Extraction device and extraction method for separating isotopes

Abstract

The present invention discloses an extraction device and an extraction method for separating isotopes, wherein the extraction device comprises an extraction unit, a temperature control unit and an air blowing unit, wherein the temperature control unit can provide a suitable extraction environment for the extraction unit, and the air blowing unit can blow gas into the extraction unit so that the extraction unit performs flotation complex extraction to simultaneously separate and enrich the first isotope and the second isotope, and the extraction device has a simple structure and strong operability. The extraction method adopts the extraction device provided by the present invention, and only needs to go through the flotation complex extraction and stripping steps to simultaneously separate and enrich the first isotope and the second isotope, without the need for centrifugal phase separation, and has a short extraction time and a high separation coefficient.

Description

Technical Field

[0001] The invention relates to the technical field of isotope separation, and in particular to an extraction device and an extraction method for separating isotopes. Background Art

[0002] Isotope separation is the study of the separation between different isotopes of the same element. The isotopes to be separated should belong to the same element with the same atomic number. The various isotopes of the same element have the same number of protons in the nucleus and the same number of electrons outside the nucleus, so their chemical properties are very similar and it is very difficult to separate them. However, they have different numbers of neutrons in the nucleus, and therefore different atomic weights, which causes differences in the thermodynamic properties of isotopes or their molecules. The purpose of separation can be achieved by using the subtle differences in the physical and chemical properties of isotopes.

[0003] Extraction is a common isotope separation method. In the prior art, if the extraction method is used for isotope separation, only one isotope ion can be separated. In order to enrich the isotope ion, multi-stage cascade extraction is required. The extraction process time is long and the separation coefficient is low. Summary of the invention

[0004] In view of the shortcomings of the prior art, the present invention provides an isotope separation extraction device and an extraction method. The extraction device has a simple structure and strong operability. The extraction method can simultaneously separate and enrich the first isotope and the second isotope without centrifugal separation, and the extraction time is short and the separation coefficient is high.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] The present invention first provides an extraction device for separating isotopes, the extraction device comprising:

[0007] An extraction unit, comprising a first extraction column, a second extraction column, and a connecting extraction part for connecting the first extraction column and the second extraction column to each other;

[0008] A temperature control unit is sleeved on the outside of the extraction unit and has a gap with the outer wall of the extraction unit to form a fluid channel, wherein the fluid channel is used to contain a temperature control liquid and allow the temperature control liquid to circulate to control the temperature of the extraction unit;

[0009] The gas blowing unit is connected to the lower ends of the first extraction column and the second extraction column, and is used to blow gas into the first extraction column and the second extraction column to perform gas flotation complex extraction.

[0010] Preferably, the first extraction column and the second extraction column are respectively connected to the connected extraction part from the upper surface of the connected extraction part; the air blowing unit includes a first air blowing component and a second air blowing component, the first air blowing component is connected to the connected extraction part from the lower surface of the connected extraction part and is opposite to the lower end of the first extraction column, and the second air blowing component is connected to the connected extraction part from the lower surface of the connected extraction part and is opposite to the lower end of the second extraction column.

[0011] More preferably, the upper ends of the first extraction column and the second extraction column are respectively formed to be open, and the connected extraction column is provided with a liquid separation port, and the liquid separation port is equipped with a sealing plug.

[0012] More preferably, the extraction unit further comprises a first reduced diameter tube; one end of the connected extraction column is closed, the other end of the connected extraction column is connected to the end with a larger diameter of the first reduced diameter tube, and the end with a smaller diameter of the first reduced diameter tube forms the liquid separation port.

[0013] Preferably, the temperature control unit comprises a first temperature control column, a second temperature control column and a connecting temperature control portion;

[0014] The communicating temperature control part is sleeved on the outer side of the communicating extraction part, and the communicating temperature control part is provided with a first through hole for the first extraction column to pass through and a second through hole for the second extraction column to pass through;

[0015] The first temperature control column is sleeved on the outside of the first extraction column, the lower end of the first temperature control column is connected to the edge of the first through hole and is connected to the connected temperature control part through the first through hole, and the upper end of the first temperature control column is sealed and connected to the outer wall of the first extraction column through a first end surface connecting plate;

[0016] The second temperature-control column is sleeved on the outside of the second extraction column, the lower end of the second temperature-control column is connected to the edge of the second through hole and is connected to the connecting temperature-control part through the second through hole; the upper end of the second temperature-control column is sealed and connected to the outer wall of the second extraction column through a second end face connecting plate.

[0017] More preferably, the temperature control unit is provided with a temperature control liquid injection port and a temperature control liquid discharge port, the temperature control liquid injection port is provided on the connecting temperature control portion, and the temperature control liquid discharge port is provided on the first temperature control column.

