KR20170030333A - Method for purification and solvent exchanging of conductive polymer solution, and conductive polymer film using thereby - Google Patents
Method for purification and solvent exchanging of conductive polymer solution, and conductive polymer film using thereby Download PDFInfo
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- 229920001940 conductive polymer Polymers 0.000 title claims abstract description 153
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- 238000000746 purification Methods 0.000 title claims description 43
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- 239000011148 porous material Substances 0.000 claims description 7
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- 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
- C08G61/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G61/12—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule
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- 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
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
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- 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
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/70—Post-treatment
- C08G2261/71—Purification
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Abstract
More particularly, the present invention relates to a method of purifying a conductive polymer solution and a method of replacing the conductive polymer solution by conducting a conductive polymer solution through a filtration membrane to remove impurities and a conductive low molecular weight in water and a solution, A conductive polymer solution for the purpose of improving the electrical characteristics of the conductive polymer solution and enhancing the coating property of the conductive polymer solution by removing impurities and conductive low molecular weight that deteriorate the conductivity and purifying the polymer solution and replacing the solvent And a conductive polymer film produced by using the same.
Description
BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a method of purifying a conductive polymer solution and a method of replacing a solvent, and more particularly, to a method of removing conductive impurities from an aqueous conductive polymer solution and replacing the conductive polymer solution with an organic solvent, A method of purifying a polymer solution and a method of replacing a solvent, and a conductive polymer film produced using the same.
Conductive polymers such as polyaniline, polythiophene, polypyrrole, polyphenylene vinylene, and polyacetylene have excellent stability and electrical conductivity, but the dispersibility and solubility of the solvent Is limited to applications in a wide variety of fields. Generally, the above-mentioned conductive polymer is prepared by including an anionic polymer such as a polymer sulfonic acid or a polymeric carboxylic acid in order to impart dispersibility to a solvent.
Particularly, the most widely known conductive polymer is poly (3,4-ethylenedioxythiophene): polystyrenesulfonic acid (PEDOT: PSS), which is a monomer such as 3,4-ethylenedioxythiophene, Sulfonic acid (polystyrene sulfonate) and a polymerization oxidant in an aqueous solvent. As described above, when a stabilizer or the like is added to impart dispersibility, an insulative material exists in the conductive polymer solution, which is an obstacle to enhancement of electrical conductivity.
In addition, when the conductive polymer solution prepared in an aqueous solvent is coated on a substrate such as glass, polymer or the like, wettability with the substrate is low, which makes it difficult to coat the conductive polymer solution. In order to overcome such disadvantages, a method of coating a surface of a substrate on which a conductive polymer is to be coated with a conductive polymer by ozone or corona treatment, coating the conductive polymer, or mixing the aqueous conductive polymer solution with an organic solvent to impart coating properties Lt; / RTI > However, the water-based conductive polymer may not be stably dispersed in an organic solvent and may be condensed, and there is a problem that purity and conductivity are lowered by using a mixed solvent.
In addition, materials in which conductive polymers are used, for example, antistatic films and electrode materials, are mostly water-sensitive materials, and when the water-based conductive polymer is used in the above materials, the stability is lowered, There was a problem.
In this connection, Korean Patent Registration No. 10-1014923 (entitled " Organic Solvent-Dispersing Thiophene Conducting Polymer Complex and Conductive Polymer Dispersion ", hereinafter referred to as Prior Art 1) A conductive polymer-ionic liquid composite having hydrophilicity is prepared by polymerizing an ionic liquid having a hydrophilic anion and polymerizing the thiophene-based conductive polymer as a dispersion stabilizer, and then the hydrophilic anion contained therein is exchanged with a hydrophobic anion Dispersing it in an organic solvent to prepare an organic solvent-dispersible conductive polymer-ionic liquid composite, thereby producing a conductive polymer dispersion.
In the prior art 1, in order to provide a conductive polymer which is stably dispersed in an organic solvent, an organic solvent-dispersible conductive polymer-ionic liquid composite is prepared through a chemical reaction in which a hydrophilic anion contained in an aqueous conductive polymer is replaced with a hydrophobic anion . However, such a method has a problem in that it is limited in improving the electrical conductivity as the purity is lowered by containing an excessive amount of components other than the conductive polymer in the organic solvent-dispersible conductive polymer solution.
