CN110124631A - A method of lithium ion blotting membrane is prepared based on automatically controlled ion exchange - Google Patents

A method of lithium ion blotting membrane is prepared based on automatically controlled ion exchange Download PDF

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Publication number
CN110124631A
CN110124631A CN201910302686.2A CN201910302686A CN110124631A CN 110124631 A CN110124631 A CN 110124631A CN 201910302686 A CN201910302686 A CN 201910302686A CN 110124631 A CN110124631 A CN 110124631A
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electrode
lithium ion
lithium
platinized platinum
stainless steel
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刘伟峰
闫光
刘旭光
杨永珍
梁琦
安卓琳
张二辉
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Taiyuan University of Technology
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Taiyuan University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/268—Polymers created by use of a template, e.g. molecularly imprinted polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
    • C08G73/0611—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B3/00—Electrolytic production of organic compounds
    • C25B3/01—Products
    • C25B3/13—Organo-metallic compounds

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  • Organic Chemistry (AREA)
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  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
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Abstract

A method of lithium ion blotting membrane is prepared based on automatically controlled ion exchange, belong to preparation and the applied technical field of electroactive ion blotting film, it can solve the problems, such as that traditional lithium method that mentions has low extraction efficiency, poor selectivity to some extent, interferes vulnerable to other metal objects in seawater and flyash environment, using the method synthesizing lithium ion blotting membrane of unipolar pulse electrochemistry, this film has good adsorptivity to the lithium ion of low concentration, it is adsorbed and is eluted and all use potentiostatic method, secondary pollution will not be caused to environment, be a kind of environmentally friendly substance.Its substance synthesized is the atrament being aggregated on platinized platinum, microscopic appearance is near-spherical substance, 2- methylol -12-crown-4 is doped in pyrroles's film, is had good adsorption capacity for the lithium ion of low concentration in solution, is a kind of synthetic method of advanced ion blotting material.

