CN115505190B - Interface micro-nano assembly forming method of fluorescent fiber composite material - Google Patents
Interface micro-nano assembly forming method of fluorescent fiber composite material Download PDFInfo
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- CN115505190B CN115505190B CN202211199711.7A CN202211199711A CN115505190B CN 115505190 B CN115505190 B CN 115505190B CN 202211199711 A CN202211199711 A CN 202211199711A CN 115505190 B CN115505190 B CN 115505190B
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 150000001413 amino acids Chemical class 0.000 claims description 6
- 125000005842 heteroatom Chemical group 0.000 claims description 6
- 229920005672 polyolefin resin Polymers 0.000 claims description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 5
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- 229920004933 Terylene® Polymers 0.000 claims description 3
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- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
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- 229910000077 silane Inorganic materials 0.000 claims description 3
- PYODKQIVQIVELM-UHFFFAOYSA-M sodium;2,3-bis(2-methylpropyl)naphthalene-1-sulfonate Chemical compound [Na+].C1=CC=C2C(S([O-])(=O)=O)=C(CC(C)C)C(CC(C)C)=CC2=C1 PYODKQIVQIVELM-UHFFFAOYSA-M 0.000 claims description 3
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- DMDRLTJRQCKPLQ-UHFFFAOYSA-N 2-(2-aminophenyl)benzenethiol Chemical compound NC1=CC=CC=C1C1=CC=CC=C1S DMDRLTJRQCKPLQ-UHFFFAOYSA-N 0.000 claims 1
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- 239000004416 thermosoftening plastic Substances 0.000 description 2
- VETPHHXZEJAYOB-UHFFFAOYSA-N 1-n,4-n-dinaphthalen-2-ylbenzene-1,4-diamine Chemical compound C1=CC=CC2=CC(NC=3C=CC(NC=4C=C5C=CC=CC5=CC=4)=CC=3)=CC=C21 VETPHHXZEJAYOB-UHFFFAOYSA-N 0.000 description 1
- PUAQLLVFLMYYJJ-UHFFFAOYSA-N 2-aminopropiophenone Chemical compound CC(N)C(=O)C1=CC=CC=C1 PUAQLLVFLMYYJJ-UHFFFAOYSA-N 0.000 description 1
- VRVRGVPWCUEOGV-UHFFFAOYSA-N 2-aminothiophenol Chemical compound NC1=CC=CC=C1S VRVRGVPWCUEOGV-UHFFFAOYSA-N 0.000 description 1
- PRWJPWSKLXYEPD-UHFFFAOYSA-N 4-[4,4-bis(5-tert-butyl-4-hydroxy-2-methylphenyl)butan-2-yl]-2-tert-butyl-5-methylphenol Chemical compound C=1C(C(C)(C)C)=C(O)C=C(C)C=1C(C)CC(C=1C(=CC(O)=C(C=1)C(C)(C)C)C)C1=CC(C(C)(C)C)=C(O)C=C1C PRWJPWSKLXYEPD-UHFFFAOYSA-N 0.000 description 1
- 235000005811 Viola adunca Nutrition 0.000 description 1
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- 235000013487 Viola odorata Nutrition 0.000 description 1
- 235000002254 Viola papilionacea Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- 239000003513 alkali Substances 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/18—Homopolymers or copolymers of nitriles
- C08J2433/20—Homopolymers or copolymers of acrylonitrile
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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- C08K5/13—Phenols; Phenolates
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- C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
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- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
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- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
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- Health & Medical Sciences (AREA)
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Abstract
The invention discloses a fluorescent fiber composite material which comprises the following raw materials in parts by weight: 0.1 to 1 part of carbon dot modified fluorescent fiber; 50-99 parts of thermoplastic resin; 0.0001 to 0.001 part of surfactant; 0.001-5 parts of surface wetting agent; 1-20 parts of compatilizer. The invention has the advantages of simple operation, low cost, high production efficiency, high fluorescence quantum yield of the product, energy conservation, environmental protection and the like, and can be suitable for the requirements of industrialized mass production.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to an interface micro-nano assembly forming method of a fluorescent fiber composite material.
Background
The existence of the counterfeit commodity has serious influence on society, so that people have to consider the prevention and identification of the counterfeit commodity, namely the anti-counterfeiting and counterfeit identification. The anti-fake technology research aims at providing anti-fake and fake distinguishing method for fake commodity from technological point of view, and this makes the fake commodity incapable of being taken out of cage or eliminated from the flow field. The anti-counterfeiting information based on the traditional anti-counterfeiting material is easy to separate from the used packaging base material, so that the problem of losing an anti-counterfeiting function is solved.
The fluorescent fiber anti-counterfeiting technology is one of core technologies of anti-counterfeiting materials. The fluorescent fiber has the characteristics of controllable excitation spectrum, special nano morphology, colorless and transparent appearance and the like, thus the fluorescent fiber has excellent adaptability in the aspect of anti-counterfeiting technology, is an important anti-counterfeiting information marker, and can be widely applied to various fields of packaging anti-counterfeiting, military camouflage, protective clothing for road and overhead operation, daily necessities, special photosensitive materials, information storage materials and the like as an anti-counterfeiting base material. The fluorescent fiber developed by the traditional technology can be heated to generate fluorescence quenching, so that the fluorescent fiber cannot be applied to film packaging materials through a thermoplastic processing process, is extremely susceptible to external conditions such as illumination, solvents, acid and alkali and the like to lose fluorescence property, and does not have a fluorescence anti-counterfeiting function. Therefore, the development of the novel dual-wavelength fluorescent anti-counterfeiting fiber with high temperature resistance, durability and high stability has great application prospect and social benefit.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides an interface micro-nano assembly forming method of a fluorescent fiber composite material.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
A fluorescent fiber composite material consists of the following raw materials in parts by weight: 0.1 to 1 part of carbon dot modified fluorescent fiber; 50-99 parts of thermoplastic resin; 0.0001 to 0.001 part of surfactant; 0.001-5 parts of surface wetting agent; 1-20 parts of compatilizer.
