CN112553484B - Method for improving flow benefit of uranium extraction by triple-fatty amine leaching - Google Patents

Method for improving flow benefit of uranium extraction by triple-fatty amine leaching Download PDF

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CN112553484B
CN112553484B CN202010928985.XA CN202010928985A CN112553484B CN 112553484 B CN112553484 B CN 112553484B CN 202010928985 A CN202010928985 A CN 202010928985A CN 112553484 B CN112553484 B CN 112553484B
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uranium
leaching
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sulfuric acid
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CN112553484A (en
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周志全
曹令华
任燕
牛玉清
张永明
赵凤岐
舒祖骏
曹笑豪
叶开凯
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Beijing Research Institute of Chemical Engineering and Metallurgy of CNNC
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02—Obtaining thorium, uranium, or other actinides
    • C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
    • C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
    • C22B60/026—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries liquid-liquid extraction with or without dissolution in organic solvents
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction 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
    • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02—Obtaining thorium, uranium, or other actinides
    • C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
    • C22B60/0221—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching
    • C22B60/0226—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors
    • C22B60/0234—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors sulfurated ion as active agent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02—Obtaining thorium, uranium, or other actinides
    • C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
    • C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
    • C22B60/0265—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries extraction by solid resins

Abstract

The invention belongs to the technical field of uranium hydrometallurgy of uranium ores, and particularly relates to a method for improving benefits of a process of uranium leaching extraction by using tri-aliphatic amine. By the method, the sulfuric acid consumption, the ammonia consumption and the ammonium sulfate generation amount in the uranium leaching process of the tri-aliphatic amine can be reduced, the economy is improved, and the emission reduction effect is achieved.

Description

Method for improving flow benefit of uranium extraction by triple-fatty amine leaching
Technical Field
The invention belongs to the technical field of uranium ore hydrometallurgy, and particularly relates to a method for improving flow benefit of uranium extraction by triple aliphatic amine leaching.
Background
Ion exchange and solvent extraction are the main methods for extracting uranium from a uranium leach solution, and both have application characteristics. In one aspect, the ion exchange method is more suitable for systems with lower uranium concentrations, and the solvent extraction method is more suitable for systems with higher uranium concentrations. For leachate with lower uranium concentration, an ion exchange adsorption-leaching-solvent extraction method, namely a leaching extraction process, can be adopted to carry out ion exchange adsorption on uranium from a system with lower uranium concentration to obtain leached qualified liquid with higher concentration, and then solvent extraction is carried out. The method conforms to the adaptation characteristics of ion exchange and solvent extraction to high and low uranium concentrations on one hand, and on the other hand, the problem of conversion from a sodium system to an ammonium system of a solution system after single ion exchange is solved, and uranium ammonium salt is prepared after solvent extraction so as to prepare uranium oxide.
In the leaching and extraction process, high-concentration sulfuric acid is generally adopted to leach the loaded resin to obtain leached qualified liquid, the uranium in the leached qualified liquid is extracted, and then back extraction is performed to obtain back extraction liquid, so that a uranium product is prepared. The extractant is acidic cation extractant, such as D2EHPA, and hydrogen ion association type weakly alkaline tri-fatty amine extractant, such as N235.
The uranium-loaded tri-aliphatic amine organic phase can be subjected to sodium carbonate back extraction, ammonium carbonate back extraction or ammonium sulfate back extraction. Compared with other back extraction methods, the ammonium sulfate back extraction method has low cost, is beneficial to preparing the ammonium salt product of uranium, is the main back extraction method at present, and adopts a multistage countercurrent process, takes ammonium sulfate and ammonia water as back extraction agents, generates the ammonium sulfate through the reaction of the ammonia and sulfuric acid in an organic phase under a proper pH condition, realizes the deprotonation process of the organic phase, and loses the extraction capacity, thereby achieving the purpose of back extraction of uranium.