Accordingly, the present invention provides a method for preparing a conductive polymer solution having excellent electrical conductivity and coating property by solving the problems of the prior art through a method of purifying and solvent-replacing a conductive polymer solution through a filtration membrane.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory and are not intended to limit the invention to the precise form disclosed. There will be.
SUMMARY OF THE INVENTION The present invention, which is directed to solve the problems of the prior art described above, includes a step of preparing a first solution comprising a first solvent, a conductive polymer and a stabilizer, initiating purification and solvent replacement by passing a first solution through a filtration membrane, The first solvent is removed while the first solution is passed through the filtration membrane, and the second solvent is gradually added to the second solvent, and the stabilizer is removed together with the first solvent through the filtration membrane to thereby purify the conductive polymer solution And a method for purifying a conductive polymer solution and a method for replacing a solvent.
The first solvent of the present invention is an aqueous solvent including water or water, and the conductive polymer is at least one polymer selected from the group consisting of polythiophene, poly (3,4-ethylenedioxythiophene), polypyrrole and polyaniline Or a copolymer thereof, and the second solvent includes one kind selected from the group consisting of an alcohol solvent, a glycol solvent, a polyol solvent, an ether solvent, a ketone solvent, a sulfoxide solvent and an amide solvent Solvent or a mixed solvent of two or more kinds.
The conductive polymer solution according to the present invention can be purified and the solvent replacement method can provide a conductive polymer solution having excellent electrical conductivity by removing the non-conductive material and the low molecular weight present in the conductive polymer solution by a simple process of passing through the filtration membrane. The present invention also has a second effect that can be easily applied to various fields by enhancing the coating property of the conductive polymer solution by simultaneously performing purification and solvent replacement of the conductive polymer solution. In addition, the purification and solvent replacement method of the conductive polymer solution according to the present invention can be economically effected in that the mass production is easy by a simple process and the manufacturing cost is reduced.
With respect to the first effect, the conductive polymer solution is recovered by passing the conductive polymer solution through the filtration membrane, and the free ion dissolved therein, the stabilizer that provides dispersibility, and the unreacted monomer that has not been recovered after preparation of the conductive polymer Lt; RTI ID = 0.0 > conductivity < / RTI > can be improved. Further, by reducing the molecular weight distribution of the conductive polymer through the filtration process, it is possible to produce a conductive polymer film of uniform physical properties.
With respect to the second effect, it is possible to improve the coating property on various substrates including glass and polymer by removing water contained in the conductive polymer solution and gradually adding a hydrophilic organic solvent to replace the solvent of the conductive polymer solution Electrode materials, antistatic films, and the like.
It should be understood that the effects of the present invention are not limited to the above effects and include all effects that can be deduced from the detailed description of the present invention or the configuration of the invention described in the claims.
1 is a flow chart showing one embodiment of a purification method and a solvent replacement method of a conductive polymer solution according to the present invention.
2 is a schematic view showing an operation of purification and solvent replacement of a conductive polymer solution according to an embodiment of the present invention.
3 is a photograph showing the contact angle measurement result of the conductive polymer solution according to an embodiment of the present invention.
4 is a photograph showing a contact angle measurement result of a conductive polymer solution according to the prior art.
FIG. 5 is a SEM photograph of a film prepared using a conductive polymer solution according to an embodiment of the present invention.
6 is a SEM photograph of a film prepared using a conductive polymer solution according to the prior art.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described with reference to the accompanying drawings. The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. In order to clearly illustrate the present invention, parts not related to the description are omitted, and similar parts are denoted by like reference characters throughout the specification.
Throughout the specification, when a part is referred to as being "connected" (connected, connected, coupled) with another part, it is not only the case where it is "directly connected" "Is included. Also, when an element is referred to as "comprising ", it means that it can include other elements, not excluding other elements unless specifically stated otherwise.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise. In this specification, the terms "comprises" or "having" and the like refer to the presence of stated features, integers, steps, operations, elements, components, or combinations thereof, But do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, or combinations thereof.
In the present specification, it is specified that the conductive polymer includes both doped and undoped conductive polymers.
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. 1 is a flow chart illustrating purification and solvent replacement of a conductive polymer solution according to an embodiment of the present invention. The present invention relates to a method for purifying a conductive polymer solution and a method for replacing a solvent, comprising the steps of: i) preparing a first solution comprising a first solvent, a conductive polymer and a stabilizer; ii) passing the first solution through a filtration membrane, And iii) passing the first solution through the filtration membrane to remove the first solvent and the stabilizer, while gradually adding the second solvent and replacing the second solvent with the second solvent. Hereinafter, the present invention will be described in detail by the above-described method for each manufacturing step.
