Resin composition containing graphene quantum dots, masterbatch, fiber, and method for producing the resin composition
A resin composition with 10 nm graphene quantum dots and graphene, chemically bonded with flavonoids, addresses dispersion and performance issues in existing graphene materials, providing enhanced antibacterial, antistatic, and heat retention properties in fibers.
Patent Information
- Application Number
- JP2024197892
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Filing Date
- 2024-11-13
- Publication Date
- 2025-07-24
- Estimated Expiration
- 2044-11-13
AI Technical Summary
Existing graphene-based materials suffer from large particle sizes, low antibacterial ability, environmental and health hazards due to metal silver use, non-uniform dispersion, excessive pressure on spinning assemblies, and reduced antistatic and heat re-radiation performance due to graphene aggregation.
A resin composition containing graphene quantum dots with a particle size of 10 nm or less, chemically bonded with flavonoids, and graphene, uniformly dispersed with a polymer matrix, using a method involving aqueous dispersion, freeze-drying, and high-speed mixing to form a masterbatch for fibers with enhanced antibacterial, antistatic, and heat retention properties.
The composition achieves excellent antibacterial, antistatic, and heat retention properties while promoting blood microcirculation, being environmentally friendly and effective against mites, with improved dispersibility and reduced ultraviolet ray penetration.
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Abstract
Description
Technical Field
[0001] The present invention relates to a resin composition containing graphene quantum dots, a masterbatch, a resin composition, and a method for producing the resin composition.
Background Art
[0002] Graphene has excellent performance and is applied in various fields. In recent years, research on the use of graphene in composite materials and spinning has also advanced. For example, Patent Document 1 discloses a graphene-nano silver composite material. Patent Document 2 discloses a method for preparing a polymer-based silver-containing graphene nano antibacterial material. Patent Document 3 discloses a graphene quantum dot-modified polymer masterbatch for functional fibers and a method for producing the same.
[0003] However, in the materials disclosed in Patent Documents 1 and 2, the particle size of graphene is large, the antibacterial ability is low, and since a metal silver material is used, it places a burden on the environment and is also harmful to health. The functional masterbatch obtained according to the production method disclosed in Patent Document 3, when used in spinning, is not uniformly dispersed when mixed with each raw material, cannot fully exhibit the nano knife effect of graphene quantum dots, and has low antibacterial properties. In addition, due to the aggregation of graphene, excessive pressure is applied to the spinning assembly, and graphene is not uniformly dispersed in the fiber matrix, resulting in a decrease in the heat re-radiation blocking effect of graphene. Furthermore, the conductive mesh of graphene in the fiber matrix is not formed, resulting in a decrease in the antistatic performance. In recent years, there has been a demand for graphene quantum dots having new functions and a resin composition containing the graphene quantum dots.
Prior Art Documents
Patent Documents
[0004]
Patent Document 1
Patent Document 2
Patent Document 3
Summary of the Invention
Problems to be Solved by the Invention
[0005] The problem to be solved by the present invention is to provide graphene quantum dots, a resin composition, a masterbatch, a fiber, and a manufacturing method thereof, which have functions of mite prevention, mold prevention, deodorization, excellent antibacterial property, antistatic property, heat storage and heat preservation property, heat re-radiation property, and promote blood microcirculation, and contain two components of graphene and the graphene quantum dots.
Means for Solving the Problems
[0006] In view of the above problems, the present inventors have conducted extensive studies and found that graphene quantum dots with flavonoids chemically bonded to their surfaces or graphene quantum dots with a particle size of 10 nm or less have additional new functions in addition to antibacterial properties. The present invention has been completed based on these findings. To achieve the above object, the present invention provides the following means.
[0009] The present invention provides a fiber containing two components of graphene quantum dots and graphene composed of the masterbatch.
[0010] The present invention provides a fabric using the fiber.
