CN110003511A - A kind of lamination fabrication PET protection film and its preparation method and application - Google Patents
A kind of lamination fabrication PET protection film and its preparation method and application Download PDFInfo
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- CN110003511A CN110003511A CN201910130003.XA CN201910130003A CN110003511A CN 110003511 A CN110003511 A CN 110003511A CN 201910130003 A CN201910130003 A CN 201910130003A CN 110003511 A CN110003511 A CN 110003511A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/0804—Manufacture of polymers containing ionic or ionogenic groups
- C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
- C08G18/0823—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing carboxylate salt groups or groups forming them
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4266—Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
- C08G18/4269—Lactones
- C08G18/4277—Caprolactone and/or substituted caprolactone
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/44—Polycarbonates
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6659—Compounds of group C08G18/42 with compounds of group C08G18/34
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/73—Polyisocyanates or polyisothiocyanates acyclic
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
- C08G18/78—Nitrogen
- C08G18/79—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates
- C08G18/791—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups
- C08G18/792—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups formed by oligomerisation of aliphatic and/or cycloaliphatic isocyanates or isothiocyanates
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C08J7/123—Treatment by wave energy or particle radiation
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/06—Polyurethanes from polyesters
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
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Abstract
The invention discloses a kind of lamination fabrication PET protection films and its preparation method and application; the protective film successively includes that the first articulamentum, biaxially oriented polyester film core layer, the second articulamentum and printing four part of adhesive layer, the printing adhesive layer are connect by the second articulamentum with biaxially oriented polyester film core layer；Printing adhesive layer and the first articulamentum can realize with card substrate printing layer and PVC band glue film effectively Nian Jie respectively under the conditions of being laminated fabrication.The PET PVC composite substrate that PET protection film of the present invention is alternatively now matched for radium-shine fabrication substrate in the industry; it is used as the card substrate with printed patterns and with the middle layer between glue film; by adjusting the thickness and degree of orientation of PET film; the planarization of card can be guaranteed into; and because product of the present invention form is PET film; simple production process, it is at low cost, requirement of the card stock market for high performance-price ratio product can be better met.
Description
Technical field
The invention belongs to be laminated fabrication technical field, especially a kind of lamination fabrication PET protection film and is answered at preparation method
With.
Background technique
Radium-shine fabrication substrate is a kind of PET base material laser film and plastics (usually PVC) sheet material are combined with each other and obtain
The certificate card material (Fig. 1) with radium-shine appearance and antifalse effect arrived, the material can by lamination or hot composition process with
Other card stocks combine, and are applied to manufacture high-end fiscard, vip card and various smart cards.Because the material of PET and PVC is poor
It is different, when single side is using radium-shine fabrication substrate layer compacting card, often there is into the problem of card bending.Current people mainly use
Card another side arrange in pairs or groups one layer have leveling effect PET PVC composite substrate solve, the PET PVC composite substrate and radium-shine system
Card substrate on the two sides at card, forms symmetrical material structure respectively, to ensure that into the planarization of card.But in view of
Radium-shine fabrication substrate and PET PVC composite substrate production technology it is essentially identical, the two selling price is very nearly the same, so very big
The further genralrlization of such personalized card stock is limited in degree.
Summary of the invention
In order to solve the problems in the existing technology, the present invention provides a kind of lamination fabrication PET protection film and its preparation
Methods and applications solve the problem of occur being bent at card when single side is using radium-shine fabrication substrate layer compacting card in the prior art.
What the present invention adopted the following technical solutions to achieve:
A kind of lamination fabrication PET protection film, the protective film successively include the first articulamentum, biaxially oriented polyester film core
Layer, the second articulamentum and printing four part of adhesive layer, the printing adhesive layer are thin by the second articulamentum and biaxial stretching polyester
The connection of film core layer；Print adhesive layer and the first articulamentum can under the conditions of being laminated fabrication, respectively with card substrate printing layer and PVC
Band glue film realizes effectively bonding.
First articulamentum and the second articulamentum are the polymeric coating layer formed after polyaminoester emulsion coating is dry, wherein
The constituent component of polyaminoester emulsion and the parts by weight difference of each component are as follows:
Trifunctional isocyanate: 1~2 part；
Two functional group's isocyanates: 12~38 parts；
Macromolecular polyester diol: 40~60 parts；
Chain extender: 4~8 parts；
Solvent: 10~30 parts；
Catalyst: 0.1~0.3 part；
Neutralizer: 3~6 parts；
Silane coupling agent: 0.6~2 part；
Glacial acetic acid: 0.1~0.3 part；
Silica dioxide granule: 2.5~6 parts；
Deionized water: 240~270 parts；
Isocyanate curing agent: 1~30 part.
