The method of producing refractory oxides of metals of loparite concentrate

 

(57) Abstract:

The invention relates to a method for producing oxides of refractory metals from loparite concentrate. It includes the grinding of the concentrate and the opening of concentrated nitric acid at atmospheric pressure and a temperature of more than 100oC with obtaining a slurry of hydrated oxide oxides of refractory metals, and subsequent fluorination to obtain fluoride solution of tantalum, niobium and titanium. Extraction of the solution are using oktilovom alcohol followed by re-extraction of water fortunelounge and Tornionjoki acids, oparka remaining fortechnology acid. Removing the oxides of tantalum and niobium from fortunelounge and Tornionjoki acid and titanium dioxide from fortechnology acid lead by high temperature pyrolysis of acid in 600 - 650oC. the Fluorination of hydrated pulp cake is carried out by absorption pulp gaseous hydrogen fluoride from flue gases resulting from the high temperature pyrolysis of percentlevel, Tornionjoki and fortechnology acids, for which the furnace gases and the slurry of hydrated cake sent in countercurrent to each other in the recirculated slurry. Technical is Britanie relates to the hydrometallurgical processing of ore concentrates, and more specifically to the processing of loparite concentrate.

Loparite concentrate is a complex raw material containing oxides of a large number of chemical elements. Used for processing of loparite concentrate brand CL-1 with the contents of loparite at least 95% in accordance with the applicable specifications contains, wt%:

the oxide of tantalum (Ta2O5) - 0,57

the oxide of niobium (Nb2O5- 8,14

the titanium oxide (TiO2) of 38.1

the oxides of rare earth metals cerium group, mainly oxides of lanthanum (La2O3), cerium oxide (Ce2O3) oxide, praseodymium (Pr2O3), neodymium oxide (Nd2O3) - 32

the sodium oxide (Na2O) - 7,9-9,06

calcium oxide (CaO) - 4,2-5,7

the strontium oxide (SrO) - 2,3-3,0

iron oxide (Fe2O3) - 2,0-2,5

silicon oxide (SiO2) - 1,95-2,5

aluminum oxide (Al2O3) - 0,6-0,7

the oxide of potassium (K2O) - 0,26-0,75

the oxide of phosphorus (P2P5) - 0,15-0,22

and the source of alpha radiation

the thorium oxide (ThO2) - 0,54

From loparite concentrate extract the most valuable oxides of tantalum, niobium, titanium, and less valuable rare-earth metal oxides. altoadige time were known and used two methods of processing of loparite concentrate, producing oxides of refractory metals, referred to as specialists of chlorine and sulfuric acid technologies.

However, chlorine technology is very dangerous and harmful for operating personnel and the environment due to the applied large quantities of chlorine, and therefore today it is absolutely not acceptable for use with the point of view of environmental safety. For this reason, chlorine technology in this application will not be considered.

The analogue of the claimed invention is a method for oxides of refractory metals by processing of loparite concentrate using concentrated sulfuric acid for the opening of loparite (see A. N. Zelikman and other "metallurgy of rare metals), metallurgy, 1991, S. 101, 103-105).

This method is based on the decomposition of loparite concentrate with sulfuric acid and separating valuable components using differences in solubility of double sulfates of titanium, niobium and tantalum, rare earth elements with sulfates of alkali metals or ammonium.

Source loparite concentrate is ground and subjected to classification. The opening of the concentrate is carried out using 95% sulfuric the x sulfates of titanium in the form of isomorphic admixture. Rare earth elements are part of the double sulphates REE - R2(SO4)3(NH4)2SO4. Product sulfatization - sulfate spec subjected to water leaching. As a result, in the solid phase remain double sulphates REE, and in the liquid phase remains sulfuric acid solution of titanium, niobium and tantalum. In this activity, due to the presence of loparite source of alpha radiation thorium Th and mesochori MsTh, is divided between the solid and liquid phases by 50%.

