A method of producing niobium pentoxide

 

(57) Abstract:

The invention relates to the field of hydrometallurgical processing of tantalum raw materials and are aimed at achieving its comprehensive use. For purification of niobium from impurities niobium raffinate after extraction of tantalum tributylphosphate partially neutralize the formed hydroxide dissolved in subsequent portions of the raffinate, acidified with his hydrofluoric and sulfuric acid to obtain a solution with a content of Nb ~ 60 g/l, HF ~ 70 g/l, N2SO4350-400 g/L. Then by extraction of niobium in 5 counter-current stages with a: = 0,7:1 and extraction in 3 counter-current stages at A:B = 1:0.7 to obtain a purified solution of niobium. From the solution obtained in the usual method of getting the niobium pentoxide Ferroalloy varieties. The technical result is to obtain a niobium pentoxide in the form of a commodity product as a result of processing the unstable composition of columbite-tantalite concentrates. 1 C.p. f-crystals, 1 table.

The proposed method of producing niobium pentoxide is used in the field of hydrometallurgical processing of tantalum raw materials and aims to achieve its comprehensive use.

The known method [1] get the Penta the elements, carried out from solutions of fluorides of tantalum and niobium, resulting decomposition tantalite (kolombatovich) concentrates. Solutions containing hydrofluoric acid and sulphuric acid. In the known method extraction separation of tantalum and niobium is carried out in four stages:

1. Joint extraction of tantalum and niobium for separation of impurities from solutions with a concentration of HF 5-8 mol/l and H2SO44-5 mol/L.

2. Election reextracted niobium from an extract of water.

3. Reextracted tantalum aqueous solutions of salts, such as ammonium fluoride.

4. From reextractors precipitated by adding ammonia solution pure hydrated oxides of niobium and tantalum.

The content of these impurities is not hundredths of a percent [1]. However, when processing the African columbite-tantalite concentrates with unstable initial composition and containing large amounts of impurities, the method of separation of tantalum and niobium and obtain a niobium pentoxide is insufficient. Niobium raffinate obtained after separation of tantalum and niobium in the processing of these concentrates, depending on the feedstock composition, poluchaetsya used to not be.

The technical result of the invention is to provide a niobium pentoxide in the form of a commercial product of the collective reextract obtained by processing the unstable composition of columbite-tantalite concentrates.

The technical result is achieved by a method of producing niobium pentoxide of tantalum - and niobium-containing solution obtained in the processing of tantalum mineral concentrates, including selective extraction of tantalum tributylphosphate obtaining niobium of the raffinate and reextraction tantalum solution of ammonium fluoride, according to the invention obtained niobium raffinate partially neutralize the ammonia water, the formed hydroxide dissolved in subsequent portions of the raffinate, acidified with his hydrofluoric and sulphuric acids to obtain solutions with a content of niobium to about 60 g/l, hydrofluoric acid 70 g/l and sulfuric acid 350-400 g/l and by extraction of niobium in 5 counter-current stages with a ratio A:B = 0,7:1 and Stripping in 3 counter-current stages with a ratio A:B = 1:0.7 to obtain a purified solution of niobium, of which the niobium pentoxide Ferroalloy varieties.

The extraction of niobium are in the presence of povyshen the economic effect can be obtained on the following parameters:

- reduction requirements concentrates on the content of tantalum and the ratio of Nb to TA and, as a consequence, the expansion of raw materials and production.

the cost of tantalum raw materials.

An example of the method.

The process was tested using three extraction pulse columns - 400 mm, h - 5 PM the First two columns with intermediate collecting and pumping the aqueous phase was carried out in 5 counter-current stages of extraction, third in 3 stages of Stripping. The process is as follows. Nb-phase with a content of niobium is less than 30 g/l is injected into the reactor precipitator and when mixed with ammonia water precipitated hydroxide niobium. After cooling below 60C the slurry is filtered on a filter press, sludge is collected in a container and store. Then it is used to increase the concentration of niobium in the subsequent portions of the NB phase by dissolving it together with the introduction of hydrofluoric acid, if necessary. In this step you create the concentration Nb of about 75 g/l and HF ~ 100 g/l After the introduction of the sulfuric acid solution is based 350-400 g/l get a solution with a concentration of Nb ~ 60 g/l and HF ~ 70 g/L. This solution at the rate of 400 l/h is fed to the head of the second column. At the bottom of this colonnade in the upper zone of the first column. In the bottom of the column first serves pure TBP. From the top of the second column, the extract is fed to the column 3 on reextraction. The correlation of phases remain as above. The following results are obtained by purification from impurities (see table). Received an experimental batch of niobium pentoxide, which are used for the production of ferroniobium brands NBF-2, NBUF-1, which became commercial products.

The source of information

A. N. Zelikman, B., Kites. Metallurgy of rare metals. M.: metallurgy, 1986, S. 253.

1. A method of producing niobium pentoxide of tantalum - and niobium-containing solution obtained in the processing of tantalum mineral concentrates, including selective extraction of tantalum tributylphosphate obtaining niobium of the raffinate and reextraction tantalum solution of ammonium fluoride, characterized in that the obtained niobium raffinate partially neutralize the ammonia water, the formed hydroxide dissolved in subsequent portions of the raffinate, acidified with his hydrofluoric and sulphuric acids to obtain solutions with a content of niobium to about 60 g/l, hydrofluoric acid 70 g/l and sulfuric acid 350-400 g/l and by extraction of niobium in 5 counter-current stages with a ratio A:B = get showing the niobium pentoxide Ferroalloy varieties.

2. The method according to p. 1, characterized in that the extraction of niobium are in the presence of high content RHO3-4ions from 2 to 8%.

 

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