CN106676291A - Method for comprehensively recovering uranium, niobium and tantalum from ore - Google Patents

Method for comprehensively recovering uranium, niobium and tantalum from ore Download PDF

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Publication number
CN106676291A
CN106676291A CN201611233203.0A CN201611233203A CN106676291A CN 106676291 A CN106676291 A CN 106676291A CN 201611233203 A CN201611233203 A CN 201611233203A CN 106676291 A CN106676291 A CN 106676291A
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China
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uranium
tantalum
niobium
ore
leaching
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CN201611233203.0A
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Chinese (zh)
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刘会武
向秋林
刘忠臣
黄永
贾秀敏
师留印
刘智
杨剑飞
陈天宝
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核工业北京化工冶金研究院
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Priority to CN201611233203.0A priority Critical patent/CN106676291A/en
Publication of CN106676291A publication Critical patent/CN106676291A/en

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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/0004Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/0005Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds, e.g. acyclic or carbocyclic compounds, heterocyclic compounds, organo- metallic compounds, alcohols, ethers, or the like
    • C22B3/004Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds, e.g. acyclic or carbocyclic compounds, heterocyclic compounds, organo- metallic compounds, alcohols, ethers, or the like using organo-metallic compounds or organo compounds of boron, silicon, phosphorus, selenium or tellurim
    • C22B3/0041Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds, e.g. acyclic or carbocyclic compounds, heterocyclic compounds, organo- metallic compounds, alcohols, ethers, or the like using organo-metallic compounds or organo compounds of boron, silicon, phosphorus, selenium or tellurim using organo-metallic compounds of a single type
    • C22B3/0043Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds, e.g. acyclic or carbocyclic compounds, heterocyclic compounds, organo- metallic compounds, alcohols, ethers, or the like using organo-metallic compounds or organo compounds of boron, silicon, phosphorus, selenium or tellurim using organo-metallic compounds of a single type using phosphorus-based acid derivatives
    • C22B3/0044Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds, e.g. acyclic or carbocyclic compounds, heterocyclic compounds, organo- metallic compounds, alcohols, ethers, or the like using organo-metallic compounds or organo compounds of boron, silicon, phosphorus, selenium or tellurim using organo-metallic compounds of a single type using phosphorus-based acid derivatives of a single type
    • C22B3/0045Acyclic compounds
    • C22B3/0063Mononuclear oxyacids of pentavalent phosphorus or their esters(-ate)
    • C22B3/0068Phosphoric ((O)P(OH)3) type
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08Sulfuric acid, other sulfurated acids or salts thereof
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/20Obtaining niobium, tantalum or vanadium
    • C22B34/24Obtaining niobium or tantalum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02Obtaining thorium, uranium, or other actinides
    • C22B60/0204Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0217Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
    • C22B60/0221Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching
    • C22B60/0226Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors
    • C22B60/023Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors halogenated ion as active agent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02Obtaining thorium, uranium, or other actinides
    • C22B60/0204Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0217Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
    • C22B60/0221Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching
    • C22B60/0226Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors
    • C22B60/0234Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors sulfurated ion as active agent
    • Y02P10/234

Abstract

The invention provides a method for comprehensively recovering uranium, niobium and tantalum from ore. The method comprises the steps that (1) the ore containing the uranium, the niobium and the tantalum is finely ground and sieved; (2) water is added into finely ground ore powder in an adjustment mode with the leaching liquid-solid ratio controlled to be 1.0-3.0 and the leaching temperature 75-100 DEG C, concentrated sulfuric acid is added for reacting for 0.5-1 h firstly, and then hydrofluoric acid is added for leaching for 2-4 h continuously; (3) leached ore slurry is filtered and washed, and the uranium, the niobium and the tantalum in leachate are separated and recovered; (4) a blended organic phase composed of P204, TBP and sulfonated kerosene is adopted for directly separating the uranium in the leachate; and (5) the acidity of a solution is adjusted through HF and H2SO4, and niobium and tantalum extraction liquid is obtained. The uranium, the niobium and the tantalum are synchronously leached by adoption of a low-concentration hydrofluoric acid-sulfuric acid system, efficient uranium extraction and separation are achieved by controlling the concentrations of the sulfuric acid and the hydrofluoric acid of the leachate, the fussy defluorination technology in the process of extracting the uranium from niobium and tantalum slag is avoided, the treatment process is simplified, reagent consumption is saved, and the waste production amount is decreaced.

