Method of a loparite concentrate processing

FIELD: hydrometallurgy; ore concentrates processing.

SUBSTANCE: the invention is pertaining to the field of hydrometallurgy, in particular, to processing of the loparite concentrate. The method includes a decomposing of the loparite concentrate at the temperatures of 103-105°C and the concentration of hydrofluoric acid of 38-42 mass % with production of the pulp containing fluorides of titanium, rare earth elements (REE), niobium, tantalum and sodium. The pulp is filtered at the temperature of 90-95°C with extraction into the fluorotitanium solution of fluorides of niobium and tantalum and no less than 58 % of sodium in terms ofNa2O and separation of the sediment containing fluorides of rare earth elements (REE) and a residual sodium. The produced solution is cooled down to 18-24°C with separation of the second sediment of sodium fluorotitanate. After that they extract niobium and a tantalum from the solution by octanol-1 extraction at a ratio of the organic and water phases as 1.1 : 1. The sediment of REE fluorides is washed from fluorotitanate by sodium water in a single phase at the temperature of 90-95°C and at the solid :liquid ratio = 1:2-2.5. The cleansing solution is separated and evaporated with extraction of the additional sediment of sodium fluorotitanate. After extraction of niobium and tantalum the fluorotitanium solution is evaporated and filtered with separation of the first sediment of sodium fluorotitanate from the concentrated solution of fluorotitanium acid, which is directed to extraction of titanium. The gained first, second and additional sediments of sodium fluorotitanate are combined and subjected to conversion with production of sodium fluorosilicate and the conversional fluorotitanium acid added to fluorotitanium solution before its evaporation. The technical result of the invention is a decrease in 2.0-2.5 times of the volume of the cleansing solutions at provision of a high degree of extraction of compounds of titanium and other target products. The produced sodium fluorotitanate contains the decreased amount of the impurity ingredients of calcium and strontium.

EFFECT: the invention ensures a decrease in two-two and a half times of the volume of the used cleansing solutions at provision of a high degree of extraction of compounds of titanium and other target products and a decreased amount of impurities of calcium and strontium in the sodium fluorotitanate.

7 cl, 1 dwg, 1 tbl, 3 ex

 

The invention relates to the hydrometallurgical processing of ore concentrates, in particular to the processing of loparite concentrate, and can be used in complex extraction of compounds of titanium, niobium, tantalum and rare earth elements.

When hydroporinae processing of loparite relatively high (95-97%) extraction of rare earth elements (REE), niobium and tantalum through the extraction of titanium is about 70% of the original. This is because in loparite is 8-9 wt.% sodium oxide. When interacting loparite with hydrofluoric acid sodium binds about 10% titanium in the form of formetanate sodium (Na2TiF6), which accounts for 25-30% of the initial content in loparite. Using formetanate sodium to extract titanium is a multistage process. The formation of large amounts of washing solutions, subject to evaporation, which is costly and is associated with significant energy consumption. In addition, a disposable pertitent sodium should contain the minimum number of impurity components of calcium and strontium for further efficient processing in titanium dioxide.

There is a method of processing of loparite concentrate (see Perkowski S.A. Hydroporinae technology extraction of rare meta is fishing from loparite // Rare metals and powder metallurgy: proc. Dokl. at the all-Russian scientific-practical use. Conf., Moscow, December 3-5, 2001 - P.7-9.), including the decomposition of loparite concentrate 20-40%hydrofluoric acid at T:W=1:2.5 to 5 for 2-4 hours with the formation of the slurry, separating the solid phase of the slurry to obtain a precipitate fluoride REE and solution of fluorides of titanium, niobium, tantalum and sodium, conversion of sediment fluoride by pyrohydrolysis in oxides with the regeneration of hydrofluoric acid, sorption selective extraction of tantalum (99,5%) and niobium (96-98%) of the fluoride solution by anion-exchangers and thermal hydrolysis solution fortechnology acid (H2TiF6with regeneration fluoride-hydrogen acid (99%) and yield commercial titanium dioxide.

The disadvantages of this method are large losses of titanium in the form of soluble salts formetanate Na2TiF6comprising about 29% of TiO2from his confinement in the loparite, as well as large volumes of dilute condensate HF obtained by thermal hydrolysis of H2TiF6.

There is also known a method for processing of loparite concentrate (see Sklarin LI, Muzhdabaeva M.A. and thunders PB Receiving group concentrates at hydroporinae processing of loparite // Materials of international scientific-technology. Conf., "Science and education - 2004" .IV, Murmansk, 7-15 April 2004 - P.66-67), which is performed once agenie loparite concentrate hydrofluoric acid with a concentration of 420-560 g/l (38-50 wt.%) with respect to T:W=1:3-3,5 and the process temperature of 80-100° With obtaining slurry containing fluorides of titanium, REE, niobium, tantalum and sodium. The degree of decomposition of the concentrate is 98-99%. The resulting slurry is cooled to 40°and extract from it the sum of niobium and tantalum by extraction with tributyl phosphate at a ratio of organic and aqueous phase is 1:2. The pulp defend and separated by decantation of the organic phase containing niobium and tantalum. Then filter pulp with sludge separation of REE fluorides containing about 70% of formetanate sodium, from fortimanager solution containing about 30% of formetanate sodium. The precipitate fluoride REE washed from formetanate sodium hot water in two stages. In the first stage washing are repulpable for 30 minutes at T:W=1:3, and the second filter with TJ=1:3. Obtained after washing and drying the precipitate fluoride REE contains 50-54% Ln2About3; 28% F. Washing solutions are combined and evaporated with sedimentation of formetanate sodium. Portianoy the solution has evaporated (in conjunction with the conversion fortechnology acid) with crystallization of the corresponding sludge formetanate sodium, which is separated by filtration from the concentrated solution fortechnology acid used for extraction of titanium. The degree of transition of sodium in the sediment is 90-95% at concentration fortimanager solution to 3.5-5.5 M for H2TiFsub> 6. The obtained precipitation formetanate sodium subjected to conversion with getting fertilitate sodium and conversion fortechnology acid, directed by evaporation together with fortimanager solution. The duration of the conversion is 3-4 hours at a concentration of H2SiF6- 1.4 M and a temperature of 20°C. the Degree of conversion is 96-98,5%. Extraction of titanium, niobium, tantalum and rare earth metals in the received group concentrates is about 95%.

