CN107376655A - A kind of preparation method and use of lithium ion trace nano composite membrane - Google Patents
A kind of preparation method and use of lithium ion trace nano composite membrane Download PDFInfo
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- CN107376655A CN107376655A CN201710551922.5A CN201710551922A CN107376655A CN 107376655 A CN107376655 A CN 107376655A CN 201710551922 A CN201710551922 A CN 201710551922A CN 107376655 A CN107376655 A CN 107376655A
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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
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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
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- 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
Abstract
The invention belongs to field of material preparation, discloses a kind of preparation method and use of lithium ion trace nano composite membrane.Synthesis is as follows：Kynoar powder and polyvinylpyrrolidone are added to N, in N ' dimethyl acetamides, under constant temperature after mechanical agitation, the constant standing of keeping temperature, PVDF basement membranes is formed by phase-inversion technologies, this PVDF basement membrane is put and preserved in deionized water；PVDF basement membranes are immersed in AgNO3In solution, xenon lamp reaction 60min, obtaining surface has the pvdf membrane of Ag nano-particle layers；12 crown ethers 4 are added in methanol with lithium chloride, the PVDF basement membranes that the surface has poly-dopamine layer are immersed in mixed solution, add GDMA and azodiisobutyronitrile, form mixed liquor, sealed after logical inert gas, be placed in thermostatic control oscillator vibration and react；The film obtained after reaction is taken off with pickling, obtains lithium ion blotting membrane.
Description
Technical field
The invention belongs to field of material preparation, is related to a kind of preparation method of lithium ion trace nano composite membrane.
Background technology
Seperation film (separation membrane), refers to the membrane material with Selective Separation function, it can make in fluid
One or more of material permeances, and other materials can not pass through, so as to play a part of separation, purifying and concentration.Film can be with
It is homogeneous or heterogeneous, symmetric figure or unsymmetrical, solid-state or liquid, neutral or charge.Envelope point
From flowing material can be liquid, can also be gaseous, film has selective penetrated property, and this is also film and membrane separating process
Inherent characteristic.The scope that seperation film is applicable separation is extremely wide, and from microsize grade to microbial cells, or even ion level has it to use force
Ground, key be to select different film types, so membrane separation technique desalinization, drink water purifying, industrial wastewater and
Sanitary sewage disposal obtains extensively should with fields such as separation, purifying and the concentrations of the industry such as reuse and chemical industry, medicine, food
With providing technical guarantee for recycling economy, clean manufacturing etc., it has also become promote industry development, improve human being's production environment
One of general character support technology.
Molecular imprinting technology (Molecularly imprinted technique, MIT) is to simulate in nature such as：Enzyme
With the Molecular Recognization of substrate, antibody and antigen etc., being prepared using target molecule as template molecule has special choosing to the molecule
A kind of skill of the macromolecule imprinted polymer (Molecularly Imprinted Polymers, MIPs) of selecting property identification function
Art.Ionic imprinting technique (Ion imprinted technique, IIT) is the branch of molecular imprinting technology, it with yin, yang from
Son is template, is interacted by the action and function such as electrostatic, coordination monomer, and template ion is removed after cross-linked polymeric and is just obtained
Rigid polymer with special groups arrangement, fixed cavitation size and shape, the three-dimensional hole of formation has to object ion
Special compatibility and identity, more and more it is used for separation, the enrichment aspect of metal ion.Ion blotting film (Ion
Imprinted membranes, IIMs) ionic imprinting technique is coupled with membrane separation technique, have as one kind and used compared with usury
Rate while the small new material of environmental pollution, are widely applied to separation, purification art.
Nanometer metallic silver is because having the advantages that antibacterial wide spectrum, sterilization of high efficiency are paid attention in antibacterial applications.Metal is received
Rice corpuscles, which is grafted to Organic polymer film materials surface, can greatly improve the hydrophily, mechanical performance and resistance tocrocking of material
Energy
Lithium (lithium) and its compound be widely used in its excellent performance Lithium Battery Industry, electronics, metallurgy,
The fields such as chemical industry, medicine, the energy, there is important strategic position in national economy and national defense construction, be described as that " 21 century is new
The energy ".Lithium consumption figure is increased with annual 7%-11% speed in recent years, but existing lithium resource is but increasingly exhausted.Therefore, carry
The rate of recovery of high lithium is necessary.
The content of the invention
It is an object of the invention to provide a kind of lithium ion trace nano composite membrane, and it is used for Li+、Mg2+The choosing that ion coexists
Selecting property identifies and separation.
