CN114713046B - Packaged ionic liquid supported liquid film and preparation method thereof - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0023—Organic membrane manufacture by inducing porosity into non porous precursor membranes
- B01D67/003—Organic membrane manufacture by inducing porosity into non porous precursor membranes by selective elimination of components, e.g. by leaching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0093—Chemical modification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0095—Drying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
- B01D69/105—Support pretreatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/12—Specific ratios of components used
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/50—Control of the membrane preparation process
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- 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
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Abstract
The invention belongs to the technical field of membranes, and particularly relates to an encapsulated ionic liquid supported liquid membrane and a preparation method thereof. The encapsulated ionic liquid supported liquid film provided by the invention shows excellent Li in application of extracting lithium from salt lake + The recovery performance and no loss of the ionic liquid after repeated use. Meanwhile, the invention optimizes the film preparation process, especially the regulation and control of the thickness of the packaging layer, so as to ensure the stability of the film and Li + The recovery rate is adjusted to be optimal, and the method has the prospect of large-scale application of lithium extraction in salt lakes.
Description
Technical Field
The invention belongs to the technical field of membranes, and particularly relates to a preparation method of a packaged ionic liquid supported liquid membrane.
Background
With the rapid development of portable electronic devices and electric automobiles, the development and utilization of lithium resources have received high attention. The salt lake of China is rich in lithium resources, the lithium reserve ratio is up to 71%, but the lithium extraction difficulty is higher due to the high magnesium-lithium ratio (Mg/Li > 30). The existing method for treating high-Mg/Li brine mainly comprises an adsorbent adsorption method and a solvent extraction method, but the methods have the defects of high cost and low efficiency, so that the production of lithium salt in China depends on imported lithium ores for a long time. Therefore, a novel technology is developed to realize the extraction of lithium from high Mg/Li brine, and the method has important significance for the development of new energy technology in China. The ionic liquid supported liquid film is a film prepared by filling and fixing ionic liquid in a porous film under the action of interfacial tension, and is widely applied to the fields of metal ion separation, cyanide-containing wastewater treatment, gas separation, organic matter separation and the like. The electrodialysis technology adopting the ionic liquid supported liquid film has the advantages of cleanness, high efficiency, low consumption and the like, and is considered as the lithium extraction technology with the most application prospect.
The Netherlands journal of membrane science (Journal of Membrane Science, 2007, 300 (1-2): 88-94) discloses a method for preparing an ionic liquid supported liquid membrane, which comprises the steps of firstly fixing a nylon membrane and a polytetrafluoroethylene porous membrane on an ultrafiltration device respectively, and then fixing 3 different ionic liquids ([ bmim) + ] [PF 6 - ](1-butyl-3-methyl hexafluorophosphate imidazolium), [ bmim ] + ] [BF 4 - ](1-butyl-3-methyl-tetrafluoroborate imidazolium), [ bmim ] + ] [NTf 2 - ](1-butyl-3-methyl bis { (trifluoromethyl) sulfonyl } imide imidazolium)) are respectively covered on the membranes, then 2 bar nitrogen is introduced to pressurize the ionic liquid to permeate the membranes, the ionic liquid is repeated for 3 times to fill the whole membranes, and finally the membranes are vertically placed overnight to remove excessive ionic liquid on the surfaces of the membranes, so that the ionic liquid supported liquid membrane is obtained. According to the method, as the membrane pores on the surfaces of porous membranes such as nylon membranes and polytetrafluoroethylene membranes are large (micron level), ionic liquid with small particle size (Emi level) cannot be effectively trapped, and when salt lake water is treated, the ionic liquid is rapidly lost due to direct contact with an aqueous solution, so that the stability of the membrane is poor and the membrane cannot be reused.
