CN110559858A - Extraction system for separating lithium isotopes and lithium isotope separation method - Google Patents
Extraction system for separating lithium isotopes and lithium isotope separation method Download PDFInfo
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- CN110559858A CN110559858A CN201910856339.4A CN201910856339A CN110559858A CN 110559858 A CN110559858 A CN 110559858A CN 201910856339 A CN201910856339 A CN 201910856339A CN 110559858 A CN110559858 A CN 110559858A
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Abstract
The invention provides an extraction system for separating lithium isotopes and a lithium isotope separation method, wherein the extraction system comprises a lithium isotope separating agent and a solvent; wherein the lithium isotope separating agent comprises a compound shown as a formula A, and the lithium isotope separating agent is easily dissolved in a solvent as an extracting agent and can be selectively reacted with the solvent6Li ions form a chelate, and the high-efficiency separation of lithium isotopes can be realized through liquid-liquid extraction or solid-liquid extraction, so that the lithium isotopes can be effectively enriched6Li ions, and a high separation coefficient (alpha).
Description
Technical Field
The invention relates to the technical field of lithium isotope separation, in particular to an extraction system for separating lithium isotopes and a lithium isotope separation method.
background
Nowadays, lithium is widely used as one of important raw materials for lithium batteries. The element lithium is naturally present6Li and7two stable isotopes of Li.7Li is present in nature in a proportion of about 93% and can be used as the primary cooling material for a nuclear fusion reactor. On the other hand, the isotope abundance ratio is about 7%6li can be converted into tritium by neutron irradiation, so that tritium energy in the fusion reactor can be continuously proliferated, thereby6Li is an important raw material in nuclear fusion reactions. That is, isotopes of elemental lithium6li and7Li plays an important role in the field of atomic force applications, respectively. Therefore, the development of isotopes6li and7The method of separation of Li is very important.
Based on the lithium isotope effect, methods for separating lithium isotopes generally include physical methods and chemical methods.
Physical methods include electromagnetic methods, molten salt electrolysis methods, electron transfer molecular distillation, laser separation, and the like, and chemical methods include lithium amalgam exchange methods, solvent extraction, particle exchange chromatography, extraction, fractional crystallization, fractional precipitation, and the like.
The lithium amalgam exchange method realizes the separation of lithium isotope by utilizing isotope exchange between lithium atoms in amalgam and lithium ions in solution, is a method which is industrially applied at present, and is separated by the method6The Li separation coefficient is about 1.05, but the lithium amalgam exchange method separates lithium isotopes to generate a large amount of mercury, which causes harm to human bodies and the environment.
Methods for separating lithium isotopes without using mercury or high energy include ion exchange methods and solution extraction methods. The separation of lithium isotopes has been successfully achieved by displacement chromatography using ion exchange resins or zeolites, but the separation efficiency is low and the separation coefficient is small. The existing crown ether extraction method mainly utilizes the isotope of crown ether as a neutral chelating extractant in the extraction process6li and7The difference of the chelating properties of Li realizes a chemical exchange method of isotope exchange and enrichment in an exchange link, but the separation coefficients of lithium isotopes in the existing crown ether extraction system are small, and multi-stage cascade enrichment and amplification production are difficult to realize.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an extraction system for separating lithium isotopes and a lithium isotope separation method.
In order to achieve the above object, a first aspect of the present invention provides an extraction system for separating lithium isotopes, comprising a lithium isotope separating agent and a solvent; the lithium isotope separating agent comprises a compound shown as a formula A;
Wherein n is 1 to 11.
As a further improvement of the technical scheme, in the extraction system, the molar concentration of the lithium isotope separating agent in the solvent is 0.001-1 mol/L; the solvent comprises one or more of dichloroethane, chloroform, benzene, toluene and water-insoluble alcohols.
In a second aspect, the present invention provides a method for separating lithium isotopes, comprising the steps of:
And (3) extraction: for liquid or solid phases containing lithium ions by means of an extraction system as described above6Extracting Li to obtain a solution containing6an extract of Li ions.
As a further improvement of the above technical solution, the method further comprises:
And (3) recovering: by using the recovery liquid to contain6The extraction liquid of the Li ions is recycled,6Li ions enter the recovery liquid to obtain the solution containing6And recovering the Li ions.