Description

A kind of method of the synthetical recovery uranium niobium tantalum from Ore

Technical field

The present invention relates to field of hydrometallurgy, is related to many metal recovery processes of uranium niobium tantalum, and in particular to one kind is from Ore The method of synthetical recovery uranium niobium tantalum.

Background technology

All containing radioelement such as uranium, thoriums in most of tantalite-columbite ores.At present, domestic and international niobium tantalum industry is main using high Concentration Fluohydric acid. and sulphuric acid extract niobium and tantalum in niobium tantalum concentrate as leaching agent, and the uranium in Ore substantially remains in leaching In slag.Because the manufacturing enterprise for processing tantalum niobium concentrate there is no effective uranium extractive technique, manufacturing enterprise is usually to seal up for safekeeping tailings.Heap Put process and not only waste uranium resource, also increase enterprise to this apoplexy due to endogenous wind cool waste management cost.

United States Patent (USP) US7282187B1 is proposed extracts the valuable metals such as separation and recovery uranium, zirconium, thorium and scandium from niobium tantalum slag Process.The method removes HF in niobium tantalum slag first with concentrated sulphuric acid pretreatment-rotary kiln low-temperature bake, then goes out to divide with water logging From recovery valuable metal.Sulfur acid pretreatment is mixed using 1.2~1.75 times of concentrated sulphuric acids with niobium tantalum slag, and niobium tantalum slag exists after mixing HF is removed under the conditions of 150 DEG C~300 DEG C in rotary kiln, the sulfuric acid conversion of fluorination niobium tantalum slag is realized.Niobium tantalum slag after sulfuric acid conversion Water leaching valuable metal is used, it is achieved thereby that the separation and recovery of the valuable metal such as uranium, zirconium, thorium and scandium.Although the technique realize The synthetical recovery of various metals, but there are the problems such as reagent consumption is big, ambient pressure is big.

Domestic face permits richness et al. using in Calx and niobium tantalum slag is except fluoro- alkaline Leaching puies forward uranium technique.The technique initially with With niobium tantalum slag in Calx, the purpose of peracid residual liquid and solid fluorine in neutralization niobium tantalum slag is realized.It is connected with technique with Calx, adopts Alkaline Leaching technique carries uranium, and uranium extraction ratio can reach 90%-93%.But the technique is present, and slag yield is big, alkali is high more than Uranium extraction liquid And cause to be difficult to directly recovery.

CN102312094A proposes a kind of method of uranium-bearing niobium tantalum leached tailings sulfuric acid leaching.The method is by niobium tantalum tailings First deionized water carries out washing leaching, and uranium-bearing leachate and solid slag are filtrated to get after leaching, then multiple with dilution heat of sulfuric acid Solid slag is leached and carries uranium, until uranium content is less than 82 μ g/g in tailings.The characteristics of the method is in acid using niobium tantalum slag, adopts Sulfuric acid leaching saves reagent consumption, but operating procedure is relatively complicated, and technical process can produce substantial amounts of fluoride waste.

In sum, it is all first to adopt Fluohydric acid. plus sulphuric acid extraction niobium that research is reclaimed in the extraction of uranium in domestic and international Nb-Ta mineral Tantalum, then be removed to the fluorine in niobium tantalum slag, to uranium carries out extraction recovery again afterwards.There is complex process, reagent and disappear in the technique The problems such as consumption is higher, and nitration mixture leaches extraction niobium tantalum process, the uranium in Ore is inevitably partly dissolved, and eventually enters into waste water Place's science and engineering continues, and not only causes metal loss, and increased wastewater treatment complexity.

The content of the invention

For the deficiencies in the prior art, the invention provides a kind of uranium niobium tantalum comprehensively extracts detached new method, by right The new technology that uranium niobium tantalum is reclaimed using leaching simultaneously, extract and separate in Ore, solves uranium-bearing tantalite-columbite ore uranium, niobium tantalum and extracts work The problems such as complex process, high cost that skill disconnection is caused.

