• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:

    公开号:SU1205778A3
    申请号:SU802885203
    申请日:1980-02-26
    公开日:1986-01-15
    发明作者:Потро Жан-Марк
    申请人:Рон-Пуленк Эндюстри (Фирма)；
    IPC主号:
    专利说明:

    The uranium in the organic phase is 20-3000 mg / l, preferably 50-500 mg / l.
    8. Method according to any one of claims 1 to 7, characterized in that a solution of phosphoric or hydrochloric acid is used as the aqueous extraction solution of the third cycle.
    9. The method according to claim 1, wherein using the comfort of a second extraction solution containing iron ions (I).
    10. The method according to claim 9, characterized in that use an aqueous solution of the second extraction with a content of 0.5-100, -O g / l of iron compounds G O.
    1. The method according to claims 1-10, about tl and the fact that the ratio of the consumption of the organic phase of the first extraction to the aqueous solution of the second extraction is 20-60,
    12. The method according to claims 1-11, about tl and - that - by the fact that the additional oxidation of uranium (IV) to uranium iVI by the action of hydrogen peroxide, air or oxygen is carried out at elevated pressure.
    13. The method according to claims 1-12, about tl and is due to the fact that the composition of the organic extraction phase of the first cycle is used as the organic extraction phase of the second cycle.
    one
    This invention relates to methods for extracting uranium from phosphoric acid obtained after leaching uranium-containing ores.
    The method of extracting uranium (yi) contained in crude phosphoric acid, in the first cycle, involves treating the purified phosphoric acid through an organic extraction phase to extract uranium (Vj) but extracting little uranium (w), followed by phase separation; back extraction of the obtained organic phase enriched in uranium (VI)
    205778
    14. A method according to claim 1, characterized in that the ratio of the flow rate of the aqueous solution of the third cycle to the flow rate of the organic phase of the second cycle is 0.2-3.0.
    15. Method according to Claim 1, characterized in that during the washing of the organic phase of the second cycle. use a solution with a titer equal to the titer of an aqueous solution of the third cycle.
    16. The method according to claims 1-15, about tl and is that the amount of iron extracted in the first cycle with an aqueous solution of the third cycle is equal to the amount of iron extracted in the third cycle by the organic phase of the second cycle.
    7. The method according to claim, characterized in that the amount of iron extracted from the organic phase of the first cycle with the aqueous solution of the third cycle is equal to the amount of iron in the solution taken from the aqueous solution after contact with the organic phase of the second cycle.
    18. Method 1, characterized by the fact that the recycling of the solution to the precipitation stage is carried out after adjusting the solution titer for carbonate and ammonium ions.
    9. The method according to claims 1-18, about tl and - the fact that the process is carried out in the anode and cathode chambers of one electrolyzer.
    by means of an aqueous solution of secondary extraction of uranium (VJ containing a redox agent in a reduced state, reducing uranium () to uranium (W), followed by phase separation and recycling of the uranium depleted organic phase into the phosphoric acid extraction stage; oxidation of the specified phase an aqueous solution enriched in uranium (VJ, due to which uranium (iy is oxidized to uranium (V () and redox in the second cycle is the treatment of the specified aqueous solution by means of the second extraction phase of uranium (Vf), followed by phase separation, washing the organic phase enriched in uranium ((y) with water or acid t, followed by separating the purified organic phase, reducing uranium by treating the purified organic phase with an aqueous solution containing carbonate ions and ammonium, due to which ammonium uranyl tricarbonate is precipitated in the aqueous phase, the recycling of the organic phase depleted in uranium depleted by the previous extraction, if necessary, after its reduction extractive form. In the third cycle, in which the aqueous solution obtained by reverse extraction in the first cycle, is processed completely in the anode chamber of the electrolyzer with a separator under direct voltage, collecting the aqueous phase containing uranium in the form 1 (U1) and oxidation-reducing; an oxidizing agent in an oxidized state, if necessary, in addition to oxidizing in and (VI) by exposure to a small amount of an oxidizing agent, and, if necessary, re-adjusting its titer of complexing acid; process the solution by means of the extraction phase of the second cycle; then, the resulting aqueous phase in the cathode chamber of the electrolyzer C is treated with a separator under direct current voltage by recycling it to the back extraction stage of the first cycle, resulting in the aqueous solution being circulated into the water. closed loop between the first and second cycles.
