CN112680607A - High-clarity crystallization back extraction method in uranium extraction process - Google Patents
High-clarity crystallization back extraction method in uranium extraction process Download PDFInfo
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Abstract
The invention relates to the field of uranium hydrometallurgy, in particular to a high-clarity crystallization back extraction method in a uranium extraction process. The high-clarity crystallization reextraction method in the uranium extraction process comprises the following steps: mixing and reacting the organic phase loaded with uranium, a back-extraction agent and uranyl tricarbonate slurry, and keeping the reaction temperature at 30-50 ℃ to obtain a mixed phase; the stripping agent is ammonium carbonate and/or ammonium bicarbonate; and inputting the mixed phase into a double-interface complementary-collection three-phase separation device, stirring the rake of the double-interface complementary-collection three-phase separation device, continuously discharging underflow slurry, and preparing the uranium tricarbonate by using the discharged crystallization mother liquor and the back-extraction agent. The invention solves the problems of difficult phase separation and poor crystal form, realizes the stable and benign operation of the crystallization back extraction, ensures that the phase separation effect is good, the two phases are clear and transparent, and the obtained AUC crystal has large particles and good crystal form, thereby achieving good back extraction and crystallization effects.
Description
Technical Field
The invention relates to the field of uranium hydrometallurgy, in particular to a high-clarity crystallization back extraction method in a uranium extraction process.
Background
In the existing industrial natural uranium hydrometallurgy process, most ore leachate is subjected to ion exchange adsorption or solvent extraction to obtain leacheate or back extraction liquid, and uranium precipitation is carried out to obtain a natural uranium product. At present, the uranium extraction leaching liquid is generally a sulfuric acid system.
The solvent extraction is generally tertiary amine extraction or P204 extraction. The P204 extractant is a phosphorus medium-strong acid cation extractant. In order to improve the uranium/hydrogen ratio in the organic phase and reduce acid and alkali consumption, TRPO can be added in the organic phase, namely P204-TRPO mixed extractant is adopted for synergistic extraction. But the phase separation performance of the P204-TRPO extractant is poor.
The P204 or P204-TRPO-loaded uranium organic phase can be back extracted by sodium carbonate to obtain a back extraction liquid of a sodium carbonate system, carbonate reacts with uranium to form complex anions, so that the complex anions are not extracted and do not precipitate under an alkaline condition, and the back extraction liquid is precipitated by adjusting acid and adding alkali or directly adding alkali to produce a sodium diuranate product. Another method for preparing uranium products from P204 or P204-TRPO-loaded uranium organic phase is to add ammonium carbonate for stripping, and because of the low solubility of uranium in the ammonium carbonate system, ammonium carbonate is added to form uranyl tricarbonate (AUC) crystals, which simultaneously include stripping and crystallization, called a crystallization stripping process.
The crystallization and back extraction process, which involves an organic phase, a water phase and a solid phase, is shorter than the process of crystallization and precipitation after back extraction, but the reaction and operation are more complicated, and the technical requirements are higher. And in the process of crystallization and back extraction, emulsification or three-phase entrainment is easy to occur. Wherein the poor organic phase has low clarity, which causes subsequent problems of extraction emulsification, excessive extraction residue, difficult treatment of transformation liquid and the like; the unclear water phase can cause the problems of difficult treatment of subsequent crystallization mother liquor, standard exceeding of products and the like.
How to improve the clarity of two phases of the crystal stripping of the P204 loaded uranium organic phase is an important technical problem in the crystal stripping process of uranium extraction.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the high-clarity crystallization back-extraction method for the uranium extraction process is provided, the problems of difficult phase separation and poor crystal form are solved, stable and benign operation of crystallization back-extraction is realized, the phase separation effect is good, two phases are clear and transparent, the obtained AUC crystal is large in particle and good in crystal form, and good back-extraction and crystallization effects are achieved.