While providing a relatively high degree of extraction of titanium compounds and other target products known method is characterized by elevated amounts of parivesh solutions due to the large consumption of wash water at the two-stage washing the precipitate fluoride REE from formetanate sodium, which reduces the adaptability of the method and increases the content of impurity components of calcium and strontium in formetanate sodium. All this adversely affects the purity of the target product, mainly titanium. Evaporation of significant volumes of washing solutions increases the consumption of the method.

The present invention is directed to solving the problem of improving the processability of the method by reducing the volume parivesh solutions while ensuring a high degree of extraction of titanium compounds and other target products. And the finding also solves the problem of reducing the amount of impurity components of calcium and strontium in formetanate sodium.

The technical result is achieved in that in the method for processing of loparite concentrate, including the decay of his hydrofluoric acid when heated with obtaining a slurry containing the fluorides of titanium, REE, niobium, tantalum and sodium, collective extraction of niobium and tantalum extraction, filtering the slurry with sludge separation of REE fluorides and part of formetanate sodium from fortimanager solution containing part of formetanate sodium, evaporation and filtration fortimanager solution separating the first precipitate of formetanate sodium from the concentrated solution fortechnology acid, which is directed to the extraction of titanium, shaded REE fluorides from formetanate sodium water at elevated temperature with the Department of the leaching solution, its evaporation from the allocation of additional sludge formetanate sodium, which is attached to the first draft of formetanate sodium, conversion of the combined sludge formetanate sodium with getting fertilitate sodium and conversion fortechnology acid attached to fortechnology solution before evaporation, according to the invention the filtering of the slurry is carried out at an elevated temperature immediately after the decomposition of concentrate allocation in portianoy solution of fluoride, niobium and tantalum and the main part of formetanate on the matter, received portianoy the solution is cooled with the second compartment sludge formetanate sodium, which is attached to the joint draft of formetanate sodium and subjected to conversion, and extraction of niobium and tantalum extraction of lead from fortimanager solution after filtration of the slurry and separating the second precipitate of formetanate sodium.

The technical result is also achieved by the fact that the decomposition of lead concentrate at a temperature of 103-105°and the concentration of hydrofluoric acid 38-42 wt.%.

The technical result is also achieved by the fact that the filtering of the slurry is conducted at a temperature of 90-95°C.

The technical result is achieved by the fact that in portianoy solution allocate not less than 58% of the sodium in terms of Na2O content in loparite concentrate.

On the technical achievement of the aims that the shaded REE fluorides from formetanate sodium is carried out in one stage at T:W=1:2-2,5 and a temperature of 90-95°C.

On the achievement of the technical result is also aimed that portianoy the solution obtained by filtering the slurry, cooled to room temperature.

On the achievement of the technical result is also aimed that the extraction of niobium and tantalum are the octanol-1 with a ratio of organic and aqueous phases 1-1,1:1.

The essence of the claimed method Zack is udaetsya is the solubility of formetanate Na2TiF6in water at a temperature of 20°With 65 g/l and at a temperature of 100°S - 152 g/L. Therefore, the filtration of the pulp, which, along with fluorides of other metals present sodium as Na2TiF6at elevated temperature (90-95° (C) reduces the coprecipitation of formetanate sodium fluorides of rare-earth elements, CA and Sr. Most of Na2TiF6remains in fortimanager solution containing Nb and TA, which is then sent for extraction and evaporation, and a smaller part of Na2TiF6goes sludge together with fluorides of rare-earth elements, CA and Sr. In fortimanager the solution formed when implementing the method, the solubility of Na2TiF6slightly lower than in water due to vicalvaro of the complex ion TiF62-therefore , when the cooling fortimanager solution to room temperature pertitent Na2TiF6is released from the solution in the form of a crystalline salt. Thanks quantitative redistribution of connections Na2TiF6between the solution and the precipitate becomes possible to abandon the two-stage washing the precipitate fluoride REE, CA and Sr, as is the case in the prototype, to exclude the operation of repulpable the above precipitate fluoride to separate sodium as Na2Ti 6and accordingly to reduce the load on the evaporator apparatus, while maintaining a high degree of extraction of target components, in particular titanium. Reduction of water consumption for flushing of sediment fluoride REE, Na, Ca and Sr can reduce the presence in the wash water of impurity components such as calcium and strontium, limiting their subsequent transition into pertitent sodium in the process of evaporation.