Realize the technical scheme of the object of the invention:A kind of method of the synthetical recovery uranium niobium tantalum from Ore, the method includes Following steps:

(1) by uranium-bearing tantalite-columbite ore it is levigate, sieve, control particle diameter<0.048mm;

(2) water rate control leaching liquid-solid ratio is added to be 1.0~3.0 by adjusting levigate rear breeze, extraction temperature is 75 ~100 DEG C, 0.5~1h of strong sulfuric acid response is initially charged, adds Fluohydric acid. and continue to leach 2~4h, added by sulphuric acid and Fluohydric acid. Enter amount control solution 0.05~1.5mol/L of sulfuric acid concentration, 0.5~3mol/L of hydrofluoric acid concentration;

(3) filtered, washed to leaching ore pulp, leachate is carried out uranium, niobium tantalum separation and recovery;

(4) the mixing organic faciess constituted using P204, TBP and sulfonated kerosene are directly carried out point to the uranium in leachate From;The mixing organic faciess that described P204, TBP and sulfonated kerosene is constituted, wherein P204 percents by volume are 3%~10%, TBP percents by volume are 0~10%, and remaining is sulfonated kerosene;Described TBP is tributyl phosphate, and P204 is two (2- ethyl hexyls Base) phosphate ester;

(5) with HF and H2SO4Acidity in solution is adjusted, makes after adjustment solution sulfuric acid concentration be 3~7mol/L, hydrogen Fluoric acid concentration is 4~8mol/L, obtains niobium tantalum extraction stock solution.

A kind of method of the synthetical recovery uranium niobium tantalum from Ore as above, it is former to the extraction of niobium tantalum after its step (5) Liquid carries out extract and separate to niobium tantalum in solution using the industrial MIBK of existing niobium tantalum, sec-octyl alcohol or acetyl amine extractant, and most Niobium pentaoxide, tantalum pentoxide product are obtained eventually.

A kind of method of the synthetical recovery uranium niobium tantalum from Ore as above, the concentrated sulphuric acid that its step (2) is added is dense Spend for 80~98wt%, the hydrofluoric acid concentration of addition is 30~50wt%.

A kind of method of the synthetical recovery uranium niobium tantalum from Ore as above, the HF concentration described in its step (5) is 60 ~80wt%, H2SO4Concentration is 80~98wt%.

A kind of method of the synthetical recovery uranium niobium tantalum from Ore as above, its step (2) leach after the completion of uranium, niobium, Tantalum leaching rate can be respectively greater than 95%, 86%, 85%.

A kind of method of the synthetical recovery uranium niobium tantalum from Ore as above, its step (3) was carried out to leaching ore pulp Filter, washing, leached mud directly mixed and stirred and abandoned after Calx after washing.

A kind of method of the synthetical recovery uranium niobium tantalum from Ore as above, its step (4) is using P204, TBP and sulphur The mixing organic faciess for changing kerosene composition are directly separated to the uranium in leachate, and uranium extraction rate is more than 99%;Load uranium is organic Mutually uranium qualifying liquid is obtained by existing anti-extraction process and Jing precipitations are obtained " 111 " product;Described " 111 " product is attached most importance to uranic acid Sodium.

Effect of the invention is that:

The invention provides a kind of method of the synthetical recovery uranium niobium tantalum from Ore, exists particular by leaching condition control Extraction while ensureing that uranium niobium tantalum is leached for uranium in leachate creates conditions;Leachate adjusts again acidity and realizes after to extracting uranium Niobium tantalum extract and separate, and uranium, niobium, tantalum product is finally obtained.The new technology that the method is reclaimed using leaching simultaneously, extract and separate, The problems such as solving uranium-bearing tantalite-columbite ore uranium, complex process, the high cost that the disconnection of niobium tantalum extraction process is caused.

Compared with the existing niobium tantalum extraction process with regard to uranium-bearing, the present invention is synchronously soaked using low concentration hydrofluoric acid-sulfuric acid system Go out uranium, niobium tantalum, while realizing the efficient extract and separate of uranium by controlling leachate sulphuric acid and hydrofluoric acid concentration, it is to avoid from niobium tantalum The loaded down with trivial details defluorinating process of uranium process is carried in slag, so as to simplify handling process, reagent consumption has been saved, waste generation is reduced Amount.

Description of the drawings

Fig. 1 is a kind of method flow diagram of synthetical recovery uranium niobium tantalum from Ore of the present invention.

Specific embodiment

Below in conjunction with the accompanying drawings with specific embodiment to a kind of side of the synthetical recovery uranium niobium tantalum from Ore of the present invention Method is further described.

