CN105949622A - Nano fluorescent fiber anti-counterfeiting film and preparation method thereof - Google Patents
Nano fluorescent fiber anti-counterfeiting film and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of functional composite materials and particularly relates to a nano fluorescent fiber anti-counterfeiting film and a preparation method thereof. The nano fluorescent fiber anti-counterfeiting film is prepared from, by weight, 5-30 parts of nano fiber, 50-95 parts of resin, 0.1-20 parts of compatilizer, 0.1-1.5 parts of antistatic agent and 0.1-1.5 parts of lubricating agent. The mass of a fluorescent dye accounts for 5-50% the mass of nano fiber. The nano fluorescent fiber anti-counterfeiting film has the advantages of being good in hiding performance, easy to identify, stable in performance and the like of traditional fluorescent anti-counterfeiting materials, and also has a special anti-counterfeiting function. Consumers can use a traditional ultraviolet lamp for easy identification, professional technicians can use professional instruments for professional detection, the film integrates the first-line anti-counterfeiting function and the second-line anti-counterfeiting function, the anti-counterfeiting efficiency and strength are effectively improved, application value is outstanding, and social benefits are good.
Description
Technical field
The invention belongs to functional composite material field, be specifically related to a kind of nano fluorescence fiber false-proof film and preparation method thereof.
Background technology
Luminescent fibre is a kind of fiber that can be luminous under visible ray or special light irradiate, can divide according to the character difference that light irradiates
For phosphorescence fiber and fluorescent fiber two kinds.Wherein, fluorescent fiber is to be blended inorganic or organic fluorescence colorant or be grafted on fiber to gather
In compound matrix so that fibrous material has fluorescent effect.Fluorescent fiber has good anti-fake effect, can be as safety fibre
It is widely used in camouflage, road and the protective garment of work high above the ground, article of everyday use, extraordinary sensitive material and information storing material etc.
Multi-field.
Plastic sheeting as a kind of important macromolecular material can be applicable to agricultural, chemical industry, print, packaging etc. multi-field, be to mould
In material material, one of widest kind of range of application, can be divided into blown film, casting films and biaxial stretching film three kinds by production technology.
Biaxial stretching film is most important one in three big plastic sheeting types, through biaxial tension in its course of processing, then in length and breadth two
Direction is height-oriented, therefore has good physical stability, a mechanical strength, preferable barrier, transparency and glossiness,
Tough and hard wear resistant, is current most widely used printing, packaging film material.
Prepare, by stretch processes, the production method that false-proof film material is a kind of most industrialization meaning, there is higher life
Produce efficiency and stable product quality and false proof usefulness.But, compared with other anti-fake materials such as anti-forge paper, false-proof film
Preparing complex, its industrialized production is the most increasingly difficult under many circumstances, its main cause be macromolecular material performance very
Special, the processing of simple physical blending is often difficult to solve its consistency problem, it is impossible to obtaining preferable composite, this is very
Big degree limits production and the application of false-proof film.
Summary of the invention
The goal of the invention of the present invention is for the deficiencies in the prior art, it is provided that a kind of nano fluorescence fiber false-proof film and preparation side thereof
Method.
For achieving the above object, the technical solution used in the present invention is:
A kind of nano fluorescence fiber false-proof film, its raw material components is by mass percentage: nanofiber 5wt%～30wt%,
Fluorescent dye 0.25wt%～15wt%, resin 50wt%～95wt%, compatilizer 0.1wt%～20wt%, antistatic additive 0.1
Wt%～1.5wt%, lubricant 0.1wt%～1.5wt%.
In such scheme, described nanofiber be polyacrylonitrile, polyester, polyamide, polystyrene, polymethyl methacrylate,
One or more in Merlon, Polycarbosilane, polyether sulfone and polyvinyl alcohol.
In such scheme, a diameter of the 10 of described nanofiber～100nm, a length of 0.5～5.0mm, softening temperature is
190～250 DEG C, melt temperature is 220～320 DEG C.
In such scheme, described fluorescent dye is rare earth, Rare Earth Derivatives, fluorescein, fluorescein derivative, rhodamine and sieve
One or more in red bright derivant.
In such scheme, described resin is in polyester, polypropylene, polyamide, polystyrene, polyethylene and polyvinyl alcohol
Plant or several.
In such scheme, described compatilizer is polyolefin elastomer class, multi-monomer grafting modified phenylethylene based elastomers class and Malaysia
One or more of acid anhydride-grafted apoplexy due to endogenous wind.
In such scheme, described antistatic additive is quaternary ammonium salt, alkyl sulfonates, fatty acid and alkyl betaine apoplexy due to endogenous wind
One or more.
In such scheme, described lubricant be saturated hydrocarbons, halogenated hydrocarbon, fatty acid, aliphatic alcohols, aliphatic amide type,
One or more in fatty acid ester, aliphatic alcohols, metal soap and polyalcohols.
