CN103981364A - Uranium-vanadium separation method - Google Patents
Uranium-vanadium separation method Download PDFInfo
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Abstract
The invention discloses a uranium-vanadium separation method for separating and recycling uranium metal and vanadium metal from an acid lixivium of uranium-vanadium ore or other uranium-vanadium paragenic (associated) ore containing uranium and vanadium. The uranium is extracted and separated by using N235, the vanadium is extracted and separated by using P204, and the potential and the pH value are adjusted after the uranium is extracted, so that the precipitate amount and the loss of vanadium are reduced, and the content of uranium in a vanadium extraction raw liquid is reduced. By adopting the technical method disclosed by the invention, high-efficiency uranium-vanadium separation is achieved, a uranium reextraction liquid does not contain vanadium, the concentration of uranium in a vanadium reextraction liquid is less than 1mg/L, and a prepared uranium-vanadium product can meet relevant standards.
Description
Technical field
The invention belongs to hydrometallurgy field, relate to a kind of uranium vanadium separation method, be specifically related to a kind of from uranium navajoite leach liquor the technological method of SEPARATION OF URANIUM and vanadium.
Background technology
The separated of uranium and vanadium can be realized with ion exchange method, solvent extration and selective precipitation, in acid leaching solution, vanadium exists with the form of tetravalence and pentavalent conventionally, and during by ion-exchange or Solvent Extraction Separation, the selectivity of uranium and vanadium depends on the valence state of vanadium.Because tetravalence vanadium can not form anion complex, so it can not be adsorbed by anionite-exchange resin, can not be extracted by amine extractant, yet alkylphosphonic acid carboxylic acid is cationic extraction agent, it can extract tetravalence vanadium and hexavalent uranium simultaneously.
Under certain condition, uranium can replace the vanadium being extracted, by control pH value, water and organic phase mutually when in organic phase the concentration of extraction agent just can make uranium and vanadium reach good separated.In addition, also simultaneously Extraction of Uranium and vanadium, and then the back extraction of selectivity substep fetch separated they.Pentavalent vanadium in acid leaching solution can come by ion exchange method separated, and pentavalent vanadium, by the uranium replacing on resin, makes uranium vanadium be able to separation, adopt in addition special ELUTION METHOD also can be from resin preferential Elution of Uranium and vanadium, to improve uranium vanadium separating effect.The amine extracted extraction difficulty that will compare uranium to the extraction of pentavalent vanadium, is mainly that extraction efficiency and condition of phase separation are poor, approaches at 2.0 o'clock extract at pH, can improve the extraction efficiency of vanadium.
Abroad from acidic solution, the typical separation method of SEPARATION OF URANIUM vanadium comprises two kinds at present:
A kind of is alkylphosphonic acid carboxylic acid stepwise solvent extraction uranium and vanadium:
Extraction of Uranium and vanadium organic phase used is two-2 ethylhexyl phosphoric acid (D
2eHPA), the mixture of tbp (TBP) and high flash point kerosene, during Extraction of Uranium, D
2the concentration of EHPA and TBP is 4%.During extracting vanadium, D
2eHPA concentration approximately 7.5%, TBP concentration approximately 3%.Because ferric iron can be by D
2eHPA extraction, before Extraction of Uranium, is first reduced, and adjusts be about-200mV of current potential, and pH value is lower than 1.7~1.8, and extraction is carried out in four-stage counter-current mixer-settler, and load organic phases is washed away vanadium by dilute sulfuric acid dip, uses 12%Na
2cO
3reextraction uranium, equipment is the band cone mixer-settler at the end, a small amount of iron cpd being precipitated out while being convenient to separated reextraction, the about 30g/L of anti-stripping agent uranium-bearing, send uranium settling system.
The method of this SEPARATION OF URANIUM vanadium, the vanadium raffinate water that contains after Extraction of Uranium regulates pH to 1.8~2.2 with ammonia, and five sections of mixer-settlers are used in vanadium extraction, and raffinate water is containing the about 150mg/L of vanadium, and 30% sulfuric acid reextraction vanadium for load organic phases, obtains 100~120g/LV
2o
5anti-stripping agent, send vanadium settling system.