[0011] The present invention relates to a method for manufacturing a resin composition containing graphene quantum dots with a particle size of 10 nm or less, A first aqueous dispersion preparation step of reacting graphene oxide, hydrogen peroxide, and aqueous ammonia to prepare a first graphene quantum dot aqueous dispersion; A second aqueous dispersion preparation step in which a reducing agent and a phosphate are added to the first graphene quantum dot aqueous dispersion, irradiated with microwaves in the range of 100 to 200 °C, and a second graphene quantum dot aqueous dispersion in which graphene quantum dots with a particle size of 10 nm or less are dispersed is prepared; 、 A freeze-drying step in which the second graphene quantum dot aqueous dispersion is freeze-dried to obtain graphene quantum dots with a particle size of 10 nm or less; The a two-component graphene powder preparation step of mixing graphene quantum dots with a particle size of 10 nm or less and graphene until they are uniform, A matrix powder preparation step of pulverizing a matrix material in a high-speed liquid nitrogen cooling atmosphere, A functional powder preparation step of preparing a functional powder by putting the two-component graphene powder, the matrix powder, and a dispersant into a mixer and mixing them, including a resin composition manufacturing method containing two components of graphene quantum dots and graphene. It can be seen that the particle size of the graphene is in the range of 300 to 800 nm. Provide a method for manufacturing a resin composition.
[0012] The method for manufacturing the resin composition preferably further includes a masterbatch preparation step of manufacturing a masterbatch containing two components of graphene quantum dots with a particle size of 10 nm or less and graphene. The masterbatch preparation step includes a granulation step of putting the resin composition into an ultra-high torque co-rotating high-performance twin-screw granulator and granulating at a temperature of 155 to 285 °C.
[0013] The present invention A fiber containing two components of graphene quantum dots with a particle size of 10 nm or less and graphene of Manufacture is a method , A first aqueous dispersion preparation step of reacting graphene oxide, hydrogen peroxide, and aqueous ammonia to prepare a first graphene quantum dot aqueous dispersion; a second aqueous dispersion preparation step in which a reducing agent and a phosphate are added to the first graphene quantum dot aqueous dispersion, irradiated with microwaves in the range of 100 to 200 °C, and a second graphene quantum dot aqueous dispersion in which graphene quantum dots with a particle size of 10 nm or less are dispersed is prepared; , A freeze-drying step in which the second graphene quantum dot aqueous dispersion is freeze-dried to obtain graphene quantum dots with a particle size of 10 nm or less; a two-component graphene powder preparation step of mixing the graphene quantum dots with a particle size of 10 nm or less and graphene until they are uniform; Ma A matrix powder preparation step of pulverizing a tricks material in a high-speed liquid nitrogen cooling atmosphere; a functional powder preparation step of putting the two-component graphene powder, the matrix powder, and a dispersant into a mixer and mixing them to prepare a functional powder; a granulation step of putting the resin composition into an ultra-high torque co-rotating high-performance twin-screw granulator and granulating at a temperature of 155 to 285 °C; and including a two-component of graphene quantum dots with a particle size of 10 nm or less and graphene obtained through the granulation step A masterbatch, a polymer matrix s , A mixed melt preparation step of mixing and melting a lubricant, sending the mixed melt to a spinning machine for spinning, cooling through a spinning sleeve to obtain continuous filament fibers with a fineness of 0.5 Dex or less, and a short fiber spinning step of cutting the filament fibers into short fibers by a cutting device to obtain short fibers and Including It can be seen that the particle size of the graphene is in the range of 300 to 800 nm. Provided is a method for producing a fiber containing a two-component of graphene quantum dots and graphene. .
Advantages of the Invention
[0014] The resin composition, masterbatch, and fiber containing two components of graphene quantum dots with a particle size of 10 nm or less and graphene of the present invention have excellent antibacterial properties with anti-mite, anti-mold, and deodorizing functions, and also have antistatic properties, heat storage and heat preservation properties, and heat re-radiation characteristics, and can promote blood microcirculation. Since they do not use silver, they can prevent pollution of the human body by heavy metals and are environmentally friendly.
Brief Description of the Drawings
[0015]
Figure 1
Embodiments for Carrying Out the Invention
[0016] The present invention will be described in more detail. Note that the "~" in the numerical range represents "from... to..." and includes both end values unless otherwise specified. Also, when a numerical range is indicated, the upper limit value and the lower limit value can be appropriately combined, and the resulting numerical range is also considered to be disclosed.