[0018] More preferably, the temperature control unit further comprises a second reduced diameter tube and a third reduced diameter tube;

[0019] One end of the communicating temperature control part is closed, and the other end of the communicating temperature control part is connected to the end of the second reduced diameter tube with a larger diameter, and the end of the second reduced diameter tube with a smaller diameter is formed as the temperature control liquid injection port;

[0020] The side wall of the first extraction column is communicated with an end of the third reduced diameter tube with a larger diameter, and an end of the third reduced diameter tube with a smaller diameter forms the temperature control liquid discharge port.

[0021] Preferably, the first air blowing assembly and the second air blowing assembly respectively comprise an air blowing conduit, a piston sleeve, a tapered tube and an air distributor plate which are connected in sequence;

[0022] The first end of the conical tube with a larger diameter is connected to the connecting extraction part, the gas distributor is connected to the first end of the conical tube, and the second end of the conical tube with a smaller diameter passes through the surface of the connecting temperature control part; a piston is assembled in the piston sleeve, and a vent hole that can connect the second end of the conical tube with the air inflation duct is formed in the piston sleeve and the piston.

[0023] More preferably, the extraction device further comprises a temperature control device and a gas source, a buffer tank and a flow meter connected in sequence, the flow meter and the air blowing unit are connected to each other; the temperature control device is connected to the fluid channel in the temperature control unit.

[0024] The present invention also provides an extraction method for separating isotopes, using the extraction device for separating isotopes as described above, and the extraction method comprises the following steps:

[0025] Start the gas blowing unit to blow gas into the first extraction column and the second extraction column and pass the temperature control liquid into the temperature control unit;

[0026] adding an extraction aqueous phase containing a first isotope and a second isotope from the first extraction column and / or the second extraction column to the extraction unit;

[0027] Adding an extraction organic phase for extracting a first isotope from the first extraction column to the extraction unit, adding an extraction organic phase for extracting a second isotope from the second extraction column to the extraction unit, extracting the first isotope by flotation complexation in the first extraction column, and extracting the second isotope by flotation complexation in the second extraction column;

[0028] After the flotation complex extraction is completed: the extracted organic phase in the first extraction column is separated and back-extracted, and the aqueous phase is collected to obtain a solution enriched in the first isotope; the extracted organic phase in the second extraction column is separated and back-extracted, and the aqueous phase is collected to obtain a solution enriched in the second isotope.

[0029] An extraction device and extraction method for separating isotopes provided in an embodiment of the present invention, the extraction device comprises an extraction unit, a temperature control unit and an air blowing unit, wherein the temperature control unit can provide a suitable extraction environment for the extraction unit, the air blowing unit can blow gas into the extraction unit so that the extraction unit performs flotation complex extraction to simultaneously separate and enrich the first isotope and the second isotope, the extraction device has a simple structure and strong operability. The extraction method adopts the extraction device provided by the present invention, and only needs to go through flotation complex extraction and stripping steps to simultaneously separate and enrich the first isotope and the second isotope, without the need for centrifugal phase separation, and the extraction time is short and the separation coefficient is high. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 is a schematic structural diagram of an extraction device according to an embodiment of the present invention;

[0031] Figure 2 is a schematic diagram of a vertical cross-section structure of an extraction device according to an embodiment of the present invention;

[0032] Figure 3 is a schematic diagram of the vertical axial structure of an extraction device according to an embodiment of the present invention;

[0033] Figure 4 is a schematic diagram of the top view of the extraction device according to an embodiment of the present invention;

[0034] Figure 5 It is a schematic diagram of the enlarged structure of the first reducing pipe connection part of an embodiment of the present invention;

[0035] Figure 6 is an enlarged structural schematic diagram of the second reducing tube connection portion of an embodiment of the present invention;

[0036] Figure 7 It is a schematic diagram of the structure of the extraction device used in the extraction method for separating isotopes in an embodiment of the present invention. DETAILED DESCRIPTION

[0037] In order to make the purpose, technical scheme and advantages of the present invention clearer, the specific embodiments of the present invention are described in detail below in conjunction with the accompanying drawings. Examples of these preferred embodiments are illustrated in the accompanying drawings. The embodiments of the present invention shown in the accompanying drawings and described according to the accompanying drawings are merely exemplary, and the present invention is not limited to these embodiments.

[0038] It should also be noted that, in order to avoid obscuring the present invention due to unnecessary details, only structures and / or processing steps closely related to the solutions according to the present invention are shown in the accompanying drawings, while other details that are not closely related to the present invention are omitted.

[0039] The embodiment of the present invention first provides an extraction device for separating isotopes. Figures 1 to 7 The extraction device includes an extraction unit 1, a temperature control unit 2 and an air blowing unit 3.

[0040] In a specific embodiment, the extraction unit 1 includes a first extraction column 11, a second extraction column 12, and a connecting extraction portion 13 for connecting the first extraction column 11 and the second extraction column 12 to each other.

[0041] It is worth mentioning that before the extraction unit 1 starts extraction, the extraction organic phase for extracting the first isotope is loaded in the first extraction column 11, and the extraction organic phase for extracting the second isotope is loaded in the second extraction column 12; the extraction aqueous phase containing the first isotope and the second isotope can be loaded only in the connected extraction part 13, or can be loaded in the connected extraction part 13, the lower end part of the first extraction column 11 and the lower end part of the second extraction column 12 at the same time.