The invention provides a high-clarity crystallization stripping method in a uranium extraction process, which comprises the following steps:
step 1: mixing and reacting the organic phase loaded with uranium, a back-extraction agent and uranyl tricarbonate slurry, and keeping the reaction temperature at 30-50 ℃ to obtain a mixed phase;
the back extractant is ammonium carbonate and/or ammonium bicarbonate, and the concentration of the back extractant is 50-150 g/L;
the flow ratio n1 of the stripping agent to the organic phase loaded with uranium is 1-4;
step 2: inputting the mixed phase into a double-interface complementary-recovery three-phase separation device, stirring by a rake of the double-interface complementary-recovery three-phase separation device, continuously discharging underflow slurry, using the discharged crystallization mother liquor for preparing uranyl tricarbonate and preparing the back-extraction agent,
the double-interface complementary-collection three-phase separation equipment comprises: s, a cylinder body, the lower part of which is conical;
the central barrel is arranged at the upper part in the S barrel and is coaxial with the S barrel;
a first mixed phase inlet disposed at the top of the core barrel;
the water phase outlets are arranged at the lower part of the side wall of the S cylinder body, are provided with a plurality of water phase outlets according to different heights and are used for discharging water phases;
the crystal outlet is arranged at the bottom of the S cylinder;
the rake paddle is arranged in the S cylinder body and penetrates through the central cylinder;
the overflow weir plate is arranged at the upper part of the S-shaped cylinder body, is lower than the upper edge of the central cylinder and is used for discharging an organic phase;
the lower edge of the central barrel and the upper edge of the overflow weir plate are provided with a plurality of triangular openings;
and the organic phase outlet is arranged at the upper part of the outer wall of the S cylinder and is used for discharging the organic phase flowing out of the overflow weir plate.
Preferably, in the step 1, the organic phase loaded with uranium, the stripping agent and the slurry of uranyl tricarbonate are added into a first reactor for mixing reaction,
the first reactor comprises: a barrel; the stirring paddle is arranged in the cylinder body and used for continuously stirring;
the replenishing port is arranged at the top of the cylinder body and is used for adding various raw materials;
the conical bottom outlet is arranged at the bottom of the cylinder and used for discharging crystals;
the second mixed phase inlet is arranged at the upper part of the side wall of the cylinder;
the mixed phase outlet is arranged at the upper part of the side wall of the cylinder body;
the height from the mixed phase inlet to the cylinder bottom is greater than the height from the mixed phase outlet to the cylinder bottom.
Preferably, the mixed phase is discharged from the first reactor and then sequentially enters 2-10 reactors for continuous treatment, and the reactors have the same structure as the first reactor.
Preferably, the crystal retention in the first reactor and the reactor is 1/10V-1/3V;
and a part of the crystals discharged from the reactor is used as a product, and a part of the crystals is returned to the first reactor and continuously and stably added.
Preferably, in the step 2, the discharge rate of the crystallization mother liquor is m1, and n1 Xm 1 is not more than 1/5.
Preferably, the first reactor and the control aqueous phase within the reactor are a continuous phase.
Preferably, the double-interface complementary-collection three-phase separation equipment intermittently discharges crystals or continuously discharges the crystals, the intermittent time is 0.5-24 hours when the crystals are intermittently discharged, and the rake paddle is started before the crystals are discharged; coarse crystals are gathered and fine crystals are suspended, and the rake paddle is closed after the discharge;
when the crystal is discharged continuously, the rake paddle rotates continuously.
Preferably, the outer wall of the double-interface complementary-recovery three-phase separation equipment is provided with a heat-insulating layer, and the temperature inside the double-interface complementary-recovery three-phase separation equipment is 30-50 ℃.
Preferably, in the step 2, when the discharged crystallization mother liquor is used for preparing uranyl tricarbonate, the method specifically comprises the following steps: the crystallization mother liquor is heated to ammonium carbonate for decomposition, uranium precipitates, and gas generated by decomposition is absorbed by water to obtain ammonium carbonate solution, and the ammonium carbonate solution is used for preparing the back-extraction agent.