Embodiment 1

Certain uranium-bearing tantalite-columbite ore uranium-bearing 0.416%, containing niobium 2.58%, containing tantalum 0.72%.Ore is levigate extremely with ball mill 0.048mm, weighs the levigate rear Ores of 100g and adds 150mL clear water, adds the concentrated sulphuric acid (concentration 98wt%) of ore deposit weight 15wt%, Leaching 1h under the conditions of 90 DEG C;Add concentration to be 40wt% Fluohydric acid. 25mL afterwards, continue leaching 3h.After the completion of leaching Ore pulp is filtered, is washed, slag meter leaching rate uranium, niobium, tantalum leaching rate can be respectively reached 98.1%, 86.2%, 85.6%.Leaching Uranium grade of slagging tap can be reduced to 0.008%, mix and stir and abandoned after Calx.Sulfuric acid concentration 0.78mol/L, hydrofluoric acid concentration in leachate 2.1mol/L, directly carries out 10 stage countercurrents extraction uranium, uranium extraction rate with 5%P204+10%TBP and sulfonated kerosene to it 99.5%.Carry uranium organic faciess and uranium qualifying liquid, and final prepared " 111 " product of Jing precipitations are obtained by existing anti-extraction process.Again With 70wt%HF and 98wt%H2SO4Acidity in solution is adjusted, makes after adjustment solution sulfuric acid concentration be 5mol/L, hydrogen fluorine Acid concentration is 6mol/L, obtains niobium tantalum extraction stock solution.Niobium tantalum extraction stock solution is using the conventional MIBK extractants of existing niobium tantalum industry Extract and separate is carried out to niobium tantalum in solution, and niobium pentaoxide, tantalum pentoxide product is finally obtained.

Embodiment 2

Certain ore dressing gained uranium-bearing niobium tantalum refined ore uranium-bearing 1.21%, containing niobium 12.35%, containing tantalum 6.72%.Weigh 100g ore deposits Stone adds 300mL clear water, adds the concentrated sulphuric acid (concentration 95wt%) of ore deposit weight 23wt%, the leaching 0.5h under the conditions of 96 DEG C; Add concentration to be 40wt% Fluohydric acid. 55mL afterwards, continue leaching 4h.Ore pulp is filtered after the completion of leaching, is washed, Slag meter leaching rate uranium, niobium, tantalum leaching rate can respectively reach 99.1%, 88.4%, 86.6%.Leached mud is mixed and stirred after Calx after washing Abandon.Sulfuric acid concentration 0.62mol/L, hydrofluoric acid concentration 0.5mol/L in leachate, directly with 10%P204+15%TBP and sulphur Changing kerosene carries out 10 stage countercurrents extraction uranium, uranium extraction rate 99.6% to it.Carry uranium organic faciess to obtain by existing anti-extraction process Uranium qualifying liquid, and Jing precipitations are finally obtained " 111 " product.70wt%HF and 98wt%H is used again2SO4Acidity in solution is adjusted It is whole, make solution sulfuric acid concentration after adjustment be 5mol/L, hydrofluoric acid concentration is 6mol/L, obtains niobium tantalum extraction stock solution.Niobium tantalum is extracted Stock solution carries out extract and separate to niobium tantalum in solution using the conventional acetyl amine extractant of existing niobium tantalum industry, and five oxygen are finally obtained Change two niobiums, tantalum pentoxide product.

Embodiment 3

Certain uranium-bearing tantalite-columbite ore uranium-bearing 0.368%, containing niobium 1.56%, containing tantalum 4.42%.Weigh 100g Ores and add 160mL Clear water, adds the concentrated sulphuric acid (concentration 90wt%) of ore deposit weight 22wt%, the leaching 1h under the conditions of 96 DEG C;Afterwards addition concentration is 40wt% Fluohydric acid. 40mL, continue leaching 4h.Ore pulp is filtered after the completion of leaching, is washed, slag meter leaching rate uranium, Niobium, tantalum leaching rate can respectively reach 97.2%, 88.5%, 86.6%.Leached mud mixed and stirred and abandoned after Calx after washing.In leachate Sulfuric acid concentration 0.95mol/L, hydrofluoric acid concentration 2.4mol/L, are directly entered with 4.5%P204+7.5%TBP and sulfonated kerosene to it The stage countercurrent of row 6 extracts uranium, uranium extraction rate 99.6%.Carry uranium organic faciess and uranium qualifying liquid, and Jing are obtained by existing anti-extraction process Precipitation is finally obtained " 111 " product.70wt%HF and 98wt%H is used again2SO4Acidity in solution is adjusted, is made molten after adjustment Molten sulfur acid concentration is 5mol/L, and hydrofluoric acid concentration is 6mol/L, obtains niobium tantalum extraction stock solution.Niobium tantalum extraction stock solution adopts existing niobium The conventional sec-octyl alcohol extractant of tantalum industry carries out extract and separate to niobium tantalum in solution, and niobium pentaoxide, five oxidations are finally obtained Two tantalum products.