The Chinese patent with application number 202110890077.0 discloses a preparation method of an ionic liquid supported liquid film, which comprises the steps of firstly forming a two-dimensional film layer on a substrate by adopting a negative pressure suction filtration method through Graphene (GO) nanosheets, and then filling the ionic liquid into a two-dimensional nano channel of the GO film by adopting a vacuum auxiliary steam traction method to obtain the ionic liquid supported liquid film. It must be noted that the ionic liquid supported liquid membrane prepared by the method also faces the problems of performance degradation and incapability of recycling caused by the loss of ionic liquid in the membrane. Based on the above, it is important to develop a membrane preparation method for stabilizing the ionic liquid supported liquid membrane.
The Netherlands journal of Desalination (Desamination, 2013, 317:11-16) discloses a method for producing a liquid film supporting an encapsulated ionic liquid, which comprises the steps of first preparing [ PP13]][TFSI](1-methyl-1-propylpiperidinebis (tris)Fluoromethylsulfonyl) imide salt) ionic liquid was filled into Gore-Tex with a thickness of 1mm TM And in the porous membrane, two Nafion 324 membranes are respectively covered on two sides of the membrane filled with the ionic liquid, so that the encapsulated ionic liquid supported liquid membrane is obtained. The method well solves the problem of ionic liquid loss, but no physical or chemical acting force exists between the Nafion membrane and the porous membrane filled with ionic liquid, the lamination between the Nafion membrane and the porous membrane filled with ionic liquid is required to be assembled in the electrodialysis brine lithium extraction device, the lamination is carried out only by virtue of the pressure generated during assembly of the assembly, and when the electrodialysis brine lithium extraction device is used for dismantling the assembly, the Nafion membrane and the porous membrane cannot be laminated due to the disappearance of the pressure, so that the ionic liquid is lost. Therefore, the membrane cannot be stored and transported by adopting the method, can only exist in the electrodialysis brine lithium extraction device, needs to be stored and transported synchronously along with the electrodialysis brine lithium extraction device, and needs to be filled in an existing state, and obviously cannot meet the large-scale use requirement of the salt lake lithium extraction.
In summary, the use of the conventional ionic liquid supported liquid membrane has the problem of serious loss of ionic liquid in the membrane. Although the problem of ionic liquid loss is solved to a certain extent in the prior art, no physical or chemical acting force exists between the packaging layer and the porous base membrane, and the packaging layer and the porous base membrane are attached only by pressure, so that the supported liquid membrane cannot exist independently and stably, the self-support of the membrane cannot be realized, and the ionic liquid cannot be effectively stored and transported due to the fact that the ionic liquid is required to be attached to an electrodialysis brine lithium extraction device. Therefore, it is very important to develop a method for encapsulating ionic liquid supported liquid films with stable encapsulation layers.
Disclosure of Invention
In view of the above, the present invention aims to provide an encapsulated ionic liquid supported liquid film with a stable encapsulation layer and a preparation method thereof, wherein the porous base film is encapsulated in situ, so as to realize self-support of the film, and solve the above problems.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention claims and protects a preparation method of an encapsulated ionic liquid supported liquid film, which comprises the steps of coating Nafion solution on the upper surface of a porous base film, controlling the thickness of the coating film, forming an encapsulation layer through heat treatment and drying, then coating glue on the side surface of the porous base film, naturally drying, soaking the porous base film in ionic liquid, wiping off superfluous ionic liquid on the surface of the film by using oil absorption wiping paper after adsorption saturation, coating the Nafion solution on the lower surface of the porous base film, controlling the thickness of the coating film, and forming the encapsulation layer through heat treatment and drying, thus finally obtaining the encapsulated ionic liquid supported liquid film.