The polyaminoester emulsion the preparation method is as follows:
(1) by trifunctional isocyanate, two functional group's isocyanates, macromolecular polyester diol, chain extender, catalyst
It is added with solvent into the reaction vessel equipped with blender and reflux condensing tube, is uniformly mixed, in an inert atmosphere temperature control
70~90 DEG C are reacted 3~6 hours, are cooled to 40~55 DEG C, and neutralizer stirring 10~after twenty minutes is added, obtains polyurethane prepolymer
Body；
(2) deionized water, silane coupling agent, glacial acetic acid are added in reaction unit, in an inert atmosphere temperature control 65
After~70 DEG C are reacted 1~2 hour, silica dioxide granule is added, 55~60 DEG C of temperature control 2~3 hours of reaction obtain modified two
Silica dispersion liquid；
(3) the base polyurethane prepolymer for use as (1) step obtained is poured into (2) improved silica dispersion liquid that step obtains and is carried out
Emulsion dispersion is added isocyanate curing agent, then obtains the first articulamentum and the second articulamentum after vacuum distillation removes solvent
Use polyaminoester emulsion.
The trifunctional isocyanate is hexamethylene-diisocyanate tripolymer；Two functional group's isocyanic acids
Ester is hexamethylene-diisocyanate；The macromolecular polyester diol is the two of them or two or more groups of following substance
Close: polycarbonate glycol that number-average molecular weight is 1000 to 3000, poly- 1,6-that number-average molecular weight is 3000 to 6000 oneself two
Sour-1,6-hexylene glycol ester dihydric alcohols, the polycaprolactone diols that number-average molecular weight is 3000 to 6000；The chain extender is two
Hydroxymethyl propionic acid or dimethylolpropionic acid；The solvent is butanone, butyl acetate or dimethyl carbonate；The catalyst is two fourths
Base tin dilaurate tin；The neutralizer is triethylamine or sulfamic acid；The silane coupling agent is γ-aminopropyl-triethoxy
Silane；The partial size of the silica dioxide granule is 1~5 micron.
The printing adhesive layer is the polymeric coating layer formed after polyaminoester emulsion coating is dry, wherein polyaminoester emulsion
The parts by weight of constituent component and each component difference is as follows:
Trifunctional isocyanate: 1~10 part；
Two functional group's isocyanates: 12~38 parts；
Macromolecular polyester diol: 40~60 parts；
Chain extender: 4~8 parts；
Solvent: 10~30 parts；
Catalyst: 0.1~0.3 part；
Neutralizer: 3~6 parts；
Silane coupling agent: 0.6~2 part；
Glacial acetic acid: 0.1~0.3 part；
Silica dioxide granule: 2.5~6 parts；
Deionized water: 240~270 parts.
The polyaminoester emulsion the preparation method is as follows:
(1) by trifunctional isocyanate, two functional group's isocyanates, macromolecular polyester diol, chain extender, catalyst
It is added with solvent into the reaction vessel equipped with blender and reflux condensing tube, is uniformly mixed, in an inert atmosphere temperature control
70~90 DEG C are reacted 3~6 hours, are cooled to 40~55 DEG C, and neutralizer stirring 10~after twenty minutes is added, obtains polyurethane prepolymer
Body；
(2) deionized water, silane coupling agent, glacial acetic acid are added in reaction unit, in an inert atmosphere temperature control 65
After~70 DEG C are reacted 1~2 hour, silica dioxide granule is added, 55~60 DEG C of temperature control 2~3 hours of reaction obtain modified two
Silica dispersion liquid；
(3) the base polyurethane prepolymer for use as (1) step obtained is poured into (2) improved silica dispersion liquid that step obtains and is carried out
Emulsion dispersion, then printing adhesive layer polyaminoester emulsion is obtained after vacuum distillation removes solvent.
The trifunctional isocyanate is hexamethylene-diisocyanate tripolymer；Two functional group's isocyanic acids
Ester is hexamethylene-diisocyanate；The macromolecular polyester diol is the two of them or two or more groups of following substance
Close: polycarbonate glycol that number-average molecular weight is 1000 to 3000, poly- 1,6-that number-average molecular weight is 3000 to 6000 oneself two
Sour-1,6-hexylene glycol ester dihydric alcohols, the polycaprolactone diols that number-average molecular weight is 3000 to 6000；The chain extender is two
Hydroxymethyl propionic acid or dimethylolpropionic acid；The solvent is butanone, butyl acetate or dimethyl carbonate；The catalyst is two fourths
Base tin dilaurate tin；The neutralizer is triethylamine or sulfamic acid；The silane coupling agent is γ-aminopropyl-triethoxy
Silane；The partial size of the silica dioxide granule is 1~5 micron.