Decomposition of loparite concentrate at a temperature of 103-105°and the concentration of hydrofluoric acid 38-42 wt.% promotes maximum recovery in the pulp of the fluorides of titanium, REE, niobium, tantalum and sodium and increased translation of titanium in solution in the subsequent filtration of the pulp.

Filtration of the pulp at high (90-95° (C) the temperature immediately after the decomposition of the concentrate connected with the direct dependence of the solubility of Na2TiF6from process temperature: the higher the temperature, the more salts of Na2TiF6remains in fortimanager solution. Filtering the slurry at a temperature of up to 95°provides the desired solubility of Na2TiF6and a further increase in temperature reduces the adaptability of the method. Filtering the slurry at a temperature of less than 90°is undesirable due to substantially reduce the solubility of Na2TiF6and increase soosai the value Na 2TiF6sediment fluoride REE.

Selection in portianoy the solution is not less than 58% of the sodium in terms of Na2O when filtering the pulp significantly (about 2 times) to reduce the amount of washing solutions coming to evaporation.

Cooling fortimanager of the solution obtained by filtering the slurry to room temperature allows you to maximize the highlight of fortimanager solution pertitent sodium in the form of the second precipitate. Cooling fortimanager solution can be produced spontaneously in air or forced, depending on the conditions of the process.

Attaching the second sludge formetanate sodium to the United draught of formetanate sodium and the subsequent conversion of the total sediment Na2TiF6reduce the number of impurities of CA and Sr, coming in conversion fortechnology acid from the precipitate fluoride REE through the washing water.

Extraction of niobium and tantalum extraction from fortimanager solution after filtration of the slurry and separating the second precipitate of formetanate sodium reduces losses titanium compared with extraction of niobium and tantalum directly from the pulp.

The use of octanol-1 for collective extraction of niobium and tantalum is connected with its ability to extract these metals from fluoride environments in p is outstay H 2TiF6and its higher stability in the extraction process, compared with tributyl phosphate, and lower solubility in aqueous solutions. The absence of water-soluble impurities, in particular phosphorus, promotes purity of the products.

Carrying out the extraction at a ratio of organic and aqueous phases 1-1,1:1 contributes to a more complete extraction of niobium and tantalum in their collective extraction. The selection of the ratio of organic and aqueous phase due to the fact that if you increase the amount of organic phase is higher than the value of 1.1:1 increase in the percentage of sextrailers titanium, which is undesirable, and reducing the volume of the organic phase below the value of 1:1 leads to an increase in the number of stages of extraction.

Implementation of cleaning fluoride REE from formetanate sodium in one stage, due to the redistribution of formetanate sodium on stage filtration of the pulp, resulting in a precipitate fluoride REE extracted low (less than 42%) number of Na2TiF6. Washing REE fluorides at a temperature of 90-95°caused directly proportional dependence of solubility of formetanate sodium in water temperature.

The mass ratio of T:W=1:2-2,5 to ensure complete washing of the precipitate fluoride REE from sodium. At lower (less than 1:2) ratio decreases the efficiency of the process of washing. To increase the mass ratio greater than 1:2,5 adversely affects the processability of the way.

For a clearer understanding of the invention and additional evaluation of the special features on the accompanying drawing shows a schematic diagram of processing of loparite concentrate according to the invention.

The method is as follows. In a pre-heated up to 40°With hydrofluoric acid containing 38-42 wt.% HF download loparite concentrate. The heating is ceased. Due to the exothermic process of decomposition temperature of the reaction mass rises to 103-105°C. the Decomposition of loparite concentrate 1 occurs within 17-25 minutes including download time, concentrate and extract pulp. The resulting slurry of the metal fluoride filter 2 under vacuum at a temperature of 90-95°obtaining fortimanager solution containing fluoride Nb, TA, Na, and sediment fluoride REE, Na, Ca, Sr.

Portianoy the solution is cooled to room 3 temperature (18-24°). This crystallizes the most part dissolved Na, which is separated by the filter 4 in the form of the second sludge 5 Na2TiF6. Portianoy solution containing, g/l: 112,7-115 TiO2; 29,9-30,5 Nb2O5; 2,10-2,14 TA2O5; 315-320 HF and 7.8 to 8.0 Na2O directed to the extraction of niobium and tantalum 6, to the activities carried out by the octanol-1. The ratio of the volumes of organic and aqueous phases Vo:Vin=1-1,1:1. Extraction of niobium and tantalum in the organic phase for the 5-speed countercurrent extraction is in the amount of 99.5%. Reextraction of niobium and tantalum (not shown) from the organic phase is carried out by processing its water reextraction with translation in the reextract niobium and tantalum. The aqueous phase, representing a solution fortechnology acid, H2TiF6, is subjected to evaporation 7 (jointly with the conversion fortechnology acid) to the concentration of H2TiF65-5,5 M one stripped off the combined solution is filtered 8 obtaining concentrated fortechnology acid, H2TiF69, which is sent on the extraction 10 titanium, and the first draft 11 crystalline salts of Na2TiF6. In the sediment covering about 95% of Na2O.