    The initial phosphoric acid is usually phosphoric acid cheese, obtained by treating phosphate ores with sulfuric acid after filtration, if necessary, after pretreatment with clarification and stabilization with respect to organic pollutants and mineral contaminants, and containing uranium (VI). In the first cycle, phosphoric acid is subjected to extraction through the orgnaic phase, extracting uranium ().
    /
    The organic phase of extraction of this first contains extractant
    25
    05778
    uranium ions (yt), which extracts a small amount of uranium. Gu), Extractant of this type contains cationic extractants, for example, mono-5 dialkylphosphoric, alkylphosphonic, alkylpyrophosphoric, alkylphenylphosphonic acids, used individually or in a mixture.
    For the extraction of uranium is used
    10 a mixture of di- (2-ethyl-hexy) phosphoric acid with trioctylphosphine oxide. The mixture may also contain anionic extractants, for example, secondary or tertiary alkylamines, insoluble
    15 in water, and extracts of neutral 1 character, for example, trialkyl phosphates.
    The organic extraction phase contains, if necessary,
    2 organic diluent, inert with respect to extractants, to improve the hydrodynamic properties of the organic phase. Many organic solvents and their mixtures can be used as a diluent, i.e. aliphatic hydrocarbons such as kerosene, aromatic hydrocarbons, halogenated hydrocarbons and petroleum ethers, etc. The concentration of the extractant in the diluent varies from 0.05 M to 100%. However, extractant solutions are commonly used. In case of using extractant in combination with synergistic extraction agent
    35 the molar ratio of the solution is increased from 0.1 to 2 for the extractant and from 0.01 to 2 for the synergistic agent.
    Extraction of the original phosphoric
     acids are carried out in the usual manner in a liquid-liquid contacting device. This contacting can be carried out in the mixer x-settlers, in vacuum columns
    45 with a nozzle or impulse, and the contact can be made by a coil or counter flow. The temperature can vary from 20 to, preferably a temperature of about 50 ° C.
    50 The cost ratio of the organic extraction ratio to the starting acid is 0.2-5.
    After separation of the phases, the organic phase contains uranium in oxidation degree 55 (v () (according to conditions
    the preparation of this solution, as well as other chemicals, depending on the conditions of its preparation.
    thirty
     In particular, phosphoric acid and other metal anions and cations, such as AE, Ee, Ti, V, etc. low concentration. The concentration of uranium in the organic phase is usually 20-3000 mg of uranium metal per liter of phase, preferably 50-500 mg per liter.
    In the second phase of this first cycle, the organic phase enriched in uranium (v) is brought into contact with an aqueous solution of secondary extraction, which is part of the third cycle.
    The aqueous solution usually contains a strong complexing acid, such as phosphoric or hydrochloric or other acids, or mixtures thereof, with the limitation that the presence of these acids does not cause the precipitation of uranium. The aqueous solution also contains a redox reducing agent for uranium (Vt) in uranium (IVJ, and the agent is in a reduced state. The electrochemical potential of this redox pair in the aqueous solution is lower than the uranium pair (V | j - uranium (y) in - the indicated solution. A typical redox pair is an iron (III) - iron (II) pair. Therefore, when using this pair, the aqueous solution contains iron in the oxidation state (). To shift the equilibrium between the reactions uranium ions. SI) and Fe ((i) and uranium (y) and Fe (III) in a direction favorable for the production of U (W) ions, it is necessary that the solution contains a significant excess of iron ions (and) in comparison with uranium ions. The concentration of iron in the oxidation state (c) in the solution is 0.5-100 g per liter. The concentration of sapnic acids in the solution can vary widely. However, in practice, to maximize the depletion of uranium in the organic solution the concentration should be selected depending on the specificity of the phases used and on the temperature, B tea, and when kompleksoobrazuyuscha strong acid aqueous solution is phosphoric acid, the concentration in the solution should be in the range 18-70% ,, preferably
    0
    five
    g
    O
    ir
    five
    0
    more than 28 wt.% P, Og. The solution may also contain iron ions in the oxidation step () Tj); ratio of concentrate. The radios of iron ions (ii) to the concentration of iron ions (JTj) can vary widely. However, in practice, a value greater than 0.1 is used, but preferably it is. must be greater than 2.
