KR20170001340A - Electrically Conductive Polyetherimide Nanofibers and Method for Manufacturing the same - Google Patents
Electrically Conductive Polyetherimide Nanofibers and Method for Manufacturing the same Download PDFInfo
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- KR20170001340A KR20170001340A KR1020150091181A KR20150091181A KR20170001340A KR 20170001340 A KR20170001340 A KR 20170001340A KR 1020150091181 A KR1020150091181 A KR 1020150091181A KR 20150091181 A KR20150091181 A KR 20150091181A KR 20170001340 A KR20170001340 A KR 20170001340A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/74—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polycondensates of cyclic compounds, e.g. polyimides, polybenzimidazoles
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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Abstract
Description
More particularly, the present invention relates to an electrically conductive polyetherimide nanofiber having excellent physical properties such as heat resistance, flame retardancy, shape stability, high temperature stiffness, chemical resistance and light weight, And a manufacturing method thereof.
Nanofibers have a large specific surface area in terms of structure and can be easily applied to textile materials and can be easily modified and functionalized. have. Methods for fabricating nanofibers include template-directed methods, solvothermal synthesis, self-assembly, electrospinning, and the like. Especially, electrospinning has been developed for over 100 years and has been widely used industrially until now, and it is possible to easily obtain a large amount of long fibers of various thicknesses ranging from several tens of nanometers to several micrometers with various materials at low cost. Therefore, many processes (synthesis and purification) in the process are required, and the utility value of the nanowires is being increased industrially compared to nanowires, which are difficult to handle due to their short length. The main materials constituting nanofibers are biodegradable polymers, thermoplastic polymers, conducting polymers, polymer / conductive filler composites, and ceramics. They are applied in a wide variety of fields such as energy-related devices and electronic devices, tissue engineering, drug patches, filters, chemical sensors, and surface engineering.
Conventionally, conductive polymers have mostly been used in thin film devices, but recently they have been applied to devices such as organic transistors made of nanofibers. In addition, a conductive nanomaterial such as a metal nanoparticle or a carbon nanotube is embedded in a fiber to form composites, which has attracted much attention as a composite fiber which is mechanically stable and exhibits electrical characteristics. These conductive nanofibers have the potential to develop new types of patterned devices out of the traditional thin film device frameworks and can be used for both high performance flexible stretchable devices and smart electronic textiles) have been studied.
The electrospinning technique of a conductive polymer or a mixture of a conductive polymer and a general-purpose polymer can be applied to future advanced nano-optical and electronic devices. Conductive polymer nanofibers with a diameter of 100 nm or less are required for this purpose. Polyaniline nanofiber having a diameter of 139 nm was prepared from electrospinning of a 20 wt% polyaniline / sulfuric acid aqueous solution using water as a coagulating liquid, and the conductivity of the nanofiber was found to be about 0.1 S / cm. Polymer nanofibers containing carbon nanotubes were also prepared to increase the conductivity of organic fibers. Studies on the production of conductive nanofibers in which polypyrrole is uniformly coated at a thickness of 20 to 25 nm by immersing polyacrylonitrile nanofibers in an aqueous solution of a pyrrole monomer have been carried out. Conductive polymer absorbs visible light and exhibits electrochromic characteristics that change its absorbance. Therefore, conductive nanofiber coating is used for functional window to control the amount of sunlight to control the color of window, electromagnetic shielding and antistatic coating Is expected.
Conductive polymer such as polyaniline or polypyrrole can be used as an electrode of a biochemical sensor for detecting various gases in the atmosphere. Increasing the effective area of the conductive polymer in such a sensor is very important for increasing the sensitivity of the sensor. Since most of the conductive polymers are very low in solubility, electrospinning technology can be well utilized in the production of conductive polymer nanofibres for increased surface area. When fabricating sensor devices with nanofibers, signal response time and surface electrical properties can be improved without degrading detection sensitivity.
Korean Patent No. 1079775 discloses a method for producing electrically conductive nanofibers that can reduce the time and cost required for the production of electrically conductive fibers, reduce cracking due to flexibility, and maintain electrical conductivity as high as that of metals. Discloses a method for producing electrically conductive nanofibers by electroless plating followed by spinning. Korean Patent Laid-Open Publication No. 2011-0109693 discloses a method for manufacturing an electrospinning liquid comprising the steps of: preparing an electrospinning liquid containing a fiber-forming polymer and an oxidizing agent serving as a polymerization initiator; Electrospinning the electrospinning liquid to produce a nanofiber having a diameter of 10 nm to 5 μm; And a step of coating the nanofibers or fibers obtained by processing the nanofibers with an electrically conductive polymer monomer by gas phase polymerization.
