CN110746600B - Ion rectifying device and preparation method thereof - Google Patents
Ion rectifying device and preparation method thereof Download PDFInfo
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- CN110746600B CN110746600B CN201910874257.2A CN201910874257A CN110746600B CN 110746600 B CN110746600 B CN 110746600B CN 201910874257 A CN201910874257 A CN 201910874257A CN 110746600 B CN110746600 B CN 110746600B
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- 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
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Abstract
The invention relates to an ion rectifying device and a preparation method thereof. The ion rectifying device comprises a polypyrrole/graphene oxide composite film, wherein the polypyrrole is distributed on the surface and between layers of one side of the polypyrrole/graphene oxide composite film, and carboxyl and hydroxyl functional groups are arranged on the surface and between layers of the polypyrrole/graphene oxide composite film. The ion rectifying device has the advantages of simple preparation process, low cost and high ion rectifying ratio, and can be further applied to the fields of ion directional transportation, salt difference power generation and the like.
Description
Technical Field
The invention relates to the field of biological ion channel bionics.
Background
In nature, various biological ion channels are present in organisms, and these biological ion channels are transmembrane proteins with special functions. Since ions in a living body cannot pass through a phospholipid bilayer but only through transmembrane proteins, biological ion channels play a crucial role in maintaining various vital activities of the living body such as material transport, energy exchange, and information transfer. An important feature of biological ion channels is the ability to direct the transport of ions preferentially from one side of the ion channel to the other, exhibiting ion rectifying properties.
By learning the properties and characteristics of the biological ion channel, the artificial ion rectifying device with the characteristics of the biological ion channel can be prepared by adopting various physical and chemical methods. However, most of the preparation methods are complex and high in cost, so that the artificial ion rectifying device with a simple and convenient preparation method and the preparation method thereof have important significance.
Disclosure of Invention
The inventors of the present invention have made extensive studies to solve the problems of the prior art, and as a result, have found that the ion rectifying device of the present invention is simple in operation and low in cost, thereby completing the present invention. The present invention includes the following configurations.
The invention provides an ion rectifying device which comprises a polypyrrole/graphene oxide composite film, wherein the polypyrrole is distributed on one side surface and among layers of the graphene oxide film, and carboxyl and hydroxyl functional groups are arranged on the surface and among layers of the polypyrrole/graphene oxide composite film.
Another aspect of the present invention provides a method for preparing a polypyrrole/graphene oxide composite film, which comprises the following steps:
preparing a graphene oxide film: stacking the graphene oxide nanosheets into a compact graphene oxide film by vacuum filtration;
the preparation process of the polypyrrole/graphene oxide composite film comprises the following steps: carrying out oxidative polymerization on pyrrole monomers on one side of the graphene oxide film prepared in the graphene oxide film preparation procedure by utilizing vapor deposition, so that polypyrrole is deposited on the surface of one side of the graphene oxide film and between layers;
construction of an ion rectifying device: construction of an ion rectifying device: and placing the polypyrrole/graphene oxide composite film in a double-chamber electrolytic cell, adding electrolyte and two electrodes, and electrically connecting to construct an ion rectifying device.
The ion rectifying device has an ion rectifying characteristic, wherein the ion rectifying characteristic is a characteristic that current values obtained under positive voltage and negative voltage with the same value are different in magnitude, and the rectifying characteristic is stronger when the difference of the current values is larger. The ion rectifying device of the present invention exhibits diode-like rectifying properties, which may be analyzed for the following reasons: one side of the polypyrrole/graphene oxide composite film, which is provided with polypyrrole, is a small hole end, the other side of the polypyrrole/graphene oxide composite film is a large hole end, and the surface of a pore channel is provided with negative charges and has selective permeability to cations. When a positive voltage is applied to the side film on which the polypyrrole is deposited, cations can easily pass through the pore channel due to the electrostatic effect to form an ion enrichment area, and the ion current is large; on the contrary, when negative voltage is applied to the side film deposited with polypyrrole, cations are not easy to pass through the pore channel to form an ion dissipation area, and the ion current is small
The ion rectifying device has the advantages of simple structure, high ion rectifying ratio and the like, and can be further applied to the fields of ion directional transportation, salt difference power generation and the like. The preparation method of the ion rectifying device has the advantages of simple process and low cost.
Drawings
Fig. 1 is an apparatus diagram of an ion rectifying device according to an embodiment of the present invention.
Fig. 2 is an environmental scanning electron microscope image of the surface of the polypyrrole/graphene oxide composite thin film prepared by one embodiment of the present invention.
Fig. 3 is an environmental scanning electron microscope image of a cross section of a polypyrrole/graphene oxide composite thin film prepared by an embodiment of the present invention.