The tri-fatty amine extractant has the advantages of good uranium selectivity, and the tri-fatty amine extractant has the defects that (1) the extraction capacity is seriously influenced by acidity, and the extraction capacity is lower under the condition of high-concentration sulfuric acid. The disadvantage (2) is that it can extract a large amount of sulphuric acid when extracting uranium, and then the sulphuric acid and ammonia water are subjected to acid-base reaction when back extracting to generate ammonium sulfate which needs to be disposed. The problems of low uranium concentration, high sulfuric acid consumption, high ammonia consumption, high ammonium sulfate generation amount and treatment need are the problems of the existing triple-fatty amine leaching process, and the method aims at solving or improving the problem and improving the economic benefit.
Disclosure of Invention
In view of the above disadvantages, the main object of the present invention is to provide a method for improving the benefit of a uranium leaching process with tri-aliphatic amine, which can reduce the consumption of sulfuric acid, the consumption of ammonia, and the generation of ammonium sulfate in the uranium leaching process with tri-aliphatic amine, improve the economy, and achieve the effect of emission reduction.
The technical scheme of the invention is as follows:
lifting deviceA method for extracting uranium process benefit by leaching high-tri-fatty amine comprises the step 1, leaching crushed ore by sulfuric acid, setting acid consumption as Q and unit as kg/t ore, leaching in situ by taking unit as kg/kg uranium, and obtaining leachate uranium concentration as C 1 In units of g/L, the sulfuric acid concentration is C H1 The unit is g/L, 1t ore, or 1kg uranium in the leaching liquid leached in situ, and the volume of the leaching liquid is V 1 The unit is L;
step 2, adsorbing the leaching solution by using strong basic resin to obtain saturated resin, wherein the volume of the adsorption tail solution is V 2 The unit is L, then leaching is carried out by adopting high-concentration sulfuric acid, and the concentration of the sulfuric acid is C HF3 In units of g/L, C HF3 Not less than 80 g/L; obtaining qualified leached liquid with the uranium concentration of C 3 In units of g/L, the sulfuric acid concentration is C H2 In g/L, the volume of the leaching solution is V 2 The unit is L;
step 3, setting the volume as V 2-2 The unit is L, the absorption tail liquid and the eluted qualified liquid are mixed, the extraction stock solution is adjusted, and the uranium concentration of the adjusted extraction stock solution is C 4 In units of g/L, the sulfuric acid concentration is C H4 In g/L, the volume of the leaching solution is V 4 Diluting the uranium concentration in the leached qualified liquid by the adsorption tail liquid with the unit of L, wherein the dilution multiple is DR;
dilution factor DR ═ V 4 /V 3 ＝(V 2-2 +V 3 )/V 3 ＝V 2-2 /V 3 +1；
Step 4, carrying out multi-stage countercurrent extraction on the adjusted extraction stock solution by using tri-aliphatic amine to obtain a saturated organic phase with the uranium concentration of C O In units of g/L, the sulfuric acid concentration is C HO The unit is g/L, and the volume of the loaded organic phase is V O The unit is L, stripping is removed;
step 5, the uranium concentration of the raffinate obtained by the multi-stage countercurrent extraction is C 5 In units of g/L, the sulfuric acid concentration is C H5 In g/L, the volume of the leaching solution is V 5 In the unit of L, wherein V 5-1 Unit is L, return eluent preparation, V 5-2 The unit is L, and the leaching agent is returned for preparation;
step (ii) of6, the preparation requirement of the back extractant meets the following condition, and the sulfuric acid is supplemented in the preparation process to ensure that the concentration of the sulfuric acid reaches C HF1 ；V 5-2 Need to satisfy V 2-2 ≤V 5-2 The conditions of (a);
step 7, carrying out multi-stage counter-current back extraction on the loaded organic phase, wherein the back extraction agents are ammonium sulfate and ammonia, and controlling the pH of each stage to be 3.8-5 to obtain a back extraction liquid;
step 8, adding ammonia into the back extraction liquid to precipitate ADU, and performing solid-liquid separation to obtain a product ADU and a mother liquid, wherein the mother liquid contains ammonium sulfate and the volume of the mother liquid is V 7 In the unit of L, wherein V 7-1 In the unit L, as stripping agent back to trans, V 7-2 The unit is L, and the waste liquid is discharged and treated;
step 9, when C H5 ×V 5 When the frequency is more than or equal to 1000Q,
it should satisfy:
Figure BDA0002669499760000031
or
Figure BDA0002669499760000032
Wherein zeta is 1-1.2;
wherein C is H5 * When DR is 1, i.e. V 2-2 0 or V 2-B C when equal to 0 H5 ；
Step 10, when C H5 ×V 5 When the frequency is less than 1000Q,
it should satisfy:
Figure BDA0002669499760000041
in the step 1, the broken and ground ore is leached in situ by adopting sulfuric acid.