As a further improvement of the above technical scheme, a separation device is adopted to realize the separation of lithium isotopes;
The separation device comprises a first container and a second container arranged in the first container, and an opening communicated with the interior of the first container is formed in the second container.
As a further improvement of the above technical solution, a stirrer is provided in the first container.
As a further improvement of the above technical solution, the lithium ions exist in a liquid phase to form a lithium ion solution, and the extracting and recovering step includes: adding the extraction system into a first container, adding the extraction system into a second container through an opening on the second container, completely immersing the opening in the extraction system, adding a lithium ion solution into the first container, adding a recovery solution into the second container,6li ions enter the recovery liquid to obtain the solution containing6recovering liquid of Li ions;
The lithium ion solution and the recovery solution are respectively immiscible with the extraction system, and the density of the extraction system is respectively greater than that of the lithium ion solution and that of the recovery solution.
As a further improvement of the above technical means, when the lithium ions exist in a solid phase to form a lithium ion solid, the lithium ion solid is prepared byThe extraction and recovery steps include: placing the extraction system, the recovery liquid and the lithium ion solid in a separation device,6Li ions enter the recovery liquid to obtain the solution containing6Recovering liquid of Li ions;
The extraction system is immiscible with the recovery liquid, and the density of the extraction system is greater than that of the recovery liquid.
As a further improvement of the above technical solution, the lithium ions exist in a liquid phase to form a lithium ion solution, the extraction system is immersed in the porous membrane, and when in use, the extraction system and the lithium ion solution are respectively located on two sides of the porous membrane.
As a further improvement of the technical scheme, the recovery liquid comprises deionized water.
The invention has the beneficial effects that:
The invention provides an extraction system for separating lithium isotopes and a lithium isotope separation method, wherein the extraction system comprises a lithium isotope separating agent and a solvent; the lithium isotope separating agent comprises a compound shown as a formula A, is easy to dissolve in a solvent as an extracting agent, and can be selectively combined with the solvent6Li ions form a chelate, and the high-efficiency separation of lithium isotopes can be realized through liquid-liquid extraction or solid-liquid extraction, so that the lithium isotopes can be effectively enriched6Li ions, and a high separation coefficient (alpha).
Drawings
To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, and it should be understood that the following drawings only illustrate some embodiments of the present invention, and therefore should not be considered as limiting the scope of the present invention.
Fig. 1 is a schematic structural diagram of a separation device of the present invention.
description of the main element symbols:
100. A first container;
200. A second container;
300. a stirrer.
Detailed Description
The terms as used herein:
"prepared from … …" is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
the conjunction "consisting of … …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of … …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when the range "1 ~ 5" is disclosed, the ranges described should be construed to include the ranges "1 ~ 4", "1 ~ 3", "1 ~ 2 and 4 ~ 5", "1 ~ 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
In these examples, the parts and percentages are by mass unless otherwise indicated.
"part by mass" means a basic unit of measure indicating a mass ratio of a plurality of components, and 1 part may represent any unit mass, for example, 1g or 2.689 g. If we say that the part by mass of the component A is a part by mass and the part by mass of the component B is B part by mass, the ratio of the part by mass of the component A to the part by mass of the component B is a: b. alternatively, the mass of the A component is aK and the mass of the B component is bK (K is an arbitrary number, and represents a multiple factor). It is unmistakable that, unlike the parts by mass, the sum of the parts by mass of all the components is not limited to 100 parts.
"and/or" is used to indicate that one or both of the illustrated conditions may occur, e.g., a and/or B includes (a and B) and (a or B).
the invention provides an extraction system for separating lithium isotopes, which comprises a lithium isotope separating agent and a solvent; the lithium isotope separating agent comprises a compound shown as a formula A;
wherein n is 1 to 11.
The lithium isotope separating agent is easily soluble in a solvent as an extractant, and can selectively react with the solvent6Li ions form a chelate, and the high-efficiency separation of lithium isotopes can be realized through liquid-liquid extraction or solid-liquid extraction, so that the lithium isotopes can be effectively enriched6Li ions, and a high separation coefficient (alpha).
compared with the existing industrialized lithium amalgam exchange method, the extraction system of the embodiment avoids using mercury, and has the characteristics of environmental protection, convenient operation and low cost.
