CN109161987A - A kind of bionical wig fiber filament of sodium alginate/graphene and its preparation and application - Google Patents
A kind of bionical wig fiber filament of sodium alginate/graphene and its preparation and application Download PDFInfo
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- CN109161987A CN109161987A CN201810900854.3A CN201810900854A CN109161987A CN 109161987 A CN109161987 A CN 109161987A CN 201810900854 A CN201810900854 A CN 201810900854A CN 109161987 A CN109161987 A CN 109161987A
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/04—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of alginates
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41G—ARTIFICIAL FLOWERS; WIGS; MASKS; FEATHERS
- A41G3/00—Wigs
- A41G3/0083—Filaments for making wigs
-
- 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
- D01F1/04—Pigments
-
- 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
-
- 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
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention relates to a kind of bionical wig fiber filament of sodium alginate/graphene and its preparations and application.The graphene that the sodium alginate and mass percentage that the fiber filament is 98-99.9% by mass percentage are 0.1-2% forms.Preparation method includes: sodium alginate/graphene dispersing solution preparation, the bionical wig fiber filament preparation of sodium alginate/graphene.Invention increases the added values of chemical fiber wire wig, and properties of product are substantially improved, and have good simulation quality, and substitution true man send out wig and pour the huge economic benefit of high-end wig market realization.
Description
Technical field
The invention belongs to composite fibre and its preparation and application field, in particular to a kind of sodium alginate/graphene is bionical
Wig fiber filament and its preparation method and application.
Background technique
The development of society and the progress of fashion allow people to liberate the pursuit of " beauty ", and wig is got over as " fashionable dress on head "
To be more accepted and welcome.There are mainly three types of wig types, first is that the true man of high-end market send out wig, first is that occupying big portion
Divide the chemical fiber wire wig of mainstream market, another kind is that class occupy the i.e. true man's clouding chemical fiber wire vacation of medium and high-grade goods between the two
Hair.Chemical fiber wire is since the advantage of its production cost and simple process occupies wig market major part specific gravity, but its market price is only
Several hundred members are to nearly 1,000 yuan, and compared with the thousands of members of high-end market send out wig to nearly ten thousand yuan of true man, economic well-being of workers and staff differs greatly.It is high-end
True man to send out the Commercial sources of wig be mainly the true hair for purchasing people, but in recent years also because of the change of the progress in epoch and social form
Change, true source shortage and at high cost, the high-end market product vacancy of delivering.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of bionical wig fiber filament of sodium alginate/graphene and its systems
Preparation Method and application, to overcome the defect of prior art middle and high end wig vacancy.
The present invention carries out bionic function by raw material of traditional chemical fibre, makes the ultimate attainment emulation of chemical fiber wire wig of low cost, does
The performance to compare favourably is sent out to true man, squeezes into high-end wig market, wins the maximization that business opportunity realizes economic benefit.
The bionical wig fiber filament of a kind of sodium alginate/graphene of the invention, the fiber filament is by mass percentage
The graphene composition that sodium alginate and mass percentage for 98-99.9% are 0.1-2% is that a kind of novel wig is fine
There is dimension natural black to exempt from dye, excellent simulated properties.
The sodium alginate is food-grade, viscosity 400-800mpa.s;Graphene parameter are as follows: electric conductivity 100-
1000S/m, oxygen content 1-10%, the number of plies are 1-5 layers, and piece diameter is having a size of 1-3um.
The filametntary preparation method of a kind of bionical wig of sodium alginate/graphene of the invention, comprising:
(1) sodium alginate/graphene dispersing solution preparation: graphene is added in Aqueous dispersions agent, in ultrasonication
Under be uniformly dispersed, be centrifuged, cryo-conservation is stand-by, and sodium alginate is added and is stirred, filters, Room-temperature seal standing and defoaming obtains
Sodium alginate/graphene dispersing solution, wherein the mass percent of graphene, sodium alginate and Aqueous dispersions agent is 0.1-2:2-3:
95-97.9;
(2) wet spinning technology process: sodium alginate/graphene dispersing solution in step (1) is squeezed out through metering pump-metered
Into calcium chloride coagulation bath, spinning solidifies, then through hydro-thermal draw orientation, washing, drying, winding, obtains sodium alginate/graphene
Bionical wig fiber filament.
Graphene in the step (1) are as follows: the graphene after electronation, electric conductivity 100-1000S/m, oxygen content are
1-10%, the number of plies are 1-5 layers, and piece diameter is having a size of 1-3um.
