CN111020190B - Process linking method for extracting uranium by two-step ion exchange method - Google Patents
Process linking method for extracting uranium by two-step ion exchange method Download PDFInfo
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- CN111020190B CN111020190B CN201911258665.1A CN201911258665A CN111020190B CN 111020190 B CN111020190 B CN 111020190B CN 201911258665 A CN201911258665 A CN 201911258665A CN 111020190 B CN111020190 B CN 111020190B
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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
- 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
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
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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
- 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
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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
- C22B60/0221—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
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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
- C22B60/0265—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
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Abstract
The invention belongs to the technical field of uranium hydrometallurgy, and particularly relates to a process linking method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange. The method comprises the following steps: (1) carrying out first-step ion exchange in an acidic sulfuric acid leaching solution by using weak base resin to extract uranium to obtain saturated resin loaded with uranium; (2) washing the saturated resin loaded with uranium obtained in the step (1) with water to obtain washed resin; (3) leaching the washed resin; (4) periodically detecting the leacheate obtained in the step (3); (5) leaching the leached resin with mixed solution of sodium bicarbonate and sodium carbonate to obtain qualified leaching solution in one step; (6) adjusting the pH value of the qualified liquid obtained by the one-step leaching by using NaOH solution; (7) and (3) carrying out two-step adsorption by using strong basic resin. The method realizes the washing process of the carbonate on the resin, obtains the qualified washing liquid with higher concentration, and avoids the problem of gas generation in the washing process of the carbonate.
Description
Technical Field
The invention belongs to the technical field of uranium hydrometallurgy, and particularly relates to a process linking method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange.
Background
In the existing industrial hydrometallurgy process of natural uranium, most ore leachate (obtained by stirring leaching, heap leaching or in-situ leaching) is subjected to ion exchange adsorption, or solvent extraction, or ion exchange and solvent extraction processes, and leaching solution or back extraction solution is obtained to perform uranium precipitation to obtain a natural uranium product. At present, a uranium extraction process adopting two-step ion exchange is not available.
At present, the uranium extraction leaching liquid is generally a sulfuric acid system. The ion exchange extraction of uranium by a sulfuric acid system generally adopts strong basic resin. The resin adsorbs sulfate and uranyl sulfate anion complexes. And leaching the saturated resin by using acid-containing sodium chloride, and replacing sulfate radical uranyl sulfate anion complexes by using chloride ions to obtain uranium leacheate containing a large amount of sulfate radicals. Adding alkali to obtain a uranium product.
The realization of resin two-step ion exchange uranium extraction has a plurality of difficulties. One important difficulty is that two-step ion exchange is difficult to join. One is that the eluent obtained by one-step ion exchange still has the characteristics of strong eluent, and is difficult to adsorb during two-step ion exchange. The reasons for this are manifold. One is that chlorine in the one-step eluent has a large proportion of chlorine remaining in the eluent, which adversely affects adsorption; but a large amount of sulfate radicals also have stronger leaching effect and can generate adverse effect on ion exchange; carbonate leaching generally has low leaching efficiency and low leaching solution concentration, and gas can be generated during leaching, so that saturated resin and leaching solution gradient are damaged.
In the conventional technical scheme, due to the defects, a process connection method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange is urgently needed to be developed, so that the problems are solved.
Disclosure of Invention
The invention aims to solve the technical problem of providing a process connection method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange, solving the process connection problem of the two-step ion exchange uranium extraction process, and enabling two-step ion exchange resin to adsorb uranium in leacheate of one-step ion exchange.
In order to realize the purpose, the invention adopts the technical scheme that:
a process linking method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange comprises the following steps:
(1) carrying out first-step ion exchange in an acidic sulfuric acid leaching solution by using weak base resin to extract uranium to obtain saturated resin loaded with uranium;
(2) washing the saturated resin loaded with uranium obtained in the step (1) with water to obtain washed resin;
(3) leaching the washed resin
(3.1) draining the washing water, and adding a NaOH solution;
(3.2) standing for a set time, and continuously pumping NaOH solution to rinse the washed resin obtained in the step (2);
(4) periodically detecting the leacheate obtained in the step (3), finishing leaching when the amount of sulfate radicals reaches 0.1-2 g/L, and transferring to the step (5);
(5) leaching the leached resin with mixed solution of sodium bicarbonate and sodium carbonate to obtain qualified leaching solution in one step;
(6) adjusting the pH value of the qualified liquid obtained by the one-step leaching to 9.5-10.5 by using NaOH solution;
(7) and (4) carrying out two-step adsorption on the one-step leaching qualified liquid obtained in the step (6) after the pH value is adjusted by adopting strong basic resin.