The concentration of the Nafion solution is 3-10g/L, the solvent is water or an organic solvent capable of dissolving Nafion, preferably methanol, n-propanol and isopropanol can be selected, and the solvents can be used singly or after being mixed;
the porous base membrane is a PTFE porous membrane and a PVDF porous membrane;
the glue is glue capable of forming a compact structure after being solidified, and is used for preventing ionic liquid from leaking from the side face of the porous base film, and preferably AB glue or phenolic resin can be selected;
the ionic liquid is an ionic liquid with excellent selective adsorptivity to lithium ions, and preferably [ PP13] [ TFSI ] (1-methyl-1-propylpiperidinebis (trifluoromethylsulfonyl) imide salt) can be selected, and has the following structure:
the coating method is spin coating, spraying and knife coating.
The film thickness of the Nafion solution on the upper and lower surfaces of the porous base film is 1-5 micrometers.
The temperature of the heating treatment is 30-70 ℃ and the time is 20-60 minutes.
The thickness of Nafion encapsulation layers on the upper surface and the lower surface of the porous base film is 0.2-1 micron, and the concentration of Nafion solution and the thickness of a coating film are controlled.
The invention also claims the encapsulated ionic liquid supported liquid film prepared by the method, which is correspondingly composed of a porous base film, ionic liquid filled in the pores of the porous base film, nafion encapsulation layers on the upper and lower surfaces of the porous base film and a glue layer encapsulating the side surfaces of the porous base film.
The invention has the remarkable advantages that:
the problem of performance reduction caused by serious leakage of the ionic liquid exists in the existing non-packaging ionic liquid support liquid film, although the leakage of the ionic liquid is effectively reduced in the existing packaging ionic liquid support liquid film, the packaging layer is a solidified film, no physical or chemical action exists between the packaging layer and the porous base film, the packaging layer is attached only by the pressure during assembly of the component, and once the pressure disappears, the packaging layer is automatically separated from the porous base film, so that the ionic liquid is leaked, and the performance is reduced. In contrast, the invention adopts Nafion solution to coat film on the porous base film, and the film is cured to form the packaging layer after heat treatment, and the packaging layer can be tightly adhered on the porous base film. The Nafion molecular chain and the porous membrane substrate (namely PVDF or PTFE) molecular chain segments are fluorine-containing fatty chain segments, and have good compatibility and strong intermolecular acting force, so that Nafion can stably exist when being solidified on the surface of the porous membrane. Therefore, the invention has the remarkable advantages that the stability of the packaging layer on the surface of the porous base film is effectively improved, thereby avoiding the leakage of the ionic liquid, keeping the performance stable, especially realizing the self-supporting effect of the packaging ionic liquid supporting liquid film and solving the problems that the traditional packaging ionic liquid supporting liquid film can not be stored and transported.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely by way of example only, and it should be apparent that the described embodiments are only some, but not all, examples of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The chemical reagents used in the examples of the present invention are all commercially available.
Comparative example
Netherlands journal of desalination(Desamination, 2013, 317:11-16) discloses a film making method for stabilizing an ionic liquid supported liquid film, which comprises the steps of firstly preparing [ PP13]][TFSI]Filling (1-methyl-1-propylpiperidinebis (trifluoromethylsulfonyl) imide) ionic liquid into Gore-Tex with a thickness of 1mm TM And in the porous membrane, two Nafion 324 membranes are respectively covered on two sides of the porous membrane after the ionic liquid is filled, so that the ionic liquid supported liquid membrane is obtained.
The membrane is subjected to electrodialysis brine lithium extraction performance and stability test: at room temperature, an ionic liquid supported liquid film was fixed in the feed chamber (1350 ppm Mg 2+ 、170ppb Li + ) And the receiving chamber (0.1M HCl), electrodialysis was performed for 2h using a 2V voltage. By testing Li of the feed chamber solution, the receiving chamber solution + 、Mg 2+ Concentration calculation of Li + (higher better), mg 2+ (lower and better) recovery ratio, the mass of the supported liquid film of the packaged ionic liquid before and after electrodialysis is weighed, and the ionic liquid residual ratio is calculated (higher and better). Experimental results show that Li + The recovery rate of (2) was 22.5%, mg 2+ The recovery rate of (2) was 0.86%, and the ionic liquid remaining rate in the membrane was 95.0%.