The wet precipitate fluoride REE, Na, Ca, Sr washed 12 on the filter with hot water with a temperature of 90-95°when the mass ratio of T:W=1:2-2,5 with obtaining sediment 13 REE fluorides, which is then subjected to drying and processing into individual elements. The resulting leaching solution 14 evaporated 15 with the crystallization and separation of additional sediment 16 formetanate Na2TiF6. Additional sediment Na2TiF6combine the first 11 and second 5 precipitation of Na2TiF6

Na2TiF6+H2SiF6→Na2SiF6+H2TiF6

The reaction is carried out at a temperature of 20-25°C for 4 hours silicofluoride acid with a concentration of 1.4 M, taken in stoichiometric quantity. Solution conversion fortechnology acid, H2TiF618 attach to the aqueous phase obtained after the extraction of niobium and tantalum, with the formation of the joint solution is subjected to evaporation 7 and forcricket Na2SiF619 is used as a commercial product.

The above features and advantages of the invention may be more clearly explained by the following examples.

Example 1. Take 100 g of loparite concentrate composition, wt.%: 39,7 TiO2; 31,9 Ln2O3; 8,54 Nb2O5; 0,6 Ta2O5; 0,6 ThO2; 4,7 CaO; 2,63 SrO; 8,0 Na2O; 0,85 SiO2and make it into a pre-heated up to 40°With hydrofluoric acid with a concentration of 42 wt.%, taken in a weight ratio of concentrate T:W=1:3,4. Due to ekzotermicheskie process the temperature of the slurry rises to 105°C. the Slurry is incubated 15 minutes and the temperature of the slurry 90°share With filtering portianoy solution containing fluoride Nb, TA, Na, and the precipitate fluoride REE, Na, a, Sr.

Received portianoy the solution is cooled to room temperature (18° (C) separating the crystallization of the second precipitate Na2TiF6. The dry weight of the second sludge Na2TiF6equal to 9.32 g, which is 33.6% Na2O with respect to its initial content in loparite.

The solution of the metal fluoride has a volume of 250 ml and contains, g/l: 115 TiO2; 30,5 Nb2O5; 2,14 TA2O3; 315 HF; 0,2 CaO; 0,4 SrO and 8.0 Na2O. the Content of Na2O 25% relative to its content in loparite. Next portianoy solution of fluorides Nb, TA and Na volume of 250 ml is directed to extraction the extraction of Nb and TA by the octanol-1 when the volume ratio between organic and aqueous phase is 1:1. The degree of extraction in the organic phase, the amount of Ta2O5and Nb2O5for 5-speed countercurrent extraction is over 99.5%. Obtained after extraction of the aqueous phase with a volume of 240 ml content, g/l: 119 TiO2; 8,4 Na2O; 0,21 CaO; 0,41 SrO, together with a conversion fortechnology acid volume 88 ml content, g/l: 109,9 TiO2; 2,6 Na2O; CaO Of 0.5; 0.7 And SrO. The combined solution volume 328 ml, containing, g/l: 116,6 TiO2; 6,9 Na2O; 0,4 CaO; 0,8 SrO, evaporated to a concentration of TiO2500 g/l In the evaporation receive the pulp from which the filter separating the first precipitate formetanate Na2TiF6in Koli is este 7.2 g (content of Na 2O 28,1% from the original loparite) and 76,3 ml of concentrated solution fortechnology acid, which is sent on the extraction of titanium.

The wet precipitate fluoride REE, Na, Ca, Sr weight 109,8 g handle on the filter with hot water with a temperature of 90°at T:W=1:2,5. Get the washing liquor in the amount of 247 ml, containing, g/l: 27,0 TiO2; 59 HF; 0,14 CaO; 0,21 SrO and 11.3 Na2O (34.9% of the original loparite), and the precipitate fluoride REE 55 g of dry residue, which is further processed into individual elements. The washing liquor is evaporated to crystallization and separation of the additional sludge formetanate Na2TiF6the number 9,39, Additional sediment Na2TiF6combine with the first and second precipitation Na2TiF6. United sediment in the number 25,91 g sent for conversion, which is carried silicofluoride acid with a concentration of 1.4 M, taken in stoichiometric quantity. Get conversion solution fortechnology acid volume 88 ml of the above composition, which is directed to the process of evaporation for concentration of titanium, and 25.1 g of commodity fertilitate Na2SiF6.

Example 2. The process is conducted in accordance with the conditions of example 1. The difference lies in the fact that the pulp obtained in the decomposition of loparite concentrate, share fil is set at a temperature of 95° With portianoy solution of fluorides Nb, TA, Na, and the precipitate fluoride REE, Na, Ca, Sr. Received portianoy the solution is cooled to room temperature (21°C), separated by crystallization of the second precipitate Na2TiF6in the amount of 11.8 g, which is 42% Na2O with respect to its initial content in loparite.

The solution of the metal fluoride has a volume of 246 ml and contains, g/l: 115 TiO2; 30,5 Nb2O5; 2,13 TA2O3; 320 HF; 0,21 CaO; 0,41 SrO; 8,0 Na2O. the Content of Na2O is 24,6% in relation to its content in loparite. From fortimanager solution of fluorides Nb, TA and Na volume of 250 ml is removed by extraction of the amount of Nb and TA in accordance with the conditions of example 1 and receive the aqueous phase displacement to 240.5 ml content, g/l: 115 TiO2; 8,0 Na2O; 0,2 CaO; 0,4 SrO, which is linked with the conversion fortechnology acid volume 93 ml content, g/l: 109,6 TiO2; 1,8 Na2O; CaO Of 0.5; 0.7 And SrO. The combined solution volume 333,5 ml, containing, g/l: 113,5 TiO2; 6,26 Na2O; 0,28 CaO; 0,48 SrO, evaporated to a concentration of TiO2500 g/l In the evaporation receive the pulp from which the filter separating the first precipitate formetanate Na2TiF6the number of 6.65 g (content of Na2O 24.7% of the original loparite) and 75.8 ml of concentrated solution fortechnology acid, which is sent on the extraction of titanium.