However, in order to utilize nanofibers for various purposes, it is necessary to develop nanofibers having improved electrical conductivity, heat resistance, flame retardancy, shape stability, high temperature stiffness and chemical resistance.
Polyetherimide polymers can be used to improve the physical properties of nanofibers. Polyetherimide polymers have excellent physical properties as a heat-resistant polymer due to rigid aromatic backbone, but have poor moldability and processability.
Conventional polyetherimide polymers are prepared by dissolving a dianhydride component and a diamine component in a solvent to form a polyamic acid as a precursor, preparing a polyamic acid film and a fiber, and heating the mixture to a high temperature, . The production of polyetherimide moldings in which nanomaterials are dispersed is mainly carried out by synthesizing polyamic acid in the presence of nanomaterials, molding the same, and then imidizing at high temperatures.
However, in the process of dispersing nanomaterials, the physical properties of the final molded product are deteriorated by severe aggregation phenomenon, and it is difficult to secure sufficient electrical conductivity. When a large amount of nanomaterials is added, the specific gravity is inevitably increased, There is a process limit that significantly increases.
As a result of intensive efforts to solve the above problems, the present inventors have found that when a colloidal-type spinning liquid prepared by mixing a carbon nanomaterial dispersion and a polyetherimide polymer solution having a multi-polar group formed therein is electrospun, heat resistance, flame retardancy, , High-temperature stiffness, chemical resistance, light weight, and the like, thereby completing the present invention.
An object of the present invention is to provide an electroconductive nanofiber excellent in physical properties such as heat resistance, flame retardancy, shape stability, high temperature stiffness, chemical resistance and light weight, and a method for producing the same.
In order to achieve the above object, the present invention provides a method for producing a carbon nanomaterial, comprising the steps of: (a) treating a carbon nanomaterial to an acid solution to prepare a carbon nanomaterial having a carboxylic acid group; (b) dispersing the carbon nanomaterial having the carboxylic acid group in a solvent, and then treating toluene diisocyanate or methylene diphenyl diisocyanate to prepare a carbon nanomaterial having an isocyanate group; (c) dispersing the carbon nanomaterial having the isocyanate group in a solvent, and then adding and mixing aminohydroxymethylpyridine to prepare a carbon nanomaterial dispersion having a multi-polar group; (d) centrifuging and filtering the dispersion of carbon nanomaterials formed with multiple polar groups to remove the precipitate; (e) dissolving the polyetherimide polymer in a solvent to prepare a polyetherimide polymer solution; (f) preparing a colloidal solution by mixing the carbon nanomaterial dispersion with the polyelectrolyte polymer solution having the filtered multipolar groups formed therein; And (g) electrospunning the spinning solution to prepare nanofibers. The present invention also provides a method for producing electroconductive polyetherimide nanofibers.
In the present invention, the carbon nanomaterial is selected from the group consisting of a single-walled carbon nanotube, a multi-walled carbon nanotube, and a carbon nanofiber.
In the present invention, the solvent is selected from the group consisting of methylpyrrolidone, dimethylacetamide, dimethylformamide and dimethylsulfoxide.
In the present invention, the nanofiber is characterized in that 30 to 100 parts by weight of the carbon nanomaterial having the multipolar group is dispersed in 100 parts by weight of the polyetherimide polymer.
The present invention also provides electroconductive polyetherimide nanofibers prepared by the above method.
The electroconductive polyetherimide nanofiber according to the present invention is excellent in properties such as heat resistance, flame retardancy, shape stability, high temperature stiffness, chemical resistance, light weight and electric conductivity and is suitable for the next generation of new technologies and new materials in the fields of information, environment, It can be applied to creation.
1 is an electron micrograph (× 2,000 times) of a nanofiber prepared by electrospinning a composite solution in which a multi-walled carbon nanotube is dispersed in a solution of polyetherimide in dimethylacetamide according to an embodiment of the present invention.