Preferably, in the step 1, the residence time of the organic phase is 0.5 to 4 hours.
Compared with the prior art, the high-clarity crystallization reextraction method in the uranium extraction process is matched with specific double-interface complementary-collection three-phase separation equipment, and has the following beneficial effects that:
(1) the P204 system is used for carrying out back extraction of an organic phase, and the depleted uranium concentration achieves an ideal effect;
(2) the obtained crystal has good shape, large crystal grains and low fine crystal content;
(3) the sharing effect is good, and the two phases are clear and transparent;
(4) realizes the recycling of the feed liquid, and is economical and environment-friendly.
Drawings
FIG. 1 shows a side view of a double-interface complementary three-phase separation apparatus;
FIG. 2 shows a cross-sectional view of a double-interface complementary three-phase separation apparatus;
FIG. 3 shows a schematic structural view of a first reactor;
FIG. 4 shows a phase-splitting schematic of a double-interface complementary three-phase separation apparatus;
FIG. 5 shows a flowchart of example 1 of the present invention.
Detailed Description
For a further understanding of the invention, embodiments of the invention are described below in conjunction with the examples, but it should be understood that these descriptions are included merely to further illustrate features and advantages of the invention, and are not intended to limit the invention.
The embodiment of the invention discloses a high-clarity crystallization stripping method in a uranium extraction process, which comprises the following steps:
step 1: mixing and reacting the organic phase loaded with uranium, a back-extraction agent and uranyl tricarbonate slurry, and keeping the reaction temperature at 30-50 ℃ to obtain a mixed phase;
the back extractant is ammonium carbonate and/or ammonium bicarbonate, and the concentration of the back extractant is 50-150 g/L;
the flow ratio n1 of the stripping agent to the organic phase loaded with uranium is 1-4;
step 2: inputting the mixed phase into a double-interface complementary-recovery three-phase separation device, stirring by a rake of the double-interface complementary-recovery three-phase separation device, continuously discharging underflow slurry, using the discharged crystallization mother liquor for preparing uranyl tricarbonate and preparing the back-extraction agent,
the double-interface complementary three-phase separation device, as shown in fig. 1 and 2, includes: s, a cylinder body 1, the lower part of which is conical;
the central barrel 2 is arranged at the upper part in the S barrel 1 and is coaxial with the S barrel;
a first mixed phase inlet 3 disposed at the top of the core barrel 2;
the water phase outlets 4 are arranged at the lower part of the side wall of the S cylinder 1, are provided with a plurality of water phase outlets according to different heights and are used for discharging water phases;
the crystal outlet 5 is arranged at the bottom of the S cylinder 1;
the rake paddle 6 is arranged in the S cylinder body 1 and penetrates through the central cylinder;
the overflow weir plate 7 is arranged at the upper part of the S-shaped cylinder body 1, is lower than the upper edge of the central cylinder and is used for discharging an organic phase;
the lower edge of the central barrel 2 and the upper edge of the overflow weir plate 6 are provided with a plurality of triangular openings;
and the organic phase outlet 8 is arranged at the upper part of the outer wall of the S cylinder 1 and is used for discharging the organic phase flowing out of the overflow weir plate.
The high-clarity crystal stripping method in the uranium extraction process of the invention is described in detail according to the specific steps.
Step 1: mixing and reacting the organic phase loaded with uranium, a back-extraction agent and uranyl tricarbonate slurry, keeping the reaction temperature at 30-50 ℃, and keeping the retention time of the organic phase at 0.5-4 hours to obtain a mixed phase;
the organic phase loaded with uranium contains H+And UO2 2+Ions, concentrations respectively CH0mol/L，CU0mol/L represents.