The present invention is achieved through the following technical solutions：
A kind of synthetic method of lithium ion trace nano composite membrane, step are as follows：
(1) Kynoar (PVDF) powder and polyvinylpyrrolidone (PVP) are added to N, N '-dimethyl acetamide
(DMAC) in, mechanical agitation under constant temperature, after the completion of mechanical agitation, the constant standing of keeping temperature, formed by phase-inversion technologies
PVDF basement membranes, this PVDF basement membrane is put and preserved in deionized water；
(2) the PVDF basement membranes that step (1) obtains are immersed in deionized water, add silver nitrate (AgNO3), at room temperature
Mechanical oscillation, it is put under xenon lamp and reacts；Obtaining surface has the PVDF basement membranes of Ag nano particles；
(3) 12- crown ethers -4 and lithium chloride are added in methanol, through A reacting forming ion imprinted polymers；Then will step
Suddenly the PVDF basement membranes that the surface that (2) obtain has Ag nano particles are immersed in the ion imprinted polymer, add diformazan
Base acrylic acid glycol ester (EGDMA) and azodiisobutyronitrile (AIBN), sealed after leading to inert gas, be placed in water bath with thermostatic control vibration
Oscillating reactions is carried out in device；After reaction terminates, nano composite membrane is taken out；
(4) nano composite membrane obtained after step (3) is reacted is taken off with pickling, obtains lithium ion trace nano composite membrane.
In step (1), the Kynoar, polyvinylpyrrolidone, the amount ratio of N, N '-dimethyl acetamide are
4g：(0.01~0.04) g：25~40mL.
In step (1), the constant temperature is 30 DEG C, and the churned mechanically time is 12h；The time of repose is 24h.
In step (2), the mass ratio of Kynoar is 1-2 in the quality and step (1) of the silver nitrate：4, xenon lamp
The lower reaction time will be 60min.
In step (3), used 12- crown ethers -4：Lithium chloride, GDMA, azodiisobutyronitrile,
The dosage of methanol is 0.6~1.2g：0.3g, 0.4~0.8mmol, 8~10mg, 50mL；The inert gas is nitrogen.
In step (3), the temperature of the A reactions is 25 DEG C, reaction time 2h.
In step (3), in the thermostatic control oscillator vibration, the temperature of oscillating reactions is 60 DEG C, and the time of reaction is 18h.
In step (4), described acid is HCl, concentration 0.2-0.5molL-1。
Described lithium ion trace nano composite membrane (IINMs) is used to adsorb lithium ion.
It is same as above that the synthesis of nonionic blotting membrane (NINMs) is added without template Li+ remaining step.
Kynoar powder described in above-mentioned technical proposal, it is used as synthesizing basal lamina material.
Lithium chloride described in above-mentioned technical proposal, it act as template ion.
12- crown ether -4 described in above-mentioned technical proposal, it act as function monomer.
GDMA described in above-mentioned technical proposal, it act as crosslinking agent.
Azodiisobutyronitrile described in above-mentioned technical proposal, it act as initiator.
In above-mentioned technical scheme, 12- crown ethers -4 and lithium chloride in methanol solution prepolymerization so that function monomer and mould
Chelation is produced between plate ion Li+, forms ion imprinted polymer.
Beneficial effects of the present invention are：
(1) products obtained therefrom of the present invention is used in PVDF membrane surface loaded Ag nano particles, effectively improve film hydrophily and
Antifouling property.12- crown ethers -4 are used as function monomer, and ion imprinted polymer is directly formed with lithium ion to improve specific recognition
Property.After loaded Ag nano particle, the antifouling property and renewable performance of membrane material are remarkably reinforced.
(2) nano combined blotting membrane of the present invention is to Li+With the advantages of selective height, separating effect is notable.
Brief description of the drawings
Fig. 1 SEM schematic diagrames, wherein, a is PVDF basement membranes, and b is PVDF membrane surface loaded Ag nanometers
Grain, c is the nano combined blotting membrane of ion；
Fig. 2 is the Staticadsorption experiment figure of embodiment 1, wherein, curve a is lithium ion blotting membrane, and curve b prints for non-lithium ion
Mark film；
Fig. 3 is the blotting membrane selective absorption lab diagram of embodiment 1, wherein, magnesium ion is competing ions, wherein separation
Fig. 4 is the Staticadsorption experiment figure of embodiment 2, wherein, curve a is lithium ion blotting membrane, and curve b prints for non-lithium ion
Mark film；
Fig. 5 is the blotting membrane selective absorption lab diagram of embodiment 2, wherein, magnesium ion is competing ions, wherein separation
Embodiment
With reference to Figure of description and specific implementation example, the present invention will be further described.