Specifically, the compound represented by the formula a is a disclosed compound, and a production method thereof is described in literature (j.chem.soc., Perkin trans.i., 1990,1649).
It is understood that the separation coefficient (α) represents the degree of separation of two substances in a certain unit separation operation or a certain separation process, and in this embodiment, refers to the quotient of the abundance ratio of lithium isotopes in the B phase and the abundance ratio of lithium isotopes in the a phase, and the size of the quotient reflects the difficulty of separation of the two components. The separation coefficient (α) is represented by the following equation:
Optionally, the solvent is an organic solvent.
Specifically, the organic solvent comprises one or more of dichloroethane, chloroform, benzene, toluene and water-insoluble alcohol.
Specifically, the water-insoluble alcohol includes monohydric alcohol having more than 4 carbon atoms, and preferably, the water-insoluble alcohol is octanol.
Optionally, in the extraction system, the molar concentration of the lithium isotope separating agent in the solvent is 0.001-1 mol/L, for example, 0.001mol/L, 0.0031mol/L, 0.01mol/L, 0.05mol/L, 0.1mol/L, 0.5mol/L, 1.0mol/L, and the like.
The invention also provides a lithium isotope separation method, which comprises the following steps:
and (3) extraction: for liquid or solid phases containing lithium ions by means of an extraction system as described above6Extracting Li to obtain a solution containing6An extract of Li ions. In the equation of the separation coefficient (. alpha.) at this time, ([ alpha ])6Li]/[7Li])(B)Showing the abundance ratio of lithium ion isotope in the extract liquid after completion of extraction, (([ 2 ]6Li]/[7Li])(A)the ratio of the isotopic abundance in the liquid phase or solid phase containing lithium ions before extraction is shown.
It will be understood that for the presence of the solid or liquid phase6the Li ions can be sufficiently extracted by the lithium isotope separating agent of the extraction system, and the above extraction operation can be repeated a plurality of times.
specifically, the liquid phase may be at least one of water, an aqueous solution, a mixed solution of water and an organic solvent, and a mixed solution of an aqueous solution and an organic solvent, and the organic solvent may be a polar solvent such as ethanol.
Optionally, the lithium isotope separation method further includes:
And (3) recovering: by using the recovery liquid to contain6The extraction liquid of the Li ions is recycled,6li ions enter the recovery liquid to obtain the solution containing6and recovering the Li ions. In the equation of the separation coefficient (. alpha.) at this time, ([ alpha ])6Li]/[7Li])(B)Showing lithium in the recovered solution after recoveryion isotope abundance ratio, ([ 2 ]6Li]/[7Li])(A)The ratio of the isotopic abundance in the liquid phase or solid phase containing lithium ions before extraction is shown.
Optionally, the recycling liquid includes deionized water.
It will be appreciated that the use of deionized water as the recovery liquid in the recovery stage enables the extraction of the extract6the Li ions are separated from the extraction liquid,6Li ions enter a recovery liquid to be separated from an extraction liquid6products of Li ions. The lithium isotope separating agent can be recovered and recycled.
In particular, in order to make the extraction in6The Li ions can be sufficiently recovered by the recovering solution, and the above recovering operation can be repeated many times.
Optionally, the separation device is used for separating lithium isotopes in the lithium isotope separation method;
Referring to fig. 1, the separation apparatus includes a first container 100 and a second container 200 disposed in the first container 100, wherein the second container 200 is provided with an opening communicated with the interior of the first container 100.
Optionally, the lithium ions are present in a liquid phase to form a lithium ion solution, and the extracting and recovering step includes: adding the extraction system into the first container 100, adding the extraction system into the second container 200 through the opening on the second container 200, completely immersing the opening in the extraction system, adding the lithium ion solution into the first container 100, adding the recovery solution into the second container 200,6Li ions enter the recovery liquid to obtain the solution containing6Recovering liquid of Li ions;
The lithium ion solution and the recovery solution are respectively immiscible with the extraction system, and the density of the extraction system is respectively greater than that of the lithium ion solution and that of the recovery solution.
