CN110975845A - Preparation method of porous material loaded with lithium ion sieve - Google Patents
Preparation method of porous material loaded with lithium ion sieve Download PDFInfo
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- CN110975845A CN110975845A CN201911313274.5A CN201911313274A CN110975845A CN 110975845 A CN110975845 A CN 110975845A CN 201911313274 A CN201911313274 A CN 201911313274A CN 110975845 A CN110975845 A CN 110975845A
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Abstract
The invention discloses a preparation method of a porous material loaded with a lithium ion sieve. The invention takes a water solution containing a certain amount of lithium manganese oxide nano particles, a surfactant, acrylamide and N, N' -methylene bisacrylamide as a water phase; hydrophobic solvent such as paraffin oil is used as oil phase; and dropping the oil phase into the water phase under the stirring action to obtain the high internal phase emulsion with stable lithium manganese oxide nano particles. Pouring the emulsion into a chromatographic column, and placing the chromatographic column in a constant-temperature oven for polymerization; and washing with cyclohexane after polymerization, and drying in a vacuum drying oven to constant weight to obtain the porous column material loaded with the lithium manganese oxide nanoparticles. And washing the porous column by using 0.5 mol/L hydrochloric acid solution, washing the porous column by using deionized water to make the pH value of the porous column neutral, and drying the porous column to constant weight, thereby obtaining the porous column material loaded with the lithium ion sieve. The preparation method is novel and unique, the application is wide, the aperture of the obtained polymer porous material can be used as a high-efficiency lithium ion selective adsorption material, and the lithium ion adsorption capacity of the lithium ion sieve reaches 35.6 mg/g.
Description
Technical Field
The invention relates to a preparation method of a porous material loaded with a lithium ion sieve, in particular to a method for dispersing a certain amount of lithium manganese oxide nano particles into an aqueous solution of acrylamide and N, N' -methylene bisacrylamide, which contain a certain amount of surfactant, and taking the aqueous solution as a water phase; hydrophobic solvent such as paraffin oil is used as oil phase; and under the stirring action, uniformly dropping the oil phase into the water phase by using a constant-pressure dropping funnel, stirring for one minute after the dropping is finished, and completely encapsulating the dropped oil phase into the water phase to obtain the required high internal phase emulsion with the stable lithium manganese oxide nano particles. Pouring the obtained emulsion into a chromatographic column, and placing the chromatographic column in a constant-temperature oven for polymerization; after polymerization, washing the polymer porous material with cyclohexane to remove an oil phase and impurities of the polymer porous material, and putting the polymer porous material in a vacuum drying oven to be dried to constant weight to obtain a final porous column material loaded with the lithium manganese oxide nanoparticles; washing the porous column material by using 0.5 mol/L hydrochloric acid solution, washing the porous column by using deionized water to enable the pH value of the porous column to be neutral, drying the porous column to constant weight to obtain the porous column material loaded with the lithium ion sieve, and adsorbing lithium ions in water by using the porous column material loaded with the lithium ion sieve.
Background
In recent years, the problem of non-renewable resources has become more serious, and new clean energy sources have been sought. Lithium and lithium salts are widely used in the fields of batteries, metallurgy, energy, pharmacy, etc., and are called "new energy sources in the twenty-first century". At present, two modes of extracting lithium from ores and seawater brine are mainly reported for obtaining lithium, and because liquid lithium resources such as salt lake brine are richer in China and the efficiency of extracting lithium from ores is low, and the yield is not high, the method is mainly used for extracting lithium from salt lake brine. At present, the following methods for extracting lithium have been researched at home and abroad: evaporation, solvent, precipitation and ion adsorption. The ion adsorption method has more practical significance due to the problem of low lithium ion concentration in seawater brine, and the key point of the method is to prepare a high-efficiency adsorbent. The ion sieve adsorption method is recognized as the most promising method for extracting lithium from brine due to the characteristics of green and high efficiencyThe method of (1). Spinel type lithium manganese oxides (e.g. LiMn)2O4) The ion sieve is an inorganic ion exchange material which is most applied, lithium in an oxide can be almost completely extracted through acid washing treatment, a complete spinel structure can be kept, good adsorbability can be realized on the lithium, and the ion sieve has the advantages of good adsorbability, cyclic utilization, high efficiency and the like.
However, most of the currently prepared ion sieves are in powder form, and because of poor fluidity and permeability, the ion sieves lose lithium ions in transportation and adsorption of brine, so that the application range is limited, and the ion sieves cannot be applied industrially. To solve this problem, there are studies showing that the powdered ion sieve is granulated or formed into a film. The granulation refers to mixing an ionic sieve and a polymer, putting the mixture into an organic solvent for swelling polymerization, and adding a certain pore-making agent to obtain granules with a certain specific surface area. PVC is a better forming agent, and the Liuwentao and the like adopt a DMF-PVC-H2O system to carry out Li ion sieve precursors1.5Mn1.6O4And (4) granulating. Film formation is another main method of ion sieve formation, and is to mix ion sieve powder and casting solution into a film, and the surface of the film has pore diameters. However, at present, both granulation and film formation have a problem that the adsorption amount after forming is reduced because the contact area between the ion sieve and the lithium-containing dilute solution after forming is reduced.