In the step 3, DR is 1.2-4.
In said step 3, DR >1 is controlled.
In said step 3, V 2-2 >0。
And in the step 3, water is distributed through a public pool, so that the water balance and DR >1 are realized.
In step 9, ζ was 1.08.
The invention has the beneficial effects that:
(1) when DR is more than 1, the qualified leaching solution is doped with other solutions, but the selectivity of the tri-fatty ammonium is good, so that the product quality is not obviously reduced compared with that when DR is 1, and an ADU product with equivalent quality can still be obtained.
(2) After DR is increased (DR is more than or equal to 1), the uranium concentration in the extracted organic phase is obviously increased, and the acid concentration is reduced. The organic phase treatment capacity is reduced, and the production pressure of the back extraction equipment is reduced.
(3)DR>1 and when proper parameters are selected, the consumption of the sulfuric acid is 1-7 t/t less than that of the sulfuric acid when DR is 1, and ammonia (100 percent of NH) is used 3 Measured) consumption is 1-5 t/t less than that when DR is 1, and the amount of waste ammonium sulfate generated is 2-10 t/t less than that when DR is 1. The benefit is obvious, and the specific data are changed according to system parameters.
(4) When the parameter flow with DR >1 is adopted, the reconstruction and operation cost is not obviously increased compared with DR equal to 1.
Drawings
Fig. 1 is a flow chart 1 of a method for improving flow benefit of uranium leaching by using tri-aliphatic amine according to the present invention.
Fig. 2 is a flow chart 2 of a method for improving the efficiency of a uranium extraction process by extracting tri-aliphatic amine.
In the figure: c Number of Denotes the uranium concentration, C H number Denotes the sulfuric acid concentration, V Number of Denotes volume, C O Denotes the concentration of uranium, C, in the organic phase HO Denotes the concentration of sulfuric acid in the organic phase, V O Indicating the volume of the organic phase.
Detailed Description
The invention is further described in detail below with reference to the drawings and specific embodiments.
Example 1:
a method for improving flow benefit of uranium extraction by extracting tri-fatty amine comprises the step 1 of leaching crushed ore by sulfuric acid, setting acid consumption as Q and unit as kg/t ore, and leaching in situTaking out uranium with the unit of kg/kg, and the uranium concentration of the leaching solution is C 1 In units of g/L, the sulfuric acid concentration is C H1 The unit is g/L, 1t ore, or 1kg uranium in-situ leaching liquid, and the volume of the leaching liquid is V 1 The unit is L;
step 2, adsorbing the leaching solution by using strong basic resin to obtain saturated resin, wherein the volume of the adsorption tail solution is V 2 The unit is L, and then high-concentration sulfuric acid is adopted for leaching, and the concentration of the sulfuric acid is C HF3 In units of g/L, C HF3 Not less than 80 g/L; obtaining leached qualified liquid with the uranium concentration of C 3 In units of g/L, the sulfuric acid concentration is C H2 In g/L, the volume of the leaching solution is V 2 The unit is L;
step 3, setting the volume as V 2-2 The unit is L, the absorption tail liquid and the eluted qualified liquid are mixed, the extraction stock solution is adjusted, and the uranium concentration of the adjusted extraction stock solution is C 4 In units of g/L, the sulfuric acid concentration is C H4 The unit is g/L, the volume of the leaching solution is V 4 Diluting the uranium concentration in the leached qualified liquid by the adsorption tail liquid with the unit of L, wherein the dilution multiple is DR;
dilution factor DR ═ V 4 /V 3 ＝(V 2-2 +V 3 )/V 3 ＝V 2-2 /V 3 +1；