FIG. 2 is an electron micrograph (× 35,000 times) of a nanofiber prepared by electrospinning a composite solution in which a multi-walled carbon nanotube is dispersed in a solution of polyetherimide in dimethylacetamide according to an embodiment of the present invention.
Fig. 3 is an electron micrograph (x1, 000 times) of a nanofiber prepared by electrospinning a spinning solution prepared according to a comparative example of the present invention.
4 is a graph showing the diameter of the nanofibers produced according to the present invention.
5 is a graph showing a TGA analysis result of the nanofibers prepared according to the comparative example of the present invention.
6 is a graph showing the results of TGA analysis of nanofibers produced according to an embodiment of the present invention.
In the present invention, the carbon nanomaterial having a multipolar group formed by introducing a multipolar group into a carbon nanomaterial is characterized in that the cohesiveness is lowered and a crosslinked structure is formed to increase the viscosity, so that the carbon nanomaterial mixed with the polyetherimide polymer solution To confirm that it is possible to produce an electroconductive nanofiber having excellent physical properties such as heat resistance, flame retardancy, shape stability, high temperature stiffness, chemical resistance and light weight when electrospinning a stable colloidal solution. Respectively.
In the present invention, a multi-walled carbon nanotube having a multi-polar group is prepared and then mixed with a polyetherimide polymer solution to prepare a spinning solution and electrospun to prepare an electroconductive polyetherimide nanofiber. As a result of evaluating physical properties of the produced nanofibers, it was confirmed that the electrical conductivity and the high thermal stability were excellent.
Accordingly, in one aspect, the present invention provides a process for producing a carbon nanomaterial comprising: (a) treating a carbon nanomaterial to an acidic solution to produce a carbon nanomaterial having a carboxylic acid group; (b) dispersing the carbon nanomaterial having the carboxylic acid group in a solvent, and then treating toluene diisocyanate or methylene diphenyl diisocyanate to prepare a carbon nanomaterial having an isocyanate group; (c) dispersing the carbon nanomaterial having the isocyanate group in a solvent, and then adding and mixing aminohydroxymethylpyridine to prepare a carbon nanomaterial dispersion having a multi-polar group; (d) centrifuging and filtering the dispersion of carbon nanomaterials formed with multiple polar groups to remove the precipitate; (e) dissolving the polyetherimide polymer in a solvent to prepare a polyetherimide polymer solution; (f) preparing a colloidal solution by mixing the carbon nanomaterial dispersion with the polyelectrolyte polymer solution having the filtered multipolar groups formed therein; And (g) electrospinning the spinning solution to produce a nanofiber. The present invention also relates to a method for producing an electroconductive polyetherimide nanofiber.
In the present invention, the carbon nanomaterial may be a single wall carbon nanotube, a multi wall carbon nanotube, or a carbon nanofiber, but is not limited thereto.
The carbon nanomaterial having the carboxylic acid group is intended to lower the cohesiveness and increase the dispersibility, and can be produced by treating the carbon nanomaterial with an acidic solution.
The carbon nanomaterial is preferably treated in an amount of 1 to 10 parts by weight based on 100 parts by weight of the acidic solution. If the range of the carbon nanomaterial is out of the range, the carbon nanomaterial may be cut to shorten the length or damage the outer layer.
The acidic solution may be sulfuric acid, nitric acid, hydrochloric acid, perchloric acid, or a mixture thereof. It is preferable that the carbon nanomaterial is treated with an acidic solution and allowed to stand at 20 to 90 ° C for 1 to 20 hours, followed by lyophilization. When the temperature and the treatment time of the acidic solution are out of the above ranges, there is a problem that the dispersibility in the solvent is not exhibited due to the cohesiveness of the carbon nanomaterial or excessive oxidation and decomposition of the carbon nanomaterial occurs.
Next, after the carbon nanomaterial having a carboxylic acid group is dispersed in a solvent, toluene diisocyanate or methylene diphenyl diisocyanate is treated to prepare a carbon nanomaterial having an isocyanate group. Examples of the solvent include, but are not limited to, methyl pyrrolidone, dimethylacetamide, dimethylformamide, dimethylsulfone oxide and the like.
The carbon nanomaterial having the carboxylic acid group is preferably added in an amount of 2 to 15 parts by weight based on 100 parts by weight of the solvent. When the amount of the carbon nanomaterial having a carboxylic acid group is less than 2, there is a problem in that the reactivity is lowered. When the amount is more than 15 parts by weight, carbon nanomaterial having a carboxylic acid group is aggregated.
