CN113667844B - Device and method for leaching sandstone uranium ore through micro-nano bubble oxidation - Google Patents
Device and method for leaching sandstone uranium ore through micro-nano bubble oxidation Download PDFInfo
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- CN113667844B CN113667844B CN202110968246.8A CN202110968246A CN113667844B CN 113667844 B CN113667844 B CN 113667844B CN 202110968246 A CN202110968246 A CN 202110968246A CN 113667844 B CN113667844 B CN 113667844B
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- 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
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- 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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Abstract
The invention discloses a device and a method for leaching sandstone uranium ore by micro-nano bubble oxidation, belonging to the technical field of leaching uranium mining, and the device comprises a reactor, a first pump, a second pump and a sampling port, wherein the reactor is provided with a first liquid inlet, a first liquid outlet, a fourth liquid inlet, a first pump liquid port and a sampling port; the micro-nano bubble generator is provided with a second liquid inlet, a second liquid outlet and a gas inlet; oxygen generator, ozone generator and CO 2 The steel cylinders are connected with the air inlet of the micro-nano bubble generator; the bottom of the reaction column is provided with a third liquid inlet which is connected with the first pump liquid inlet through a peristaltic pump; a fluid replenishment tank having a second pump fluid port: the fourth liquid inlet is connected with the second pump liquid inlet through a peristaltic pump; the liquid collecting tank is connected with the exhaust liquid outlet; the liquid collecting tank is provided with an air outlet; and the absorption tank is filled with KI solution. According to the invention, the sandstone uranium ore is quickly oxidized and leached by adopting the micro-nano bubble generator, the oxidation leaching rate and the oxidation rate of uranium are greatly improved, the consumption of oxygen and carbon dioxide is reduced, the generated impurities are less, and the method is green and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of leaching uranium mining, and particularly relates to a device and a method for oxidizing and leaching sandstone uranium ore by using micro-nano bubbles.
Background
Internationally, the technique of in-situ uranium mining has become an important method of uranium mining, where CO is used 2 +O 2 The leaching process is formally and industrially applied in a plurality of production areas after years of experimental research in China. But CO 2 +O 2 The problems of high energy consumption for preparing leaching solution, high oxygen consumption, low oxygen utilization rate, insufficient oxidation efficiency and the like exist in the uranium leaching process.
In the traditional ozone treatment process in the prior art, because ozone concentration is low, the solubility in water is poor, the energy consumption in the production process is high, the ozone utilization efficiency is low, and the traditional chemical agent is used, but the addition of the agent can cause harm to the environment, and the quality performance of the recovered stock solution is influenced.
The micro-nano bubbles have small size, have the excellent characteristics of long existence time, high mass transfer efficiency, high zeta potential formed by surface charges, capability of releasing free radicals and the like, and have obvious technical advantages in multiple fields. Therefore, at present, CO 2 +O 2 Under the condition of the in-situ leaching uranium extraction process, how to replace an oxygen pressurization dissolving process by using a micro-nano oxygen generator on site improves the oxygen utilization rate, saves the oxygen consumption, improves the oxidation effect, effectively reduces the production cost of the uranium leaching process, and has very important practical significance.
Therefore, an apparatus and a method for oxidizing sandstone uranium ore by micro-nano bubbles, which can improve the oxidation efficiency, improve the leaching effect of uranium, accelerate the leaching of uranium and improve the economic benefit, are urgently needed.
Disclosure of Invention
The invention provides a device and a method for oxidizing sandstone uranium ores by micro-nano bubbles, which can improve oxidation efficiency, improve leaching effect of uranium, accelerate leaching of uranium and improve economic benefit, and adopts the following technical scheme:
a device that micro-nano bubble oxidation leached sandstone uranium ore, includes:
the device comprises a reactor, a first liquid outlet, a second liquid outlet, a third liquid outlet, a fourth liquid outlet, a first pump liquid port and a sampling port, wherein a mechanical stirrer is arranged in the reactor;
the micro-nano bubble generator is provided with a second liquid inlet, a second liquid outlet and an air inlet, and the second liquid inlet and the second liquid outlet are respectively connected with the first liquid outlet and the first liquid inlet;
oxygen generator, ozone generator and CO 2 Steel cylinder, oxygen generator, ozone generator and CO 2 The steel cylinders are connected with the air inlet of the micro-nano bubble generator;
the bottom of the reaction column is provided with a third liquid inlet, and the top of the reaction column is provided with an exhaust liquid outlet; the third liquid inlet is connected with the first pump liquid inlet through a peristaltic pump;
a make-up tank having a second pump port; the fourth liquid inlet is connected with the second pump liquid inlet through a peristaltic pump;
the liquid collecting tank is connected with the exhaust liquid outlet; the liquid collecting tank is provided with an air outlet;
the absorption tank is provided with an air inlet, and the air inlet of the absorption tank is connected with the air outlet of the liquid collecting tank; ozone is filled in the absorption tank, passes through KI solution and is used for absorbing the ozone discharged by the reactor.