Fig. 4 is a graph of static water contact angles of both sides of a graphene oxide thin film and a polypyrrole/graphene oxide composite thin film prepared according to an embodiment of the present invention.
FIG. 5 is a graph of current-voltage curves of an ion rectifying device prepared according to an embodiment of the present invention tested in 1mmol/L electrolyte.
Description of the reference numerals
KCl electrolyte solution, 2: polypyrrole/graphene oxide composite film, 3: Ag/AgCl electrode, 4: double-chamber electrolytic cell
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that the upper and lower limits of the range, and each intervening value therebetween, is specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control. Unless otherwise indicated, "%" is percent by weight.
[ ion rectifying device ]
The ion rectifying device comprises a polypyrrole/graphene oxide composite film, wherein the polypyrrole is distributed on one side surface and among layers of the graphene oxide film, and carboxyl and hydroxyl functional groups are arranged on the surface and among layers of the polypyrrole/graphene oxide composite film.
The distribution of polypyrrole on one side surface and between layers of the polypyrrole/graphene oxide composite film means that polypyrrole is present unevenly on one side surface and between layers of the polypyrrole/graphene oxide composite film. As one of the modes of the method, for example, the concentration of polypyrrole gradually decreases from the surface of the side where polypyrrole is present to the other side of the polypyrrole/graphene oxide composite film. In another embodiment, for example, when the concentration of polypyrrole on one surface is the maximum concentration, the concentration of polypyrrole between layers gradually decreases, and the concentration of polypyrrole decreases to zero at a position half the thickness of the polypyrrole/graphene oxide composite film.
The thickness of the polypyrrole/graphene oxide composite film contained in the ion rectifying device is 5-500 μm, preferably 5-200 μm, and more preferably 10-50 μm.
In the polypyrrole/graphene oxide composite film included in the ion rectifying device of the present invention, a carboxyl group and a hydroxyl group are present on the surface and between layers of the composite film. The carboxyl and hydroxyl functional groups are derived from graphene oxide. The graphene oxide is obtained by oxidizing graphene. In the oxidation process, the graphene is functionalized by carboxyl and hydroxyl groups so as to have carboxyl and hydroxyl functional groups.
The ion rectifying device of the present invention further includes an electrolytic cell, an electrolytic solution, two electrodes, and other components. The choice of the electrolytic cell, the electrolyte and the electrodes is not subject to any restrictions and can be selected by the person skilled in the art as desired.
The two electrodes are preferably Ag/AgCl electrodes.
Examples of the electrolyte include KCl solution and K2SO4The electrolyte solution is not particularly limited, but is preferably a KCl electrolyte solution having a concentration of 1 to 100mM, and more preferably a KCl electrolyte solution having a concentration of 5 to 50 mM.
As an embodiment of the ion rectifying device of the present invention, as shown in fig. 1, the ion rectifying device includes a polypyrrole/graphene oxide composite thin film 2, a double-chamber electrolytic cell 4, a KCl electrolyte solution 1, and two Ag/AgCl electrodes 3. Wherein the surface and the interlayer of the graphene oxide film have carboxyl and hydroxyl functional groups.
[ method for producing ion rectifying device ]
The preparation method of the ion rectifying device comprises the following steps:
preparing a graphene oxide film: stacking the graphene oxide nanosheets into a compact graphene oxide film by vacuum filtration;
the preparation process of the polypyrrole/graphene oxide composite film comprises the following steps: polymerizing pyrrole monomers on one side of the graphene oxide film prepared in the graphene oxide film preparation procedure by utilizing vapor deposition, so that polypyrrole is deposited on the surface of one side of the graphene oxide film and between layers;
construction of an ion rectifying device: and placing the polypyrrole/graphene oxide composite film in a double-chamber electrolytic cell, adding electrolyte and two electrodes, and electrically connecting to construct an ion rectifying device.
The thickness of the polypyrrole/graphene oxide composite film is about 5-500 μm.
As one embodiment of the method for manufacturing an ion rectifying device of the present invention, the following manufacturing method may be mentioned: carrying out ultrasonic treatment on the single-layer graphene oxide dispersion liquid, then using a water-phase nylon filter membrane as a substrate, carrying out suction filtration on the graphene oxide dispersion liquid by using a circulating water type vacuum pump to form a compact graphene oxide film stacked by graphene oxide sheets, and then volatilizing monomer pyrrole into gas by adopting a vapor deposition method to polymerize on the surface and between layers of the graphene oxide to form the polypyrrole/graphene oxide composite film. And then, placing the polypyrrole/graphene oxide composite film in the middle of a double-chamber electrolytic cell, adding a KCl electrolyte, and electrifying by using an Ag/AgCl electrode to form the ion rectifying device.