The toluene diisocyanate or methylenediphenyl diisocyanate is preferably added in an amount of 1 to 10 parts by weight based on 100 parts by weight of the carbon nanomaterial dispersion having a carboxylic acid group. When toluene diisocyanate or methylene diphenyl diisocyanate is less than 1 part by weight or exceeds 10 parts by weight, the reactivity is lowered.
The toluene diisocyanate or methylenediphenyl diisocyanate is preferably treated and left at 20 to 50 ° C for 12 to 24 hours. When the temperature and the treatment time are out of the above range, sufficient polar bonding is not formed between the carbon nanomaterials, resulting in a problem of not exhibiting a stable dispersion effect.
The prepared carbon nanomaterial having an isocyanate group has a property of forming a multipole bond with an adjacent carbon nanomaterial and having a stable dispersibility due to a network structure.
When a carbon nanomaterial having an isocyanate group is prepared, it is dispersed in a solvent, and then aminohydroxymethylpyridine is added and mixed to prepare a carbon nanomaterial dispersion having a multi-polar group. The solvent used herein is not limited to methyl pyrrolidone, dimethylacetamide, dimethylformamide, dimethylsulfone oxide, and the like.
The carbon nanomaterial having an isocyanate group is preferably added in an amount of 2 to 15 parts by weight based on 100 parts by weight of the solvent. When the amount of the carbon nanomaterial having an isocyanate group is less than 2, there is a problem that the reactivity is lowered. When the amount is more than 15 parts by weight, the carbon nanomaterial having an isocyanate group is aggregated.
The aminohydroxymethylpyridine is preferably added in an amount of 2 to 15 parts by weight based on 100 parts by weight of the carbon nanomaterial dispersion having an isocyanate group. When the amount of the aminohydroxymethylpyridine is less than 2 parts by weight or exceeds 15 parts by weight, the reactivity is lowered.
In order to obtain a more stable dispersion effect, it is preferable to treat triethylamine or triethyl acetate in addition to the carbon nanomaterial dispersion in which the produced multipolar group is formed, and to perform the reaction for 16 to 24 hours.
Next, in order to remove unreacted carbon nanomaterials, the carbon nanomaterial dispersion in which the multipolar group is formed is centrifuged and vacuum filtered to remove the precipitate.
When a carbon nanomaterial dispersion having a multi-polar group is prepared, a colloidal solution is prepared by mixing with a polyetherimide polymer solution.
The polyetherimide polymer solution can be prepared by dissolving the polyetherimide in a solvent such as methylpyrrolidone, dimethylacetamide, dimethylformamide, dimethylsulfone oxide, etc., and the concentration is preferably 15 to 25% by weight.
The polyetherimide polymer solution and the carbon nanomaterial dispersion in which the multipolar group is formed can be prepared by dispersing 30 to 100 parts by weight of the carbon nanomaterial having the multipolar group formed on 100 parts by weight of the polyetherimide polymer in the nanofiber prepared by electrospinning a spinning solution It is preferable that they are mixed so as to be dispersed. When the amount of the carbon nanomaterial having a multipolar group is less than 30 parts by weight based on 100 parts by weight of the polyetherimide polymer, there is a problem that the electrical conductivity is not increased. When the amount is more than 100 parts by weight, the basic properties of the polyetherimide polymer are maintained There is a difficult problem.
Finally, the prepared spinning solution is electrospun to produce nanofibers. Electrospinning can be carried out by a generally known method, but it is preferably carried out under conditions that the diameter of the nozzle is 23 to 25 gauge (0.5 to 0.6 mm), the voltage is 15 to 21 kV, and the extrusion rate is 13 to 19 m / s.
The present invention relates to electroconductive polyetherimide-based nanofibers produced by the above method from a different point of view.
The nanofibers are characterized in that 30 to 100 parts by weight of the carbon nanomaterial having the multipolar group is dispersed in 100 parts by weight of the polyetherimide polymer.
The nanofibers are characterized by high heat resistance of the polyetherimide polymer and excellent dispersibility of the carbon nanomaterial, resulting in excellent heat resistance and electrical conductivity.