Furthermore, the oxygen generator is an air source, and the concentration of the generated oxygen is 90-96%; the ozone generator belongs to an air source air-cooling ozone and oxygen integrated machine, and the ozone yield is 10 g.h -1 (ii) a The CO is 2 A first connecting pipe is arranged between the steel cylinder and the micro-nano bubble generator, and a pressure reducing valve and a gas flowmeter are arranged on the first connecting pipe.
Further, the micro-nano bubble generator is provided with a cooling water pipeline for adjusting the temperature of the liquid in the reactor.
A method for oxidizing and leaching sandstone uranium ore by using micro-nano bubbles is a device for oxidizing and leaching sandstone uranium ore by using any one of the micro-nano bubbles, and comprises the following steps:
s10, preparing a micro-nano bubble solution: filling tap water with a certain volume into a reactor and a solution supplementing tank, and adjusting the pH value of the solution by sulfuric acid or sodium hydroxide; simultaneously turning on the micro-nano generator, the ozone generator, the oxygen generator and the CO 2 A steel cylinder, setting relevant parameters, and completing the preparation of the micro-nano bubble solution in the reactor after the standby device runs stably;
s20, monitoring dissolved oxygen of the micro-nano bubble solution: starting a mechanical stirrer to fully and uniformly mix the micro-nano bubble solution, and sampling from a sampling port at regular intervals to analyze the concentration of ozone in the solution;
s30, micro-nano bubble solution column leaching: filling a reaction column with an ore sample to be leached, setting the rotating speed of a peristaltic pump, extracting the mixed solution in the reactor at a constant speed, and injecting the mixed solution from the bottom of the reaction column; the mixed solution is guided to a liquid collecting tank through an exhaust liquid outlet or directly guided to a reactor; after normal operation, sampling and analyzing within a set time;
s40, leaching the sandstone uranium ore treated by the micro-nano ozone bubbles for half an hour under the acidic condition by stirring and leaching according to preset gas flow and ozone concentration in the solution; or under neutral condition, continuously introducing CO 2 Stirring and leaching, wherein leaching is carried out for two hours according to the preset gas flow and the ozone concentration in the solution;
s50, absorbing the ozone discharged by the reaction column by an absorption tank.
Further, in step S10, the micro-nano generator, the ozone generator, the oxygen generator, and the CO are turned on simultaneously 2 And a steel cylinder, wherein gas flow and generated gas concentration parameters are set, and after the standby device runs for 5min stably, the preparation of the micro-nano bubble solution is completed in the reactor.
Further, in step S20, the micro-nano bubble generator generates bubbles with a diameter of 100nm to 10 μm; in step S30, the adjustable liquid flow rate of the peristaltic pump is 0-2L/h.
Further, in step S40, under agitation leaching under acidic conditions of pH 1, leaching was performed for half an hour with an ozone concentration of 11mg/L in the solution at a gas flow rate of 1L/min; or continuously introducing CO under the neutral condition of pH 6.8 2 And (4) stirring and leaching for two hours according to the gas flow rate of 1L/min and the ozone concentration of 11mg/L in the solution.
Has the advantages that:
according to the device for oxidizing and leaching sandstone uranium ore by using micro-nano bubbles, provided by the invention, the sandstone uranium ore is quickly oxidized and leached by using the micro-nano bubble generator, the oxidation leaching rate and the oxidation rate of uranium are greatly improved, the use amounts of oxygen and carbon dioxide are reduced, the generated impurities are few, and the device is green and environment-friendly.
At the same time, is beneficial to perfecting and developing CO 2 +O 2 The in-situ leaching uranium mining technology provides basic theory and technical support for the sustainable development of the technology.
