Extraction method of beryllium from beryllium-bearing spodumene concentrate

FIELD: metallurgy.

SUBSTANCE: invention relates to metallurgy, particularly to extraction method of beryllium from beryllium -bearing spodumene concentrate. Method includes hydrometallurgical treatment of the concentrate with receiving of lithium carbonate, alum-sodium alums and beryllium-bearing filter cakes. Filter cakes are treated with receiving of rough beryllium hydroxide and it is received from it pure beryllium hydroxide. Additionally rough beryllium hydroxide is transferred into main beryllium carbonate by leaching of ammonium carbonate solution, taken from the calculation 29-35 g of ammonium carbonate per 1 g of beryllium, with formation of solution of ammonium-beryllium carbonate and insoluble residue. It is separated solution of ammonium-beryllium carbonate from the rest. Solution is subject to decomposition by boiling with formation of insoluble basic beryllium carbonate. It is separated from the mother solution and it is received from it pure beryllium hydroxide.

EFFECT: receiving of commercially pure beryllium hydroxide .

1 tbl, 1 ex

 

The invention relates to metallurgy, in particular to the processing bewildering spodumene concentrate.

One of the main industrial sources of beryllium is the mineral beryl [Ve3Al2(SiO3)6]concentrate which is processed by sulphate or fluoride technologies [Chemistry and technology of rare and scattered elements. 2 so, Ed. Khasbulatov. - Volume 2: Technology of rare and scattered elements. - M.: Higher school, 1969. - P.113, 117-126]. Due to the close Association of beryllium and lithium lithium ores flotation always contain an admixture of beryllium [Chemistry and technology of rare and scattered elements. 2 so, Ed. Khasbulatov. - Volume 2: Technology of rare and scattered elements. - M.: Higher school, 1969. - P.16-19, 115-116; Moskovich MM Mineral resources, the production and consumption of beryllium, lithium, niobium and tantalum in the capitalist countries. - M.: Nedra, Moscow (1966). - S-93, 89, 122-159]. So, the content of beryl in the flotation concentrate spodumene

[LiAl(Si2O6)] may be of 0.13 wt.% (in terms of beryllium) when the lithium content in the specified concentrate about 3 wt.%. Spodumene concentrates, traditionally processed on technical compounds of lithium [Chemistry and technology of rare and scattered elements. 2 so, Ed. Khasbulatov. - Volume 2: Technology of rare and scattered elements. - M.: High the second school, 1969. - P.29-34], with increased content of beryllium in these concentrates can also be considered as an industrial source of beryllium. Although barillari spodumene concentrate is characterized by a relatively low content of beryllium (0.13 wt.%), he is a promising source of beryllium, because the consumption of lithium in tens times higher than the consumption of beryllium, and complex processing of this material on technical compounds of lithium and beryllium becomes possible along with lithium to extract large amounts of beryllium.

The method for extracting beryllium from bewildering spodumene concentrate [Samoilov V. & Kulenova N.A. Functional distribution of beryllium in sulfuric acid production of lithium carbonate from spodumene concentrates Tsvet. - M., 2007. No. 8. - 74-77], taken as the analog and providing preliminary decrepitude roasting of the concentrate, which leads to the formation of easily breakable sulfuric acid spodumene with the transfer of lithium in water-soluble sulfate. Decrepitude roasting of the concentrate practically does not change the crystal lattice of beryl. Therefore, in the method-analogue can separate the beryllium from lithium on stage acid leaching descriptionmanage concentrate, in which lithium izvlekaete is in sulphate solution, while beryllium at ~88 wt.% remains in the insoluble cake. Forth from the cake by selective grinding and classification allocate a large fraction representing low-grade beryl concentrate containing beryllium 0,41.1 wt.%. Received beryl concentrate processed by fluoride technology involving the sintering of the concentrate with sodium silicofluoride to extract beryllium in water-soluble forbairt sodium. After leaching SPECA water the resulting solution of Forbearance sodium is treated with caustic soda solution with precipitation of beryllium hydroxide. While Al and other impurities coming from concentrate in a solution of Forbearance sodium remain in the mother solution, which is separated from the precipitated hydroxide of beryllium filter.