The specific operation is as follows: when lithium ions are present in the liquid phase to form a lithium ion solution, an extraction system is added to the first container 100, added to the extraction system, and passed through an opening in the bottom of the second container 200 into the second container 200, and the opening is completedafter the lithium ion solution is completely immersed in the extraction system, the lithium ion solution is added into the first container 100, the recovery solution is added into the second container 200, at the moment, the extraction system is directly contacted and not dissolved with the recovery solution, and the extraction system is directly contacted and not dissolved with the lithium ion solution. The separating agent being selective for lithium isotope and being in solution with lithium ions6Li ions form a chelate, thereby leading to6Separating Li ions from the lithium ion solution to obtain a solution containing Li ions6Extraction of Li ions, followed by6Li ions enter the recovery liquid to obtain the solution containing6And (3) a product of a Li ion recovery solution.
Optionally, the molar concentration of the lithium ion solution is 0.5-2 mol/L, and may be, for example, 0.5mol/L, 0.8mol/L, 1.0mol/L, 1.5mol/L, 2mol/L, and the like.
Optionally, the volume ratio of the extraction system to the lithium ion solution is (1-5): 1, for example, can be 1:1, 2:1, 3: 1; 4: 1; 5:1, etc.
Optionally, when the lithium ions exist in the solid phase to form a lithium ion solid, the extracting and recovering step includes: placing the extraction system, the recovery liquid and the lithium ion solid in a separation device,6Li ions enter the recovery liquid to obtain the solution containing6Recovering liquid of Li ions;
The extraction system is immiscible with the recovery liquid, and the density of the extraction system is greater than that of the recovery liquid.
The specific operation is as follows: when lithium ions exist in a solid phase to form a lithium ion solid matter, adding an extraction system into a separation device, adding the lithium ion solid matter and a recovery liquid into the extraction system, wherein the extraction system is directly contacted with and not dissolved in the recovery liquid, and a lithium isotope separating agent is selectively mixed with lithium ion solid matter6Li ions form a chelate, thereby leading to6Li ions are separated from the lithium ion solid to obtain a lithium ion battery6Extraction of Li ions, followed by6Li ions enter the recovery liquid to obtain the solution containing6And (3) a product of a Li ion recovery solution.
Optionally, the lithium ion solid includes, but is not limited to, lithium halide solid, such as lithium iodide, lithium chloride, lithium bromide, and the like.
the separation device has simple structure, and when the separation device is used for separating the lithium isotope by an extraction system, the extraction and the recovery processes can be carried out simultaneously, so that the separation device can be used for separating the lithium isotope by the extraction system6Li ions are enriched in the recovery liquid, the separation coefficient (alpha) is high, and the operation is simple and convenient.
Optionally, a stirrer 300 is disposed in the first container 100. The stirrer 300 is provided to allow the lithium isotope separating agent to react with the lithium ion-containing liquid phase or solid phase6The Li ions are extracted sufficiently.
optionally, the opening is disposed at the bottom of the second container 200.
Optionally, the first container 100 and the second container 200 are both glass containers.
Alternatively, the cross-sectional shapes of the first container 100 and the second container 200 may be circular, square, irregular, etc.
Optionally, the lithium ions exist in a liquid phase to form a lithium ion solution, the extraction system is immersed in the porous membrane, and when the porous membrane is used, the extraction system and the lithium ion solution are respectively located on two sides of the porous membrane.
specifically, the porous film may be a polyolefin porous film, for example, a polyethylene porous film, a polypropylene porous film, or the like; in other embodiments, the porous membrane may be a nonwoven fabric or a porous membrane made of a nonwoven fabric material.
embodiments of the present invention will be described in detail below with reference to specific examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
A separation apparatus is prepared, which includes a first container 100 and a second container 200 provided in the first container 100, and the bottom of the second container 200 is provided with an opening for communicating with the inside of the first container 100.