Description

A method of lithium ion blotting membrane is prepared based on automatically controlled ion exchange
Technical field
The invention belongs to the preparation of electroactive ion blotting film and applied technical fields, and in particular to one kind based on it is automatically controlled from Sub- exchange system has specific recognition to lithium ion using the synthesis of automatically controlled ion exchange technique for the method for lithium ion blotting membrane Film.
Background technique
Lithium is in metal known to nature than lightest metal, and lithium has good chemical property, it almost can be with It reacts with nonmetallic in addition to rare gas.Furthermore lithium also has very high energy, and compound also has good Electric conductivity.So along with the rapid development of global economy, lithium and its compound products have penetrated into the production and life of people In work.The demand of the lithium battery of the battery of big electricity capacity, industrial aluminium lithium alloy and electric car is increased sharply.Lithium simple substance also by with Make nuclear power source, alloy is since with light weight, toughness is strong and the characteristics such as intensity is high are widely used in aerospace industry.
Currently, the annual consumption of lithium resource is 400,000 tons, and in fast-developing trend, this make mainly by salt lake and The lithium reserves (39,500,000 tons) contained in ore, far from meeting the market demand.And lithium resource rich in seawater, it is total Also contain a large amount of lithium resource in 26,000,000,000 tons of content and the flyash in China.So developing effective Extracting Lithium from Seawater and powder Coal ash, which proposes lithium technology, has important strategic importance to the development of national economy and military field.
Currently, the method for mentioning lithium from seawater, the method for Extracting Lithium from Seawater mainly includes ion exchange, the precipitation method, UF membrane With adsorbent method.But for the seawater that lithium concentration is only 0.17 mg/L, traditional lithium method that mentions is deposited to some extent Extraction efficiency is low, poor selectivity, interfered vulnerable to other metal objects in seawater and flyash environment the disadvantages of.
Automatically controlled ion exchange is had received ardent in recent years due to friendly, green and the high efficiency to environment Concern；During carrying out ionic adsorption, electroactive material is fixed on conductive material, passes through what is aoxidized or restore Mode, selective absorbs and releases ion, will not generate secondary pollution to environment during progress, use electroactive material Manufactured film can be used repeatedly；In recent years molecule and ion blotting because its structure can predictive and special selection Property is by scholar's extensive concern；It is mainly fixed against function monomer and object ion in shape to the specificity identification of specific ion Size, there is the three-dimensional structure to match each other in size in shape, by electrostatic, complexing, covalent and non-covalent bond effect, reach To the purpose of recognition template molecule or ion；Technique plans automatically controlled method and engram technology combines, synthesize a kind of pair of lithium from Son has single-minded absorption, specific binding, adsorption capacity strong, no pollution to the environment and having of being used repeatedly conductive The lithium ion blotting membrane of property.
Summary of the invention
There is low extraction efficiency, poor selectivity to some extent, vulnerable to seawater for traditional lithium method that mentions in the present invention And the problem of other metal objects are interfered in flyash environment, it provides and a kind of lithium ion blotting membrane is prepared based on automatically controlled ion exchange Method.
The present invention adopts the following technical scheme:
A method of lithium ion blotting membrane is prepared based on automatically controlled ion exchange, is carried out under three-electrode system: work electricity Pole: platinized platinum, to electrode: stainless steel substrates, reference electrode: saturation calomel is recycled 6000 times using the method for unipolar pulse electropolymerization It is made: wherein operating potential :+0.8 V, duration: 0.4 s, open circuit potential :+0.3V, duration: 4.0 s；Including such as Lower step:
The first step measures ultrapure water 20mL, ± 0.0001 g of 0.0212 g of lithium chloride, ± 0.0001 g of 0.3728 g of potassium chloride, It is added in beaker, stirring is completely dissolved to lithium chloride and potassium chloride, obtains mixed solution A；
Second step measures 0.1400mL ± 0.0001mL pyrroles in mixed solution A, and constant speed stirs 10min, obtains mixed solution B measures ± 0.0001 mL 2- methylol of 0.0870mL -12-crown-4 in mixed solution B, continues to stir 12min, be mixed Close solution C；
Third step after platinized platinum is polished, is flushed three times with deionized water, and dehydrated alcohol flushes three times, and drying records the matter of platinized platinum Amount；After stainless steel substrates are polished, three times, dehydrated alcohol is flushed three times for washing；Use electrode clamping respectively platinized platinum and stainless steel substrates Fixed, the corresponding electrode holder of platinized platinum connects working electrode, and the corresponding electrode connection of stainless steel substrates is saturated calomel and is directly connected to electrode Reference electrode is dipped in mixed solution C；