The lithium sulfate solution from the stage acid leaching descriptionmanage bewildering spodumene concentrate processed in the framework of classical sulfuric acid technology with obtaining lithium carbonate. The processing solution includes cleansing it of impurities (aluminum, iron, magnesium, calcium) and evaporation. Impurities are precipitated from the solution in cleaning residues form in the form of hydroxides of aluminum, iron, magnesium and calcium carbonate. Cake cleanup is separated from the solution of lithium sulfate by filtration. Beryllium, PE is esedi in a solution of sulphate of lithium bewildering spodumene concentrate, also precipitates cake purification in the form of a hydroxide of beryllium extraction ~90 wt.%. From refined and one stripped off solution of lithium sulfate and soda ash precipitated less soluble lithium carbonate, which is separated from the mother liquor by filtration.

Thus, when processing bewildering spodumene of concentrate to produce lithium carbonate by the method similar only ~12 wt.% contained in concentrate beryllium is extracted in cyclotourisme cake cleanup sulfate solution. The remaining ~88% of beryllium are derived from the lithium process in the form of a chemically inert with beryl cecom pulp leaching descriptionmanage bewildering spodumene concentrate. To highlight beryl concentrate of cake leaching and subsequent receipt of the concentrate of beryllium hydroxide is required to use an expensive, multi-stage technology, due to the low content of beryllium in the cake, chemical inertness beryl.

The disadvantage of this method is analogue processing bewildering spodumene concentrate on Li2CO3low extraction of beryllium from concentrate in cyclotourisme residues form a cleaning solution of lithium sulfate (~12 wt.%).

The closest set of features of the claimed invention is a method of extracting beryl the Oia from bewildering spodumene concentrate [Samoilov V. Hydrometallurgical processing literarilly concentrates with a low content of beryllium. // Chemical technology. - M., 2006. No. 10. - P.32-36]is adopted for the prototype and including activating the preparation of the concentrate (its melting soda ash, water granulation of the melt, grinding granules), sulfuric acid leaching of the activated concentrate, separating the pulp leaching in waste silica cake and the solution of the sulfates of lithium, beryllium, aluminum, sodium and impurities, subsequent chemical processing sulphate solution with obtaining lithium carbonate, aumontzey alum and beryllium-containing Chekov cleaning solution from impurities. Chemical processing sulphate solution by the method prototype includes evaporation and subsequent cooling crystallization aumontzey alum, which is separated from the sulphate solution by filtration. After separation of the alum solution is neutralized with caustic soda to a pH of~7 for the removal of beryllium, aluminum and iron, which precipitated cake purification in the form of hydroxides and then sulfate was filtered from the solution. Next, the neutralized solution is further treated with caustic soda to precipitate magnesium and residual beryllium in the form of hydroxides at pH=1214, is then treated with a small amount of soda ash for USAID the deposits of calcium in the form of carbonate. At the final stage of purification sulfate solution deposited from him KEK cleaning (a mixture of hydroxides of beryllium, magnesium and calcium carbonate is filtered off. The purified solution is neutralized with sulfuric acid to pH~7, then from his soda ash precipitated less soluble lithium carbonate, which is filtered off and subjected to the filter repulations leaching by water. Beryllium-containing residues form process producing crude hydroxide of beryllium. To this end, the cake is dissolved in sulfuric acid solution by boiling with getting saturated with sulphate of aluminium, iron and magnesium beryllium-containing solution is mixed with gypsum. The solution is filtered from the plaster, then neutralized with caustic soda to pH~1 and is cooled by performing crystallization aumontzey alum. Next alum sulfate is separated from the solution by filtration. The filtered solution is neutralized with caustic soda to pH~7, precipitating draft beryllium hydroxide which is separated from the magnesium-containing mother liquor by filtration. Draft beryllium hydroxide, obtained by the method prototype is heavily contaminated by aluminum and iron hydroxides and therefore contains only about 0.5 wt.% beryllium, which is a much lower content of beryllium in draft hydroxide obtained in hydrometallurgy of beryllium from beryl concentrate the content of the m beryllium ~2 wt.%. Classic clean draft of beryllium hydroxide produced from beryl concentrate, it includes cleansing hydroxide from aluminum with sodium hydroxide solution and subsequent washing of the hydroxide of iron sulfuric acid solution [Samoilov Century. And., Borsuk A.N. Methods of joint processing of bertrandite, beryl, phenakite and in hydrometallurgy beryllium. - Ust-Kamenogorsk: Media Alliance, 2006. - P.12-17, 25-29] and allows to obtain beryllium hydroxide containing beryllium at least 18 wt.% However, the use of a specified treatment technology draft hydroxide of beryllium in the method-prototype allows to increase the content of beryllium in it with ~0.5 wt.% only up to 13 wt.%, i.e. to obtain a hydroxide of low quality.