The protective film is with a thickness of 5~100 μm, and preferably 10~60 μm.
A kind of preparation method being laminated fabrication PET protection film, comprising the following steps:
(1) biaxially oriented polyester film core layer two sides is surface-treated, its surface tension is made all to reach 48dyn/
Cm or more；
(2) in the first articulamentum of coated on one side of biaxially oriented polyester film core layer；
(3) the second articulamentum and printing adhesive layer are successively coated in the another side of biaxially oriented polyester film core layer；
(2) and (3) do not have sequencing in above step, both can first implementation steps (2), then implementation steps (3)；It can also
With first implementation steps (3), then implementation steps (2).
A kind of lamination fabrication PET protection film is preparing the application in Payment Card, accumulating card and member card.
Compared with the existing technology compared with, the beneficial effects of the present invention are:
1, aiming at the problem that single side is easily bent using the radium-shine fabrication substrate layer compacting card of PET base material, by another in card
The suitable and equally oriented PET protection film of the present invention of face one thickness of collocation, can effectively improve into card planarization.
2, PET protection film of the invention is produced using offline coating method, is easily worked, and production cost is total far below multilayer
It squeezes and waits method of modifying, there is very big superiority of effectiveness.
3, the first articulamentum, the second articulamentum and the printing adhesive layer that PET protection film of the invention is included all have excellent
Different ageing-resistant performance can guarantee into and be stuck in 50 DEG C, relative humidity 93%, and 90 ° after aging 14 days between different composite layer
Peel strength minimum value is in 7N/cm or more.
4, PET protection film of the invention is being laminated fabrication as with the materials'use between glue film and card base printed patterns
Under the conditions of may be implemented for effective bonding with glue film and card substrate printing material, and assign Payment Card better material
The problems such as energy, the removing and fracture of the traditional polyvinyl chloride card of improvement, to extend the service life of Payment Card.
5, after PET base material protective film of the invention is all pasted on Payment Card two sides, because there are also band glue films to protect institute for outermost layer
Can satisfy the manufacture craft including tape fitting, heat lamination and surface thermoprint technical property requirements, while being also able to satisfy table
Face individualize it is required include type/character cut in bas-relief printing, scald color, thermal transfer, photo printing, bar code processing, two dimensional code processing and swash
The manufacture craft of photoetching print technical property requirements.
The PET PVC composite substrate that PET protection film of the present invention is alternatively now matched for radium-shine fabrication substrate in the industry,
It is used as the card substrate with printed patterns and with the middle layer between glue film, by adjusting the thickness and degree of orientation of PET film,
The planarization of card can be guaranteed into, and because product of the present invention form is PET film, simple production process is at low cost, Neng Gougeng
Good meets requirement of the card stock market for high performance-price ratio product.In addition, product of the present invention can satisfy lamination fabrication work
Requirement of the skill for performances such as surface tension and temperature tolerances has higher heatproof compared to now commonly used PVC material
Grade and ageing-resistant performance can provide better protection for card surface, and then make it have longer service life.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of product of the present invention.
Wherein: (1) (3) second articulamentum (4) of the first articulamentum (2) polyester film core layer prints adhesive layer.
Specific embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
(1) PET film is surface-treated
Sided corona treatment is carried out to a thickness of 16 μm of biaxial tension PET film two sides, surface tension is made all to reach 48dyn/cm
More than.
(2) it is coated with the first articulamentum
In a nitrogen environment, into the reaction vessel equipped with blender and reflux condensing tube, it is different that 1 part of six methine two is added
Cyanate tripolymer, 30 parts of hexamethylene-diisocyanates, the polycarbonate glycol that 6 number average molecular weights are 1000,30 parts
The polycaprolactone diols that number-average molecular weight is 3000,4 parts of dimethylolpropionic acids, 27 parts of butanone, 0.1 part of dibutyl tin cinnamic acid
Tin after mixing, controls 85 DEG C of temperature, reacts 5 hours, is cooled to 45 DEG C, 3 parts of triethylamines are added after mixing evenly, are gathered
Urethane performed polymer.In a nitrogen environment, into the reaction vessel equipped with blender and reflux condensing tube, 240 parts is separately added into and is gone
Ionized water, 0.6 part of γ-aminopropyl triethoxysilane, 0.1 part of glacial acetic acid, 70 DEG C of temperature control are reacted 1 hour, add 5 parts of grains
The silica dioxide granule that diameter is 3 μm, 55 DEG C of temperature control are reacted 3 hours, obtain improved silica dispersion liquid.Derived above is gathered
Urethane performed polymer pours into and carries out emulsion dispersion in improved silica dispersion liquid, 1 part of HDI trimer resin is added, then through depressurizing
Solvent is distilled off, obtains the first articulamentum polyaminoester emulsion.