Preferably, the carbon dot modified fluorescent fiber has a carbon dot particle diameter of 5 to 10nm, a fiber diameter of 0.1 to 20 μm, and a fiber length of 0.5 to 20mm.
Preferably, the thermoplastic resin is one or a mixture of more than one of polyolefin, polyester, polyvinyl alcohol, nylon and biodegradable resin.
Preferably, the compatilizer is one or a mixture of more of polyolefin resin grafted maleic anhydride, polyolefin resin grafted acrylic acid and epoxy resin grafted polyamide.
Preferably, the surface wetting agent is one or a mixture of several of nekal BX, K12, K14, KMT-7001 and industrial white oil.
An interface micro-nano assembly forming method of a fluorescent fiber composite material comprises the following steps:
S1, preparing carbon point modified fluorescent fibers:
1) Synthesis of carbon dots: mixing a carbon source raw material for synthesizing carbon points and a heteroatom doping raw material in a solvent to form a uniform solution, transferring the solution into a high-pressure reaction kettle taking polytetrafluoroethylene as a lining, sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into a baking oven, setting the reaction temperature to be 60-200 ℃, reacting for 4-10 hours, closing the baking oven after the reaction is finished, and cooling the reaction kettle to room temperature to obtain yellowish-brown liquid;
2) Separation of carbon dots: transferring the product into deionized water, stirring uniformly, centrifuging at 5000-10000 rpm for 15-30 min to remove larger particle impurities, filtering with 0.1-10 um filter membrane to remove insoluble substances, dialyzing the yellow supernatant with dialysis membrane for 24h, and replacing deionized water every 4h to remove unreacted raw materials, thereby obtaining the aqueous solution with the carbon point of 5-10 nm.
3) Surface treatment of fibrous substrates: putting the fiber substrate with the length of 3-20 mm into absolute ethyl alcohol, performing ultrasonic treatment for 0.5-3 h, then cleaning with deionized water, and drying for later use;
4) Preparation of fluorescent fibers: placing 1-5 g of surface modified fiber and 30-45 mL of carbon dot solution into 80mL of high-pressure reaction kettle with polytetrafluoroethylene lining, adding 10-20 mL of deionized water to ensure that the fiber is immersed into the liquid, sealing the high-pressure reaction kettle and reacting for 4-10 hours at 60-200 ℃ in an oven, taking out a sample after the reaction kettle is cooled, carrying out suction filtration, washing for 5-10 times with the deionized water until the filtrate has no fluorescent reaction, and drying the obtained fiber in a vacuum drying oven at 40-60 ℃ for 12-48 hours to finally obtain fluorescent fiber with the length of 3-20 mm;
S2, preparing a finished product:
1) Adding the thermoplastic resin and the compatilizer into a feeding area of a high-speed mixer through a liquid metering pump quantitative feeding device according to mass components, and fully and uniformly mixing in the high-speed mixer;
2) Extruding and granulating the blend by using a double-screw extruder, and respectively setting the temperature of each heating section as follows: the first stage is 150-200 ℃, the second stage is 155-200 ℃, the third stage is 160-200 ℃, the fourth stage is 165-200 ℃, and the fifth stage is 170-200 ℃;
3) Vacuum drying the granulated composite material at 50-80 ℃ for 12-24h to ensure that the water content is less than or equal to 0.1wt% to obtain resin granules;
4) Mixing 1-5 g of synthesized fluorescent fiber, 5-15 ml of surface wetting agent, 0.001-0.05 g of surfactant and 100-300 ml of absolute ethyl alcohol for ultrasonic treatment for 2-6 hours, and drying for 10-24 hours after suction filtration;
5) Fully and uniformly mixing the fluorescent fibers subjected to surface treatment with resin granules in a high-speed mixer;
6) And then adding the resin granules adsorbed with the fluorescent fibers into a surface layer material cylinder through a sheet extruder, and preparing the carbon-point modified fluorescent fiber composite material through an extrusion tabletting method.
Preferably, the molecular retention of the dialysis membrane in the step S1 is MWCO:1000.
Preferably, the carbon source raw material in the step S1 is one or more of citric acid, acrylic acid, glucose, amino acid, vitamin, lignin, starch, protein, polyurethane, polyacrylamide and polyethylene glycol.
Preferably, the heteroatom doping raw material in the step S1 is one or more of phenylenediamine, ethylenediamine, polyethyleneimine, o-phenylenediamine dimer, urea, ammonia water, amino acid, silane, 2-aminophenylsulfiol, phosphoric acid and melamine.
Preferably, the solvent in the step S1 is one or more of water, urea and ethanol.
Preferably, the fiber substrate in the step S1 is one or more of polyester fiber, polyacrylonitrile fiber, nylon fiber, aramid fiber, nylon fiber, terylene, acrylon, spandex, vinylon, polypropylene fiber, chlorfiber and soybean fiber.
