CN106752889A - A kind of shock resistance oxygen fluorinated graphene compound polyimide powdery paints and preparation method thereof - Google Patents
A kind of shock resistance oxygen fluorinated graphene compound polyimide powdery paints and preparation method thereof Download PDFInfo
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- CN106752889A CN106752889A CN201611166931.4A CN201611166931A CN106752889A CN 106752889 A CN106752889 A CN 106752889A CN 201611166931 A CN201611166931 A CN 201611166931A CN 106752889 A CN106752889 A CN 106752889A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09D179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
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Abstract
The invention discloses a kind of shock resistance oxygen fluorinated graphene compound polyimide powdery paints, it is made up of the raw material of following weight parts：Polyimides 100 110, fluorographite 10 14, potassium peroxydisulfate 0.1 0.3, sodium nitrate 12, potassium permanganate 0.1 0.4, SA 46, phosphorus pentoxide 0.5 1, dicyclohexylcarbodiimide 0.1 0.2, 4 dimethylamino naphthyridines 0.1 0.2, trimethylolpropane 0.1 0.3, ammonium fluozirconate 24, sldium lauryl sulfate 0.7 1, sorbitan monooleate 0.4 1, alkylolamides 0.8 2, stannous sulfide 0.5 1, dibatyl phithalate 57, dimethylformamide, sulfuric acid, appropriate absolute ethyl alcohol.Coating surface intensity of the invention is high, and impact resistance is strong, and good toughness, combination property is superior.
Description
Technical field
The present invention relates to powder coating technology field, more particularly to a kind of shock resistance oxygen fluorinated graphene compound polyimide
Powdery paints and preparation method thereof.
Background technology
Fluorinated graphene maintains the Two-dimensional Carbon Rotating fields of Graphene, and chemical composition has concurrently again like polytetrafluoroethylene (PTFE)
Two kinds of properties of material of Graphene and polytetrafluoroethylene (PTFE).Fluorinated graphene has the heat-resisting quantity suitable with polytetrafluoroethylene (PTFE), temperature
Just start slow decomposition when degree is higher than 260 DEG C, temperature is increased to more than 400 DEG C and decomposes rapid.The hydrophobicity of fluorinated graphene,
The property such as solvent resistance and chemical inertness is also especially prominent.As graphene oxide, fluorinated graphene is also because introduce sp3's
The original height conjugated structure of C-C structures and heavy damage, thus the good electric conductivity of Graphene is lost, but due to
F contents in fluorinated graphene can be adjusted in the preparation, therefore can within the specific limits adjust the electricity of fluorinated graphene
Energy subband structure；
The high temperature resistant of fluorinated graphene, chemical inertness and solvent resistance make it can be used for high-temperaure coating.And fluorinated graphene
High resistance it is can be used as insulating materials.Additionally, its electronic band structure has a controllability, thus in semiconductor applications and
Electronic device etc. is also with a wide range of applications；
It is different by big very big concern in field of composite material preparation from graphene oxide, using fluorinated graphene as carrier or as
The preparation that enhanced additive is used for composite is still a urgently research field leaved for development.Fluorinated graphene is used for inorganic multiple
The preparation of condensation material or polymer composites, key point is the hypopolarization rate for how overcoming fluorinated graphene itself relatively low,
To meet inorganic nano-particle uniform adsorption in its surface, or stronger interface interaction is formed between polymer molecule, made most
Obtained fluorinated graphene composite can really give play to good combination property eventually；
Polyimides has excellent heat endurance, is one of heat endurance highest kind so far in polymer.Polyamides
The heat-resisting quantity of imines be also manifested by Thermocurable polyimide can more than 300 DEG C long-term use, even if at 380 DEG C or higher