Dissolving a lithium isotope separating agent (the lithium isotope separating agent is a compound represented by formula A, and n is 3) in dichloromethane at room temperature of 25 ℃ to form an extraction system for separating lithium isotopes, wherein the concentration of the lithium isotope separating agent in dichloromethane is 3.1X 10-3Adding 30ml of extraction system into the first container 100, wherein the extraction system enters the second container 200 through the opening at the bottom of the second container 200, completely immersing the opening in the extraction system, adding 15ml of 1.0mol/l lithium chloride aqueous solution into the first container 100, adding 15ml of deionized water (namely recovery solution) into the second container 200, and standing for 48 hours to obtain the lithium ion battery6recovering liquid of Li ions, using isotope mass spectrometer6Li and7The isotopic abundance ratio of Li was measured.
using isotope mass spectrometer for aqueous lithium chloride solution before extraction6Li and7The isotopic abundance ratio of Li was measured. The calculation was performed according to the formula for the separation coefficient (α) described above, in which the a phase was an aqueous solution of lithium chloride and the B phase was a recovered solution, and the separation coefficient (α) of lithium isotope was 1.043.
example 2
A separation apparatus is prepared, which includes a first container 100 and a second container 200 provided in the first container 100, and the bottom of the second container 200 is provided with an opening for communicating with the inside of the first container 100.
Dissolving a lithium isotope separating agent (the lithium isotope separating agent is a compound represented by formula A, and n is 8) in dichloromethane at room temperature of 25 ℃ to form an extraction system for separating lithium isotopes, wherein the concentration of the lithium isotope separating agent in dichloromethane is 3.1X 10-3Adding 30ml of extraction system into the first container 100, wherein the extraction system enters the second container 200 through the bottom opening of the second container 200, completely submerging the opening in the extraction system, adding 15ml of 1.0mol/l lithium chloride aqueous solution into the first container 100, and adding 15ml of deionized water (namely recovery solution) into the second container 200After standing for 48 hours, the product is obtained6recovering liquid of Li ions, using isotope mass spectrometer6Li and7The isotopic abundance ratio of Li was measured.
Using isotope mass spectrometer for aqueous lithium chloride solution before extraction6li and7the isotopic abundance ratio of Li was measured. The calculation was performed according to the formula of the separation coefficient (α) described above, in which the phase a was an aqueous solution of lithium chloride and the phase B was a recovered solution, to obtain a separation coefficient (α) of lithium isotope of 1.057.
Example 3
A separation apparatus is prepared, which includes a first container 100 and a second container 200 provided in the first container 100, and the bottom of the second container 200 is provided with an opening for communicating with the inside of the first container 100.
dissolving a lithium isotope separating agent (the lithium isotope separating agent is a compound represented by formula A, and n is 1) in dichloromethane at room temperature of 25 ℃ to form an extraction system for separating lithium isotopes, wherein the concentration of the lithium isotope separating agent in dichloromethane is 3.1 × 10-3Adding 30ml of extraction system into the first container 100, wherein the extraction system enters the second container 200 through the opening at the bottom of the second container 200, completely immersing the opening in the extraction system, adding 15ml of 1.0mol/l lithium chloride aqueous solution into the first container 100, adding 15ml of deionized water (namely recovery solution) into the second container 200, and standing for 48 hours to obtain the lithium ion battery6Recovering liquid of Li ions, using isotope mass spectrometer6Li and7The isotopic abundance ratio of Li was measured.
Using isotope mass spectrometer for aqueous lithium chloride solution before extraction6Li and7The isotopic abundance ratio of Li was measured. The calculation was carried out according to the formula for the separation coefficient (α) as described above, wherein phase a was an aqueous solution of lithium chloride and phase B was a recovered solution, and the separation coefficient (α) of lithium isotope was 1.035.
Example 4
A separation apparatus is prepared, which includes a first container 100 and a second container 200 provided in the first container 100, and the bottom of the second container 200 is provided with an opening for communicating with the inside of the first container 100.
Dissolving a lithium isotope separating agent (the lithium isotope separating agent is a compound represented by formula A, and n is 11) in dichloromethane at room temperature of 25 ℃ to form an extraction system for separating lithium isotopes, wherein the concentration of the lithium isotope separating agent in dichloromethane is 3.1X 10-3Adding 30ml of extraction system into the first container 100, wherein the extraction system enters the second container 200 through the opening at the bottom of the second container 200, completely immersing the opening in the extraction system, adding 15ml of 1.0mol/l lithium chloride aqueous solution into the first container 100, adding 15ml of deionized water (namely recovery solution) into the second container 200, and standing for 48 hours to obtain the lithium ion battery6Recovering liquid of Li ions, using isotope mass spectrometer6li and7The isotopic abundance ratio of Li was measured.