Step 4, carrying out multi-stage countercurrent extraction on the adjusted extraction stock solution by using tri-aliphatic amine to obtain a saturated organic phase with the uranium concentration of C O In units of g/L, the sulfuric acid concentration is C HO The unit is g/L, and the volume of the loaded organic phase is V O The unit is L, stripping is removed;
step 5, the uranium concentration of the raffinate obtained by the multi-stage countercurrent extraction is C 5 In units of g/L, the sulfuric acid concentration is C H5 In g/L, the volume of the leaching solution is V 5 In the unit of L, wherein V 5-1 Unit is L, return eluent preparation, V 5-2 The unit is L, and the leaching agent is returned for preparation;
step 6, the preparation of the back extractant meets the following conditions, and the sulfuric acid is supplemented in the preparation process to ensure that the concentration of the sulfuric acid reaches C HF1 ；V 5-2 Need to satisfy V 2-2 ≤V 5-2 The conditions of (a);
step 7, carrying out multi-stage counter-current back extraction on the loaded organic phase, wherein the back extraction agents are ammonium sulfate and ammonia, and controlling the pH of each stage to be 3.8-5 to obtain a back extraction liquid;
step 8, adding ammonia into the back extraction liquid to precipitate ADU, and performing solid-liquid separation to obtain a product ADU and a mother liquid, wherein the mother liquid contains ammonium sulfate and the volume of the mother liquid is V 7 In the unit of L, wherein V 7-1 In the unit L, as stripping agent back to trans, V 7-2 The unit is L, and the waste liquid is discharged and treated;
step 9, when C H5 ×V 5 When the frequency is more than or equal to 1000Q,
it should satisfy:
Figure BDA0002669499760000061
or
Figure BDA0002669499760000062
Wherein zeta is 1-1.2;
wherein C is H5 * When DR is 1, i.e. V 2-2 0 or V 2-B C when equal to 0 H5 ；
Step 10, when C H5 ×V 5 When the frequency is less than 1000Q,
it should satisfy:
Figure BDA0002669499760000063
in the step 1, the broken and ground ore is leached in situ by adopting sulfuric acid.
In the step 3, DR is 1.2-4.
In said step 3, DR >1 is controlled.
In said step 3, V 2-2 >0。
And in the step 3, water is distributed through a public pool, so that the water balance and DR >1 are realized.
In step 9, ζ was 1.08.
Example 2:
the uranium grade of a uranium ore is 0.117 percent, and the uranium ore is stirred and leached by adopting conventional sulfuric acid. The acid consumption was 30kg/t ore. The solid ratio of the leaching solution is 2L/kg. Uranium in the leachate is adsorbed by adopting a density of 201 multiplied by 7, and 50mg/ml of saturated resin is obtained. And leaching the saturated resin by using 100g/L sulfuric acid, wherein the volume of the leaching solution is 25BV, the uranium concentration of the leached qualified solution is 2.02g/L, and the sulfuric acid concentration is 99.2 g/L.
When DR is 1, N235 organic phase relative leaching qualified liquid is used for extraction, the saturated uranium concentration is 1.95g/L, 54.3% of extraction residue is returned to be leached (the volume accounts for 13.8% of the leaching agent, the extraction return sulfuric acid is 25kg/t ore), and 45.7% is returned to be eluted with the eluent for preparation (the volume accounts for 45.7% of the eluent, and the sulfuric acid accounts for 41.6% of the eluent). And (3) carrying out back extraction on the saturated organic phase by adopting ammonia water and ammonium sulfate to obtain a back extraction liquid with the uranium concentration of 5.85g/L, adding ammonia to precipitate ADU, returning a mother solution to the back extraction preparation, treating and discharging part of the mother solution, wherein the discharge amount of ammonium sulfate is 6.2t/t uranium.