In order to solve the problems, the lithium ion sieve powder can be loaded into a polymer porous material, and the lithium ion sieve is used for extracting lithium ions from brine by taking a porous columnar material as a carrier. The polymer porous material has the characteristic of high porosity, and according to the stabilization mechanism of the particle-stabilized high internal phase emulsion, the ionic sieve powder serving as the stabilizer is fixed on the wall of a macroporous hole and can be fully contacted with brine during the extraction of lithium ions, so that the problem of poor flowability of the ionic sieve powder is solved, and the adsorption capacity is ensured not to be reduced.
The invention uses lithium ion sieve precursor lithium manganese oxide nano particle (LiMn)2O4) Preparing pickering high internal phase emulsion as stabilizer, and initiating continuous phase monomer to polymerize in chromatographic column to obtain porous column loaded with Li-Mn-O nano particleA material. Preparing a lithium ion sieve through acid washing treatment, and adsorbing lithium ions; the invention is novel, unique, simple and feasible.
Disclosure of Invention
The technical problem to be solved by the invention is to disclose a preparation method of a porous material loaded with a lithium ion sieve, so as to endow the polymer porous material with functionalization, widen the application range of the polymer porous material and improve the adsorption efficiency of the lithium ion sieve on lithium ions. The method for preparing the polymer porous material loaded with the lithium ion sieve comprises the following steps of dispersing a certain amount of lithium manganese oxide nano particles into an aqueous solution of acrylamide and N, N' -methylene-bisacrylamide, wherein the aqueous solution is used as a water phase; hydrophobic solvent such as paraffin oil is used as oil phase; and under the stirring action, uniformly dropping the oil phase into the water phase by using a constant-pressure dropping funnel, stirring for one minute after the dropping is finished, and completely encapsulating the dropped oil phase into the water phase to obtain the required high internal phase emulsion with the stable lithium manganese oxide nano particles. Pouring the obtained emulsion into a chromatographic column, and placing the chromatographic column in a constant-temperature oven for polymerization; after polymerization, washing the polymer porous material with cyclohexane to remove an oil phase and impurities of the polymer porous material, and putting the polymer porous material in a vacuum drying oven to be dried to constant weight to obtain a final porous column material loaded with the lithium manganese oxide nanoparticles; washing the porous column material by using 0.5 mol/L hydrochloric acid solution, washing the porous column by using deionized water to enable the pH value of the porous column to be neutral, drying the porous column to constant weight to obtain the porous column material loaded with the lithium ion sieve, and adsorbing lithium ions in water by using the porous column material loaded with the lithium ion sieve.
The hydrophobic solvent is paraffin oil, toluene, cyclohexane, tetradecane, hexadecane or a mixture of two or more of the paraffin oil, the toluene, the cyclohexane, the tetradecane and the hexadecane;
the mass fraction of the acrylamide and the N, N' -methylene bisacrylamide in the water phase is 10-40%;
the oil phase accounts for 75-90% of the volume fraction of the emulsion;
the water-soluble initiator is potassium persulfate, ammonium persulfate or a mixture of the potassium persulfate and the ammonium persulfate;
the surfactant is one or two of Tween 60, Tween 20 and Triton, and the mass fraction of the surfactant in the water phase is 1% -5%;
the mass fraction of the lithium manganese oxide nano particles in the water phase is 1-6%.
Observing the morphology of the polymer porous material by adopting a Scanning Electron Microscope (SEM) S-3400 (Japanese JEOL company), and determining the hole spacing and the hole diameter; the lithium ion concentration in the solution was measured using an inductively coupled plasma emission spectrometer Agilent 725-ES (Agilent, USA).
The preparation method is simple and convenient to operate, and the obtained polymer porous material has the aperture of 20-500 microns and can efficiently adsorb lithium ions in an aqueous solution. The adsorption efficiency of the lithium ion sieve can reach 35.6 mg/g.