[Example]
Hereinafter, the present invention will be described in more detail with reference to Examples. It is to be understood by those skilled in the art that these embodiments are only for illustrating the present invention and that the scope of the present invention is not construed as being limited by these embodiments.
Example 1: Preparation of electroconductive polyetherimide nanofiber
1-1: Preparation of carbon nanomaterial dispersion with multiple polar groups
The multiwalled carbon nanotube (MWCNT) (JEIO CO.) Was treated with a sulfuric acid: nitric acid mixed solution (7: 3 by volume) at 50 ° C for 5 hours, washed with water and lyophilized to obtain a multiwalled carbon nanotube (MWCNT-COOH). Next, the multiwalled carbon nanotube (MWCNT-COOH) having a carboxylic acid group prepared was dispersed in dimethylformamide (DMF), and the toluene diisocyanate was treated at 50 DEG C for 24 hours to obtain a multiwalled carbon nanotube having an isocyanate group (MWCNT-NCO).
Next, aminohydroxymethylpyrimidine (2.7 g) was dispersed in DMF (30 ml) and mixed with 300 ml of a multi-walled carbon nanotube (MWCNT-NCO) solution having an isocyanate group. Then, triethylamine (6.3 ml) And the mixture was reacted for 20 hours to prepare a multi-walled carbon nanotube dispersion having a multi-polar group, followed by centrifugation, and the precipitate was filtered.
1-2: Preparation of polyetherimide polymer solution
A polyetherimide polymer solution was prepared by dissolving 15 wt% of a polyetherimide polymer (Ultem 1000, SABIC CO.) In 1.9 ml of dimethylacetamide.
1-3: Production of spinning solution
In the polyetherimide polymer solution prepared in 1-2, a spinning solution was prepared such that the multi-walled carbon nanotubes formed with 1-1 multi-walled carbon nanotubes prepared in 1-1 were dispersed in 5, 9 and 12 wt%, respectively.
1-4: Fabrication of nanofibers by electrospinning
The nanofibers were prepared by electrospinning the spinning solution prepared in 1-3. The electrospinning was carried out by injecting the spinning solution into a syringe and applying a high voltage of 15, 17 and 19 kV to electrospray. At this time, the used syringe needle was 23 to 25 gauge, the spinning distance from the syringe needle to the collector was 10 cm, the release speed of the solution was 13 and 15 m / s, and the spinning time was 0.5 hour.
Example 2: Preparation of electroconductive polyetherimide nanofiber
2-1: Preparation of dispersion of carbon nanomaterials with multiple polar groups
A dispersion of carbon nanomaterials in which multiple polar groups were formed was prepared in the same manner as in Example 1-1.
2-2: Preparation of polyetherimide polymer solution
A polyetherimide polymer solution was prepared by dissolving 17 wt% of a polyetherimide polymer (Ultem 1000, SABIC CO.) In 1.63 ml of dimethylacetamide.
2-3: Preparation of spinning solution
A spinning solution was prepared so that 10 wt% of the multi-walled carbon nanotubes formed with the multipolar group prepared in 2-1 was dispersed in the polyetherimide polymer solution prepared in 2-2.
2-4: Fabrication of nanofibers by electrospinning
Nanofibers were prepared by electrospinning with the spinning solution prepared in 2-3. The electrospinning was carried out by injecting the spinning solution into the syringe and applying a high voltage of 21 kV. At this time, the used syringe needle was 23 gauge, the spinning distance from the syringe needle to the collector was 10 cm, the release speed of the solution was 17 m / s, and the spinning time was 0.5 hour.
Example 3: Preparation of electroconductive polyetherimide nanofiber
3-1: Preparation of dispersion of carbon nanomaterials with multiple polar groups
A dispersion of carbon nanomaterials in which multiple polar groups were formed was prepared in the same manner as in Example 1-1.
3-2: Preparation of polyetherimide polymer solution
A polyetherimide polymer solution was prepared by dissolving 20 wt% of a polyetherimide polymer (Ultem 1000, SABIC CO.) In 1.40 ml of dimethylacetamide.
3-3: Production of spinning solution
A spinning solution was prepared so that 6 wt% of the multi-walled carbon nanotubes formed with the multipolar group prepared in 3-1 was dispersed in the polyetherimide polymer solution prepared in 3-2.