Prototype method allows us to extract from the raw material mixture bewildering spodumene concentrate with soda more than 90 wt.% beryllium and almost entirely lithium, aluminum, and sodium. However, processing obtained by the method prototype beryllium-containing Chekov gives beryllium hydroxide with low content of beryllium (not more than 13 wt.%), what is the disadvantage of the prototype method.

The task, which is aimed by the invention, selection of the conditions for the extraction of beryllium from bewildering spodumene concentrate, allowing to obtain a technically clean Be(OH)2.

The essence of the claimed socobespechenija beryllium from bewildering spodumene concentrate is in contrast to the known method of the prototype, including hydrometallurgical processing of concentrate to produce lithium carbonate, aumontzey alum and beryllium-containing Chekov, processing Chekov producing crude hydroxide beryllium, obtaining pure beryllium hydroxide, according to the present method roughing beryllium hydroxide is transferred to the basic beryllium carbonate leaching solution of ammonium carbonate, is taken 2935 g of ammonium carbonate per 1 g of beryllium, with formation of a solution ammonialike carbonate and insoluble residue, separating the solution ammonialike carbonate from the residue and subsequent decomposition of the solution ammonialike carbonate it by boiling with formation of insoluble basic beryllium carbonate, which is separated from the mother liquor and receive from it the pure beryllium hydroxide.

Problem solving and the achievement of relevant technical results achieved by the fact that in the inventive method, beryllium hydroxide, present in beryllium-containing cakes in the amount of ~0.5 wt.% (beryllium), selectively dissolved in a solution of ammonium carbonate does not dissolve aluminum and iron hydroxides. Formed during leaching Chekov solution ammonialike carbonate is separated from nearest Oronogo balance. Subsequent decomposition of the solution ammonialike carbonate receive insoluble carbonate basic beryllium content of beryllium at least 10 wt.%. Cleaning is separated from the mother liquor of the basic beryllium carbonate by the present method performed by the classical technology of purification of the crude beryllium hydroxide obtained from beryl concentrate [Samoilov V., Borsuk A.N. Methods of joint processing of bertrandite, beryl, phenakite and in hydrometallurgy beryllium. - Ust-Kamenogorsk: Media Alliance, 2006. - P.12-17,

25-29]. The treatment of the basic beryllium carbonate receive beryllium hydroxide containing beryllium at least 20 wt.%.

An example of the method.