[0017] <Graphene Quantum Dots> The graphene quantum dots of the present invention are graphene quantum dots with a particle size of 10 nm or less. These graphene quantum dots have excellent bactericidal and deodorizing performance. When they come into contact with bacteria, pressure is applied to the cell membrane, and an oxidation reaction occurs between the functional groups of the graphene quantum dots and the cell membrane, breaking through the cell wall, causing the RNA or DNA inside the bacterial cell to flow out, and being inactivated. Also, the specific surface area of the graphene quantum dots of the present invention with a particle size of 10 nm or less is extremely large, reaching 500 - 1000 m 2 / g, and its adsorption capacity is particularly strong, having an excellent adsorption and removal effect on odors, being excellent in biocompatibility, toxicity, and safety, and being environmentally friendly.
[0018] The graphene quantum dots of the present invention have flavonoids chemically bonded to their surface. By grafting flavonoids onto the graphene quantum dots, the graphene quantum dots can be modified, which helps in killing mites and can impart the effect of avoiding mites. As a raw material for flavonoids, it is preferable to use mugwort extract.
[0019] The graphene quantum dots of the present invention preferably have flavonoids chemically bonded to the surface and a particle size of 10 nm or less. By grafting flavonoids onto the surface of the graphene quantum dots, an anti-mite effect is imparted, and since the particle size is 10 nm and the specific surface area is extremely large, the deodorizing and antibacterial effects can be improved. Furthermore, the graphene quantum dots with a particle size of 10 nm or less form a prism-like diffuse reflection effect on ultraviolet rays in the long wavelength region, effectively dissipate the ultraviolet rays, and can reduce the damage to the skin.
[0020] <Resin composition> The resin composition of the present invention contains graphene quantum dots with a particle size of 10 nm or less, graphene, and a polymer matrix.
[0021] The graphene quantum dots with a particle size of 10 nm or less are preferably flavonoid-modified graphene quantum dots with flavonoids chemically bonded to the surface.
[0022] The particle size of the graphene is preferably in the range of 300 to 800 nm, more preferably in the range of 300 to 500 nm. As a natural carbon material, graphene generates far-infrared waves. When the frequency thereof coincides with the vibration frequency of molecules, resonance occurs, the energy of the far-infrared waves is absorbed by the molecules, and a resonance absorption phenomenon appears. The graphene in the range of the particle size of 300 to 800 nm generates far-infrared waves of 8 to 14 μm close to the wavelength of the human body, and since its vibration frequency coincides with the vibration frequency of water molecules, the energy of the graphene is completely absorbed by the water molecules, activating the activity of biopolymers, promoting vasodilation, and having a physiotherapy effect of improving metabolism. If used continuously, it can relieve human fatigue and alleviate problems such as body pain.
[0023] In the present invention, by blending the graphene quantum dots and the graphene, an excellent heat preservation effect can be realized while maintaining the anti-mite, deodorizing, and antibacterial properties.
[0024] It is preferable that the polymer matrix contains at least one of polyester, polyamide 6, polypropylene, and polyethylene.
[0025] The polyester includes at least one selected from the group consisting of polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polyethylene-2,6-naphthalate (PEN), polymethylene terephthalate (PMT), polypropylene terephthalate (PPT), polyethylene-p-oxybenzoate (PEOB), poly-1,4-cyclohexylene dimethylene terephthalate (PCT), polyesters copolymerized with diol components such as diethylene glycol, neopentyl glycol, and polyalkylene glycol, dicarboxylic acid components such as adipic acid, sebacic acid, phthalic acid, isophthalic acid, and 2,6-naphthalenedicarboxylic acid (excluding biodegradable polyesters), liquid crystal polyester, polylactic acid, polyhydroxyalkanoate, polybutylene succinate, cellulose acetate, polyvinyl alcohol, polyglycolic acid, polybutylene succinate-co-adipate, polybutylene adipate terephthalate, and polyethylene terephthalate succinate.