Embodiment 4

As shown in figure 1, a kind of method of synthetical recovery uranium niobium tantalum from Ore of the present invention, it includes following step Suddenly:

(1) uranium-bearing tantalite-columbite ore Jing is levigate, sieve, and controls particle diameter<0.048mm.

(2) water rate control leaching liquid-solid ratio is added to be 1.0 by adjusting levigate rear breeze, extraction temperature is 75 DEG C, first 80wt% strong sulfuric acid response 1h are added, 30wt% Fluohydric acid .s is added and is continued to leach 4h, by sulphuric acid and Fluohydric acid. addition control Solution sulfuric acid concentration 0.05mol/L processed, hydrofluoric acid concentration 0.5mol/L.

(3) filtered, washed to leaching ore pulp, leached mud directly mixed and stirred and abandoned after Calx after washing;Leachate is carried out Uranium, niobium tantalum separation and recovery.

(4) using the mixing organic faciess of percent by volume 10%P204+90% sulfonated kerosene composition directly in leachate Uranium separated, uranium extraction rate be more than 99%.Uranium organic faciess are carried by existing anti-extraction process acquisition uranium qualifying liquid and Jing sinks Form sediment and " 111 " product is obtained.

(5) with 60wt%HF and 80wt%H2SO4Acidity in solution is adjusted, makes the solution sulfuric acid concentration after adjustment be 3mol/L, hydrofluoric acid concentration is 4mol/L, obtains niobium tantalum extraction stock solution.

(6) niobium tantalum extraction stock solution can adopt the extractants such as the conventional MIBK of existing niobium tantalum industry, sec-octyl alcohol or acetamide Extract and separate is carried out to niobium tantalum in solution, and niobium pentaoxide, tantalum pentoxide product is finally obtained.

Embodiment 5

As shown in figure 1, a kind of method of synthetical recovery uranium niobium tantalum from Ore of the present invention, it includes following step Suddenly:

(1) uranium-bearing tantalite-columbite ore Jing is levigate, sieve, and controls particle diameter<0.048mm.

(2) water rate control leaching liquid-solid ratio is added to be 2.0 by adjusting levigate rear breeze, extraction temperature is 90 DEG C, first 95wt% strong sulfuric acid response 0.6h are added, 40wt% Fluohydric acid .s is added and is continued to leach 3h, by sulphuric acid and Fluohydric acid. addition Control solution sulfuric acid concentration 1.0mol/L, hydrofluoric acid concentration 2mol/L.Uranium, niobium, tantalum leaching rate can be respectively greater than after the completion of leaching 95%th, 86%, 85%.

(3) filtered, washed to leaching ore pulp, leached mud directly mixed and stirred and abandoned after Calx after washing;Leachate is carried out Uranium, niobium tantalum separation and recovery.

(4) using the mixing organic faciess of percent by volume 8%P204+5%TBP+87% sulfonated kerosene composition directly to leaching The uranium gone out in liquid is separated, and uranium extraction rate is more than 99%.Carry uranium organic faciess and uranium qualifying liquid is obtained by existing anti-extraction process And Jing precipitations are obtained " 111 " product.

(5) with 70wt%HF and 98wt%H2SO4Acidity in solution is adjusted, makes the solution sulfuric acid concentration after adjustment be 5mol/L, hydrofluoric acid concentration is 6mol/L, obtains niobium tantalum extraction stock solution.

(6) niobium tantalum extraction stock solution can adopt the extractants such as the conventional MIBK of existing niobium tantalum industry, sec-octyl alcohol or acetamide Extract and separate is carried out to niobium tantalum in solution, and niobium pentaoxide, tantalum pentoxide product is finally obtained.

Embodiment 6

As shown in figure 1, a kind of method of synthetical recovery uranium niobium tantalum from Ore of the present invention, it includes following step Suddenly:

(1) uranium-bearing tantalite-columbite ore Jing is levigate, sieve, and controls particle diameter<0.048mm.

(2) water rate control leaching liquid-solid ratio is added to be 3.0 by adjusting levigate rear breeze, extraction temperature is 100 DEG C, first 98wt% strong sulfuric acid response 0.5h are added, 50wt% Fluohydric acid .s is added and is continued to leach 2h, by sulphuric acid and Fluohydric acid. addition Control solution sulfuric acid concentration 1.5mol/L, hydrofluoric acid concentration 3mol/L.

