CN105949622B - A kind of nano fluorescence fiber false-proof film and preparation method thereof - Google Patents
A kind of nano fluorescence fiber false-proof film and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to functional composite material fields, and in particular to a kind of nano fluorescence fiber false-proof film and preparation method thereof.The each raw material component of the nano fluorescence fiber false-proof film matches：5~30 parts by weight of nanofiber, 50~95 parts by weight of resin, 0.1~20 parts by weight of compatilizer, 0.1~1.5 parts by weight of antistatic agent, 0.1~1.5 parts by weight of lubricant；The quality of fluorescent dye is the 5%~50% of nanofiber quality.Nano fluorescence fiber false-proof film of the present invention has the characteristics that conventional fluorescent anti-fake material good concealment, is easy to discriminating, performance stabilization, also there is special antiforge function, consumer can simply be differentiated using traditional UV lamps, professional technician may also be combined with special instrument and carry out professional detection, have both a line, two wires antiforge function, anti-fake efficiency and dynamics are effectively improved, there is application value outstanding and good social benefit.
Description
Technical field
The invention belongs to functional composite material fields, and in particular to a kind of nano fluorescence fiber false-proof film and its preparation
Method.
Background technology
Luminescent fibre is a kind of fiber that can be shone under visible light or the irradiation of special light, not according to the property of light irradiation
It is same to be divided into two kinds of phosphorescence fiber and fluorescent fiber.Wherein, fluorescent fiber is that inorganic or organic fluorescence colorant is blended or is grafted
In fibre-forming polymer matrix so that fibrous material has fluorescent effect.Fluorescent fiber has good anti-fake effect, can be used as
Protective garment, daily necessities, extraordinary photosensitive material and the information that safety fibre is widely used in camouflage, road and working at height are deposited
It is multi-field to store material etc..
It is multi-field that plastic film as a kind of important high molecular material can be applied to agricultural, chemical industry, printing, packaging etc.,
It is one of widest type of application range in plastic material, can be divided into blown film, casting films and biaxial tension by production technology
Three kinds of film.Biaxial stretching film is most important one kind in three big plastic film types, through biaxial tension in process, then
Both direction is height-oriented in length and breadth, thus with good physical stability, mechanical strength, preferable barrier property, transparency and
Glossiness, tough and hard wear resistant are current most widely used printing, packaging film material.
By stretch processes prepare false-proof film material be it is a kind of most industrialize meaning production method, have compared with
The product quality of high production efficiency and stabilization and anti-fake efficiency.It is anti-fake but compared with other anti-fake materials such as anti-forge paper
Preparing for film is complex, its industrialized production is also more difficult in many cases, the main reason is that high molecular material
Performance is very special, and simple physical blending processing is difficult often to solve its consistency problem, is unable to get ideal composite wood
Material, this largely limits the production and application of false-proof film.
Invention content
The goal of the invention of the present invention be in view of the deficiencies of the prior art, provide a kind of nano fluorescence fiber false-proof film and its
Preparation method.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of nano fluorescence fiber false-proof film, raw material components are by mass percentage：Nanofiber 5wt%~
30wt%, fluorescent dye 0.25wt%~15wt%, resin 50wt%~95wt%, compatilizer 0.1wt%~20wt% resist quiet
Electric agent 0.1wt%~1.5wt%, lubricant 0.1wt%~1.5wt%.
In said program, the nanofiber is polyacrylonitrile, polyester, polyamide, polystyrene, poly-methyl methacrylate
One or more of ester, makrolon, Polycarbosilane, polyether sulfone and polyvinyl alcohol.
In said program, a diameter of 10~100nm of the nanofiber, length is 0.5~5.0mm, and softening temperature is
190~250 DEG C, melting temperature is 220~320 DEG C.
In said program, the fluorescent dye be rare earth, Rare Earth Derivatives, fluorescein, fluorescein derivative, rhodamine and
One or more of Rhodamine Derivatives.
In said program, the resin is in polyester, polypropylene, polyamide, polystyrene, polyethylene and polyvinyl alcohol
It is one or more of.
In said program, the compatilizer is polyolefin elastomer class, multi-monomer grafting modified phenylethylene based elastomers class
It is grafted one or more of class with maleic anhydride.
In said program, the antistatic agent is quaternary ammonium salt, alkyl sulfonates, fatty acid and alkyl betaines bases
One or more of.
In said program, the lubricant is saturated hydrocarbons, halogenated hydrocarbon, fatty acid, aliphatic alcohols, aliphatic amide
One or more of class, fatty acid ester, aliphatic alcohols, metal soap and polyalcohols.