[0026] The polyethylene includes at least one selected from the group consisting of low-density polyethylene, medium-density polyethylene, high-density polyethylene, and ultra-high-density polyethylene.
[0027] In the resin composition containing the two components of graphene quantum dots and graphene of the present invention, it is preferable to contain a dispersant. The dispersant preferably includes at least one selected from the group consisting of dopamine and polyvinylpyrrolidone, and more preferably dopamine and polyvinylpyrrolidone. In particular, by using dopamine and polyvinylpyrrolidone in combination, a synergistic effect is produced, and the dispersibility in the matrix of graphene and graphene quantum dots and the compatibility with the matrix are improved.
[0028] <Masterbatch> The masterbatch of the present invention contains the resin composition.
[0029] In the masterbatch of the present invention, the content of the graphene quantum dots is preferably 1 to 5% by mass. The content of the graphene is preferably 1 to 10% by mass, more preferably 4 to 10% by mass. The content of the polymer matrix is preferably, more preferably 80 to 93% by mass. The content of the dispersant is preferably, more preferably 2 to 5% by mass.
[0030] In the resin composition of the present invention, the content of the graphene quantum dots is preferably 1 to 5% by mass. The content of the graphene is preferably 5 to 10% by mass.
[0031] <Fiber> The present invention relates to a fiber composed of the masterbatch and containing two components of graphene quantum dots and graphene. In the fiber containing the two components of graphene quantum dots and graphene, the content of the graphene quantum dots is preferably 0.1 to 0.5% by mass, and the content of the graphene is more preferably 0.1 to 0.5% by mass. The graphene is uniformly dispersed in the fiber, can efficiently absorb ultraviolet blue light and ultraviolet red light, effectively reduce the penetration of ultraviolet rays, and can protect human skin.
[0032] The fiber containing two components of graphene quantum dots and graphene of the present invention can be used in bedding, household goods, clothing, etc.
[0033] <Fabric> The present invention relates to a fabric composed of the fiber and containing two components of graphene quantum dots and graphene. The graphene can effectively increase the movement and conduction of electrons, reduce the accumulation of static electricity on the fabric surface, and enhance the antistatic property of the fabric.
[0034] <Method for manufacturing graphene quantum dots> The method for manufacturing graphene quantum dots with a particle size of 10 nm or less according to the present invention is A first aqueous dispersion preparation step of preparing a first graphene quantum dot aqueous dispersion by reacting graphene oxide, hydrogen peroxide, and aqueous ammonia; A second aqueous dispersion preparation step of adding a reducing agent and a phosphate to the first graphene quantum dot aqueous dispersion, irradiating with microwaves in the range of 100 to 200 °C, and preparing a second graphene quantum dot aqueous dispersion in which graphene quantum dots with a particle size of 10 nm or less are dispersed; and A freeze-drying step of freeze-drying the second graphene quantum dot aqueous dispersion to obtain graphene quantum dots with a particle size of 10 nm or less.
[0035] The method for producing graphene quantum dots with a particle size of 10 nm or less according to the present invention preferably further includes a flavonoid reaction step of mixing the second graphene quantum dot aqueous dispersion and a flavonoid, performing ultrasonic treatment at 185 to 200 °C for 2 to 5 hours, and reacting the graphene quantum dots with the flavonoid.
[0036] Examples of the flavonoid include flavonoid-containing substances such as mugwort extract. In the flavonoid reaction step, the mass ratio of the second graphene quantum dot aqueous dispersion to the mugwort extract is preferably in the range of 50 to 70:50 to 30.
[0037] The graphene quantum dots produced by the production method of the present invention have a particle size of 10 nm or less and a uniform particle size, and their specific surface area is extremely large, so the deodorizing and antibacterial effects can be improved. In addition, by grafting flavonoids on the surface, an excellent mite repellent effect is imparted.