At a temperature of can also use hundreds of hours, polyimides simultaneously also have lower temperature resistance, such as in -269 DEG C of liquid helium still not
Meeting brittle failure, and thermoplastic polyimides temperature in use can as little as -240 DEG C, with excellent oil resistant and organic solvent resistance,
Almost all of aliphatic hydrocarbon is to the non-corrosive effect of Thermocurable polyimide, and TPI then can be with molten
In usual vehicle, with radiation resistance, polyimides has self-extinguishment to solution when burning, and smoke rate is low.In addition, polyimides material
Material is nontoxic, and with good biocompatibility, Kapton can be used for motor slot insulation, cable, printing, traction horse
Up to, the field such as wiring board, transformer, electromagnetic wire, capacitor.Kapton can also be used for microelectronics industry, can make
Be the dielectric layer in microelectronic component, play layer insulation, stress buffer, protection device exempt to be affected by the external environment, shield α-
Particle etc. is acted on, and its coating is used for electromagnetic wire as insulated paint, or is used as high-temperature resistant coating；
The Graphene and its derivative of two-dimension plane structure have the performances such as excellent light, electricity, mechanics, thus between polymer
With very strong complementarity.Additionally, Graphene and its derivative big draw ratio and specific surface area, make it relative to the richness of zero dimension
Strangle the carbon materials such as the graphite of alkene, one-dimensional CNT and three-dimensional, it is easier to be dispersed in polymeric matrix, so that more
The excellent properties of its own are played well, effectively improve the performance of polymer/graphene nano composite material each side, Graphene
Lifting to polymer performance depends on good dispersion of the Graphene in polymeric matrix with strong interface effect.Due to
Graphene film is easily reunited, and often lacks stronger interface interaction, therefore the polymer for directly being prepared as filler with Graphene is multiple
Condensation material performance boost is simultaneously not up to expected.Graphene is acted on by π-π stackings or chemical action is chemically modified, one
Determine to be solved the above problems in degree.And from graphene oxide, it is compound with polymer again after functionalization, reduction, be
Graphene easily one of most effective approach of reunion problem is solved so far.By the polymer/functionalization obtained by the approach
The performances such as graphene composite material significant increase mechanics, electricity, calorifics；
Functionalization graphene or graphene oxide are combined with polyimides, the power of polyimides can be not only obviously improved
Intensity is learned, while the heat endurance of polyimides, thermal conductivity and thermal expansivity etc. can also be improved, polyimides/Graphene
Composite achieves larger breakthrough at the aspect such as high-performance and multifunction.But as the derivative of Graphene, it is fluorinated stone
Black alkene is not as graphene oxide and is widely used in like that in the preparation of polyimides/graphene composite material, with graphite oxide
Alkene chemical constitution and qualitative difference, make research of the fluorinated graphene in composite polyimide material also seem especially heavy
Will.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of shock resistance oxygen fluorinated graphene is compound poly-
Acid imide powdery paints and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of shock resistance oxygen fluorinated graphene compound polyimide powdery paints, it is made up of the raw material of following weight parts：
Polyimides 100-110, fluorographite 10-14, potassium peroxydisulfate 0.1-0.3, sodium nitrate 1-2, potassium permanganate 0.1-0.4,
SA 4-6, phosphorus pentoxide 0.5-1, dicyclohexylcarbodiimide 0.1-0.2, DMAP 0.1-0.2, three hydroxyls
Methylpropane 0.1-0.3, ammonium fluozirconate 2-4, sldium lauryl sulfate 0.7-1, sorbitan monooleate 0.4-1, alkylolamides
0.8-2, stannous sulfide 0.5-1, dibatyl phithalate 5-7, dimethylformamide, sulfuric acid, appropriate absolute ethyl alcohol.