Example 1
Preparing Nafion methanol solution with the concentration of 10g/L as casting solution, spin-coating the casting solution on the upper surface of a PVDF porous base film (model GVHP04700 of Millipore company) with the thickness of 125 micrometers, controlling the thickness of the coating film to be 5 micrometers, baking at 30 ℃ for 60 minutes to solidify a Nafion encapsulation layer, uniformly coating phenolic resin glue on the side surface of the porous base film, naturally solidifying at room temperature for 20 minutes to form a compact glue layer, soaking the porous base film in [ PP13] [ TFSI ] ionic liquid for 1 hour to ensure that the ionic liquid completely fills the film holes of the porous film, removing redundant ionic liquid on the film surface by using oil absorption wiping paper, spin-coating the casting solution on the lower surface of the porous base film, controlling the thickness of the coating film to be 5 micrometers, and baking at 30 ℃ for 60 minutes to solidify the Nafion encapsulation layer. Finally, the encapsulated ionic liquid supported liquid film is obtained. The thickness of Nafion packaging layers on the upper surface and the lower surface is 1 micrometer through observation of a scanning electron microscope.
Electrodialysis brine lithium extraction performance test under the same conditions as comparative exampleAnd testing the stability performance of the film. The results show that the encapsulated ionic liquid prepared in this example supports a liquid film of Li + The recovery rate of (2) was 30.1%, mg 2+ The recovery rate of the ionic liquid in the membrane is 0.53 percent, and the residual rate of the ionic liquid in the membrane is 99.2 percent. On this basis, the above experiment was repeated 6 times to test the stability of the film. The results show that after 6 repeated tests, li + The recovery rate of (2) was 29.7%, mg 2+ The recovery rate of the ionic liquid in the membrane is 0.58 percent, and the residual rate of the ionic liquid in the membrane is 99.0 percent, which indicates that the ionic liquid can exist stably in the porous base membrane.
Compared with the encapsulated ionic liquid supported liquid film prepared in the comparative example, the encapsulated ionic liquid supported liquid film prepared in the embodiment has the ionic liquid residual rate (95.0% of 99.2%) and Li + Recovery rate (22.5% of 30.1%) and Mg 2+ The recovery rate (0.53 percent to 0.86 percent) is greatly improved. Based on the method, the prepared packaging support ionic liquid membrane has more outstanding performance advantages.
Example 2
An encapsulated ionic liquid supported liquid film was prepared in a similar manner to example 1 except that the concentration of Nafion in methanol was changed to 3g/L, the coating thickness of Nafion solution was changed to 1 micron, and the thickness of both the upper and lower Nafion encapsulation layers was measured to be 0.2 micron.
The electrodialysis brine lithium extraction performance test and the membrane stability performance test are carried out under the same conditions of the comparative example. The results show that Li + The recovery rate of (2) was 35.1%, mg 2+ The recovery rate of the ionic liquid in the membrane is 0.81 percent, and the residual rate of the ionic liquid in the membrane is 96.2 percent. Measured after 6 repeated experiments: li (Li) + The recovery rate of (2) was 34.7%, mg 2+ The recovery rate of the ionic liquid in the membrane is 0.84 percent and the residual rate of the ionic liquid in the membrane is 96.0 percent.
Compared with the example 1, the encapsulated ionic liquid supported liquid film prepared in the example 2 has Li when extracting lithium + And Mg (magnesium) 2 + The recovery rate of (2) was improved because the Nafion solution concentration and film thickness were reduced from 10g/L and 5 microns to 3g/L and 1 micron, respectively, from example 1 to example 2, resulting in a reduction in Nafion encapsulation film thickness from 1 micron to 0.2 microns, thereby accelerating the rate of dissolutionThe speed of ion transport is reduced. Example 2 has a higher Li than the ionic liquid supported liquid film prepared in the comparative example + Recovery rate of similar Mg 2+ And ionic liquid residual rate.