2; 57 HF, 0,17 CaO; 0,26 SrO and 13.6 Na2O (34% from the original loparite), and the precipitate fluoride REE in the number of 54.8 g of dry residue, which is further processed into individual elements. The washing liquor is evaporated to crystallization and separation of the additional sludge formetanate Na2TiF6the number 8,62, Additional sediment Na2TiF6combine with the first and second precipitation Na2TiF6. United sediment in the amount of 27 g sent for conversion, which is carried silicofluoride acid with a concentration of 1.4 M, taken in stoichiometric quantity. Get conversion solution fortechnology acid volume 93 ml of the above composition, which is directed to the process of evaporation for concentration of titanium, and 26,46 g commodity fertilitate Na2SiF6.

Example 3. Take 100 g of loparite concentrate composition, wt.%: 39,7 TiO2; 31,9 Ln2O3; 8,54 Nb2O5; 0,6 Ta2O5; 0,6 ThO2; 4,7 CaO; 2,63 SrO; 8,0 Na2O; 0,85 SiO2and make it into a pre-heated up to 40°With hydrofluoric acid with a concentration of 38 wt.%, taken in a weight ratio of concentrate T:W=1:3,3. Due to the ind is terminate process the temperature of the slurry rises to 103° C. the Slurry is incubated 15 minutes and the temperature of the slurry 92°share With filtering portianoy solution containing fluoride Nb, TA, Na, and the precipitate fluoride REE, Na, CA, Sr.

Received portianoy the solution is cooled to room temperature (24°C), separated by crystallization of the second precipitate Na2TiF6. The dry weight of the second sludge Na2TiF6equal to 10.62 g, representing 39.5% of Na2O with respect to its original content will poprice.

Portianoy solution has a volume of 255 ml and contains, g/l: 112,7 TiO2; 29,9 Nb2O5; 2,1 TA2O5; 320 HF; 0,13 CaO; 0.2 To SrO and 7.8 Na2O. the Content of Na2O is 24,9% in relation to its content in loparite. Next portianoy solution is directed to extraction the extraction of Nb and TA by the octanol-1 when the volume ratio between organic and aqueous phases of 1.1:1. The degree of extraction in the organic phase amount TA2About5and Nb2O5for 5-speed countercurrent extraction is 99,3%. Obtained after extraction of the aqueous phase volume 244 ml content, g/l: 117,8 TiO2; 8,2 Na2O; 0,14 CaO; 0,21 SrO, together with a conversion fortechnology acid by volume to 90 ml with content, g/l: 109,3 TiO2; 1,78 Na2O; CaO Of 0.5; 0.7 And SrO. The combined solution volume 334 ml, containing, g/l: 115,3 TiO2; 6,4 Na2O; 0,24 CaO; 0,34 SrO, evaporated to a concentration of TiO2500 g/l as a Result of evaporation receive the pulp, from which the filter separating the first precipitate formetanate Na2TiF6the number 6,87 g (content of Na2O 25,6% of the original loparite) and 76,95 ml of concentrated solution fortechnology acid, which is sent on the extraction of titanium.

The wet precipitate fluoride REE, Na, CA, Sr weight of 112.8 g handle on the filter with hot water with a temperature of 90°at T:W=1:2,5. Get the washing liquor in the amount of 250 ml, containing, g/l: 27,5 TiO2; 52 HF; CaO of 0.5; 0.6 To SrO and 11.4 Na2O (35.6 percent from the original loparite), and the precipitate fluoride REE in the number of 54.5 g of dry residue, which is further processed into individual elements. The washing liquor is evaporated to crystallization and separation of the additional sludge formetanate Na2TiF6in the amount of 8.6, Additional sediment Na2TiF6combine with the first and second precipitation Na2TiF6. United sediment in the number 26,09 g sent for conversion, which is carried silicofluoride acid with a concentration of 1.4 M, taken in stoichiometric quantity. Get conversion solution fortechnology acid by volume to 90 ml of the above composition, which is directed to the process of evaporation for concentration of titanium, and 25,56 g commodity fertilitate Na2TiF6.

The table shows the comparative characteristics of STRs is mandatory processing of loparite concentrate according to the invention and of the prototype.

From the above examples and data the table shows that the inventive method allows to 2.0-2.5 times to reduce the amount of washing solutions, while ensuring a high degree of extraction of titanium compounds and other target products. Get pertitent sodium contains much lower amounts of impurity components of calcium and strontium.