Removing oxides of refractory metals from their sulfate solution begins with the separation of titanium from niobium and tantalum. For the separation of titanium from niobium and tantalum using precipitation with ammonium sulfate soluble titanium salt (NH4)2TiO(SO4)2H2O. In the sediment stands out 70-80% of the titanium content in the solution. Double sulfate of titanium is used as an effective tanning agent in the leather industry. Thermal him decomposition receive technical titanium dioxide. Remaining after separation of the titanium salt solution, referred to as the sulfuric acid mother liquor contains tantalum, niobium and remainder titanium. This solution is subjected to fluorination 40% of pravicovy Th, mesochori MsTh).

Then for the extraction of tantalum and niobium in the process of the separation of extraction at 100% tributyl phosphate TBP. After extraction with tributyl phosphate with tantalum and niobium are sent to the alternate reextraction. As a result of this get the reextractors tantalum and niobium in the form of portantly and pornobabe solutions, which are further hydrometallurgical processing. For this alignment is tantalum and niobium is treated with ammonia, resulting in a gain hydroxide tantalum and niobium(OH)5and Ni(OH)5. Hydroxide is subjected to successive washing, drying and calcination, resulting in getting the finished product - pentoxide tantalum and niobium Ta2O5and Ni2O5.

To enable subsequent extraction of rare earth metals conduct additional independent technological cycle of conversion of double sulfates of REE carbonates, which is not the subject of this application and therefore the application will not be considered. Remaining after removal of the oxides of refractory metals, the raffinate is subjected to processing for disposal and recycling. Neutralized raffinate is subjected to filtration, resulting in what concentratie (NH4)2SO4= 300 g/l evaporated and disposed of as low ammonium sulfate, used as a nitrogen fertilizer.

In this method of producing oxides of refractory metals from loparite concentrate for the opening of the concentrate is used in more environmentally friendly chemical reagent compared to chlorine technology. However, this method has several significant disadvantages. The main of them are significant losses of oxides of refractory metals in the process of their extraction. This is because immediately at the first stage - the opening of the concentrate, there is a showdown and the release of the most valuable components that go into sulphate solution and distributed among the less valuable components in the solid phase. As a result of this we have to separate from the most valuable components of the less valuable the double sulphate of REE, which takes in various forms up to 25-30% of tantalum and niobium. To return tantalum and niobium is necessary to carry out additional processing of the dump cake remaining after the processing of double sulphates REE. In addition, there irretrievable loss of tantalum and niobium with crystals of titanium is enta tributyl phosphate makes the extraction process of the oxides of tantalum and niobium fluoride from their solutions time-consuming and laborious. The selection of titanium sulfate solutions in the form of dual titanium salt leads to large losses of titanium due to the significant solubility of the titanium salt in these conditions. In this regard, through the extraction of titanium in finished products is not more than 72%. Extracted this way oxides of refractory metals have increased activity due to a shift in their sulfuric acid solution of about 50% of the original activity. Moreover, scarce and expensive hydrofluoric acid is used for sulfate-fluoride extraction of tantalum and niobium, in this way is not utilized because the fluoride concentration in the raffinate after extraction is only 25-30 g/l, which makes recycling economically feasible. When implementing the method has a high consumption of sulfuric acid, because the acid from refined is removed, and only disposed of as low ammonium sulfate. All this makes the method complicated, inefficient and uneconomical.