This step, preferably carried out in a first reactor, is: adding the organic phase loaded with uranium, a stripping agent and uranyl tricarbonate slurry into a first reactor for mixing reaction;
the first reactor, as shown in fig. 3, comprises: a cylinder 9;
the stirring paddle 14 is arranged in the cylinder body and used for continuously stirring;
the replenishing port 11 is arranged at the top of the cylinder body and is used for adding various raw materials;
a conical bottom outlet 13 arranged at the bottom of the cylinder body and used for discharging crystals;
a second mixed phase inlet 10 arranged at the upper part of the side wall of the cylinder body;
a mixed phase outlet 12 arranged at the upper part of the side wall of the cylinder body;
the height of the second mixed phase inlet 12 from the cylinder bottom is greater than that of the mixed phase outlet 10 from the cylinder bottom.
The back extractant is ammonium carbonate and/or ammonium bicarbonate, and the concentration of the back extractant is 50-150 g/L;
the flow ratio n1 of the stripping agent to the organic phase loaded with uranium is 1-4;
and discharging the mixed phase from the first reactor, and then sequentially entering 2-10 reactors for continuous treatment, wherein the reactors have the same structure as the first reactor.
The first reactor and the control water phase in the reactor are continuous phases.
The crystal retention in the first reactor and the reactor is 1/10V-1/3V;
and a part of the crystals discharged from the reactor is used as a product, and a part of the crystals is returned to the first reactor and continuously and stably added.
Step 2: inputting the mixed phase into a double-interface complementary-recovery three-phase separation device, stirring by a rake of the double-interface complementary-recovery three-phase separation device, continuously discharging underflow slurry, and using the discharged crystallization mother liquor for preparing uranyl tricarbonate and preparing the back-extraction agent;
the height of the interface is controlled by the double-interface complementary collection three-phase separation equipment, and the height comprises a first interface 15 and a second interface 16; the first interface is the interface of the organic phase and the water phase in the central barrel, and the second interface is the interface of the organic phase and the water phase in the S barrel.
The interface outside the central barrel is controlled by controlling the height of the water phase outlet, so that the interface outside the central barrel is higher than the lower edge of the central barrel, namely: the second interface is higher than the first interface, as shown in fig. 4;
intermittently discharging crystals or continuously discharging crystals by the double-interface complementary-collection three-phase separation equipment, wherein when the crystals are intermittently discharged, the intermittent time is 0.5-24 hours, and a rake paddle is started before the crystals are discharged; coarse crystals are gathered and fine crystals are suspended, and the rake paddle is closed after the discharge;
when the crystal is discharged continuously, the rake paddle rotates continuously.
Preferably, the outer wall of the double-interface complementary-recovery three-phase separation equipment is provided with a heat-insulating layer, and the temperature inside the double-interface complementary-recovery three-phase separation equipment is 30-50 ℃.
The discharge rate of the crystallization mother liquor is m1, and n1 Xm 1 is not more than 1/5.
When the discharged crystallization mother liquor is used for preparing uranyl tricarbonate, the method specifically comprises the following steps: the crystallization mother liquor is heated to ammonium carbonate for decomposition, uranium precipitates, and gas generated by decomposition is absorbed by water to obtain ammonium carbonate solution, and the ammonium carbonate solution is used for preparing the back-extraction agent.
For further understanding of the present invention, the method for high-clarity crystal stripping in uranium extraction provided by the present invention is described in detail below with reference to the following examples, and the scope of the present invention is not limited by the following examples.