Drawings
FIG. 1 is a schematic structural diagram of a device for oxidizing and leaching sandstone uranium ore by using micro-nano bubbles, which is provided by the invention;
wherein, 1, a reactor; 2. a micro-nano bubble generator; 3. an oxygen generator; 4. an ozone generator; 5. CO2 2 A steel cylinder; 6. a sampling port; 7. a gas flow meter; 8. a reaction column; 9. a liquid collecting tank; 10. a peristaltic pump; 11. an absorption tank; 12. a pressure reducing valve; 13. an outer pipe of the cooling water pipeline; 14. a mechanical stirrer; 15. an exhaust liquid outlet; 16. and a liquid supplementing tank.
Detailed Description
Example 1
A device for leaching sandstone uranium ore by micro-nano bubble oxidation (refer to figure 1) comprises a reactor 1, a micro-nano bubble generator 2, an oxygen generator 3, an ozone generator 4 and CO 2 A steel cylinder 5, a reaction column 8, a liquid collecting tank 9 and an absorption tank 11.
The reactor 1 is provided with a first liquid inlet, a first liquid outlet, a fourth liquid inlet, a first pump liquid port and a sampling port 6, and a mechanical stirrer 14 is arranged in the reactor 1.
In this embodiment, the micro-nano bubble generator 2 has a second liquid inlet, a second liquid outlet and an air inlet, and the second liquid inlet and the second liquid outlet are respectively connected with the first liquid outlet and the first liquid inlet.
In the present embodiment, oxygen generator 3, ozone generator 4 and CO 2 The steel cylinders 5 are connected with the air inlet of the micro-nano bubble generator 2.
The bottom of the reaction column 8 is provided with a third liquid inlet, and the top is provided with an exhaust liquid outlet 15; the third liquid inlet is connected with the first pump liquid inlet through a peristaltic pump 10.
The liquid collecting groove 9 is connected with an exhaust liquid outlet 15; the sump 9 has an exhaust.
The bottom of the liquid supplementing tank 16 is provided with a second pump liquid port; the fourth liquid inlet is connected with the second pump liquid inlet through a peristaltic pump 10;
an absorption tank 11, wherein the absorption tank 11 is provided with an air inlet, and the air inlet of the absorption tank 11 is connected with an air outlet of the liquid collecting tank 9; KI solution is filled in the absorption tank 11 and is used for absorbing ozone discharged from the reactor 1.
In the embodiment, the oxygen generator 3 is an air source, and the concentration of the generated oxygen is 90-96%; the ozone generator 4 belongs to an air source air cooling ozone and oxygen integrated machine, and the ozone yield is 10 g.h -1 ；CO 2 A first connecting pipe is arranged between the steel cylinder 5 and the micro-nano bubble generator 2, a pressure reducing valve 12 and a gas flowmeter 7 are arranged on the first connecting pipe, and the micro-nano bubble generator 2 can be supplied with stable flow CO 2 A gas.
In this embodiment, micro-nano bubble generator 2 is provided with the cooling water pipeline of the liquid temperature in adjusting reactor 1, and the micro-nano bubble generator 2 outside is provided with cooling water pipeline outer tube 13 for the input cooling water. Wherein, the temperature of the liquid in the reactor 1 can be adjusted to about 25 ℃ at normal temperature by adjusting the cooling water pipeline when the micro-nano generator 2 generates heat in operation.
Wherein, the cooling circulation setting of cooling water pipeline is prior art, and is not repeated here.
In this embodiment, a circulation pump is disposed inside the micro-nano bubble generator 2, so that the liquid between the micro-nano bubble generator 2 and the reactor 1 flows.
In this embodiment, in the micro-nano generator 2, the mixed gas is directly injected into the liquid.
Example 2
The embodiment provides a method for leaching sandstone uranium ore through micro-nano bubble oxidation, and the device for leaching sandstone uranium ore through micro-nano bubble oxidation provided by the embodiment 1 comprises the following steps:
s10, preparing a micro-nano bubble solution: a certain volume of tap water is filled in the reactor 1 and the liquid supplementing tank 16, and the pH value of the solution is adjusted by sulfuric acid or sodium hydroxide; simultaneously turning on the micro-nano generator, the ozone generator 4, the oxygen generator 3 and CO 2 The steel bottle 5 to set for relevant parameter, standby device operation after stable, the preparation of micro-nano bubble solution is accomplished in the reactor 1 promptly.