Using coated on one side the first articulamentum polyaminoester emulsion of high-speed coating equipment film obtained by step (1), apply
Between 3 to 5 μm, Coating Speed is controlled in 15~40m/min layer thickness control；It after coating and is dried, use is red
External heating type drying tunnel drying system is dried, and highest drying temperature is not higher than 100 DEG C, winds after dry.
(3) the second articulamentum of coating and printing adhesive layer
In a nitrogen environment, into the reaction vessel equipped with blender and reflux condensing tube, it is different that 2 part of six methine two is added
Cyanate tripolymer, 30 parts of hexamethylene-diisocyanates, the polycarbonate glycol that 13 number average molecular weights are 2000,60 parts
Number-average molecular weight is poly- the 1 of 6000,6-adipic acids-1,6-hexylene glycol ester dihydric alcohol, 4 parts of dimethylolpropionic acids, 27 parts of fourths
Ketone, 0.1 part of dibutyl tin dilaurate after mixing, control 85 DEG C of temperature, react 5 hours, are cooled to 45 DEG C, are added 3 parts
Triethylamine after mixing evenly, obtains base polyurethane prepolymer for use as.In a nitrogen environment, to the reaction that blender and reflux condensing tube are housed
In container, it is separately added into 240 parts of deionized waters, 0.6 part of γ-aminopropyl triethoxysilane, 0.1 part of glacial acetic acid, 70 DEG C of temperature control
Reaction 1 hour adds the silica dioxide granule that 5 parts of partial sizes are 3 μm, and 55 DEG C of temperature control are reacted 3 hours, obtains improved silica
Dispersion liquid.It by base polyurethane prepolymer for use as derived above, pours into and carries out emulsion dispersion in improved silica dispersion liquid, and be added 10
Part HDI trimer type isocyanate curing agent, then solvent is removed through vacuum distillation, obtain the second articulamentum polyaminoester emulsion.
In a nitrogen environment, into the reaction vessel equipped with blender and reflux condensing tube, it is different that 2 part of six methine two is added
Cyanate tripolymer, 30 parts of hexamethylene-diisocyanates, 26 number average molecular weights be 4000 poly- 1,6-adipic acid-1,
6-hexylene glycol ester dihydric alcohols, the polycaprolactone diols that 30 number average molecular weights are 3000,4 parts of dimethylolpropionic acids, 27 parts of fourths
Ketone, 0.1 part of dibutyl tin dilaurate after mixing, control 85 DEG C of temperature, react 5 hours, are cooled to 45 DEG C, are added 3 parts
Triethylamine after mixing evenly, obtains base polyurethane prepolymer for use as.In a nitrogen environment, to the reaction that blender and reflux condensing tube are housed
In container, it is separately added into 240 parts of deionized waters, 0.6 part of γ-aminopropyl triethoxysilane, 0.1 part of glacial acetic acid, 70 DEG C of temperature control
Reaction 1 hour adds the silica dioxide granule that 5 parts of partial sizes are 3 μm, and 55 DEG C of temperature control are reacted 3 hours, obtains improved silica
Dispersion liquid.It by base polyurethane prepolymer for use as derived above, pours into and carries out emulsion dispersion in improved silica dispersion liquid, then through depressurizing
Solvent is distilled off, obtains printing adhesive layer polyaminoester emulsion.
Coating apparatus non-coat side of film obtained by the step (2) is used successively to be coated with both the above aqueous polyurethane as the
Two linking layers and printing adhesive layer, at 3.0~5.0 μm, Coating Speed is controlled in 10~40m/min for coating layer thickness control；Coating
It afterwards and being dried, is dried using hot-air heating type drying tunnel drying system, highest drying temperature is not higher than 100 DEG C,
It is wound after drying.Gained PET film is labeled as 1#.
Embodiment 2
(1) PET film is surface-treated
Sided corona treatment is carried out to a thickness of 16 μm of biaxial tension PET film two sides, surface tension is made all to reach 48dyn/cm
More than.