The preparation method of above-mentioned nano fluorescence fiber false-proof film, comprises the steps:
(1) nanofiber is dissolved in solvent and is prepared as the spinning solution that concentration is 5～50%；
(2) syringe that spinning solution is injected into high-voltage electrostatic spinning machine connects high-voltage power cathode, using aluminium foil as reception
Plate connects negative pole, starts circulation silicone oil heating mantle, controls spinning solution quantity delivered by dosing pump, connects conical flask and collects spinning
During volatilization solvent, prepared the nanofiber of entanglement by spinning technique；
(3) utilize fluorescent dye that nanofiber is carried out chemical staining, make fluorescent dye be grafted on nanofiber surface, then with
Solvent fully extracts the unreacted fluorescent dye of removal, prepares the nano fluorescence fiber with fluorescent characteristic after vacuum drying；
(4) utilize surfactant that nano fluorescence fiber carries out pretreatment: by fine to surfactant and nano fluorescent
Dimension joins in dehydrated alcohol, after high speed emulsion dispersion, prepares nano fluorescence fiber dispersion liquid；
(5) in nano fluorescence fiber dispersion liquid, add resin, compatilizer, antistatic additive and lubricant, be dried after mixing and make
Grain, obtains hybrid resin；
(6) by stretch processes, gained hybrid resin is prepared as nano fluorescence fiber false-proof film.
In such scheme, the parameter of step (2) described spinning technique is: voltage is set as 10～30KV, and spinning temperature sets
Being 20～50 DEG C, the jet velocity of dosing pump is set as 0.001～0.5mm/min, and ambient temperature is set as 20～30 DEG C.
In such scheme, step (6) described stretch processes is: setting feeding section temperature 140～190 DEG C, compression section
170～240 DEG C, melt zone 185～260 DEG C, homogenizing zone 170～240 DEG C, metering section 160 DEG C～230 DEG C, in extruder, make thing
Material fully plastifies and mixes, and sets the mold body sections 160 DEG C～190 DEG C of head, mouth die section 160 DEG C～230 DEG C, sets slab
Roll temperature 160 DEG C～230 DEG C, sharp cooling roll temperature 20 DEG C～40 DEG C；Thin film after cooling enters the vertical section of drawing, at the roller of vertical machine drawing
Carry out the thin slice of preheating under speed difference effect indulging and draw, longitudinal drawing temperature 80 DEG C～160 DEG C, longitudinal stretching multiple 2.5～5.5 times,
Utilize thickness measuring gantry to measure and control sheet thickness and keep Uniform Tension；Subsequently into the horizontal section of drawing, transverse stretching machine clamper is clamped thin
Sheet edge makes it laterally broaden by the track of definite shape, horizontal tentering temperature 100 DEG C～180 DEG C, horizontal Lapie 3.0～10,
Utilize thickness measuring gantry to measure and control film thickness and keep Uniform Tension, heat setting temperature 160 DEG C～230 DEG C；Through biaxial tension
Thin film through chill roll, the most expanded roller of thin film being drawn off, flatten thin film, be allowed to cool down completely and relax, it is to avoid adhesion
And contraction, last rolling device carries out rolling.
The false-proof film produced by preparation method of the present invention be may utilize fluorescence spectrophotometer and excitation spectrum detected, and
200～380nm ultraviolet light spectral coverages and 380～780nm visible spectrum have different fluorescent absorption peaks, utilize polarizing microscope,
Scanning electron microscope can be observed diameter 10～100nm, the nanofibrous structures of length 0.5～5.0mm.
Beneficial effects of the present invention: nano fluorescence fiber false-proof film of the present invention is disguised except having conventional fluorescent anti-fake material
Well, it is prone to the features such as discriminating, stable performance, also there is special antiforge function, do not affecting the same of thin-film material key property
Time have fluorescent characteristic and nanofibrous structures concurrently, consumer may utilize traditional UV lamps and simply differentiates, on this basis specialty
Technical staff may also be combined with the special instrument such as fluorescence spectrophotometer, polarizing microscope and scanning electron microscope and carries out specialty detection, from
And make nano fluorescence fiber false-proof film have a line, two wires antiforge function concurrently, its false proof usefulness and dynamics can be effectively improved, have
Prominent using value and good social benefit.
Accompanying drawing explanation
The high-voltage electrostatic spinning process schematic of a kind of nano fluorescence fiber false-proof film that Fig. 1 is involved in the present invention.
The nanofiber scanning electron microscope diagram that a kind of nano fluorescence fiber false-proof film involved in the present invention for Fig. 2 tangles.
The production process schematic diagram of a kind of nano fluorescence fiber false-proof film that Fig. 3 the present invention relates to.
Detailed description of the invention
In order to be more fully understood that the present invention, it is further elucidated with present disclosure below in conjunction with embodiment, accompanying drawing, but the present invention
Content is not limited solely to the following examples.