Another kind is first with Trifatty amine Extraction of Uranium, use alkylphosphonic acid carboxylic acid extracting vanadium again:
The pH of solution is adjusted to 1.0~1.2 with sodium hydroxide or ammoniacal liquor, delivers in 4 grades of mixer-settlerss and extract uranium, putting forward uranium organic phase is 5% Trifatty amine+92.5% kerosene+2.5% isodecyl alcohol, uranium load organic phases Na
2cO
3strip, anti-stripping agent send uranium settling system.
In this method, the water of carrying after uranium enters current potential regulating tank, with iron powder the current potential of solution is adjusted to-below 150mV, make most of ferric iron be reduced into ferrous iron, vanadium is also reduced into tetravalence vanadium, and the object of reduction is to reduce the rate of recovery that iron is extracted to improve vanadium, then with ammoniacal liquor, pH value of solution is adjusted to 2.0, send into 5 grades of mixer-settlers and extract vanadium, putting forward uranium organic phase is 6% 2-2-ethylhexyl phosphoric acid+91% kerosene+3% isodecyl alcohol, at first 4 grades, keeps pH2.0.Vanadium load organic phases is sent into reextraction groove, uses 15%H
2sO
4strip, containing vanadium anti-stripping agent, send settling system.
In the uranium resources of having found on China Hunan, Shaanxi and other places, a part is uranium navajoite, and also some is uranium navajoite to overseas uranium resources development project, and in addition, in a large amount of bone coal navajoites of China, a part also contains uranium.Prior art is commonly used sulfuric acid and is made leaching agent, obtains the leach liquor of acid uranium-bearing vanadium, reclaim uranium and vanadium wherein, must carry out the separated of uranium and vanadium to leach liquor.Therefore and the similar uranium navajoite of the temporary untapped mistake of China resource need to provide corresponding uranium vanadium isolation technique method, thereby provide technical support for the uranium navajoite development of resources of China.
Summary of the invention
The problem existing for solving above-mentioned prior art, the invention provides a kind of uranium vanadium separation method, and by N235 Extraction of Uranium and P204 extracting vanadium, the method can realize uranium vanadium high efficiency separation, and the percentage extraction of uranium and vanadium is high, and uranium anti-stripping agent is not containing vanadium; In vanadium anti-stripping agent, uranium concentration is lower than 1mg/L.
In acid leaching solution, uranium is sexavalence, mainly with uranyl sulfate complex anion form, exists, and has Fe in leach liquor
2+exist, the overwhelming majority of the vanadium in leach liquor is tetravalence vanadium, with vanadium acyl cationic form, exist, uranium vanadium separation method provided by the invention is to carry out separation according to its different ions existence form in solution, adopts Trifatty amine extracting and separating uranium, two-2 ethylhexyl phosphoric acid extracting and separating vanadium.
Fig. 1 is uranium vanadium separation process scheme figure of the present invention, the acid leaching solution pH value of uranium-bearing, vanadium is lower than 1.6, as extraction stoste, first use extraction agent Trifatty amine (N235) Extraction of Uranium, without adjusting current potential and pH value, the saturated organic phase that Extraction of Uranium obtains washs with acidified water, washing lotion after washing merges with extraction stoste, saturated organic phase after washing is stripped with sodium carbonate solution, the qualifying liquid input uranium settling system obtaining, and lean organic phase returns to uranium extraction system after acidifying.The raffinate water of Extraction of Uranium obtains vanadium extraction stoste after adjusting current potential and pH value with iron powder, with two-2 ethylhexyl phosphoric acids (P204), carry out vanadium extraction, raffinate water after extracting vanadium returns to leaching or carries out wastewater treatment, the saturated organic phase that extracting vanadium obtains is stripped with sulphuric acid soln, the qualifying liquid input vanadium settling system obtaining, lean organic phase returns to vanadium extracting system.