WhereinSimultaneously turning on the micro-nano generator, the ozone generator 4, the oxygen generator 3 and CO 2 And a steel cylinder 5, wherein gas flow and generated gas concentration parameters are set, and the preparation of the micro-nano bubble solution is completed in the reactor 1 after the operation of the standby device is stable for 5 min.
S20, stirring and leaching the micro-nano bubble solution: and starting the mechanical stirrer 14 to fully and uniformly mix the micro-nano bubble solution, and sampling from the sampling port 6 at regular intervals to analyze the concentration of ozone (dissolved oxygen) in the solution.
Wherein, the diameter of the bubbles generated by the micro-nano bubble generator 2 is 100nm-10 μm.
S30, micro-nano bubble solution column leaching: filling a reaction column 8 with an ore sample to be leached, setting the rotating speed of a peristaltic pump 10, extracting the mixed solution in the reactor 1 at a constant speed, injecting the mixed solution from the bottom of the reaction column 8, extracting the mixed solution in a solution supplementing tank 16 at a constant speed, injecting the mixed solution from the top of the reactor 1, and supplementing the solution to the reactor 1; the mixed solution is guided to the liquid collecting tank 9 through the exhaust liquid outlet 15 or directly guided to the reactor 1; after normal operation, sampling and analyzing within a set time.
Wherein, the adjustable liquid flow of the peristaltic pump 10 is 0-4L/h.
S40, leaching the sandstone uranium ore treated by the micro-nano ozone bubbles for half an hour under the acidic condition by stirring and leaching according to preset gas flow and ozone concentration in the solution; or under neutral condition, continuously introducing CO 2 And (4) stirring and leaching, wherein leaching is carried out for two hours according to the preset gas flow and the ozone concentration in the solution.
In step S40, under the acidic condition of pH 1, under the condition of agitation leaching, according to the air flow rate of 1L/min, the ozone concentration in the solution is 11mg/L, the leaching is carried out for half an hour, and the leaching rate can reach 96.31%; or continuously introducing CO under the neutral condition of pH 6.8 2 And (3) stirring and leaching, wherein the leaching rate can reach 95.25% in two hours according to the gas flow rate of 1L/min and the ozone concentration of 11mg/L in the solution.
S50, ozone discharged from the reaction column 8 is absorbed by the absorption tank 11.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (6)
1. The method for oxidizing and leaching sandstone uranium ore by using micro-nano bubbles is characterized in that the device for oxidizing and leaching sandstone uranium ore by using micro-nano bubbles is used for oxidizing and leaching, and comprises the following steps:
the device comprises a reactor, a first liquid outlet, a second liquid outlet, a third liquid outlet, a fourth liquid outlet, a first pump liquid port and a sampling port, wherein a mechanical stirrer is arranged in the reactor;
the micro-nano bubble generator is provided with a second liquid inlet, a second liquid outlet and an air inlet, and the second liquid inlet and the second liquid outlet are respectively connected with the first liquid outlet and the first liquid inlet;
oxygen generator, ozone generator and CO 2 The oxygen generator, the ozone generator and the CO2 steel cylinder are all connected with an air inlet of the micro-nano bubble generator;
the bottom of the reaction column is provided with a third liquid inlet, and the top of the reaction column is provided with an exhaust liquid outlet; the third liquid inlet is connected with the first pump liquid inlet through a peristaltic pump;
a make-up tank having a second pump port; the fourth liquid inlet is connected with the second pump liquid inlet through a peristaltic pump;
the liquid collecting tank is connected with the exhaust liquid outlet; the liquid collecting tank is provided with an air outlet;
the absorption tank is provided with an air inlet, and the air inlet of the absorption tank is connected with the air outlet of the liquid collecting tank; KI solution is filled in the absorption tank and is used for absorbing ozone discharged by the reactor;
the method comprises the following steps:
s10, preparing a micro-nano bubble solution: filling tap water with a certain volume into the reactor and the liquid supplementing tank, and adjusting the pH value of the solution by sulfuric acid or sodium hydroxide; simultaneously turning on the micro-nano generator and the ozone generator,Oxygen generator, CO 2 A steel cylinder, setting relevant parameters, and completing the preparation of the micro-nano bubble solution in the reactor after the standby device runs stably;
s20, monitoring dissolved oxygen of the micro-nano bubble solution: starting a mechanical stirrer to fully and uniformly mix the micro-nano bubble solution, and sampling from a sampling port at regular intervals to analyze the concentration of ozone in the solution;
s30, micro-nano bubble solution column leaching: filling a reaction column with an ore sample to be leached, setting the rotating speed of a peristaltic pump, extracting the mixed solution in the reactor at a constant speed, injecting the mixed solution from the bottom of the reaction column, extracting the mixed solution in the liquid supplementing tank at a constant speed, and injecting the mixed solution from the top of the reactor; the mixed solution is guided to a liquid collecting tank through an exhaust liquid outlet or directly guided to a reactor; after normal operation, sampling and analyzing within a set time;
s40, leaching the sandstone uranium ore treated by the micro-nano ozone bubbles for half an hour under the acidic condition by stirring and leaching according to preset gas flow and ozone concentration in the solution; or under neutral condition, continuously introducing CO 2 Stirring and leaching, wherein leaching is carried out for two hours according to the preset gas flow and the ozone concentration in the solution;
s50, absorbing the ozone discharged from the reaction column by an absorption tank.