[0042] Specifically, the first extraction column 11 and the second extraction column 12 are respectively connected to the connected extraction part 13 from the upper surface of the connected extraction part 13; the air blowing unit 3 includes a first air blowing component 3a and a second air blowing component 3b, the first air blowing component 3a is connected to the connected extraction part 13 from the lower surface of the connected extraction part 13 and is opposite to the lower end of the first extraction column 11, and the second air blowing component 3b is connected to the connected extraction part 13 from the lower surface of the connected extraction part 13 and is opposite to the lower end of the second extraction column 12.

[0043] More specifically, the upper ends of the first extraction column 11 and the second extraction column 12 are respectively formed to be open, and the connecting extraction column 13 is provided with a liquid separation port 14 , and the liquid separation port 14 is equipped with a sealing plug 15 .

[0044] It should be noted that the position of the liquid separation port 14 on the connected extraction part 13 is not limited, and can be set at any position of the connected extraction part 13, as long as it can be separated by smoothly discharging the liquid in the connected extraction part 13, the lower layer liquid of the first extraction column 11 and the lower layer liquid of the second extraction column 12 by pulling out the sealing plug 15 after flotation complexation extraction.

[0045] In fact, the extraction unit 1 provided in an embodiment of the present invention also includes a first reduced diameter tube 16; one end of the connected extraction column 13 is closed, and the other end of the connected extraction column 13 is connected to the end with a larger diameter of the first reduced diameter tube 16, and the end with a smaller diameter of the first reduced diameter tube 16 forms the liquid separation port 14.

[0046] In a specific solution, the temperature control unit 2 is sleeved on the outside of the extraction unit 1 and has a gap with the outer wall of the extraction unit 1 to form a fluid channel 2a, and the fluid channel 2a is used to accommodate a temperature control liquid and allow the temperature control liquid to circulate to control the temperature of the extraction unit 1.

[0047] Specifically, the temperature control unit 2 includes a first temperature control column 21, a second temperature control column 22 and a connecting temperature control portion 23; the connecting temperature control portion 23 is sleeved on the outer side of the connecting extraction portion 13, and is provided with a first through hole 24 for the first extraction column 11 to pass through and a second through hole 25 for the second extraction column 12 to pass through; the first temperature control column 21 is sleeved on the outer side of the first extraction column 11, the lower end of the first temperature control column 21 is connected to the edge of the first through hole 24 and is connected to the connecting temperature control portion 23 through the first through hole 24, and the upper end of the first temperature control column 21 is sealed and connected to the outer wall of the first extraction column 11 through a first end surface connecting plate 41; the second temperature control column 22 is sleeved on the outer side of the second extraction column 12, the lower end of the second temperature control column 22 is connected to the edge of the second through hole 25 and is connected to the connecting temperature control portion 23 through the second through hole 25; the upper end of the second temperature control column 22 is sealed and connected to the outer wall of the second extraction column 12 through a second end surface connecting plate 42.

[0048] It can be understood that the first end face connecting plate 41 is an annular structure to seal and connect the upper end of the first temperature control column 21 and the outer wall of the first extraction column 11; the second end face connecting plate 42 is an annular structure to seal and connect the upper end of the second temperature control column 22 and the outer wall of the second extraction column 12.

[0049] More specifically, the temperature control unit 2 is provided with a temperature control liquid injection port 26 and a temperature control liquid discharge port 27 . The temperature control liquid injection port 26 is provided on the connecting temperature control portion 23 , and the temperature control liquid discharge port 27 is provided on the first temperature control column 21 .

[0050] More specifically, the temperature control unit 2 also includes a second reduced diameter tube 28 and a third reduced diameter tube 29; one end of the connecting temperature control portion 23 is closed, and the other end of the connecting temperature control portion 23 is connected to the end with a larger diameter of the second reduced diameter tube 28, and the end with a smaller diameter of the second reduced diameter tube 28 is formed as the temperature control liquid injection port 26; the side wall of the first extraction column 11 is connected to the end with a larger diameter of the third reduced diameter tube 29, and the end with a smaller diameter of the third reduced diameter tube 29 is formed as the temperature control liquid discharge port 27.

[0051] In a specific solution, the gas blowing unit 3 is connected to the lower ends of the first extraction column 11 and the second extraction column 12, and is used to blow gas into the first extraction column 11 and the second extraction column 12 to perform gas flotation complex extraction.

[0052] In an embodiment of the present invention, the air blowing unit 3 includes a first air blowing component 3a and a second air blowing component 3b, and the first air blowing component 3a and the second air blowing component 3b respectively include an air blowing duct 31, a piston sleeve 32, a conical tube 33 and an air distribution plate 34 which are connected in sequence; the first end of the conical tube 33 with a larger diameter is connected to the connecting extraction part 13, the air distribution plate 34 is connected to the first end of the conical tube 33, and the second end of the conical tube 33 with a smaller diameter passes through the surface of the connecting temperature control part 23; the piston sleeve 32 is equipped with a piston 35, and the piston sleeve 32 and the piston 35 are formed with an air vent 36 which can connect the second end of the conical tube 33 with the air blowing duct 31.