Technological method of the present invention is:
A uranium vanadium separation method, the method,,, comprises the following steps by two-2 ethylhexyl phosphoric acid extracting and separating vanadium by Trifatty amine extracting and separating uranium lower than 1.6 uranium-bearing vanadium acid leaching solution pH value:
1) take Trifatty amine as extraction agent, directly to acid leaching solution Extraction of Uranium, obtain the raffinate water after uranium saturated organic phase and Extraction of Uranium;
2) to step 1) the uranium saturated organic phase that obtains strips, and the anti-stripping agent obtaining is uranium qualifying liquid;
3) to step 1) raffinate water after Extraction of Uranium adjusts redox potential and pH value simultaneously, make redox potential after adjusting-below 200mV, pH value is 2.0~3.0, obtain vanadium and extract stoste;
4) to step 3) vanadium that obtains extraction stoste extracts, and extraction agent is two-2 ethylhexyl phosphoric acids, obtains the raffinate water after vanadium saturated organic phase and extracting vanadium;
5) to step 4) the vanadium saturated organic phase that obtains strips, and the anti-stripping agent obtaining is vanadium qualifying liquid.
In above-mentioned uranium vanadium separation method, further:
Step 1) the mixing organic phase that Extraction of Uranium extraction agent used is specifically comprised of 3%~5% Trifatty amine, 3%~15% tbp and sulfonated kerosene, makes the transition with sulfuric acid before extraction.Extraction of Uranium carries out in Pyatyi mixer-settler, and it is 1.0~2.0 that O/A is compared in operation, and be 2~5min duration of contact; Being extracted uranium capacity in the saturated organic phase after uranium is 2.0g/L~4.0g/L, and in raffinate water, uranium content is lower than 5mg/L.
Step 2) in, stripping is that sodium carbonate solution with 100g/L~120g/L is made strippant, in three grades of mixer-settlers, carries out, and two-phase duration of contact is 2~5min, and the about 20g/L~40g/L of uranium concentration of the anti-stripping agent obtaining, containing vanadium.
Step 3) the raffinate water after Extraction of Uranium is adjusted redox potential and pH value by iron powder simultaneously; Also remaining a part of uranium can be removed simultaneously, in the vanadium extraction stoste obtaining, uranium content is down to below 1mg/L, the clear liquid that the precipitation producing while adjusting redox potential and pH value obtains after filtration and vanadium extraction stoste merge for extracting vanadium, and the throw out obtaining returns to leaching system.
Step 4) the mixing organic phase that extracting vanadium extraction agent used is specifically comprised of 10%~20% two-2 ethylhexyl phosphoric acids, 5%~15% tbp and sulfonated kerosene.Extracting vanadium is carried out in 5~10 grades of mixer-settlers, and it is 1.0~2.0 that O/A is compared in operation, and be 5~20min duration of contact; Being extracted vanadium capacity in the saturated organic phase after vanadium is 5.0~7.5g/L, and in raffinate water, content of vanadium is lower than 10mg/L.
Step 5) in, vanadium saturated organic phase being stripped is to make strippant with 120~200g/L sulphuric acid soln, in five~ten grades of mixer-settlers, carries out, and be 3~10min duration of contact; In the vanadium qualifying liquid that reextraction obtains, vanadium concentration 50g/L~70g/L, uranium content is less than 1mg/L.