2. The method for the oxidative leaching of sandstone uranium ore through micro-nano bubbles according to claim 1, wherein the oxygen generator is an air source, and the produced oxygen concentration is 90% -96%; the ozone generator belongs to an air source air cooling ozone and oxygen integrated machine, and the ozone yield is 10 g.h < -1 >; a first connecting pipe is arranged between the CO2 steel cylinder and the micro-nano bubble generator, and a pressure reducing valve and a gas flowmeter are arranged on the first connecting pipe.
3. The method for the oxidative leaching of sandstone uranium ores according to claim 1, wherein the micro-nano bubble generator is provided with a cooling water pipeline for adjusting the temperature of liquid in the reactor.
4. The method for the oxidative leaching of sandstone uranium ore through micro-nano bubbles according to claim 1, wherein in step S10, the micro-nano generator, the ozone generator, the oxygen generator and the CO are turned on simultaneously 2 And a steel cylinder, wherein gas flow and generated gas concentration parameters are set, and after the standby device runs for 5min stably, the preparation of the micro-nano bubble solution is completed in the reactor.
5. The method for the oxidative leaching of sandstone uranium ore through micro-nano bubbles according to claim 1, wherein in step S20, the micro-nano bubble generator generates bubbles with diameters of 100nm to 10 μm; in step S30, the adjustable liquid flow rate of the peristaltic pump is 0-4L/h.
6. The method for the oxidative leaching of sandstone uranium ore through micro-nano bubbles according to claim 1, wherein in step S40, under the acidic condition of pH =1, leaching is carried out for half an hour according to the gas flow rate of 1L/min and the ozone concentration of 11mg/L in the solution; or, at neutral conditions of pH =6.8, continuously feeding CO 2 The solution is leached out for two hours under the conditions that the air flow is 1L/min and the ozone concentration in the solution is 11 mg/L.
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| CN116240406A (en) * | 2021-12-08 | 2023-06-09 | 核工业北京化工冶金研究院 | Sandstone uranium ore strong oxidation leaching method adopting micro-nano bubbles |
| CN115305357B (en) * | 2022-08-17 | 2023-09-05 | 四川省银河化学股份有限公司 | Method for preparing sodium chromate by taking vanadium-chromium reduction slag as raw material |
| CN115612869B (en) * | 2022-09-27 | 2024-02-13 | 核工业北京化工冶金研究院 | Neutral in-situ uranium ore mountain secondary intensified leaching method |
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| CN107460349A (en) * | 2017-07-06 | 2017-12-12 | 核工业北京化工冶金研究院 | A kind of in-situ acid uranium leaching laboratory simulation device and test method |
| CN109825700A (en) * | 2019-03-18 | 2019-05-31 | 中国科学院过程工程研究所 | A kind of method of valuable metal in low-temperature atmosphere-pressure selective extraction nickel sulfide concentrate |
| CN111074084A (en) * | 2019-12-20 | 2020-04-28 | 核工业北京化工冶金研究院 | Ground soaks uranium mining full-flow circulation experimental apparatus |
| CN111187925A (en) * | 2020-02-28 | 2020-05-22 | 南华大学 | Device and method for strengthening uranium leaching by pulse microwave synergistic dielectric barrier gas discharge |
| CN211999868U (en) * | 2020-02-28 | 2020-11-24 | 南华大学 | Gas-liquid phase pulse spark discharge strengthened uranium leaching device |
Also Published As
| Publication number | Publication date |
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| CN113667844A (en) | 2021-11-19 |
| JP2023031231A (en) | 2023-03-08 |
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