Example 1
The flow of this embodiment is shown in fig. 5. By using M1～M3Reactor and double-interface complementary-recovery three-phase separation equipment S1. The effective volume of 3 reactors is 1m3. The extractant is P204-TRPO-kerosene, the concentration of P204 is 0.15mol/L, and the concentration of uranium in the uranium-loaded organic phase is 9 g/L. The concentration of the stripping agent is 100g/L ammonium carbonate and 15g/L ammonium bicarbonate. The stripping agent is added to the first reactor at the same time as the loaded organic, i.e., M1In the equipment. AUC crystals were added continuously at the same time, AUC was added as a slurry with 50% solids. The flow ratio of the stripping agent, the loaded organic phase and the slurry is QA1/QO1/QS 1-2/1/1, n 1-2, and the flow rates are 0.5m respectively3/h、0.25m3/h、0.25m3H is used as the reference value. The retention time of the organic phase is 1h, the reaction temperature is 40 ℃, and the crystal content in the equipment is (V/V) 12.5%. The mixed phase enters a reactor M in sequence2A reactor M3Double-interface complementary-collection three-phase separation equipment S1. The double-interface complementary-collection three-phase separation equipment controls the liquid interface outside the central barrel to be higher than the lower edge of the central barrel, the rake paddle is used for stirring at a low speed, the underflow slurry is continuously pumped out, one part returns, the other part is reserved as a product, and the product amount is 2.25 kgU/h. The crystallization mother liquor return rate was 1-m1 ═ 0.95, and n1 × m1 was 0.1. And (4) evaporating ammonia to precipitate uranium from the discharged crystallization mother liquor. Adding water to absorb ammonium bicarbonate to obtain a concentrated ammonium bicarbonate solution, and using the concentrated ammonium bicarbonate solution for preparing a stripping agent and carrying out AUC transformation crystallization. Each M device discharged large precipitated crystals at irregular intervals. All crystals were washed and filtered to give the AUC product. The poor organic phase is clarified and not carried, the uranium concentration is 8mg/L, the crystallization mother liquor is clarified and not carried, and the AUC product is a large-particle crystal.
Example 2
By using M1～M4Reactor and double-interface complementary-recovery three-phase separation equipment S1. The effective volume of 4 reactors is 3m3. The extractant is P204-kerosene, the concentration of P204 is 0.15mol/L, and the concentration of uranium in the uranium-loaded organic phase is 7 g/L. The concentration of the stripping agent is 130g/L ammonium carbonate and 20g/L ammonium bicarbonate. The stripping agent is added to the first reactor at the same time as the loaded organic, i.e., M1In the equipment. AUC crystals were added continuously at the same time, AUC was added as a slurry with 50% solids. The flow ratio of the stripping agent, the loaded organic phase and the slurry is QA1/QO1/QS 1-1/1/1, n 1-1, and the flow rates are 0.5m respectively3/h、0.5m3/h、0.5m3H is used as the reference value. The retention time of the organic phase is 2h, the reaction temperature is 50 ℃, and the crystal content in the equipment is 16.7 percent (V/V). The mixed phase enters a reactor M in sequence2A reactor M3A reactor M4Double-interface complementary-collection three-phase separation equipment S1. The double-interface complementary-collection three-phase separation equipment controls the liquid interface outside the central barrel to be higher than the lower edge of the central barrel, the rake paddle is used for stirring at a low speed, the underflow slurry is continuously pumped out, one part returns, the other part is reserved as a product, and the product amount is 3.5 kgU/h. The crystallization mother liquor return rate was 1-m 1-0.95, and n 1-m 1-0.05. And (4) evaporating ammonia to precipitate uranium from the discharged crystallization mother liquor. Adding water to absorb ammonium bicarbonate to obtain a concentrated ammonium bicarbonate solution, and using the concentrated ammonium bicarbonate solution for preparing a stripping agent and carrying out AUC transformation crystallization. Each M device discharged large precipitated crystals at irregular intervals. All crystals were washed and filtered to give the AUC product. The poor organic phase is clarified and not carried, the uranium concentration is 15mg/L, the crystallization mother liquor is clarified and not carried, and the AUC product is a large-particle crystal.