Heretofore described absorption property analysis test method is specially：
(1) Static Adsorption is tested
The IINMs and NINMs of the quality such as selection are added in corresponding test solution, are stood in constant temperature waters, test fluid
It is placed on the adsorbance that IINMs and NINMs is investigated after standing certain time respectively in 25 DEG C of water-bath, ion concentration after adsorption equilibrium
Determined with Atomic Absorption Spectrometer (AAS).If the test solution added is VmL, the initial concentration for matching somebody with somebody solution is C0, a timing
Between balance after its concentration be Ct, the quality of film is m, then the adsorbance Q for having film is：
(2) selective absorption is tested
Choose Li+、Mg2+For competitive Adsorption substrate, the aqueous solution of both the above compound is respectively configured.Take and configure in right amount
Solution be added in conical flask, be separately added into a piece of load weighted IINMs and NINMs, test fluid be placed on 25 DEG C of water-bath
It is middle to stand 8.0h respectively；After the completion of time of repose, IINMs and NINMs is taken out, each ion concentration Atomic absorption after adsorption equilibrium
Spectrometer (AAS) determines.
Embodiment 1
1. taking 4g Kynoar powder (PVDF) to be blended with 0.04g polyvinylpyrrolidones (PVP), 40mlN is added,
N '-dimethyl acetamide (DMAc) solution, mechanical agitation 12 hours under the conditions of 30 DEG C, constant static 24 hours of keeping temperature are de-
Bubble, PVDF basement membranes are formed by phase-inversion technologies.This pvdf membrane is put and preserved in deionized water, in case testing in next step.
2. PVDF basement membranes are immersed in 200ml deionized waters, 2g silver nitrates (AgNO is taken3) be added in above-mentioned solution,
60min is reacted under the conditions of xenon lamp, one layer of Ag nano particle is loaded in PVDF membrane surfaces.
3. 1.2g 12- crown ethers -4,0.3gLiCl, which are added in 50ml methanol solutions, forms ion imprinted polymer.By table
The PVDF basement membranes that face has Ag nano particles are immersed in above-mentioned solution, take 0.8mmol GDMAs (EGDMA)
, 10mg azodiisobutyronitriles (AIBN) be added in above-mentioned solution, sealed after logical nitrogen 20min, be placed in 60 degree of waters bath with thermostatic control and shake
Swing and 18h is reacted in device.
4. being taken the film out after reaction, with HCl eluted template ions, wherein HCl concentration is 0.5mol L-1, by Li+It is de-
Remove, then deionized water is washed until washing is into neutrality repeatedly, and ion blotting nano composite membrane (IINMs) is prepared,
It is same as above that the synthesis of non-trace nano composite membrane (NINMs) is added without lithium ion remaining step.
5. Static Adsorption is tested
10mg/L LiCl solution is prepared, solvent deionized water, takes a piece of trace and non-blotting membrane to be respectively put into 10mL's
In solution, after standing 8.0h at room temperature, remaining Li in solution is determined+Concentration.
As Fig. 2 results are shown：The adsorbance of blotting membrane is the adsorbance 16.9mg/g that 29.9mg/g is much larger than non-blotting membrane.
6. selective absorption is tested
Select Mg2+For competitive Adsorption substrate, Li is prepared+、Mg2+The aqueous solution of two kinds of materials, the concentration of every kind of substrate are all
10mg/L；Respectively take a piece of IINMs and NINMs to be put into 10mL solution, 8.0h is stood respectively in 25 DEG C of water-bath；Time of repose
After the completion of, each ion concentration is determined with Atomic Absorption Spectrometer (AAS).
As Fig. 3 results are shown：Blotting membrane is to Mg2+Separation factor reach 5.91, show blotting membrane to Li+There is special selection
Property evident characteristics.
Embodiment 2
1. 4g Kynoar powder (PVDF) is blended with 0.15g polyvinylpyrrolidones (PVP), and addition 25mlN, N '-
Dimethyl acetamide (DMAc) solution, mechanical agitation 12 hours under the conditions of 30 DEG C, the constant static deaeration in 24 hours of keeping temperature, leads to
Cross phase-inversion technologies and form PVDF basement membranes.This pvdf membrane is put and preserved in deionized water, in case testing in next step.