    The organic phase containing uranium in the oxidation state (Vlj and the aqueous solution is brought into contact with each other. The contact temperature is 20-80 ° C, preferably 5 ° C.
    The ratio of the flow rate of the organic phase to the aqueous extraction solution entering the contact zone should be kept as high as possible in order to extract uranium as a concentrated solution, preferably 20-60 °. This interval does not take into account possible internal recycling in the apparatus.
    In the course of contacting, the equilibrium distribution of uranium (V) with the organic phase and the aqueous solution is established quickly, while the recovery of uranium (in an aqueous solution by means of a reducing agent is slow. The knowledge of this reduction kinetics and isotherms of the distribution of uranium (Vf) and uranium (W) between both phases allows different contact parameters to be adjusted in order to obtain the maximum extraction result.
     After contacting and separating the phases, the uranium-depleted organic phase is recycled to the extraction of the starting phosphoric acid in the form of a circulation loop constituting the first cycle of the invention,
    The aqueous phase 5 containing the uranium ions (SV), the oxidizing-reducing agent in the partially oxidized state, is completely fed into the anode chamber of the electrolyzer with a separator under direct current voltage, as a result of which the aqueous phase containing uranium is mainly collected in the form of uranium (I) and / redox agent in the oxidized state,
    The electrolyzers used to implement the proposed method are the known electro /
    separators with separators. As a separator, it is possible to use a porous material, for example, ceramics, or a plastic material, the porosity of which is provided by sintering or by introducing a porous binder, or an ion-exchange membrane, it is preferable to use a cation-exchange membrane consisting of a perforated polymer with sulfonic acid groups. The anodes are made of graphite or a metal with an electroactive coating, and the cathodes are made of various metals, such as platinum, lead, or alloys. The configuration of these cells is flat with a large one. electrode surface and with a small gap between the electrodes. It is preferable to use a battery of electrolyzers installed in series in a multi-chamber filter-type device. In this embodiment, the feeding of the cathode chambers can be carried out either sequentially or in parallel in order to control the flow of fluid in each element. To promote electrochemical reactions, it is advisable to increase the active surface of the electrodes or to cause additional mixing of the solutions by means of a set of partitions. The power supply of the anode chambers is also carried out in series or in parallel. In addition, to balance the pressures in both chambers, it is possible to ensure the recycling of the effluent solution.
    A particular case of the proposed method is the use of anode and cathode chambers, combined with a separator under direct current voltage.
    Example. Unpurified phosphorus-. wet acid, pretreated by stabilizing organic and mineral substances, containing 30 wt.% and 100 mg / l of uranium (W) at a flow rate of 96 is introduced into an extractor, which is a mechanically agitated column, to which the solution is introduced. 0.5 mol of di- (2-ethylhexyl) phosphoric acid and .0.125 mol of trioctylphosphine oxide in kerosene, at a rate of A8, carried out the entire process at 50 s.
    057788
    The organic phase enriched in uranium enters the secondary extraction apparatus, in which the temperature is maintained at 55 ° C. In the secondary extraction apparatus, it contacts with an aqueous solution containing: 30 wt.% PjOs; 23.6 g / l of iron ions; CI) ;. 6.1 g / l of iron ions (| G |) at flow
    10 1.3.
    An organic stream is recycled in the apparatus. The resulting water flow feeds all seven anode chambers of the battery cell with a membrane consisting of perfluoro-sulfopolymer. These chambers are sized with flat graphite electrodes and are equipped with staggered electrodes.