In the step (1) Aqueous dispersions agent include: mass percentage concentration be 0.5-3% PVP K30,
The water that the kayexalate and mass percentage concentration that mass percentage concentration is 0.2-0.5% are 96.5-99.3%.
Ultrasonic power is 10-25w in the step (1), and ultrasonic time is 4-6 hours.
Centrifugal rotational speed is 300-500r/min, centrifugation time 5min in the step (1).
It is stirred in the step (1) specifically: be stirred 30min at 3-10 DEG C, be warming up to 60 DEG C and be stirred for mixing
Close 30min.
Filtering is using 300 mesh filter screens in the step (1).
Standing and defoaming temperature is 20~30 DEG C in the step (1), and the standing and defoaming time is 10~15h.
Cryo-conservation temperature is 3-10 DEG C in the step (1).
The condition of spinning in the step (2) are as follows: spinning pressure 0.2-0.7Mpa, spinning temperature are 40-60 DEG C, shearing
Rate is 1-10s-1。
The mass concentration of calcium chloride is 6~8% in coagulating bath in the step (2), setting time 1-2min.
Hydro-thermal draw conditions in the step (2) are as follows: mass concentration be 5% calcium chloride in 90 DEG C of hydro-thermal drawing-off 0.5-
1.5 again.
It is dry in the step (2) are as follows: 150 DEG C of heated-air dryings, moisture content is less than 0.5% (mass percent).
The filametntary application of a kind of bionical wig of sodium alginate/graphene of the invention.
Present invention process process is followed successively by graphene aqueous dispersion liquid, sodium alginate/graphene dispersing solution, wet spinning mistake
Journey.Wherein wet spinning main technological steps are successively the processes such as coagulating bath solidification, hydro-thermal drawing-off, washing, drying, winding.
The present invention is dispersed in water graphene uniform by non-covalent bond modification and molecular interface acting regulatory, then leads to
The regulation for crossing compatibility prepares the homogeneous spinning solution of sodium alginate/graphene, obtains through wet spinning technology a kind of based on alginic acid
The bionical wig fiber filament of sodium/graphene.
The present invention carries out wet spinning into fibre using graphene as biomimetic modification nanofiller, in conjunction with sodium alginate, not only exists
Market structure takes advantage, and the advantage and characteristic that there is traditional chemical fibre not have.The addition of pure graphene eliminates rear road
Reducing process imparts fiber excellent antistatic, anti-microbial property, while fiber being made to have the speciality of natural black without dye
The mode of color, composite spinning avoids falling off for graphene at fibre.Since the characteristic of sodium alginate makes the wig fiber with good
Good natural halogen-free flame retardant feature.
The present invention carries out bionic function by raw material of traditional chemical fibre, and the chemical fiber wire of low cost is made by wet spinning technology
The ultimate attainment emulation of wig is accomplished to send out the performance to compare favourably with true man, squeezes into high-end wig market, wins business opportunity and realizes economic benefit
It maximizes.With Guo Jing, Li Xuecai et al. (201210457178.X);Zhang Xingxiang, Li Wei et al. (201210015803.5);Wang Ji
The patent of state, Wu Jianli et al. (201510475443.0) report is compared, and the present invention collects antistatic, antibacterial, moisture absorption, fire-retardant more function
The problem of capable of being integrated, specifically addressing the dyeing of the above patent black hair.
Beneficial effect
(1) present invention realizes the Aqueous dispersions of pure graphene using composite dispersing agent, and bionical using graphene progress
It is modified to make composite fibre that there is good black to exempt to contaminate characteristic, while there is the characteristic of antistatic, antibacterial, moisture absorption, halogen-free flameproof.
(2) sodium alginate of the present invention/graphene biomimetic modification increases the added value of chemical fiber wire wig, keeps properties of product big
Width is promoted, and has good simulation quality, and substitution true man send out wig and pour the huge economic benefit of high-end wig market realization.
(3) present invention production preparation process makees solvent with water, realizes greenization production.
Detailed description of the invention
Fig. 1 is that true man send out the filametntary material object of the bionical wig of sodium alginate/graphene in digital photograph (a) and embodiment 3
Photo (b).