4th step, opens electrochemical workstation, and parameter: operating potential :+0.8 is arranged in the method for selecting any constant potential staircase waveform V, ETAD expected time of arrival and departure: 0.4 s；Open circuit potential :+0.3V, the time: 4.0 s is closed；Cycle-index: 6000 times；
5th step closes electrochemical workstation after reaction, by platinized platinum, stainless steel substrates and is saturated calomel from mixed solution C Middle taking-up, saturated calomel electrode are put into the Klorvess Liquid of saturation, and stainless steel substrates alcohol washes, drying will close on platinized platinum At lithium ion blotting membrane with ultrapure water 3 times, be put into drying for standby in baking oven；
6th step, storage, the lithium ion imprinted material of preparation is stored in surface plate, 20 DEG C of storage temperature, and relative humidity≤ 10%。
Beneficial effects of the present invention are as follows:
Have compared with the background technology, the present invention it is apparent advanced, be about low concentration in seawater and acid system lithium from Son is difficult to the problem of extracting, and experiment is mutually to tie the automatically controlled ion exchange technique in electrochemical process with conventional ion imprinting techniques It closes, using the method synthesizing lithium ion blotting membrane of unipolar pulse electrochemistry, this film has good suction to the lithium ion of low concentration Attached property, is adsorbed and is eluted and all use potentiostatic method, will not cause secondary pollution to environment, is a kind of environmental-friendly Type substance.Its substance synthesized is the atrament being aggregated on platinized platinum, and microscopic appearance is near-spherical substance, due to 2- hydroxyl first Base -12-crown-4 has lithium ion the recognition reaction of specificity, and pyrroles can be used as conductive agent and crosslinking agent for 2- hydroxyl first Base -12-crown-4 is doped in pyrroles's film, is had good adsorption capacity for the lithium ion of low concentration in solution, is a kind of Advanced ion print has the synthetic method of mark material.
Detailed description of the invention
Fig. 1 is the device figure that preparation method of the invention uses；
Fig. 2 is the SEM figure of the lithium ion blotting membrane of preparation of the embodiment of the present invention；
Fig. 3 is the energy spectrum diagram of the lithium ion blotting membrane of preparation of the embodiment of the present invention；
Fig. 4 is the infrared spectrogram of the lithium ion blotting membrane of preparation of the embodiment of the present invention；
Fig. 5 is that the lithium ion blotting membrane of preparation of the embodiment of the present invention and non-imprinted material adsorption capacity compare figure；
Wherein: 1- electrochemical workstation；2- electrochemical workstation switch；The channel 3-；4- electrode wires；5- is to electrode；6- reference electricity Pole；7- working electrode；8- platinized platinum；Substance in 9- polymerization；10- beaker；11- mixed solution C.
Specific embodiment
As shown in Figure 1, being ion blotting membrane preparation device figure, the position of all components, connection relationship will accurately match according to quantity Than sequentially operating.
The magnitude for preparing the chemical substance used is determined by pre-set range, is measurement unit with gram, microlitre.
Electrochemical workstation be it is three-dimensional, have control switch on electrochemical workstation, have channel by switch, set on channel There are three strip electrode lines, by three strip electrode lines respectively and to electrode (stainless steel substrates), reference electrode (saturated calomel electrode), work electricity Pole is attached, on the working electrode (s fix platinized platinum, then by reference electrode (saturated calomel electrode), working electrode, to electrode (no Rust steel disc electrode) it is immersed in the mixed solution of beaker, relevant parameter is set, turns on the switch and is polymerize, gradually generate black Solid mixture matter.
A kind of preparation method of lithium ion imprinted material, includes the following steps:
The first step, will carry out the chemical substance material that uses of preparation selected, and carry out quality purity, concentration, content control:
Lithium chloride: solid state purity 99%；2- methylol -12-crown-4: liquid liquid purity 97%；Pyrroles: liquid liquid purity 99%；Potassium chloride: solid state purity 99.5%；Ultrapure water: liquid liquid purity 99.99%；
Second step, the preparation of lithium ion blotting membrane:
The preparation of lithium ion blotting membrane is carried out under three-electrode system: working electrode: platinized platinum, to electrode: stainless steel substrates, ginseng Than electrode: saturation calomel, recycle 6000 times using the method for unipolar pulse electropolymerization and be made: wherein operating potential :+0.8 V is held The continuous time: 0.4 s, open circuit potential :+0.3V, duration: 4.0 s；