Example 3
By using M1～M6Reactor and double-interface complementary-recovery three-phase separation equipment S1. The effective volume of 6 reactors is 1m3. The extractant is P204-kerosene, the concentration of P204 is 0.10mol/L, and the concentration of uranium in the uranium-loaded organic phase is 5 g/L. The concentration of the stripping agent is 70g/L ammonium carbonate and 10g/L ammonium bicarbonate. The stripping agent is added to the first reactor at the same time as the loaded organic, i.e., M1In the equipment. AUC crystals were added continuously at the same time, AUC was added as a slurry with 50% solids. The flow ratio of the stripping agent, the loaded organic phase and the slurry is QA1/QO1/QS 1-2/1/1, n 1-2, and the flow rates are 1m respectively3/h、0.25m3/h、0.25m3H is used as the reference value. The retention time of the organic phase is 0.5h, the reaction temperature is 40 ℃, and the crystal content in the equipment is (V/V)12.5 percent. The mixed phase enters a reactor M in sequence2A reactor M3A reactor M4A reactor M5A reactor M6Double-interface complementary-collection three-phase separation equipment S1. The double-interface complementary-collection three-phase separation equipment controls the liquid interface outside the central barrel to be higher than the lower edge of the central barrel, crystals are discharged intermittently, the intermittent time is 2 hours, and the rake is started for 10min before the crystals are discharged. Aggregate the coarse crystalsThe fine grains are suspended, and the rake paddles are closed after the discharge. A part of the discharged slurry is returned, and a part of the discharged slurry is reserved as a product, wherein the product amount is 2.5 kgU/h. The crystallization mother liquor return rate was 1-m1 ═ 0.95, and n1 × m1 was 0.1. And (4) evaporating ammonia to precipitate uranium from the discharged crystallization mother liquor. Adding water to absorb ammonium bicarbonate to obtain a concentrated ammonium bicarbonate solution, and using the concentrated ammonium bicarbonate solution for preparing a stripping agent and carrying out AUC transformation crystallization. Each M device discharged large precipitated crystals at irregular intervals. All crystals were washed and filtered to give the AUC product. The lean organic phase is clarified and not entrained, the uranium concentration is 20mg/L, the crystallization mother liquor is clarified and not entrained, and the AUC product is a large-particle crystal.
Example 4
By using M1～M3Reactor and double-interface complementary-recovery three-phase separation equipment S1. The effective volume of 3 reactors is 4m3. The extractant is P204-kerosene, the concentration of P204 is 0.15mol/L, and the concentration of uranium in the uranium-loaded organic phase is 7 g/L. The concentration of the stripping agent is 100g/L ammonium carbonate and 15g/L ammonium bicarbonate. The stripping agent is added to the first reactor at the same time as the loaded organic, i.e., M1In the equipment. AUC crystals were added continuously at the same time, AUC was added as a slurry with 50% solids. The flow ratio of the stripping agent, the loaded organic phase and the slurry is QA1/QO1/QS 1-1/1/2, n 1-1, and the flow rates are 0.25m respectively3/h、0.25m3/h、0.5m3H is used as the reference value. The retention time of the organic phase is 4h, the reaction temperature is 30 ℃, and the crystal content in the equipment is 25 percent (V/V). The mixed phase enters a reactor M in sequence2A reactor M3Double-interface complementary-collection three-phase separation equipment S1. The double-interface complementary-collection three-phase separation equipment controls the liquid interface outside the central barrel to be higher than the lower edge of the central barrel, the rake paddle is used for stirring at a low speed, the underflow slurry is continuously pumped out, one part returns, the other part is reserved as a product, and the product amount is 1.75 kgU/h. The crystallization mother liquor return rate was 1-m 1-0.95, and n 1-m 1-0.05. And (4) evaporating ammonia to precipitate uranium from the discharged crystallization mother liquor. Adding water to absorb ammonium bicarbonate to obtain a concentrated ammonium bicarbonate solution, and using the concentrated ammonium bicarbonate solution for preparing a stripping agent and carrying out AUC transformation crystallization. Each M device discharged large precipitated crystals at irregular intervals. All crystals were washed and filtered to give the AUC product. The poor organic phase is clarified and not carried, the uranium concentration is 5mg/L, the crystallization mother liquor is clarified and not carried, and the AUC product is a large-particle crystal.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The high-clarity crystallization stripping method in the uranium extraction process is characterized by comprising the following steps of:
step 1: mixing and reacting the organic phase loaded with uranium, a back-extraction agent and uranyl tricarbonate slurry, and keeping the reaction temperature at 30-50 ℃ to obtain a mixed phase;
the back extractant is ammonium carbonate and/or ammonium bicarbonate, and the concentration of the back extractant is 50-150 g/L;
the flow ratio n1 of the stripping agent to the organic phase loaded with uranium is 1-4;
step 2: inputting the mixed phase into a double-interface complementary-recovery three-phase separation device, stirring by a rake of the double-interface complementary-recovery three-phase separation device, continuously discharging underflow slurry, using the discharged crystallization mother liquor for preparing uranyl tricarbonate and preparing the back-extraction agent,
the double-interface complementary-collection three-phase separation equipment comprises: s, a cylinder body, the lower part of which is conical;
the central barrel is arranged at the upper part in the S barrel and is coaxial with the S barrel;
a first mixed phase inlet disposed at the top of the core barrel;
the water phase outlets are arranged at the lower part of the side wall of the S cylinder body, are provided with a plurality of water phase outlets according to different heights and are used for discharging water phases;
the crystal outlet is arranged at the bottom of the S cylinder;
the rake paddle is arranged in the S cylinder body and penetrates through the central cylinder;
the overflow weir plate is arranged at the upper part of the S-shaped cylinder body, is lower than the upper edge of the central cylinder and is used for discharging an organic phase;
the lower edge of the central barrel and the upper edge of the overflow weir plate are provided with a plurality of triangular openings;
and the organic phase outlet is arranged at the upper part of the outer wall of the S cylinder and is used for discharging the organic phase flowing out of the overflow weir plate.
2. The method for high-clarity crystal stripping in the uranium extraction process according to claim 1, wherein in the step 1, the organic phase loaded with uranium, the stripping agent and the slurry of the uranyl tricarbonate are added into a first reactor for mixing reaction,
the first reactor comprises: a barrel; the stirring paddle is arranged in the cylinder body and used for continuously stirring;
the replenishing port is arranged at the top of the cylinder body and is used for adding various raw materials;
the conical bottom outlet is arranged at the bottom of the cylinder and used for discharging crystals;
the second mixed phase inlet is arranged at the upper part of the side wall of the cylinder;
the mixed phase outlet is arranged at the upper part of the side wall of the cylinder body;
the height from the mixed phase inlet to the cylinder bottom is greater than the height from the mixed phase outlet to the cylinder bottom.
3. The high-clarity crystal stripping method in the uranium extraction process according to claim 2, wherein the mixed phase is discharged from the first reactor and then sequentially enters 2-10 reactors for further treatment, and the reactors have the same structure as the first reactor.
4. A method for high-clarity crystal stripping in a uranium extraction process according to claim 3, wherein the crystal retention in the first reactor and the reactor is 1/10V-1/3V;
and a part of the crystals discharged from the reactor is used as a product, and a part of the crystals is returned to the first reactor and continuously and stably added.
5. The method for high-clarity crystal stripping in uranium extraction process according to claim 1, wherein in step 2, the discharge rate of the crystallization mother liquor is m1, and n1 x m1 is no more than 1/5.
6. A uranium extraction process high clarity crystal stripping process according to claim 1, wherein the first reactor and the control aqueous phase within the reactor are continuous.
7. The high-clarity crystal stripping method in the uranium extraction process according to claim 1, wherein the double-interface complementary three-phase separation equipment intermittently discharges crystals or continuously discharges crystals, the intermittent time is 0.5-24 hours when the crystals are intermittently discharged, and a rake paddle is started before the crystals are discharged; coarse crystals are gathered and fine crystals are suspended, and the rake paddle is closed after the discharge;
when the crystal is discharged continuously, the rake paddle rotates continuously.