Compared with the prior art, the invention has the beneficial effects that:
1. The invention adopts a bottom-up method to prepare carbon dots, and the carbon dots are obtained by carbonizing small molecules or polymers under certain reaction conditions, so that the raw materials are widely available; the hydrothermal synthesis method is utilized to dissolve the micromolecular precursor in water or other solvents, has the advantages of simple operation, low cost, high production efficiency, high fluorescence Quantum Yield (QY) of the product, energy conservation, environmental protection and the like, and can meet the requirements of industrial mass production;
2. According to the invention, carbon dots are used as fluorescent substances and are combined with the fiber base material in a chemical grafting mode, so that aggregation state fluorescence quenching of the carbon dots is avoided, meanwhile, an antioxidant is added in the processing process, the fluorescent substances are prevented from being oxidized by dissolved oxygen in the processing process to generate fluorescence quenching, and the processing temperature is reduced in a plasticizer adding mode, so that the fluorescent substances are prevented from being thermally quenched at an excessive temperature.
Drawings
FIG. 1 is an infrared spectrum of a carbon dot nanoparticle of the present invention;
FIG. 2 is a graph showing the average particle diameter distribution of carbon dot nanoparticles according to the present invention;
FIG. 3 is an excitation spectrum of the carbon dot modified fluorescent fiber and the fluorescent fiber after surface treatment according to the present invention;
FIG. 4 shows a scanning electron microscope pattern 1 of a carbon dot modified fluorescent fiber after surface treatment according to the present invention and a resin containing a different dose of a compatibilizer;
FIG. 5 shows a scanning electron microscope pattern 2 of a carbon dot modified fluorescent fiber after surface treatment according to the present invention and a resin containing a different dose of a compatibilizer;
FIG. 6 shows a scanning electron microscope pattern 3 of a carbon dot modified fluorescent fiber after surface treatment according to the present invention and a resin containing a different dose of a compatibilizer;
FIG. 7 is a graph showing the contact angle of the neat PP according to the present invention;
FIG. 8 is a graph showing the contact angle of PP according to the invention with 10% PP-g-MAH;
FIG. 9 is a graph showing the contact angle of PP according to the invention with 15% PP-g-MAH;
fig. 10 is a graph of the surface energy test of the fiber after the surface treatment.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
A fluorescent fiber composite material consists of the following raw materials in parts by weight: 0.1 to 1 part of carbon dot modified fluorescent fiber; 50-99 parts of thermoplastic resin; 0.0001 to 0.001 part of surfactant; 0.001-5 parts of surface wetting agent; 1-20 parts of compatilizer.
The carbon dot particle diameter of the carbon dot modified fluorescent fiber is 5-10 nm, the fiber diameter of the carbon dot modified fluorescent fiber is 0.1-20 mu m, and the fiber length of the carbon dot modified fluorescent fiber is 0.5-20 mm.
The thermoplastic resin is one or a mixture of more of polyolefin, polyester, polyvinyl alcohol, nylon and biodegradable resin.
The compatilizer is one or a mixture of more of polyolefin resin grafted maleic anhydride, polyolefin resin grafted acrylic acid and epoxy resin grafted polyamide.
The surface wetting agent is one or more of nekal BX, K12, K14, KMT-7001 and industrial white oil.
An interface micro-nano assembly forming method of a fluorescent fiber composite material comprises the following steps:
S1, preparing carbon point modified fluorescent fibers:
1) Synthesis of carbon dots: mixing a carbon source raw material for synthesizing carbon points and a heteroatom doping raw material in a solvent to form a uniform solution, transferring the solution into a high-pressure reaction kettle taking polytetrafluoroethylene as a lining, sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into a baking oven, setting the reaction temperature to be 60-200 ℃, reacting for 4-10 hours, closing the baking oven after the reaction is finished, and cooling the reaction kettle to room temperature to obtain yellowish-brown liquid;
2) Separation of carbon dots: transferring the product into deionized water, stirring uniformly, centrifuging at 5000-10000 rpm for 15-30 min to remove larger particle impurities, filtering with 0.1-10 um filter membrane to remove insoluble substances, dialyzing the yellow supernatant with dialysis membrane for 24h, and replacing deionized water every 4h to remove unreacted raw materials, thereby obtaining the aqueous solution with the carbon point of 5-10 nm.
3) Surface treatment of fibrous substrates: putting the fiber substrate with the length of 3-20 mm into absolute ethyl alcohol, performing ultrasonic treatment for 0.5-3 h, then cleaning with deionized water, and drying for later use;
4) Preparation of fluorescent fibers: placing 1-5 g of surface modified fiber and 30-45 mL of carbon dot solution into 80mL of high-pressure reaction kettle with polytetrafluoroethylene lining, adding 10-20 mL of deionized water to ensure that the fiber is immersed into the liquid, sealing the high-pressure reaction kettle and reacting for 4-10 hours at 60-200 ℃ in an oven, taking out a sample after the reaction kettle is cooled, carrying out suction filtration, washing for 5-10 times with the deionized water until the filtrate has no fluorescent reaction, and drying the obtained fiber in a vacuum drying oven at 40-60 ℃ for 12-48 hours to finally obtain fluorescent fiber with the length of 3-20 mm;
S2, preparing a finished product:
1) Adding the thermoplastic resin and the compatilizer into a feeding area of a high-speed mixer through a liquid metering pump quantitative feeding device according to mass components, and fully and uniformly mixing in the high-speed mixer;
2) Extruding and granulating the blend by using a double-screw extruder, and respectively setting the temperature of each heating section as follows: the first stage is 150-200 ℃, the second stage is 155-200 ℃, the third stage is 160-200 ℃, the fourth stage is 165-200 ℃, and the fifth stage is 170-200 ℃;
3) Vacuum drying the granulated composite material at 50-80 ℃ for 12-24h to ensure that the water content is less than or equal to 0.1wt% to obtain resin granules;
4) Mixing 1-5 g of synthesized fluorescent fiber, 5-15 ml of surface wetting agent, 0.001-0.05 g of surfactant and 100-300 ml of absolute ethyl alcohol for ultrasonic treatment for 2-6 hours, and drying for 10-24 hours after suction filtration;
5) Fully and uniformly mixing the fluorescent fibers subjected to surface treatment with resin granules in a high-speed mixer;
6) And then adding the resin granules adsorbed with the fluorescent fibers into a surface layer material cylinder through a sheet extruder, and preparing the carbon-point modified fluorescent fiber composite material through an extrusion tabletting method.