When DR is 2, diluting the qualified leaching solution with adsorption tail liquid, extracting with N235 organic phase-opposite qualified leaching solution to obtain saturated uranium with a concentration of 3g/L, leaching the raffinate 51.6% and returning to leach (the volume is 26.5% of the leaching agent, and the extraction return sulfuric acid is 25kg/t ore), and preparing 48.4% and returning to leach (the volume is 96.8% of the leaching agent, and the sulfuric acid is 45.7% of the leaching agent). And (2) carrying out back extraction on the saturated organic phase by adopting ammonia water and ammonium sulfate to obtain a back extraction liquid with the uranium concentration of 6g/L, adding ammonia for precipitation to prepare ADU with the same quality, returning a mother solution for back extraction preparation, treating and discharging part of the mother solution, and discharging the ammonium sulfate with the discharge amount of 3.85t/t uranium. Saving 1.76t/t uranium sulfate and saving ammonia (by 100% NH) when DR is 2 to 1 3 Metering) 1.22t/t uranium, less discharging 2.37t/t uranium ammonium sulfate and 38 percent of emission reduction rate.
Example 3:
the uranium grade of a uranium ore is 0.117 percent, and the uranium ore is stirred and leached by adopting conventional sulfuric acid. The acid consumption was 30kg/t ore. The solid ratio of the leaching solution is 2L/kg. Uranium in the leachate is adsorbed by adopting a density of 201 multiplied by 7, and 50mg/ml of saturated resin is obtained. And leaching the saturated resin by using 100g/L sulfuric acid, wherein the volume of the leaching solution is 25BV, the uranium concentration of the leached qualified solution is 2.04g/L, and the sulfuric acid concentration is 99.2 g/L.
When DR is 1, N235 organic phase relative leaching qualified liquid is used for extraction, the saturated uranium concentration is 1.95g/L, 21.9% of raffinate is returned to leaching (the volume accounts for 5.5% of the leaching agent, and the extraction return sulfuric acid is 10kg/t ore), and 78.1% is returned to leaching agent preparation (the volume accounts for 78.1% of the leaching agent, and the sulfuric acid accounts for 70.9% of the leaching agent). And (3) carrying out back extraction on the saturated organic phase by adopting ammonia water and ammonium sulfate to obtain a back extraction liquid with the uranium concentration of 5.85g/L, adding ammonia to precipitate ADU, returning a mother liquid to the back extraction preparation, treating and discharging part of the mother liquid, wherein the discharge amount of ammonium sulfate is 6.2t/t uranium.
When ζ is 1.08, the DR maximum is calculated to be 2.53, and DR is taken to be 2.53. Diluting the qualified leaching solution with water in a public water tank, extracting the qualified leaching solution by adopting N235 organic phase to obtain saturated uranium with the concentration of 3.5g/L, returning and leaching 60.5% of raffinate (the volume accounts for 39.8% of the leaching agent, and the extraction return sulfuric acid accounts for 30kg/t ore), and preparing 39.5% of return eluent (the volume accounts for 99.9% of the eluent, and the sulfuric acid accounts for 37.7% of the eluent). And (2) carrying out back extraction on the saturated organic phase by adopting ammonia water and ammonium sulfate to obtain a back extraction liquid with the uranium concentration of 6.3g/L, adding ammonia for precipitation to prepare ADU with the same quality, returning a mother solution for back extraction preparation, treating and discharging part of the mother solution, and discharging 3.22t/t uranium ammonium sulfate. 2.23t/t uranium sulfate and ammonia (100% NH) can be saved when DR is 2.53 and DR is 1 3 Calculated) 1.54t/t uranium, less discharge of 3.00t/t uranium ammonium sulfate and 48 percent of emission reduction rate.
Example 4:
the uranium grade of a uranium ore is 0.117%, and heap leaching is carried out by adopting sulfuric acid. The acid consumption was 30kg/t ore. The solid ratio of the leaching solution is 2L/kg. Uranium in the leachate is adsorbed by adopting a density of 201 multiplied by 7, and 50mg/ml of saturated resin is obtained. And leaching the saturated resin by using 100g/L sulfuric acid, wherein the volume of the leaching solution is 5BV, the uranium concentration of the leached qualified solution is 5.05g/L, and the sulfuric acid concentration is 97.94 g/L.
