CN117438123A - Method and device for determining uranium extraction zone in extraction column and method for controlling position of uranium extraction zone - Google Patents

Method and device for determining uranium extraction zone in extraction column and method for controlling position of uranium extraction zone Download PDF

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Publication number
CN117438123A
CN117438123A CN202311778214.7A CN202311778214A CN117438123A CN 117438123 A CN117438123 A CN 117438123A CN 202311778214 A CN202311778214 A CN 202311778214A CN 117438123 A CN117438123 A CN 117438123A
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extraction column
extraction
uranium
zone
organic phase
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CN117438123B (en
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陈勇
王博
侯学锋
杨昕未
田阳
李磊
刘继连
高明媛
徐明吕
武婧
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China Nuclear Power Engineering Co Ltd
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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04—Treating liquids
    • G21F9/06—Processing
    • G21F9/12—Processing by absorption; by adsorption; by ion-exchange
    • G21F9/125—Processing by absorption; by adsorption; by ion-exchange by solvent extraction
    • 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
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
    • C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
    • C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K13/00—Thermometers specially adapted for specific purposes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
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  • Environmental & Geological Engineering (AREA)
  • Geology (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • High Energy & Nuclear Physics (AREA)
  • General Engineering & Computer Science (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention discloses a method and a device for determining a uranium extraction zone in an extraction column and a method for controlling the position of the uranium extraction zone, wherein the method for determining the uranium extraction zone comprises the following steps: respectively introducing water phase and organic phase into the extraction column from two ends of the extraction column, wherein uranium-containing substances are dissolved in the water phase, extracting uranium in the extraction column through organic phase to uranium-containing substances in the water phase, determining an exothermic standard temperature distribution area on the extraction column through time accumulation of the temperature of the extraction column, and determining a uranium extraction area in the extraction column according to the exothermic standard temperature distribution area. The invention can measure the temperature at different positions of the extraction column; judging the uranium extraction zone according to the temperature measurement result, and adjusting the position of the actual uranium extraction zone by adjusting the flow of an organic phase or a water phase after comparing the position of the actual uranium extraction zone with the position of the designed uranium extraction zone; the device is easy to overhaul, has no moving parts and adopts a modularized device.

Description

Method and device for determining uranium extraction zone in extraction column and method for controlling position of uranium extraction zone
Technical Field
The invention belongs to the technical field of spent fuel aftertreatment, and particularly relates to a method and a device for determining a uranium extraction zone in an extraction column and a method for controlling the position of the uranium extraction zone.
Background
The extraction of uranium is an important unit operation in a process of post-treatment of PUREX by a spent fuel water method and a process of pre-treatment of uranium. Extraction columns are a classical device in the unit operations described above. Aiming at controlling the position of an extraction zone of an extraction column, the countries such as China, japan, america and the like respectively carry out research work of related methods. The Japanese establishes a temperature detection model by using water phase simulation extraction processes with different temperatures on a set of laboratory-scale pulse extraction columns, but the model can only be used for temperature measurement and cannot realize a control process. Meanwhile, the device is only suitable for laboratory-scale equipment, and a measuring method for industrial-scale equipment is not yet verified.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art and provides a method and a device for determining a uranium extraction zone in an extraction column and a method for controlling the position of the uranium extraction zone, and the operation process has the characteristics of good controllability and easiness in operation.
The technical scheme adopted for solving the technical problems of the invention is to provide a method for determining a uranium extraction zone in an extraction column, which comprises the following steps:
respectively introducing water phase and organic phase into the extraction column from two ends of the extraction column, wherein uranium-containing substances are dissolved in the water phase, extracting uranium in the extraction column through organic phase to uranium-containing substances in the water phase, determining an exothermic standard temperature distribution area on the extraction column through time accumulation of the temperature of the extraction column, and determining a uranium extraction area in the extraction column according to the exothermic standard temperature distribution area.
Preferably, the aqueous phase material introduced into the extraction column contains nitric acid, and the concentration of nitric acid is 0.01mol/L to 14.5mol/L.
Preferably, the organic phase material introduced into the extraction column contains tributyl phosphate, and the concentration of tributyl phosphate is 0.01-99.9 mas%.
More preferably, the concentration of tributyl phosphate is 1 to 95mas%.
Preferably, the method for determining the uranium extraction zone in the extraction column further includes the following steps:
and introducing gas pulses into the extraction column, wherein the frequency of the gas pulses is 0.05 Hz-100 Hz.
Preferably, the pressure of the air source of the pulse generator used for introducing the air pulse is-20 MPa-50 MPa.
Preferably, the ratio of the flow rate of the organic phase to the flow rate of the aqueous phase is 0.01 to 10.
More preferably, the ratio of the flow rate of the organic phase to the flow rate of the aqueous phase is 0.02 to 9.9.
Preferably, the concentration of hexavalent uranium in the water phase feed is 0.01 g/L-1000 g/L, and the concentration of hydrogen ions is 0.01 mol/L-10 mol/L;
the concentration of hexavalent uranium in the water phase discharging is 0.00001 g/L-1000 g/L, and the concentration of hydrogen ions is 0.01 mol/L-10 mol/L.
Preferably, the flow rate of the aqueous phase introduced into the extraction column is 0.1L/h to 4999L/h.
Preferably, the concentration of hexavalent uranium in the organic phase feed is 0.00001 g/L-1000 g/L, and the concentration of hydrogen ions is 0.01 mol/L-10 mol/L;
The concentration of hexavalent uranium in the organic phase discharge is 0.01 g/L-1000 g/L, and the concentration of hydrogen ions is 0.01 mol/L-10 mol/L.
Preferably, the flow rate of the organic phase introduced into the extraction column is 0.1L/h to 4999L/h.
Preferably, the specific steps of respectively introducing the aqueous phase and the organic phase into the extraction column from two ends of the extraction column are as follows:
the organic phase is introduced into the extraction column from the bottom of the extraction column, and the aqueous phase is introduced into the extraction column from the top of the extraction column.
The invention provides a device used for the method for determining the uranium extraction zone in an extraction column, which comprises the following components:
an extraction column in which uranium-containing substances in an organic relative aqueous phase are extracted;
the water phase feeding groove is connected with a first end inlet of the extraction column and is used for introducing water phase into the extraction column, and uranium-containing substances are dissolved in the water phase;
the water phase receiving groove is connected with the outlet of the second end of the extraction column and is used for receiving water phase flowing out of the extraction column;
an organic phase feed tank connected with the second end inlet of the extraction column, wherein the organic phase feed tank is used for introducing an organic phase into the extraction column;
an organic phase receiving tank connected with the outlet of the first end of the extraction column, the organic phase receiving tank being used for receiving the organic phase flowing out of the extraction column;
The temperature measuring unit is arranged on the extraction column, and is used for measuring the temperature of each position on the extraction column and sending the temperature to the control unit;
and the control unit is used for determining an exothermic standard temperature distribution area on the extraction column through time accumulation of the temperature of the extraction column, and determining a uranium extraction area in the extraction column according to the exothermic standard temperature distribution area.