The molecular retention of the dialysis membrane in step S1 is MWCO:1000.
The carbon source raw material in the step S1 is one or more of citric acid, acrylic acid, glucose, amino acid, vitamin, lignin, starch, protein, polyurethane, polyacrylamide and polyethylene glycol.
The heteroatom doping raw materials in the step S1 are one or more of phenylenediamine, ethylenediamine, polyethyleneimine, o-phenylenediamine dimer, urea, ammonia water, amino acid, silane, 2-amino thiophenol, phosphoric acid and melamine.
The solvent in the step S1 is one or a mixture of more of water, urea and ethanol.
The fiber base material in the step S1 is one or a mixture of more of polyester fiber, polyacrylonitrile fiber, nylon fiber, aramid fiber, nylon, terylene, acrylon, spandex, vinylon, polypropylene fiber, polyvinyl chloride fiber and soybean fiber.
Example 1
1) Mixing 5g of citric acid and 3g of ethylenediamine in deionized water to form a uniform solution, transferring the solution into a high-pressure reaction kettle taking polytetrafluoroethylene as a lining, sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into an oven, setting the reaction temperature to 180 ℃, setting the reaction time to be 6 hours, closing the oven after the reaction is finished, and cooling the reaction kettle to room temperature to obtain yellowish-brown liquid;
2) Transferring the product into ultrapure water, stirring uniformly, centrifuging at 10000rpm for 30min to remove larger particle impurities, placing the filtrate in a refrigerator, refrigerating for 12h, filtering with a 2um filter membrane to remove insoluble substances, and removing the insoluble substances with a dialysis membrane (molecular cut-off amount is MWCO:1000 Dialyzing the yellow supernatant for 24 hours, and replacing ultrapure water every 4 hours to remove unreacted raw materials, thereby finally obtaining a carbon dot aqueous solution with the average particle size of 5.7 nm;
3) Putting the polyester fiber with the length of 16mm into absolute ethyl alcohol, performing ultrasonic treatment for 2 hours, then washing with deionized water, and drying for later use;
4) Placing 3g of polyester fiber with 30mL of carbon dot solution after surface modification into a 80mL high-pressure reaction kettle with a polytetrafluoroethylene lining, adding 10mL of deionized water to ensure that the fiber is immersed into the liquid, sealing the high-pressure reaction kettle and reacting for 8 hours at 180 ℃ in an oven, taking out a sample after the reaction kettle is cooled, carrying out suction filtration, washing for 8 times with the deionized water until filtrate has no fluorescent reaction, and drying the obtained fiber in a vacuum drying oven at 50 ℃ for 12 hours to finally obtain the fluorescent fiber with the length of 8mm;
5) 3g of synthesized fluorescent fiber, 10ml of surface wetting agent, 0.003 surfactant and 200ml of absolute ethyl alcohol are mixed and ultrasonically treated for 4 hours, and after suction filtration, the mixture is dried for 18 hours;
6) The preparation method comprises the following steps of: polyethylene: 85 parts; PE-g-MAH:10 parts; antioxidant CA:0.6 parts; antioxidant DNP:0.4 parts;
the liquid metering pump is used for metering the feeding device to a feeding area of the high-speed mixer, and the feeding area is fully and uniformly mixed in the high-speed mixer;
7) Extruding and granulating the blend by using a double-screw extruder, and respectively setting the temperature of each heating section as follows: the first section is 160 ℃, the second section is 170 ℃, the third section is 180 ℃, the fourth section is 200 ℃, and the fifth section is 200 ℃;
8) Vacuum drying the granulated carbon-point modified fluorescent fiber composite material for 12 hours at 50 ℃ to ensure that the water content is less than or equal to 0.1wt% to obtain composite resin granules;
9) Adding the fluorescent fiber subjected to surface treatment and the composite resin into a high-speed blender, adding 5 parts of white oil, and fully and uniformly mixing;
10 And then adding the resin granules adsorbed with the fluorescent fibers into a surface layer cylinder by using an extrusion sheet machine, and obtaining the carbon point modified composite material by using an extrusion tabletting method.