In following example, described high-voltage electrostatic spinning process as shown in Figure 1:
(1) syringe 2 that the spinning solution 1 configured injects high-voltage electrostatic spinning machine connects high-voltage power cathode 3, with
Aluminium foil connects negative pole 5 as receiving plate 4, and setting voltage is 10～30KV；
(2) starting circulation silicone oil heating mantle 6, sets spinning temperature as 20～50 DEG C, connection conical flask 7 collects spinning process
The solvent 8 of middle volatilization；
(3) open dosing pump 9 to be extruded by spinning solution 1 in syringe 2, set jet velocity as 0.001～0.5m m/min,
Keeping ambient temperature is 20～30 DEG C；
(4) with microscope slide, nanofiber 10 is carried out stochastic sampling, utilize its structure of polarized light microscope observing and size, and
Regulation voltage and jet velocity, make the nanofiber 10 preparing entanglement meet requirement accordingly.
Carry out high-voltage electrostatic spinning by above-mentioned processing step and can form receiving of having that smooth planar surface and relatively big L/D ratio tangle
Rice fiber 10 (nanofiber scanning electron microscope diagram is shown in Fig. 2), its a diameter of 10～100nm, a length of 0.5～5.0mm.
The production process of nano fluorescence fiber false-proof film as shown in Figure 3, can carry out the continuous of this false-proof film and produce:
(1) in nano fluorescence fiber dispersion liquid, add resin, compatilizer, antistatic additive and lubricant, be dried after mixing and make
Grain, obtains hybrid resin；
(2) hybrid resin is added the loading hopper 2 of extruder 1, setting feeding section temperature 140～190 DEG C, compression section
170～240 DEG C, melt zone 185～260 DEG C, homogenizing zone 170～240 DEG C, metering section 160 DEG C～230 DEG C, in extruder, make thing
Material fully plastifies and mixes, and sets the mold body sections 160 DEG C～190 DEG C of head 3, mouth die section 160 DEG C～230 DEG C, sets casting
Sheet roller 4 temperature 160 DEG C～230 DEG C, sharp cooling roll temperature 20 DEG C～40 DEG C；Thin film after cooling enters the vertical section of drawing, in vertical machine drawing 6
Roller speed difference effect under the thin slice of preheating carried out vertical drawing, longitudinal drawing temperature 80 DEG C～160 DEG C, longitudinal stretching multiple
2.5～5.5 times, utilize thickness measuring gantry 5 to measure and control sheet thickness holding Uniform Tension；Subsequently into the horizontal section of drawing, transverse stretching machine
Chip edge clamped by 7 clampers makes it laterally broaden by the track of definite shape, horizontal tentering temperature 100 DEG C～180 DEG C,
Horizontal Lapie 3.0～10, utilizes thickness measuring gantry 8 to measure and controls film thickness holding Uniform Tension, heat setting temperature 160 DEG C
～230 DEG C；Through the thin film of biaxial tension through chill roll, the most expanded roller of thin film being drawn off, flatten thin film, be allowed to the coldest
But with lax, it is to avoid adhesion and contraction, last rolling device 9 carries out rolling.
Embodiment 1
A kind of nano fluorescence fiber false-proof film, each component proportion is shown in Table 1, is prepared via a method which to obtain:
(1) polyacrylonitrile is dissolved in DMF and prepares the spinning solution that concentration is 7wt%；
(2) syringe that spinning solution injects high-voltage electrostatic spinning machine connects high-voltage power cathode, using aluminium foil as receiving plate
Connecting negative pole, setting voltage is 18KV, starts circulation silicone oil heating mantle, sets spinning temperature as 40 DEG C, connects conical flask receipts
In collection spinning process, the solvent of volatilization, controls spinning solution quantity delivered by dosing pump, sets jet velocity as 0.05mm/min,
Keeping ambient temperature is 20 DEG C, prepares the nanofiber of entanglement；
(3) utilize fluorescein that nanofiber is carried out chemical staining, fluorescein is grafted on nanofiber surface, and with solvent
Unreacted fluorescent dye is removed in fully extracting, is vacuum dried 2h, prepares nano fluorescence fiber；
(4) utilize surfactant (Tween 80) that nano fluorescence fiber carries out pretreatment: by glimmering to surfactant and nanometer
Fiber optics joins in dehydrated alcohol, high speed emulsion dispersion, and rate of dispersion is 7000r/min, prepares nano fluorescence fiber and divides
Dissipate liquid；
(5) in nano fluorescence fiber dispersion liquid, add resin, compatilizer, antistatic additive and lubricant, be dried after mixing and make
Grain, obtains hybrid resin；
(6) by stretch processes, gained hybrid resin is prepared nano fluorescence fiber false-proof film: by hybrid resin
Addition extruder loading hopper, setting feeding section temperature 165 DEG C, 180 DEG C, compression section, melt zone 195 DEG C, homogenizing zone 180 DEG C,
Metering section 165 DEG C, makes material fully plastify and mix in extruder, sets the mold body sections 165 DEG C of head, mouth die section
160 DEG C, set slab roller temperature 160 DEG C, sharp cooling roll temperature 20 DEG C；Thin film after cooling enters the vertical section of drawing, in vertical machine drawing
Under roller speed difference effect, the thin slice of preheating is carried out vertical drawing, longitudinal drawing temperature 80 DEG C, longitudinal stretching multiple 5.5 times, utilizes
Thickness measuring gantry measures and controls sheet thickness and keeps Uniform Tension；Subsequently into the horizontal section of drawing, thin slice limit clamped by transverse stretching machine clamper
Edge makes it laterally broaden by the track of definite shape, horizontal tentering temperature 100 DEG C, and horizontal Lapie 9 utilizes thickness measuring gantry
Measure and control film thickness and keep Uniform Tension, heat setting temperature 160 DEG C；Through the thin film of biaxial tension through chill roll, quilt
The most expanded roller of thin film involved, flattens thin film, is allowed to cool down completely and relax, it is to avoid adhesion and contraction, last rolling dress
Put and carry out rolling and i.e. obtain finished product.