Fig. 2 is sodium alginate of the present invention/graphene dispersing solution wet spinning technology flow chart, wherein 1. frequency converters;2. material
Cylinder;3. metering pump;4. filter;5. spinneret;6. coagulating bath;7. conducting wire pole;8. godet;9. damp and hot stretching;10. washing;
11. dry;12. desalination brush.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Graphene physical characteristics control and centrifugation, filtering, storage, dissolution and the control of condition of molding are determined in the embodiment of the present invention
Whether the compound success or not of uniformity, seaweed and graphene and solution for having determined graphene dispersion can be spun.
Main agents source: sodium alginate comes from Qingdao Mingyue Marine Alga Group Corp., Ltd.;Graphene is by improved
The preparation of hummer ' s method one kettle way, the method is as follows:
1. it is as follows to weigh reaction mass mass ratio, graphite powder: potassium permanganate: potassium nitrate: the concentrated sulfuric acid=2:12:1:84.?
Graphite powder, potassium nitrate are once added in there-necked flask, the concentrated sulfuric acid is transferred to stir about 10min under condition of ice bath, dissolves to potassium nitrate
It is slowly added portionwise to feed intake in potassium permanganate 1h afterwards and finish.Continue to be stirred to react 2h under condition of ice bath after feeding intake.
2. oxidation is with intercalation stripping process: after reacting 2h, being to slowly warm up to 35 DEG C of reaction 6h.It is dropped after completion of the reaction by 35 DEG C
Temperature keeps the temperature 10min to 0 DEG C, is then added dropwise plus 4 gallic acid amount water of water dilutes, 98 DEG C are gone to after dilution and keeps the temperature 10min again.It stirs
After mixing uniformly, the hydrogen peroxide of acid amount 1/5 is added dropwise while stirring, is changed into golden yellow to solution, continues to stir 1h, washing is taken out
Filter, drying.
Embodiment 1
(1) by mass percentage concentration be 0.5% PVP K30, mass percentage concentration be 0.2% polyphenyl
Mixed dissolution in beaker is added in vinyl sulfonic acid sodium, the water that mass percentage concentration is 99.3%.Graphene (knot after taking electronation
Structure performance parameter are as follows: electric conductivity 100S/m, oxygen content 1%, 1 layer of the number of plies, piece diameter size 1um) it is added in beaker.It is super in 10w
Under sound effect, then graphene dispersing solution is centrifuged, centrifugal rotational speed 300r/min, centrifugation time is by ultrasound 4 hours
5min.Low temperature storage temperature is 3 DEG C.In 3 DEG C of water-bath, sodium alginate is added into graphene dispersing solution, wherein graphene,
Sodium alginate and the mass percent of Aqueous dispersions agent are 0.1:2:97.9.Mixed process need to be in 3 DEG C of low-temperature mixeds, mixed dissolution
After 30min, gradually it is warming up to 60 DEG C and continues to dissolve 30min.With 300 mesh filter screen filtrations, 25 DEG C of standing and defoaming 12h after having dissolved
For use.
(2) spinning process: above-mentioned sodium alginate/graphene spinning solution is transferred in spinning machine batch can, spinning pressure
0.2Mpa, 40 DEG C of spinning temperature, shear rate 1s-1Under the conditions of through measure pump-metered be squeezed into 7% calcium chloride coagulation bath it is solidifying
Gu setting time 1min.Then 0.5 times of hydro-thermal drawing-off, hydro-thermal drawing-off bath are 90 DEG C of 5% calcium chloride, then 150 DEG C of hot air dryings
It is dry to moisture content less than 0.5%, winding, obtain the bionical wig fiber filament of sodium alginate/graphene.
Properties of product: monofilament specific resistance is 106Ω/cm;Escherichia coli antibiotic rate is greater than 95%;Moisture absorption 5.5%, limit oxygen
Index is 40, and product economy added value promotes 10%.
Embodiment 2
(1) by mass percentage concentration be 3% PVP K30, mass percentage concentration be 0.5% polyphenyl second
Mixed dissolution in beaker is added in alkene sodium sulfonate, the water that mass percentage concentration is 96.5%.Graphene (structure after taking electronation
Performance parameter are as follows: electric conductivity 1000S/m, oxygen content 10%, 5 layers of the number of plies, piece diameter size 3um) it is added in beaker.It is super in 25w
Under sound effect, then graphene dispersing solution is centrifuged, centrifugal rotational speed 500r/min, centrifugation time is by ultrasound 6 hours
5min.Low temperature storage temperature is 10 DEG C.In 10 DEG C of water-bath, sodium alginate is added into graphene dispersing solution, wherein graphite
The mass percent of alkene, sodium alginate and Aqueous dispersions agent is 2:3:95.Mixed process need to be in 10 DEG C of low-temperature mixeds, mixed dissolution
After 30min, gradually it is warming up to 60 DEG C and continues to dissolve 30min.With 300 mesh filter screen filtrations, 25 DEG C of standing and defoaming 12h after having dissolved
For use.