Preferably, the device further comprises:
the first metering pump is respectively connected with the first end inlet of the extraction column and the water phase feed tank;
the second metering pump is respectively connected with the second end outlet of the extraction column and the water phase receiving groove;
the third metering pump is respectively connected with the second end inlet of the extraction column and the organic phase feed tank; wherein,
the first end outlet of the extraction column is connected with the organic receiving groove, the organic receiving groove is positioned below the height of the first end outlet of the extraction column, the first end of the extraction column is the top end of the extraction column, and the second end of the extraction column is the bottom end of the extraction column.
Preferably, the device further comprises:
the pulse generator is connected with the extraction column and is used for introducing gas pulses into the extraction column.
Preferably, the extraction column is any one of baffle plate pulse extraction column, annular baffle plate pulse extraction column, nozzle plate pulse extraction column, sieve plate pulse extraction column, rotary disc extraction column and vibration sieve plate extraction column.
Preferably, in the device, the temperature measuring unit includes at least three temperature measuring points, and the number of the temperature measuring points of the temperature measuring unit is 3-1000.
Preferably, the temperature measuring unit can measure the temperature range from minus 35 ℃ to 135 ℃, the measuring accuracy range is 0.0001 ℃ to 20 ℃ and can be adjusted, and the measuring altitude range is minus 10000m to 8848m.
Preferably, the first metering pump, the second metering pump and the third metering pump can be adjusted according to the measurement result of the temperature measurement unit, the flow adjustment range is 0L/h-5000L/h, and the flow adjustment precision range is 0.0001L/h-100L/h.
The invention also provides a method for controlling the position of the uranium extraction zone in the extraction column, which comprises the following steps:
1) Determining a uranium extraction zone in the extraction column by using the method;
2) Detecting the temperature of the extraction column in real time, comparing the real-time temperature of the uranium extraction zone with the exothermic standard temperature distribution zone, and judging whether to adjust the flow of the water phase and/or the organic phase introduced into the extraction column to adjust the exothermic standard temperature distribution zone corresponding to the real-time temperature of the uranium extraction zone.
Preferably, the step compares the real-time temperature of the uranium extraction zone with an exothermic standard temperature distribution zone, and judges whether to adjust the flow rate of the aqueous phase and/or the organic phase introduced into the extraction column to adjust the exothermic standard temperature distribution zone corresponding to the real-time temperature of the uranium extraction zone, specifically:
When the real-time temperature of the uranium extraction zone corresponds to the exothermic standard temperature distribution zone, maintaining the flow of the water phase and the organic phase which are introduced into the extraction column;
when the real-time temperature of the uranium extraction zone is changed relative to the exothermic standard temperature distribution zone, the flow of the water phase or the organic phase which is introduced into the extraction column is adjusted to adjust the real-time temperature of the uranium extraction zone, and the real-time temperature corresponds to the exothermic standard temperature distribution zone.
Preferably, when the real-time temperature of the uranium extraction zone is changed relative to the exothermic standard temperature distribution zone, the flow rate of the aqueous phase or the organic phase introduced into the extraction column is adjusted to adjust the real-time temperature of the uranium extraction zone, and the exothermic standard temperature distribution zone corresponds to the steps of:
when the real-time temperature of the uranium extraction zone is changed relative to the exothermic standard temperature distribution zone, detecting the real-time temperature distribution zone corresponding to the exothermic standard temperature distribution zone on the extraction column, and adjusting the flow of the water phase or the organic phase introduced into the extraction column according to the position of the real-time temperature distribution zone to adjust the real-time temperature of the uranium extraction zone, wherein the real-time temperature corresponds to the exothermic standard temperature distribution zone.
Preferably, the step adjusts the flow rate of the aqueous phase or the organic phase introduced into the extraction column to adjust the real-time temperature of the uranium extraction zone according to the position of the real-time temperature distribution zone, and the real-time temperature of the uranium extraction zone corresponds to the exothermic standard temperature distribution zone, specifically:
When the real-time temperature distribution area deviates to the organic phase inlet of the extraction column relative to the uranium extraction area, the flow rate of the organic phase introduced into the extraction column is increased or the flow rate of the water phase introduced into the extraction column is reduced, and the real-time temperature of the uranium extraction area is adjusted to correspond to the exothermic standard temperature distribution area.
Preferably, the step adjusts the flow rate of the aqueous phase or the organic phase introduced into the extraction column to adjust the real-time temperature of the uranium extraction zone according to the position of the real-time temperature distribution zone, and the real-time temperature of the uranium extraction zone corresponds to the exothermic standard temperature distribution zone, specifically:
when the real-time temperature distribution area deviates to the water phase inlet of the extraction column relative to the uranium extraction area, increasing the water phase flow rate introduced into the extraction column or reducing the organic phase flow rate introduced into the extraction column, and adjusting the real-time temperature of the uranium extraction area to correspond to the exothermic standard temperature distribution area.
The method and the device for determining the uranium extraction zone in the extraction column and the method for controlling the uranium extraction zone position provided by the invention have the following outstanding advantages:
(1) The temperature at different positions of the extraction column can be measured; (2) Long service life and radiation resistance, so that the fluorescent dye can be used under the radioactive condition; (3) Judging the uranium extraction zone according to the temperature measurement result, and adjusting the position of the actual uranium extraction zone by adjusting the flow of an organic phase or a water phase after comparing the position of the actual uranium extraction zone with the position of the designed uranium extraction zone; (4) The device is easy to overhaul, has no moving parts and adopts a modularized device.
Drawings
FIG. 1 is a schematic diagram of the apparatus used in the method of determining the uranium extraction zone in an extraction column according to example 2 of the present invention.
Fig. 2 is a flow chart of a method of determining the uranium extraction zone in an extraction column in example 2 of the present invention.
Fig. 3 is a flow chart of a method of controlling the location of a uranium extraction zone in an extraction column according to example 2 of the present invention.
In the figure: 1-a pulse generator; 2-an extraction column; 3-a temperature measurement unit; 41-a first metering pump; 42-a second metering pump; 43-a third metering pump; 5-an aqueous phase feed tank; 6-an aqueous phase receiving tank; 7-an organic phase feed tank; 8-an organic phase receiving tank.
Detailed Description
The present invention will be described in further detail below with reference to the drawings and detailed description for the purpose of better understanding of the technical solution of the present invention to those skilled in the art.
Embodiments of the present patent are described in detail below, examples of which are illustrated in the accompanying drawings, wherein the same or similar reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below by referring to the drawings are exemplary only for explaining the present patent and are not to be construed as limiting the present patent.
In the description of this patent, it should be understood that the terms "center," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate orientations or positional relationships based on the orientation or positional relationships shown in the drawings, merely to facilitate describing the patent and simplify the description, and do not indicate or imply that the devices or elements being referred to must have a particular orientation, be configured and operated in a particular orientation, and are therefore not to be construed as limiting the patent.
In the description of this patent, it should be noted that, unless explicitly stated and limited otherwise, the terms "mounted," "connected," and "disposed" are to be construed broadly, and may be fixedly connected, disposed, detachably connected, disposed, or integrally connected, disposed, for example. The specific meaning of the terms in this patent will be understood by those of ordinary skill in the art as the case may be.