[0053] Specifically, the gas separation disk 34 has a circumferential array of pores with the same diameter to disperse the gas into bubbles with the same diameter in the connected extraction part 13 for flotation complexation extraction.

[0054] For more details, see Figure 7 The extraction device further comprises a temperature control device 5 and a gas source 6, a buffer tank 7 and a flow meter 8 connected in sequence, wherein the flow meter 8 and the gas blowing unit 3 are connected to each other; the temperature control device 5 is connected to the fluid channel 2a in the temperature control unit 2. Figure 7 wherein the extraction water containing the first isotope and the second isotope is simultaneously loaded into the connecting extraction part 13, the lower end portion of the first extraction column 11 and the lower end portion of the second extraction column 12; 6 The Li extraction phase is an organic phase for extracting the first isotope, which is loaded in the first extraction column 11 and covers the top of the extraction aqueous phase containing the first isotope and the second isotope; 7 The Li extraction phase is an organic phase for extracting the second isotope, which is loaded into the second extraction column 12 and covers the top of the extraction aqueous phase containing the first isotope and the second isotope.

[0055] It should be noted that the extraction device described above performs flotation complex extraction in combination with the extraction unit 1, the temperature control unit 2 and the air blowing unit 3. The principle of the flotation complex extraction is as follows:

[0056] After the blowing unit 3 blows gas into the lower ends of the first extraction column 11 and the second extraction column 12, the blown gas is dispersed into bubbles and forms airflow in the first extraction column 11 and the second extraction column 12. At this time, the first isotope ions in the extraction water phase are adsorbed on the surface of the bubbles and move upward with the airflow of the first extraction column 11, thereby exchanging with the extraction organic phase for extracting the first isotope covering the top of the extraction water phase, thereby enriching the second isotope ions in the water phase and enriching the first isotope ions in the organic phase in the first extraction column 11; the second isotope ions in the extraction water phase are adsorbed on the surface of the bubbles and move upward with the airflow of the second extraction column 12, thereby exchanging with the extraction organic phase for extracting the second isotope covering the top of the extraction water phase, thereby enriching the first isotope ions in the water phase and enriching the second isotope ions in the organic phase in the second extraction column 12.

[0057] It can be seen that the extraction unit can separate the first isotope and the second isotope at the same time, and due to the provision of the connected extraction part 13, the first isotope and the second isotope can flow in the extraction unit 1, which promotes the enrichment of the first isotope and the second isotope, and improves the separation effect and abundance of the first isotope and the second isotope.

[0058] The extraction device for separating isotopes as described above comprises an extraction unit, a temperature control unit and an air blowing unit, wherein the temperature control unit can provide a suitable extraction environment for the extraction unit, and the air blowing unit can blow gas into the extraction unit so that the extraction unit performs air flotation complex extraction to simultaneously separate and enrich the first isotope and the second isotope. The extraction device has a simple structure and strong operability.

[0059] Based on the above principle and the above extraction device for separating isotopes, the present invention also provides an extraction method for separating isotopes, and the extraction method includes step S1, step S2, step S3 and step S4.

[0060] Specifically, the step S1 is: starting the gas blowing unit 3 to blow gas into the first extraction column 11 and the second extraction column 12 and passing the temperature control liquid into the temperature control unit 2 .

[0061] It should be noted that the gas blown into the air blowing unit 3 is nitrogen or an inert gas. When the gas blown into the air blowing unit 3 is nitrogen or an inert gas, the following beneficial effects are achieved:

[0062] ① Compared with compressed air, the nitrogen or inert gas has a single component and no impurities are introduced, which is beneficial to the accuracy and repeatability of the extraction method.

[0063] ② The nitrogen or inert gas has stable chemical properties and is not easy to react with the extraction organic phase used to extract the first isotope and the extraction organic phase used to extract the second isotope, which can increase the service life of the extraction organic phase used to extract the first isotope and the extraction organic phase used to extract the second isotope.

[0064] It is worth mentioning that during the blowing process of the blowing unit 3, in order to achieve the optimal efficiency of the flotation complex extraction of the blowing unit 3 and the extraction unit 1, the gas flow rate blown into the blowing unit 3 is 10mL / min to 30mL / min, for example, it can be 10mL / min, 12mL / min, 14mL / min, 16mL / min, 18mL / min, 20mL / min, 22mL / min, 24mL / min, 26mL / min, 28mL / min or 30mL / min.

[0065] In addition, in an embodiment of the present invention, the flotation complex extraction is efficiently carried out at -10°C to 20°C, and the temperature of the temperature-controlling liquid can be, for example, -10°C, -5°C, 0°C, 5°C, 10°C, 15°C or 20°C.