The preparation method of above-mentioned nano fluorescence fiber false-proof film, includes the following steps：
(1) nanofiber is dissolved in the spinning solution that solvent is prepared into a concentration of 5~50%；
(2) by spinning solution be injected into high-voltage electrostatic spinning machine syringe connect high-voltage power cathode, using aluminium foil as
Receiver board connects cathode, starts cycle silicone oil heating mantle, controls spinning solution supply amount by constant displacement pump, connection conical flask is collected
The nanofiber of entanglement is prepared by spinning technique for the solvent to volatilize in spinning process；
(3) chemical staining is carried out to nanofiber using fluorescent dye, fluorescent dye is made to be grafted on nanofiber surface, then
The unreacted fluorescent dye of removal is fully extracted with solvent, and it is fine that the nano fluorescent with fluorescent characteristic is prepared after vacuum drying
Dimension；
(4) nano fluorescence fiber is pre-processed using surfactant：By surfactant and nano fluorescence fiber
It is added in absolute ethyl alcohol, after high speed emulsion dispersion, nano fluorescence fiber dispersion liquid is prepared；
(5) resin, compatilizer, antistatic agent and lubricant are added in nano fluorescence fiber dispersion liquid, is dried after mixing
It is granulated, obtains hybrid resin；
(6) as stretch processes, the hybrid resin by obtained by is prepared into nano fluorescence fiber false-proof film.
In said program, the parameter of step (2) described spinning technique is：Voltage is set as 10~30KV, and spinning temperature is set
It is set to 20~50 DEG C, the jet velocity of constant displacement pump is set as 0.001~0.5mm/min, and environment temperature is set as 20~30 DEG C.
In said program, step (6) described stretch processes are：Set 140~190 DEG C of feeding section temperature, compression section
170~240 DEG C, 185~260 DEG C of melt zone, 170~240 DEG C of homogenizing zone, 160 DEG C~230 DEG C of metering section makes in extruder
Material be fully plasticized and mix, and sets 160 DEG C~190 DEG C of the mold body sections of head, 160 DEG C~230 DEG C of mouth mold section, setting casting
160 DEG C~230 DEG C of piece roll temperature, 20 DEG C~40 DEG C of Quench roll temperature；Film after cooling enters vertical drawing section, in the roller of vertical machine drawing
The thin slice of preheating is subjected to vertical drawing under cylinder speed difference effect, 80 DEG C~160 DEG C of longitudinal drawing temperature, longitudinal stretching multiple 2.5~
It 5.5 times, is measured using thickness measuring scanning support and controls sheet thickness holding Uniform Tension；Subsequently into horizontal drawing section, transverse stretching machine clamping
Device clamps chip edge makes it broaden laterally by the track of definite shape, 100 DEG C~180 DEG C of lateral tentering temperature, horizontal drawing
Than 3.0~10, is measured using thickness measuring scanning support and control film thickness holding Uniform Tension, heat setting temperature 160 DEG C~230
℃；Film through biaxial tension passes through chill roll, and the film being drawn off expanded roller again flattens film, be allowed to it is completely cooling and
Relaxation, avoids adhesion and contraction, and last rolling device is wound.
The false-proof film of the preparation method production can detect excitation spectrum using Fluorescence Spectrometer through the invention, and
And there is different fluorescent absorption peaks from 380~780nm visible spectrums in 200~380nm ultraviolet lights spectral coverage, it is aobvious using polarisation
10~100nm of diameter, the nanofibrous structures of 0.5~5.0mm of length can be observed in micro mirror, scanning electron microscope.
Beneficial effects of the present invention：Nano fluorescence fiber false-proof film of the present invention, which removes, has conventional fluorescent anti-fake material
Good concealment is easy to the features such as discriminating, performance stabilization, also has special antiforge function, is not influencing thin-film material basic nature
Fluorescent characteristic and nanofibrous structures are had both while energy, consumer can simply be differentiated using traditional UV lamps, in this base
Professional technician may also be combined with the special instruments such as Fluorescence Spectrometer, petrographic microscope and scanning electron microscope and carry out specially on plinth
Industry detect, to make nano fluorescence fiber false-proof film have both a line, two wires antiforge function, can effectively improve its anti-fake efficiency with
Dynamics has application value outstanding and good social benefit.
Description of the drawings
A kind of Fig. 1 high-voltage electrostatic spinning process schematics of nano fluorescence fiber false-proof film according to the present invention.
A kind of Fig. 2 nanofiber scanning electron microscope that nano fluorescence fiber false-proof film tangles according to the present invention
Figure.
A kind of Fig. 3 production process schematic diagrames of nano fluorescence fiber false-proof film of the present invention.