More effective is a method for oxides of refractory metals from loparite concentrate on the patent of Russia No. 2149912 from 27.12.99 on M CL722 In 34/24, which was developed by the applicants and is the prototype of the proposed the particles is not more than 0.075 mm wet grinding with the classification of the particles and the thickening of the pulp loparite concentrate. Then carry out attackone opening of the pulp loparite at atmospheric pressure nitric acid HNO3with concentration C=650-700 g/l at temperature t=115-118oC. Because the process azotnokislogo of pulp exposure are discussed in detail in the previously filed application by the same applicant, in this application it is disclosed in the aggregated form. After azotnokislogo opening receive the pulp opening - nitrate slurry of hydrated oxide oxides of refractory metals (GCP). In the opening in the solution passed all the oxides of rare earth metals into soluble form nitrates of rare-earth elements R(NO3)3. At the same time in the process of opening under the influence of nitric acid in the solution is passed in the form of nitrates and all impurities loparite, including the source of the alpha activity of the oxide of thorium, mesochori. The most valuable of allocated components of loparite - oxides of tantalum, niobium and titanium is practically not dissolved by nitric acid, and therefore, completely, 100%, remain in the solid part of the slurry into a hydrated oxides of refractory metals - hydrate cake oxides of refractory metals. In the KEK these components are in the mixture, just as they nait full single branch of the most valuable components (tantalum, niobium), remaining hydrated Keke without any losses from the less valuable components that have fallen into the solution. When hydrated, the cake is almost free from radioactivity, since ~95% of thorium oxide and mesochori is a nitric acid solution of nitrates of rare-earth elements and impurities, and therefore, if further processing is not required, a special process of decontamination cake ELEVATION. Then nitrate hydrate slurry cake is diluted with water to 1.5-2.0 times and cool. After cooling are filtered solution of nitrate slurry of hydrated oxide and its subsequent washing from nitric acid solutions of nitrates of rare-earth elements and impurities. In the hillshade get pure hydrated cake MARK in the form of a slurry with a concentration of nitrates NO3-2 g/l and the concentration of solid WITHtin= 150-200 g/l of Pure hydrate cake is the starting product for the issuance of oxides of refractory metals, which are completely left in him.

Removing oxides of refractory metals from the pulp pure hydrate cake implement it by fluorination with hydrofluoric acid with a concentration of at least 40% or more on HF. Fluoridation is with great heat. To reduce temp fluoride slurry is subjected to sedimentation and filtration for removal of fluoride solution of tantalum, niobium and titanium undissolved part of the cake ELEVATION, consisting mainly of REE fluorides, calcium and silicon. The amount does not exceed 10% of the initial mass of hydrated cake. Sediment otdovat on the moisture filter the air. Sediment Rasulova lime milk, resulting fluorine transformed into an insoluble precipitate, and pumped to the tailings pond.

Pure fluoride solution of tantalum, niobium and titanium is directed to the extraction of tantalum and niobium with 100% oktilovom alcohol, also known as the octanol-1,1-axiostar or octanol. The octanol-rich tantalum and niobium, is directed to 2-contour alternately reextraction (flush with octanol) of niobium and tantalum with clean water. As a result of this get ferniany and fortuntely the reextractors in the form of pure pornoviejas acid HNbF6and percentlevel acid HTaF6and portianoy the raffinate as fortechnology acid.

Extracted with pure octanol tornieria and Tarantella acid is then subjected to high-temperature pyrolysis at a temperature of 600-650oC, resulting in a gain oxides (pentoxide) tantalum and niobium Ta2O5and Nb2O5the two the Hanks to use as extractant octanol, reextraction which is pure water.

In this way the percentage of extraction of oxides of tantalum and niobium from loparite concentrate reaches at least 95%, and they are almost completely devoid of radioactivity, because it does not contain thorium Th and mesochori MsTh. This is explained by the fact that about 5% of the radioactivity passing in hydrated cake at the opening of loparite concentrate nitric acid, remain bound in the sediment remaining from the cake after its dissolution with hydrofluoric acid. This finished product is particularly valuable source product for metallurgy, electronics and semiconductor technology.

After extraction of tantalum and niobium, the raffinate is subjected to processing to extract the remaining Dookie titanium. Almost all of the titanium present in the raffinate as the fluorine-Titanic acid, H2TiF6. Before processing the raffinate evaporated 1.5-2.0 to increase the concentration of TiO2to = 350-400 g/l Processing the raffinate is in high-temperature pyrolysis one stripped off the fluorine-titanium acid at a temperature of 600-650oC. In the pyrolysis of getting titanium dioxide. If necessary, it can be calcined at a temperature of t = 900 - pigment in the paint industry. The method provides a high degree of selection of titanium in the finished product. This end-to-end extraction of titanium is at least 98%.