The method is carried out in conventional equipment using bewildering spodumene concentrate containing beryllium, lithium, aluminum and iron of 0.13 wt.%, to 2.85 wt.%, 15,30 wt.% and 0.41 wt.% respectively. For the implementation of the proposed method specified concentrate processed by the method prototype with obtaining lithium carbonate, aumontzey alum and beryllium-containing Chekov that process producing crude hydroxide of beryllium. Received draft beryllium hydroxide containing of 0.55 wt.% beryllium is used for implementing the inventive method. When implementing saleemul the way hinge draft hydroxide beryllium by weight of 2 g for beryllium treated with different amounts of a solution of carbonate of ammonia (conc. 300 g/l) and the resulting slurry is stirred 1 h at 5055C, leaching beryllium in solution ammonialike carbonate. Then the solution ammonialike carbonate is separated from the insoluble hydroxides of aluminum and iron by filtration and boiled for 1 h at 95100C, precipitating carbonate basic beryllium content of beryllium at the level of 10 wt.% Besieged basic beryllium carbonate is separated from the mother liquor by filtration and then dissolved in caustic soda solution (conc. 620 g/l) for separation of beryllium from aluminum. In the specified caustic soda solution, is taken as 78 g (NaOH) per 1 g of beryllium in the main carbonate, beryllium, download basic beryllium carbonate and 1.01.5 h at ~120C. under these conditions, the basic beryllium carbonate and mixture of aluminum hydroxide are dissolved with the formation of a solution of beryllate sodium and sodium aluminate. For the most complete dissolution of aluminum hydroxide obtained alkaline solution is boiled for a further 1 h (while maintaining the achieved volume of distilled water and stirring), then diluted with distilled water until the content of free NaOH in the solution of ~20 g/l When diluted hydrolysis beryllate sodium hydroxide precipitation of beryllium and aluminum remains in solution in the form of sodium aluminate. To ensure the most complete selection of beryllium hydroxide race the thief obtained after dilution of the alkaline solution to the slurry of the hydroxide of beryllium boiled for 1 h and then filtered, separating beryllium hydroxide from sodium aluminate solution. Filtered alkaline hydroxide beryllium Rasulova in sulfuric acid (conc. 70 g/l), taken from a rate of 60 ml per 1 g of beryllium in alkaline hydroxide of beryllium, for 1 h at 25C. under these conditions is virtually complete dissolution of impurities of iron hydroxide, beryllium hydroxide dissolves to a small extent. Next beryllium hydroxide is filtered from the solution of ferric sulfate, and then subjected to 2-fold filter repulations leaching from the sulfate-ion battery with distilled water. Each rinse should be performed within 15 min at 25C and water flow rate of 75 ml per 1 g of beryllium to wash the hydroxide. The washed hydroxide beryllium analyze the content of beryllium.

For comparison with the inventive method provide hydrometallurgical processing of the above bewildering spodumene concentrate on the method prototype with obtaining lithium carbonate, aumontzey alum and beryllium-containing Chekov that process producing crude hydroxide beryllium containing of 0.55 wt.% beryllium. In the implementation of the prototype method perform dissolution sample draft hydroxide beryllium by weight of 2 g for beryllium in caustic soda solution (conc. 620 g/l) for separation of beryllium from aluminium the Oia. In the specified caustic soda solution, is taken as 1723 g (NaOH) per 1 g of beryllium in draft hydroxide beryllium, download rough beryllium hydroxide and 1.01.5 h at ~120C. To fully dissolve the aluminum hydroxide obtained alkaline solution is boiled for a further 1 h (while maintaining the achieved volume of distilled water and stirring), then diluted with distilled water until the content of free NaOH in the solution of ~20 g/l To ensure the most complete selection of beryllium hydroxide obtained after dilution of the alkaline solution to the slurry of the hydroxide of beryllium boiled for 1 h and then filtered separating beryllium hydroxide from the mother liquor of sodium aluminate. The prototype method is characterized by a noticeably large number of beryllium remaining in the mother solution, compared with the inventive method, since the method-prototype obtained a much larger volume of a specified stock solution than in the claimed method. This is because the basic beryllium carbonate obtained by the present method, contains significantly less aluminum, and cleaning basic beryllium carbonate is not required to spend large quantities of caustic soda, as it must be done in the method-prototype cleanup from aluminum draft hydroxide beryllium (see above). Filtered method-proto is the IPA alkaline hydroxide beryllium Rasulova in sulfuric acid (conc. 70 g/l), taken at the rate of 75 ml per 1 g of beryllium in alkaline hydroxide of beryllium, for 1 h at 25C. Next, beryllium hydroxide is filtered off from the acidic stock solution of ferric sulfate, and then subjected to 2-fold filter repulations leaching from the sulfate-ion battery with distilled water. Each rinse should be performed within 15 min at 25C and water flow rate of 75 ml per 1 g of beryllium to wash the hydroxide. The washed hydroxide beryllium analyze the content of beryllium. The prototype method is characterized by a noticeably large number of beryllium remaining in the acidic mother solution, compared with the inventive method, since the method-prototype obtained significantly large amounts specified the mother liquor than in the claimed method. This is because the basic beryllium carbonate produced in the present method contains much less iron and washing of iron derived from the basic beryllium carbonate of alkali hydroxide of beryllium, is not required to spend large amounts of sulfuric acid solution, as it must be done in the method-prototype cleanup from rough iron hydroxide beryllium (see above).