1. Method for processing of loparite concentrate, including the decay of his hydrofluoric acid when heated with obtaining a slurry containing the fluorides of titanium, REE, niobium, tantalum and sodium, collective extraction of niobium and tantalum extraction, filtering the slurry with sludge separation of REE fluorides and part of formetanate sodium from fortimanager solution containing part of formetanate sodium, evaporation and filtration fortimanager solution separating the first precipitate of formetanate sodium from the concentrated solution fortechnology acid, which is directed to the extraction of titanium, shaded REE fluorides from formetanate sodium water at elevated temperature with the Department of the leaching solution, its evaporation with the allocation of additional sludge formetanate sodium, which is attached to the first draft of formetanate sodium, conversion of the combined sludge formetanate sodium with getting fertilitate sodium and to the versioned fortechnology acid, attached to fortechnology solution before evaporation, characterized in that the filtering of the slurry is carried out at an elevated temperature immediately after the decomposition of concentrate allocation in portianoy solution of fluoride, niobium and tantalum and the main part of formetanate sodium obtained portianoy the solution is cooled with the second compartment sludge formetanate sodium, which is attached to the joint draft of formetanate sodium and subjected to conversion, and extraction of niobium and tantalum extraction of lead from fortimanager solution after filtration of the slurry and separating the second precipitate of formetanate sodium.

2. The method according to claim 1, characterized in that the decomposition of lead concentrate at a temperature of 103-105°and the concentration of hydrofluoric acid 38-42 wt.%.

3. The method according to claim 1, characterized in that the filtering of the slurry is conducted at a temperature of 90-95°C.

4. The method according to claim 1, characterized in that the filtering of the slurry are emitting in portianoy the solution is not less than 58% of the sodium in terms of Na2O content in loparite concentrate.

5. The method according to claim 1, characterized in that the washing REE fluorides from formetanate sodium is carried out in one stage at T:W=1:2-2,5 and a temperature of 90-95°C.

6. The method according to claim 1, characterized in that portianoy the solution obtained by filtering bullets is s, cool to room temperature.

7. The method according to claim 1, characterized in that the extraction of niobium and tantalum are the octanol-1 with a ratio of organic and aqueous phases 1-1,1:1.



 

Same patents:

FIELD: non-ferrous metallurgy; methods of production of scandium-containing ligatures.

SUBSTANCE: the invention is pertaining to the field of non-ferrous metallurgy. The method of production of scandium-containing addition alloys includes a metallothermic restoration in halogenide melts. According to the invention the halogenide melt containing 1.0-1.4 mass % of scandium oxide is added with 1.4-1.7 mass % of zirconium oxide and conduct restoration by an alloy of aluminum with magnesium at the ratio of the halogenide melt to the aluminum-magnesium alloy from 1.2 up to 1.6. The technical result of the invention is production of a synthesized addition alloy containing scandium and zirconium with the maximal strengthening effect, decreased value of the produced addition alloy (by 30-40 %) due to decrease of consumption of the cost intensive scandium oxide by 50 %.

EFFECT: the invention ensures production of a synthesized scandium and zirconium ligature with maximal strength, allows to decrease significantly its production cost and consumption of expensive scandium oxide.

1 tbl, 1 ex

FIELD: metallurgy; hydrochemical methods of a complex processing of a multicomponent, polymetallic scrap.

SUBSTANCE: the invention is pertaining to the field of metallurgy, in particular, to the hydrochemical methods of a complex processing of a multicomponent, polymetallic scrap used in nonferrous metallurgy with extraction of valuable components and production of various commercial products. The technical result at reprocessing and neutralization of wastes of production of titanium tetrachloride consists in concentration of radioactive metals in the "head" of the process, transfer of the secondary wastes of production in an ecologically secure form suitable for a long-term entombment and-or storing, as well as in production of an additional commercial products - deficient and expensive black thermo- resistant inorganic pigments based on iron oxides, manganese and copper oxides. The method provides for a discharge of the spent melt of titanium chlorates into water; concentrating of a pulp by circulation; the pulp thickening; settling of metals oxyhydrates from the clarified solutions in succession in three stages: on the first stage - conduct a settling at pH = 3.-5.0 with separation of the formed settling of hydroxides of chrome, aluminum and scandium from the solution; on the second stage - conduct settling at presence of an oxidizing agent at pH = 2.5-3.5 within 20-50 hours with separation of the settling; on the third stage - conduct settling at pH = 9.5-11.0. The pulp at its circulation and concentration is added with sodium sulfite in amount of 5 - 15 g/dm3, then after circulation the pulp is treated with a solution of barium chloride in amount of 10-20 g/dm3 for cosettling of ions of thorium and radium, in the formed pulp of the first stage of settling introduce a high-molecular flocculant, and before settling process on the third stage of the process the solution is previously mixed with copper(II)-containing solution formed after lixiviation of a fusion cake of the process of cleanout of the industrial titanium tetrachloride from vanadium oxychloride by copper powder, then the produced settling of iron, manganese and copper oxyhydrates is filtered off, cleansed, dried and calcined at the temperature of 400-700°C.

EFFECT: the invention allows to concentrate radioactive metals in the "head" of the process, to transfer the process secondary wastes in the ecologically secure deficient and expensive black thermo-resistant inorganic pigments.

5 cl, 1 ex

FIELD: non-iron metallurgy, in particular scandium oxide recovery from industrial waste.