(2) it is coated with the first articulamentum
In a nitrogen environment, into the reaction vessel equipped with blender and reflux condensing tube, it is different that 2 part of six methine two is added
Cyanate tripolymer, 30 parts of hexamethylene-diisocyanates, the polycaprolactone diols that 26 number average molecular weights are 4000,30 parts
Number-average molecular weight is poly- the 1 of 3000,6-adipic acids-1,6-hexylene glycol ester dihydric alcohol, 4 parts of dimethylolpropionic acids, 27 parts of fourths
Ketone, 0.1 part of dibutyl tin dilaurate after mixing, control 85 DEG C of temperature, react 5 hours, are cooled to 45 DEG C, are added 3 parts
Triethylamine after mixing evenly, obtains base polyurethane prepolymer for use as.In a nitrogen environment, to the reaction that blender and reflux condensing tube are housed
In container, it is separately added into 240 parts of deionized waters, 0.6 part of γ-aminopropyl triethoxysilane, 0.1 part of glacial acetic acid, 70 DEG C of temperature control
Reaction 1 hour adds the silica dioxide granule that 5 parts of partial sizes are 3 μm, and 55 DEG C of temperature control are reacted 3 hours, obtains improved silica
Dispersion liquid.It by base polyurethane prepolymer for use as derived above, pours into and carries out emulsion dispersion in improved silica dispersion liquid, be added 10 parts
HDI trimer resin type isocyanate curing agent, then solvent is removed through vacuum distillation, obtain the first articulamentum polyurethane cream
Liquid.
Using coated on one side the first articulamentum polyaminoester emulsion of high-speed coating equipment film obtained by step (1), apply
Between 3 to 5 μm, Coating Speed is controlled in 20~40m/min layer thickness control；It after coating and is dried, use is red
External heating type drying tunnel drying system is dried, and highest drying temperature is not higher than 120 DEG C, winds after dry.
(3) the second articulamentum of coating and printing adhesive layer
In a nitrogen environment, into the reaction vessel equipped with blender and reflux condensing tube, it is different that 1 part of six methine two is added
Cyanate tripolymer, 30 parts of hexamethylene-diisocyanates, 26 number average molecular weights be 4000 poly- 1,6-adipic acid-1,
4-butanediol ester dihydric alcohols, 30 number average molecular weights be 3000 poly- 1,6-adipic acids-1,6-hexylene glycol ester dihydric alcohol, 4
Part dimethylolpropionic acid, 27 parts of butanone, 0.1 part of dibutyl tin dilaurate after mixing, control 85 DEG C of temperature, reaction 5 is small
When, 45 DEG C are cooled to, 3 parts of triethylamines are added after mixing evenly, obtain base polyurethane prepolymer for use as.In a nitrogen environment, to equipped with stirring
In the reaction vessel for mixing device and reflux condensing tube, it is separately added into 240 parts of deionized waters, 0.6 part of γ-aminopropyl-triethoxy silicon
Alkane, 0.1 part of glacial acetic acid, 70 DEG C of temperature control are reacted 1 hour, add the silica dioxide granule that 5 parts of partial sizes are 3 μm, and 55 DEG C of temperature control anti-
It answers 3 hours, obtains improved silica dispersion liquid.By base polyurethane prepolymer for use as derived above, improved silica dispersion is poured into
Emulsion dispersion is carried out in liquid, and 30 parts of HDI trimer type isocyanate curing agents are added, then removes solvent through vacuum distillation, is obtained
To the second articulamentum polyaminoester emulsion.
In a nitrogen environment, into the reaction vessel equipped with blender and reflux condensing tube, it is different that 2 part of six methine two is added
Cyanate tripolymer, 30 parts of hexamethylene-diisocyanates, the polycarbonate glycol that 13 number average molecular weights are 2000,30 parts
The polycaprolactone diols that number-average molecular weight is 3000,4 parts of dimethylolpropionic acids, 27 parts of butanone, 0.1 part of dibutyl tin cinnamic acid
Tin after mixing, controls 85 DEG C of temperature, reacts 5 hours, is cooled to 45 DEG C, 3 parts of triethylamines are added after mixing evenly, are gathered
Urethane performed polymer.In a nitrogen environment, into the reaction vessel equipped with blender and reflux condensing tube, 240 parts is separately added into and is gone
Ionized water, 0.6 part of γ-aminopropyl triethoxysilane, 0.1 part of glacial acetic acid, 70 DEG C of temperature control are reacted 1 hour, add 5 parts of grains
The silica dioxide granule that diameter is 3 μm, 55 DEG C of temperature control are reacted 3 hours, obtain improved silica dispersion liquid.Derived above is gathered
Urethane performed polymer pours into and carries out emulsion dispersion in improved silica dispersion liquid, then removes solvent through vacuum distillation, is printed
Adhesive layer polyaminoester emulsion.