[0066] Specifically, the step S2 includes: adding an extraction aqueous phase containing the first isotope and the second isotope from the first extraction column 11 and / or the second extraction column 12 to the extraction unit 1 .

[0067] In an embodiment of the present invention, the separation 6 Li and 7 Taking Li as an example, the extraction aqueous phase includes a lithium-containing solution and an alkaline regulating solution, wherein the lithium-containing solution is selected from at least one of LiCl solution, LiBr solution, LiI solution, LiN(CF3SO2)2 solution and LiOH solution, and the alkaline regulating solution is selected from NaOH solution, KOH solution or LiOH solution.

[0068] Specifically, the step S3 is: adding an extraction organic phase for extracting a first isotope from the first extraction column 11 to the extraction unit 1, adding an extraction organic phase for extracting a second isotope from the second extraction column 12 to the extraction unit 1, extracting the first isotope by flotation complexation in the first extraction column 11, and extracting the second isotope by flotation complexation in the second extraction column 12.

[0069] In an embodiment of the present invention, the extraction organic phase for extracting the first isotope comprises 6 Li extraction agent, 6 Li co-extractant and diluent, the organic phase for extracting the second isotope comprises 7 Li extraction agent, 7 Li synergist and diluent.

[0070] Among them, the 6 The Li extractant is benzo-15-crown-5 and its derivatives. 6 The Li co-extractant is an imidazole ionic liquid whose anion is bistrifluoromethanesulfonyl imide and whose cation is an alkyl carbon chain of different lengths.

[0071] Said 7 Li extractant 10-hydroxybenzoquinoline, the 7 The Li co-extractant is an imidazole ionic liquid whose anion is hexafluorophosphate and whose cation is an alkyl carbon chain of different lengths.

[0072] The diluent is selected from at least one of anisole, kerosene, octanone, chloroform, dichloromethane, carbon tetrachloride, tetrachloroethylene, toluene, xylene, diethylbenzene, bromobenzene, anisole, nitromethane, 2-methylcyclohexanone, methyl isobutyl ketone, chlorobenzene, dichlorobenzene, trichlorobenzene and diphenyl ether.

[0073] Specifically, step S4 is: after the flotation complex extraction is completed: separating the extracted organic phase in the first extraction column 11 and performing back extraction, collecting the aqueous phase to obtain a solution enriched in the first isotope; separating the extracted organic phase in the second extraction column 12 and performing back extraction, collecting the aqueous phase to obtain a solution enriched in the second isotope.

[0074] It can be seen that after the flotation complexation extraction is completed, the extracted organic phase of the first extraction column 11 is 6 Li, water phase 7 Li; the extracted organic phase of the second extraction column 12 is 7 Li, water phase 6 Li.

[0075] In an embodiment of the present invention, the organic phase extracted from the first extraction column 11 is separated and a stripping agent is added for stripping, and the stripping is repeated for multiple times, and the aqueous phase is collected to obtain an enriched 6 Li solution, and enriched 6 The lithium isotope value and lithium isotope abundance of the solution of Li are calculated. The organic phase extracted from the second extraction column 12 is separated and a stripping agent is added for stripping. The stripping is repeated for multiple times and the aqueous phase is collected to obtain the enriched 7 Li solution, and enriched 7 Lithium isotope values ​​and lithium isotope abundances are calculated for Li solutions.

[0076] It should be noted that the lithium isotope value (δ) is obtained by normalizing the sample to be tested with the standard substance L-SVEC and converting the sample lithium isotope test results into relative thousandths of deviation δ 7 Li(‰) is expressed. When the test result δ 7When Li(‰)>0 is a positive value, it means that the test sample is relatively enriched. 7 Li; when the test result δ 7 When Li(‰)<0 is a negative value, it means that the test sample is relatively enriched. 6 Li, the larger the absolute value, the better the enrichment effect, that is, the better the separation effect of the experiment. Its calculation formula is:

[0077]

[0078] In the formula, ( 7 Li / 6 Li) L-SVEC =12.1025±0.0016, which is the standard lithium used by the test unit. 7 Li and 6 The abundance ratio of Li, δ 7 Li(‰) is the relative deviation of one thousandth, which is directly given by the test instrument. Therefore, according to the above formula, the amount of 7 Li / 6 The value of Li sample.

[0079] The calculation method of lithium isotope abundance is as follows: Since the total content of the two isotopes of lithium is 100%, 6 The abundance of Li is x, then 7 The abundance of Li is 1-x, then 7 Li / 6 Li sample = (1-x) / x; similarly, let 7 The abundance of Li is x, then 6 The abundance of Li is 1-x, then 7 Li / 6 Li sample = x / (1-x), so we can get 6 Li and 7 The specific value of Li abundance x.

[0080] In addition, the stripping agent used in the stripping of the embodiment of the present invention is selected from water, hydrochloric acid solution or aqueous solution of inorganic salt.