[0038] <Method for producing a resin composition containing graphene quantum dots> The method for producing a resin composition containing graphene quantum dots with a particle size of 10 nm or less according to the present invention is as follows: A two-component graphene powder preparation step of uniformly mixing graphene quantum dots with a particle size of 10 nm or less and graphene until uniform; A matrix powder preparation step of pulverizing a matrix material in a high-speed liquid nitrogen cooling atmosphere, A functional powder preparation step of putting the two-component graphene powder, the matrix powder, and a dispersant into a mixer, mixing them, and preparing a functional powder, is included.
[0039] The particle size of the graphene is preferably in the range of 300 to 800 nm, more preferably in the range of 300 to 500 nm. It is preferable that the polymer matrix contains at least one of polyester, polyamide 6, polypropylene, and polyethylene.
Example
[0040] Hereinafter, the present invention will be described in more detail based on examples, but the present invention is not limited thereto.
[0041] [Example 1] <Preparation of Graphene Quantum Dots> Graphene oxide, hydrogen peroxide, and aqueous ammonia were reacted in a 1 L glass reactor, the temperature was gradually raised from 70 °C to 90 °C, and the reaction was carried out for 4 hours to obtain a first graphene quantum dot aqueous dispersion. 50 mL of sodium hypophosphite solution was taken and put into a 100 mL glass reactor. 9 g of the above graphene quantum dot aqueous dispersion was added, and after stirring until uniform, ultrasonic treatment was carried out for 40 minutes. The glass reactor was put into a microwave reactor, the temperature was set to 150 °C, the microwave output was set to 600 W, and microwave treatment was carried out for 30 minutes. After the obtained liquid was cooled to room temperature, it was centrifuged at 9000 r / min for 10 minutes in a high-speed centrifuge, the supernatant was removed, and a second graphene quantum dot aqueous dispersion was obtained. The above second graphene quantum dot aqueous dispersion and mugwort extract were mixed in a glass container at a mass ratio of 70:30, and ultrasonic treatment was carried out for 2 to 5 hours with an ultrasonic rod of 200 watts or more under the conditions of 185 to 200 °C to obtain a graphene quantum dot aqueous dispersion in which flavonoids are chemically bonded to the surface. To the graphene quantum dot aqueous dispersion with flavonoid chemically bonded to the surface, 3.5 mass times of deionized water was added, and filtration was performed three times to obtain a purified dispersion. Freeze-drying treatment was carried out at -70 °C for 7 hours using a freeze dryer to obtain graphene quantum dot powder with a particle size of 10 nm or less having an anti-mite function.
[0042] <Preparation of masterbatch> 2.5 parts by mass of the graphene quantum dot powder with a particle size of 10 nm or less having the anti-mite function and 2 parts by mass of graphene with a particle size of 500 nm or less were mixed in a negative pressure supercritical mixing device, and preliminary mixing was carried out for 2.5 hours under the conditions of a temperature of 55 °C and a rotation speed of 16,000 R / min to obtain a two-component graphene powder uniformly dispersed. Polyester chips with a viscosity of 1.0 or more were pulverized in a liquid nitrogen pulverizer at -169 °C for 45 minutes to obtain matrix powder. The above two-component graphene powder, 93 parts by mass of the above matrix powder, and 2.5 parts by mass of dopamine were put into a mixing device (independently developed by the company) and mixed until uniform to obtain a functional powder. The stirring speed was 35 - 65 r / min, the stirring time was 1.5 - 2 hours, and the heating temperature was 45 - 85 °C. The above functional powder was put into an ultra-high torque co-directional high-performance twin-screw granulator (CX-HO26, manufactured by Ruiya Co., Ltd.), and granulation was carried out at a temperature of 155 - 285 °C for 15 minutes to obtain a semi-finished product of the masterbatch. Crystallization drying treatment was carried out in a dryer at 105 °C for 3 hours to obtain a masterbatch with a water content of less than 1% and a uniform distribution.