Example 1
The embodiment provides a method for determining a uranium extraction zone in an extraction column, which comprises the following steps:
respectively introducing water phase and organic phase into the extraction column from two ends of the extraction column, wherein uranium-containing substances are dissolved in the water phase, extracting uranium in the extraction column through organic phase to uranium-containing substances in the water phase, determining an exothermic standard temperature distribution area on the extraction column through time accumulation of the temperature of the extraction column, and determining a uranium extraction area in the extraction column according to the exothermic standard temperature distribution area.
The embodiment provides an apparatus for determining a uranium extraction zone in an extraction column, including:
an extraction column in which uranium-containing substances in an organic relative aqueous phase are extracted;
The water phase feeding groove is connected with a first end inlet of the extraction column and is used for introducing water phase into the extraction column, and uranium-containing substances are dissolved in the water phase;
the water phase receiving groove is connected with the outlet of the second end of the extraction column and is used for receiving water phase flowing out of the extraction column;
an organic phase feed tank connected with the second end inlet of the extraction column, wherein the organic phase feed tank is used for introducing an organic phase into the extraction column;
an organic phase receiving tank connected with the outlet of the first end of the extraction column, the organic phase receiving tank being used for receiving the organic phase flowing out of the extraction column;
the temperature measuring unit is arranged on the extraction column, and is used for measuring the temperature of each position on the extraction column and sending the temperature to the control unit;
and the control unit is used for determining an exothermic standard temperature distribution area on the extraction column through time accumulation of the temperature of the extraction column, and determining a uranium extraction area in the extraction column according to the exothermic standard temperature distribution area.
The embodiment also provides a method for controlling the position of a uranium extraction zone in an extraction column, which comprises the following steps:
1) Determining a uranium extraction zone in the extraction column by using the method;
2) Detecting the temperature of the extraction column in real time, comparing the real-time temperature of the uranium extraction zone with the exothermic standard temperature distribution zone, and judging whether to adjust the flow of the water phase and/or the organic phase introduced into the extraction column to adjust the exothermic standard temperature distribution zone corresponding to the real-time temperature of the uranium extraction zone.
The method, the device and the method for controlling the position of the uranium extraction zone in the extraction column provided by the embodiment have the following outstanding advantages:
(1) The temperature at different positions of the extraction column can be measured; (2) Long service life and radiation resistance, so that the fluorescent dye can be used under the radioactive condition; (3) Judging the uranium extraction zone according to the temperature measurement result, and adjusting the position of the actual uranium extraction zone by adjusting the flow of an organic phase or a water phase after comparing the position of the actual uranium extraction zone with the position of the designed uranium extraction zone; (4) The device is easy to overhaul, has no moving parts and adopts a modularized device.
Example 2
As shown in fig. 2, the present embodiment provides a method for determining a uranium extraction zone in an extraction column 2, including the following steps:
s201, respectively introducing water phase and organic phase into the extraction column 2 from two ends of the extraction column 2, wherein uranium-containing substances are dissolved in the water phase;
s202, extracting uranium in an organic relative water phase in an extraction column 2 through uranium-containing substances, wherein the extraction of uranium is an exothermic reaction;
s203, determining an exothermic standard temperature distribution area on the extraction column 2 through time accumulation of the temperature of the extraction column 2;
s204, determining a uranium extraction zone in the extraction column 2 according to the exothermic standard temperature distribution zone.
The temperature distribution in the middle section of the extraction column 2 in the height direction varies considerably because of the large amount of heat released during the extraction. Judging and controlling the position of the uranium extraction zone according to the morphology of the temperature distribution is an important method.
Preferably, the aqueous phase material introduced into the extraction column 2 contains nitric acid, and the concentration of nitric acid is 0.01mol/L to 14.5mol/L.
Specifically, the nitric acid concentration in this example was 7mol/L.
Specifically, the aqueous phase material in this embodiment is a solution of uranyl nitrate.
Preferably, the organic phase material introduced into the extraction column 2 contains tributyl phosphate, and the concentration of tributyl phosphate is 0.01-99.9 mas%.
More preferably, the concentration of tributyl phosphate is 1 to 95mas%.
Specifically, the tributyl phosphate concentration in this example was 50mas%.
Specifically, the organic phase material in this embodiment is a mixture of tributyl phosphate and kerosene.
Preferably, the method for determining the uranium extraction zone in the extraction column 2 further includes the following steps:
and introducing gas pulse into the extraction column 2, wherein the frequency of the gas pulse is 0.05 Hz-100 Hz.
Specifically, the frequency of the gas pulse in this embodiment is 50Hz.
Preferably, the pressure of the air source of the pulse generator 1 used for introducing the air pulse is-20 MPa-50 MPa.
Specifically, in this embodiment, the pressure of the air source of the pulse generator 1 used for introducing the air pulse is 20MPa.
Preferably, the ratio of the flow rate of the organic phase to the flow rate of the aqueous phase is 0.01 to 10.
More preferably, the ratio of the flow rate of the organic phase to the flow rate of the aqueous phase is 0.02 to 9.9.
Specifically, the ratio of the flow rate of the organic phase to the flow rate of the aqueous phase in this example was 1.
The temperature change in the axial direction of the middle section of the extraction column 2 is remarkable, and the present embodiment is directed to the above flow ratio range.
Preferably, the concentration of hexavalent uranium in the water phase feed is 0.01 g/L-1000 g/L, and the concentration of hydrogen ions is 0.01 mol/L-10 mol/L;
the concentration of hexavalent uranium in the water phase discharging is 0.00001 g/L-1000 g/L, and the concentration of hydrogen ions is 0.01 mol/L-10 mol/L.
Specifically, in the embodiment, the concentration of hexavalent uranium in the aqueous phase feed is 500g/L, and the concentration of hydrogen ions is 5mol/L;
the concentration of hexavalent uranium in the water phase discharge is 420g/L, and the concentration of hydrogen ions is 6.8mol/L.
Preferably, the flow rate of the aqueous phase introduced into the extraction column 2 is 0.1L/h to 4999L/h.
Specifically, the flow rate of the aqueous phase introduced into the extraction column 2 in this example was 2500L/h.
Preferably, the concentration of hexavalent uranium in the organic phase feed is 0.00001 g/L-1000 g/L, and the concentration of hydrogen ions is 0.01 mol/L-10 mol/L;
The concentration of hexavalent uranium in the organic phase discharge is 0.01 g/L-1000 g/L, and the concentration of hydrogen ions is 0.01 mol/L-10 mol/L.
Specifically, in the embodiment, the concentration of hexavalent uranium in the organic phase feed is 0.5g/L, and the concentration of hydrogen ions is 5mol/L;
the concentration of hexavalent uranium in the discharged organic phase is 80.5g/L, and the concentration of hydrogen ions is 3.2mol/L.
Preferably, the flow rate of the organic phase introduced into the extraction column 2 is 0.1. 0.1L/h to 4999L/h.
Specifically, the flow rate of the organic phase introduced into the extraction column 2 in this example was 2500L/h.
Preferably, the specific steps of respectively introducing the aqueous phase and the organic phase into the extraction column 2 from the two ends of the extraction column 2 are as follows:
the organic phase is introduced into the extraction column 2 from the bottom of the extraction column 2, and the aqueous phase is introduced into the extraction column 2 from the top of the extraction column 2.