(2) spinning process: above-mentioned sodium alginate/graphene spinning solution is transferred in spinning machine batch can, spinning pressure
0.7Mpa, 60 DEG C of spinning temperature, shear rate 10s-1Under the conditions of through measure pump-metered be squeezed into 7% calcium chloride coagulation bath it is solidifying
Gu setting time 1min.Then 1.5 times of hydro-thermal drawing-off, hydro-thermal drawing-off bath are 90 DEG C of 5% calcium chloride, then 150 DEG C of heated-air dryings
To moisture content less than 0.5%, winding obtains the bionical wig fiber filament of sodium alginate/graphene.
Properties of product: monofilament specific resistance is 105Ω/cm;Escherichia coli antibiotic rate is greater than 98%;Moisture absorption 5%, limit oxygen refer to
Number is 39, and product economy added value promotes 15%.
Embodiment 3
(1) by mass percentage concentration be 1% PVP K30, mass percentage concentration be 0.3% polyphenyl second
Mixed dissolution in beaker is added in alkene sodium sulfonate, the water that mass percentage concentration is 98.7%.Graphene (structure after taking electronation
Performance parameter are as follows: electric conductivity 800S/m, oxygen content 6%, 4 layers of the number of plies, piece diameter size 2um) it is added in beaker.In 20w ultrasound
Under effect, then graphene dispersing solution is centrifuged, centrifugal rotational speed 400r/min, centrifugation time is by ultrasound 5 hours
5min.Low temperature storage temperature is 5 DEG C.In 5 DEG C of water-bath, sodium alginate is added into graphene dispersing solution, wherein graphene,
Sodium alginate and the mass percent of Aqueous dispersions agent are 1:2.5:96.5.Mixed process need to mix molten in 5 DEG C of low-temperature mixeds
After solving 30min, gradually it is warming up to 60 DEG C and continues to dissolve 30min.With 300 mesh filter screen filtrations, 25 DEG C of standing and defoamings after having dissolved
12h is stand-by.
(2) spinning process: above-mentioned sodium alginate/graphene spinning solution is transferred in spinning machine batch can, spinning pressure
0.5Mpa, 50 DEG C of spinning temperature, shear rate 4s-1Under the conditions of through measure pump-metered be squeezed into 7% calcium chloride coagulation bath it is solidifying
Gu setting time 1min.Then 1 times of hydro-thermal drawing-off, hydro-thermal drawing-off bath are 90 DEG C of 5% calcium chloride, and then 150 DEG C of heated-air dryings are extremely
For moisture content less than 0.5%, winding obtains the bionical wig fiber filament of sodium alginate/graphene.
Properties of product: monofilament specific resistance is 106Ω/cm;Escherichia coli antibiotic rate is greater than 95%;Moisture absorption 5%, limit oxygen refer to
Number is 40, and product economy added value promotes 12%.
Fig. 1 shows: sodium alginate/graphene wig compared with true man send out (a), has outer well with composite fibre (b)
Simulation quality is seen, and compound wig fiber has good black characteristic.
Comparative example 1
Wang Jiguo, Wu Jianli et al., which are reported, a kind of prepares the method that hair meets fiber with quail feather
(201510475443.0), it is raw material by wet spinning that this method, which is using quail feather protein, sodium alginate and polyvinyl alcohol,
The artificial hair of technology preparation.Obtained wig hairlines have excellent anti-flammability, heat resistance.This patent product exists in contrast
The good antistatic performance of wig fiber, excellent anti-microbial property are imparted while with excellent flame characteristic.