In step i) of the present invention, the first solvent can be aqueous-based, including water or water, and the conductive polymer is selected from the group consisting of polythiophene, poly (3,4-ethylenedioxythiophene), polypyrrole and polyaniline One or more polymers selected therefrom, or copolymers thereof. In addition, the conductive polymer may be a conductive polymer combined with a stabilizer that provides dispersibility. For example, poly (3,4-ethylenedioxythiophene): polystyrene sulfonic acid (PEDOT: PSS), polypyrrole: polystyrene sulfonic acid (PP: PSS), polyaniline: polystyrene sulfonic acid (PANI: PSS) , 4-ethylenedioxythiophene): polyacrylic acid (PEDOT: PAA), and copolymers thereof may also be possible. In addition, the stabilizer may be an anionic compound including a sulfonic acid or a carboxylic acid, and may be tetrafluoroborate, hexafluorophosphate, or the like. In addition, the stabilizer may be an anionic polymer such as polyacrylic acid, polymethacrylic acid, polystyrenesulfonic acid, polyvinylsulfonic acid, or a copolymer thereof. In addition, the first solution may contain potassium ions, sulfate ions, ammonium ions, etc. formed by dissolving unreacted monomers that have not been removed after production of the conductive polymer, additives used in production, and surplus stabilizers. As described above, the substance contained in the first solution except for the conductive polymer lowers the purity of the conductive polymer solution and also contains an insoluble substance, which causes deterioration of the electrical conductivity, and therefore, a process for purifying the conductive polymer solution is required .
Step ii) of the present invention is a step of passing the first solution through the filtration membrane in order to remove the above-mentioned impurities and to start the substitution of the solvent. In the present invention, the filtration membrane may be provided with pores having a size of 0.001 to 1 μm, and the fraction molecular weight may be 1000 to 1,000,000 g / mol. It should be noted that the range may be a property of a filtration membrane preferable for recovering the conductive polymer while effectively removing impurities contained in the conductive polymer solution, but is not limited thereto. However, if a filtration membrane having a pore size exceeding 1 m is used, a problem may occur that the conductive polymer is passed through. When the pore size is less than 0.001 탆, impurities may not be effectively removed, There is a problem that the efficiency of the process is deteriorated due to an increase in the time. In the present invention, the fractional molecular weight is specifically determined by partially removing the conductive polymer having a relatively small molecular weight, which is less than the lower limit of the cut-off molecular weight (1,000 g / mol), thereby reducing the molecular weight distribution of the conductive polymer. By reducing the molecular weight distribution of the conductive polymer, the conductive polymer material having uniform physical properties can be produced and the conductivity can be expected to be improved. Also, when a flexible material is prepared using a conductive polymer solution, a low molecular weight material may have a problem of deteriorating the flexibility of the film. In addition, when the cutoff molecular weight of the filtration membrane exceeds 1,000,000 g / mol, not only the low molecular weight conductive polymer but also the high molecular weight conductive polymer can be discharged together with the waste solvent.
Next, step iii) of the present invention is a step of removing the first solvent, the impurities dissolved in the first solution, and the conductive polymer corresponding to the lower limit of the cut-off molecular weight, and gradually adding the second solvent to replace the solvent. In the present invention, the second solvent may be at least one solvent selected from the group consisting of an alcohol solvent, a glycol solvent, a polyol solvent, an ether solvent, a ketone solvent, a sulfoxide solvent and an amide solvent, Solvent, but is not limited thereto. However, hydrophilic organic solvents such as methanol, ethanol, propanol, butanol, N-dimethylpyrrolidone, acetone and the like are included in order to improve coating property and dispersion stability. In step iii) of the present invention, a mixed solvent of a second solvent and a first solvent may be gradually added to perform purification and solvent replacement. When purification and solvent replacement are carried out in the above-described embodiment, it may be preferable to gradually increase the proportion of the second solvent in the mixed solvent and to remove the first solvent.