(1) 20 mL ultrapure waters are measured with the graduated cylinder of 25mL first；With Experimental electron balance weigh 0.0212 g of lithium chloride ± 0.0001 g, it weighs in the beaker of ± 0.0001 g of 0.3728 g of potassium chloride addition 25mL, with glass bar stirring until lithium chloride It is completely dissolved with potassium chloride；
(2) measure 0.1400mL ± 0.0001mL pyrroles in above-mentioned solution, with magnetic stirring apparatus constant speed stir 10 minutes, then ± 0.0001 mL 2- methylol of 0.0870mL -12-crown-4 is measured in beaker, continues stirring 12 minutes；
(3) platinized platinum is slightly polished with sand paper, is flushed three times with deionized water, dehydrated alcohol flushes three times, drying, with reality Test the quality that electronic balance weighs platinized platinum；Stainless steel substrates are polished with sand paper, three times, dehydrated alcohol is washed three times for washing；It will Platinized platinum and stainless steel substrates use electrode clamping fixed respectively, and electrode holder corresponding to platinized platinum connects working electrode, and stainless steel iron plate institute is right The electrode holder connection answered is saturated calomel and is directly connected to reference electrode to electrode；
(4) electrochemical workstation and test software are opened, any this method of constant potential staircase waveform is selected, to used method Parameter is configured: operating potential :+0.8 V, ETAD expected time of arrival and departure: 0.4 s, this period are ETAD expected time of arrival and departure, are that pyrrole monomer aggregates into pyrrole It coughs up film and removes the lithium ion that self assembly enters in composite membrane；Open circuit potential :+0.3V, the time: 4.0 s, this period is closed It is to carry out the doping of 2- methylol -12-crown-4 and the self assembly of 2- methylol -12-crown-4 and lithium ion；Operating potential is opened After time, open circuit potential, the setting of pass time, cycle-index is arranged: 6000 times, cycle-index is to form a stabilization Lithium ion blotting membrane of good performance；
(5) after the completion of reaction, turn off electrochemical workstation, platinized platinum, stainless steel substrates and saturation calomel taken out from solution, Saturated calomel electrode is put into the Klorvess Liquid of saturation, stainless steel substrates alcohol washes, drying, by the lithium synthesized on platinized platinum from Sub- blotting membrane is put into drying for standby in baking oven with ultrapure water 3 times；
Third step, product storage:
The lithium ion imprinted material of preparation is stored in surface plate, 20 DEG C of storage temperature, relative humidity≤10%.
Test, analysis and characterization
The form of the ion blotting material of synthesis, color, specific ingredient, the property of the physics of chemistry, the ability of absorption are carried out Characterization, test and analysis；
Morphology analysis is carried out to lithium ion blotting membrane using field emission scanning electron microscope；
It is carried out using energy disperse spectroscopy to the microcosmic elemental analysis of lithium ion blotting membrane；
Surface functional group analysis is carried out to lithium ion blotting membrane using infrared spectrometer；
Concentration analysis is carried out to the solution after absorption with inductive coupling plasma emission spectrograph；
It is macroscopically black solid as shown in Fig. 2, being lithium ion blotting membrane shape appearance figure, microcosmic upper presentation near-spherical pattern.
As shown in figure 3, having C, N, O element on ion blotting film as shown in the figure for ion blotting film energy spectrum diagram, showing 2- methylol -12-crown-4 is doped in pyrroles's film during pyrroles polymerize.
As shown in figure 4, being ion blotting film infrared spectrogram, 1056 cm-1It is the bending vibration of-N-H key, 1450 cm-1 With 1615 cm-1It is the asymmetry and symmetrical stretching vibration of pyrrole ring respectively.1263 cm-1It is the stretching vibration of-C-O key, it was demonstrated that 2 methylol 12-crown-4s are successfully doped in polypyrrole film.
As shown in figure 5, comparing figure for blotting membrane and non-blotting membrane adsorption capacity, as shown in the figure, blotting membrane is to lithium ion The time that removal reaches balance needs 2 hours, and maximal absorptive capacity is 8.42 mg/g；Maximum adsorption of the non-blotting membrane to lithium ion Amount is 3.58 mg/g, and blotting membrane is non-blotting membrane to 2.35 times of the adsorbance of lithium ion to the adsorbance of lithium ion.
Conclusion: lithium ion blotting membrane is macroscopically rendered as black solid material, micro- under field emission microscope It is in near-spherical pattern in sight, by being doped with 2- hydroxyl first in the characterization and analytical proof hybrid films of energy disperse spectroscopy and infrared spectrometer Base -12-crown-4, and just can reach adsorption equilibrium state in 2 hours, equilibrium adsorption capacities are non-blotting membranes up to 8.42 mg/g There is certain adsorption capacity to 2.35 times of lithium ions to low concentration of the adsorbance of lithium ion, therefore in lithium resource extraction side There is very big application prospect in face.