The results of examples 1 and 2 are combined to demonstrate that the lithium extraction performance of the membrane can be regulated and controlled by controlling the thickness of the encapsulation layer by adopting the encapsulated ionic liquid support liquid membrane prepared by the invention.
Example 3
Preparing Nafion methanol solution with the concentration of 5g/L as casting solution, spin-coating the casting solution on the upper surface of a PVDF porous base film (model GVHP04700 of Millipore company) with the thickness of 125 micrometers, controlling the thickness of the coating film to be 5 micrometers, baking at 70 ℃ for 20 minutes to solidify a Nafion encapsulation layer, uniformly coating phenolic resin glue on the side surface of the porous base film, naturally solidifying at room temperature for 20 minutes, soaking the porous base film in [ PP13] [ TFSI ] ionic liquid for 1 hour to ensure that the ionic liquid completely fills the film holes of the porous film, removing redundant ionic liquid on the surface of the film by using oil absorption wiping paper, spin-coating the casting solution on the lower surface of the porous base film, controlling the thickness of the coating film to be 5 micrometers, baking at 70 ℃ for 20 minutes to solidify the Nafion encapsulation layer, and finally obtaining the encapsulated ionic liquid supported liquid film. The thickness of the Nafion encapsulation layer on both the upper and lower surfaces was measured to be 0.5 microns.
The electrodialysis brine lithium extraction performance test and the membrane stability performance test are carried out under the same electrodialysis conditions in comparative examples, and the result shows that Li + The recovery rate of (2) was 33.5%, mg 2+ The recovery rate of the ionic liquid in the membrane is 0.64%, and the residual rate of the ionic liquid in the membrane is 97.5%. Measured after 6 repeated experiments: li (Li) + The recovery rate of (2) was 33.2%, mg 2+ The recovery rate of the ionic liquid in the membrane is 0.68 percent, and the residual rate of the ionic liquid in the membrane is 97.3 percent.
Example 4
An encapsulated ionic liquid supporting liquid film was prepared in a similar manner to example 3, except that the PVDF porous base film was changed to a PTFE porous base film having a thickness of 80 μm (Advantec company, model T020a 047A), to obtain an encapsulated ionic liquid supporting liquid film comparable to the performance thereof, and the thickness of the Nafion encapsulation layer on both the upper and lower surfaces thereof was 0.75 μm.
The electrodialysis brine lithium extraction performance test and the membrane stability performance test are carried out under the same electrodialysis conditions in comparative examples, and the result shows that Li + The recovery rate of (2) was 34.8%, mg 2+ The recovery rate of the ionic liquid in the membrane is 0.66 percent, and the residual rate of the ionic liquid in the membrane is 97.4 percent. Measured after 6 repeated experiments: li (Li) + The recovery rate of (2) was 34.6%, mg 2+ The recovery rate of the ionic liquid in the membrane is 0.68 percent, and the residual rate of the ionic liquid in the membrane is 97.2 percent.
The results of example 3 and example 4 together demonstrate that the encapsulation technique employed in the present invention is applicable to porous base films of different materials.
Example 5
An encapsulated ionic liquid supporting liquid film was prepared by a method similar to that of example 3, except that the method of coating film was changed to a coating method, to obtain an encapsulated ionic liquid supporting liquid film equivalent in performance to that of the film.
Example 6
An encapsulated ionic liquid supporting liquid film was prepared by a method similar to that of example 3, except that the method of coating film was changed to a spray coating method, to obtain an encapsulated ionic liquid supporting liquid film having comparable performance.
Example 7
An encapsulated ionic liquid supporting liquid film was prepared in a similar manner to example 3 except that the method of coating the film was changed to a knife coating method, to obtain an encapsulated ionic liquid supporting liquid film having comparable performance.