Detailed Description
Example 1
An amount of 0.04 g of lithium manganese oxide nanoparticles was dispersed in 4 ml of an aqueous solution of tween 60 at a concentration of 1% at room temperature, and then 0.3 g of monomeric acrylamide, 0.1g N, N' -methylenebisacrylamide and 0.04 g of an initiator were dissolved in the aqueous solution as an aqueous phase. And (3) taking 12 ml of paraffin oil as an oil phase, dripping the oil phase into the water phase at a constant speed by using a constant-pressure dropping funnel under the magnetic stirring action of 500 rpm, stirring for several minutes after finishing dripping, and completely wrapping the dripped oil phase into the water phase to obtain the required Pickering high internal phase emulsion. The obtained emulsion is poured into a chromatographic column to be sealed, and the chromatographic column is placed in a constant-temperature oven at the temperature of 60 ℃ to be polymerized for 24 hours. After polymerization, the polymer porous material is connected to a constant flow pump, and washed by cyclohexane for 24 hours at the rotating speed of 30rpm/min to remove the dispersed phase, and then washed by distilled water after vacuum drying. And finally, placing the porous column material in a 50 ℃ vacuum drying oven to be dried to constant weight to obtain the final porous column material loaded with the lithium manganese oxide nanoparticles. Washing the porous column material by using 0.5 mol/L hydrochloric acid solution, washing the porous column by using deionized water to enable the pH value of the porous column to be neutral, drying the porous column to constant weight to obtain the porous column material loaded with the lithium ion sieve, and adsorbing lithium ions in water by using the porous column material loaded with the lithium ion sieve.
The pore diameter of the obtained polymer porous material is about 370 microns, the obtained polymer porous material is used for lithium ion adsorption, and the lithium ion adsorption capacity of the lithium ion sieve is about 31 mg/g.
Example 2
An amount of 0.12 g of lithium manganese oxide nanoparticles was dispersed in 4 ml of an aqueous solution of tween 20 at 2% at room temperature, and then 1.42 g of acrylamide, 0.31g N, N' -methylenebisacrylamide and 0.08 g of an initiator were dissolved in the above aqueous solution as an aqueous phase. Taking 16 ml of paraffin oil as an oil phase, dripping the oil phase into a water phase at a constant speed by using a constant-pressure dropping funnel under the magnetic stirring action of 500 rpm, stirring for several minutes after finishing dripping, and completely encapsulating the dripped oil phase into the water phase to obtain the required Pickering high internal phase emulsion. The obtained emulsion is poured into a chromatographic column to be sealed, and the chromatographic column is placed in a constant temperature oven at 60 ℃ to be polymerized for 24 hours. After polymerization, the polymer porous material is connected to a constant flow pump, and washed by cyclohexane for 24 hours at the rotating speed of 30rpm/min to remove the dispersed phase, and then washed by distilled water after vacuum drying. And finally, placing the porous column material in a 50 ℃ vacuum drying oven to be dried to constant weight to obtain the final porous column material loaded with the lithium manganese oxide nanoparticles. Washing the porous column material by using 0.5 mol/L hydrochloric acid solution, washing the porous column by using deionized water to enable the pH value of the porous column to be neutral, drying the porous column to constant weight to obtain the porous column material loaded with the lithium ion sieve, and adsorbing lithium ions in water by using the porous column material loaded with the lithium ion sieve.
The pore diameter of the obtained polymer porous material is about 220 microns, the obtained polymer porous material is used for lithium ion adsorption, and the lithium ion adsorption capacity of the lithium ion sieve is about 35.6 mg/g.
Example 3
An amount of 0.16 g of lithium manganese oxide nanoparticles was dispersed in 4 ml of an aqueous solution of tween triton 100 at a concentration of 2% at room temperature, and then 1.42 g of acrylamide, 0.31g N, N' -methylenebisacrylamide and 0.08 g of an initiator were dissolved in the above aqueous solution as an aqueous phase. Taking 36 ml of paraffin oil as an oil phase, dripping the oil phase into a water phase at a constant speed by using a constant-pressure dropping funnel under the magnetic stirring action of 500 rpm, stirring for several minutes after finishing dripping, and completely encapsulating the dripped oil phase into the water phase to obtain the required Pickering high internal phase emulsion. The obtained emulsion is poured into a chromatographic column to be sealed, and the chromatographic column is placed in a constant-temperature oven at the temperature of 60 ℃ to be polymerized for 24 hours. After polymerization, the polymer porous material is connected to a constant flow pump, and washed by cyclohexane for 24 hours at the rotating speed of 30rpm/min to remove the dispersed phase, and then washed by distilled water after vacuum drying. And finally, placing the porous column material in a 50 ℃ vacuum drying oven to be dried to constant weight to obtain the final porous column material loaded with the lithium manganese oxide nanoparticles. Washing the porous column material by using 0.5 mol/L hydrochloric acid solution, washing the porous column by using deionized water to enable the pH value of the porous column to be neutral, drying the porous column to constant weight to obtain the porous column material loaded with the lithium ion sieve, and adsorbing lithium ions in water by using the porous column material loaded with the lithium ion sieve.