Claims (1)

1. a kind of method for preparing lithium ion blotting membrane based on automatically controlled ion exchange, it is characterised in that: under three-electrode system into Capable: working electrode: platinized platinum, to electrode: stainless steel substrates, reference electrode: saturation calomel, using the method for unipolar pulse electropolymerization It is made for circulation 6000 times: wherein operating potential :+0.8 V, duration: 0.4 s, open circuit potential :+0.3V, duration: 4.0 s；Include the following steps:
The first step measures ultrapure water 20mL, ± 0.0001 g of 0.0212 g of lithium chloride, ± 0.0001 g of 0.3728 g of potassium chloride, It is added in beaker, stirring is completely dissolved to lithium chloride and potassium chloride, obtains mixed solution A；
Second step measures 0.1400mL ± 0.0001mL pyrroles in mixed solution A, and constant speed stirs 10min, obtains mixed solution B measures ± 0.0001 mL 2- methylol of 0.0870mL -12-crown-4 in mixed solution B, continues to stir 12min, be mixed Close solution C；
Third step after platinized platinum is polished, is flushed three times with deionized water, and dehydrated alcohol flushes three times, and drying records the matter of platinized platinum Amount；After stainless steel substrates are polished, three times, dehydrated alcohol is flushed three times for washing；Use electrode clamping respectively platinized platinum and stainless steel substrates Fixed, the corresponding electrode holder of platinized platinum connects working electrode, and the corresponding electrode connection of stainless steel substrates is saturated calomel and is directly connected to electrode Reference electrode is dipped in mixed solution C；
4th step, opens electrochemical workstation, and parameter: operating potential :+0.8 is arranged in the method for selecting any constant potential staircase waveform V, ETAD expected time of arrival and departure: 0.4 s；Open circuit potential :+0.3V, the time: 4.0 s is closed；Cycle-index: 6000 times；
5th step closes electrochemical workstation after reaction, by platinized platinum, stainless steel substrates and is saturated calomel from mixed solution C Middle taking-up, saturated calomel electrode are put into the Klorvess Liquid of saturation, and stainless steel substrates alcohol washes, drying will close on platinized platinum At lithium ion blotting membrane with ultrapure water 3 times, be put into drying for standby in baking oven；
6th step, storage, the lithium ion imprinted material of preparation is stored in surface plate, 20 DEG C of storage temperature, and relative humidity≤ 10%。
CN201910302686.2A 2019-04-16 2019-04-16 A method of lithium ion blotting membrane is prepared based on automatically controlled ion exchange Pending CN110124631A (en)

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CN110681367A (en) * 2019-09-04 2020-01-14 太原理工大学 Preparation method of nitrogen-doped carbon microsphere graphene composite aerogel lithium imprinted membrane for extracting lithium from acidic system
CN111530510A (en) * 2020-04-16 2020-08-14 太原理工大学 Preparation method of electric control ion exchange membrane extraction material and application of electric control ion exchange membrane extraction material in iodide ion removal
CN114797799A (en) * 2022-04-15 2022-07-29 东北电力大学 Preparation method of MOFs-based lithium ion imprinting composite nanofiber membrane

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110681367A (en) * 2019-09-04 2020-01-14 太原理工大学 Preparation method of nitrogen-doped carbon microsphere graphene composite aerogel lithium imprinted membrane for extracting lithium from acidic system
CN110681367B (en) * 2019-09-04 2022-03-15 太原理工大学 Preparation method of nitrogen-doped carbon microsphere graphene composite aerogel lithium imprinted membrane for extracting lithium from acidic system
CN111530510A (en) * 2020-04-16 2020-08-14 太原理工大学 Preparation method of electric control ion exchange membrane extraction material and application of electric control ion exchange membrane extraction material in iodide ion removal
CN111530510B (en) * 2020-04-16 2023-04-18 太原理工大学 Preparation method of electric control ion exchange membrane extraction material and application of electric control ion exchange membrane extraction material in iodide ion removal
CN114797799A (en) * 2022-04-15 2022-07-29 东北电力大学 Preparation method of MOFs-based lithium ion imprinting composite nanofiber membrane
CN114797799B (en) * 2022-04-15 2023-08-01 东北电力大学 Preparation method of MOFs-based lithium ion imprinting composite nanofiber membrane

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