The invention has the beneficial effects as follows:
The invention provides a kind of uranium vanadium separation method, take Trifatty amine as extraction agent, directly to acid leaching solution Extraction of Uranium; Raffinate water after Extraction of Uranium is adjusted redox potential and pH value simultaneously, obtains vanadium extraction stoste.The present invention adjusts current potential and pH value after Extraction of Uranium, can reduce the loss of uranium and vanadium and reduce the content of uranium, is conducive to vanadium uranium separated.The method can realize uranium vanadium high efficiency separation, and uranium, vanadium percentage extraction are high, and uranium anti-stripping agent is containing vanadium, and " 111 " product of preparation reaches first grade standard promulgated by the ministries or commissions of the Central Government.In vanadium anti-stripping agent, uranium concentration is lower than 1mg/L, and its impurity content of Vanadium Pentoxide in FLAKES product of preparation all can reach metallurgical 98 grades of Vanadium Pentoxide in FLAKES standards, and radionuclide is all lower than nonferrous metal product radioactivity national standard.Technological method provided by the invention can be used for Separation and Recovery uranium metal and vanadium metal from the acid leaching solution of uranium navajoite or other uranium vanadium symbiosis or association ore uranium-bearing vanadium.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the technology of the present invention method.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail, but the scope not limiting the present invention in any way.
Fig. 1 is uranium vanadium separation process scheme figure of the present invention, acid leaching solution is extraction stoste, first use extraction agent Trifatty amine (N235) Extraction of Uranium, without adjusting current potential and pH value, the saturated organic phase that Extraction of Uranium obtains washs with acidified water, and the washing lotion after washing merges with extraction stoste, and the saturated organic phase after washing is stripped with sodium carbonate solution, the qualifying liquid input uranium settling system obtaining, lean organic phase returns to uranium extraction system after acidifying.The raffinate water of Extraction of Uranium obtains vanadium extraction stoste after adjusting current potential and pH value with iron powder, with two-2 ethylhexyl phosphoric acids (P204), carry out vanadium extraction, raffinate water after extracting vanadium returns to leaching or carries out wastewater treatment, the saturated organic phase that extracting vanadium obtains is stripped with sulphuric acid soln, the qualifying liquid input vanadium settling system obtaining, lean organic phase returns to vanadium extracting system.
It is separated that embodiment mono-, two and three all carries out uranium vanadium by uranium vanadium separation process scheme as shown in Figure 1 to the acid leaching solution of uranium-bearing, vanadium, obtains respectively uranium qualifying liquid and vanadium qualifying liquid.
(1) embodiment mono-
The pH of extraction stoste is 1.05, and wherein, uranium content ρ (U) is 537mg/L, and content of vanadium ρ (V) is 4.20g/L, and total iron content ρ (∑ Fe) is 29.8g/L, ferrous iron content ρ (Fe
2+) be 28.3g/L; Organic phase for Extraction of Uranium is 5%N235+8%TBP+87% sulfonated kerosene; The operational condition of Extraction of Uranium is: compare: O/A=1.5, stream than A/O=7, duration of contact 3min.
In the uranium saturated organic phase obtaining after Extraction of Uranium, uranium content ρ (U) is about 3.7g/L; In uranium raffinate water after Extraction of Uranium, uranium content ρ (U) <5mg/L.
The uranium saturated organic phase obtaining after Extraction of Uranium is carried out to uranium reextraction, the sodium carbonate solution that uranium strippant is 150g/L; Reextraction uranium operational condition is: compare O/A=1.5, stream is than O/A=10, and be 3min duration of contact.In the uranium anti-stripping agent obtaining after reextraction uranium, uranium content ρ (U) is about 36g/L, and content of vanadium ρ (V) is about 0mg/L.
It is that consumption is 14kg/m with iron powder that uranium raffinate after Extraction of Uranium is adjusted
3, Eh=-180mV, pH=2.8, obtains vanadium extraction stoste.Organic phase for extracting vanadium is 14%P204+5%TBP+81% sulfonated kerosene; The operational condition of extracting vanadium is for comparing O/A=1.5, and stream is than A/O=1.5, and be 10min duration of contact.In the vanadium saturated organic phase obtaining after extracting vanadium, content of vanadium ρ (V) is about 6.1g/L; In vanadium raffinate water after extracting vanadium, content of vanadium ρ (V) <50mg/L.