Example 2
1) Mixing 4g of citric acid and 2g of polyethyleneimine in 30mL of deionized water to form a uniform solution, transferring the solution into a high-pressure reaction kettle taking polytetrafluoroethylene as a lining, sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into a baking oven, setting the reaction temperature to 160 ℃, setting the reaction time to 10 hours, closing the baking oven after the reaction is finished, and cooling the reaction kettle to room temperature to obtain yellowish-brown liquid;
2) The product was transferred to ultrapure water, stirred well and centrifuged at 8000rpm for 30min to remove larger particulate impurities, the filtrate was placed in a refrigerator for cold storage for 12h, and insoluble matter was removed by filtration with a 2um filter membrane, and a dialysis membrane (molecular cut-off amount is MWCO:1000 Dialyzing the yellow supernatant for 24 hours, and replacing ultrapure water every 4 hours to remove unreacted raw materials, thereby finally obtaining a carbon dot aqueous solution with the average particle size of 6.3 nm;
3) Putting the polyester fiber with the length of 8mm into absolute ethyl alcohol, performing ultrasonic treatment for 3 hours, then washing with deionized water, and drying for later use;
4) Placing 3g of polyester fiber with clean surface and 30mL of carbon dot solution into a high-pressure reaction kettle, adding 10mL of deionized water to ensure that the fiber is immersed into the liquid, sealing the high-pressure reaction kettle, reacting for 10 hours at 160 ℃ in an oven, cooling, filtering, washing until the fiber is neutral, and drying the obtained fiber for 12 hours at 80 ℃ to finally obtain the fluorescent fiber with the length of 4 mm;
5) 3g of synthesized fluorescent fiber, 10ml of surface wetting agent, 0.004 surfactant and 200ml of absolute ethyl alcohol are mixed and ultrasonically treated for 4 hours, and after suction filtration, the mixture is dried for 16 hours;
6) Mixing the following components in percentage by mass: polypropylene: 76 parts; PP-g-MAH:20 parts;
the liquid metering pump is used for metering the feeding device to a feeding area of the high-speed mixer, and the feeding area is fully and uniformly mixed in the high-speed mixer;
7) Extruding and granulating the blend by using a double-screw extruder, and respectively setting the temperature of each heating section as follows: first section 160 ℃, second section 175 ℃, third section 175 ℃, fourth section 180 ℃, and fifth section 180 ℃;
8) Vacuum drying the granulated resin for 24 hours at 80 ℃ to ensure that the water content is less than or equal to 0.1 weight percent, thus obtaining composite resin granules;
9) Adding the fluorescent fiber subjected to surface treatment and the composite resin into a high-speed blender, adding 5 parts of white oil, and fully and uniformly mixing;
10 And then adding the resin granules adsorbed with the fluorescent fibers into a surface layer cylinder by using an extrusion sheet machine, and obtaining the carbon point modified composite material by using an extrusion tabletting method.
Example 3
1) Mixing 5g of acrylic acid and 3g of ethylenediamine in 30mL of deionized water to form a uniform solution, transferring the solution into a high-pressure reaction kettle taking polytetrafluoroethylene as a lining, sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into a baking oven, setting the reaction temperature to 180 ℃, setting the reaction time to be 10 hours, closing the baking oven after the reaction is finished, and cooling the reaction kettle to room temperature to obtain yellowish-brown liquid;
2) The product was transferred to ultrapure water, stirred uniformly and centrifuged at 10000rpm for 25min to remove larger particulate impurities, the filtrate was placed in a refrigerator and refrigerated for 12h, insoluble matters were removed by filtration with a 1um filter membrane, and the residue was purified by dialysis membrane (molecular cut-off amount is MWCO:1000 Dialyzing the yellow supernatant for 24 hours, and replacing ultrapure water every 4 hours to remove unreacted raw materials, thereby finally obtaining a carbon dot aqueous solution with the average particle size of 5.8 nm;
3) Putting polyacrylonitrile fiber with the length of 6mm into absolute ethyl alcohol, performing ultrasonic treatment for 1h, then washing with deionized water, and drying for later use;
4) Placing 3g of polyacrylonitrile fiber with clean surface and carbon dot powder into a high-pressure reaction kettle, adding 40mL of deionized water to ensure that the fiber is immersed into liquid, sealing the high-pressure reaction kettle, reacting for 8 hours at 175 ℃ in an oven, cooling, filtering, washing until the fiber is neutral, and drying the obtained fiber for 12 hours at 60 ℃ to finally obtain the fluorescent fiber with the length of 6 mm;
5) 3g of synthesized fluorescent fiber, 10ml of surface wetting agent, 0.004 surfactant and 200ml of absolute ethyl alcohol are mixed and ultrasonically treated for 4 hours, and after suction filtration, the mixture is dried for 16 hours;
6) Mixing the following components in percentage by mass: polypropylene: 78.6 parts; PP-g-ST:18 parts of a mixture of two or more components,
The liquid metering pump is used for metering the feeding device to a feeding area of the high-speed mixer, and the feeding area is fully and uniformly mixed in the high-speed mixer;
7) Extruding and granulating the blend by using a double-screw extruder, and respectively setting the temperature of each heating section as follows: first section 160 ℃, second section 175 ℃, third section 175 ℃, fourth section 180 ℃, and fifth section 180 ℃;
8) Vacuum drying the granulated resin for 24 hours at 80 ℃ to ensure that the water content is less than or equal to 0.1 weight percent, thus obtaining composite resin granules;
9) Adding the fluorescent fiber subjected to surface treatment and the composite resin into a high-speed blender, adding 5 parts of white oil, and fully and uniformly mixing;
10 And then adding the resin granules adsorbed with the fluorescent fibers into a surface layer cylinder by using an extrusion sheet machine, and obtaining the carbon point modified composite material by using an extrusion tabletting method.