The table shows the results of the implementation of the proposed method and, for comparison, the prototype method.

Comparative results of the proposed method and the prototype method.
# exampleMethod of implementationConsumption (NH4)2CO3on the dissolution of the draft Be(OH)2, g/g Be the Be(OH)2Content Be cleaned, Be(OH)2Direct access Be from rough
Be(OH)2to Be cleaned(OH)2, % [Be purified(OH)2]
gwt.%
1The inventive method251,4020,570
2291,6020,580
3351,7020,085
4391,7018,085
5JV the property-placeholder -1,7011,085
6-1,6013,080
7-1,66to 12.083
Note: initial draft Be(OH)2cleaning from impurities in examples 1-7 is 2 g in terms of beryllium.

From the table it follows that when cleaning rough hydroxides of beryllium by the present method (examples 2 and 3) content of beryllium treated hydroxides of beryllium is 20,0to 20.5 wt.%. This direct access beryllium from rough hydroxide in purified beryllium hydroxide is 8085%.

For comparison, when cleaning rough hydroxides of beryllium by the method prototype peeled hydroxides of beryllium are characterized by low quality, as they contain not more than 13 wt.% beryllium (table, examples 5-7), and direct access beryllium from rough beryllium hydroxide in purified beryllium hydroxide in the method prototype, as well as in the claimed method, is 8085%. Although in the present method a to icesto beryllium remains in the insoluble residue after dissolution draft hydroxide in a solution of ammonium carbonate, the inventive method is characterized by a significantly smaller residual amount of beryllium in the mother solution after cleaning basic beryllium carbonate from aluminum and iron, than remain in said mother solution in the processing of draft hydroxide of beryllium by the method prototype (see above). Therefore, the inventive method unlike the prototype method allows us to extract from draft hydroxide in purified beryllium hydroxide same amount of beryllium 8085%. If in the inventive method, the consumption of ammonium carbonate dissolution draft hydroxide of beryllium above the stated limit (35 g per 1 g of beryllium in its hydroxide), in the process of dissolution draft hydroxide beryllium increases the transition of impurities in the resulting solution ammonialike carbonate, which ultimately reduces the content of beryllium hydroxide in purified beryllium to 18 wt.% (PL., example 4). At a flow rate of ammonium carbonate dissolution draft hydroxide of beryllium below the stated limit (29 g per 1 g of beryllium in its hydroxide), the content of beryllium hydroxide in purified is not increased, but direct access beryllium from rough beryllium hydroxide in purified beryllium hydroxide is significantly reduced from 80% to 70% (table, example 1), because not enough of a solution of carbonate of ammonia (conc. 300 g/l) for a more complete pixelation what I beryllium in solution ammonialike carbonate.

Thus, the inventive method makes it possible to extract from bewildering spodumene concentrate in technically pure compounds not only lithium and aluminum, and beryllium.