The vanadium saturated organic phase obtaining after extracting vanadium is carried out to vanadium reextraction, the sulphuric acid soln that vanadium strippant is 15%; Reextraction uranium operational condition is for comparing O/A=1.5, and stream is than O/A=8, and be 5min duration of contact; In the vanadium anti-stripping agent obtaining after reextraction vanadium, content of vanadium ρ (V) is about 48g/L, and uranium content ρ (U) is about 0.8mg/L, and iron level ρ (Fe) is 4.3g/L.
(2) embodiment bis-
The pH of extraction stoste is 1.25, and wherein, uranium content ρ (U) is 490mg/L, and content of vanadium ρ (V) is 3.25g/L, and total iron content ρ (∑ Fe) is 11.2g/L, ferrous iron content ρ (Fe
2+) be 10.8g/L; Organic phase for Extraction of Uranium is 5%N235+5%TBP+90% sulfonated kerosene; The operational condition of Extraction of Uranium is: compare O/A=1.5, stream is than A/O=8, and be 5min duration of contact.
In the uranium saturated organic phase obtaining after Extraction of Uranium, uranium content ρ (U) is about 3.9g/L; In uranium raffinate water after Extraction of Uranium, uranium content ρ (U) <5mg/L.
The uranium saturated organic phase obtaining after Extraction of Uranium is carried out to uranium reextraction, the sodium carbonate solution that uranium strippant is 100g/L; Reextraction uranium operational condition is: compare O/A=1.5, stream is than O/A=10, and be 2min duration of contact.In the uranium anti-stripping agent obtaining after reextraction uranium, uranium content ρ (U) is about 39g/L, and content of vanadium ρ (V) is about 0mg/L.
It is that consumption is 5.6kg/m with iron powder that uranium raffinate after Extraction of Uranium is adjusted
3, Eh=-165mV, pH=2.6, obtains vanadium extraction stoste.Organic phase for extracting vanadium is 15%P204+5%TBP+80% sulfonated kerosene; The operational condition of extracting vanadium is for comparing O/A=1.5, and stream is than A/O=2.0, and be 12min duration of contact.In the vanadium saturated organic phase obtaining after extracting vanadium, content of vanadium ρ (V) is about 6.4g/L; In vanadium raffinate water after extracting vanadium, content of vanadium ρ (V) <20mg/L.
The vanadium saturated organic phase obtaining after extracting vanadium is carried out to vanadium reextraction, the sulphuric acid soln that vanadium strippant is 15%; Reextraction uranium operational condition is for comparing O/A=1.5, and stream is than O/A=9, and be 8min duration of contact; In the vanadium vanadium anti-stripping agent obtaining after reextraction vanadium, content of vanadium ρ (V) is about 57g/L, and uranium content ρ (U) is about 0.7mg/L, and iron level ρ (Fe) is 1.9g/L.
(3) embodiment tri-
The pH of extraction stoste is 1.45, and wherein, uranium content ρ (U) is 750mg/L, and content of vanadium ρ (V) is 5.10g/L, and total iron content ρ (∑ Fe) is 4.2g/L, ferrous iron content ρ (Fe
2+) be 3.6g/L; Organic phase for Extraction of Uranium is 4.5%N235+5%TBP+90.5% sulfonated kerosene; The operational condition of Extraction of Uranium is: compare O/A=1.5, stream is than A/O=5, and be 3min duration of contact.
In the uranium saturated organic phase obtaining after Extraction of Uranium, uranium content ρ (U) is about 3.8g/L; In uranium raffinate water after Extraction of Uranium, uranium content ρ (U) is <3mg/L.
The uranium saturated organic phase obtaining after Extraction of Uranium is carried out to uranium reextraction, the sodium carbonate solution that uranium strippant is 120g/L; Reextraction uranium operational condition is: compare O/A=1.5, stream is than O/A=10, and be 3min duration of contact.In the uranium anti-stripping agent obtaining after reextraction uranium, uranium content ρ (U) is about 39g/L, and content of vanadium ρ (V) is about 0mg/L.