Using coating apparatus, the second articulamentum and printing are viscous more than the non-coat side of step (2) gained film is successively coated with
Connect layer polyaminoester emulsion.Anilox roll selects 130~150 mesh density, and coating layer thickness control is at 3.0~8.0 μm, Coating Speed control
System is in 20~40m/min；It after coating and is dried, is dried using hot-air heating type drying tunnel drying system, highest
Drying temperature is not higher than 160 DEG C, winds after dry.Gained PET film is labeled as 2#.
Embodiment 3
(1) PET film is surface-treated
Sided corona treatment is carried out to a thickness of 16 μm of biaxial tension PET film two sides, surface tension is made all to reach 48dyn/cm
More than.
(2) it is coated with the first articulamentum
In a nitrogen environment, into the reaction vessel equipped with blender and reflux condensing tube, it is different that 2 part of six methine two is added
Cyanate tripolymer, 30 parts of hexamethylene-diisocyanates, the polycarbonate glycol that 26 number average molecular weights are 4000,30 parts
Number-average molecular weight is poly- the 1 of 3000,6-adipic acids-1,6-hexylene glycol ester dihydric alcohol, 4 parts of dimethylolpropionic acids, 27 parts of fourths
Ketone, 0.1 part of dibutyl tin dilaurate after mixing, control 85 DEG C of temperature, react 5 hours, are cooled to 45 DEG C, are added 3 parts
Triethylamine after mixing evenly, obtains base polyurethane prepolymer for use as.In a nitrogen environment, to the reaction that blender and reflux condensing tube are housed
In container, it is separately added into 240 parts of deionized waters, 0.6 part of γ-aminopropyl triethoxysilane, 0.1 part of glacial acetic acid, 70 DEG C of temperature control
Reaction 1 hour adds the silica dioxide granule that 5 parts of partial sizes are 3 μm, and 55 DEG C of temperature control are reacted 3 hours, obtains improved silica
Dispersion liquid.It by base polyurethane prepolymer for use as derived above, pours into and carries out emulsion dispersion in improved silica dispersion liquid, and be added 30
Part HDI trimer type isocyanate curing agent, then solvent is removed through vacuum distillation, obtain the first articulamentum polyaminoester emulsion.
Using coated on one side the first articulamentum polyaminoester emulsion of high-speed coating equipment film obtained by step (1), apply
The anilox roll of cloth selects 200 mesh density, and coating layer thickness controls between 3 to 5 μm, and Coating Speed is controlled in 20~40m/min；It applies
It after cloth and is dried, is dried using infrared heating type drying tunnel drying system, highest drying temperature is not higher than 120
DEG C, it is wound after dry.
(3) the second articulamentum of coating and printing adhesive layer
In a nitrogen environment, into the reaction vessel equipped with blender and reflux condensing tube, it is different that 1 part of six methine two is added
Cyanate tripolymer, 30 parts of hexamethylene-diisocyanates, the polycarbonate glycol that 13 number average molecular weights are 2000,30 parts
The polycaprolactone diols that number-average molecular weight is 3000,4 parts of dimethylolpropionic acids, 27 parts of butanone, 0.1 part of dibutyl tin cinnamic acid
Tin after mixing, controls 85 DEG C of temperature, reacts 5 hours, is cooled to 45 DEG C, 3 parts of triethylamines are added after mixing evenly, are gathered
Urethane performed polymer.In a nitrogen environment, into the reaction vessel equipped with blender and reflux condensing tube, 240 parts is separately added into and is gone
Ionized water, 0.6 part of γ-aminopropyl triethoxysilane, 0.1 part of glacial acetic acid, 70 DEG C of temperature control are reacted 1 hour, add 5 parts of grains
The silica dioxide granule that diameter is 3 μm, 55 DEG C of temperature control are reacted 3 hours, obtain improved silica dispersion liquid.Derived above is gathered
Urethane performed polymer pours into and carries out emulsion dispersion in improved silica dispersion liquid, and 15 parts of HDI trimer type isocyanic acids are then added
Ester curing agent, then solvent is removed through vacuum distillation, obtain the second articulamentum polyaminoester emulsion.