Example 8
An encapsulated ionic liquid supported liquid membrane was prepared in a manner similar to that of example 3, except that the solvent of the Nafion solution was changed to water, to obtain an encapsulated ionic liquid supported liquid membrane comparable in performance thereto.
Example 9
An encapsulated ionic liquid supported liquid membrane was prepared in a similar manner to example 3 except that the solvent of the Nafion solution was changed to n-propanol to give an encapsulated ionic liquid supported liquid membrane comparable in performance.
Example 10
An encapsulated ionic liquid supported liquid membrane was prepared in a similar manner to example 3 except that the solvent of the Nafion solution was changed to isopropanol to give an encapsulated ionic liquid supported liquid membrane comparable in performance thereto.
Example 11
An encapsulated ionic liquid support liquid membrane was prepared by a method similar to that of example 3, except that the solvent of the Nafion solution was changed to a mixed solution of water, ethanol, n-propanol and isopropanol in a volume ratio of 1:1:1:1, to obtain an encapsulated ionic liquid support liquid membrane comparable to that of the same.
Example 12
A packaged ionic liquid supporting liquid film was prepared by a method similar to that of example 3, except that the glue was changed to AB glue, to obtain a packaged ionic liquid supporting liquid film equivalent to that in performance.
The results of the above examples show that by adopting the preparation method of the invention, the properties of the prepared encapsulated ionic liquid supported liquid film can be effectively controlled by controlling various conditions in the film preparation process, so that the encapsulated ionic liquid supported liquid film with optimal performance is selected. Meanwhile, the encapsulated ionic liquid supported liquid film prepared by the method has excellent lithium extraction performance, and is expected to realize practical application of extracting lithium from salt lakes.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (5)
1. A preparation method of a packaged ionic liquid supported liquid film is characterized in that Nafion solution is coated on the upper surface of a porous base film, a packaging layer is formed by heating, drying and forming, glue is coated on the side surface of the porous base film, naturally airing and solidifying are carried out, the porous base film is soaked in ionic liquid, excessive ionic liquid on the surface of the film is wiped off by oil absorption wiping paper after adsorption saturation, then the Nafion solution is coated on the lower surface of the porous base film, and the packaging layer is formed by heating, drying and forming, so that the packaged ionic liquid supported liquid film is finally obtained;
the porous base membrane is a PTFE porous membrane or a PVDF porous membrane;
the ionic liquid is [ PP13] [ TFSI ] (1-methyl-1-propylpiperidinebis (trifluoromethyl sulfonyl) imide salt);
the Nafion encapsulation layers on the upper surface and the lower surface of the porous base film have the thickness of 0.2-1 micron.
2. The method for preparing the encapsulated ionic liquid supported liquid membrane according to claim 1, wherein the concentration of the Nafion solution is 3-10g/L, and the solvent is one or more of water, methanol, n-propanol and isopropanol.
3. The method for preparing the encapsulated ionic liquid supported liquid membrane according to claim 1, wherein the coating film is prepared by spin coating, spraying or knife coating, and the thickness of the coating film is 1-5 micrometers.
4. The method for preparing a liquid film supported by an encapsulated ionic liquid according to claim 1, wherein the heating treatment is carried out at a temperature of 30-70 ℃ for 20-60 minutes.
5. An encapsulated ionic liquid supported liquid membrane prepared according to the method of any one of claims 1-4.
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CN107803117B (en) * | 2016-09-09 | 2020-12-04 | 中国科学院青岛生物能源与过程研究所 | High-stability mesoporous polymer confined ionic liquid supported liquid membrane and preparation method and application thereof |
CN110090566A (en) * | 2019-05-10 | 2019-08-06 | 郑州大学 | A kind of sulfonated polyether-ether-ketone-ionic liquid composite membrane, preparation method and its in CO2Application in separation |
CN113540488B (en) * | 2020-04-20 | 2022-09-30 | 中国科学院过程工程研究所 | Organic lithium ion flow battery diaphragm with sandwich structure and preparation method thereof |
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