It is that consumption is 1.9kg/m with iron powder that uranium raffinate after Extraction of Uranium is adjusted
3, Eh=-140mV, pH=2.5, obtains vanadium extraction stoste.Organic phase for extracting vanadium is 17%P204+8%TBP+75% sulfonated kerosene; The operational condition of extracting vanadium is for comparing O/A=1.5, and stream is than A/O=1.5, and be 10min duration of contact.In the vanadium saturated organic phase obtaining after extracting vanadium, content of vanadium ρ (V) is about 7.5g/L; In vanadium raffinate water after extracting vanadium, content of vanadium ρ (V) is about 8mg/L.
The vanadium saturated organic phase obtaining after extracting vanadium is carried out to vanadium reextraction, the sulphuric acid soln that vanadium strippant is 15%; Reextraction uranium operational condition is for comparing O/A=1.5, and stream is than O/A=8, and be 5min duration of contact; In the vanadium anti-stripping agent obtaining after reextraction vanadium, content of vanadium ρ (V) is about 60g/L, and uranium content ρ (U) is about 0.6mg/L, and iron level ρ (Fe) is 0.8g/L.
Claims (8)
1. a uranium vanadium separation method, described method,,, comprises the following steps by two-2 ethylhexyl phosphoric acid extracting and separating vanadium by Trifatty amine extracting and separating uranium lower than 1.6 uranium-bearing vanadium acid leaching solution pH value:
1) with Trifatty amine, make extraction agent, directly to acid leaching solution Extraction of Uranium, obtain the raffinate water after uranium saturated organic phase and Extraction of Uranium;
2) to step 1) the uranium saturated organic phase that obtains strips, and the anti-stripping agent obtaining is uranium qualifying liquid;
3) to step 1) raffinate water after Extraction of Uranium adjusts redox potential and pH value simultaneously, make redox potential after adjusting-below 200mV, pH value is 2.0~3.0, obtain vanadium and extract stoste;
4) to step 3) vanadium that obtains extraction stoste extracts, and extraction agent is two-2 ethylhexyl phosphoric acids, obtains the raffinate water after vanadium saturated organic phase and extracting vanadium;
5) to step 4) the vanadium saturated organic phase that obtains strips, and the anti-stripping agent obtaining is vanadium qualifying liquid.
2. uranium vanadium separation method as claimed in claim 1, it is characterized in that, step 1) the mixing organic phase that Extraction of Uranium organic phase used is specifically comprised of 3%~5% Trifatty amine, 3%~15% tbp and sulfonated kerosene, makes the transition with sulfuric acid before extraction.
3. uranium vanadium separation method as claimed in claim 1, is characterized in that step 1) Extraction of Uranium carries out in Pyatyi mixer-settler, and it is 1.0~2.0 that O/A is compared in operation, and be 2~5min duration of contact.
4. uranium vanadium separation method as claimed in claim 1, is characterized in that step 2) in to strip be that sodium carbonate solution with 100g/L~120g/L is made strippant, in three grades of mixer-settlers, carry out, two-phase duration of contact is 2~5min.
5. uranium vanadium separation method as claimed in claim 1, is characterized in that step 3) raffinate water after Extraction of Uranium adjusts redox potential and pH value by iron powder simultaneously.
6. uranium vanadium separation method as claimed in claim 1, is characterized in that step 4) the mixing organic phase that specifically formed by 10%~20% two-2 ethylhexyl phosphoric acids, 5%~15% tbp and sulfonated kerosene of extracting vanadium organic phase used.
7. uranium vanadium separation method as claimed in claim 1, is characterized in that step 4) extracting vanadium carries out in five~ten grades of mixer-settlers, and it is 1.0~2.0 that O/A is compared in operation, and be 5~20min duration of contact.
8. uranium vanadium separation method as claimed in claim 1, it is characterized in that, step 5) in, vanadium saturated organic phase being stripped is to make strippant with 120~200g/L sulphuric acid soln, in five~ten grades of mixer-settlers, carries out, and be 3~10min duration of contact.
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