As shown in fig. 1, this embodiment provides an apparatus for determining a uranium extraction zone in an extraction column 2, including:
an extraction column 2, wherein uranium-containing substances in an organic relative water phase are extracted in the extraction column 2;
the water phase supply tank 5 is connected with the first end inlet of the extraction column 2, the water phase supply tank 5 is used for introducing water phase into the extraction column 2, and uranium-containing substances are dissolved in the water phase;
the water phase receiving tank 6 is connected with the outlet of the second end of the extraction column 2, and the water phase receiving tank 6 is used for receiving the water phase flowing out of the extraction column 2;
An organic phase feed tank 7 connected with the second end inlet of the extraction column 2, wherein the organic phase feed tank 7 is used for introducing an organic phase into the extraction column 2;
an organic phase receiving tank 8 connected to the outlet of the first end of the extraction column 2, the organic phase receiving tank 8 being configured to receive the organic phase flowing out of the extraction column 2;
the temperature measuring unit 3 is arranged on the extraction column 2, and the temperature measuring unit 3 is used for measuring the temperature of each position on the extraction column 2 and sending the temperature to the control unit;
and the control unit is used for determining an exothermic standard temperature distribution area on the extraction column 2 through time accumulation of the temperature of the extraction column 2, and determining a uranium extraction area in the extraction column 2 according to the exothermic standard temperature distribution area.
Specifically, the temperature measurement unit 3 in the present embodiment is a temperature sensor.
Preferably, the device further comprises:
the first metering pump 41 is respectively connected with the first end inlet of the extraction column 2 and the water phase feed tank 5;
the second metering pump 42 is respectively connected with the second end outlet of the extraction column 2 and the water phase receiving tank 6;
a third metering pump 43 connected to the second inlet of the extraction column 2 and the organic phase feed tank 7, respectively; wherein,
the first end outlet of the extraction column 2 is connected with an organic phase receiving tank 8, the organic receiving tank is positioned below the first end outlet height of the extraction column 2, the first end of the extraction column 2 is the top end of the extraction column 2, and the second end of the extraction column 2 is the bottom end of the extraction column 2.
Preferably, the device further comprises:
the pulse generator 1 is connected with the extraction column 2, and the pulse generator 1 is used for introducing gas pulses into the extraction column 2.
The pulse generator 1 converts the pressure provided by the compressed air into periodic air pulses which provide input energy to the extraction column 2.
Preferably, the extraction column 2 is any one of a baffle plate pulse extraction column, an annular baffle plate pulse extraction column, a nozzle plate pulse extraction column, a sieve plate pulse extraction column, a rotary disc extraction column and a vibration sieve plate extraction column. The extraction column 2 is a two-phase contact reactor that can achieve liquid-liquid extraction.
Specifically, the extraction column 2 in this embodiment is a baffle pulse extraction column.
Preferably, in the device, the temperature measuring unit 3 includes at least three temperature measuring points, and the number of the temperature measuring points of the temperature measuring unit 3 is 3-1000.
Preferably, the temperature measuring unit 3 can measure the temperature ranging from minus 35 ℃ to 135 ℃, the measuring accuracy ranging from 0.0001 ℃ to 20 ℃ and can be adjusted, and the measuring altitude ranging from minus 10000m to 8848m.
Preferably, the first metering pump 41, the second metering pump 42 and the third metering pump 43 can be adjusted according to the measurement result of the temperature measuring unit 3, the flow rate adjustment range is 0L/h-5000L/h, and the flow rate adjustment precision range is 0.0001L/h-100L/h.
The aqueous phase is fed to the extraction column 2 by means of a first metering pump 41, the organic phase is fed to the extraction column 2 by means of a third metering pump 43, and the organic phase flows out of the extraction column 2 in a free-flowing manner. The water phase is added from the upper part of the extraction column 2, and flows out from the lower part of the extraction column 2 through a second metering pump 42; the organic phase is added from the lower part of the extraction column 2 and flows out from the upper part of the extraction column 2. Periodic pulses are generated by a pulse generator 1 and fed into an extraction column 2. The temperature of the middle section of the extraction column 2 is measured by a temperature measuring unit 3.
After the aqueous phase and the organic phase are mixed in the middle of the extraction column 2, the phase separation is realized in the upper and lower expansion sections of the extraction column 2. The water phase separation is realized in the lower expansion section, and the organic phase separation is realized in the upper expansion section. The temperature measuring unit 3 is respectively arranged at the upper and lower expansion sections and the middle part of the extraction column 2, and a plurality of measuring points are arranged at the middle part of the extraction column 2 along the height direction, so that the temperature change at different heights is measured. The method can be used for controlling the position of the uranium extraction zone in the extraction column 2 by adjusting the flow through a method for monitoring the temperature change.
The embodiment also provides a method for controlling the position of the uranium extraction zone in the extraction column 2, which comprises the following steps:
1) Determining a uranium extraction zone in the extraction column 2 by using the method described above;
2) Detecting the temperature of the extraction column 2 in real time, comparing the real-time temperature of the uranium extraction zone with the exothermic standard temperature distribution zone, and judging whether to adjust the flow of the water phase and/or the organic phase introduced into the extraction column 2 to adjust the real-time temperature of the uranium extraction zone to correspond to the exothermic standard temperature distribution zone.
The embodiment provides a method for controlling the position of a uranium extraction zone in an extraction column 2, which judges the position of the real-time uranium extraction zone through temperature distribution and can realize targeted real-time uranium extraction zone position adjustment.
Preferably, the step compares the real-time temperature of the uranium extraction zone with the exothermic standard temperature distribution zone, and judges whether to adjust the flow rate of the aqueous phase and/or the organic phase introduced into the extraction column 2 to adjust the real-time temperature of the uranium extraction zone to correspond to the exothermic standard temperature distribution zone, specifically:
when the real-time temperature of the uranium extraction zone corresponds to the exothermic standard temperature distribution zone, maintaining the flow of the aqueous phase and the organic phase which are introduced into the extraction column 2;
when the real-time temperature of the uranium extraction zone is changed relative to the exothermic standard temperature distribution zone, the flow of the water phase or the organic phase which is introduced into the extraction column 2 is adjusted to adjust the real-time temperature of the uranium extraction zone, and the real-time temperature corresponds to the exothermic standard temperature distribution zone.
Preferably, when the real-time temperature of the uranium extraction zone is changed relative to the exothermic standard temperature distribution zone, the flow rate of the aqueous phase or the organic phase introduced into the extraction column 2 is adjusted to adjust the real-time temperature of the uranium extraction zone, and the exothermic standard temperature distribution zone corresponds to the steps of:
when the real-time temperature of the uranium extraction zone is changed relative to the exothermic standard temperature distribution zone, the real-time temperature distribution zone corresponding to the exothermic standard temperature distribution zone is detected on the extraction column 2, and the flow of the water phase or the organic phase which is introduced into the extraction column 2 is adjusted according to the position of the real-time temperature distribution zone to adjust the real-time temperature of the uranium extraction zone, so as to correspond to the exothermic standard temperature distribution zone.