(3) filtered, washed to leaching ore pulp, leached mud directly mixed and stirred and abandoned after Calx after washing;Leachate is carried out Uranium, niobium tantalum separation and recovery.

(4) using the mixing organic faciess of percent by volume 3%P204+10%TBP+87% sulfonated kerosene composition directly to leaching The uranium gone out in liquid is separated, and uranium extraction rate is more than 99%.Carry uranium organic faciess and uranium qualifying liquid is obtained by existing anti-extraction process And Jing precipitations are obtained " 111 " product.

(5) with 80wt%HF and 98wt%H2SO4Acidity in solution is adjusted, makes the solution sulfuric acid concentration after adjustment be 7mol/L, hydrofluoric acid concentration is 8mol/L, obtains niobium tantalum extraction stock solution.

(6) niobium tantalum extraction stock solution can adopt the extractants such as the conventional MIBK of existing niobium tantalum industry, sec-octyl alcohol or acetamide Extract and separate is carried out to niobium tantalum in solution, and niobium pentaoxide, tantalum pentoxide product is finally obtained.

Claims (7)

1. a kind of method of the synthetical recovery uranium niobium tantalum from Ore, it is characterised in that:The method comprises the steps:
(1) by uranium-bearing tantalite-columbite ore it is levigate, sieve, control particle diameter<0.048mm;
(2) water rate control leaching liquid-solid ratio is added to be 1.0~3.0 by adjusting levigate rear breeze, extraction temperature is 75~100 DEG C, 0.5~1h of strong sulfuric acid response is initially charged, add Fluohydric acid. and continue to leach 2~4h, by sulphuric acid and Fluohydric acid. addition control 0.05~1.5mol/L of solution sulfuric acid concentration processed, 0.5~3mol/L of hydrofluoric acid concentration;
(3) filtered, washed to leaching ore pulp, leachate is carried out uranium, niobium tantalum separation and recovery;
(4) the mixing organic faciess constituted using P204, TBP and sulfonated kerosene are directly separated to the uranium in leachate;Institute The mixing organic faciess of P204, TBP for stating and sulfonated kerosene composition, wherein P204 percents by volume are 3%~10%, TBP bodies Product percentage ratio is 0~10%, and remaining is sulfonated kerosene;Described TBP is tributyl phosphate, and P204 is two (2- ethylhexyls) phosphorus Acid esters;
(5) with HF and H2SO4Acidity in solution is adjusted, makes after adjustment solution sulfuric acid concentration be 3~7mol/L, Fluohydric acid. Concentration is 4~8mol/L, obtains niobium tantalum extraction stock solution.
2. the method for a kind of synthetical recovery uranium niobium tantalum from Ore according to claim 1, it is characterised in that:Step (5) Afterwards, stock solution is extracted to niobium tantalum using the industrial MIBK of existing niobium tantalum, sec-octyl alcohol or acetyl amine extractant to niobium tantalum in solution Extract and separate is carried out, and niobium pentaoxide, tantalum pentoxide product is finally obtained.
3. the method for a kind of synthetical recovery uranium niobium tantalum from Ore according to claim 1, it is characterised in that:Step (2) The concentrated sulphuric acid concentration for being added is 80~98wt%, and the hydrofluoric acid concentration of addition is 30~50wt%.
4. the method for a kind of synthetical recovery uranium niobium tantalum from Ore according to claim 1, it is characterised in that:Step (5) Described HF concentration is 60~80wt%, H2SO4Concentration is 80~98wt%.
5. the method for a kind of synthetical recovery uranium niobium tantalum from Ore according to claim 1, it is characterised in that:Step (2) Uranium, niobium, tantalum leaching rate can be respectively greater than 95%, 86%, 85% after the completion of leaching.
6. the method for a kind of synthetical recovery uranium niobium tantalum from Ore according to claim 1, it is characterised in that:Step (3) Filtered, washed to leaching ore pulp, leached mud directly mixed and stirred and abandoned after Calx after washing.
7. the method for a kind of synthetical recovery uranium niobium tantalum from Ore according to claim 1, it is characterised in that:Step (4) The mixing organic faciess constituted using P204, TBP and sulfonated kerosene are directly separated to the uranium in leachate, and uranium extraction rate is more than 99%;Load uranium organic faciess obtain uranium qualifying liquid by existing anti-extraction process and Jing precipitations are obtained " 111 " product;Described " 111 " product is sodium diuranate.
CN201611233203.0A 2016-12-28 2016-12-28 Method for comprehensively recovering uranium, niobium and tantalum from ore CN106676291A (en)

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