High temperature pyrolysis is carried out in a known tower spray pyrolysis furnaces powered by natural gas or fuel oil. Subjected to pyrolysis concentrated portentosa, tornieria and fortiana acid spray nozzles in the upper parts of the furnace. Oxides of refractory metals formed by pyrolysis, remove from baking ovens. Hot gaseous products of pyrolysis containing hydrogen fluoride HF, directed from the upper parts of the furnace first to clear the solid products of pyrolysis in the cyclone, and then cooling and absorption of HF pure water. As a result of this get 40% hydrofluoric acid, which in return turnover by dissolving hydrated cake.

Thanks to this solution in hydrated Keke focused almost 100% of the recoverable oxides of refractory metals. The method provides full lossless their removal in the finished product. Reextracted tantalum and niobium with oktanovogo alcohol, carried out with clean water, provides the reextractors in the form of pure (without harmful premise the slot, exposed to high-temperature pyrolysis. Due to pyrolysis occurs simultaneous production of pure oxides of refractory metals and highlighting together with gaseous products of pyrolysis of hydrogen fluoride HF, which is easily absorbed by water, turning into hydrofluoric acid, is returned into circulation. This allows you to recycle up to 98% expensive hydrofluoric acid used in the production cycle. All this provides significant compared to sulfuric acid technology simplified way, improving its efficiency and effectiveness.

But with all the advantages of this method it has some weaknesses due to fluoridation of hydrated pulp cake hydrofluoric acid. When fluoridation slurry of hydrated cake hydrofluoric acid with a concentration of HF 40% and above are forced to withdraw from the reaction vessel through water-cooled coils large amount of heat that is lost. The material of the reaction vessel and cooling equipment must have high corrosion resistance due to excess fluorine at elevated temperatures. This greatly complicates and increases the cost aparature equipment used when ft is periodic mode to provide translation into the solution extracted valuable components (TA, Ni, Ti) without losing them from the undissolved residue. Formed after fluorination pulp poorly filtered and has a filtration rate just from 0.07 to 0,113 m3/m2hour. Due to the high concentration of fluoride ion in the fluorinating agent received fluoride compounds of tantalum, niobium and titanium are polluted with impurities (iron, silicon, sodium, etc). The use of hydrofluoric acid leads to the dilution of the obtained fluoride solutions on valuable components in 1.6 times, which creates difficulties for subsequent extraction due to the large volume of the aqueous phase. For hydrofluoric acid at the site of its utilization carry out the absorption of water vapor of hydrogen fluoride from a gaseous pyrolysis products, which further complicates the apparatus and equipment of the way and the way.

The present invention was based on the objective to develop a method of producing oxides of refractory metals from loparite concentrate, in which fluoridation slurry of hydrated cake would be carried out in such a reagent and proceeded under such conditions as to ensure the simplification of the way, increasing its efficiency and effectiveness.

The problem is solved in that in the method of gaining anantanubandhi nitric acid at atmospheric pressure and a temperature of more than 100oC with obtaining a slurry of hydrated oxide oxides of refractory metals, and subsequent fluorination to obtain fluoride solution of tantalum, niobium and titanium extraction from solution using oktilovom alcohol followed by re-extraction of water fortunelounge and Tornionjoki acids, oparka remaining fortechnology acid, and removing the oxides of tantalum and niobium from fortunelounge and Tornionjoki acid and titanium dioxide from fortechnology acid by high temperature pyrolysis of the acid at a temperature of 600-650oC, what's new is that fluoridation of hydrated pulp cake is carried out by absorption pulp gaseous hydrogen fluoride from flue gases resulting from the high temperature pyrolysis of percentlevel, Tornionjoki and fortechnology acids, for which the furnace gases and the slurry of hydrated cake sent in countercurrent to each other in the recirculated slurry.