Further, the process connection method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange is described as follows, in step (1): the type of the weak base resin is one of D301, D302, D303 and D331.
Further, the process connection method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange is described as follows, in step (1): the adsorption capacity of the weak alkaline resin to uranium is 5 mg/ml-80 mg/ml.
Further, the process connection method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange is described as follows, in step (1): the volume of the acid sulfuric acid leaching solution is 10 BV-8000 BV, and the retention time is 5 min-30 min.
Further, the process connection method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange is described as follows, and in the step (2): the volume of water is 1-3 BV, and the washing time is 5-30 min.
Further, a process linking method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange is described above, wherein in the step (3.1): the concentration of the NaOH solution is more than or equal to 80g/L, and the adding speed is more than or equal to 0.1 BV/min.
Further, a process linking method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange is described above, wherein in the step (3.2): standing for 15 min-2 h, and continuously pumping NaOH solution with the concentration of 40 g/L-160 g/L; contact time t for rinsing washed resinContact withIs 30 min-2 h.
Further, the process connection method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange is described as follows, and in the step (5): the concentration of the sodium bicarbonate is 40-80 g/L, and the concentration of the sodium carbonate is 20-50 g/L; the leaching volume is 2-10 BV, and the first 1-5 BV is taken as qualified liquid for one-step leaching.
Further, the process connection method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange is described as follows, and in the step (7): the model of the strong basic resin is D201 x 7, and the adsorption capacity to uranium is 30 mg/ml-100 mg/ml; the adsorption retention time in the two-step adsorption is 0.5-2 h, and the adsorption volume is 8-80 BV.
The technical scheme of the invention has the beneficial effects that:
(1) the elution of the ion exchange weak-base resin in one step is realized, and the eluted resin can be circularly adsorbed.
(2) The method realizes the washing process of the carbonate on the resin, obtains the qualified washing liquid with higher concentration, and avoids the problem of gas generation in the washing process of the carbonate.
(3) By the process, sulfate radicals in the system are removed, and the problem that the sulfate radicals enter uranium products and become impurities is solved.
(4) Because no adverse effect of sulfate radicals on the two-step adsorption is caused, the adsorption capacity of the sulfate radicals on the two-step ion exchange can be greatly improved.
(5) And impurities such as molybdenum, vanadium and the like dissolved in strong basicity are favorably removed through the strong basicity leaching process.
(6) The obtained eluent can be used for two-step ion exchange adsorption, and the connection of two-step ion exchange is realized.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The technical scheme of the invention is explained in detail in the following by combining the drawings and the specific embodiment.
As shown in figure 1, the invention relates to a process connection method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange, which comprises the following steps:
(1) carrying out first-step ion exchange in an acidic sulfuric acid leaching solution by using weak base resin to extract uranium to obtain saturated resin loaded with uranium;
the type of the weak base resin is one of D301, D302, D303 and D331; the adsorption capacity of the alkalescent resin to uranium is 5 mg/ml-80 mg/ml; the volume of the acid sulfuric acid leaching solution is 10 BV-8000 BV, and the retention time is 5 min-30 min.
(2) Washing the saturated resin loaded with uranium obtained in the step (1) with water to obtain washed resin;
the volume of water is 1-3 BV, and the washing time is 5-30 min.
(3) Leaching the washed resin
(3.1) draining the washing water, and adding a NaOH solution; the concentration of the NaOH solution is more than or equal to 80g/L, and the adding speed is more than or equal to 0.1 BV/min.
(3.2) standing for a set time, and continuously pumping NaOH solution to rinse the washed resin obtained in the step (2);
specifically, after standing for 15min to 2h, continuously pumping NaOH solution with the concentration of 40g/L to 160 g/L; contact time t for rinsing washed resinContact withIs 30 min-2 h.