Embodiment 2
A kind of nano fluorescence fiber false-proof film, each component proportion is shown in Table 1, is prepared via a method which to obtain:
(1) polyester is dissolved in hexafluoroisopropanol and prepares the spinning solution that concentration is 10wt%；
(2) syringe injecting high-voltage electrostatic spinning machine is connected high-voltage power cathode by spinning solution, using aluminium foil as receiving plate
Connecting negative pole, setting voltage is 25KV, starts circulation silicone oil heating mantle, sets spinning temperature as 50 DEG C, connects conical flask receipts
In collection spinning process, the solvent of volatilization, controls spinning solution quantity delivered by dosing pump, sets jet velocity as 0.001mm/min,
Keeping ambient temperature is 20 DEG C, prepares the nanofiber of entanglement；
(3) utilize rare earth that nanofiber is carried out chemical staining, rare earth is grafted on nanofiber surface, and fully takes out with solvent
Carry the unreacted fluorescent dye of removal, be vacuum dried 2h, prepare nano fluorescence fiber；
(4) utilize surfactant (sodium lauryl sulphate) that nano fluorescence fiber carries out pretreatment: by surfactant and
Nano fluorescence fiber joins in dehydrated alcohol, high speed emulsion dispersion, and rate of dispersion is 12000r/min, prepares nanometer glimmering
Fiber optics dispersion liquid；
(5) in nano fluorescence fiber dispersion liquid, resin, compatilizer, antistatic additive and lubricant are added, drying-granulating after mixing,
Obtain hybrid resin；
(6) by stretch processes, gained hybrid resin is prepared nano fluorescence fiber false-proof film: added by hybrid resin
Enter extruder loading hopper, set feeding section temperature 155 DEG C, 170 DEG C, compression section, melt zone 185 DEG C, homogenizing zone 170 DEG C, meter
Amount section 155 DEG C, makes material fully plastify and mix in extruder, the mold body sections 155 DEG C of setting head, mouth die section 150 DEG C,
Set slab roller temperature 150 DEG C, sharp cooling roll temperature 20 DEG C；Thin film after cooling enters the vertical section of drawing, at the roller speed of vertical machine drawing
Under difference effect, the thin slice of preheating is carried out vertical drawing, longitudinal drawing temperature 70 DEG C, longitudinal stretching multiple 5 times, utilizes thickness measuring gantry
Measure and control sheet thickness and keep Uniform Tension；Subsequently into the horizontal section of drawing, transverse stretching machine clamper clamps chip edge by certain
The track of shape makes it laterally broaden, horizontal tentering temperature 90 DEG C, and horizontal Lapie 9 utilizes thickness measuring gantry to measure and controls thin
Film thickness keeps Uniform Tension, heat setting temperature 150 DEG C；Through the thin film of biaxial tension through chill roll, the thin film being drawn off is again
Expanded roller, flattens thin film, is allowed to cool down completely and relax, it is to avoid adhesion and contraction, and last rolling device carries out rolling i.e.
Obtain finished product.
Embodiment 3～4
In embodiment 3～4, each component proportion of nano fluorescence fiber false-proof film is shown in Table 1, preparation process substantially with embodiment 2, its
The parameter of middle stretch processes is shown in Table 2.