The pore diameter of the obtained polymer porous material is about 390 microns, the obtained polymer porous material is used for lithium ion adsorption, and the lithium ion adsorption capacity of the lithium ion sieve is about 19 mg/g.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (1)
1. The invention discloses a preparation method of a porous material loaded with a lithium ion sieve, which is characterized by comprising the following steps: dispersing a certain amount of lithium manganese oxide nano particles and a water-soluble initiator into an aqueous solution of acrylamide and N, N' -methylene-bisacrylamide containing a certain amount of surfactant, and taking the aqueous solution as a water phase; using hydrophobic solvent as oil phase; under the stirring action, uniformly dropping an oil phase into a water phase by using a constant-pressure dropping funnel, stirring for one minute after the dropping is finished, completely encapsulating the dropped oil phase into the water phase to obtain a required high internal phase emulsion with stable lithium manganese oxide nano particles, pouring the obtained emulsion into a chromatographic column, and placing the chromatographic column in a constant-temperature oven for polymerization; after polymerization, washing the polymer porous material with cyclohexane to remove an oil phase and impurities of the polymer porous material, and putting the polymer porous material in a vacuum drying oven to be dried to constant weight to obtain a final porous column material loaded with the lithium manganese oxide nanoparticles; washing the porous column material by using 0.5 mol/L hydrochloric acid solution, washing the porous column by using deionized water to enable the pH value of the porous column to be neutral, and drying the porous column to constant weight to obtain the porous column material loaded with the lithium ion sieve;
the hydrophobic solvent is paraffin oil, toluene, cyclohexane, tetradecane, hexadecane or a mixture of two or more of the paraffin oil, the toluene, the cyclohexane, the tetradecane and the hexadecane;
the mass fraction of the acrylamide and the N, N' -methylene bisacrylamide in the water phase is 10-40%; the mass fraction ratio of acrylamide to N, N' -methylene bisacrylamide is 10: 1-3: 1;
the oil phase accounts for 75-90% of the volume fraction of the emulsion;
the water-soluble initiator is potassium persulfate, ammonium persulfate or a mixture of the potassium persulfate and the ammonium persulfate;
the surfactant is one or two of Tween 60, Tween 20 and Triton, and the mass fraction of the surfactant in the water phase is 1% -5%;
the mass fraction of the lithium manganese oxide nano particles in the water phase is 1-6%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115672256A (en) * | 2022-11-01 | 2023-02-03 | 北京碧水源膜科技有限公司 | Micron-sized lithium ion sieve micro-H 2 TiO 3 Preparation method of the ion sieve and salt lake lithium extraction system applying the ion sieve |
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| CN101955210A (en) * | 2010-09-14 | 2011-01-26 | 华东理工大学 | Granular lithium ion sieve |
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| CN103316623A (en) * | 2013-07-10 | 2013-09-25 | 华东理工大学 | Method for preparing spherical lithium ion sieve adsorbent |
| CN103613704A (en) * | 2013-10-10 | 2014-03-05 | 华东理工大学 | Photocatalyst nanopacticle-loaded polymer porous bead carrier material preparation method |
| CN104310568A (en) * | 2014-11-07 | 2015-01-28 | 华东理工大学 | Wastewater treatment method by utilizing Fenton reaction |
| WO2018161155A1 (en) * | 2017-03-06 | 2018-09-13 | Moasis Inc. | Porous crosslinked hydrophilic polymeric materials prepared from high internal phase emulsions containing hydrophilic polymers |
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- 2019-12-18 CN CN201911313274.5A patent/CN110975845A/en active Pending
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| JPH04118048A (en) * | 1990-03-30 | 1992-04-20 | Agency Of Ind Science & Technol | Granular lithium adsorbent, its manufacture and method for concentrating lithium |
| CN101955210A (en) * | 2010-09-14 | 2011-01-26 | 华东理工大学 | Granular lithium ion sieve |
| CN102391416A (en) * | 2011-09-02 | 2012-03-28 | 华东理工大学 | Preparation method of porous material based on inorganic nanoparticles for stabilizing high internal phase emulsion |
| CN103316623A (en) * | 2013-07-10 | 2013-09-25 | 华东理工大学 | Method for preparing spherical lithium ion sieve adsorbent |
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| CN104310568A (en) * | 2014-11-07 | 2015-01-28 | 华东理工大学 | Wastewater treatment method by utilizing Fenton reaction |
| WO2018161155A1 (en) * | 2017-03-06 | 2018-09-13 | Moasis Inc. | Porous crosslinked hydrophilic polymeric materials prepared from high internal phase emulsions containing hydrophilic polymers |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115672256A (en) * | 2022-11-01 | 2023-02-03 | 北京碧水源膜科技有限公司 | Micron-sized lithium ion sieve micro-H 2 TiO 3 Preparation method of the ion sieve and salt lake lithium extraction system applying the ion sieve |
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