    2Q in order with partitions that allow the electrolyte to lengthen and increase its speed. The gap between the anode and the membrane is 5 mm. In all the cathode chambers phosphorus acid is circulated with a titer of 30% at a flow rate of 1.8 M / h, from which hydrogen is released. Flat electrodes made from Inkolo are 5 mm from the membrane. A constant current of 6800 A is applied to the electrolytic cell with a voltage of 2.9 V that is installed on the clamps. Hydrogen peroxide is supplied to the aqueous stream leaving the anode chambers with a 70% weight concentration at a flow rate of 0.19 kg / h, and
     the resulting stream containing 7 g / l of uranium (V () and 30 g / l of iron (W)) goes to an extraction apparatus consisting of six mixer-sumps, in which
     temperature, and goes to supply to all fifteen cathode chambers a battery of electrolyzers with a perfluoro-sulfopolymer membrane. cameras of size I MV m contain
     Lead flat electrodes are equipped with staggered walls arranged to increase the electrolyte path and increase its speed. Distance
    50 between the cathode and the membrane 5 mm. In all fifteen cathode chambers, phosphoric acid with a content of 30% PJ 05 is circulated at a flow rate of 1.8, from which hydrogen is extracted. Flat electrodes of platinum ruthenium alloy on titanium are 5 mm from the membrane. Direct current is applied to the cell.
    14700 A at a voltage of 2.9 V.
    A stream with a flow rate of 2.1 organic extraction phase of 0.3 mol NVENR and 0.075 mol / TOPO is introduced into the extraction apparatus of the tacles. in kerosene. The effluent organic phase enters the flushing battery containing three mixer-settlers, where it is flowed at a flow rate of 0.21 water leaving the highly dilute phosphoric acid solution containing 0.75% PfiOs- The washed organic phase enters the secondary extractives (ai, consisting of two mixer-settlers, where a molar solution of ammonium carbonate 0.5 mol with a passage of 100 l / h and an aqueous solution of ammonium carbonate 2 mol at a consumption of 4.2 is brought into contact. The organic phase exhausted by uranium subjected to reg generation in an apparatus consisting of a mixer-settler by means of an aqueous solution of sulfuric acid with a concentration of 25 wt.% at a flow rate of 2.1 m / h. Assembled the editor A.Lezhnin
    Compiled by O. Golyzhnikova
    Tehred I.Astalosh Corrector I. Erdeyi
    8551/62
    Circulation 567Subscribe
    VNIIPI USSR State Committee
    for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5
    Branch PIP Patent, Uzhgorod, Proektna St., 4

    ten
    15
    205778 O
    Mixing solution at a flow rate of 2.2 m / l, titer 10.7 kgMNz / h,
    The aqueous suspension is filtered, the mother liquors are recycled, the cake 5 is calcined in order to obtain Uj Og.
    The daily consumption of the installation capacity of 300 thousand tons. per year for the treatment of phosphoric acid, expressed in, is: iron - an insignificant amount; hydrogen peroxide at a concentration of 70%. on the basis of the efficiency of electrolytic oxidation of uranium 90% - 4.5 KG1 electricity - 1500 kWh
    As a variant of this example, you can use a battery of electrolyzers with one separator. The chambers are separated by a membrane made of perfluoro-sulfopolymer with a gap of 5 mm between the electrode and the membrane. A direct current A is applied to the cell with a voltage of 2.9 V.
    20
    The daily power consumption is then reduced to 1020 kW.