2. PVDF basement membranes are immersed in 200ml deionized waters, 1g silver nitrates (AgNO is taken3) be added in above-mentioned solution,
60min is reacted under the conditions of xenon lamp, one layer of Ag nano particle is loaded in PVDF membrane surfaces.
3. 0.6g12- crown ethers -4,0.3gLiCl are added in 50ml methanol solutions and form ion imprinted polymer.By surface
PVDF basement membranes with Ag nano particles are immersed in above-mentioned solution, take 0.4mmol GDMAs (EGDMA)
, 8mg azodiisobutyronitriles (AIBN) be added in above-mentioned solution, sealed after logical 10~20min of nitrogen, be placed in 60 degree of waters bath with thermostatic control
18h is reacted in oscillator.
4. being taken the film out after reaction, with HCl eluted template ions, wherein HCl concentration is 0.2mol L-1, by Li+It is de-
Remove, then deionized water is washed until washing is into neutrality repeatedly, and ion blotting nano composite membrane (IINMs) is prepared,
It is same as above that the synthesis of non-trace nano composite membrane (NINMs) is added without lithium ion remaining step.
5. Static Adsorption is tested
10mg/L LiCl solution is prepared, solvent deionized water, takes a piece of trace and non-blotting membrane to be respectively put into 10mL's
In solution, after standing 8.0h at room temperature, remaining Li in solution is determined+Concentration.
As Fig. 4 results are shown：The adsorbance of blotting membrane is the adsorbance 16.9mg/g that 27.8mg/g is much larger than non-blotting membrane.
6. selective absorption is tested
Select Mg2+For competitive Adsorption substrate, Li is prepared+、Mg2+The aqueous solution of two kinds of materials, the concentration of every kind of substrate are all
10mg/L；Respectively take a piece of IINMs and NINMs to be put into 10mL solution, 8.0h is stood respectively in 25 DEG C of water-bath；Time of repose
After the completion of, each ion concentration is determined with Atomic Absorption Spectrometer (AAS).
As Fig. 5 results are shown：Blotting membrane is to Mg2+Separation factor reach 5.2, show blotting membrane to Li+There is special selection
Property evident characteristics.
In Fig. 1, a is the scanning electron microscope diagram of PVDF basement membranes, and b is sweeping for PVDF membrane surface loaded Ag nano particles
Electron microscope picture is retouched, c is the scanning electron microscope diagram of the nano combined blotting membrane of ion；It can be clearly seen that, PVDF in a
Basement membrane is smooth porous surface structure, is loose structure in b while has the Ag nano particles significantly loaded, compound print in c
Mark film is the rougher loose structure that surface forms imprinted layer.
Claims (10)
1. a kind of synthetic method of lithium ion trace nano composite membrane, it is characterised in that step is as follows：
(1) Kynoar (PVDF) powder and polyvinylpyrrolidone (PVP) are added to N, N '-dimethyl acetamide
(DMAC) in, mechanical agitation under constant temperature, after the completion of mechanical agitation, the constant standing of keeping temperature, formed by phase-inversion technologies
PVDF basement membranes, this PVDF basement membrane is put and preserved in deionized water；
(2) the PVDF basement membranes that step (1) obtains are immersed in deionized water, add silver nitrate (AgNO3), it is mechanical at room temperature
Vibration, is put under xenon lamp and reacts；Obtaining surface has the PVDF basement membranes of Ag nano particles；
(3) 12- crown ethers -4 and lithium chloride are added in methanol, through A reacting forming ion imprinted polymers；Then by step
(2) the PVDF basement membranes that the surface obtained has Ag nano particles are immersed in the ion imprinted polymer, add dimethyl
Acrylic acid glycol ester (EGDMA) and azodiisobutyronitrile (AIBN), sealed after leading to inert gas, be placed in thermostatic control oscillator vibration
Middle carry out oscillating reactions；After reaction terminates, nano composite membrane is taken out；
(4) nano composite membrane obtained after step (3) is reacted is taken off with pickling, obtains lithium ion trace nano composite membrane.
A kind of 2. synthetic method of lithium ion trace nano composite membrane according to claim 1, it is characterised in that step
(1) in, the Kynoar, polyvinylpyrrolidone, the amount ratio of N, N '-dimethyl acetamide are 4g：(0.01~
0.04)g：25~40mL.
A kind of 3. synthetic method of lithium ion trace nano composite membrane according to claim 1, it is characterised in that step
(1) in, the constant temperature is 30 DEG C, and the churned mechanically time is 12h；The time of repose is 24h.