A kind of preparation method of the shock resistance oxygen fluorinated graphene compound polyimide powdery paints, including following step
Suddenly：
（1）Above-mentioned ammonium fluozirconate is added in the deionized water of 30-40 times of its weight, is stirred, add above-mentioned sorb smooth
Monoleate, it is 57-60 DEG C to rise high-temperature, and the sulfuric acid of 10-13mol/l is added dropwise, and regulation pH is 1-2, insulated and stirred 20-30 points
Clock, adds above-mentioned fluorographite, and stirring reaction 40-50 minutes, precipitation was washed in filtering 3-4 times, and air drying must be pre-processed
Fluorographite；
（2）By above-mentioned pretreatment fluorographite, potassium peroxydisulfate, phosphorus pentoxide mix, be added to 5-7 times of compound weight,
In the sulfuric acid solution of 96-98%, it is sent in 80-90 DEG C of oil bath, insulated and stirred 8-9 hours, discharges, precipitation is washed in filtering
3-4 times, dried at 60-65 DEG C 10-12 hours, mixed with above-mentioned sodium nitrate, be added to 17-20 times of compound weight, 90-
In 95% sulfuric acid solution, it is sent in ice-water bath, adds above-mentioned potassium permanganate, stirring reaction 4-5 hours, discharging rose high-temperature
It is 35-40 DEG C, insulation reaction 1-2 hours, adds the distilled water of 10-15 times of mixed system weight, it is 90-95 to continue to rise high-temperature
DEG C, insulation reaction 10-20 minutes, 10-15 hours is stood, centrifugation, by precipitation washing 2-3 times, freeze-drying 40-50 is small
When, obtain oxygen fluorographite；
（3）Abovementioned alkyl alkylolamides is added in 30-40 times of its weight, 60-75% ethanol solution, is stirred, added
Above-mentioned oxygen fluorographite, trimethylolpropane, ultrasonic 10-20 minutes, filtering, by precipitation absolute ethyl alcohol, deionized water successively
Washing 2-3 times, is vacuum dried 1-2 hours at 80-90 DEG C, obtains modified oxygen fluorographite；
（4）Above-mentioned modified oxygen fluorographite, SA are mixed, the dimethyl formyl of 100-110 times of compound weight is added to
In amine, it is 57-60 DEG C to rise high-temperature, and insulated and stirred 20-25 hours, cooling was ultrasonically treated 1-2 hours under 60-65w, obtains graphite
Dispersion liquid；
（5）Above-mentioned DMAP, dicyclohexylcarbodiimide are mixed, the two of 23-40 times of compound weight are added to
In NMF, stir, obtain catalysis dispersion liquid；
（6）Above-mentioned graphite dispersing solution is added in ice-water bath, above-mentioned catalysis dispersion liquid, stirring reaction 2- after completion of dropping is added dropwise
3 hours, discharging, it is 60-64 DEG C to rise high-temperature, insulated and stirred 40-50 hours, adds above-mentioned stannous sulfide, is stirred, and is centrifuged
Separate, precipitation dimethylformamide, absolute ethyl alcohol, deionized water are washed 3-4 times successively, freeze-drying, obtain grafting graphite
Alkene；
（7）Above-mentioned graft grapheme is mixed with remaining each raw material, is stirred, be sent in extruder, melting extrusion is cold
But, fine powder is worn into, is sieved, obtain final product the compound polyimide powdery paints.
It is an advantage of the invention that：Be grafted to SA in dispersed preferably oxygen fluorinated graphene first by the present invention,
Each SA fat chain end of composite there remains a carboxyl with chemical reactivity, and these structural factors promote
Make polyimide molecule chain be more easy to insert oxygen fluorinated graphene piece interlayer, and oxygen fluorinated graphene and polyimides two can be strengthened
Alternate interface interaction, thus can effectively improve dispersiveness of the grafted inorganic particle between polymer；The present invention will grafting
Graphene mixes with polyimides, makes the section of polyimide composite film and becomes very coarse, and it is more uniformly dispersed simultaneously
It is embedded in polyimide matrix, good dispersiveness can increase the interface phase interaction between polymeric matrix and inorganic filler
With, so that the load acted on polymer molecular chain can be effectively passed on inorganic molecule, so as to improve finished product film
Surface mechanical properties, and the high strength of Graphene is inherited due to graft grapheme, thus to the rigidity of polyimides
Intensity has obvious humidification；Graft grapheme of the invention can also between polyimide molecule with covalent bond, hydrogen bond with
And Van der Waals force etc. interacts, so as to reduce the combination of polyimide matrix molecule and water, while in the Graphene being grafted
There is hydrophobic C-F keys so as to film there is good hydrophobicity；
Coating surface intensity of the invention is high, and impact resistance is strong, and good toughness, combination property is superior.