3-4: Fabrication of nanofibers by electrospinning
The nanofibers were prepared by electrospinning with the spinning solution prepared in 3-3. The electrospinning was carried out by injecting the spinning solution into the syringe and applying a high voltage of 21 kV. At this time, the used syringe needle was 23 gauge, the spinning distance from the syringe needle to the collector was 10 cm, the release speed of the solution was 19 m / s, and the spinning time was 0.5 hour.
Comparative Example: Preparation of polyetherimide nanofiber
A spinning solution was prepared using only 25 wt% of the polyetherimide polymer without using a dispersion of the carbon nanomaterials in which the multiple polar groups were formed, and nanofibers were prepared under the same spinning conditions as in Example 3-4.
Experimental Example 1: Evaluation of physical properties of electroconductive polyetherimide nanofiber
In order to evaluate the physical properties of the nanofibers prepared in Examples 1 to 3 and Comparative Examples, electron microscopic observation, TGA analysis and electrical conductivity analysis were carried out.
Electron microscope observation
1 and 2 are electron micrographs (× 2,000 times and × 35,000 times, respectively) of the nanofibers produced in Example 1, and FIG. 3 is an electron micrograph (× 1,000 times) of the nanofibers produced in Comparative Example .
FIG. 4 shows the results of measuring the diameters of the nanofibers produced in Examples 1 to 3 and Comparative Examples,
It was confirmed that the thickness of the nanofiber varies depending on the content of the carbon nanomaterial (MWCNT) and the polyetherimide solution (PEI / DMAc) and the spinning conditions of the multi-polar group.
TGA analysis
The thermal properties of the nanofibers were measured using a thermogravimetric analyzer (TGA Q500, TA Instrument). The temperature range was from 100 ℃ to 800 ℃ under a nitrogen atmosphere at a rate of 10 ℃ / min And the results are shown in Figs. 5 and 6. Fig.
As a result of TGA analysis of the comparative example, FIG. 5 shows that the decomposition temperature is not lower than about 500 ° C. and that the decomposed residue is present in an amount of not less than 40% at 700 ° C. or higher.
On the other hand, FIG. 6 is a TGA analysis result of Example 2, and it was confirmed that more than 60% of the decomposed residue was present at 700 o C or higher. Therefore, it can be seen that the high thermal stability is further improved as compared with the comparative example using the polyetherimide spinning solution alone.
Electrical conductivity analysis
The electrical conductivities of the nanofibers prepared in Examples 1 to 3 and Comparative Examples were measured using a 4-point probe apparatus and are shown in Table 1 below.
From Table 1, it can be seen that the multi-walled carbon nanotubes in which the multipolar polarity is formed have a polyether (meth) acrylate content of 3.5 x 10 2 S / cm, 3.3 x 10 2 S / cm and 3.8 x 10 2 S / (Comparative example) of the present invention.
While the present invention has been particularly shown and described with reference to specific embodiments thereof, those skilled in the art will appreciate that such specific embodiments are merely preferred embodiments and that the scope of the present invention is not limited thereto will be. Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.
Claims (5)
(b) dispersing the carbon nanomaterial having the carboxylic acid group in a solvent, and then treating toluene diisocyanate or methylene diphenyl diisocyanate to prepare a carbon nanomaterial having an isocyanate group;
(c) dispersing the carbon nanomaterial having the isocyanate group in a solvent, and then adding and mixing aminohydroxymethylpyridine to prepare a carbon nanomaterial dispersion having a multi-polar group;
(d) centrifuging and filtering the dispersion of carbon nanomaterials formed with multiple polar groups to remove the precipitate;
(e) dissolving the polyetherimide polymer in a solvent to prepare a polyetherimide polymer solution;
(f) preparing a colloidal solution by mixing the carbon nanomaterial dispersion with the polyelectrolyte polymer solution having the filtered multipolar groups formed therein; And
(g) electrospinning the spinning solution to produce a nanofiber. The method of manufacturing an electroconductive polyetherimide nanofiber according to claim 1,
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| CN115948816A (en) * | 2023-02-14 | 2023-04-11 | 无锡聚新科技股份有限公司 | Method for manufacturing white polyester composite conductive fiber |
| CN115948816B (en) * | 2023-02-14 | 2023-09-05 | 无锡聚新科技股份有限公司 | Manufacturing method of white polyester composite conductive fiber |
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