In a nitrogen environment, into the reaction vessel equipped with blender and reflux condensing tube, it is different that 1 part of six methine two is added
Cyanate tripolymer, 30 parts of hexamethylene-diisocyanates, the polycarbonate glycol that 13 number average molecular weights are 2000,30 parts
The polycaprolactone diols that number-average molecular weight is 3000,4 parts of dimethylolpropionic acids, 27 parts of butanone, 0.1 part of dibutyl tin cinnamic acid
Tin after mixing, controls 85 DEG C of temperature, reacts 5 hours, is cooled to 45 DEG C, 3 parts of triethylamines are added after mixing evenly, are gathered
Urethane performed polymer.In a nitrogen environment, into the reaction vessel equipped with blender and reflux condensing tube, 240 parts is separately added into and is gone
Ionized water, 0.6 part of γ-aminopropyl triethoxysilane, 0.1 part of glacial acetic acid, 70 DEG C of temperature control are reacted 1 hour, add 5 parts of grains
The silica dioxide granule that diameter is 3 μm, 55 DEG C of temperature control are reacted 3 hours, obtain improved silica dispersion liquid.Derived above is gathered
Urethane performed polymer pours into and carries out emulsion dispersion in improved silica dispersion liquid, then removes solvent through vacuum distillation, is printed
Adhesive layer polyaminoester emulsion.
Using coating apparatus, the second articulamentum and printing are viscous more than the non-coat side of step (2) gained film is successively coated with
Connect layer polyaminoester emulsion.Anilox roll selects 130~150 mesh density, and coating layer thickness control is at 3.0~8.0 μm, Coating Speed control
System is in 40~80m/min；It after coating and is dried, is dried using hot-air heating type drying tunnel drying system, highest
Drying temperature is not higher than 160 DEG C, winds after dry.Gained PET film is labeled as 3#.
It is emphasized that embodiment of the present invention be it is illustrative, without being restrictive, therefore the present invention is simultaneously
It is not limited to embodiment described in specific embodiment, it is all to be obtained according to the technique and scheme of the present invention by those skilled in the art
Other embodiments, also belong to the scope of protection of the invention.
Claims (10)
1. a kind of lamination fabrication PET protection film, it is characterised in that: the protective film successively includes that the first articulamentum, biaxial tension are poly-
Ester film core layer, the second articulamentum and printing four part of adhesive layer, the printing adhesive layer pass through the second articulamentum with it is two-way
The connection of oriented polyester film core layer；Print adhesive layer and the first articulamentum can under the conditions of being laminated fabrication, respectively with card substrate
Printing layer and PVC band glue film realize effectively bonding.
2. a kind of lamination fabrication PET protection film according to claim 1, it is characterised in that: first articulamentum and
Two articulamentums are the polymeric coating layer formed after polyaminoester emulsion coating is dry, wherein the constituent component and each group of polyaminoester emulsion
The parts by weight difference divided is as follows:
Trifunctional isocyanate: 1~2 part；
Two functional group's isocyanates: 12~38 parts；
Macromolecular polyester diol: 40~60 parts；
Chain extender: 4~8 parts；
Solvent: 10~30 parts；
Catalyst: 0.1~0.3 part；
Neutralizer: 3~6 parts；
Silane coupling agent: 0.6~2 part；
Glacial acetic acid: 0.1~0.3 part；
Silica dioxide granule: 2.5~6 parts；
Deionized water: 240~270 parts；
Isocyanate curing agent: 1~30 part.
3. a kind of lamination fabrication PET protection film according to claim 2, it is characterised in that: the system of the polyaminoester emulsion
Preparation Method is as follows:
(1) by trifunctional isocyanate, two functional group's isocyanates, macromolecular polyester diol, chain extender, catalyst and molten
Agent is added into the reaction vessel equipped with blender and reflux condensing tube, is uniformly mixed, in an inert atmosphere temperature control 70~
90 DEG C are reacted 3~6 hours, are cooled to 40~55 DEG C, and neutralizer stirring 10~after twenty minutes is added, obtains base polyurethane prepolymer for use as；
(2) deionized water, silane coupling agent, glacial acetic acid are added in reaction unit, in an inert atmosphere temperature control 65~70
DEG C after reaction 1~2 hour, silica dioxide granule is added, 55~60 DEG C of temperature control 2~3 hours of reaction obtain being modified titanium dioxide
Silicon dispersion liquid；
(3) the base polyurethane prepolymer for use as (1) step obtained is poured into (2) improved silica dispersion liquid that step obtains and is emulsified
Isocyanate curing agent is added in dispersion, then obtains after vacuum distillation removes solvent the first articulamentum and the second articulamentum with poly-
Urethane lotion.