A kind of 4. synthetic method of lithium ion trace nano composite membrane according to claim 1, it is characterised in that step
(2) in, the mass ratio of Kynoar is 1-2 in the quality and step (1) of the silver nitrate：4, the xenon lamp lower reaction time is
60min。
A kind of 5. synthetic method of lithium ion trace nano composite membrane according to claim 1, it is characterised in that step
(3) in, used 12- crown ethers -4：Lithium chloride, GDMA, azodiisobutyronitrile, the dosage of methanol are
0.6~1.2g：0.3g, 0.4~0.8mmol, 8~10mg, 50mL；The inert gas is nitrogen.
A kind of 6. synthetic method of lithium ion trace nano composite membrane according to claim 1, it is characterised in that step
(3) in, the temperature of the A reactions is 25 DEG C, reaction time 2h.
A kind of 7. synthetic method of lithium ion trace nano composite membrane according to claim 1, it is characterised in that step
(3) in, in the thermostatic control oscillator vibration, the temperature of oscillating reactions is 60 DEG C, and the time of reaction is 18h.
A kind of 8. synthetic method of lithium ion trace nano composite membrane according to claim 1, it is characterised in that step
(4) in, described acid is HCl, concentration 0.2-0.5molL-1。
9. a kind of lithium ion trace nano composite membrane, it is characterised in that be by any one claim described in claim 1-8
What the preparation method was worth.
10. a kind of lithium ion trace nano composite membrane described in claim 9 to be used for the purposes for adsorbing lithium ion.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108328804A (en) * | 2018-04-13 | 2018-07-27 | 湖南科技大学 | A kind of processing method of platiniferous waste water |
| CN109438619A (en) * | 2018-09-28 | 2019-03-08 | 昆明理工大学 | It is a kind of using α-methacrylic acid as the preparation method and application of the hexavalent chromium trace composite membrane of function monomer |
| CN109731559A (en) * | 2019-03-21 | 2019-05-10 | 吉林师范大学 | Enrofloxacin HCL in trace film preparation and selective enumeration method water based on Surface enhanced Raman scattering |
| CN110078873A (en) * | 2019-04-20 | 2019-08-02 | 太原理工大学 | A kind of preparation method of magnetism carbon-based lithium ion imprinted material |
| CN112394053A (en) * | 2019-08-16 | 2021-02-23 | 吉林师范大学 | Preparation method of ultrasensitive SERS flexible composite membrane and application of ultrasensitive SERS flexible composite membrane in detection of enrofloxacin hydrochloride in water body |
| CN113509913A (en) * | 2021-04-21 | 2021-10-19 | 东北电力大学 | Preparation method and application of lithium ion imprinting nano composite membrane with high magnetism, high adsorption amount and high selectivity |
| CN113522061A (en) * | 2021-07-21 | 2021-10-22 | 昆明理工大学 | Preparation method of high-adsorption-capacity lithium ion imprinting nano composite membrane |
| 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 (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108328804A (en) * | 2018-04-13 | 2018-07-27 | 湖南科技大学 | A kind of processing method of platiniferous waste water |
| CN109438619A (en) * | 2018-09-28 | 2019-03-08 | 昆明理工大学 | It is a kind of using α-methacrylic acid as the preparation method and application of the hexavalent chromium trace composite membrane of function monomer |
| CN109731559A (en) * | 2019-03-21 | 2019-05-10 | 吉林师范大学 | Enrofloxacin HCL in trace film preparation and selective enumeration method water based on Surface enhanced Raman scattering |
| CN110078873A (en) * | 2019-04-20 | 2019-08-02 | 太原理工大学 | A kind of preparation method of magnetism carbon-based lithium ion imprinted material |
| CN112394053A (en) * | 2019-08-16 | 2021-02-23 | 吉林师范大学 | Preparation method of ultrasensitive SERS flexible composite membrane and application of ultrasensitive SERS flexible composite membrane in detection of enrofloxacin hydrochloride in water body |
| CN113509913A (en) * | 2021-04-21 | 2021-10-19 | 东北电力大学 | Preparation method and application of lithium ion imprinting nano composite membrane with high magnetism, high adsorption amount and high selectivity |
| CN113522061A (en) * | 2021-07-21 | 2021-10-22 | 昆明理工大学 | Preparation method of high-adsorption-capacity lithium ion imprinting nano composite membrane |
| 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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