Specific embodiment
A kind of shock resistance oxygen fluorinated graphene compound polyimide powdery paints, it is made up of the raw material of following weight parts
's：
Polyimides 100, fluorographite 10, potassium peroxydisulfate 0.1, sodium nitrate 1, potassium permanganate 0.1, SA 4, phosphorus pentoxide
0.5th, dicyclohexylcarbodiimide 0.1,4 dimethylamino naphthyridines 0.1, trimethylolpropane 0.1, ammonium fluozirconate 2, laruyl alcohol sulfuric acid
Sodium 0.7, sorbitan monooleate 0.4, alkylolamides 0.8, stannous sulfide 0.5, dibatyl phithalate 5, dimethyl formyl
Amine, sulfuric acid, appropriate absolute ethyl alcohol.
A kind of preparation method of the shock resistance oxygen fluorinated graphene compound polyimide powdery paints, including following step
Suddenly：
（1）Above-mentioned ammonium fluozirconate is added in the deionized water of 30 times of its weight, is stirred, add the smooth single oil of above-mentioned sorb
Acid esters, it is 57 DEG C to rise high-temperature, and the sulfuric acid of 10mol/l is added dropwise, and regulation pH is 1, and insulated and stirred 20 minutes adds above-mentioned fluorination stone
Ink, stirring reaction 40 minutes, filtering, by precipitation washing 3 times, air drying obtains pretreatment fluorographite；
（2）By above-mentioned pretreatment fluorographite, potassium peroxydisulfate, phosphorus pentoxide mix, be added to 5 times of compound weight, 96%
Sulfuric acid solution in, be sent in 80 DEG C of oil bath, insulated and stirred 8 hours, discharge, filtering, will precipitation washing 3 times, at 60 DEG C
Lower drying 10 hours, mixes with above-mentioned sodium nitrate, is added in 17 times of compound weight, 90% sulfuric acid solution, is sent to ice
In water-bath, above-mentioned potassium permanganate is added, stirring reaction 4 hours discharges, it is 35 DEG C to rise high-temperature, and insulation reaction 1 hour is added
The distilled water that 10 times of mixed system weight, it is 90 DEG C to continue to rise high-temperature, and insulation reaction 10 minutes stands 10 hours, centrifugation point
From by precipitation washing 2 times, freeze-drying 40 hours obtains oxygen fluorographite；
（3）Abovementioned alkyl alkylolamides is added in 30 times of its weight, 60% ethanol solution, is stirred, add above-mentioned oxygen
Precipitation absolute ethyl alcohol, deionized water are washed in fluorographite, trimethylolpropane, ultrasound 10 minutes, filtering 2 times successively,
It is vacuum dried 1 hour at 80 DEG C, obtains modified oxygen fluorographite；
（4）Above-mentioned modified oxygen fluorographite, SA are mixed, are added in the dimethylformamide of 100 times of compound weight,
It is 57 DEG C to rise high-temperature, and insulated and stirred 20 hours, cooling ultrasonically treated 1 hour under 60w, obtains graphite dispersing solution；
（5）Above-mentioned 4 dimethylamino naphthyridine, dicyclohexylcarbodiimide are mixed, the dimethyl of 23 times of compound weight is added to
In formamide, stir, obtain catalysis dispersion liquid；
（6）Above-mentioned graphite dispersing solution is added in ice-water bath, above-mentioned catalysis dispersion liquid, stirring reaction 2 after completion of dropping is added dropwise
Hour, discharging, it is 60 DEG C to rise high-temperature, and insulated and stirred 40 hours adds above-mentioned stannous sulfide, stirs, centrifugation, will
Precipitation dimethylformamide, absolute ethyl alcohol, deionized water are washed 3 times successively, and freeze-drying obtains graft grapheme；
（7）Above-mentioned graft grapheme is mixed with remaining each raw material, is stirred, be sent in extruder, melting extrusion is cold
But, fine powder is worn into, is sieved, obtain final product the compound polyimide powdery paints.
Tensile strength：133MPa；
Elongation at break：66%.
Claims (2)
1. a kind of shock resistance oxygen fluorinated graphene compound polyimide powdery paints, it is characterised in that it is by following weight parts
Raw material be made：
Polyimides 100-110, fluorographite 10-14, potassium peroxydisulfate 0.1-0.3, sodium nitrate 1-2, potassium permanganate 0.1-0.4,
SA 4-6, phosphorus pentoxide 0.5-1, dicyclohexylcarbodiimide 0.1-0.2, DMAP 0.1-0.2, three hydroxyls
Methylpropane 0.1-0.3, ammonium fluozirconate 2-4, sldium lauryl sulfate 0.7-1, sorbitan monooleate 0.4-1, alkylolamides
0.8-2, stannous sulfide 0.5-1, dibatyl phithalate 5-7, dimethylformamide, sulfuric acid, appropriate absolute ethyl alcohol.