Using isotope mass spectrometer for aqueous lithium chloride solution before extraction6Li and7the isotopic abundance ratio of Li was measured. The separation coefficient (α) was calculated according to the above-mentioned formula for the separation coefficient (α), wherein the phase a was an aqueous solution of lithium chloride and the phase B was a recovered solution, and the separation coefficient (α) of lithium isotope was 1.054.
Example 5
A separation apparatus is prepared, which includes a first container 100 and a second container 200 provided in the first container 100, and the bottom of the second container 200 is provided with an opening for communicating with the inside of the first container 100.
Dissolving a lithium isotope separating agent (the lithium isotope separating agent is a compound shown as a formula A, and n is 11) in dichloromethane at room temperature of 25 ℃ to form an extraction system for separating lithium isotopes, wherein the concentration of the lithium isotope separating agent in dichloromethane is 1.0mol/l, adding 30ml of the extraction system into a first container 100, enabling the extraction system to enter a second container 200 through an opening at the bottom of the second container 200, completely immersing the opening in the extraction system, and taking 2mol/l of the extraction systemAdding 15ml of lithium chloride aqueous solution into the first container 100, adding 15ml of deionized water (i.e. recovering solution) into the second container 200, standing for 48 hr to obtain a solution containing6Recovering Li ions by isotope mass spectrometer6Li and7The isotopic abundance ratio of Li was measured.
Using isotope mass spectrometer for aqueous lithium chloride solution before extraction6Li and7The isotopic abundance ratio of Li was measured. The calculation was performed according to the formula of the separation coefficient (α) described above, in which the a phase was an aqueous solution of lithium chloride and the B phase was a recovered solution, and the separation coefficient (α) of lithium isotope was 1.048.
Example 6
A separation apparatus is prepared, which includes a first container 100 and a second container 200 provided in the first container 100, and the bottom of the second container 200 is provided with an opening for communicating with the inside of the first container 100.
dissolving a lithium isotope separating agent (the lithium isotope separating agent is a compound shown as a formula A, and n is 11) in dichloromethane at room temperature of 25 ℃ to form an extraction system for separating lithium isotopes, wherein the concentration of the lithium isotope separating agent in dichloromethane is 0.1mol/l, adding 30ml of the extraction system into a first container 100, enabling the extraction system to enter a second container 200 through an opening at the bottom of the second container 200, completely immersing the opening in the extraction system, adding 15ml of 1.5mol/l lithium chloride aqueous solution into the first container 100, adding 15ml of deionized water (namely a recovery solution) into the second container 200, standing for 48 hours to obtain a solution containing 1.5mol/l lithium isotopes6Recovering liquid of Li ions, using isotope mass spectrometer6Li and7The isotopic abundance ratio of Li was measured.
using isotope mass spectrometer for aqueous lithium chloride solution before extraction6Li and7the isotopic abundance ratio of Li was measured. The separation coefficient (α) was calculated according to the formula described above, wherein the phase a was an aqueous solution of lithium chloride and the phase B was a recovered solution, and the separation coefficient of lithium isotope was 1.051.
Example 7
A separation apparatus is prepared, which includes a first container 100 and a second container 200 provided in the first container 100, and the bottom of the second container 200 is provided with an opening for communicating with the inside of the first container 100.
Dissolving a lithium isotope separating agent (the lithium isotope separating agent is a compound represented by formula A, and n is 3) in dichloromethane at room temperature of 25 ℃ to form an extraction system for separating lithium isotopes, wherein the concentration of the lithium isotope separating agent in dichloromethane is 3.1X 10-3Adding 30ml of extraction system into a first container 100, respectively adding 0.6g of lithium chloride solid and 30ml of deionized water (namely recovery solution) into the extraction system, and standing for 48 hours to obtain a solution containing6Recovering liquid of Li ions, using isotope mass spectrometer6Li and7The isotopic abundance ratio of Li was measured.
using isotope mass spectrometer for lithium chloride solid before extraction6Li and7The isotopic abundance ratio of Li was measured. The separation coefficient (α) of lithium isotope was 1.013 by calculation in accordance with the above-mentioned formula of separation coefficient (α), wherein phase a was a lithium chloride solid and phase B was a recovered solution.
