficient sediment washed from impurities and salts of scandium contaminated by impurities. Thus, the whole set of essential features of the proposed solution allows their use to obtain the final product - the scandium oxide of high purity and with minimal losses.

The proposed method can be implemented as follows. As the original take poor scandium concentrate obtained after processing by the carbonate leaching of red mud waste production in the processing of bauxite to alumina. Scandium-containing concentrate is dissolved in sulfuric acid with a concentration of 150-300 g/DM³for 4 hours at a temperature of 95±5°C. After removal of the acid-insoluble precipitate adjusting the sulfuric acid concentration in the filtrate to 540-600 g/DM³and at a temperature of 50-70°C. is introduced into a solution of ammonium chloride NH₄Cl in the number 26,7-53,5 g/DM³followed by exposure with stirring for 1-2 hours. Then incubated for another 24 hours without stirring and filtered. According to the chemical analysis of the obtained salt of scandium containing scandium to 20 wt.%. The precipitate is dried at a temperature of 11-120°C and calcined at a temperature of 800-850°C for at least 2 hours. According to x-ray phase and chemical analyses are trademark oxide of scandium Sc₂O₃purity 99,0%. The extraction of scandium is 97-98%. Loss of scandium does not exceed 2-4%.

The method allows for the separation of scandium from impurities in the solutions at the following ratios of concentrations as follows: Sc: (1-6) Ti: (0,5-2,5) Fe: 0,1-3,5) Zn: (5-13,5) Zr: (0,5-0,1) Ca: (0.1 to 0.5) Al: (0.01 to 0.3) Mg: (0,002-0,1) Th: (is 0.0002-0,008) U.

The proposed method is illustrated by the following examples.

Example 1. Take 50 g of scandium-containing concentrate composition, wt.%: Sc - 1,6; Ti - 5,3; Fe - 3,7; Zn and 0.3, Zr - 10,7; Na - 17,5; Ca - 4,2; Si - 1,4; Th - 3,5; U - 0,13; dissolved in 500 DM³sulfuric acid concentration of 300 g/DM³remove acid-insoluble precipitate and adjusting the sulfuric acid concentration in the filtrate to 540 g/DM³. The solution is injected 26.7 g NH₄Cl (53,5 g/DM³) at 50°C and maintained under stirring for 1 hour. Then incubated for 24 hours without stirring. The obtained precipitate was separated by filtration on a filter SCHOTT and washed with ethyl alcohol in a quantity of 50 ml (volume ratio of sediment: ethanol = 1:10). Then the precipitate is dried at 120°C for 10 hours to obtain a constant weight and calcined at 850°C for 2 hours. Get the scandium oxide purity 99,0% with a yield of 97.3%. Loss of scandium - 2,69%.

Example 2. Take 50 g of scandium-containing conc is the composition, wt.%: Sc - 1,6; Ti - 5,3; Fe - 3,7; Zn and 0.3, Zr - 10,7; Na - 17,5; Ca - 4,2; Si - 1,4; Th - 3,5; U - 0,13; dissolved in 500 DM³sulfuric acid concentration of 300 g/DM³remove acid-insoluble precipitate and adjusting the sulfuric acid concentration in the filtrate to 600 g/DM³. In the enter solution of 13.4 g of NH₄Cl (26.7 g/ DM³) at 70°C and maintained for 2 hours under stirring. Then incubated for 24 hours without stirring. The obtained precipitate was separated by filtration on a filter SCHOTT and washed with ethyl alcohol 55 ml (volume ratio of sediment: ethanol = 1:11). Then the precipitate is dried at 120°C for 12 hours and calcined at 800°C for 2 hours. Get the scandium oxide purity 99,0% with a yield of 97.8%. Loss of scandium amount of 2.16%.

Example 3. Take 50 g of scandium-containing concentrate composition, wt.%: Sc - 1,96; Ti - 2,85; Fe - 1,42; Zn - of 6.71; Zr - 18,13; Na - 17,7; Ca - 0,4; Si - 1,1; Th - 0,17; U - 0,015; dissolved in 500 DM³sulfuric acid concentration of 300 g/DM³remove acid-insoluble precipitate and adjusting the sulfuric acid concentration in the filtrate to 600 g/DM³. The solution is injected 26.7 g NH₄Cl (53,5 g/DM³) at 50°C and maintained for 2 hours under stirring. Then incubated for 24 hours without stirring. The obtained precipitate was separated by filtration on a filter SCHOTT and washed with ethyl alcohol is m 55 ml (volume ratio of sediment: ethanol = 1:10). Then the precipitate is dried at 120°C for 12 hours and calcined at 800°C for 2 hours. Get the scandium oxide purity 99,0% with a yield of 97.8%. Loss of scandium amount to 2.2%.

Thus, the authors propose a technically simple method of obtaining a trademark of scandium oxide of high purity 99,0% with the yield up to 97-98% of the poor scandium concentrate obtained after processing by the carbonate leaching of red mud waste production in the processing of bauxite to alumina.

The method of producing oxide of scandium, including the dissolution of scandium-containing concentrate sulfuric acid, removing the acid-insoluble precipitate, the translation of scandium in the sediment in the presence of ammonium compounds, filtering, washing, drying and calcination to obtain a precipitate of oxide of scandium, characterized in that after removal of the acid-insoluble precipitate the sulfuric acid concentration in the filtrate is brought to 540-600 g/DM³as ammonium compounds using ammonium chloride, is introduced into the solution in the amount 26,7-53,5 g/DM³at a temperature of 50-70°C, followed by exposure for 1-2 h under stirring, and washing the obtained precipitate is carried out with ethyl alcohol in a volume ratio of 1 - 10÷11.