Specific implementation mode
For a better understanding of the present invention, with reference to embodiment, the attached drawing content that the present invention is furture elucidated, but this hair
Bright content is not limited solely to the following examples.
In following embodiment, the high-voltage electrostatic spinning process is as shown in Figure 1：
(1) syringe that the spinning solution configured is injected to high-voltage electrostatic spinning machine connects high-voltage power cathode, with aluminium
Foil connects cathode as receiver board, sets voltage as 10~30KV；
(2) start cycle silicone oil heating mantle, set spinning temperature as 20~50 DEG C, connection conical flask is collected in spinning process
The solvent of volatilization；
(3) it opens constant displacement pump to squeeze out spinning solution in syringe, sets jet velocity as 0.001~0.5mm/min, protect
It is 20~30 DEG C to hold environment temperature；
(4) random sampling is carried out to nanofiber with glass slide, using its structure of polarized light microscope observing and size, and according to
This adjusts voltage and jet velocity, and the nanofiber that entanglement is prepared is made to meet the requirements.
It can be formed with smooth planar surface by above-mentioned processing step progress high-voltage electrostatic spinning and be twined compared with big L/D ratio
The nanofiber (nanofiber scanning electron microscope diagram is shown in Fig. 2) of knot, a diameter of 10~100nm, length be 0.5~
5.0mm。
The production process of nano fluorescence fiber false-proof film as shown in Figure 3, can carry out the continuous production of the false-proof film：
(1) resin, compatilizer, antistatic agent and lubricant are added in nano fluorescence fiber dispersion liquid, is dried after mixing
It is granulated, obtains hybrid resin；
(2) hybrid resin is added to the loading hopper of extruder, 140~190 DEG C of setting feeding section temperature, compression section 170~
240 DEG C, 185~260 DEG C of melt zone, 170~240 DEG C of homogenizing zone, 160 DEG C~230 DEG C of metering section, make in extruder material into
Row fully plasticizing and mixing, sets 160 DEG C~190 DEG C of the mold body sections of head, and 160 DEG C~230 DEG C of mouth mold section sets slab roller temperature
160 DEG C~230 DEG C of degree, 20 DEG C~40 DEG C of Quench roll temperature；Film after cooling enters vertical drawing section, in the roller speed of vertical machine drawing
The thin slice of preheating is subjected to vertical drawing under difference effect, 80 DEG C~160 DEG C of longitudinal drawing temperature, 2.5~5.5 times of longitudinal stretching multiple,
It is measured using thickness measuring scanning support and controls sheet thickness and keep Uniform Tension；Subsequently into horizontal drawing section, transverse stretching machine clamper is clamped
Chip edge makes it broaden laterally by the track of definite shape, 100 DEG C~180 DEG C of lateral tentering temperature, and horizontal Lapie 3.0~
10, it is measured using thickness measuring scanning support and controls film thickness holding Uniform Tension, 160 DEG C~230 DEG C of heat setting temperature；Through two-way
The film of stretching passes through chill roll, and expanded roller, flattening film are allowed to cooling completely and relaxation, avoid the film being drawn off again
Adhesion and contraction, last rolling device are wound.
Embodiment 1
A kind of nano fluorescence fiber false-proof film, each group distribution ratio are shown in Table 1, are prepared via a method which to obtain：
(1) polyacrylonitrile is dissolved in the spinning solution that n,N-Dimethylformamide prepares a concentration of 7wt%；
(2) syringe that spinning solution is injected to high-voltage electrostatic spinning machine connects high-voltage power cathode, using aluminium foil as connecing
It receives plate and connects cathode, set voltage as 18KV, start cycle silicone oil heating mantle, set spinning temperature as 40 DEG C, connect conical flask
The solvent to volatilize in spinning process is collected, spinning solution supply amount is controlled by constant displacement pump, sets jet velocity as 0.05mm/
Min, it is 20 DEG C to keep environment temperature, and the nanofiber of entanglement is prepared；
(3) chemical staining is carried out to nanofiber using fluorescein, fluorescein is grafted on nanofiber surface, and with molten
Agent fully extracts the unreacted fluorescent dye of removal, is dried in vacuo 2h, nano fluorescence fiber is prepared；
(4) nano fluorescence fiber is pre-processed using surfactant (Tween 80)：By surfactant and nanometer
Fluorescent fiber is added in absolute ethyl alcohol, high speed emulsion dispersion, rate of dispersion 7000r/min, and nano fluorescent fibre is prepared
Tie up dispersion liquid；
(5) resin, compatilizer, antistatic agent and lubricant are added in nano fluorescence fiber dispersion liquid, is dried after mixing
It is granulated, obtains hybrid resin；
(6) as stretch processes, nano fluorescence fiber false-proof film is prepared in the hybrid resin by obtained by：It will mixing
Resin addition extruder loading hopper, 165 DEG C of setting feeding section temperature, 180 DEG C of compression section, 195 DEG C of melt zone, 180 DEG C of homogenizing zone,
165 DEG C of metering section makes material be fully plasticized and mix in extruder, sets 165 DEG C of the mold body sections of head, mouth mold section
160 DEG C, 160 DEG C of setting slab roll temperature, 20 DEG C of Quench roll temperature；Film after cooling enters vertical drawing section, in the roller of vertical machine drawing
The thin slice of preheating is subjected to vertical drawing, 80 DEG C of longitudinal drawing temperature under cylinder speed difference effect, 5.5 times of longitudinal stretching multiple utilizes survey
Thick scanning support, which measures and controls sheet thickness, keeps Uniform Tension；Subsequently into horizontal drawing section, transverse stretching machine clamper clamps thin slice side
Edge makes it broaden laterally by the track of definite shape, 100 DEG C of lateral tentering temperature, horizontal Lapie 9, is surveyed using thickness measuring scanning support
Determine and control film thickness to keep Uniform Tension, 160 DEG C of heat setting temperature；Film through biaxial tension passes through chill roll, is led
Expanded roller, flattening film are allowed to cooling completely and relaxation, avoid adhesion and contraction the film gone out again, last rolling device
It is wound and obtains finished product.