When DR is 1, N235 organic phase relative leaching qualified liquid is used for extraction, the saturated uranium concentration is 1.95g/L, the extraction residue is 6.06% returned to be leached (the volume accounts for 0.6% of the leaching agent, the extraction returned sulfuric acid is 1kg/t ore), and 93.9% returned to be leached to be prepared (the volume accounts for 93.9% of the leaching agent, and the sulfuric acid accounts for 77.5% of the leaching agent). And (3) carrying out back extraction on the saturated organic phase by adopting ammonia water and ammonium sulfate to obtain a back extraction liquid with the uranium concentration of 7g/L, adding ammonia to precipitate ADU, returning a mother solution to the back extraction preparation, treating and discharging part of the mother solution, wherein the discharge amount of ammonium sulfate is 4.72t/t uranium.
When ζ is 1.08, DR maximum is calculated to be 11, and DR is taken to be 9. Diluting the qualified leaching solution with water in a public water tank, extracting the qualified leaching solution by adopting N235 organic phase to obtain saturated uranium with the concentration of 3.6g/L, returning and leaching 97.1% of raffinate (the volume accounts for 95.8% of the leaching agent, and the extraction return sulfuric acid is 19kg/t ore), and preparing 2.9% of return eluent (the volume accounts for 26.0% of the eluent, and the sulfuric acid accounts for 2.6% of the eluent). And (3) carrying out back extraction on the saturated organic phase by adopting ammonia water and ammonium sulfate to obtain a back extraction liquid with the uranium concentration of 6.48g/L, adding ammonia for precipitation to prepare ADU with the same quality, returning a mother solution for back extraction preparation, treating and discharging part of the mother solution, wherein the discharge amount of ammonium sulfate is 3.11t/t uranium. When DR is 9 to 1, the method saves 1.20t/t uranium sulfate and ammonia (by 100 percent NH) 3 Calculated) 0.83t/t uranium, less discharge of 1.61t/t uranium ammonium sulfate and 34 percent of emission reduction rate.
Example 5:
some sulphuric acid process leach in situ. The acid consumption is 80t/t uranium. The uranium concentration of the leachate is 0.02 g/L. The uranium in the leachate was adsorbed by using a method of 201X 7 to obtain a saturated resin of 10 mg/ml. And (3) leaching the saturated resin by using 103g/L sulfuric acid, wherein the volume of the leaching solution is 10BV, the uranium concentration of the leached qualified solution is 1.04g/L, and the sulfuric acid concentration is 102 g/L.
When DR is 1, N235 organic relative leaching qualified liquid is used for extraction, the saturated uranium concentration is 1.45g/L, the extraction residue is 10.3% of the extraction residue and is returned to be leached (the volume accounts for 0.2% of the leaching agent, and the sulfuric acid accounts for 12.5% of the leaching agent), and 89.7% of the extraction residue and is returned to be leached to be prepared (the volume accounts for 89.7% of the leaching agent, and the sulfuric acid accounts for 84.2% of the leaching agent). And (3) carrying out back extraction on the saturated organic phase by adopting ammonia water and ammonium sulfate to obtain a back extraction liquid with the uranium concentration of 4.35g/L, adding ammonia to precipitate ADU, returning a mother liquid to the back extraction preparation, treating and discharging part of the mother liquid, wherein the discharge amount of ammonium sulfate is 8.55t/t uranium.