8. The high-clarity crystallization stripping method in the uranium extraction process according to claim 1, wherein an insulating layer is arranged on the outer wall of the double-interface replenishment three-phase separation equipment, and the temperature in the double-interface replenishment three-phase separation equipment is 30-50 ℃.
9. The method for high-clarity crystal stripping in the uranium extraction process according to claim 1, wherein in the step 2, when the discharged crystallization mother liquor is used for preparing uranyl tricarbonate, the method specifically comprises the following steps: the crystallization mother liquor is heated to ammonium carbonate for decomposition, uranium precipitates, and gas generated by decomposition is absorbed by water to obtain ammonium carbonate solution, and the ammonium carbonate solution is used for preparing the back-extraction agent.
10. The method for high-clarity crystal stripping in the uranium extraction process according to claim 1, wherein in the step 1, the residence time of the organic phase is 0.5-4 hours.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2235127A1 (en) * | 1995-10-19 | 1997-04-24 | Bayer Aktiengesellschaft | Multistage three-phase extractor |
| CN106507819B (en) * | 2007-12-26 | 2011-02-16 | 核工业北京化工冶金研究院 | The technique of back extraction crystallization production ammonium uranyl tricarbonate |
| CN102127639A (en) * | 2010-12-23 | 2011-07-20 | 核工业北京化工冶金研究院 | Preparation method of high-clarity uranium solution |
| WO2012097480A1 (en) * | 2011-01-19 | 2012-07-26 | 中国科学院过程工程研究所 | Liquid-liquid-liquid three-phase continuous countercurrent extraction device and use thereof |
| CN202527171U (en) * | 2012-03-20 | 2012-11-14 | 中国天辰工程有限公司 | Reaction device applied to gas-liquid-liquid-solid multiphase reaction |
| CN103397184A (en) * | 2013-07-31 | 2013-11-20 | 南昌航空大学 | Method for separating uranium and iron from tertiary amine organic phase by back extraction |
| CN110144455A (en) * | 2018-12-29 | 2019-08-20 | 核工业北京化工冶金研究院 | A kind of back extraction device and method loading molybdenum TFA organic phase |
-
2020
- 2020-12-16 CN CN202011487262.7A patent/CN112680607B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2235127A1 (en) * | 1995-10-19 | 1997-04-24 | Bayer Aktiengesellschaft | Multistage three-phase extractor |
| CN106507819B (en) * | 2007-12-26 | 2011-02-16 | 核工业北京化工冶金研究院 | The technique of back extraction crystallization production ammonium uranyl tricarbonate |
| CN102127639A (en) * | 2010-12-23 | 2011-07-20 | 核工业北京化工冶金研究院 | Preparation method of high-clarity uranium solution |
| WO2012097480A1 (en) * | 2011-01-19 | 2012-07-26 | 中国科学院过程工程研究所 | Liquid-liquid-liquid three-phase continuous countercurrent extraction device and use thereof |
| CN202527171U (en) * | 2012-03-20 | 2012-11-14 | 中国天辰工程有限公司 | Reaction device applied to gas-liquid-liquid-solid multiphase reaction |
| CN103397184A (en) * | 2013-07-31 | 2013-11-20 | 南昌航空大学 | Method for separating uranium and iron from tertiary amine organic phase by back extraction |
| CN110144455A (en) * | 2018-12-29 | 2019-08-20 | 核工业北京化工冶金研究院 | A kind of back extraction device and method loading molybdenum TFA organic phase |
Non-Patent Citations (3)
| Title |
|---|
| 《铀水冶基础知识》编写组: "《铀水冶基础知识》", 31 December 1978, 原子能出版社 * |
| 张伟强: "《固态金属及合金中的相变》", 31 May 2016, 国防工业出版社 * |
| 韦悦周等: "《最新核燃料循环》", 31 March 2016, 上海交通大学出版社 * |
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