2. a kind of preparation method of shock resistance oxygen fluorinated graphene compound polyimide powdery paints as claimed in claim 1, its
It is characterised by, comprises the following steps：
（1）Above-mentioned ammonium fluozirconate is added in the deionized water of 30-40 times of its weight, is stirred, add above-mentioned sorb smooth
Monoleate, it is 57-60 DEG C to rise high-temperature, and the sulfuric acid of 10-13mol/l is added dropwise, and regulation pH is 1-2, insulated and stirred 20-30 points
Clock, adds above-mentioned fluorographite, and stirring reaction 40-50 minutes, precipitation was washed in filtering 3-4 times, and air drying must be pre-processed
Fluorographite；
（2）By above-mentioned pretreatment fluorographite, potassium peroxydisulfate, phosphorus pentoxide mix, be added to 5-7 times of compound weight,
In the sulfuric acid solution of 96-98%, it is sent in 80-90 DEG C of oil bath, insulated and stirred 8-9 hours, discharges, precipitation is washed in filtering
3-4 times, dried at 60-65 DEG C 10-12 hours, mixed with above-mentioned sodium nitrate, be added to 17-20 times of compound weight, 90-
In 95% sulfuric acid solution, it is sent in ice-water bath, adds above-mentioned potassium permanganate, stirring reaction 4-5 hours, discharging rose high-temperature
It is 35-40 DEG C, insulation reaction 1-2 hours, adds the distilled water of 10-15 times of mixed system weight, it is 90-95 to continue to rise high-temperature
DEG C, insulation reaction 10-20 minutes, 10-15 hours is stood, centrifugation, by precipitation washing 2-3 times, freeze-drying 40-50 is small
When, obtain oxygen fluorographite；
（3）Abovementioned alkyl alkylolamides is added in 30-40 times of its weight, 60-75% ethanol solution, is stirred, added
Above-mentioned oxygen fluorographite, trimethylolpropane, ultrasonic 10-20 minutes, filtering, by precipitation absolute ethyl alcohol, deionized water successively
Washing 2-3 times, is vacuum dried 1-2 hours at 80-90 DEG C, obtains modified oxygen fluorographite；
（4）Above-mentioned modified oxygen fluorographite, SA are mixed, the dimethyl formyl of 100-110 times of compound weight is added to
In amine, it is 57-60 DEG C to rise high-temperature, and insulated and stirred 20-25 hours, cooling was ultrasonically treated 1-2 hours under 60-65w, obtains graphite
Dispersion liquid；
（5）Above-mentioned DMAP, dicyclohexylcarbodiimide are mixed, the two of 23-40 times of compound weight are added to
In NMF, stir, obtain catalysis dispersion liquid；
（6）Above-mentioned graphite dispersing solution is added in ice-water bath, above-mentioned catalysis dispersion liquid, stirring reaction 2- after completion of dropping is added dropwise
3 hours, discharging, it is 60-64 DEG C to rise high-temperature, insulated and stirred 40-50 hours, adds above-mentioned stannous sulfide, is stirred, and is centrifuged
Separate, precipitation dimethylformamide, absolute ethyl alcohol, deionized water are washed 3-4 times successively, freeze-drying, obtain grafting graphite
Alkene；
（7）Above-mentioned graft grapheme is mixed with remaining each raw material, is stirred, be sent in extruder, melting extrusion is cold
But, fine powder is worn into, is sieved, obtain final product the compound polyimide powdery paints.
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Cited By (1)
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| CN116219568A (en) * | 2023-02-15 | 2023-06-06 | 泰州市广源化纺有限公司 | Antibacterial polypropylene filament and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116219568A (en) * | 2023-02-15 | 2023-06-06 | 泰州市广源化纺有限公司 | Antibacterial polypropylene filament and preparation method thereof |
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