    权利要求:
    Claims (19)
    [1]
    1. METHOD FOR EXTRACTION OF URANIUM FROM PHOSPHORIC ACID, including extraction of uranium (VI.) With a mixture of di-2-ethylhexylphosphoric. acids and trioctylphosphine oxides in a diluent at 25-65 ° C (first cycle), reextraction of uranium (VI) with simultaneous reduction of uranium (bonds) to uranium (IV.) by the action of iron (II), oxidation of uranium (Tu) to uranium (vi ) in one phase, extraction of the aqueous solution with the organic phase of the first extraction (second cycle), separation of the phases, washing the organic phase containing uranium (V £) with an acid and / or water solution, reducing uranium with a solution of ammonium carbonate from the organic phase, separating ammonium uranyl tricarbonate and recycling the solution, characterized in that In order to reduce energy consumption, the oxidation of uranium (] V) is carried out in the anode chamber of an electrolyzer with a separator under direct current voltage, with additional oxidation of uranium (7y) to uranium (U1) by the action of hydrogen peroxide, air or oxygen, the resulting aqueous solution, containing uranium (yy), is subjected to reduction in the cathode chamber of the same electrolyzer (third cycle), washing of the organic phase of the second extraction is carried out with a solution of phosphoric acid with a concentration of 1870 wt.%, not containing iron, and then with water, washing the intramural solution is combined with the aqueous solution of the third cycle and brought into contact with the organic phase for a second extraction, and the amount necessary to maintain a constant flow rate of the solution in the cycle is taken from the obtained aqueous solution.
    [2]
    2. The method of pop. 1, characterized in that the concentration of the initial phosphoric acid is 20-60 wt.% And the uranium content in it is 30-300 mg / l.
    [3]
    3. The method of pops 1 and 2, characterized in that as the organic phase of the first cycle using a solution of secondary or tertiary amines, preferably tributyl phosphate.
    [4]
    4. The method according to claims 1 to 3, characterized in that aliphatic or aromatic hydrocarbons, preferably kerosene, are used as a diluent.
    [5]
    5. The method according to claims 1-3, with the fact that the concentration of di-2-ethylhexylphosphoric acid in the diluent is 0.1-2.0 M,
    [6]
    6. The method according to claims 1-5, about l and h βίο щ and th with the fact that the concentration of trioctylphosphine is 0.01-
    2.0 M.
    [7]
    7. The method according to claims 1 to 6, with the exception of the fact that the concentration .1205778 of uranium in the organic phase is
    20-3000 mg / L, preferably SOSOO mg / L.
    [8]
    8. The method according to claims 1 to 7, characterized in that a solution of phosphoric or hydrochloric acid is used as an aqueous solution of extraction of the third cycle.
    [9]
    9. The method according to π.1, characterized in that they use an aqueous solution of the second extraction containing iron ions (U).
    [10]
    10. The method according to claim 9, characterized in that they use an aqueous solution of the second extraction with a content of 0.5-100.0 g / l of iron compounds to it).
    [11]
    11. The method according to claims 1-10, wherein the ratio of the flow rate of the organic phase of the first extraction to the aqueous solution of the second extraction is 20-60.
    [12]
    12. The method according to claims 1-11, wherein the additional oxidation of uranium () to uranium (VI) by the action of hydrogen peroxide, air or oxygen is carried out at elevated pressure.
    [13]
    13. The method according to claims 1-12, wherein the composition of the organic extraction phase of the first cycle is used as the organic extraction phase of the second cycle.
    [14]
    14. The method of pop. 1, characterized in that the ratio of the flow rate of the aqueous solution of the Third cycle to the flow rate of the organic phase of the second cycle is 0.2-3.0.
    [15]
    15. The method of pop. 1, characterized in that when washing the organic phase of the second cycle. use a solution with a titer equal to the titer of an aqueous solution of the third cycle.
    [16]
    16. The method according to claims 1-15, wherein the amount of iron extracted in the first cycle with an aqueous solution of the third cycle is equal to the amount of iron extracted * in the third cycle with the organic phase of the second cycle.
    [17]
    17. The method of pop. 1, characterized in that the amount of iron extracted from the organic phase of the first cycle with an aqueous solution of the third cycle is equal to the amount of iron in the solution taken from the aqueous solution after contact with the organic phase of the second cycle.
    [18]
    18. The method of pop. 1, characterized in that the solution is recycled to the precipitation stage after the titer of the solution is regulated by carbonate and ammonium ions.
    [19]
    19. The method according to claims 1 to 18, wherein the process is carried out in the anode and cathode chambers of one electrolyzer.