Embodiment 2
A kind of nano fluorescence fiber false-proof film, each group distribution ratio are shown in Table 1, are prepared via a method which to obtain：
(1) polyester is dissolved in the spinning solution that hexafluoroisopropanol prepares a concentration of 10wt%；
(2) by spinning solution will inject high-voltage electrostatic spinning machine syringe connect high-voltage power cathode, using aluminium foil as
Receiver board connects cathode, sets voltage as 25KV, starts cycle silicone oil heating mantle, sets spinning temperature as 50 DEG C, connects taper
Bottle collects the solvent that volatilizees in spinning process, and spinning solution supply amount is controlled by constant displacement pump, set jet velocity as
0.001mm/min, it is 20 DEG C to keep environment temperature, and the nanofiber of entanglement is prepared；
(3) chemical staining is carried out to nanofiber using rare earth, rare earth is grafted on nanofiber surface, and fill with solvent
Divide extracting to remove unreacted fluorescent dye, is dried in vacuo 2h, nano fluorescence fiber is prepared；
(4) nano fluorescence fiber is pre-processed using surfactant (lauryl sodium sulfate)：By surface-active
Agent and nano fluorescence fiber are added in absolute ethyl alcohol, high speed emulsion dispersion, and rate of dispersion 12000r/min is prepared and receives
Rice fluorescent fiber dispersion liquid；
(5) resin, compatilizer, antistatic agent and lubricant are added in nano fluorescence fiber dispersion liquid, is dried after mixing
It is granulated, obtains hybrid resin；
(6) as stretch processes, nano fluorescence fiber false-proof film is prepared in the hybrid resin by obtained by：It will mixing
Resin addition extruder loading hopper, 155 DEG C of setting feeding section temperature, 170 DEG C of compression section, 185 DEG C of melt zone, 170 DEG C of homogenizing zone,
155 DEG C of metering section makes material be fully plasticized and mix in extruder, sets 155 DEG C of the mold body sections of head, mouth mold section
150 DEG C, 150 DEG C of setting slab roll temperature, 20 DEG C of Quench roll temperature；Film after cooling enters vertical drawing section, in the roller of vertical machine drawing
The thin slice of preheating is subjected to vertical drawing, 70 DEG C of longitudinal drawing temperature under cylinder speed difference effect, 5 times of longitudinal stretching multiple utilizes thickness measuring
Scanning support, which measures and controls sheet thickness, keeps Uniform Tension；Subsequently into horizontal drawing section, transverse stretching machine clamper clamps chip edge
It is set to broaden laterally by the track of definite shape, 90 DEG C of lateral tentering temperature, horizontal Lapie 9 is measured using thickness measuring scanning support
And it controls film thickness and keeps Uniform Tension, 150 DEG C of heat setting temperature；Film through biaxial tension passes through chill roll, is drawn off
Film expanded roller again, flatten film, be allowed to completely cooling and relaxation, avoid adhesion and contraction, last rolling device into
Row winding obtains finished product.
Embodiment 3~4
The each group distribution ratio of nano fluorescence fiber false-proof film is shown in Table 1 in embodiment 3~4, and preparation process is substantially the same as implementation
The parameter of example 2, wherein stretch processes is shown in Table 2.