This solution is primarily provided purification from gaseous hydrogen fluoride furnace gases from pyrolysis, which eliminates the need for site disposal of gaseous hydrogen fluoride compared with the method of the prototype. To vidspenthouse the evaporation of water, i.e., the fluoride concentration of the solution as valuable components of (TA, Nb, Ti). When fluoridation slurry of hydrated cake gaseous hydrogen fluoride in solution in the first pass of valuable components. The resulting cleaner fluoride solutions on the subsequent extraction will give a cleaner finished product. The concentration of gaseous hydrogen fluoride in the combustion gases is small, which creates a gentle corrosive conditions for operation of equipment. When fluoridation gaseous hydrogen fluoride there is no dilution of the obtained fluoride solution with water, which increases the concentration of extractable further valuable components. As a result, one can achieve simplification of the way, increasing its efficiency and effectiveness.

The inventive method of producing oxides of refractory metals from loparite concentrate is an improvement of the prototype method of the same applicant and differs from it only by the type of reagent used for the fluorination of hydrated cake and the process of utilization of hydrogen fluoride from the gaseous products of pyrolysis. The inventive method is carried out as follows.

Source loparite concentrate of ismelda the pulp loparite concentrate. Then carry out attackone opening of the pulp loparite at atmospheric pressure nitric acid HNO3with concentration C = 650-700 g/l at temperature t = 115-118oC. Because the process azotnokislogo of pulp exposure are discussed in detail in the previously filed application by the same applicant, in this application it is disclosed in the aggregate.

After azotnokislogo opening receive the pulp opening - nitrate slurry of hydrated oxide oxides of refractory metals (GCP). In the opening in the solution passed all the oxides of rare earth metals into soluble form nitrates of rare-earth elements R(NO33). At the same time in the process of opening under the influence of nitric acid in the solution is passed in the form of nitrates and all impurities loparite, including the source of the alpha activity of the oxide of thorium, mesochori.

The most valuable of allocated components of loparite - oxides of tantalum, niobium and titanium is practically not dissolved by nitric acid, and therefore, completely, 100%, remain in the solid part of the slurry into a hydrated oxides of refractory metals - hydrate cake oxides of refractory metals. In the KEK these components are in the mixture, and nitric acid is full of single branch of the most valuable components (tantalum, niobium), remaining hydrated Keke without any losses from the less valuable components that have fallen into the solution. When hydrated, the cake is almost free from radioactivity, since ~95% of thorium oxide and mesochori is a nitric acid solution of nitrates of rare-earth elements and impurities, and therefore, if further processing is not required, a special process of decontamination cake MARK.

Then nitrate slurry of hydrated cake diluted working solution in 1.5-2.0 times and cool. After cooling are filtered solution of nitrate slurry of hydrated oxide and its subsequent washing from nitric acid solutions of nitrates of rare-earth elements and impurities. In the hillshade get pure hydrated cake MARK in the form of a slurry with a concentration of nitrates NO3~ 2 g/l and the concentration of solid WITHtin= 150 - 200 g/l of Pure hydrate cake is the starting product for the issuance of oxides of refractory metals, which are completely left in him. Thus, the process of opening loparite concentrate in the present method completely coincides with the stage in the method prototype.

For the extraction of oxides of refractory metals from the pulp pure hydrated cake is mocnych gases, coming from the pyrolysis fornabai, fortuntely and fortimanager solutions. Fluoridation is the process of Assortie plate absorbers, irrigated pulp hydrate cake (concentration of about 600 g/l solid) in the recirculated slurry, when the counter-current gas and irrigate the pulp in the whole site of absorption, without heat. Fluoridation of hydrated pulp cake gaseous hydrogen fluoride mode altable has a number of advantages.

First of all, it provides purification from gaseous hydrogen fluoride furnace gases from pyrolysis, which eliminates the need for site disposal of gaseous hydrogen fluoride compared with the method of the prototype.

Released during the fluoridation of hydrated pulp cake fluoride hydrogen heat (260 kcal per 1 kg cake) it is not necessary to take, because it will be used for evaporation of water, i.e., the fluoride concentration of the solution as valuable components of (TA, Nb, Ti). This is possible due to the fact that when fluoridation mode absorption in irrigated column apparatus of the contact surface phase gas-liquid huge.