4. a kind of lamination fabrication PET protection film according to claim 3, it is characterised in that: the trifunctional isocyanide
Acid esters is hexamethylene-diisocyanate tripolymer；Two functional group's isocyanates are hexamethylene-diisocyanate；Institute
State the two of them or two or more combinations that macromolecular polyester diol is following substance: number-average molecular weight is 1000 to 3000
Polycarbonate glycol, number-average molecular weight be 3000 to 6000 poly- 1,6-adipic acid-1,6-hexylene glycol ester dihydric alcohol,
The polycaprolactone diols that number-average molecular weight is 3000 to 6000；The chain extender is dihydromethyl propionic acid or dihydroxymethyl fourth
Acid；The solvent is butanone, butyl acetate or dimethyl carbonate；The catalyst is dibutyl tin dilaurate；The neutralization
Agent is triethylamine or sulfamic acid；The silane coupling agent is γ-aminopropyl triethoxysilane；The silica dioxide granule
Partial size be 1~5 micron.
5. a kind of lamination fabrication PET protection film according to claim 1, it is characterised in that: the printing adhesive layer is poly-
The polymeric coating layer formed after urethane emulsion coating is dry, wherein parts by weight of the constituent component of polyaminoester emulsion and each component
It is as follows respectively:
Trifunctional isocyanate: 1~10 part；
Two functional group's isocyanates: 12~38 parts；
Macromolecular polyester diol: 40~60 parts；
Chain extender: 4~8 parts；
Solvent: 10~30 parts；
Catalyst: 0.1~0.3 part；
Neutralizer: 3~6 parts；
Silane coupling agent: 0.6~2 part；
Glacial acetic acid: 0.1~0.3 part；
Silica dioxide granule: 2.5~6 parts；
Deionized water: 240~270 parts.
6. a kind of lamination fabrication PET protection film according to claim 5, it is characterised in that: the system of the polyaminoester emulsion
Preparation Method is as follows:
(1) by trifunctional isocyanate, two functional group's isocyanates, macromolecular polyester diol, chain extender, catalyst and molten
Agent is added into the reaction vessel equipped with blender and reflux condensing tube, is uniformly mixed, in an inert atmosphere temperature control 70~
90 DEG C are reacted 3~6 hours, are cooled to 40~55 DEG C, and neutralizer stirring 10~after twenty minutes is added, obtains base polyurethane prepolymer for use as；
(2) deionized water, silane coupling agent, glacial acetic acid are added in reaction unit, in an inert atmosphere temperature control 65~70
DEG C after reaction 1~2 hour, silica dioxide granule is added, 55~60 DEG C of temperature control 2~3 hours of reaction obtain being modified titanium dioxide
Silicon dispersion liquid；
(3) the base polyurethane prepolymer for use as (1) step obtained is poured into (2) improved silica dispersion liquid that step obtains and is emulsified
Dispersion, then printing adhesive layer polyaminoester emulsion is obtained after vacuum distillation removes solvent.
7. a kind of lamination fabrication PET protection film according to claim 6, it is characterised in that: the trifunctional isocyanide
Acid esters is hexamethylene-diisocyanate tripolymer；Two functional group's isocyanates are hexamethylene-diisocyanate；Institute
State the two of them or two or more combinations that macromolecular polyester diol is following substance: number-average molecular weight is 1000 to 3000
Polycarbonate glycol, number-average molecular weight be 3000 to 6000 poly- 1,6-adipic acid-1,6-hexylene glycol ester dihydric alcohol,
The polycaprolactone diols that number-average molecular weight is 3000 to 6000；The chain extender is dihydromethyl propionic acid or dihydroxymethyl fourth
Acid；The solvent is butanone, butyl acetate or dimethyl carbonate；The catalyst is dibutyl tin dilaurate；The neutralization
Agent is triethylamine or sulfamic acid；The silane coupling agent is γ-aminopropyl triethoxysilane；The silica dioxide granule
Partial size be 1~5 micron.
8. a kind of lamination fabrication PET protection film according to claim 1, it is characterised in that: the protective film with a thickness of 5~
100μm。
9. a kind of preparation method for being laminated fabrication PET protection film, it is characterised in that the following steps are included:
(1) biaxially oriented polyester film core layer two sides is surface-treated, make its surface tension all reach 48dyn/cm with
On；
(2) in the first articulamentum of coated on one side of biaxially oriented polyester film core layer；
(3) the second articulamentum and printing adhesive layer are successively coated in the another side of biaxially oriented polyester film core layer；
(2) and (3) do not have sequencing in above step, both can first implementation steps (2), then implementation steps (3)；It can also be first
Implementation steps (3), then implementation steps (2).
10. a kind of lamination fabrication PET protection film is preparing the application in Payment Card, accumulating card and member card.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114456735A (en) * | 2021-12-10 | 2022-05-10 | 吕拴力 | Special orange peel resistant adhesive film for laser card and preparation method thereof |
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