The method of extracting beryllium from bewildering spodumene concentrate, including hydrometallurgical processing of concentrate to produce lithium carbonate, aumontzey alum and beryllium-containing Chekov, processing Chekov producing crude hydroxide beryllium, obtaining pure beryllium hydroxide, characterized in that draft beryllium hydroxide is transferred to the basic beryllium carbonate leaching solution of ammonium carbonate, taken 29-35 g of ammonium carbonate per 1 g of beryllium, with formation of a solution ammonialike carbonate and insoluble residue, separating the solution ammonialike carbonate from the residue and subsequent decomposition of the solution ammonialike carbonate it by boiling with formation of insoluble basic beryllium carbonate, which is separated from the mother liquor and receive from it the pure beryllium hydroxide.



 

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1 tbl, 1 ex

FIELD: metallurgy.

SUBSTANCE: lithium extraction method includes batch preparation from the mixture of concentrates and flux, activating batch preparation and water leaching of activated batch. Additionally batch preparation is implemented from the mixture of lepidolite and spodumene concentrates per receiving mass ratio SiO2/(Na2O+K2O+Li2O) in mixture, equal to 4.5, and flux in the form of lithium carbonate per receiving of mass ratio SiO2/(Na2O+K2O+Li2O) in batch, equal to 2.3. Activating batch preparation is implemented by means of its melting at the temperature 1350C, melt granulations by water, granulated melt crushing. Water leaching of activated batch is implemented while sulfuric acid presence.

EFFECT: receiving of relative clean by sodium lithium sulphate solutions, ability of lithium deep extraction from mentioned solutions into lithium carbonate.

3 tbl, 1 ex

FIELD: metallurgy.

SUBSTANCE: method includes concentrate activation, its sulphation and leaching with extraction of aluminium sulfates and lithium into sulphate solution. From sulphate solution it is implemented deposition lithiumaluminiumbearing sediment. Before it sulphate solution is treated by caustic soda solution with deposition mixture of aluminium hydroxide and admixtures at pH=7.58.0, mixture is separated from sulphate solution. From separated of mixture solution it is deposited lithiumaluminiumbearing sediment in the form of lithium hydrox-di- aluminate by solution of sodium aluminate and caustic soda, prepared by means of dissolution of technological aluminium hydroxide and precipitated from sulfate solution mixture of aluminium hydroxide and admixtures in solution of caustic soda, with following separation of received solution of sodium aluminate and caustic soda from insolubles. Deposited lithium hydrox-di-aluminate is tempered at temperature 400450C with forming of stripped lithium-bearing alumina with increased content of lithium.

EFFECT: receiving of lithium-bearing alumina with increased content of lithium and low content of iron and silicon.

1 ex, 2 tbl

FIELD: metallurgy.

SUBSTANCE: method includes causticisation of lithium carbonate by slaked lime with receiving of lithium hydroxide solution and insoluble calcium carbonate. After separating of lithium hydroxide solution from calcium carbonate it is implemented evaporation of lithium hydroxide solution, crystallisation of rough monohydrate of lithium hydroxide from evaporated solution, separation of rough monohydrate of lithium hydroxide from growth solution. Additionally lithium hydroxide solution from the stage of causticisation is evaporated per 8590% volume. Growth solution after crystallisation of rough monohydrate of lithium hydroxide is evaporated and from it there is crystallised technical monohydrate of lithium hydroxide. Technical monohydrate of lithium hydroxide is separated from growth solution, which is evaporated in closed loop in common to growth solution from the stage of crystallisation of rough monohydrate of lithium hydroxide.

EFFECT: reduction of volume of rough monohydrate of lithium hydroxide, requiring recrystallisation, and reduction on this basis expenditures for recrystallisation.

1 tbl, 1 ex

FIELD: metallurgy.

SUBSTANCE: invention refers to method of processing spodumene concentrates. The purpose of the suggested invention is development of such method of processing spodumene concentrate. The method consists in activation of the concentrate by means of melting with lithium carbonate taken on consideration of obtaining weight ratio SiO2/(Li2O+Na2O) in charge equal to 2.7-3.0. After activation there is performed sulphuric acid leaching of activated material.

EFFECT: production of sodium pure solutions of lithium sulphate further allowing deep extraction of lithium out of said solutions into lithium carbonate.

2 tbl

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