CN110499111A - A kind of polyolefin optical glue film and preparation method thereof that UV crosslinking curing is modified - Google Patents

A kind of polyolefin optical glue film and preparation method thereof that UV crosslinking curing is modified Download PDF

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Publication number
CN110499111A
CN110499111A CN201910587096.9A CN201910587096A CN110499111A CN 110499111 A CN110499111 A CN 110499111A CN 201910587096 A CN201910587096 A CN 201910587096A CN 110499111 A CN110499111 A CN 110499111A
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crosslinking curing
ester
bis
derivative
glue film
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Inventor
杨之亮
张好宾
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Shenzhen Lixin Optical Material Technology Co Ltd
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Shenzhen Lixin Optical Material Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J4/00Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
    • C09J4/06Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/10Adhesives in the form of films or foils without carriers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2203/00Applications of adhesives in processes or use of adhesives in the form of films or foils
    • C09J2203/318Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2423/00Presence of polyolefin
    • C09J2423/04Presence of homo or copolymers of ethene
    • C09J2423/045Presence of homo or copolymers of ethene in the release coating
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2467/00Presence of polyester
    • C09J2467/005Presence of polyester in the release coating

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)

Abstract

The invention discloses a kind of modified polyolefin optical glue films and preparation method thereof of UV crosslinking curing, use the positive octene copolymer of ethylene-and ethylene-n-butene copolymer polyolefin resin for base-material, the range for the weight ratio that the positive octene copolymer of the ethylene-accounts for polyolefin blend resin is 0~100%;It is 100 parts according to polyolefin resin mixture base-material total weight, the modified polyolefin optical glue film of the UV crosslinking curing further includes following raw material by weight: 0.05~5 part of photoinitiator, 0.05~5 part of thermal initiator, 0.05~5 part of multi-group crosslink agent, 0.01~2 part of antioxidant, 0.01~2 part of light stabilizer, 0.1~3 part of tackifier, 1~20 part of tackifying resin.UV of the present invention, which solidifies cross-linking modified polyolefin optical glue film, to be had fast high reaction speed, high mechanical properties, the polar group that hydrolysis generates corrosion functional sheet will not occur, and weather resistance and block-water performance are with the unrivaled advantage of OCA and LOCA.