Embodiment 5
A kind of nano fluorescence fiber false-proof film, each group distribution ratio are shown in Table 1, are prepared via a method which to obtain：
(1) polyacrylonitrile is dissolved in the spinning solution that n,N-Dimethylformamide prepares a concentration of 8wt%；
(2) by spinning solution will inject high-voltage electrostatic spinning machine syringe connect high-voltage power cathode, using aluminium foil as
Receiver board connects cathode, sets voltage as 19KV, starts cycle silicone oil heating mantle, sets spinning temperature as 40 DEG C, connects taper
Bottle collects the solvent to volatilize in spinning process, controls spinning solution supply amount by constant displacement pump, sets jet velocity as 0.10mm/
Min, it is 20 DEG C to keep environment temperature, and the nanofiber of entanglement is prepared；
(3) chemical staining is carried out to nanofiber using fluorescein, fluorescein is grafted on nanofiber surface, and with molten
Agent fully extracts the unreacted fluorescent dye of removal, is dried in vacuo 2h, the fluorescent nano-fiber with fluorescent characteristic is prepared；
(4) nano fluorescence fiber is pre-processed using surfactant (neopelex)：Surface is lived
Property agent and nano fluorescence fiber are added in absolute ethyl alcohol, and high speed emulsion dispersion, rate of dispersion 7000r/min is prepared
Nano fluorescence fiber dispersion liquid；
(5) resin, compatilizer, antistatic agent and lubricant are added in nano fluorescence fiber dispersion liquid, is dried after mixing
It is granulated, obtains hybrid resin；
(6) as stretch processes, nano fluorescence fiber false-proof film is prepared in the hybrid resin by obtained by：It will mixing
Resin addition extruder loading hopper, 165 DEG C of setting feeding section temperature, 180 DEG C of compression section, 195 DEG C of melt zone, 180 DEG C of homogenizing zone,
165 DEG C of metering section makes material be fully plasticized and mix in extruder, sets 165 DEG C of the mold body sections of head, mouth mold section
160 DEG C, 160 DEG C of setting slab roll temperature, 20 DEG C of Quench roll temperature；Film after cooling enters vertical drawing section, in the roller of vertical machine drawing
The thin slice of preheating is subjected to vertical drawing, 80 DEG C of longitudinal drawing temperature under cylinder speed difference effect, 5.5 times of longitudinal stretching multiple utilizes survey
Thick scanning support, which measures and controls sheet thickness, keeps Uniform Tension；Subsequently into horizontal drawing section, transverse stretching machine clamper clamps thin slice side
Edge makes it broaden laterally by the track of definite shape, 100 DEG C of lateral tentering temperature, horizontal Lapie 9, is surveyed using thickness measuring scanning support
Determine and control film thickness to keep Uniform Tension, 160 DEG C of heat setting temperature；Film through biaxial tension passes through chill roll, is led
Expanded roller, flattening film are allowed to cooling completely and relaxation, avoid adhesion and contraction the film gone out again, last rolling device
It is wound and obtains finished product.
Embodiment 6
The each group distribution ratio of nano fluorescence fiber false-proof film is shown in Table 1 in the present embodiment, the substantially same embodiment of preparation process
5, the parameter of wherein stretch processes is shown in Table 2.
Embodiment 7
A kind of nano fluorescence fiber false-proof film, each group distribution ratio are shown in Table 1, are prepared via a method which to obtain：
(1) polymethyl methacrylate is dissolved in the spinning solution that acetone prepares a concentration of 15wt%；
(2) by spinning solution will inject high-voltage electrostatic spinning machine syringe connect high-voltage power cathode, using aluminium foil as
Receiver board connects cathode, sets voltage as 20KV, starts cycle silicone oil heating mantle, sets spinning temperature as 30 DEG C, connects taper
Bottle collects the solvent to volatilize in spinning process, controls spinning solution supply amount by constant displacement pump, sets jet velocity as 0.05mm/
Min, it is 25 DEG C to keep environment temperature, and the nanofiber of entanglement is prepared；
(3) chemical staining is carried out to nanofiber using fluorescein sodium, fluorescein sodium is grafted on nanofiber surface, and
The unreacted fluorescent dye of removal is fully extracted with solvent, is dried in vacuo 2h, the nano fluorescent with fluorescent characteristic is prepared
Fiber；
(4) nano fluorescence fiber is pre-processed using surfactant (alkyl glycosides)：By surfactant and receive
Rice fluorescent fiber is added in absolute ethyl alcohol, and nano fluorescent is prepared in high speed emulsion dispersion, rate of dispersion 15000r/min
Fiber dispersion；
(5) resin, compatilizer, antistatic agent and lubricant are added in nano fluorescence fiber dispersion liquid, is dried after mixing
It is granulated, obtains hybrid resin；