[0043] <Preparation of fiber> The above masterbatch was put into a drum drying circulator, and drying treatment was carried out at 85 °C for 8 hours so that the water content of the masterbatch became 1 mass% or less. The above masterbatch and polyester chips with a viscosity of 1.0 or more were mixed in a negative pressure pump circulation type mixer to obtain a mixed melt. The mixing time was 2 - 2.5 hours, the mixing temperature was 85 °C, the pump pressure was 2.5 standard atmospheres, and the circulation mixing speed was 45 r / min. The above-mentioned mixed melt was sent to a spinning machine by a metering pump through a negative pressure extraction device, spun at a temperature of 150 to 285 °C and a pressure of 20 to 28 standard atmospheres, and cooled through a spinning sleeve to obtain continuous filament fibers with a fineness of 0.5 Dex or less.
[0044] [Example 2] Instead of the material composition of 2.5 parts by mass of graphene quantum dot powder with an anti-mite function and a particle size of 10 nm or less, 2 parts by mass of graphene with a particle size of 500 nm or less, 93 parts by mass of matrix powder, and 2.5 parts by mass of dopamine, a material composition of 3 parts by weight of graphene quantum dot powder with an anti-mite function and a particle size of 10 nm or less, 3 parts by mass of graphene with a particle size of 500 nm or less, 91 parts by mass of matrix powder, and 3 parts by mass of dopamine was used. In the same manner as in Example 1, a masterbatch and fibers containing two components of graphene quantum dots and graphene were obtained.
[0045] [Example 3] Instead of the material composition of 2.5 parts by mass of graphene quantum dot powder with an anti-mite function and a particle size of 10 nm or less, 2 parts by mass of graphene with a particle size of 500 nm or less, 93 parts by mass of matrix powder, and 2.5 parts by mass of dopamine, a material composition of 5 parts by mass of graphene quantum dot powder with an anti-mite function and a particle size of 10 nm or less, 4 parts by mass of graphene with a particle size of 500 nm or less, 86 parts by mass of matrix powder, and 5 parts by mass of dopamine was used. In the same manner as in Example 1, a masterbatch and fibers containing two components of graphene quantum dots and graphene were obtained.
[0046] In the examples, various physical properties were measured or calculated as follows.
[0047] The particle size of the graphene quantum dots produced in Example 1 was detected using a transmission electron microscope (Talos STEM, manufactured by Thermo Fisher Scientific). The results are shown in Figure 1.
[0048] According to the JIS L1096 A method (constant temperature method), the heat storage and heat preservation performance of the fibers containing the two components of graphene quantum dots and graphene produced in Examples 1 to 3 was detected. The results are shown in Table 1.
[0049] According to the 45-degree parallel re-radiation method, which is a test method for evaluating the heat re-radiation characteristics certified by the Far-infrared Association, the heat re-radiation performance of the fibers containing the two components of graphene quantum dots and graphene produced in Examples 1 to 3 was detected. The results are shown in Table 1.
[0050] According to the bacterial liquid absorption method of JIS L 1902, the antibacterial activity of the fibers containing the two components of graphene quantum dots and graphene produced in Examples 1 to 3 was detected. The results are shown in Table 1.
[0051] According to the glass tube A method of JIS L 1920, the anti-mite performance of the fibers containing the two components of graphene quantum dots and graphene produced in Examples 1 to 3 was detected. The results are shown in Table 1.
[0052] According to the chargeability test method for woven and knitted fabrics of JIS L 1094, the antistatic performance of the fibers containing the two components of graphene quantum dots and graphene produced in Examples 1 to 3 was detected. The results are shown in Table 1.
[0053] Figure 1 shows the particle size of the graphene quantum dots produced in Example 1. In the image taken by the transmission electron microscope in Figure 1 (TEM measurement photo), the graphene quantum dots are shown as black dots. Using the particle size distribution measurement function of the transmission electron microscope, the particle size and distribution of the graphene quantum dots were measured. As shown in Figure 1, the particle size of the graphene quantum dots was 10 nm or less, and the graphene quantum dots with a particle size of about 3 nm accounted for about 70% of the whole.
[0054]
Table 1
[0055] Table 1 shows the performance parameters of the fibers containing the two components of graphene quantum dots and graphene produced in Examples 1 to 3. As shown in Table 1, the fibers containing the two components of graphene quantum dots and graphene of the present invention have good heat storage and heat preservation properties and excellent heat re-radiation characteristics. The antibacterial activity was 2.2 or more, and it was also found to have acarid-proof performance. In addition, the fibers containing the two components of graphene quantum dots and graphene of the present invention were found to have an antistatic effect.