Description

A kind of polyolefin optical glue film and preparation method thereof that UV crosslinking curing is modified
Technical field
The present invention relates to the formula of optical adhesive film and its processing methods, technological parameter, in particular to a kind of to be applied to touch The modified polyolefin optical glue film and preparation method thereof of the UV crosslinking curing that screen, panel of LCD and naked eye 3D are bonded entirely.
Background technique
As touch screen, liquid crystal display and naked eye 3D screen are using more and more extensive, its full fitting proposed with raw material New requirement, there is high light transmission, be adapted to large scale, easy deaeration, high-weatherability etc..Lead at present it is to be applied have OCA and LOCA optical cement.OCA optical cement is a kind of two-sided fitting adhesive tape of no basis material, it is touch screen and liquid crystal display panel attachment Most common adhesive, but its be bonded difficulty it is big, to required precision height, especially to the touch screen of larger size and liquid crystal Screen (such as 7 inches or more) is very difficult to be bonded, and is easy to produce bubble, and cannot do over again.LOCA is on the basis of OCA optical cement A kind of liquid optical cement of development, it is a kind of UV cured acrylic esters liquid optical cement, is suitable for touch screen and liquid crystal display The problems such as panel bonds, but its generally existing easy gummosis, bubble difficulty are removed, and production efficiency is low.Therefore, it is badly in need of one in display field Kind simple process, high production efficiency, the novel optical material for reducing fitting fraction defective, to adapt to the development of display field especially The demand of large size panel product fitting.
Summary of the invention
For overcome the deficiencies in the prior art, the polyolefin optical glue film modified the invention proposes a kind of UV crosslinking curing And preparation method thereof, applied to the full fitting field of touch screen, liquid crystal display and naked eye 3D, not only have attaching process it is easy, It can do over again, improve production efficiency, reduce the characteristics of fraction defective and production cost, simultaneously because polyolefin is nonpolar high durable Polymer material, the generation polar group corrosion functional sheet that will not be hydrolyzed, has excellent weather resistance, water vapor barrier property Energy.
A kind of technical solution of the modified polyolefin optical glue film of UV crosslinking curing proposed by the present invention is as follows: using second The positive octene copolymer of alkene-and ethylene-n-butene copolymer polyolefin resin are base-material, the positive octene copolymer of the ethylene- The range for accounting for the weight ratio of polyolefin blend resin is 0~100%;It is according to polyolefin resin mixture base-material total weight 100 parts, the modified polyolefin optical glue film of the UV crosslinking curing further includes following raw material by weight:
As further technical solution of the present invention, the photoinitiator can be contracted by benzoin and its derivative, benzil Ketone derivatives, benzophenone and its derivative, acetophenone derivs, alkylbenzene ketone and its derivative, aroyl phosphine oxide And its derivative, aroyl phosphate and its derivative, Sulfo-benzophenone class compound, esterification oximinoketone compound, aryl mistake Oxygen ester compounds, halogenated methyl arone, benzoyl formiate, benzophenone and its derivative, thioxanthone and its derivative, anthracene Quinone and its derivative, triaryl salt compounded of iodine and its derivative, alkyl salt compounded of iodine and its derivative, triaryl sulfonium salts and its derivative The mixture of one or more of object, isopropylbenzene cyclopentadienyl iron and its derivative.
As further technical solution of the present invention, the free radical thermal initiator can be by tert-butyl hydroperoxide isobutyl carbonate third Bis- (tert-butyl peroxy base) hexanes of ester, 2,5- dimethyl -2,5-, bis- (tert-butyl peroxide) -3 1-, 3,5- trimethyl-cyclohexanes, Tert-butyl hydroperoxide carbonic acid -2- ethylhexyl, bis- (t-butyl peroxy) -3 1,1-, the bis- (uncles of 3,5- trimethyl-cyclohexanes, 1,1- Amyl peroxy) -3, bis- (t-amyl peroxy) hexamethylenes of 3,5- trimethyl-cyclohexanes, 1,1-, bis- (t-butyl peroxy) hexamethylenes of 1,1- Bis- (t-butyl peroxy) butane of alkane, 2,2-, peroxidating 2- ethylhexyl carbonate tert-pentyl ester, 2,5- dimethyl 2, the bis- (benzoyls of 5- Peroxide)-hexane, peroxidating carbonic acid tert-pentyl ester, 3,3,5 trimethylhexanoate of peroxidating it is one or more press any proportion Mixing composition.
As further technical solution of the present invention, the multi-group crosslink agent be cyanuric acid triacrylate, three Polyisocyanate triacrylate, trimethylolpropane trimethacrylate, pentaerythritol triacrylate, tripropylene glycol dipropyl One kind of olefin(e) acid ester, hydroxyethyl meth acrylate, isobornyl methacrylate and other acrylate derivatives or two Kind or more mixture.