Preferably, the step adjusts the flow rate of the aqueous phase or the organic phase introduced into the extraction column 2 to adjust the real-time temperature of the uranium extraction zone according to the position of the real-time temperature distribution zone, and the real-time temperature of the uranium extraction zone corresponds to the exothermic standard temperature distribution zone, specifically:
when the real-time temperature distribution area deviates to the organic phase inlet of the extraction column 2 relative to the uranium extraction area, the flow rate of the organic phase introduced into the extraction column 2 is increased or the flow rate of the water phase introduced into the extraction column 2 is reduced, and the real-time temperature of the uranium extraction area is adjusted to correspond to the exothermic standard temperature distribution area.
Preferably, the step adjusts the flow rate of the aqueous phase or the organic phase introduced into the extraction column 2 to adjust the real-time temperature of the uranium extraction zone according to the position of the real-time temperature distribution zone, and the real-time temperature of the uranium extraction zone corresponds to the exothermic standard temperature distribution zone, specifically:
when the real-time temperature distribution area deviates to the water phase inlet of the extraction column 2 relative to the uranium extraction area, the water phase flow rate introduced into the extraction column 2 is increased or the organic phase flow rate introduced into the extraction column 2 is reduced, and the real-time temperature of the uranium extraction area is adjusted to correspond to the exothermic standard temperature distribution area.
As shown in fig. 3, in particular, the method for controlling the position of the uranium extraction zone in the extraction column 2 according to this embodiment includes the following steps:
s201, respectively introducing water phase and organic phase into the extraction column 2 from two ends of the extraction column 2, wherein uranium-containing substances are dissolved in the water phase;
s202, extracting uranium in an organic relative water phase in an extraction column 2 through uranium-containing substances, wherein the extraction of uranium is an exothermic reaction;
s203, determining an exothermic standard temperature distribution area on the extraction column 2 through time accumulation of the temperature of the extraction column 2;
s204, determining a uranium extraction zone in the extraction column 2 according to the exothermic standard temperature distribution zone;
s205, detecting the temperature of the extraction column 2 in real time;
S206, comparing the real-time temperature of the uranium extraction zone with an exothermic standard temperature distribution zone;
s207, judging whether the real-time temperature of the uranium extraction zone corresponds to the exothermic standard temperature distribution zone;
s208, when the real-time temperature of the uranium extraction zone corresponds to the exothermic standard temperature distribution zone, maintaining the flow of the water phase and the organic phase which are introduced into the extraction column 2;
s209, when the real-time temperature of the uranium extraction zone is changed relative to the exothermic standard temperature distribution zone, detecting a real-time temperature distribution zone corresponding to the exothermic standard temperature distribution zone on the extraction column 2;
s210, comparing the position of the real-time temperature distribution area with the position of the heat release standard temperature distribution area;
s211, judging whether the real-time temperature distribution area deviates to an organic phase inlet of the extraction column 2 relative to the uranium extraction area;
s212, when the real-time temperature distribution area deviates to the organic phase inlet of the extraction column 2 relative to the uranium extraction area, increasing the flow of the organic phase introduced into the extraction column 2 or reducing the flow of the water phase introduced into the extraction column 2, and adjusting the real-time temperature of the uranium extraction area to correspond to the exothermic standard temperature distribution area;
and S213, when the real-time temperature distribution area deviates to the water phase inlet of the extraction column 2 relative to the uranium extraction area, increasing the water phase flow rate introduced into the extraction column 2 or reducing the organic phase flow rate introduced into the extraction column 2, and adjusting the real-time temperature of the uranium extraction area to correspond to the exothermic standard temperature distribution area.
The embodiment provides a method, a device and a method for determining a uranium extraction zone in an extraction column 2, wherein the method is used for controlling the position of the uranium extraction zone, a plurality of temperature measurement points of a temperature measurement unit 3 are used as means for measuring temperature changes at different heights to obtain temperature distribution, then the position of the uranium extraction zone is judged, and two-phase flow is adjusted according to the calculated position of the uranium extraction zone. The embodiment also provides a method for controlling the position of the uranium extraction zone in the extraction column 2, namely an operation process, and has the characteristics of good controllability and easy operation.
The present embodiment provides a method of controlling the position of the uranium extraction zone in an extraction column 2 in which extraction columns 2 for the extraction process are fully extracted in a region where the top of the extraction column 2 is narrow, since the uranium extraction process proceeds very quickly and the extraction column 2 is of sufficient height. In this embodiment, this region is referred to as the "uranium extraction region". Since the extraction of uranium is an exothermic reaction, a heat source is present in the uranium extraction zone and a corresponding accumulation of the temperature profile through time is established. The same changes in temperature distribution will occur if the uranium extraction zone moves to the lower portion of the column 2. When some disturbance occurs, such as a decrease in the organic phase flow, a decrease in tributyl phosphate concentration in the organic phase, an increase in the aqueous phase flow, and an increase in the uranium concentration in the aqueous phase, the uranium concentration in the organic phase at the top of the extraction column 2 exceeds the saturation value and the real-time uranium extraction zone moves toward the bottom of the column. It is therefore important to ascertain the location of the real-time uranium extraction zone.
The method, the device and the method for controlling the position of the uranium extraction zone in the extraction column 2 provided by the embodiment have the following outstanding advantages:
(1) The temperatures at different positions of the extraction column 2 can be measured; (2) Long service life and radiation resistance, so that the fluorescent dye can be used under the radioactive condition; (3) Judging the uranium extraction zone according to the temperature measurement result, and adjusting the position of the actual uranium extraction zone by adjusting the flow of an organic phase or a water phase after comparing the position of the actual uranium extraction zone with the position of the designed uranium extraction zone; (4) The device is easy to overhaul, has no moving parts and adopts a modularized device.
Example 3
The difference between the method for determining the uranium extraction zone in the extraction column according to the embodiment 2 is that:
the aqueous phase material introduced into the extraction column contained nitric acid, the nitric acid concentration being 14.5mol/L.
The organic phase material introduced into the extraction column contained tributyl phosphate at a concentration of 99.9mas%.
And introducing gas pulse into the extraction column, wherein the frequency of the gas pulse is 1.0Hz.
The pressure of the gas source of the pulse generator used for introducing the gas pulse is 0.1MPa.
The ratio of the flow rate of the organic phase to the flow rate of the aqueous phase was 0.65.
The concentration of hexavalent uranium in the water phase feed is 150g/L, and the concentration of hydrogen ions is 3.0mol/L;
the concentration of hexavalent uranium in the water phase discharge is 0.5g/L, and the concentration of hydrogen ions is 2.5mol/L.
The flow rate of the aqueous phase to the extraction column was 4999L/h.
The concentration of hexavalent uranium in the organic phase feed is 0.5g/L, and the concentration of hydrogen ions is 0.1mol/L;
the concentration of hexavalent uranium in the discharged organic phase is 105g/L, and the concentration of hydrogen ions is 0.17mol/L.
The flow rate of the organic phase to the extraction column was 3200L/h.
The present embodiment provides an apparatus for determining a uranium extraction zone in an extraction column, which is different from the apparatus in embodiment 2 in that:
the extraction column in this embodiment is an annular baffle pulse extraction column.