[0081] The extraction method for separating isotopes provided by the embodiment of the present invention only needs to go through the steps of flotation complex extraction and stripping. Since the flotation complex extraction adopts the method of mass transfer with the help of bubbles, the extraction method of the two phases is transformed from liquid-liquid mixed exchange to liquid-liquid contact exchange and gas-liquid contact exchange with a larger contact surface area, which reduces the loss of the extractant in the organic phase, and makes the isotope chemical exchange between the extracted organic phase and the aqueous phase take place on the contact surface of the two phases. After the reaction is completed, there is no need for centrifugal phase separation, which can effectively improve the ability of extracting and separating isotopes and obtain better extraction and separation effects. After stripping, the isotope separation coefficient is high.

[0082] In order to further illustrate the present invention, an isotope separation extraction device and extraction method provided by the present invention are described in detail below in combination with embodiments, but they should not be construed as limiting the scope of protection of the present invention.

[0083] Example 1

[0084] An extraction method for separating lithium isotopes, wherein the isotopes are 6 Li and 7 Li, using the extraction device provided by the embodiment of the present invention, the extraction device refers to Figure 1 to Figure 7 , the extraction method comprises the following steps:

[0085] Step S1, start the gas blowing unit 3 to blow nitrogen with a gas flow rate of 10 mL / min into the first extraction column 11 and the second extraction column 12, and pass a temperature control liquid at 0°C into the temperature control unit 2.

[0086] Step S2: adding lithium chloride and sodium hydroxide-containing alkaline solution from the first extraction column 11.

[0087] Step S3: adding the extractant for extraction from the first extraction column 11 to the extraction unit 1 6 The organic phase of Li extraction is extracted by flotation complexation in the first extraction column 11 6 Li, wherein the 6 The extractant in the organic phase of Li extraction is 4-aminobenzo-15-crown-5-ether, the co-extractant is the ionic liquid of 1-butyl-3-imidazole bis(trifluoromethanesulfonyl)imide salt ([BMIm][NTf2]), and the diluent is anisole.

[0088] The second extraction column 12 is added to the extraction unit 1 for extraction 7 The organic phase of Li extraction is extracted by flotation complexation in the second extraction column 12 7 Li, used for extraction 7 The extractant in the organic phase of Li extraction is 10-hydroxybenzoquinoline, the co-extractant is 1-hexyl-3-methylimidazolium hexafluorophosphate ([HMIm]PF6), and the diluent is anisole.

[0089] Step S4, after 60 minutes of flotation complex extraction: separate the extracted organic phase in the first extraction column 11 and add hydrochloric acid for stripping, repeat stripping three times, the stripping rate is 99%, collect the aqueous phase to obtain the enriched 6 Li solution and calculate the lithium isotope value and lithium isotope abundance to obtain δ 7 Li(‰)=-38.54, after single separation and enrichment 6The abundance of Li reaches 7.92%.

[0090] The extracted organic phase in the second extraction column 12 is separated and added with pure water for back extraction. The back extraction is repeated three times, and the back extraction rate is 98%. The aqueous phase is collected to obtain the enriched 7 Li solution and calculate the lithium isotope value and lithium isotope abundance to obtain δ 7 Li(‰)=39.86, after single separation and enrichment 7 The abundance of Li reaches 92.64%.

[0091] Example 2

[0092] An extraction method for separating lithium isotopes, wherein the isotopes are 6 Li and 7 Li, using the extraction device provided by the embodiment of the present invention, the extraction device refers to Figure 1 to Figure 7 , the extraction method comprises the following steps:

[0093] Step S1, start the gas blowing unit 3 to blow nitrogen with a gas flow rate of 20 mL / min into the first extraction column 11 and the second extraction column 12, and pass a temperature control liquid at 10°C into the temperature control unit 2.

[0094] Step S2, adding lithium hydroxide and sodium hydroxide-containing alkaline solution from the first extraction column 11.

[0095] Step S3: adding the extractant for extraction from the first extraction column 11 to the extraction unit 1 6 The organic phase of Li extraction is extracted by flotation complexation in the first extraction column 11 6 Li, wherein the 6 The extractant in the organic phase of Li extraction is 4-bromobenzo-15-crown-5-ether, the co-extractant is the ionic liquid of the ionic liquid of 1-hexyl-3-imidazole bis(trifluoromethanesulfonyl)imide salt ([HMIm][NTf2]), and the diluent is anisole.

[0096] The second extraction column 12 is added to the extraction unit 1 for extraction 7 The organic phase of Li extraction is extracted by flotation complexation in the second extraction column 12 7 Li, used for extraction 7 The extractant in the organic phase of Li extraction is 10-hydroxybenzoquinoline, the co-extractant is 1-octyl-3-methylimidazolium hexafluorophosphate ([OMIm]PF6), and the diluent is anisole.

[0097] Step S4, after 60 minutes of flotation complex extraction: separate the extracted organic phase in the first extraction column 11 and add hydrochloric acid for stripping, repeat stripping three times, the stripping rate is 99%, collect the aqueous phase to obtain the enriched 6 Li solution and calculate the lithium isotope value and lithium isotope abundance to obtain δ 7 Li(‰)=-32.96, after single separation and enrichment 6 The abundance of Li reaches 7.87%.