Example 4
1) Mixing 4g of starch and 3g of urea in 30mL of deionized water to form a uniform solution, transferring the solution into a high-pressure reaction kettle taking polytetrafluoroethylene as a lining, sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into a baking oven, setting the reaction temperature to be 200 ℃, setting the reaction time to be 10 hours, closing the baking oven after the reaction is finished, and cooling the reaction kettle to room temperature to obtain yellowish-brown liquid;
2) The product was transferred to ultrapure water, stirred well and centrifuged at 9000rpm for 30min to remove larger particulate impurities, the filtrate was placed in a refrigerator for cold storage for 12h, insoluble matter was removed by filtration with a 2um filter membrane, and the residue was purified by dialysis membrane (molecular cut-off amount is MWCO:1000 Dialyzing the yellow supernatant for 24 hours, and replacing ultrapure water every 4 hours to remove unreacted raw materials, thereby finally obtaining a carbon dot aqueous solution with the average particle size of 7.8 nm;
3) Putting nylon fiber with the length of 12mm into absolute ethyl alcohol, performing ultrasonic treatment for 2 hours, then washing with deionized water, and drying for later use;
4) Placing 3g of nylon fiber with clean surface and 30mL of carbon dot solution into a high-pressure reaction kettle, adding 10mL of deionized water to ensure that the fiber is immersed into the liquid, sealing the high-pressure reaction kettle, reacting for 10 hours at 190 ℃ in an oven, cooling, filtering, washing until the fiber is neutral, and drying the obtained fiber for 12 hours at 70 ℃ to finally obtain the fluorescent fiber with the length of 5 mm;
5) 3g of synthesized fluorescent fiber, 10ml of surface wetting agent, 0.004 surfactant and 200ml of absolute ethyl alcohol are mixed and ultrasonically treated for 4 hours, and after suction filtration, the mixture is dried for 16 hours;
6) Mixing the following components in percentage by mass: polyethylene terephthalate: 81 parts; POE-g-MAH:15 parts of a mixture of two or more components,
The liquid metering pump is used for metering the feeding device to a feeding area of the high-speed mixer, and the feeding area is fully and uniformly mixed in the high-speed mixer;
7) Extruding and granulating the blend by using a double-screw extruder, and respectively setting the temperature of each heating section as follows: first section 160 ℃, second section 175 ℃, third section 175 ℃, fourth section 180 ℃, and fifth section 180 ℃;
8) Vacuum drying the granulated resin for 24 hours at 80 ℃ to ensure that the water content is less than or equal to 0.1 weight percent, thus obtaining composite resin granules;
9) Adding the fluorescent fiber subjected to surface treatment and the composite resin into a high-speed blender, adding 5 parts of white oil, and fully and uniformly mixing;
10 And then adding the resin granules adsorbed with the fluorescent fibers into a surface layer material cylinder through a sheet extruder, and preparing the carbon point modified fluorescent fiber composite material through extrusion tabletting.
Example 5
1) Mixing 5g of glucose and 2g of polyethylenimine in 35mL of deionized water to form a uniform solution, transferring the solution into a high-pressure reaction kettle taking polytetrafluoroethylene as a lining, sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into a baking oven, setting the reaction temperature to be 180 ℃, setting the reaction time to be 10 hours, closing the baking oven after the reaction is finished, and cooling the reaction kettle to room temperature to obtain yellowish-brown liquid;
2) The product was transferred to ultrapure water, stirred uniformly and centrifuged at 10000rpm for 25min to remove larger particulate impurities, the filtrate was placed in a refrigerator to cool for 24 hours, and insoluble matters were removed by filtration with a 1um filter membrane, and a dialysis membrane (molecular cut-off amount is MWCO:1000 Dialyzing the yellow supernatant for 24 hours, and replacing ultrapure water every 4 hours to remove unreacted raw materials, thereby finally obtaining a carbon dot aqueous solution with the average particle size of 8.3 nm;
3) Putting the aramid fiber with the length of 8mm into absolute ethyl alcohol, performing ultrasonic treatment for 4 hours, then washing with deionized water, and drying for later use;
4) Placing 3g of polyester fiber with clean surface and carbon dot powder into a high-pressure reaction kettle, adding 30mL of deionized water to ensure that the fiber is immersed into liquid, sealing the high-pressure reaction kettle, reacting for 10 hours at 175 ℃ in an oven, cooling, filtering, washing until the fiber is neutral, and drying the obtained fiber for 12 hours at 80 ℃ to finally obtain the fluorescent fiber with the length of 6mm;
5) 3g of synthesized fluorescent fiber, 10ml of surface wetting agent, 0.004 surfactant and 200ml of absolute ethyl alcohol are mixed and ultrasonically treated for 4 hours, and after suction filtration, the mixture is dried for 16 hours;
6) Mixing the following components in percentage by mass: carbon dot modified fluorescent fiber: 0.8 parts; polyethylene: 78.6 parts; PE-g-ST:18 parts of a mixture of two or more components,
The liquid metering pump is used for metering the feeding device to a feeding area of the high-speed mixer, and the feeding area is fully and uniformly mixed in the high-speed mixer;
7) Extruding and granulating the blend by using a double-screw extruder, and respectively setting the temperature of each heating section as follows: first section 160 ℃, second section 175 ℃, third section 175 ℃, fourth section 180 ℃, and fifth section 180 ℃;
8) Vacuum drying the granulated resin for 24 hours at 80 ℃ to ensure that the water content is less than or equal to 0.1 weight percent, thus obtaining composite resin granules;
9) Adding the fluorescent fiber subjected to surface treatment and the composite resin into a high-speed blender, adding 5 parts of white oil, and fully and uniformly mixing;
10 And then adding the resin granules adsorbed with the fluorescent fibers into a surface layer cylinder by using an extrusion sheet machine, and obtaining the carbon point modified composite material by using an extrusion tabletting method.