The embodiment provides a method for controlling the position of a uranium extraction zone in an extraction column, which comprises the following steps:
1) Determining a uranium extraction zone in the extraction column by using the method;
2) Detecting the temperature of the extraction column in real time, comparing the real-time temperature of the uranium extraction zone with the exothermic standard temperature distribution zone, and judging whether to adjust the flow of the water phase and/or the organic phase introduced into the extraction column to adjust the exothermic standard temperature distribution zone corresponding to the real-time temperature of the uranium extraction zone.
The embodiment provides a method for controlling the position of a uranium extraction zone in an extraction column, which uses a plurality of temperature measurement points of a temperature measurement unit as a means for measuring temperature changes at different heights to obtain temperature distribution, then judges the position of the uranium extraction zone, and adjusts two-phase flow according to the calculated position of the uranium extraction zone. The operation process has the characteristics of good controllability and easy operation.
Example 4
The difference between the method for determining the uranium extraction zone in the extraction column according to the embodiment 2 is that:
the aqueous phase material introduced into the extraction column contained nitric acid, the nitric acid concentration being 0.01mol/L.
The organic phase material introduced into the extraction column contained tributyl phosphate at a concentration of 0.01mas%.
And introducing gas pulse into the extraction column, wherein the frequency of the gas pulse is 2Hz.
The pressure of the gas source of the pulse generator used for introducing the gas pulse is 0.2MPa.
The ratio of the organic phase flow to the aqueous phase flow was 0.616.
The concentration of hexavalent uranium in the water phase feed is 200g/L, and the concentration of hydrogen ions is 3.5mol/L;
the concentration of hexavalent uranium in the water phase discharge is 50.5g/L, and the concentration of hydrogen ions is 2.4mol/L.
The flow rate of the aqueous phase to the extraction column was 500L/h.
The concentration of hexavalent uranium in the organic phase feed is 0.01g/L, and the concentration of hydrogen ions is 0.01mol/L;
the concentration of hexavalent uranium in the discharged organic phase is 242g/L, and the concentration of hydrogen ions is 1.78mol/L.
The flow rate of the organic phase to the extraction column was 308L/h.
The present embodiment provides an apparatus for determining a uranium extraction zone in an extraction column, which is different from the apparatus in embodiment 2 in that:
The extraction column in this embodiment is a nozzle plate pulse extraction column.
The embodiment provides a method for controlling the position of a uranium extraction zone in an extraction column, which comprises the following steps:
1) Determining a uranium extraction zone in the extraction column by using the method;
2) Detecting the temperature of the extraction column in real time, comparing the real-time temperature of the uranium extraction zone with the exothermic standard temperature distribution zone, and judging whether to adjust the flow of the water phase and/or the organic phase introduced into the extraction column to adjust the exothermic standard temperature distribution zone corresponding to the real-time temperature of the uranium extraction zone.
The embodiment provides a method for controlling the position of a uranium extraction zone in an extraction column, which uses a plurality of temperature measurement points of a temperature measurement unit as a means for measuring temperature changes at different heights to obtain temperature distribution, then judges the position of the uranium extraction zone, and adjusts two-phase flow according to the calculated position of the uranium extraction zone. The operation process has the characteristics of good controllability and easy operation.
Example 5
The difference between the method for determining the uranium extraction zone in the extraction column according to the embodiment 2 is that:
firstly, a pulse generator is started, the air source pressure is 0.05Mpa, and the generated pulse frequency is 0.5Hz. And then, by starting a metering pump, the countercurrent contact of the aqueous phase and the organic phase in the extraction column is realized, at the moment, the feeding and discharging flow of the aqueous phase is 100L/h, the feeding and discharging flow of the organic phase is 250L/h, and the flow ratio obtained through flow calculation is 2.5. At this time, the temperature distribution in the middle section of the extraction column can be obtained by the temperature sensor, and when the number of temperature measuring points is 10, the measurement results are (from bottom to top) 25 ℃,25 ℃,25 ℃,25 ℃,35 ℃,45 ℃,55 ℃ and 60 ℃. When the real-time temperature distribution area deviates to the organic phase inlet of the extraction column relative to the uranium extraction area, the flow of the organic phase introduced into the extraction column is increased to 300L/h. Of course, it is also possible to reduce the flow of aqueous phase to the extraction column.
The present embodiment provides an apparatus for determining the uranium extraction zone in an extraction column, which differs from the apparatus of embodiment 2 in that:
the extraction column in this embodiment is a sieve plate pulse extraction column.
The embodiment provides a method for controlling the position of a uranium extraction zone in an extraction column, which uses a plurality of temperature measurement points of a temperature measurement unit as a means for measuring temperature changes at different heights to obtain temperature distribution, then judges the position of the uranium extraction zone, and adjusts two-phase flow according to the calculated position of the uranium extraction zone. The operation process has the characteristics of good controllability and easy operation.
Example 6
The difference between the method for determining the uranium extraction zone in the extraction column according to this embodiment and the method for determining the uranium extraction zone in the extraction column according to embodiment 5 is that:
in this example, the procedure is similar to example 5, except that the gas source pressure of the pulse generator is 0.03MPa and the pulse frequency is 0.3Hz. The water phase feeding and discharging flow is 120L/h, and the organic phase feeding and discharging flow is 300L/h. The number of temperature measurement points is 15. And when the flow ratio obtained through flow calculation is 2.75 and the real-time temperature distribution area deviates to the water phase inlet of the extraction column relative to the uranium extraction area, reducing the flow of the organic phase into the extraction column to 270L/h. Of course, it is also possible to increase the flow of aqueous phase to the extraction column.
The present embodiment provides an apparatus for determining the uranium extraction zone in an extraction column, which differs from the apparatus of embodiment 2 in that:
the extraction column in this embodiment is a rotating disk extraction column.
The embodiment provides a method for controlling the position of a uranium extraction zone in an extraction column, which uses a plurality of temperature measurement points of a temperature measurement unit as a means for measuring temperature changes at different heights to obtain temperature distribution, then judges the position of the uranium extraction zone, and adjusts two-phase flow according to the calculated position of the uranium extraction zone. The operation process has the characteristics of good controllability and easy operation.
Example 7
The difference between the method for determining the uranium extraction zone in the extraction column according to this embodiment and the method for determining the uranium extraction zone in the extraction column according to embodiment 5 is that:
in this example, the procedure is similar to example 5, except that the gas source pressure of the pulse generator is 0.07MPa and the pulse frequency is 0.7Hz. The water phase feeding and discharging flow is 80L/h, and the organic phase feeding and discharging flow is 200L/h. The number of temperature measurement points is 8. And when the flow ratio obtained through flow calculation is 2.75 and the real-time temperature distribution area deviates to the water phase inlet of the extraction column relative to the uranium extraction area, reducing the flow of the organic phase into the extraction column to 180L/h. Of course, it is also possible to increase the flow of aqueous phase to the extraction column.
The present embodiment provides an apparatus for determining the uranium extraction zone in an extraction column, which differs from the apparatus of embodiment 2 in that:
the extraction column in this embodiment is a vibrating screen plate extraction column.
The embodiment provides a method for controlling the position of a uranium extraction zone in an extraction column, which uses a plurality of temperature measurement points of a temperature measurement unit as a means for measuring temperature changes at different heights to obtain temperature distribution, then judges the position of the uranium extraction zone, and adjusts two-phase flow according to the calculated position of the uranium extraction zone. The operation process has the characteristics of good controllability and easy operation.