When ζ is 1.08, the DR maximum is calculated to be 50.74, and DR is taken to be 2. Diluting the qualified leaching solution with the tail adsorption solution, extracting with N235 organic phase-to-qualified leaching solution to obtain saturated uranium with concentration of 2.05g/L, and returning extraction residue of 57.2% to leaching (volume accounts for2.4% of the leaching agent, 75% of sulfuric acid and 42.8% of the leaching agent are returned to the eluent for preparation (the volume of the eluent is 85.6%, and the sulfuric acid is 41.1% of the eluent). And (2) carrying out back extraction on the saturated organic phase by adopting ammonia water and ammonium sulfate to obtain a back extraction liquid with the uranium concentration of 6.15g/L, adding ammonia for precipitation to prepare ADU with the same quality, returning mother liquor for back extraction preparation, treating and discharging part of the mother liquor, and discharging 5.88t/t uranium ammonium sulfate. When DR is 2 to 1, the method saves 1.97t/t uranium sulfate and ammonia (100% NH) 3 Calculated) 1.38t/t uranium, less discharge of 2.66t/t uranium ammonium sulfate and 31 percent of emission reduction rate.
Example 6:
some sulphuric acid process leach in situ. The acid consumption is 80t/t uranium. The uranium concentration of the leachate is 0.02 g/L. The uranium in the leachate was adsorbed by using a method of 201X 7 to obtain a saturated resin of 10 mg/ml. And leaching the saturated resin by using 123g/L sulfuric acid, wherein the volume of the leaching solution is 10BV, the uranium concentration of the leached qualified solution is 1.05g/L, and the sulfuric acid concentration is 122.6 g/L.
When DR is equal to 1, N235 organic phase-relative leaching qualified liquid is used for extraction, the saturated uranium concentration is 0.95g/L, 8.8% of raffinate is returned to leaching (volume accounts for 0.18% of leaching agent, sulfuric acid accounts for 12.5% of leaching agent), and 91.2% is returned to leaching agent preparation (volume accounts for 91.2% of leaching agent, and sulfuric acid accounts for 83.9% of leaching agent). And (3) carrying out back extraction on the saturated organic phase by adopting ammonia water and ammonium sulfate to obtain a back extraction liquid with the uranium concentration of 5.7g/L, adding ammonia to precipitate ADU, returning a mother liquid to the back extraction preparation, treating and discharging part of the mother liquid, wherein the discharge amount of ammonium sulfate is 13.3t/t uranium.
When ζ is 1.08, the DR maximum is calculated to be 50.78, and DR is taken to be 2.5. Diluting the qualified leaching solution by using adsorption tail solution, extracting by using N235 organic phase relative qualified leaching solution to obtain saturated uranium with the concentration of 2.83g/L, returning and leaching the extraction residue of 61.5% (the volume of the extraction residue is 3.3% of the leaching agent, and the sulfuric acid is 100% of the leaching agent), and preparing the 38.5% returned leaching agent (the volume of the extraction residue is 96.3% of the leaching agent, and the sulfuric acid is 37.6% of the leaching agent). And (3) carrying out back extraction on the saturated organic phase by adopting ammonia water and ammonium sulfate to obtain a back extraction liquid with the uranium concentration of 5.66g/L, adding ammonia for precipitation to prepare ADU with the same quality, returning a mother solution for back extraction preparation, treating and discharging part of the mother solution, and discharging the ammonium sulfate with the discharge amount of 4.10t/t uranium. DR 2.5 to DR1 time, 6.85t/t uranium sulfate is saved, and ammonia (100 percent NH) is saved 3 Calculated) 4.76t/t uranium, less discharge of 9.23t/t uranium ammonium sulfate and 69 percent emission reduction.