Comparative example 2
Yang Cui, Li whole people et al. (201410217874.2) report a kind of wig modified acrylic fibre for preparing
Gel-colored method, specific process be, retarding agents and the dye of positive ion are used separately by when dyeing: by as-spun fibre with 20~
The speed of 60m/min enters the slow dye bath containing retarding agents, and stops 3~10 seconds at 30~50 DEG C;Rinsing, roll compacting;Into 0
~5 DEG C of the dye bath containing the dye of positive ion is disseminated 2~8 seconds;After extruding remaining dye liquor by pressure roller, into 40~80 DEG C of heat
Case heats 3~10min, finally obtains lovely luster, the polyacrylonitrile-radical wig fiber with simulated effect.With the patent phase
Than the invention patent, which realizes the wig product of black, exempts from dyer's sequence, while assigning the good static electricity resistance of fiber, resisting
Bacterium, moisture absorption, halogen-free flame retardant feature.The invention patent product optimal performance are as follows: monofilament specific resistance is 105Ω/cm;Escherichia coli are anti-
Bacterium rate is greater than 98%;Moisture absorption 5.5%, limit oxygen index 40, product economy added value promote 15%.
Claims (10)
1. a kind of bionical wig fiber filament of sodium alginate/graphene, which is characterized in that the fiber filament is by mass percentage
The graphene composition that sodium alginate and mass percentage for 98-99.9% are 0.1-2%.
2. fiber filament according to claim 1, which is characterized in that the sodium alginate is food-grade, viscosity 400-
800mpa.s;The parameter of graphene are as follows: electric conductivity 100-1000S/m, oxygen content 1-10%, the number of plies are 1-5 layers, piece diameter ruler
Very little is 1-3um.
3. a kind of filametntary preparation method of bionical wig of sodium alginate/graphene, comprising:
(1) graphene is added in Aqueous dispersions agent, ultrasound, centrifugation, sodium alginate is added and is stirred, filters, stood de-
Bubble, obtains sodium alginate/graphene dispersing solution, wherein the mass percent of graphene, sodium alginate and Aqueous dispersions agent is
0.1-2:2-3:95-97.9;
(2) sodium alginate/graphene dispersing solution in step (1) is squeezed into spinning in calcium chloride coagulation bath to solidify, then is led through hydro-thermal
Orientation, washing, drying, winding are stretched, the bionical wig fiber filament of sodium alginate/graphene is obtained.
4. preparation method according to claim 3, which is characterized in that graphene in the step (1) are as follows: after electronation
Graphene, electric conductivity 100-1000S/m, oxygen content 1-10%, the number of plies be 1-5 layers, piece diameter is having a size of 1-3um.
5. preparation method according to claim 3, which is characterized in that Aqueous dispersions agent includes: quality in the step (1)
The kayexalate that PVP K30 that percentage concentration is 0.5-3%, mass percentage concentration are 0.2-0.5%
The water for being 96.5-99.3% with mass percentage concentration.
6. preparation method according to claim 3, which is characterized in that ultrasonic power is 10-25w in the step (1), is surpassed
The sound time is 4-6 hours;Centrifugal rotational speed is 300-500r/min, centrifugation time 5min.
7. preparation method according to claim 3, which is characterized in that be stirred in the step (1) specifically: in 3-
10 DEG C are stirred 30min, are warming up to 60 DEG C and are stirred for mixing 30min;Standing and defoaming temperature is 20~30 DEG C, when standing and defoaming
Between be 10~15h.
8. preparation method according to claim 3, which is characterized in that the condition of spinning in the step (2) are as follows: spinning pressure
Power is 0.2-0.7Mpa, and spinning temperature is 40-60 DEG C, shear rate 1-10s-1;The mass concentration of calcium chloride is 6 in coagulating bath
~8%, setting time 1-2min.
9. preparation method according to claim 3, which is characterized in that hydro-thermal draw conditions in the step (2) are as follows: in matter
Measure 90 DEG C of 0.5-1.5 times of hydro-thermal drawing-offs in the calcium chloride that concentration is 5%.
10. a kind of filametntary application of bionical wig of sodium alginate/graphene as described in claim 1.
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Cited By (2)
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WO2024043710A1 (en) * | 2022-08-24 | 2024-02-29 | 주식회사 네오엔프라 | Composition for use in wig comprising polyester, polybutylene terephthalate, and graphene |
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徐龙华等编著: "《伟晶岩型铝硅酸盐矿物晶体各向异性及其浮选应用》", 31 July 2017, 冶金工业出版社 * |
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KR20220147415A (en) * | 2021-04-27 | 2022-11-03 | 주식회사 네오엔프라 | Composite resin composition for wigs |
KR102499745B1 (en) * | 2021-04-27 | 2023-02-14 | 주식회사 네오엔프라 | Composite resin composition for wigs |
WO2024043710A1 (en) * | 2022-08-24 | 2024-02-29 | 주식회사 네오엔프라 | Composition for use in wig comprising polyester, polybutylene terephthalate, and graphene |
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