SUBSTANCE: method for preparation of scandium oxide from red mud being waste of alumina production includes: multiple subsequent leaching of red mud with mixture of sodium carbonate and hydrocarbonate solutions; washing and precipitate separation; addition into obtained solution zinc oxide, dissolved in sodium hydroxide; solution holding at elevated temperature under agitation; precipitate separation and treatment with sodium hydroxide solution at boiling temperature; separation, washing, and drying of obtained product followed by scandium oxide recovery using known methods. Leaching is carried out by passing through mixture of sodium carbonate and hydrocarbonate solutions gas-air mixture containing 10-17 vol.% of carbon dioxide, and repeated up to scandium oxide concentration not less than 50 g/m3; solid sodium hydroxide is introduced into solution to adjust concentration up to 2-3.5 g/m3 as calculated to Na2O (caustic); and mixture is hold at >=800C followed by flocculating agent addition, holding, and separation of precipitate being a titanium concentrate. Obtained mixture is electrolyzed with solid electrode, cathode current density of 2-4 A/dm3, at 50-750C for 1-2 h to purify from impurities. Zinc oxide solution in sodium hydroxide is added into purified after electrolysis solution up to ratio ZnO/Sc2O3 = (10-25):1, and flocculating agent is introduced. Solution is hold at 100-1020C for 4-8 h. Separated precipitate is treated with 5-12 % sodium hydroxide solution, flocculating agent is introduced again in amount of 2-3 g/m3, mixture is hold, and precipitate is separated. Method of present invention is useful in bauxite reprocessing to obtain alumina.

EFFECT: improved recovery ratio of finished product into concentrate; decreased impurity concentration in concentrate, reduced sodium hydrocarbonate consumption, as well as reduced process time due to decreased time of fine-dispersed precipitate.

2 cl, 2 ex

FIELD: chemical technology; deactivation and decontamination of radioactive industrial products and/or wastes.

SUBSTANCE: proposed method designed for deactivation and decontamination of radioactive industrial products and/or production wastes incorporating Th-232 and its daughter decay products (Ra-228, Ra-224), as well as rare-earth elements, Fe, Cr, Mn, Al, Ti, Zr, Nb, Ta, Ca, Mg, Na, K, and the like and that ensures high degree of coprecipitation of natural radionuclides of filtrates, confining of radioactive metals, and their conversion to environmentally safe form (non-dusting water-insoluble solid state) includes dissolution of wastes, their treatment with barium chloride, sulfuric acid, and lime milk, and separation of sediment from solution. Lime milk treatment is conducted to pH = 9-10 in the amount of 120-150% of that stoichiometrically required for precipitation of total content of metal oxyhydrate; then pulp is filtered and barium chloride is injected in filtrate in the amount of 0.4 - 1.8 kg of BaCl2 per 1 kg of CaCl2 contained in source solution or in pulp and pre-dissolved in sulfuric acid of chlorine compressors spent 5-20 times in the amount of 0.5 - 2.5 kg of H2SO4 per 1 kg of BaCl2. Then lime milk is added up to pH = 11 - 12 and acid chloride wash effluents of equipment and production floors are alternately introduced in sulfate pulp formed in the process at pulp-to-effluents ratio of 1 : (2-3) to pH = 6.5 - 8.5. Filtrate pulp produced in this way is filtered, decontaminated solution is discharged to sewerage system, sediment of barium and calcium sulfates and iron oxysulfate are mixed up with oxyhydrate sediment formed in source pulp neutralization, inert filler and 0.5 - 2 parts by weight of calcium sulfate are introduced in pasty mixture while continuously stirring them. Compound obtained in the process is placed in molds, held therein at temperature of 20 - 50 oC for 12 - 36 h, and compacted in blocks whose surfaces are treated with water-repelling material.

EFFECT: reduced radioactivity of filtrates upon separation of radioactive cakes.

8 cl, 1 dwg, 1 ex

FIELD: metallurgy; reworking wastes of alumina production process.

SUBSTANCE: proposed method includes preparation of batch of charge containing red mud and carbon reductant, heating the charge in melting unit to solid-phase iron reduction temperature, three-phase reduction of ferric oxides in charge by carbon reductant and saturation of iron with carbon in charge thus prepared, melting the reduced charge for obtaining metal phase in form of cast iron and slag phase in form of primary slag, separation of cast iron from primary slag in melt heated to temperature of 40 C, reduction of silicon and titanium from oxides contained in primary slag by aluminum and removal of cast iron and primary slag from melting unit; during preparation of charge, concentrate of titanomagnetite ore containing titanium oxide in the amount from 1 to 15% is added to red mud; besides that, additional amount of carbon reductant and additives are introduced; after separation of primary slag from cast iron in melting unit, cast iron is heated to 1500-1550 C and product containing ferric oxide is added to it; iron is reduced by carbon of cast iron for converting the cast iron into steel at obtaining secondary slag; main portion of steel is removed from melting unit, secondary slag is added to primary slag and silicon and titanium are converted into steel residue in melting unit by reduction with aluminum, thus obtaining final slag-saturated slag and master alloy containing iron, titanium and silicon; main portion of master alloy is removed from melting unit; after removal of final slag for converting the master alloy residue to steel in melting unit, titanium and silicon are converted into slag phase by oxidation and next portion of charge is fed to slag phase formed after converting the master alloy residue to steel. Proposed method ensures high efficiency due to obtaining iron-titanium silicon master alloy in form of independent product and production of alumina from high-alumina final slag or high-alumina cement and concentrate of rare-earth metals.

EFFECT: enhanced efficiency due to avoidance of intermediate remelting of steel.

10 cl, 2 dwg

The invention relates to a technology developing concentrates of rare earth elements from natural phosphate concentrates

The invention relates to the technology of extraction of rare earth elements (REE) from phosphogypsum obtained by sulphuric acid processing of Apatite concentrate on mineral fertilizers

The invention relates to the metallurgy of rare metals, more specifically to the technology of aluminum alloys with rare-earth elements, scandium, yttrium and lanthanides

The invention relates to the hydrometallurgical processing of ore concentrates, and more particularly to the processing of loparite concentrate and can be used in complex extraction of compounds of titanium, niobium and tantalum

The invention relates to metallurgy, in particular to methods metallothermic alloys of transition and rare-earth elements doped and can be used to produce alloys and special alloys

FIELD: metallurgy of rare and dispersed metals, chemical technology.