The reaction equation involved in the invention is:
in the present invention,
1) The security information marker is difficult to separate. The nanometer organic fluorescent fiber is obtained by adopting a chemical loading mode for fluorescent marking, the migration rate of the used fluorescent substance is extremely low, and the sampling separation and the component analysis cannot be carried out by adopting the existing analytical instrument. The anti-counterfeiting performance is incomparable with the traditional anti-counterfeiting technology, and has huge market potential.
2) Successfully combines fluorescent fibers with a resin matrix into a whole with a continuous phase structure through thermoplastic processing. The anti-fake information markers such as the nano structure and the fluorescent substance are difficult to separate, and the anti-fake information marker is suitable for global anti-fake of the resin composite material, improves the overall technical safety and effectively avoids illegal control and anti-fake information theft.
3) And avoid fluorescence quenching phenomenon caused by thermal processing. The single fiber dispersion of the nano fluorescent fiber in the resin base material is realized in the thermal processing process through the treatment of the surfactant and the antioxidant, the fluorescence quenching phenomenon caused by thermal processing is avoided, the compatibility among the components is effectively improved through the addition of the compatilizer, the core problem of poor compatibility of the anti-counterfeiting base material and the matrix material is solved, and the design and the molding of the fluorescent fiber anti-counterfeiting sheet are realized.
4) The carbon-point modified fluorescent fiber composite anti-counterfeiting sheet has the characteristics of good concealment, easy identification, stable performance and the like of the traditional fluorescent anti-counterfeiting material, has a special anti-counterfeiting function, has fluorescent characteristics and a fiber structure without affecting the basic properties of the sheet, and has the first-line and second-line anti-counterfeiting functions.
Referring to FIG. 1, FIG. 1 is an infrared spectrum of a carbon dot nanoparticle of the present invention, wherein (a) CDs; (b) PANF; (c) PANF-g-CDs, analyzing the CDs, PANF and PANF-g-CDs by using a Fourier infrared spectrometer, and finding that obvious characteristic peaks exist at 1643cm < -1 >, 1560cm < -1 >, 1470cm < -1 > and 1389cm < -1 > in the infrared spectrogram of the CDs. According to the related data, the peak at 1643cm-1 is assigned to the C=O stretching vibration peak, the characteristic peak at 1560cm-1 is assigned to the N-H bending vibration peak, the peak at 1470cm-1 is assigned to the C=H stretching vibration peak, and the peak at 1389cm-1 is assigned to the C-N stretching vibration peak. The PANF infrared spectrogram has obvious characteristic peaks at 2956cm-1 and 1731 cm-1. According to the related data, the peak at 2956cm-1 was assigned to the-C.ident.N stretching vibration peak, and the peak at 1731cm-1 was assigned to the C-H bending vibration peak. PAN-g-CDs compared to PAN, PAN-g-CDs showed two new characteristic peaks at 1479cm-1 and 1271cm-1, corresponding to the N-H and N-C stretching vibrations on the secondary amide, respectively, indicating that CDs were successfully grafted onto PAN.
Referring to fig. 2, fig. 2 is a graph showing the average particle size distribution of the carbon dot nanoparticles according to the present invention, and the result of the particle size distribution test by a dynamic light scattering meter shows that the carbon dot particles are uniformly distributed, indicating that the carbon dot has good dispersibility in an aqueous solution, no agglomeration occurs, the particle size distribution of the carbon dot is narrower, the particle size is uniform, and the average particle size is 5.5nm.
Referring to fig. 3, fig. 3 shows excitation spectra of the carbon dot modified fluorescent fiber and the surface-treated fluorescent fiber, and the emission peak is observed to be at 460nm under ultraviolet excitation of 340nm, which indicates that the fluorescent fiber can emit blue-violet fluorescence under ultraviolet irradiation of 340nm, and the fluorescence intensity of the surface-treated fiber is slightly improved without changing the wavelength.
Referring to fig. 4, 5 and 6, fig. 4, 5 and 6 are scanning electron microscope images of the carbon dot modified fluorescent fiber after surface treatment and the resin containing the compatilizer with different dosages, and it can be seen that the bonding performance of the fiber material and the matrix after modification is effectively improved along with the improvement of the compatilizer capacity.
Referring to fig. 7, fig. 7 is a graph showing contact angle test of neat PP, with angles of 63.52 ° 68.68 ° 67.30 ° in order, and the measured solid surface energy calculated according to the equation according to the Berthelot rule was 35.6mJ/m.
Referring to FIG. 8, FIG. 8 is a graph of a PP contact angle test with 10% PP-g-MAH, at angles of 60.99 ℃63.29℃ 61.70 ℃in order, and the measured solid surface energy was calculated to be 39.3mJ/m according to the equation given by the Berthelot rule.