Example 8
The embodiment provides a method for determining a uranium extraction zone in an extraction column, which differs from the method for determining a uranium extraction zone in an extraction column in embodiment 2 in that:
in this example, the flow rate of the aqueous phase introduced into the extraction column was 0.01L/h.
In this example, the flow rate of the organic phase fed to the extraction column was 0.01L/h.
The embodiment provides a method for controlling the position of a uranium extraction zone in an extraction column, which uses a plurality of temperature measurement points of a temperature measurement unit as a means for measuring temperature changes at different heights to obtain temperature distribution, then judges the position of the uranium extraction zone, and adjusts two-phase flow according to the calculated position of the uranium extraction zone. The operation process has the characteristics of good controllability and easy operation.
Example 9
The difference between the method for determining the uranium extraction zone in the extraction column according to the embodiment 2 is that:
the flow rate of the aqueous phase passing into the extraction column in this example was 4999L/h.
The flow rate of the organic phase fed to the extraction column in this example was 4999L/h.
The embodiment provides a method for controlling the position of a uranium extraction zone in an extraction column, which uses a plurality of temperature measurement points of a temperature measurement unit as a means for measuring temperature changes at different heights to obtain temperature distribution, then judges the position of the uranium extraction zone, and adjusts two-phase flow according to the calculated position of the uranium extraction zone. The operation process has the characteristics of good controllability and easy operation.
Example 10
The difference between the method for determining the uranium extraction zone in the extraction column according to the embodiment 2 is that:
in this example, the ratio of the flow rate of the organic phase to the flow rate of the aqueous phase was 10:1.
In this example, the flow rate of the aqueous phase introduced into the extraction column was 250L/h.
In this example, the flow rate of the organic phase fed to the extraction column was 2500L/h.
In the embodiment, the concentration of hexavalent uranium in the aqueous phase feed is 0.01g/L, and the concentration of hydrogen ions is 0.1mol/L.
In this example, the concentration of hexavalent uranium in the organic phase feed was 1000g/L and the concentration of hydrogen ions was 0.2mol/L.
The concentration of hexavalent uranium in the water phase discharge is 0.00001g/L, and the concentration of hydrogen ions is 0.05mol/L.
In this example, the concentration of hexavalent uranium in the organic phase feed was 1000g/L and the concentration of hydrogen ions was 0.205mol/L.
The embodiment provides a method for controlling the position of a uranium extraction zone in an extraction column, which uses a plurality of temperature measurement points of a temperature measurement unit as a means for measuring temperature changes at different heights to obtain temperature distribution, then judges the position of the uranium extraction zone, and adjusts two-phase flow according to the calculated position of the uranium extraction zone. The operation process has the characteristics of good controllability and easy operation.
Example 11
The difference between the method for determining the uranium extraction zone in the extraction column according to the embodiment 2 is that:
in this example, the ratio of the flow rate of the organic phase to the flow rate of the aqueous phase was 1:10.
In this example, the flow rate of the aqueous phase introduced into the extraction column was 10L/h.
In this example, the flow rate of the organic phase introduced into the extraction column was 1L/h.
In the embodiment, the concentration of hexavalent uranium in the aqueous phase feed is 1000g/L, and the concentration of hydrogen ions is 10mol/L.
In this example, the concentration of hexavalent uranium in the organic phase feed was 0.001g/L and the concentration of hydrogen ions was 5mol/L.
The concentration of hexavalent uranium in the water phase discharge is 800g/L, and the concentration of hydrogen ions is 5mol/L.
In the embodiment, the concentration of hexavalent uranium in the organic phase feed is 1000g/L, and the concentration of hydrogen ions is 55mol/L.
The embodiment provides a method for controlling the position of a uranium extraction zone in an extraction column, which uses a plurality of temperature measurement points of a temperature measurement unit as a means for measuring temperature changes at different heights to obtain temperature distribution, then judges the position of the uranium extraction zone, and adjusts two-phase flow according to the calculated position of the uranium extraction zone. The operation process has the characteristics of good controllability and easy operation.
Example 12
The difference between the method for determining the uranium extraction zone in the extraction column according to the embodiment 2 is that:
in this example, the ratio of the flow rate of the organic phase to the flow rate of the aqueous phase was 5:1.
In this example, the flow rate of the aqueous phase introduced into the extraction column was 500L/h.
In this example, the flow rate of the organic phase fed to the extraction column was 2500L/h.
In the embodiment, the concentration of hexavalent uranium in the aqueous phase feed is 350g/L, and the concentration of hydrogen ions is 10.5mol/L.
In the embodiment, the concentration of hexavalent uranium in the organic phase feed is 700g/L, and the concentration of hydrogen ions is 9mol/L.
The concentration of hexavalent uranium in the water phase discharge is 600g/L, and the concentration of hydrogen ions is 8mol/L.
In this example, the hexavalent uranium concentration in the organic phase feed was 650g/L and the hydrogen ion concentration was 9.5mol/L.
The embodiment provides a method for controlling the position of a uranium extraction zone in an extraction column, which uses a plurality of temperature measurement points of a temperature measurement unit as a means for measuring temperature changes at different heights to obtain temperature distribution, then judges the position of the uranium extraction zone, and adjusts two-phase flow according to the calculated position of the uranium extraction zone. The operation process has the characteristics of good controllability and easy operation.
It is to be understood that the above embodiments are merely illustrative of the application of the principles of the present invention, but not in limitation thereof. Various modifications and improvements may be made by those skilled in the art without departing from the spirit and substance of the invention, and are also considered to be within the scope of the invention.

Claims (21)

1. A method of determining a uranium extraction zone in an extraction column, comprising the steps of:
Respectively introducing water phase and organic phase into the extraction column from two ends of the extraction column, wherein uranium-containing substances are dissolved in the water phase, extracting uranium in the extraction column through organic phase to uranium-containing substances in the water phase, determining an exothermic standard temperature distribution area on the extraction column through time accumulation of the temperature of the extraction column, and determining a uranium extraction area in the extraction column according to the exothermic standard temperature distribution area.
2. The method for determining a uranium extraction zone in an extraction column according to claim 1, wherein the aqueous phase material introduced into the extraction column contains nitric acid at a concentration of 0.01mol/L to 14.50mol/L.
3. The method for determining a uranium extraction zone in an extraction column according to claim 1, wherein the organic phase material introduced into the extraction column contains tributyl phosphate at a concentration of 0.01 to 99.9mas%.
4. The method of determining the uranium extraction zone in an extraction column of claim 1, further comprising the steps of:
and introducing gas pulses into the extraction column, wherein the frequency of the gas pulses is 0.05 Hz-100 Hz.
5. The method for determining a uranium extraction zone in an extraction column according to claim 4, wherein a pressure of a gas source of a pulse generator used for introducing the gas pulse is-20 mpa to 50mpa.
6. The method for determining a uranium extraction zone in an extraction column according to claim 1, wherein a ratio of an organic phase flow rate to an aqueous phase flow rate is 0.01 to 10.