Examples
(1) And (3) characterizing the polypyrrole/graphene oxide composite film:
the microscopic morphology of the sample was observed using a scanning electron microscope environment Quanta FEG 250, FEI USA. The water contact angle of the film surface was measured using a POWEREACH JC2000D1 model contact angle meter.
(2) Testing the rectification characteristic:
the current-voltage properties of the samples were tested using a Keithley company 6487 pean meter, usa. The polypyrrole/graphene oxide composite film obtained in the example is placed in the middle of a double-chamber electrochemical cell, a potassium chloride solution with the concentration of 1mmol/L is filled in the double chambers of the electrochemical cell, 1 pair of silver/silver chloride electrodes are used for applying transmembrane voltage, one side of the polypyrrole is fixed as an anode, and an ion rectifying device is assembled. The ion current of the ion rectifying device at different voltages is recorded by using a picoammeter, and the device is shown as the figure 1.
Example 1
Taking 3mL of single-layer graphene oxide dispersion liquid with the concentration of 2mg/mL, carrying out ultrasonic treatment for 1 hour, then using a water-phase nylon filter membrane as a substrate, carrying out suction filtration on the graphene oxide dispersion liquid by using a circulating water type vacuum pump to obtain a compact graphene oxide film stacked by graphene oxide sheets, then volatilizing monomer pyrrole into gas by using a vapor deposition method, and polymerizing the gas on the surface and between layers of the graphene oxide to form the polypyrrole/graphene oxide film, wherein the vapor deposition time is 8 hours. And (3) placing the polypyrrole/graphene oxide film in the middle of a double-chamber electrolytic cell, adding a KCl electrolyte, and electrifying by using an Ag/AgCl electrode to obtain the ion rectifying device 1.
Fig. 2 is an environmental scanning electron microscope image of the surface of the polypyrrole/graphene oxide composite thin film obtained in example 1, and fig. 3 is an environmental scanning electron microscope image of the cross section of the polypyrrole/graphene oxide composite thin film obtained in example 1. As can be seen from fig. 2, the surface of the graphene oxide film is covered with a layer of polypyrrole, and as can be seen from fig. 3, the upper layer is polypyrrole/graphene oxide with a more densely-packed layered structure, and the lower layer is a graphene oxide film. Fig. 4 is a static water contact angle diagram of a graphene oxide film and a polypyrrole/graphene oxide composite film, where a in the diagram is an upper surface of the graphene oxide film, b in the diagram is a lower surface of the graphene oxide film, c in the diagram is a side of the polypyrrole/graphene oxide composite film on which the polypyrrole is deposited, and d in the diagram is a side of the polypyrrole/graphene oxide composite film on which the polypyrrole is not deposited, and it can be seen that a contact angle of the side on which the polypyrrole is deposited is significantly increased.
For the separation obtained in example 1The current-voltage curve obtained by testing the rectifying characteristics of the sub-rectifying device is shown in FIG. 5, the ion rectifying ratio I+2V/I-2VWas 2.1.
Example 2
Taking 2mL of single-layer graphene oxide dispersion liquid with the concentration of 2mg/mL, carrying out suction filtration to obtain a graphene oxide film, then carrying out gas-phase precipitation on polypyrrole for 8 hours to obtain a polypyrrole/graphene oxide composite film, placing the polypyrrole/graphene oxide composite film in the middle of a double-chamber electrolytic cell, adding KCl electrolyte, and electrifying by using an Ag/AgCl electrode to obtain the ion rectifying device 2.
Example 3
Taking 4mL of single-layer graphene oxide dispersion liquid with the concentration of 2mg/mL, carrying out suction filtration to obtain a graphene oxide film, then carrying out gas-phase precipitation on polypyrrole for 8 hours to obtain a polypyrrole/graphene oxide composite film, placing the polypyrrole/graphene oxide composite film in the middle of a double-chamber electrolytic cell, adding KCl electrolyte, and electrifying by using an Ag/AgCl electrode to obtain the ion rectifying device 3.
Example 4
Taking 3mL of single-layer graphene oxide dispersion liquid with the concentration of 2mg/mL, carrying out suction filtration to obtain a graphene oxide film, then carrying out gas-phase precipitation on polypyrrole for 4 hours to obtain a polypyrrole/graphene oxide composite film, placing the polypyrrole/graphene oxide composite film in the middle of a double-chamber electrolytic cell, adding KCl electrolyte, and electrifying by using an Ag/AgCl electrode to obtain the ion rectifying device 4.