Referring to FIG. 9, FIG. 9 is a graph showing a contact angle test of PP containing 15% PP-g-MAH at an angle of 53.17℃ 53.14 ℃ 54.01 ℃in order, and the measured solid surface energy was calculated to be 46.1mJ/m according to the equation given by the Berthelot rule
FIG. 10 is a graph showing the surface energy of the fluorescent fiber after the surface treatment according to the present invention, wherein the surface energy of the fluorescent fiber is 41-44 mJ/m, which is similar to the resin with 15% of the content of the compatibilizer.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (6)
1. The fluorescent fiber composite material is characterized by comprising the following raw materials in parts by weight: 0.1 to 1 part of carbon dot modified fluorescent fiber; 50-99 parts of thermoplastic resin; 0.0001 to 0.001 part of surfactant; 0.001-5 parts of surface wetting agent; 1-20 parts of compatilizer; the carbon dot particle diameter of the carbon dot modified fluorescent fiber is 5-10 nm, the fiber diameter of the carbon dot modified fluorescent fiber is 0.1-20 mu m, and the fiber length of the carbon dot modified fluorescent fiber is 0.5-20 mm;
the preparation method comprises the following steps:
S1, preparing carbon point modified fluorescent fibers:
1) Synthesis of carbon dots: mixing a carbon source raw material for synthesizing carbon points and a heteroatom doping raw material in a solvent to form a uniform solution, transferring the solution into a high-pressure reaction kettle taking polytetrafluoroethylene as a lining, sealing the high-pressure reaction kettle, putting the high-pressure reaction kettle into a baking oven, setting the reaction temperature to be 60-200 ℃, reacting for 4-10 hours, closing the baking oven after the reaction is finished, and cooling the reaction kettle to room temperature to obtain yellowish-brown liquid;
2) Separation of carbon dots: transferring the product into deionized water, stirring uniformly, centrifuging at 5000-10000 rpm for 15-30 min to remove larger particle impurities, filtering with a 0.1-10 um filter membrane to remove insoluble substances, dialyzing the yellow supernatant with a dialysis membrane for 24h, and replacing deionized water every 4h to remove unreacted raw materials, thereby finally obtaining an aqueous solution with a carbon point of 5-10 nm in size;
3) Surface treatment of fibrous substrates: putting the fiber substrate with the length of 3-20 mm into absolute ethyl alcohol, performing ultrasonic treatment for 0.5-3 h, then cleaning with deionized water, and drying for later use;
4) Preparation of fluorescent fibers: placing 1-5 g of surface modified fiber and 30-45 mL of carbon dot solution into 80mL of high-pressure reaction kettle with polytetrafluoroethylene lining, adding 10-20 mL of deionized water to ensure that the fiber is immersed into the liquid, sealing the high-pressure reaction kettle and reacting for 4-10 hours at 60-200 ℃ in an oven, taking out a sample after the reaction kettle is cooled, carrying out suction filtration, washing for 5-10 times with the deionized water until the filtrate has no fluorescent reaction, and drying the obtained fiber in a vacuum drying oven at 40-60 ℃ for 12-48 hours to finally obtain fluorescent fiber with the length of 3-20 mm;
S2, preparing a finished product:
1) Adding the thermoplastic resin and the compatilizer into a feeding area of a high-speed mixer through a liquid metering pump quantitative feeding device according to mass components, and fully and uniformly mixing in the high-speed mixer;
2) Extruding and granulating the blend by using a double-screw extruder, and respectively setting the temperature of each heating section as follows: the first stage is 150-200 ℃, the second stage is 155-200 ℃, the third stage is 160-200 ℃, the fourth stage is 165-200 ℃, and the fifth stage is 170-200 ℃;
3) Vacuum drying the granulated composite material at 50-80 ℃ for 12-24h to ensure that the water content is less than or equal to 0.1wt% to obtain resin granules;
4) Mixing 1-5 g of synthesized fluorescent fiber, 5-15 ml of surface wetting agent, 0.001-0.05 g of surfactant and 100-300 ml of absolute ethyl alcohol for ultrasonic treatment for 2-6 hours, and drying for 10-24 hours after suction filtration;
5) Fully and uniformly mixing the fluorescent fibers subjected to surface treatment with resin granules in a high-speed mixer;
6) Adding resin granules adsorbed with fluorescent fibers into a surface layer material cylinder through a sheet extruder, and preparing the carbon-point modified fluorescent fiber composite material through an extrusion tabletting method;
The thermoplastic resin is one or a mixture of more of polyolefin, polyester, polyvinyl alcohol, nylon and biodegradable resin; the compatilizer is one or a mixture of more of polyolefin resin grafted maleic anhydride, polyolefin resin grafted acrylic acid and epoxy resin grafted polyamide.
2. The fluorescent fiber composite according to claim 1, wherein the surface wetting agent is one or more of nekal BX, K12, K14, KMT-7001 and industrial white oil.
3. The method for assembling and forming the interface micro-nano of the fluorescent fiber composite material according to claim 1, wherein the molecular retention of the dialysis membrane in the step S1 is MWCO:1000.
4. The method for assembling and forming the interface micro-nano of the fluorescent fiber composite material according to claim 1, wherein the carbon source raw material in the step S1 is one or more of citric acid, acrylic acid, glucose, amino acid, vitamin, lignin, starch, protein, polyurethane, polyacrylamide and polyethylene glycol.
5. The method for assembling and forming the interface micro-nano of the fluorescent fiber composite material according to claim 1, wherein the heteroatom doping raw material in the step S1 is one or a mixture of more of phenylenediamine, ethylenediamine, polyethyleneimine, o-phenylenediamine dimer, urea, ammonia water, amino acid, silane, 2-aminophenylthiophenol, phosphoric acid and melamine.
6. The method for assembling and forming the interface micro-nano of the fluorescent fiber composite material according to claim 1, wherein the solvent in the step S1 is one or more of water, urea and ethanol; the fiber base material in the step S1 is one or a mixture of more of polyester fiber, polyacrylonitrile fiber, nylon fiber, aramid fiber, nylon fiber, terylene, acrylic fiber, spandex, vinylon fiber, polypropylene fiber, chloridion fiber and soybean fiber.
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