Embodiment 5
A kind of nano fluorescence fiber false-proof film, each component proportion is shown in Table 1, is prepared via a method which to obtain:
(1) polyacrylonitrile is dissolved in DMF and prepares the spinning solution that concentration is 8wt%；
(2) syringe injecting high-voltage electrostatic spinning machine is connected high-voltage power cathode by spinning solution, using aluminium foil as receiving plate
Connecting negative pole, setting voltage is 19KV, starts circulation silicone oil heating mantle, sets spinning temperature as 40 DEG C, connects conical flask receipts
In collection spinning process, the solvent of volatilization, controls spinning solution quantity delivered by dosing pump, sets jet velocity as 0.10mm/min,
Keeping ambient temperature is 20 DEG C, prepares the nanofiber of entanglement；
(3) utilize fluorescein that nanofiber is carried out chemical staining, fluorescein is grafted on nanofiber surface, and fills with solvent
Divide extracting to remove unreacted fluorescent dye, be vacuum dried 2h, prepare the fluorescent nano-fiber with fluorescent characteristic；
(4) utilize surfactant (dodecylbenzene sodium sulfonate) that nano fluorescence fiber is carried out pretreatment: by surfactant
Joining in dehydrated alcohol with nano fluorescence fiber, high speed emulsion dispersion, rate of dispersion is 7000r/min, prepares nanometer glimmering
Fiber optics dispersion liquid；
(5) in nano fluorescence fiber dispersion liquid, resin, compatilizer, antistatic additive and lubricant are added, drying-granulating after mixing,
Obtain hybrid resin；
(6) by stretch processes, gained hybrid resin is prepared nano fluorescence fiber false-proof film: added by hybrid resin
Enter extruder loading hopper, set feeding section temperature 165 DEG C, 180 DEG C, compression section, melt zone 195 DEG C, homogenizing zone 180 DEG C, meter
Amount section 165 DEG C, makes material fully plastify and mix in extruder, the mold body sections 165 DEG C of setting head, mouth die section 160 DEG C,
Set slab roller temperature 160 DEG C, sharp cooling roll temperature 20 DEG C；Thin film after cooling enters the vertical section of drawing, at the roller speed of vertical machine drawing
Under difference effect, the thin slice of preheating is carried out vertical drawing, longitudinal drawing temperature 80 DEG C, longitudinal stretching multiple 5.5 times, utilizes thickness measuring to scan
Frame measures and controls sheet thickness and keeps Uniform Tension；Subsequently into the horizontal section of drawing, transverse stretching machine clamper clamps chip edge by one
The track of shaped makes it laterally broaden, horizontal tentering temperature 100 DEG C, and horizontal Lapie 9 utilizes thickness measuring gantry to measure and control
Made membrane thickness keeps Uniform Tension, heat setting temperature 160 DEG C；Through the thin film of biaxial tension through chill roll, be drawn off is thin
The most expanded roller of film, flattens thin film, is allowed to cool down completely and relax, it is to avoid adhesion and contraction, and last rolling device is received
Volume i.e. obtains finished product.
Embodiment 6
In the present embodiment, each component proportion of nano fluorescence fiber false-proof film is shown in Table 1, and preparation process is substantially with embodiment 5, wherein
The parameter of stretch processes is shown in Table 2.
Embodiment 7
A kind of nano fluorescence fiber false-proof film, each component proportion is shown in Table 1, is prepared via a method which to obtain:
(1) polymethyl methacrylate is dissolved in acetone and prepares the spinning solution that concentration is 15wt%；
(2) syringe injecting high-voltage electrostatic spinning machine is connected high-voltage power cathode by spinning solution, using aluminium foil as receiving plate
Connecting negative pole, setting voltage is 20KV, starts circulation silicone oil heating mantle, sets spinning temperature as 30 DEG C, connects conical flask receipts
In collection spinning process, the solvent of volatilization, controls spinning solution quantity delivered by dosing pump, sets jet velocity as 0.05mm/min,
Keeping ambient temperature is 25 DEG C, prepares the nanofiber of entanglement；
(3) utilize fluorescein sodium that nanofiber is carried out chemical staining, fluorescein sodium is grafted on nanofiber surface, and with molten
Agent fully extracts the unreacted fluorescent dye of removal, is vacuum dried 2h, prepares the nano fluorescence fiber with fluorescent characteristic；
(4) utilize surfactant (alkyl polyglucoside) that nano fluorescence fiber carries out pretreatment: by glimmering to surfactant and nanometer
Fiber optics joins in dehydrated alcohol, high speed emulsion dispersion, and rate of dispersion is 15000r/min, prepares nano fluorescence fiber
Dispersion liquid；
(5) in nano fluorescence fiber dispersion liquid, resin, compatilizer, antistatic additive and lubricant are added, drying-granulating after mixing,
Obtain hybrid resin；
(6) by stretch processes, gained hybrid resin is prepared nano fluorescence fiber false-proof film: added by hybrid resin
Enter extruder loading hopper, set feeding section temperature 140 DEG C, 200 DEG C, compression section, melt zone 260 DEG C, homogenizing zone 260 DEG C, meter
Amount section 260 DEG C, makes material fully plastify and mix in extruder, the mold body sections 250 DEG C of setting head, mouth die section 230 DEG C,
Set slab roller temperature 230 DEG C, sharp cooling roll temperature 40 DEG C；Thin film after cooling enters the vertical section of drawing, at the roller speed of vertical machine drawing
Under difference effect, the thin slice of preheating is carried out vertical drawing, longitudinal drawing temperature 180 DEG C, longitudinal stretching multiple 2.5 times, utilizes thickness measuring to sweep
Retouch frame measure and control sheet thickness holding Uniform Tension；Subsequently into the horizontal section of drawing, transverse stretching machine clamper is clamped chip edge and is passed through
The track of definite shape makes it laterally broaden, horizontal tentering temperature 200 DEG C, horizontal Lapie 3.5, utilizes thickness measuring gantry to measure also
Control film thickness and keep Uniform Tension, heat setting temperature 230 DEG C；Through the thin film of biaxial tension through chill roll, it is drawn off
The most expanded roller of thin film, flattens thin film, is allowed to cool down completely and relax, it is to avoid adhesion and contraction, and last rolling device is carried out
Rolling i.e. obtains finished product.