Example 5
Taking 3mL of single-layer graphene oxide dispersion liquid with the concentration of 2mg/mL, carrying out suction filtration to obtain a graphene oxide film, then carrying out vapor deposition on polypyrrole for 6h to obtain a polypyrrole/graphene oxide composite film, placing the polypyrrole/graphene oxide composite film in the middle of a double-chamber electrolytic cell, adding KCl electrolyte, and electrifying by using an Ag/AgCl electrode to obtain the ion rectifying device 5.
Example 6
Taking 3mL of single-layer graphene oxide dispersion liquid with the concentration of 2mg/mL, carrying out suction filtration to obtain a graphene oxide film, then carrying out vapor deposition on polypyrrole for 10 hours to obtain a polypyrrole/graphene oxide composite film, placing the polypyrrole/graphene oxide composite film in the middle of a double-chamber electrolytic cell, adding KCl electrolyte, and electrifying by using an Ag/AgCl electrode to obtain the ion rectifying device 6.
Example 7
Taking 3mL of single-layer graphene oxide dispersion liquid with the concentration of 2mg/mL, carrying out suction filtration to obtain a graphene oxide film, then carrying out vapor deposition on polypyrrole for 12h to obtain a polypyrrole/graphene oxide composite film, placing the polypyrrole/graphene oxide composite film in the middle of a double-chamber electrolytic cell, adding KCl electrolyte, and electrifying by using an Ag/AgCl electrode to obtain the ion rectifying device 7.
Example 8
Taking 3mL of single-layer graphene oxide dispersion liquid with the concentration of 2mg/mL, carrying out suction filtration to obtain a graphene oxide film, then carrying out vapor deposition on polypyrrole for 24 hours to obtain a polypyrrole/graphene oxide composite film, placing the polypyrrole/graphene oxide composite film in the middle of a double-chamber electrolytic cell, adding KCl electrolyte, and electrifying by using an Ag/AgCl electrode to obtain the ion rectifying device 8.
And performing morphology characterization and rectification characteristic test on the ion rectification devices 2 to 8 obtained in the embodiments 2 to 8. The appearance characterization shows that the surface of the graphene oxide film is covered with a layer of polypyrrole, the upper layer is polypyrrole/graphene oxide with a layered structure which is more tightly stacked, and the lower layer is a graphene oxide film.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
Claims (9)
1. An ion rectifying device comprises a polypyrrole/graphene oxide composite film, wherein the concentration of polypyrrole is gradually reduced from the surface of one side where polypyrrole exists to the other side of the polypyrrole/graphene oxide composite film, and carboxyl and hydroxyl functional groups are arranged on the surface and between layers of the polypyrrole/graphene oxide composite film.
2. An ion rectifying device comprises a polypyrrole/graphene oxide composite film, wherein in the polypyrrole/graphene oxide composite film, when the concentration of polypyrrole on the surface of one side of the graphene oxide film is the maximum concentration, the concentration of polypyrrole between layers of the graphene oxide film is gradually reduced, the concentration of polypyrrole is reduced to zero at a position half of the thickness of the polypyrrole/graphene oxide composite film, and carboxyl and hydroxyl functional groups are arranged on the surface and between layers of the polypyrrole/graphene oxide composite film.
3. The ion rectifying device according to claim 1 or 2, wherein the thickness of the polypyrrole/graphene oxide composite thin film is 5 to 500 μm.
4. The ion rectifying device of claim 1 or 2, further comprising an electrolytic cell, an electrolyte, and two electrodes.
5. The ion rectifying device of claim 4, wherein the two electrodes are Ag/AgCl electrodes.
6. The ion rectifying device according to claim 4, wherein the electrolyte is a KCl electrolyte having a concentration of 1 to 100 mM.
7. A method for manufacturing an ion rectifying device according to any one of claims 1 to 6, comprising the steps of:
preparing a graphene oxide film: stacking the graphene oxide nanosheets into a compact graphene oxide film by vacuum filtration;
the preparation process of the polypyrrole/graphene oxide composite film comprises the following steps: polymerizing pyrrole monomers on one side of the graphene oxide film prepared in the graphene oxide film preparation procedure by utilizing vapor deposition, so that polypyrrole is deposited on the surface of one side of the graphene oxide film and between layers;
construction of an ion rectifying device: and placing the polypyrrole/graphene oxide composite film in a double-chamber electrolytic cell, adding electrolyte and two electrodes, and electrically connecting to construct an ion rectifying device.
8. The method of claim 7, wherein the two electrodes are Ag/AgCl electrodes.
9. The method for manufacturing an ion rectifying device according to claim 7 or 8, wherein the electrolyte is a KCl electrolyte with a concentration of 1-100 mM.
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