Also, in the present invention, steps ii) and iii) may be performed at -20 to 150 ° C, but are not limited thereto. It may be desirable to perform the temperature at a lower temperature in consideration of the boiling point of the first solvent and the second solvent. However, if the temperature is lower than -20 ° C, the process efficiency may be lowered. If the temperature is higher than 100 ° C, excessive vapor may be formed due to evaporation of the solvent, which may cause safety problems. Resulting in deterioration of electrical characteristics. Also, step ii) and step iii) may be performed in a pressure range of 0.0001 to 10 bar (1 bar = 1000 kPa). When the purification and solvent replacement process is performed under pressure or reduced pressure, the process time can be shortened and the purification efficiency can be improved. However, if the upper limit of the pressure range (10 bar) is exceeded, solids may accumulate on the surface of the filtration membrane, resulting in a reduction in purification efficiency and a problem that the durability of the filtration membrane is deteriorated.
In addition, step iii) of the present invention may be performed until 100 parts by weight of the total solution becomes 99 parts by weight or more of the second solvent. When the content of the second solvent after the purification and the solvent substitution is less than 5 parts by weight, there is a problem that the effect of improving the coating property of the conductive polymer solution is insufficient. In addition, the concentration of the solid content in the first solution when the tablet and the solvent are substituted according to the present invention may be 0.1 to 50 wt% from the viewpoint of process efficiency. When the solid content is less than 0.1 wt%, the solid content is insufficient and the refining process may be difficult. When the solid content is more than 50 wt%, the solid content may accumulate in the filtration film and the process efficiency may be lowered.
Further, the purification and solvent replacement method of the present invention can be characterized by satisfying the following formula (1).
[Equation 1] P2 / P1? 0.7
In the formula (1), P1 represents the contact angle of the conductive polymer solution (the conductive polymer solution before the step of substituting the solvent) not subjected to the solvent substitution step, P2 represents the contact angle of the conductive polymer Means the contact angle of the solution. This means that it is possible to improve the wettability of the conductive polymer solution on the substrate through the purification and solvent replacement method according to the present invention, thereby facilitating the production of the film through the coating method.
Further, the purification and solvent substitution method of the present invention can be characterized by satisfying the following formula (2).
&Quot; (2) " S2 / S1 > = 1.2
In the formula (2), S 1 means the electric conductivity of the film prepared using the conductive polymer solution (the conductive polymer solution before the purification and solvent substitution step) not subjected to the purification and solvent replacement step, and S 2 means the electric conductivity Refers to the electrical conductivity of a film produced using a conductive polymer solution that has undergone a displacement process. This may mean that the electrical conductivity of the conductive polymer solution can be improved through the purification and solvent replacement method according to the present invention.
Next, referring to FIG. 2, a purification and solvent replacement system of a conductive polymer solution according to an embodiment of the present invention will be described. The purification and solvent replacement of the conductive polymer solution according to the present invention can be performed using any one of a microfiltration apparatus, an ultrafiltration apparatus, a reverse osmosis or ultrafiltration apparatus, a dialysis apparatus, and a vacuum filtration apparatus, It is also possible to use a filtration device provided with a hollow fiber type module, a spiral type module, a tubular type module, a flat type module, and the like, but not limited thereto. In addition, purification and solvent replacement may be performed using either a pressure-resistant driving method in which a target solution to be replaced with a solvent flows in the film and an external pressure driving method in which the solution is flowed from the outside of the film. FIG. 2 is a view showing one embodiment of the present invention in which a conductive polymer solution is purified and solvent-substituted using a filtration apparatus using a hollow fiber module and using an external pressure type permeation method. When the conductive polymer solution is introduced into the
In addition, a conductive polymer film, an electrode (transparent electrode), an antistatic film, an electromagnetic wave shielding film, and a solid capacitor are manufactured using the conductive polymer solution prepared by the purification and solvent substitution method of the conductive polymer solution according to the present invention .
Hereinafter, the effects of the present invention will be described in more detail with reference to Examples and Experiments of the present invention.
[Example 1]
1. Purification and Solvent Replacement of Conductive Polymer Solutions
(For example, CLEVIOS PH1000 manufactured by Heraeus) was pressurized to 3 bar by using an ultrafilter device (PALL-XLAB 5) containing a filtration membrane having a pore size of 50 nm and filtration was performed. A purification and solvent replacement process was carried out while gradually adding isopropyl alcohol while performing the filtration process. The components other than PEDOT: PSS were removed through a purification and solvent replacement process, and a PEDOT: PSS solution having a solid concentration of 1.5 wt% was obtained.