Claims (7)

1. A method for improving flow benefit of uranium extraction by triple fatty amine leaching is characterized by comprising the following steps:
step 1, leaching broken and ground ore by adopting sulfuric acid, setting acid consumption as Q and unit as kg/t ore, leaching in situ to obtain uranium with unit as kg/kg, and leaching liquor with uranium concentration as C 1 In units of g/L, the sulfuric acid concentration is C H1 The unit is g/L, 1t ore, or the volume of the leachate is V when 1kg of uranium in the leachate is leached in situ 1 The unit is L;
step 2, adsorbing the leaching solution by using strong basic resin to obtain saturated resin, wherein the volume of the adsorption tail solution is V 2 The unit is L, and then high-concentration sulfuric acid is adopted for leaching, and the concentration of the sulfuric acid is C HF3 In units of g/L, C HF3 Not less than 80 g/L; obtaining leached qualified liquid with the uranium concentration of C 3 In units of g/L, the sulfuric acid concentration is C H2 In g/L, the volume of the leaching solution is V 2 The unit is L;
step 3, setting the volume as V 2-2 The unit is L, the absorption tail liquid and the eluted qualified liquid are mixed, the extraction stock solution is adjusted, and the uranium concentration of the adjusted extraction stock solution is C 4 In units of g/L, the sulfuric acid concentration is C H4 In g/L, the volume of the leaching solution is V 4 Diluting the uranium concentration in the leached qualified liquid by the adsorption tail liquid with the unit of L, wherein the dilution multiple is DR;
dilution factor DR ═ V 4 /V 3 ＝(V 2-2 +V 3 )/V 3 ＝V 2-2 /V 3 +1；
And 4, performing multistage countercurrent extraction on the adjusted extraction stock solution by adopting N235 to obtain a saturated organic phase with the uranium concentration of C O In units of g/L, the sulfuric acid concentration is C HO The unit is g/L, and the volume of the loaded organic phase is V O The unit is L, stripping is removed;
step 5, the uranium concentration of the raffinate obtained by the multi-stage countercurrent extraction is C 5 In units of g/L, the sulfuric acid concentration is C H5 In g/L, the volume of the leaching solution is V 5 In the unit of L, wherein V 5-1 Unit is L, return eluent preparation, V 5-2 The unit is L, and the leaching agent is returned for preparation;
step 6, the preparation of the back extractant meets the following conditions, and the sulfuric acid is supplemented in the preparation process to ensure that the concentration of the sulfuric acid reaches C HF1 ；V 5-2 Need to satisfy V 2-2 ≤V 5-2 The conditions of (a);
step 7, carrying out multi-stage counter-current back extraction on the loaded organic phase, wherein the back extraction agents are ammonium sulfate and ammonia, and controlling the pH of each stage to be 3.8-5 to obtain a back extraction liquid;
step 8, adding ammonia into the back extraction liquid to precipitate ADU, and performing solid-liquid separation to obtain a product ADU and a mother liquid, wherein the mother liquid contains ammonium sulfate and the volume of the mother liquid is V 7 In the unit of L, wherein V 7-1 In the unit L, as stripping agent back to trans, V 7-2 The unit is L, and the waste liquid is discharged and treated;
step 9, when C H5 ×V 5 When the frequency is more than or equal to 1000Q,
it should satisfy:
Figure FDA0003729498410000021
or
Figure FDA0003729498410000022
Wherein zeta is 1-1.2;
wherein C is H5 * When DR is 1, i.e. V 2-2 0 or V 2-B C when equal to 0 H5 ；
Step 10, when C H5 ×V 5 When the frequency is less than 1000Q,
it should satisfy:
Figure FDA0003729498410000023
2. the method for improving the efficiency of the uranium leaching process of the tri-aliphatic amine according to claim 1, wherein the method comprises the following steps: in the step 1, the broken and ground ore is leached in situ by adopting sulfuric acid.
3. The method for improving the efficiency of the uranium leaching process of the tri-aliphatic amine according to claim 1, wherein the method comprises the following steps: in the step 3, DR is 1.2-4.
4. The method for improving the efficiency of the uranium leaching process of the tri-aliphatic amine according to claim 1, wherein the method comprises the following steps: in said step 3, DR >1 is controlled.
5. The method for improving the efficiency of the uranium leaching process of the tri-aliphatic amine according to claim 1, wherein the method comprises the following steps: in said step 3, V 2-2 >0。
6. The method for improving the efficiency of the uranium leaching process of the tri-aliphatic amine according to claim 1, wherein the method comprises the following steps: and in the step 3, water is distributed through a public pool, so that the water balance and DR >1 are realized.
7. The method for improving the efficiency of the uranium leaching process of the tri-aliphatic amine according to claim 1, wherein: in step 9, ζ was 1.08.
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