(4) Periodically detecting the leacheate obtained in the step (3), finishing leaching when the amount of sulfate radicals reaches 0.1-2 g/L, and transferring to the step (5);
(5) leaching the leached resin with mixed solution of sodium bicarbonate and sodium carbonate to obtain qualified leaching solution in one step;
the concentration of the sodium bicarbonate is 40-80 g/L, and the concentration of the sodium carbonate is 20-50 g/L; the leaching volume is 2-10 BV, and the first 1-5 BV is taken as qualified liquid for one-step leaching.
(6) Adjusting the pH value of the qualified liquid obtained by the one-step leaching to 9.5-10.5 by using NaOH solution;
(7) performing two-step adsorption on the one-step leaching qualified liquid obtained in the step (6) after the pH value is adjusted by using strong basic resin;
the model of the strong basic resin is D201 x 7, and the adsorption capacity to uranium is 30 mg/ml-100 mg/ml; the adsorption retention time in the two-step adsorption is 0.5-2 h, and the adsorption volume is 8-80 BV.
Claims (1)
1. A process linking method for extracting uranium from a sulfuric acid system by adopting two-step ion exchange is characterized by comprising the following steps:
(1) carrying out first-step ion exchange in an acidic sulfuric acid leaching solution by using weak base resin to extract uranium to obtain saturated resin loaded with uranium;
(2) washing the saturated resin loaded with uranium obtained in the step (1) with water to obtain washed resin;
(3) leaching the washed resin
(3.1) draining the washing water, and adding a NaOH solution;
(3.2) standing for a set time, and continuously pumping NaOH solution to rinse the washed resin obtained in the step (2);
(4) periodically detecting the leacheate obtained in the step (3), finishing leaching when the amount of sulfate radicals reaches 0.1-2 g/L, and transferring to the step (5);
(5) leaching the leached resin with mixed solution of sodium bicarbonate and sodium carbonate to obtain qualified leaching solution in one step;
(6) adjusting the pH value of the qualified liquid obtained by the one-step leaching to 9.5-10.5 by using NaOH solution;
(7) performing two-step adsorption on the one-step leaching qualified liquid obtained in the step (6) after the pH value is adjusted by using strong basic resin;
in the step (1): the type of the weak base resin is one of D301, D302, D303 and D331; the adsorption capacity of the alkalescent resin to uranium is 5 mg/mL-80 mg/mL; the volume of the acid sulfuric acid leaching solution is 10 BV-8000 BV, and the retention time is 5 min-30 min;
in the step (2): the volume of water is 1-3 BV, and the washing time is 5-30 min;
in the step (3.1): the concentration of the NaOH solution is more than or equal to 80g/L, and the adding speed is more than or equal to 0.1 BV/min;
in the step (3.2): standing for 15 min-2 h, and continuously pumping NaOH solution with the concentration of 40 g/L-160 g/L; contact time t for rinsing washed resinContact withIs 30min to 2 h;
in the step (5): the concentration of the sodium bicarbonate is 40-80 g/L, and the concentration of the sodium carbonate is 20-50 g/L; leaching the qualified liquid at a leaching volume of 2-10 BV, and taking the first 1-5 BV as the qualified liquid for one-step leaching;
in the step (7): the model of the strong basic resin is D201 x 7, and the adsorption capacity of the strong basic resin to uranium is 30 mg/mL-100 mg/mL; the adsorption retention time in the two-step adsorption is 0.5-2 h, and the adsorption volume is 8-80 BV.
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| CN112680608B (en) * | 2020-12-16 | 2022-08-19 | 核工业北京化工冶金研究院 | Method for extracting uranium from chlorinated carbonate system |
| CN115572848B (en) * | 2022-09-26 | 2023-12-15 | 核工业北京化工冶金研究院 | Technological method capable of realizing efficient leaching of uranium-bearing resin and regeneration of leaching agent |
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| RO122641B1 (en) * | 2005-09-29 | 2009-10-30 | Institutul Naţional De Cercetare-Dezvoltare Pentru Metale Şi Resurse Radioactive - Icpmrr | Process for recovering uranium from acid uranium-bearing leach solutions by ion exchange |
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