When fluoridation slurry of hydrated oxide gas is in solution only when the excess hydrogen fluoride, that almost never happens. The resulting cleaner fluoride solutions on the subsequent extraction will give a cleaner finished product.

The concentration of gaseous hydrogen fluoride in the combustion gases is small, which creates a gentle corrosive conditions for operation of the equipment.

When fluoridation gaseous hydrogen fluoride there is no dilution of the obtained fluoride solution with water, which increases the concentration of extractable further valuable components.

The process of fluorination unlike the prototype can be run in continuous mode, since the fluorine-containing flue gases are discharged from the pyrolysis gases continuously during the day.

Next, the process proceeds in the same way as in the method prototype. After fluorination the slurry is subjected to filtration for removal of fluoride solution of tantalum, niobium and titanium undissolved part of the cake ELEVATION, consisting mainly of REE fluorides, calcium and silicon. Sediment otdovat on the moisture filter the air. Sediment Rasulova lime milk, resulting fluorine transformed into an insoluble precipitate, and pumped to the tailings pond. Pure fluoride solution of tantalum, niobium and authorities octanol-1,1-axiostar or octanol. When the fluorine-Titanic acid (H2TiF6facilitates the transition of fluoride compounds tantalum and niobium in octanol. The octanol-rich tantalum and niobium, is directed to 2-contour alternately reextraction (flush with octanol) of niobium and tantalum with clean water. As a result of this get ferniany and fortuntely the reextractors in the form of pure pornoviejas acid HNbF6and percentlevel acid HNaF6and portianoy the raffinate as fortechnology acid.

Extracted with pure octanol tornieria and portentosa acid is then subjected to high-temperature pyrolysis at a temperature of 600-650oC, resulting in a gain oxides (pentoxide) tantalum and niobium Ta2O5and Nb2O5, which is the finished product resulting from implementation of the proposed method. In the present method the percentage of extraction of oxides of tantalum and niobium from loparite concentrate reaches at least 95%, and they are almost completely devoid of radioactivity, because it does not contain thorium Th and mesochori MsTh. This is explained by the fact that about 5% of the radioactivity passing in hydrated cake at the opening of loparite concentrate nitric sour is the first product is a particularly valuable source product for metallurgy, electronics and semiconductor technology.

Portianoy the raffinate is subjected to processing to extract the remaining Dookie titanium. Almost all of the titanium present in the raffinate as the fluorine-Titanic acid, H2TiF6. Before processing the raffinate evaporated 1.5-2.0 to increase the concentration of TiO2to = 350-400 g/L. one stripped off the fluorine-Titanic acid as fornabaio and percentlevel acid, is subjected to high-temperature pyrolysis at a temperature of 600-650oC. In the pyrolysis of getting titanium dioxide. If necessary, it can be calcined at a temperature of t = 900-950oC and put it in rutilio the form that is preferred for use as a pigment in paint industry. The inventive method provides a high degree of selection of titanium in the finished product. This end-to-end extraction of titanium is at least 98%.

High temperature pyrolysis is carried out in a known tower spray pyrolysis furnaces powered by natural gas, propane or fuel oil. Subjected to pyrolysis concentrated portentosa, tornieria and fortiana acid spray nozzles in voracia gaseous products of pyrolysis, containing hydrogen fluoride HF, directed from the upper parts of the furnace first to clear the solid products of pyrolysis in the cyclone, and then on the absorption of gaseous hydrogen fluoride pulp hydrated oxide oxides of refractory metals. In the chemisorption of hydrogen fluoride contained in the pyrolysis gases, pulp hydrate cake, get almost pure, without hydrogen fluoride exhaust gas and perftorirovannye slurry of hydrated oxide oxides of refractory metals. In the solution has passed all of tantalum, niobium, titanium, and some pollutants, and solid remained insoluble fluoride impurities and rare earth elements.

Thanks to the use of the pyrolysis process, the regeneration of hydrogen fluoride and return it to the technology is implemented without the use of any chemicals, and the subsequent absorption of hydrogen fluoride by the mechanism of chemisorption combined with parallel processes fluoridation slurry of hydrated cake and parki formed fluoride solution TA, Nb, Ti, which is advantageous for subsequent extraction. When it returned in turnover hydrogen fluoride is up to 98% of the total amount of HF used in technology.