Embodiment 8～10
In embodiment 8～10, each component proportion of nano fluorescence fiber false-proof film is shown in Table 1, preparation process substantially with embodiment 7,
Wherein the parameter of stretch processes is shown in Table 2.
Embodiment 11
A kind of nano fluorescence fiber false-proof film, each component proportion is shown in Table 1, is prepared via a method which to obtain:
(1) polyacrylonitrile is dissolved in DMF and prepares the spinning solution that concentration is 9wt%；
(2) syringe injecting high-voltage electrostatic spinning machine is connected high-voltage power cathode by spinning solution, using aluminium foil as receiving plate
Connecting negative pole, setting voltage is 20KV, starts circulation silicone oil heating mantle, sets spinning temperature as 40 DEG C, connects conical flask receipts
In collection spinning process, the solvent of volatilization, controls spinning solution quantity delivered by dosing pump, sets jet velocity as 0.15mm/min,
Keeping ambient temperature is 20 DEG C, prepares the nanofiber of entanglement；
(3) utilize fluorescein that nanofiber is carried out chemical staining, fluorescein is grafted on nanofiber surface, and fills with solvent
Divide extracting to remove unreacted fluorescent dye, be vacuum dried 2h, prepare the nano fluorescence fiber with fluorescent characteristic；
(4) utilize surfactant (lauric acid amide of ethanol) that nano fluorescence fiber is carried out pretreatment: by surfactant
Joining in dehydrated alcohol with nano fluorescence fiber, high speed emulsion dispersion, rate of dispersion is 15000r/min, prepares nanometer
Fluorescent fiber dispersion liquid；
(5) in nano fluorescence fiber dispersion liquid, resin, compatilizer, antistatic additive and lubricant are added, drying-granulating after mixing,
Obtain hybrid resin；
(6) by stretch processes, gained hybrid resin is prepared nano fluorescence fiber false-proof film, hybrid resin is added
Enter extruder loading hopper, set feeding section temperature 165 DEG C, 180 DEG C, compression section, melt zone 195 DEG C, homogenizing zone 180 DEG C, meter
Amount section 165 DEG C, makes material fully plastify and mix in extruder, the mold body sections 165 DEG C of setting head, mouth die section 160 DEG C,
Set slab roller temperature 160 DEG C, sharp cooling roll temperature 20 DEG C；Thin film after cooling enters the vertical section of drawing, at the roller speed of vertical machine drawing
Under difference effect, the thin slice of preheating is carried out vertical drawing, longitudinal drawing temperature 80 DEG C, longitudinal stretching multiple 4.5 times, utilizes thickness measuring to scan
Frame measures and controls sheet thickness and keeps Uniform Tension；Subsequently into the horizontal section of drawing, transverse stretching machine clamper clamps chip edge by one
The track of shaped makes it laterally broaden, horizontal tentering temperature 100 DEG C, and horizontal Lapie 8 utilizes thickness measuring gantry to measure and control
Made membrane thickness keeps Uniform Tension, heat setting temperature 160 DEG C；Through the thin film of biaxial tension through chill roll, be drawn off is thin
The most expanded roller of film, flattens thin film, is allowed to cool down completely and relax, it is to avoid adhesion and contraction, and last rolling device is received
Volume i.e. obtains finished product.
Embodiment 12
Each component proportion of the present embodiment nano fluorescence fiber false-proof film is shown in Table 1, and preparation process is substantially with embodiment 7, Qi Zhongshuan
It is shown in Table 2 to the parameter of drawing process.