[0098] The extracted organic phase in the second extraction column 12 is separated and added with pure water for back extraction. The back extraction is repeated three times, and the back extraction rate is 98%. The aqueous phase is collected to obtain the enriched 7 Li solution and calculate the lithium isotope value and lithium isotope abundance to obtain δ 7 Li(‰)=42.39, after single separation and enrichment 7 The abundance of Li reaches 92.65%.

[0099] Example 3

[0100] An extraction method for separating lithium isotopes, wherein the isotopes are 6 Li and 7 Li, using the extraction device provided by the embodiment of the present invention, the extraction device refers to Figure 1 to Figure 7 , the extraction method comprises the following steps:

[0101] Step S1, start the gas blowing unit 3 to blow nitrogen with a gas flow rate of 30 mL / min into the first extraction column 11 and the second extraction column 12, and pass a temperature control liquid at 20°C into the temperature control unit 2.

[0102] Step S2, adding sodium hydroxide-containing alkaline solution containing lithium iodide from the first extraction column 11.

[0103] Step S3: adding the extractant for extraction from the first extraction column 11 to the extraction unit 1 6 The organic phase of Li extraction is extracted by flotation complexation in the first extraction column 11 6 Li, wherein the 6 The extractant in the organic phase of Li extraction is benzo-15-crown-5-ether, the co-extractant is the ionic liquid of 1-octyl-3-imidazole bis(trifluoromethanesulfonyl)imide salt ([OMIm][NTf2]), and the diluent is anisole.

[0104] The second extraction column 12 is added to the extraction unit 1 for extraction 7 The organic phase of Li extraction is extracted by flotation complexation in the second extraction column 12 7 Li, used for extraction 7The extractant in the organic phase of Li extraction is 10-hydroxybenzoquinoline, the co-extractant is 1-butyl-3-methylimidazolium hexafluorophosphate ([HMIm]PF6), and the diluent is anisole.

[0105] Step S4, after 60 minutes of flotation complex extraction: separate the extracted organic phase in the first extraction column 11 and add hydrochloric acid for stripping, repeat stripping three times, the stripping rate is 99%, collect the aqueous phase to obtain the enriched 6 Li solution and calculate the lithium isotope value and lithium isotope abundance to obtain δ 7 Li(‰)=-22.63, after single separation and enrichment 6 The abundance of Li reaches 7.80%.

[0106] The extracted organic phase in the second extraction column 12 is separated and added with pure water for back extraction. The back extraction is repeated three times, and the back extraction rate is 98%. The aqueous phase is collected to obtain the enriched 7 Li solution and calculate the lithium isotope value and lithium isotope abundance to obtain δ 7 Li(‰)=35.56, after single separation and enrichment 7 The abundance of Li reaches 92.61%.

[0107] In summary, the present invention provides an extraction device and an extraction method for separating isotopes, wherein the extraction device comprises an extraction unit, a temperature control unit and an air blowing unit, wherein the temperature control unit can provide a suitable extraction environment for the extraction unit, and the air blowing unit can blow gas into the extraction unit so that the extraction unit performs flotation complex extraction to simultaneously separate and enrich the first isotope and the second isotope, and the extraction device has a simple structure and strong operability. The extraction method adopts the extraction device provided by the present invention, and only needs to go through the flotation complex extraction and stripping steps to simultaneously separate and enrich the first isotope and the second isotope, without the need for centrifugal phase separation, and the extraction time is short and the separation coefficient is high.

[0108] The above is only a specific implementation of the present application. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present application. These improvements and modifications should also be regarded as the scope of protection of the present application.

Claims

1. An extraction device for separating isotopes, characterized in that: The extraction device comprises: An extraction unit (1) comprises a first extraction column (11), a second extraction column (12), and a connecting extraction portion (13) for connecting the first extraction column (11) and the second extraction column (12) to each other; a temperature control unit (2) which is sleeved on the outside of the extraction unit (1) and has a gap with the outer wall of the extraction unit (1) to form a fluid channel (2a); the fluid channel (2a) is used to contain a temperature control liquid and allow the temperature control liquid to circulate to control the temperature of the extraction unit (1); an air blowing unit (3), connected to the lower ends of the first extraction column (11) and the second extraction column (12), and used for blowing gas into the first extraction column (11) and the second extraction column (12) to perform air flotation complex extraction; The first extraction column (11) and the second extraction column (12) are respectively connected to the connected extraction part (13) from the upper surface of the connected extraction part (13); the air blowing unit (3) comprises a first air blowing component (3a) and a second air blowing component (3b), the first air blowing component (3a) is connected to the connected extraction part (13) from the lower surface of the connected extraction part (13) and is directly opposite to the lower end of the first extraction column (11), and the second air blowing component (3b) is connected to the connected extraction part (13) from the lower surface of the connected extraction part (13) and is directly opposite to the lower end of the second extraction column (12).