Nism nitrate opening 1000 kg loparite concentrate brand CL-1 of the above structure.

The opening of the concentrate was carried out under the following conditions.

1. After the initial wet grinding concentrate > 95% of the particles have a particle size of not more than 0,074 mm

2. The solid content in the pulp opening - 600 g/L.

3. Initial concentration of nitric acid - 700 g/l

4. Temperature autopsy - 115-118oC.

5. Autopsy - 40 hours.

6. Intensive mixing with a mechanical stirrer (speed n= 200-220 rpm).

At the opening of loparite concentrate was consumed.

1. Nitric acid 70% - 1440 kg

2. Technical water - 400 kg.

3. Heating steam (deaf) - 550 kg.

4. Water for washing hydrate cake OTM - 3000 kg

In the nitrate processing reached the opening of loparite concentrate (total rare earth elements) - 95%.

Received the washed hydrate cake GCP - 575 kg (dry) of the following composition, %:

TA2O5- 0,99

Nb2O5- 14,5

TiO2- 66,2

the amount of oxides REE - 2,78

ThO2- 0,05

CaO - 0,4

Na2O - 0,75

Fe2O3- 0,35

SiO2- 3,5

NO3- 0,1

Deactivated the nitrate Rasta slurry with a solid content ~ 800 g/l processed by fluoride technology, i.e. we ferromoly gaseous hydrogen fluoride. Then filtered fluoride solution was applied for the extraction redistribution of obtaining paticia tantalum and niobium. The remaining raffinate was processed with obtaining titanium dioxide. Disposed after pyrolysis hydrogen fluoride returned to the fluoridation of hydrated pulp cake.

As a result of processing 575 kg of hydrated cake for the claimed fluoride technology was obtained:

- pentoxide tantalum - 5,407 kg; end-to-end retrieval - 95,0% Ta2O5;

- niobium pentoxide - 79,2 kg; end-to-end retrieval - 95,0% Nb2O5;

- titanium dioxide - 373 kg; end-to-end retrieval - 98,0% TiO2.

The consumption of reagents to obtain the product in accordance with the inventive method compared to sulfuric acid technology are presented in table 1.

From the specific embodiments of the claimed invention for any specialist in this field are obvious possibilities for its realization with the simultaneous solution of the set task. However it is also clear that the invention can be made small changes, which, however, will not be out the produce oxides of refractory metals from loparite concentrate provides a complete single branch of the most valuable components of tantalum, niobium and titanium from less valuable components and impurities. The most valuable components are extracted with virtually no losses and is absolutely clean from radioactivity. The method has high economic efficiency, as particularly environmentally harmful hydrogen fluoride is almost completely regenerated after use and recycled. The method is much simpler in hardware design in comparison with the method of the prototype and is amenable to full automation because of the practical continuity of the process. The method creates a more gentle (less corrosive) conditions for operation of equipment. Reduces the cost and complexity of maintaining equipment in working condition, and the number of staff.

The method of producing refractory oxides of metals of loparite concentrate, including the grinding of the concentrate and the opening of concentrated nitric acid at atmospheric pressure and a temperature of more than 100oC with obtaining a slurry of hydrated oxide oxides of refractory metals, and subsequent fluorination to obtain fluoride solution of tantalum, niobium and titanium extraction from solution using oktilovom alcohol with the following rlie oxides of tantalum and niobium from fortunelounge and Tornionjoki acid and titanium dioxide from fortechnology acid lead by high temperature pyrolysis of acid in 600 - 650oC, characterized in that the fluoridation of hydrated pulp cake is carried out by absorption pulp gaseous hydrogen fluoride from flue gases resulting from the high temperature pyrolysis of percentlevel, Tornionjoki and fortechnology acids, for which the furnace gases and the slurry of hydrated cake sent in countercurrent to each other in the recirculated slurry.

 

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