Embodiment 13
A kind of nano fluorescence fiber false-proof film, each component proportion is shown in Table 1, is prepared via a method which to obtain:
(1) polyvinyl alcohol is dissolved in distilled water and prepares the spinning solution that concentration is 17wt%；
(2) syringe injecting high-voltage electrostatic spinning machine is connected high-voltage power cathode, using aluminium foil as reception by spinning solution
Plate connects negative pole, and setting voltage is 30KV, starts circulation silicone oil heating mantle, sets spinning temperature as 50 DEG C, connection conical flask
Collect the solvent of volatilization in spinning process, control spinning solution quantity delivered by dosing pump, set jet velocity as 0.20mm/min,
Keeping ambient temperature is 20 DEG C, prepares the nanofiber of entanglement；
(3) utilize rare earth that nanofiber is carried out chemical staining, rare earth is grafted on nanofiber surface, and abundant with solvent
Unreacted fluorescent dye is removed in extracting, is vacuum dried 2h, prepares the nano fluorescence fiber with fluorescent characteristic；
(4) utilize surfactant that nano fluorescence fiber carries out pretreatment: surfactant and nano fluorescence fiber to be added
In dehydrated alcohol, high speed emulsion dispersion, rate of dispersion is 20000r/min, prepares nano fluorescence fiber dispersion liquid；
(5) in nano fluorescence fiber dispersion liquid, add resin, compatilizer, antistatic additive and lubricant, be dried after mixing and make
Grain, obtains hybrid resin；
(6) by stretch processes, gained hybrid resin is prepared nano fluorescence fiber false-proof film, by hybrid resin
Addition extruder loading hopper, setting feeding section temperature 210 DEG C, 225 DEG C, compression section, melt zone 240 DEG C, homogenizing zone 225 DEG C,
Metering section 210 DEG C, makes material fully plastify and mix in extruder, sets the mold body sections 210 DEG C of head, mouth die section
190 DEG C, set slab roller temperature 190 DEG C, sharp cooling roll temperature 30 DEG C；Thin film after cooling enters the vertical section of drawing, in vertical machine drawing
Under roller speed difference effect, the thin slice of preheating is carried out vertical drawing, longitudinal drawing temperature 140 DEG C, longitudinal stretching multiple 2.5 times, profit
Measure with thickness measuring gantry and control sheet thickness and keep Uniform Tension；Subsequently into the horizontal section of drawing, thin slice clamped by transverse stretching machine clamper
Edge makes it laterally broaden by the track of definite shape, horizontal tentering temperature 160 DEG C, and horizontal Lapie 3 utilizes thickness measuring to scan
Frame measures and controls film thickness and keeps Uniform Tension, heat setting temperature 190 DEG C；Through the thin film of biaxial tension through chill roll,
The most expanded roller of thin film being drawn off, flattens thin film, is allowed to cool down completely and relax, it is to avoid adhesion and contraction, the most rolling
Device carries out rolling and i.e. obtains finished product.
Embodiment 14～15
In embodiment 14～15, each component proportion of nano fluorescence fiber false-proof film is shown in Table 1, preparation process substantially with embodiment 13,
Wherein the parameter of stretch processes is shown in Table 2.
Each constituent mass proportioning of table 1 nano fluorescence fiber false-proof film
Each parameter of table 2 stretch processes
Obviously, above-described embodiment is only by clearly demonstrating made example, and not restriction to embodiment.For institute
For the those of ordinary skill in genus field, can also make other changes in different forms on the basis of the above description.
Here without also cannot all of embodiment be given exhaustive.And the obvious change therefore amplified or variation still in
Within the protection domain of the invention.
Claims (10)
1. a nano fluorescence fiber false-proof film, it is characterised in that its raw material components is by mass percentage: nanofiber 5 wt% ~ 30wt%, fluorescent dye 0.25wt% ~ 15wt%, resin 50 wt% ~ 90wt%, compatilizer 0.1
Wt% ~ 20wt%, antistatic additive 0.1 wt% ~ 1.5wt%, lubricant 0.1 wt% ~ 1.5wt%.
Nano fluorescence fiber false-proof film the most according to claim 1, it is characterized in that, described nanofiber is one or more in polyacrylonitrile, polyester, polyamide, polystyrene, polymethyl methacrylate, Merlon, Polycarbosilane, polyether sulfone and polyvinyl alcohol.
Nano fluorescence fiber false-proof film the most according to claim 1, it is characterised in that a diameter of 10 ~ 100nm of described nanofiber, a length of 0.5 ~ 5.0mm, softening temperature is 190 ~ 250 DEG C, and melt temperature is 220 ~ 320 DEG C.
Nano fluorescence fiber false-proof film the most according to claim 1, it is characterised in that described fluorescent dye is one or more in rare earth, Rare Earth Derivatives, fluorescein, fluorescein derivative, rhodamine and Rhodamine Derivatives.
Nano fluorescence fiber false-proof film the most according to claim 1, it is characterised in that described resin is one or more in polyester, polypropylene, polyamide, polystyrene, polyethylene and polyvinyl alcohol.
Nano fluorescence fiber false-proof film the most according to claim 1, it is characterised in that described compatilizer is one or more of polyolefin elastomer class, multi-monomer grafting modified phenylethylene based elastomers class and maleic anhydride grafting apoplexy due to endogenous wind.
Nano fluorescence fiber false-proof film the most according to claim 1, it is characterised in that described antistatic additive is one or more of quaternary ammonium salt, alkyl sulfonates, fatty acid and alkyl betaine apoplexy due to endogenous wind.
8. the preparation method of the arbitrary described nano fluorescence fiber false-proof film of claim 1 ~ 7, it is characterised in that comprise the steps:
(1) nanofiber is dissolved in solvent and is prepared as the spinning solution that concentration is 5 ~ 50wt%；
(2) syringe that spinning solution is injected into high-voltage electrostatic spinning machine connects high-voltage power cathode, negative pole is connected using aluminium foil as receiving plate, start circulation silicone oil heating mantle, spinning solution quantity delivered is controlled by dosing pump, connect conical flask and collect the solvent of volatilization in spinning process, prepared the nanofiber of entanglement by spinning technique；
(3) utilize fluorescent dye that nanofiber is carried out chemical staining, make fluorescent dye be grafted on nanofiber surface, more fully extract the unreacted fluorescent dye of removal with solvent, after vacuum drying, prepare the nano fluorescence fiber with fluorescent characteristic；
(4) utilize surfactant that nano fluorescence fiber carries out pretreatment: to join in dehydrated alcohol by surfactant and nano fluorescence fiber, after high speed emulsion dispersion, prepare nano fluorescence fiber dispersion liquid；
(5) in nano fluorescence fiber dispersion liquid, add resin, compatilizer, antistatic additive and lubricant, drying-granulating after mixing, obtain hybrid resin；
(6) by stretch processes, gained hybrid resin is prepared as nano fluorescence fiber false-proof film.