(6) as stretch processes, nano fluorescence fiber false-proof film is prepared in the hybrid resin by obtained by：It will mixing
Resin addition extruder loading hopper, 140 DEG C of setting feeding section temperature, 200 DEG C of compression section, 260 DEG C of melt zone, 260 DEG C of homogenizing zone,
260 DEG C of metering section makes material be fully plasticized and mix in extruder, sets 250 DEG C of the mold body sections of head, mouth mold section
230 DEG C, 230 DEG C of setting slab roll temperature, 40 DEG C of Quench roll temperature；Film after cooling enters vertical drawing section, in the roller of vertical machine drawing
The thin slice of preheating is subjected to vertical drawing, 180 DEG C of longitudinal drawing temperature under cylinder speed difference effect, 2.5 times of longitudinal stretching multiple utilizes survey
Thick scanning support, which measures and controls sheet thickness, keeps Uniform Tension；Subsequently into horizontal drawing section, transverse stretching machine clamper clamps thin slice side
Edge makes it broaden laterally by the track of definite shape, and 200 DEG C of lateral tentering temperature, horizontal Lapie 3.5 utilizes thickness measuring scanning support
It measures and controls film thickness and keep Uniform Tension, 230 DEG C of heat setting temperature；Film through biaxial tension passes through chill roll, quilt
Expanded roller, flattening film are allowed to cooling completely and relaxation, avoid adhesion and contraction the film involved again, last rolling dress
It sets to be wound and obtains finished product.
Embodiment 8~10
The each group distribution ratio of nano fluorescence fiber false-proof film is shown in Table 1 in embodiment 8~10, and preparation process is substantially the same as implementation
The parameter of example 7, wherein stretch processes is shown in Table 2.
Embodiment 11
A kind of nano fluorescence fiber false-proof film, each group distribution ratio are shown in Table 1, are prepared via a method which to obtain：
(1) polyacrylonitrile is dissolved in the spinning solution that n,N-Dimethylformamide prepares a concentration of 9wt%；
(2) by spinning solution will inject high-voltage electrostatic spinning machine syringe connect high-voltage power cathode, using aluminium foil as
Receiver board connects cathode, sets voltage as 20KV, starts cycle silicone oil heating mantle, sets spinning temperature as 40 DEG C, connects taper
Bottle collects the solvent to volatilize in spinning process, controls spinning solution supply amount by constant displacement pump, sets jet velocity as 0.15mm/
Min, it is 20 DEG C to keep environment temperature, and the nanofiber of entanglement is prepared；
(3) chemical staining is carried out to nanofiber using fluorescein, fluorescein is grafted on nanofiber surface, and with molten
Agent fully extracts the unreacted fluorescent dye of removal, is dried in vacuo 2h, the nano fluorescence fiber with fluorescent characteristic is prepared；
(4) nano fluorescence fiber is pre-processed using surfactant (lauric acid amide of ethanol)：Surface is lived
Property agent and nano fluorescence fiber are added in absolute ethyl alcohol, and high speed emulsion dispersion, rate of dispersion 15000r/min is prepared
Nano fluorescence fiber dispersion liquid；
(5) resin, compatilizer, antistatic agent and lubricant are added in nano fluorescence fiber dispersion liquid, is dried after mixing
It is granulated, obtains hybrid resin；
(6) as stretch processes, nano fluorescence fiber false-proof film is prepared in the hybrid resin by obtained by, will mix
Resin addition extruder loading hopper, 165 DEG C of setting feeding section temperature, 180 DEG C of compression section, 195 DEG C of melt zone, 180 DEG C of homogenizing zone,
165 DEG C of metering section makes material be fully plasticized and mix in extruder, sets 165 DEG C of the mold body sections of head, mouth mold section
160 DEG C, 160 DEG C of setting slab roll temperature, 20 DEG C of Quench roll temperature；Film after cooling enters vertical drawing section, in the roller of vertical machine drawing
The thin slice of preheating is subjected to vertical drawing, 80 DEG C of longitudinal drawing temperature under cylinder speed difference effect, 4.5 times of longitudinal stretching multiple utilizes survey
Thick scanning support, which measures and controls sheet thickness, keeps Uniform Tension；Subsequently into horizontal drawing section, transverse stretching machine clamper clamps thin slice side
Edge makes it broaden laterally by the track of definite shape, 100 DEG C of lateral tentering temperature, horizontal Lapie 8, is surveyed using thickness measuring scanning support
Determine and control film thickness to keep Uniform Tension, 160 DEG C of heat setting temperature；Film through biaxial tension passes through chill roll, is led
Expanded roller, flattening film are allowed to cooling completely and relaxation, avoid adhesion and contraction the film gone out again, last rolling device
It is wound and obtains finished product.