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    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    FR1397587A|1964-05-04|1965-04-30|Le Ministre De La Defense|Improvements in uranium extraction processes|
    US3616276A|1969-04-14|1971-10-26|Allied Chem|Process for changing the valence of a metal of variable valence in an organic solution|
    US3737513A|1970-07-02|1973-06-05|Freeport Minerals Co|Recovery of uranium from an organic extractant by back extraction with h3po4 or hf|
    US3711591A|1970-07-08|1973-01-16|Atomic Energy Commission|Reductive stripping process for the recovery of uranium from wet-process phosphoric acid|
    US3770612A|1970-08-24|1973-11-06|Allied Chem|Apparatus for electrolytic oxidation or reduction, concentration, and separation of elements in solution|
    US3835214A|1972-08-15|1974-09-10|Atomic Energy Commission|Oxidative stripping process for the recovery of uranium from wet-process phosphoric acid|
    US3966872A|1973-11-01|1976-06-29|Westinghouse Electric Corporation|Coupled cationic and anionic method of separating uranium|
    DE2449590C3|1974-10-18|1980-06-12|Kernforschungszentrum Karlsruhe Gmbh, 7500 Karlsruhe|Process for the purification of actinides in low oxidation states|
    US4105741A|1976-03-08|1978-08-08|Freeport Minerals Company|Process for recovery of uranium from wet process phosphoric acid|
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    US4234393A|1979-04-18|1980-11-18|Amax Inc.|Membrane process for separating contaminant anions from aqueous solutions of valuable metal anions|
    US4279705A|1980-02-19|1981-07-21|Kerr-Mcgee Corporation|Process for oxidizing a metal of variable valence by constant current electrolysis|US4652432A|1981-02-26|1987-03-24|Prodeco, Inc.|Process for recovering uranium using an alkyl pyrophosphoric acid and alkaline stripping solution|
    US4652431A|1981-02-26|1987-03-24|Prodeco, Inc.|Process for recovering uranium using an alkyl pyrophosphoric acid and alkaline stripping solution|
    CA1194320A|1981-06-15|1985-10-01|Paul L. Valint, Jr.|Liquid membrane process for uranium recovery|
    CA1195508A|1981-06-15|1985-10-22|Paul L. Valint, Jr.|Liquid membrane process for uranium recovery|
    FR2539549B1|1983-01-17|1988-10-14|Rhone Poulenc Chim Base|PROCESS FOR GLOBAL RECOVERY OF URANIUM, YTTRIUM, THORIUM AND RARE EARTH CONTAINED IN AN ORGANIC PHASE|
    US4578249A|1983-09-02|1986-03-25|International Minerals & Chemical Corp.|Process for recovery of uranium from wet process H3 PO4|
    GB8719045D0|1987-08-12|1987-10-07|Atomic Energy Authority Uk|Liquid treatment process|
    US4855081A|1988-06-07|1989-08-08|Nutech, Inc.|Method for decontaminating conventional plastic materials which have become radioactively contaminated, and articles|
    US5419880A|1993-10-08|1995-05-30|Falconbridge, Ltd.|Controlled acid-strong acid strip process|
    JPH11199541A|1997-11-14|1999-07-27|Daicel Chem Ind Ltd|Recovery equipment and recovery method for sorbic acid|
    ITBO20010108A1|2001-02-28|2002-08-28|Azionaria Costruzioni Automati|MACHINE FOR FILLING CONTAINERS|
    KR101389877B1|2008-07-31|2014-04-29|우르텍, 엘엘씨|Extraction of uranium from wet-process phosphoric acid|
    US8883096B2|2008-07-31|2014-11-11|Urtek, Llc|Extraction of uranium from wet-process phosphoric acid|
    WO2014018422A1|2012-07-21|2014-01-30|K-Technologies, Inc.|Processes for the recovery of uranium from wet-process phosphoric acid using a single dual or dual single cycle ion exchange approaches|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR7905155A|FR2450233B1|1979-02-28|1979-02-28|
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