Preparation method the most according to claim 8, it is characterized in that, the parameter of step (2) described spinning technique is: voltage is set as that 10 ~ 30KV, spinning temperature are set as 20 ~ 50 DEG C, the jet velocity of dosing pump is set as that 0.001 ~ 0.5mm/min, ambient temperature are set as 20 ~ 30 DEG C.
Preparation method the most according to claim 8, it is characterized in that, step (6) described stretch processes is: set feeding section temperature 140 ~ 190 DEG C, 170 ~ 240 DEG C, compression section, melt zone 185 ~ 260 DEG C, homogenizing zone 170 ~ 240 DEG C, metering section 160 DEG C ~ 230 DEG C, make material fully plastify and mix in extruder, set the mold body sections 160 DEG C ~ 190 DEG C of head, mouth die section 160 DEG C ~ 230 DEG C, sets slab roller temperature 160 DEG C ~ 230 DEG C, sharp cooling roll temperature 20 DEG C ~ 40 DEG C；Thin film after cooling enters the vertical section of drawing, and the thin slice of preheating carries out under the roller speed difference effect of vertical machine drawing vertical drawing, longitudinal drawing temperature 80 DEG C ~ 160 DEG C, longitudinal stretching multiple 2.5 ~ 5.5 times, utilizes thickness measuring gantry to measure and controls sheet thickness holding Uniform Tension；Subsequently into the horizontal section of drawing, chip edge clamped by transverse stretching machine clamper makes it laterally broaden by the track of definite shape, horizontal tentering temperature 100 DEG C ~ 180 DEG C, horizontal Lapie 3.0 ~ 10, utilize thickness measuring gantry to measure and control film thickness and keep Uniform Tension, heat setting temperature 160 DEG C ~ 230 DEG C；Through the thin film of biaxial tension through chill roll, the most expanded roller of thin film being drawn off, flatten thin film, be allowed to cool down completely and relax, it is to avoid adhesion and contraction, last rolling device carries out rolling.
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| CN106436019A (en) * | 2016-10-20 | 2017-02-22 | 东华大学 | Fluorescent nano-fiber membrane and preparation method thereof |
| CN109554912A (en) * | 2018-11-23 | 2019-04-02 | 青岛大学 | A kind of preparation method of fluorescence falsification preventing camel wool fiber and products thereof and purposes |
| CN113234434A (en) * | 2021-05-12 | 2021-08-10 | 河北工业大学 | Preparation method of water-resistant rhodamine B/zirconia composite fluorescent film |
| CN113293448A (en) * | 2021-05-24 | 2021-08-24 | 河南大学 | Micro-nano optical unclonable anti-counterfeiting mark based on electrostatic spinning nanofiber cloth and preparation method and application thereof |
| CN115505190A (en) * | 2022-09-29 | 2022-12-23 | 武汉工程大学 | Interface micro-nano assembly forming method of fluorescent fiber composite material |
| CN115625948A (en) * | 2022-09-30 | 2023-01-20 | 武汉工程大学 | Carbon dot modified fluorescent fiber composite anti-counterfeiting film material and preparation method thereof |
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| CN106436019A (en) * | 2016-10-20 | 2017-02-22 | 东华大学 | Fluorescent nano-fiber membrane and preparation method thereof |
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| CN109554912A (en) * | 2018-11-23 | 2019-04-02 | 青岛大学 | A kind of preparation method of fluorescence falsification preventing camel wool fiber and products thereof and purposes |
| CN113234434A (en) * | 2021-05-12 | 2021-08-10 | 河北工业大学 | Preparation method of water-resistant rhodamine B/zirconia composite fluorescent film |
| CN113293448A (en) * | 2021-05-24 | 2021-08-24 | 河南大学 | Micro-nano optical unclonable anti-counterfeiting mark based on electrostatic spinning nanofiber cloth and preparation method and application thereof |
| CN113293448B (en) * | 2021-05-24 | 2022-07-08 | 河南大学 | Micro-nano optical unclonable anti-counterfeiting mark based on electrostatic spinning nanofiber cloth and preparation method and application thereof |
| CN115505190A (en) * | 2022-09-29 | 2022-12-23 | 武汉工程大学 | Interface micro-nano assembly forming method of fluorescent fiber composite material |
| CN115505190B (en) * | 2022-09-29 | 2024-06-18 | 武汉工程大学 | Interface micro-nano assembly forming method of fluorescent fiber composite material |
| CN115625948A (en) * | 2022-09-30 | 2023-01-20 | 武汉工程大学 | Carbon dot modified fluorescent fiber composite anti-counterfeiting film material and preparation method thereof |
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