2. Preparation of Conductive Polymer Film
5 wt% DMSO was added to the PEDOT: PSS solution prepared according to the above method, and the mixture was uniformly mixed. The mixture was applied to a glass substrate using a bar coater and dried at 120 ° C for 15 minutes to prepare a PEDOT: PSS film.
[Example 2]
The conductive polymer solution was purified under the same conditions as in Example 1, except that water was added instead of the alcohol-based solvent. Further, a conductive polymer film was produced under the same conditions as in the film production method of Example 1.
[Comparative Example 1]
A CLEVIOS PH1000 solution of Heraeus, which had not been subjected to purification and solvent replacement, was used as Comparative Example 1, and a conductive polymer film was prepared under the same conditions as in Example 1.
In order to evaluate the change of physical properties before and after the purification process of the conductive polymer and the solvent replacement process, the properties of the conductive polymer solution and the film according to Example 1, Example 2 and Comparative Example 1 were measured under the following conditions, Are shown in Tables 1, 2 and 3 to 6.
1. Viscosity measurement
Viscosity of the conductive polymer solution according to Example 1, Example 2 and Comparative Example 1 was measured at room temperature using a rotary viscometer (Brookfield DV-III).
2. Contact angle measurement
The contact angle was measured by dropping the conductive polymer solution according to Example 1 and Comparative Example 1 on a glass substrate using a contact angle meter (Phoenix of SEO Korea).
3. Film electrical conductivity measurement
The electrical conductivity of the conductive polymer film (thickness: 80 nm) according to Example 1 and Comparative Example 1 was measured at 25 캜 using an electrical conductivity meter (Loresta-GP MCP-T600 from Mitsubichi Chemical Corporation).
4. Liquid electrical conductivity measurement
The electrical conductivity of the conductive polymer solution according to Example 2 and Comparative Example 1 was measured at 25 캜 using an electric conductivity meter (CM-30R of TOADKK).
5. pH measurement
The pH of the conductive polymer solution according to Example 2 and Comparative Example 1 was measured at 25 DEG C using a digital pH meter (HM-30R of TOADKK).
Example 1
Comparative Example 1
Viscosity [cP]
14
194
Contact angle [°]
6
24
Film Electrical Conductivity [S / cm]
1,250
800
Referring to Table 1, it can be confirmed that the viscosity of the solution is lowered by performing the purification and solvent replacement process of the conductive polymer solution according to an embodiment of the present invention. This result can be attributed to the removal of the conductive low molecular weight component corresponding to the fraction molecular weight of the nonconductive material (PSS, etc.) and the filtration membrane in the conductive polymer solution. In addition, it can be confirmed that the electric conductivity of Example 1 was improved 1.5 times or more as compared with Comparative Example 1 for the same reason as described above. Referring to the photographs shown in Table 1, FIG. 3 and FIG. 4, it can be seen that the contact angle of the conductive polymer solution after the purification and solvent replacement process according to the present invention is lowered. The low contact angle means that the wettability with respect to the substrate is large, and it can be confirmed that when the conductive polymer solution is purified and the solvent is substituted by the method according to the present invention, the coating property to the substrate can be improved.
Example 2
Comparative Example 1
Viscosity [cP]
57
194
pH
2.4
2.0
Liquid electrical conductivity [mS]
0.71
2.97
Film Electrical Conductivity [S / cm]
1,270
800
Referring to Table 2, it can be confirmed that the viscosity of Example 2 is lower than that of Comparative Example 1, and the pH is increased. This is because the non-conductive material (PSS or the like) in the conductive polymer solution through the filtration membrane And the conductive low molecular weight corresponding to the fraction molecular weight of the impurities and the filtration membrane is removed. As a result of the measurement of the liquid electrical conductivity, it was confirmed that the liquid electroconductivity of the conductive polymer solution according to Example 2 was 0.71 mS / cm, and that of the conductive polymer solution according to Comparative Example 1 was 2.97 mS / cm. It can be concluded that a large amount of ionic substances in the solution of Example 2 is removed.
From the measurement of the pH and the measurement results of the liquid electroconductivity, it can be confirmed that the non-conductive material, various ionic substances and conductive low molecular weight substances can be effectively removed by the purification method according to the present invention. It was confirmed that the film electrical conductivity of Example 2 was improved by 1.5 times or more as compared with Comparative Example 1 as the materials for lowering the electrical conductivity of the conductive polymer film were removed.