[0056] Although the present invention has been described in detail based on the above embodiments, these are only a part of the embodiments of the present invention and not all embodiments. It should also be understood that other embodiments can be obtained based on these embodiments, and all of these embodiments belong to the protection scope of the present invention.
Claims
1. A method for producing a resin composition containing graphene quantum dots with a particle size of 10 nm or less, comprising: a first aqueous dispersion preparation step of reacting graphene oxide, hydrogen peroxide, and aqueous ammonia to prepare a first graphene quantum dot aqueous dispersion; a second aqueous dispersion preparation step of adding a reducing agent and a phosphate to the first graphene quantum dot aqueous dispersion, irradiating with microwaves in the range of 100 to 200 °C, and preparing a second graphene quantum dot aqueous dispersion in which graphene quantum dots with a particle size of 10 nm or less are dispersed; a freeze-drying step of freeze-drying the second graphene quantum dot aqueous dispersion to obtain graphene quantum dots with a particle size of 10 nm or less; a two-component graphene powder preparation step of mixing the graphene quantum dots with a particle size of 10 nm or less and graphene until uniform; a matrix powder preparation step of pulverizing a matrix material in a high-speed liquid nitrogen cooling atmosphere; including a functional powder preparation step of putting the two-component graphene powder, the matrix powder, and a dispersant into a mixer and mixing them to prepare a functional powder, A method for producing a resin composition containing a two-component of graphene quantum dots and graphene, characterized in that the particle size of the graphene is in the range of 300 to 800 nm.
2. further including a masterbatch preparation step of producing a masterbatch containing a two-component of graphene quantum dots with a particle size of 10 nm or less and graphene, the masterbatch preparation step includes a granulation step of charging the resin composition into an ultra-high torque co-rotating high-performance twin-screw granulator and granulating at a temperature of 155 to 285 °C. The method for producing a resin composition containing a two-component of graphene quantum dots and graphene according to claim 1.
3. A method for producing a fiber containing a two-component of graphene quantum dots with a particle size of 10 nm or less and graphene, comprising: a first aqueous dispersion preparation step of reacting graphene oxide, hydrogen peroxide, and aqueous ammonia to prepare a first graphene quantum dot aqueous dispersion; a second aqueous dispersion preparation step of adding a reducing agent and a phosphate to the first graphene quantum dot aqueous dispersion, irradiating with microwaves in the range of 100 to 200 °C, and preparing a second graphene quantum dot aqueous dispersion in which graphene quantum dots with a particle size of 10 nm or less are dispersed; A freeze-drying step in which the second graphene quantum dot aqueous dispersion is freeze-dried to obtain graphene quantum dots with a particle size of 10 nm or less; A two-component graphene powder preparation step of mixing the graphene quantum dots with a particle size of 10 nm or less and graphene until they are uniform; A matrix powder preparation step of pulverizing a matrix material in a high-speed liquid nitrogen cooling atmosphere; A functional powder preparation step of putting the two-component graphene powder, the matrix powder, and a dispersant into a mixer and mixing them to prepare a functional powder; A granulation step of putting the resin composition into an ultra-high torque co-rotating high-performance twin-screw granulator and granulating at a temperature of 155 to 285°C; A mixed melt preparation step of mixing and melting a masterbatch containing a two-component of graphene quantum dots with a particle size of 10 nm or less and graphene obtained through the granulation step, a polymer matrix, and a lubricant; A filament fiber spinning step of sending the mixed melt to a spinning machine for spinning and cooling it through a spinning sleeve to obtain continuous filament fibers with a fineness of 0.5 Dtex or less; Including a short fiber spinning step of cutting the filament fibers into short fibers by a cutting device to obtain short fibers; A method for manufacturing a fiber containing a two-component of graphene quantum dots and graphene, characterized in that the particle size of the graphene is in the range of 300 to 800 nm.
Citation Information
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