SUBSTANCE: invention relates to a method for extraction separation of tantalum and niobium. Method involves extraction separation of tantalum from niobium with organic solvent. As an organic solvent method involves using a mixture of methyl isobutyl ketone taken in the amount 40-80 vol.% with aliphatic (C7-C9)-alcohol taken in the amount 20-60 vol.%. At the extraction process tantalum transfers into organic phase and niobium - into aqueous phase. Then organic and aqueous phases are separated. Invention provides enhancing the extraction degree of tantalum into organic phase and to enhance the separation degree of tantalum and niobium in extraction.

EFFECT: improved separating method.

5 tbl, 5 ex

FIELD: metallurgy; methods of preparation of charges for production of niobium-bearing material.

SUBSTANCE: the invention is dealt with production of niobium-bearing materials used for production of special steels. The technical result is an increased degree of transition of niobium into an alloy, decreased share of impurities in the alloy, decreased production costs. For this purpose the charge for production of a niobium-bearing material contains the raw material containing niobium pentaoxide, a nickel-bearing material, aluminum, calcium oxide, calcium fluoride and an exothermic oxidative additive. At that in the capacity of the exothermic oxidative additive it contains potassium chlorate with moisture of 2-12% at the following ratio in shares in respect to the total weight of the charge: niobium pentaoxide - 0.470-0.520, nickel - 0.190-0.270, aluminum - 0.180-0.200, calcium oxide - 0.030-0.040, calcium fluoride - 0.003-0.004, potassium chlorate with moisture of 2-12% - 0.043-0.049. At preparation of the charge after mixing of components it is exposed to compaction in the crucible up to the value of the plastic strength of 0.4-10.0 MPa.

EFFECT: the invention ensures an increased degree of niobium transition into an alloy, decreased share of impurities in the alloy, decreased production costs.

2 cl, 1 tbl, 3ex

FIELD: electrometallurgy, namely processes for producing high-purity niobium ingots used in power generation plants operating with use of low-temperature superconductivity effect.

SUBSTANCE: method comprises steps of electron-beam refining of consumable niobium blank; using blank of niobium of given kind containing niobium uniformly distributed along its length and produced by iodide refining as consumable blank in order to produce niobium ingots with predetermined (in range 200 - 500) relation of specific resistances at temperature values 193K and 9.2K; determining mass relation of niobium of given kind and niobium produced by iodide refining according to relation of specific resistances at temperature values 193 K and 9.2 K with use of expression mn/mu = (500 - ρ2939.2)/(800 + 2 x ρ2939.2) where mn - mass of niobium of given kind, g; mu - mass of niobium produced by iodide refining, g; ρ293 - specific resistance of niobium at temperature 193K, ohm x m2/m ; ρ9.2 - specific resistance of niobium at temperature 9.2K, ohm x m2/m.

EFFECT: enhanced efficiency of process, lowered cost price of high-purity niobium ingots.

2 tbl, 2 ex

FIELD: production of pure niobium.

SUBSTANCE: method includes reducing fusion of niobium pentoxide with aluminum and calcium to provide crude ingots followed by heat treatment and multiple electron beam refining. As an additional raw material in step of reducing fusion sublimates (preferably in non-oxidized form) from second and subsequent electron beam refining are used. Such sublimates are obtained by subsequent cooling of furnace smelting chamber under residual pressure of 10-2-10-4 mmHg for 1.0-3.0 h, letting-to-helium under 1-3 mmHg for 1.0-3.0 h, and letting-to-air for 20-40 min. Sublimates are added in amount of 4.5 % based to feeding niobium pentoxide. Claimed method affords the ability to increase niobium pentoxide consumption by 73 kg in respect to 1000 kg of pure niobium in crude ingots.

EFFECT: production of pure niobium with increased effectiveness without deterioration of refined niobium quality.

2 cl, 1 tbl

The invention relates to pyrometallurgy, in particular the production of niobium from its oxide, and can be used for the production of ferroniobium

The invention relates to the field of hydrometallurgical processing of tantalum raw materials and are aimed at achieving its complex use

The invention relates to ferrous metallurgy and can be used to obtain alloy powders of tantalum or niobium

The invention relates to metals, in particular tantalum, and products made from tantalum, as well as to methods of obtaining and processing of tantalum

The invention relates to metallurgy tantalum production for structural products and tantalum capacitors

The invention relates to the hydrometallurgical processing of ore concentrates, and more particularly to the processing of loparite concentrate and can be used in complex extraction of compounds of titanium, niobium and tantalum

FIELD: non-ferrous metallurgy.

SUBSTANCE: device comprises reducing apparatus provided with lid, drain device, and mounted in the furnace with electric heaters. The furnace has casing and lining provided with passages for supplying air to the furnace and discharging air from the furnace and bottom. The bottom of the furnace is provided with passages inclined at an angle of 20-30° and directed to the drain device of the apparatus. The passages receive pipes for supplying compressed air and connected with the system for supplying compressed air.

EFFECT: enhanced efficiency and safety.

1 dwg

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