Embodiment 12
The each group distribution ratio of the present embodiment nano fluorescence fiber false-proof film is shown in Table 1, preparation process substantially with embodiment 7,
The parameter of wherein stretch processes is shown in Table 2.
Embodiment 13
A kind of nano fluorescence fiber false-proof film, each group distribution ratio are shown in Table 1, are prepared via a method which to obtain：
(1) polyvinyl alcohol is dissolved in the spinning solution that distilled water prepares a concentration of 17wt%；
(2) by spinning solution will inject high-voltage electrostatic spinning machine syringe connect high-voltage power cathode, using aluminium foil as
Receiver board connects cathode, sets voltage as 30KV, starts cycle silicone oil heating mantle, sets spinning temperature as 50 DEG C, connects taper
Bottle collects the solvent to volatilize in spinning process, controls spinning solution supply amount by constant displacement pump, sets jet velocity as 0.20mm/
Min, it is 20 DEG C to keep environment temperature, and the nanofiber of entanglement is prepared；
(3) chemical staining is carried out to nanofiber using rare earth, rare earth is grafted on nanofiber surface, and fill with solvent
Divide extracting to remove unreacted fluorescent dye, is dried in vacuo 2h, the nano fluorescence fiber with fluorescent characteristic is prepared；
(4) nano fluorescence fiber is pre-processed using surfactant：By surfactant and nano fluorescence fiber
It is added in absolute ethyl alcohol, high speed emulsion dispersion, rate of dispersion 20000r/min, nano fluorescence fiber dispersion is prepared
Liquid；
(5) resin, compatilizer, antistatic agent and lubricant are added in nano fluorescence fiber dispersion liquid, is dried after mixing
It is granulated, obtains hybrid resin；
(6) as stretch processes, nano fluorescence fiber false-proof film is prepared in the hybrid resin by obtained by, will mix
Resin addition extruder loading hopper, 210 DEG C of setting feeding section temperature, 225 DEG C of compression section, 240 DEG C of melt zone, 225 DEG C of homogenizing zone,
210 DEG C of metering section makes material be fully plasticized and mix in extruder, sets 210 DEG C of the mold body sections of head, mouth mold section
190 DEG C, 190 DEG C of setting slab roll temperature, 30 DEG C of Quench roll temperature；Film after cooling enters vertical drawing section, in the roller of vertical machine drawing
The thin slice of preheating is subjected to vertical drawing, 140 DEG C of longitudinal drawing temperature under cylinder speed difference effect, 2.5 times of longitudinal stretching multiple utilizes survey
Thick scanning support, which measures and controls sheet thickness, keeps Uniform Tension；Subsequently into horizontal drawing section, transverse stretching machine clamper clamps thin slice side
Edge makes it broaden laterally by the track of definite shape, 160 DEG C of lateral tentering temperature, horizontal Lapie 3, is surveyed using thickness measuring scanning support
Determine and control film thickness to keep Uniform Tension, 190 DEG C of heat setting temperature；Film through biaxial tension passes through chill roll, is led
Expanded roller, flattening film are allowed to cooling completely and relaxation, avoid adhesion and contraction the film gone out again, last rolling device
It is wound and obtains finished product.
Embodiment 14~15
The each group distribution ratio of nano fluorescence fiber false-proof film is shown in Table 1 in embodiment 14~15, and preparation process is substantially the same as real
Example 13 is applied, the parameter of wherein stretch processes is shown in Table 2.
The each component quality proportioning of 1 nano fluorescence fiber false-proof film of table
Each parameter of 2 stretch processes of table
Obviously, above-described embodiment be only intended to clearly illustrate made by example, and not limitation to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation or change therefore amplified
It moves within still in the protection domain of the invention.
Claims (7)
1. a kind of nano fluorescence fiber false-proof film, which is characterized in that its raw material components is by mass percentage：Nanofiber
5 wt% ~ 30wt%, fluorescent dye 0.25wt% ~ 15wt%, 50 wt% of resin ~ 90wt%, 0.1 wt% of compatilizer ~ 20wt% are antistatic
0.1 wt% of agent ~ 1.5wt%, 0.1 wt% of lubricant ~ 1.5wt%；The nanofiber is polyacrylonitrile, polyester, polyamide, polyphenyl
One or more of ethylene, polymethyl methacrylate, makrolon, Polycarbosilane, polyether sulfone and polyvinyl alcohol；It is described to receive
A diameter of 10 ~ 100nm of rice fiber, length are 0.5 ~ 5.0mm, and softening temperature is 190 ~ 250 DEG C, and melting temperature is 220 ~ 320
℃。
2. nano fluorescence fiber false-proof film according to claim 1, which is characterized in that the fluorescent dye be rare earth,
One or more of Rare Earth Derivatives, fluorescein, fluorescein derivative, rhodamine and Rhodamine Derivatives.