Example 8
A separation apparatus is prepared, which includes a first container 100 and a second container 200 provided in the first container 100, and the bottom of the second container 200 is provided with an opening for communicating with the inside of the first container 100.
Dissolving a lithium isotope separating agent (the lithium isotope separating agent is a compound shown as a formula A, and n is 11) in dichloromethane at the room temperature of 25 ℃ to form an extraction system for separating lithium isotopes, wherein the concentration of the lithium isotope separating agent in the dichloromethane is 0.1mol/l, adding 30ml of the extraction system into a first container 100, respectively adding 1.5g of lithium chloride solid and 30ml of deionized water (namely a recovery solution) into the extraction system, and standing for 48 hours to obtain a solution containing the lithium isotopes6Recovering liquid of Li ions, using isotope mass spectrometer6Li and7Isotopic abundance ratio of Lithe values are measured.
Using isotope mass spectrometer for lithium chloride solid before extraction6li and7The isotopic abundance ratio of Li was measured. The calculation was performed according to the formula of the separation coefficient (α) described above, in which the a phase was a lithium chloride solid and the B phase was a recovered solution, to obtain a separation coefficient (α) of lithium isotope of 1.028.
finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features included in other embodiments, rather than other features, combinations of features of different embodiments are meant to be within the scope of the invention and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Claims (10)
1. An extraction system for separating lithium isotopes is characterized by comprising a lithium isotope separating agent and a solvent; the lithium isotope separating agent comprises a compound shown as a formula A;
Wherein n is 1 to 11.
2. The extraction system for separating lithium isotopes as claimed in claim 1, wherein the molar concentration of the lithium isotope separating agent in the solvent in the extraction system is 0.001-1 mol/L; the solvent comprises one or more of dichloroethane, chloroform, benzene, toluene and water-insoluble alcohols.
3. A method for separating lithium isotopes is characterized by comprising the following steps:
and (3) extraction: use of an extraction system according to any of claims 1 to 2 for the treatment of lithium ion-containing liquid or solid phases6Extracting Li to obtain a solution containing6an extract of Li ions.
4. The lithium isotope separation method according to claim 3, further comprising:
and (3) recovering: by using the recovery liquid to contain6the extraction liquid of the Li ions is recycled,6li ions enter the recovery liquid to obtain the solution containing6And recovering the Li ions.
5. The lithium isotope separation method according to claim 4, wherein separation of the lithium isotopes is performed using a separation apparatus;
the separation device comprises a first container and a second container arranged in the first container, and an opening communicated with the interior of the first container is formed in the second container.
6. The method for separating lithium isotopes as claimed in claim 5, wherein a stirrer is provided in said first container.
7. The method for separating lithium isotopes of claim 5 wherein the lithium ions are present in a liquid phase to form a lithium ion solution, and wherein the extracting and recovering step comprises: adding the extraction system to a first container, adding the extraction system to a second container through an opening in the second container, and completely submerging the opening in the second containerAfter the extraction system is finished, adding the lithium ion solution into a first container, adding the recovery liquid into a second container,6Li ions enter the recovery liquid to obtain the solution containing6Recovering liquid of Li ions;
The lithium ion solution and the recovery solution are respectively immiscible with the extraction system, and the density of the extraction system is respectively greater than that of the lithium ion solution and that of the recovery solution.
8. The method for separating lithium isotopes as claimed in claim 5, wherein the step of extracting and recovering the lithium ions in the solid phase to form a solid lithium ion comprises: placing the extraction system, the recovery liquid and the lithium ion solid in a separation device,6Li ions enter the recovery liquid to obtain the solution containing6recovering liquid of Li ions;
the extraction system is immiscible with the recovery liquid, and the density of the extraction system is greater than that of the recovery liquid.
9. The method for separating lithium isotopes as claimed in claim 3, wherein the lithium ions are present in a liquid phase to form a lithium ion solution, the extraction system is impregnated in a porous membrane, and in use, the extraction system and the lithium ion solution are located on two sides of the porous membrane, respectively.
10. The lithium isotope separation method according to claim 4, wherein the recovery liquid includes deionized water.
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