7. The method for determining a uranium extraction zone in an extraction column according to any one of claims 1 to 6, wherein hexavalent uranium concentration in the aqueous phase feed is 0.01g/L to 1000g/L and hydrogen ion concentration is 0.01mol/L to 10mol/L;
the concentration of hexavalent uranium in the water phase discharging is 0.00001 g/L-1000 g/L, and the concentration of hydrogen ions is 0.01 mol/L-10 mol/L.
8. The method for determining a uranium extraction zone in an extraction column according to any one of claims 1 to 6, wherein a flow rate of aqueous phase introduced into the extraction column is 0.1L/h to 4999L/h.
9. The method for determining a uranium extraction zone in an extraction column according to any one of claims 1 to 6, wherein hexavalent uranium concentration in the organic phase feed is 0.00001g/L to 1000g/L and hydrogen ion concentration is 0.01mol/L to 10mol/L;
the concentration of hexavalent uranium in the organic phase discharge is 0.01 g/L-1000 g/L, and the concentration of hydrogen ions is 0.01 mol/L-10 mol/L.
10. The method for determining a uranium extraction zone in an extraction column according to any one of claims 1 to 6, wherein the flow rate of the organic phase introduced into the extraction column is 0.1L/h to 4999L/h.
11. The method for determining uranium extraction regions in an extraction column according to any one of claims 1 to 6, wherein the specific steps of respectively introducing the aqueous phase and the organic phase into the extraction column from both ends of the extraction column are as follows:
the organic phase is introduced into the extraction column from the bottom of the extraction column, and the aqueous phase is introduced into the extraction column from the top of the extraction column.
12. An apparatus for use in a method of determining the uranium extraction zone of an extraction column according to any one of claims 1 to 11, comprising:
an extraction column in which uranium-containing substances in an organic relative aqueous phase are extracted;
the water phase feeding groove is connected with a first end inlet of the extraction column and is used for introducing water phase into the extraction column, and uranium-containing substances are dissolved in the water phase;
the water phase receiving groove is connected with the outlet of the second end of the extraction column and is used for receiving water phase flowing out of the extraction column;
an organic phase feed tank connected with the second end inlet of the extraction column, wherein the organic phase feed tank is used for introducing an organic phase into the extraction column;
an organic phase receiving tank connected with the outlet of the first end of the extraction column, the organic phase receiving tank being used for receiving the organic phase flowing out of the extraction column;
The temperature measuring unit is arranged on the extraction column, and is used for measuring the temperature of each position on the extraction column and sending the temperature to the control unit;
and the control unit is used for determining an exothermic standard temperature distribution area on the extraction column through time accumulation of the temperature of the extraction column, and determining a uranium extraction area in the extraction column according to the exothermic standard temperature distribution area.
13. The apparatus as recited in claim 12, further comprising:
the first metering pump is respectively connected with the first end inlet of the extraction column and the water phase feed tank;
the second metering pump is respectively connected with the second end outlet of the extraction column and the water phase receiving groove;
the third metering pump is respectively connected with the second end inlet of the extraction column and the organic phase feed tank; wherein,
the first end outlet of the extraction column is connected with the organic receiving groove, the organic receiving groove is positioned below the height of the first end outlet of the extraction column, the first end of the extraction column is the top end of the extraction column, and the second end of the extraction column is the bottom end of the extraction column.
14. The apparatus as recited in claim 12, further comprising:
the pulse generator is connected with the extraction column and is used for introducing gas pulses into the extraction column.
15. The apparatus of any one of claims 12 to 14, wherein the extraction column is any one of a baffle pulse extraction column, an annular baffle pulse extraction column, a nozzle plate pulse extraction column, a sieve plate pulse extraction column, a turntable extraction column, and a vibrating sieve plate extraction column.
16. The device according to any one of claims 12 to 14, wherein the temperature measuring unit comprises at least three temperature measuring points, and the number of the temperature measuring points of the temperature measuring unit is 3 to 1000.
17. A method of controlling the position of a uranium extraction zone in an extraction column, comprising the steps of:
1) Determining a uranium extraction zone in an extraction column using the method of any one of claims 1 to 11;
2) Detecting the temperature of the extraction column in real time, comparing the real-time temperature of the uranium extraction zone with the exothermic standard temperature distribution zone, and judging whether to adjust the flow of the water phase and/or the organic phase introduced into the extraction column to adjust the exothermic standard temperature distribution zone corresponding to the real-time temperature of the uranium extraction zone.
18. The method according to claim 17, wherein the step of comparing the real-time temperature of the uranium extraction zone with the exothermic standard temperature distribution zone and determining whether to adjust the flow rate of the aqueous phase and/or the organic phase introduced into the extraction column to adjust the real-time temperature of the uranium extraction zone to correspond to the exothermic standard temperature distribution zone comprises:
When the real-time temperature of the uranium extraction zone corresponds to the exothermic standard temperature distribution zone, maintaining the flow of the water phase and the organic phase which are introduced into the extraction column;
when the real-time temperature of the uranium extraction zone is changed relative to the exothermic standard temperature distribution zone, the flow of the water phase or the organic phase which is introduced into the extraction column is adjusted to adjust the real-time temperature of the uranium extraction zone, and the real-time temperature corresponds to the exothermic standard temperature distribution zone.
19. The method according to claim 18, wherein the step of adjusting the flow rate of the aqueous phase or the organic phase introduced into the extraction column to adjust the real-time temperature of the uranium extraction zone when the real-time temperature of the uranium extraction zone changes with respect to the exothermic standard temperature distribution zone corresponds to the exothermic standard temperature distribution zone, specifically:
when the real-time temperature of the uranium extraction zone is changed relative to the exothermic standard temperature distribution zone, detecting the real-time temperature distribution zone corresponding to the exothermic standard temperature distribution zone on the extraction column, and adjusting the flow of the water phase or the organic phase introduced into the extraction column according to the position of the real-time temperature distribution zone to adjust the real-time temperature of the uranium extraction zone, wherein the real-time temperature corresponds to the exothermic standard temperature distribution zone.
20. The method according to claim 19, wherein the step of adjusting the flow rate of the aqueous phase or the organic phase introduced into the extraction column to adjust the real-time temperature of the uranium extraction zone according to the position of the real-time temperature distribution zone corresponds to the exothermic standard temperature distribution zone, specifically:
When the real-time temperature distribution area deviates to the organic phase inlet of the extraction column relative to the uranium extraction area, the flow rate of the organic phase introduced into the extraction column is increased or the flow rate of the water phase introduced into the extraction column is reduced, and the real-time temperature of the uranium extraction area is adjusted to correspond to the exothermic standard temperature distribution area.
21. The method according to claim 19, wherein the step of adjusting the flow rate of the aqueous phase or the organic phase introduced into the extraction column to adjust the real-time temperature of the uranium extraction zone according to the position of the real-time temperature distribution zone corresponds to the exothermic standard temperature distribution zone, specifically:
when the real-time temperature distribution area deviates to the water phase inlet of the extraction column relative to the uranium extraction area, increasing the water phase flow rate introduced into the extraction column or reducing the organic phase flow rate introduced into the extraction column, and adjusting the real-time temperature of the uranium extraction area to correspond to the exothermic standard temperature distribution area.
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