3. nano fluorescence fiber false-proof film according to claim 1, which is characterized in that the resin is polyester, poly- third
One or more of alkene, polyamide, polystyrene, polyethylene and polyvinyl alcohol.
4. nano fluorescence fiber false-proof film according to claim 1, which is characterized in that the compatilizer is polyolefin bullet
Property one or more of body class, multi-monomer grafting modified phenylethylene based elastomers class and maleic anhydride grafting class.
5. nano fluorescence fiber false-proof film according to claim 1, which is characterized in that the antistatic agent is quaternary ammonium salt
One or more of class, alkyl sulfonates, fatty acid and alkyl betaines bases.
6. the preparation method of any nano fluorescence fiber false-proof film of claim 1 ~ 5, which is characterized in that including walking as follows
Suddenly：
（1）Nanofibre polymer is dissolved in the spinning solution that solvent is prepared into a concentration of 5 ~ 50wt%；
（2）The syringe that spinning solution is injected into high-voltage electrostatic spinning machine connects high-voltage power cathode, using aluminium foil as reception
Plate connects cathode, starts cycle silicone oil heating mantle, controls spinning solution supply amount by constant displacement pump, connection conical flask collects spinning
The nanofiber of entanglement is prepared by spinning technique for the solvent to volatilize in the process；The parameter of the spinning technique is：Voltage
It is set as 10 ~ 30KV, spinning temperature is set as 20 ~ 50 DEG C, and the jet velocity of constant displacement pump is set as 0.001 ~ 0.5mm/min, ring
Border temperature is set as 20 ~ 30 DEG C；
（3）Chemical staining is carried out to nanofiber using fluorescent dye, so that fluorescent dye is grafted on nanofiber surface, then with molten
Agent fully extracts the unreacted fluorescent dye of removal, and the nano fluorescence fiber with fluorescent characteristic is prepared after vacuum drying；
（4）Nano fluorescence fiber is pre-processed using surfactant：Surfactant and nano fluorescence fiber are added
Into absolute ethyl alcohol, after high speed emulsion dispersion, nano fluorescence fiber dispersion liquid is prepared；
（5）It is added resin, compatilizer, antistatic agent and lubricant in nano fluorescence fiber dispersion liquid, drying-granulating after mixing,
Obtain hybrid resin；
（6）It is prepared into nano fluorescence fiber false-proof film as stretch processes hybrid resin by obtained by.
7. preparation method according to claim 6, which is characterized in that step（6）The stretch processes are：Setting adds
Expect 140 ~ 190 DEG C of section temperature, 170 ~ 240 DEG C of compression section, 185 ~ 260 DEG C of melt zone, 170 ~ 240 DEG C of homogenizing zone, 160 DEG C of metering section
~ 230 DEG C, so that material be fully plasticized and mix in extruder, set 160 DEG C ~ 190 DEG C of the mold body sections of head, mouth mold section
160 DEG C ~ 230 DEG C, 160 DEG C ~ 230 DEG C of setting slab roll temperature, 20 DEG C ~ 40 DEG C of Quench roll temperature；Film after cooling enters vertical
Section is drawn, the thin slice of preheating is subjected to vertical drawing under the roller speed difference effect of vertical machine drawing, 80 DEG C ~ 160 DEG C of longitudinal drawing temperature is indulged
To 2.5 ~ 5.5 times of draw ratio, is measured using thickness measuring scanning support and control sheet thickness holding Uniform Tension；Subsequently into horizontal drawing
Section, transverse stretching machine clamper clamps chip edge makes it broaden laterally by the track of definite shape, 100 DEG C of lateral tentering temperature
~ 180 DEG C, horizontal Lapie 3.0 ~ 10 is measured using thickness measuring scanning support and controls film thickness holding Uniform Tension, heat setting temperature
160℃~230℃；Film through biaxial tension passes through chill roll, and expanded roller, flattening film have been allowed to the film being drawn off again
Complete cooling and relaxation, avoids adhesion and contraction, and last rolling device is wound.
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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 |
| CN113234434B (en) * | 2021-05-12 | 2022-08-30 | 河北工业大学 | Preparation method of water-resistant rhodamine B/zirconia composite fluorescent film |
| 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 |
| 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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| CN104311990A (en) * | 2014-09-19 | 2015-01-28 | 金发科技股份有限公司 | Polypropylene anti-counterfeiting film and preparation method thereof |
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