2. The extraction device for separating isotopes according to claim 1, characterized in that: The upper ends of the first extraction column (11) and the second extraction column (12) are respectively formed to be open, and the connecting extraction part (13) is provided with a liquid separation port (14), and the liquid separation port (14) is equipped with a sealing plug (15).

3. The extraction device for separating isotopes according to claim 2, characterized in that: The extraction unit (1) further comprises a first reduced diameter tube (16); one end of the connecting extraction portion (13) is closed, the other end of the connecting extraction portion (13) is connected to an end of the first reduced diameter tube (16) with a larger diameter, and an end of the first reduced diameter tube (16) with a smaller diameter forms the liquid separation port (14).

4. The extraction device for separating isotopes according to claim 1, characterized in that: The temperature control unit (2) comprises a first temperature control column (21), a second temperature control column (22) and a connecting temperature control portion (23); The communicating temperature control portion (23) is sleeved on the outer side of the communicating extraction portion (13), and the communicating temperature control portion (23) is provided with a first through hole (24) for the first extraction column (11) to pass through and a second through hole (25) for the second extraction column (12) to pass through; The first temperature control column (21) is sleeved on the outside of the first extraction column (11); the lower end of the first temperature control column (21) is connected to the edge of the first through hole (24) and is connected to the connected temperature control portion (23) through the first through hole (24); the upper end of the first temperature control column (21) is sealed and connected to the outer wall of the first extraction column (11) through a first end surface connecting plate (41); The second temperature control column (22) is sleeved on the outside of the second extraction column (12); the lower end of the second temperature control column (22) is connected to the edge of the second through hole (25) and is connected to the connected temperature control portion (23) through the second through hole (25); the upper end of the second temperature control column (22) is sealed and connected to the outer wall of the second extraction column (12) through a second end surface connecting plate (42).

5. The extraction device for separating isotopes according to claim 4, characterized in that: The temperature control unit (2) is provided with a temperature control liquid injection port (26) and a temperature control liquid discharge port (27); the temperature control liquid injection port (26) is provided on the connecting temperature control portion (23), and the temperature control liquid discharge port (27) is provided on the first temperature control column (21).

6. The extraction device for separating isotopes according to claim 5, characterized in that: The temperature control unit (2) further comprises a second reduced diameter tube (28) and a third reduced diameter tube (29); One end of the communicating temperature control portion (23) is closed, and the other end of the communicating temperature control portion (23) is communicated with the end of the second reduced diameter tube (28) with a larger diameter, and the end of the second reduced diameter tube (28) with a smaller diameter forms the temperature control liquid injection port (26); The side wall of the first extraction column (11) is connected to the end of the third reduced diameter tube (29) with a larger diameter, and the end of the third reduced diameter tube (29) with a smaller diameter forms the temperature control liquid discharge port (27).

7. The extraction device for separating isotopes according to claim 4, characterized in that: The first air blowing assembly (3a) and the second air blowing assembly (3b) respectively comprise an air blowing conduit (31), a piston sleeve (32), a tapered tube (33) and an air distribution plate (34) which are connected in sequence; The first end of the conical tube (33) with a larger diameter is connected to the connecting extraction part (13), the gas distribution plate (34) is connected to the first end of the conical tube (33), and the second end of the conical tube (33) with a smaller diameter passes through the surface of the connecting temperature control part (23); a piston (35) is installed in the piston sleeve (32), and a vent hole (36) capable of connecting the second end of the conical tube (33) and the air blowing duct (31) is formed in the piston sleeve (32) and the piston (35).

8. The extraction device for separating isotopes according to claim 7, characterized in that: The extraction device further comprises a temperature control device (5) and a gas source (6), a buffer tank (7) and a flow meter (8) which are connected in sequence, wherein the flow meter (8) and the air blowing unit (3) are connected to each other; the temperature control device (5) is connected to a fluid channel (2a) in the temperature control unit (2).

9. An extraction method for separating isotopes, characterized in that: Using the extraction device for separating isotopes as described in any one of claims 1 to 8, the extraction method comprises the following steps: Starting the gas blowing unit (3) to blow gas into the first extraction column (11) and the second extraction column (12) and passing a temperature control liquid into the temperature control unit (2); Adding an extraction aqueous phase containing a first isotope and a second isotope into the extraction unit (1) from the first extraction column (11) and / or the second extraction column (12); adding an extraction organic phase for extracting a first isotope from the first extraction column (11) to the extraction unit (1), adding an extraction organic phase for extracting a second isotope from the second extraction column (12) to the extraction unit (1), extracting the first isotope by flotation complexation in the first extraction column (11), and extracting the second isotope by flotation complexation in the second extraction column (12); After the flotation complex extraction is completed: the extracted organic phase in the first extraction column (11) is separated and back-extracted, and the aqueous phase is collected to obtain a solution enriched in the first isotope; the extracted organic phase in the second extraction column (12) is separated and back-extracted, and the aqueous phase is collected to obtain a solution enriched in the second isotope.

Images