In order to analyze the surface structure of the conductive polymer film according to Example 2 and Comparative Example 1, SEM measurement was performed. The results are shown in FIG. 5 and FIG. 6. Referring to FIG. 5, it can be seen that the conductive polymer film according to Example 2 has a conductive polymer having a uniform particle size distributed over the entire surface of the film. It can be seen that the conductive polymer film has non-uniform distribution of particles having a relatively large size distribution.
It will be understood by those skilled in the art that the foregoing description of the present invention is for illustrative purposes only and that those of ordinary skill in the art can readily understand that various changes and modifications may be made without departing from the spirit or essential characteristics of the present invention. will be. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive. For example, each component described as a single entity may be distributed and implemented, and components described as being distributed may also be implemented in a combined form.
The scope of the present invention is defined by the appended claims, and all changes or modifications derived from the meaning and scope of the claims and their equivalents should be construed as being included within the scope of the present invention.
100: hollow fiber module
110: filtration membrane
200: aquarium
10: Conductive polymer
11: High molecular weight conductive polymer
12: Low molecular weight conductive polymer
30: Additive
Claims (16)
i) preparing a first solution comprising a first solvent, a conductive polymer and a stabilizer;
ii) passing the first solution through a filtration membrane to initiate purification and solvent displacement;
iii) passing the first solution through the filtration membrane to remove the first solvent while slowly adding the second solvent and replacing the second solvent with the second solvent; Lt; / RTI >
Wherein the stabilizer is removed together with the first solvent through the filtration membrane to purify the conductive polymer solution.
Wherein the step iii) is repeated until 100 parts by weight of the total solution becomes 99 parts by weight or more of the second solvent.
Wherein the filtration membrane is provided with pores having a size of 0.001 to 1 mu m, and the purification and solvent replacement method of the conductive polymer solution.
Wherein the fractionated molecular weight of the filtration membrane is from 1000 to 1,000,000 g / mol.
Wherein the first solvent is an aqueous solvent containing water or water.
Wherein the conductive polymer comprises at least one polymer selected from the group consisting of polythiophene, poly (3,4-ethylenedioxythiophene), polypyrrole, and polyaniline, or a copolymer thereof. And a solvent substitution method.
The second solvent may be one kind of solvent selected from the group consisting of an alcohol type solvent, a glycol type solvent, a polyol type solvent, an ether type solvent, a ketone type solvent, a sulfoxide type type solvent and an amide type type solvent, Wherein the conductive polymer solution is purified and the solvent is replaced.
Wherein the step ii) and the step iii) are carried out at -20 to 150 ° C.
Wherein a pressure of 0.0001 to 10 bar is applied during the step ii) and the step iii).
And gradually adding a mixed solution of the first solvent and the second solvent between the step ii) and the step iii).
A method for purification and solvent replacement of a conductive polymer solution satisfying the following formula (1).
[Equation 1]
P2 / P1? 0.7
(In the above formula (1)
P1 represents the contact angle of the conductive polymer solution before performing the solvent substitution process,
And P2 is the contact angle of the conductive polymer solution solvent-substituted with the second solvent in the first solvent).
A method for purification and solvent replacement of a conductive polymer solution satisfying the following formula (2).
&Quot; (2) "
S2 / S1 > = 1.2
(In the above equation (2)
S1 is the electrical conductivity of the film prepared using the conductive polymer solution before the purification and solvent replacement process,
S2 is the electrical conductivity of the film prepared using the conductive polymer solution after purification and solvent replacement.)
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| KR20200106275A (en) * | 2019-03-04 | 2020-09-14 | 한국생산기술연구원 | Method for preparing conductive polymer dispersion with improved physical properties |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101014923B1 (en) | 2007-12-06 | 2011-02-15 | 광 석 서 | Organic solvent dispersible thiophene conductive polymer complex and conductive polymer dispersion |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101014923B1 (en) | 2007-12-06 | 2011-02-15 | 광 석 서 | Organic solvent dispersible thiophene conductive polymer complex and conductive polymer dispersion |
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| KR20200106275A (en) * | 2019-03-04 | 2020-09-14 | 한국생산기술연구원 | Method for preparing conductive polymer dispersion with improved physical properties |
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