As further technical solution of the present invention, the antioxidant is phosphoric acid ester, phosphorous acid esters, Hinered phenols The mixture of one or more of antioxidant.The hindered phenol anti-oxidants are four [β-(3,5- di-t-butyls Phenyl) propionic acid] Ji Shusi alcohol ester, three (2,4- di-tert-butyl-phenyl) phosphite esters, β-(3,5- di-tert-butyl-hydroxy phenyl) Propionic acid n-octadecyl alcohol ester, ethylene bis- (oxyethylene groups) is bis- [3- (5- tertiary butyl-4-hydroxy-tolyl) propionic ester], described Phosphate-based antioxidants and phosphite antioxidant be triphenyl phosphite, triphenyl phosphate, one benzene two of phosphorous acid Different monooctyl ester, the different monooctyl ester of phosphorous acid hexichol one, phosphorous acid 4,4- bis- isodigeranyl phenol (12-14) carbon Arrcostab, phosphorous acid three (2,4 '-two T-butyl-phenyl) ester it is one or more kinds of according to any than mixing composition.
As further technical solution of the present invention, the light stabilizer is hindered amine light stabilizer, by 3,5-, bis- uncle Butyl -4- hydroxy-benzoic acid cetyl ester, three (1,2,2,6,6- pentamethyl -4- piperidyl) phosphite esters, decanedioic acid be double - 2,2,6,6- tetramethyl piperidine alcohol esters, double -1- decane oxygroups -2,2,6,6- tetramethyl piperidine -4- alcohol sebacates, succinic acid and 4- hydroxyl -2,2, polymer, the N of 6,6- tetramethyl -1- piperidine alcohols, bis- (2,2,6, the 6- tetramethyl -4- piperidyls) -1,6- of N ' - Hexamethylene diamine and 2, chloro- 6- (1,1,3, the 3- tetramethyl butyl) amino -1,3,5-triazines of 4- bis- polymer, N, N '-it is bis- (2,2, 6,6- tetramethyl 4- piperidyls) -1,6- hexamethylene diamine and morpholine -2, one kind or more of the polymer of 4,6- tri- chloro-1,3,5-triazines Kind is by any proportion mixing composition.
As further technical solution of the present invention, the tackifier are gamma-aminopropyl-triethoxy-silane, 3- contracting Water glyceryl etheroxypropyltrimethoxysilane, γ-methacryloxypropyl trimethoxy silane, N- (β-aminoethyl)- Gamma-aminopropyl-triethoxy-silane, vinyltrimethoxysilane, vinyl three (β-methoxy ethoxy) silane, γ-mercapto Propyl-triethoxysilicane, 3- piperazinopropyl methyl dimethoxysilane, anilinomethyl triethoxysilane, γ-(2,3- rings The third oxygen of oxygen) one or more of propyl trimethoxy silicane mixture.
As further technical solution of the present invention, the tackifying resin is by the oligomeric of acrylic resin or derivatives thereof Resin composition, the oligomeric resin of described acrylic resin or derivatives thereof are unsaturated polyester (UP), epoxy acrylate, polyurethane third Olefin(e) acid ester, polyester acrylate, polyethers acrylic ester, pure acrylic resin, epoxy resin, one or both of organic siliconresin Above mixture.
Another aspect of the present invention, in order to prepare the modified polyolefin optical glue film of above-mentioned UV crosslinking curing, the present invention Additionally provide a kind of preparation method of UV crosslinking curing improved polyalkene optical adhesive film, comprising the following steps:
S101, by weight ratio by the positive octene polymer of ethylene-or ethylene-n-butene polymer resin, light-initiated Agent, thermal initiator, multi-group crosslink agent, antioxidant, light stabilizer, tackifier and the tackifying resin high speed in high-speed mixer It is mixed, obtains being uniformly mixed mixture;
S102, the mixture of step S101 is uniformly mixed and is squeezed out by double screw extruder, extrusion temperature for 80~ 120 DEG C, extrudate is through supercooling, and traction, pelletizing is at particle master batch;
S103, master batch investment single screw rod is cast in extruder, it is solid to obtain UV crosslinking for repressed, cooling, traction, winding Change improved polyalkene optical adhesive film, the UV crosslinking curing improved polyalkene optical adhesive film with a thickness of 0.1~0.9mm.
Further, in step s 103, one is respectively enclosed simultaneously in the front and back of the extrudate of single screw rod curtain coating extruding zone Layer PE and PET protection film, and through curtain coating, compacting, cooling, traction, winding, obtaining upper and lower level is PE and PET protection film, and centre is The polyolefin optical glue film of optical adhesive layer, the polyolefin optical glue film with a thickness of 0.1-0.9mm.
Enclosing one layer of PET simultaneously at the extrudate back side of curtain coating section can prevent extrudate in curtain coating, traction, wrapup procedure The elastic stretching deformation occurred by tractive force;Protection work can be played to the surface of extrudate by enclosing one layer of PE protective film simultaneously in front With, prevent optical adhesive layer during production, cross cutting, transport, fitting be contaminated, more convenient operation, efficiency during fitting It is higher, while optical adhesive layer service life is longer.In the prior art without using this technology, cause in practical applications very Retraction and deformation phenomenon occur after cross cutting for big waste of material and generation optical adhesive film.
As further technical solution of the present invention, among above-mentioned steps, the polyolefin optical glue film is in 50-80 DEG C vacuum laminator precompressed fitting after, the spoke at 400~4000Mw of light intensity, the mercury lamp or LED lamp source of 200~500nm of wavelength According to 10 seconds~5 minutes, i.e. cross-linkable solidifying.
Compared with prior art, the beneficial effects of the present invention are:
1) UV of the present invention, which solidifies cross-linking modified polyolefin optical glue film, may replace traditional OCA and LOCA optics Glue, when this method is bonded for touch screen and liquid crystal display, simple process, energy conservation and environmental protection, bubble-free can do over again, greatly mention Height fitting production efficiency, reduces fitting fraction defective and production cost;
2) UV of the present invention solidify cross-linking modified polyolefin optical glue film have fast high reaction speed, high mechanical properties, The polar group that hydrolysis generates corrosion functional sheet will not occur, weather resistance and block-water performance have OCA and LOCA without comparable Quasi- advantage.Also have excellent translucency, caking property, thermal stability, antidetonation anti-knock properties strong simultaneously, long service life can expire Sufficient modern touch-screen is especially vehicle-mounted, outdoor display screen, large scale touch screen are to the higher performance requirement of optical film, is more advantageous to Touch screen industry advances.
Detailed description of the invention
Fig. 1 is a kind of preparation method flow chart element of UV crosslinking curing improved polyalkene optical adhesive film of the embodiment of the present invention Figure.
Specific embodiment
Specific embodiments of the present invention will be further explained below.It should be noted that for these implementations The explanation of mode is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, invention described below Technical characteristic involved in each embodiment can be combined with each other as long as they do not conflict with each other.
The present invention provides a kind of technical solution of the modified polyolefin optical glue film of UV crosslinking curing is as follows: using second The positive octene copolymer of alkene-and ethylene-n-butene copolymer polyolefin resin are base-material, the positive octene copolymer of the ethylene- The range for accounting for the weight ratio of polyolefin blend resin is 0~100%;It is according to polyolefin resin mixture base-material total weight 100 parts, the modified polyolefin optical glue film of the UV crosslinking curing further includes following raw material by weight:
As shown in Figure 1, in order to prepare the modified polyolefin optical glue film of above-mentioned UV crosslinking curing, the present invention also provides A kind of preparation method of UV crosslinking curing improved polyalkene optical adhesive film, comprising the following steps:
S101, by weight ratio by the positive octene polymer of ethylene-or ethylene-n-butene polymer resin, light-initiated Agent, thermal initiator, multi-group crosslink agent, antioxidant, light stabilizer, tackifier and the tackifying resin high speed in high-speed mixer It is mixed, obtains being uniformly mixed mixture;
S102, the mixture of step S101 is uniformly mixed and is squeezed out by double screw extruder, extrusion temperature for 80~ 120 DEG C, extrudate is through supercooling, and traction, pelletizing is at particle master batch;
S103, master batch investment single screw rod is cast in extruder, it is solid to obtain UV crosslinking for repressed, cooling, traction, winding Change improved polyalkene optical adhesive film, the UV crosslinking curing improved polyalkene optical adhesive film with a thickness of 0.1~0.9mm.
Embodiment 1:
The positive octene copolymer of ethylene-by weight ratio, MI 15,60 DEG C 100 parts of fusing point, photoinitiator 1- hydroxyl ring 1.5 parts of hexyl phenyl ketone, 0.5 part of multi-group crosslink agent of thermal initiator peroxidating 2- ethylhexyl carbonate tert-pentyl ester, three hydroxyl first 2 parts of base propane trimethyl acrylic ester, 0.2 part of the polymer of light stabilizer 4- hydroxyl -2,2,6,6- tetramethyl -1- piperidine alcohols, 0.2 part of antioxidant β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecyl alcohol ester, tackifier 3- methacryloxypropyl 2 parts of base propyl trimethoxy silicane, mixed at high speed uniformly obtains mixture, and mixture is put into double screw extruder, squeezes out Temperature is 100 DEG C, cooling, and pelletizing obtains master batch;By master batch put into single screw rod extrudate through curtain coating, compacting, cooling, traction, Winding, while one layer of PE and PET protection film are respectively enclosed in the front and back of the extrudate in curtain coating section, and through curtain coating, compacting, cooling, Traction, winding, obtain upper and lower layer be PE and PET protection film, centre be optical adhesive layer optical film, optical adhesive layer with a thickness of 0.25mm。
Embodiment 2:
The positive octene copolymer of ethylene-by weight ratio, MI 15,60 DEG C 70 parts of fusing point, ethylene-n-butene copolymer, MI is 45,45 DEG C 30 parts of fusing point, 1.5 parts of photoinitiator 1- hydroxycyclohexyl phenyl ketone, and thermal initiator peroxidating 2- ethyl hexyl 0.5 part of base carbonic acid tert-pentyl ester, 2 parts of multi-group crosslink agent's trimethylol-propane trimethacrylate, light stabilizer 4- hydroxyl- 0.2 part of polymer, antioxidant β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid of 2,2,6,6- tetramethyl -1- piperidine alcohols Positive 0.2 part of octadecanol ester, 2 parts of tackifier 3- methacryloxypropyl trimethoxy silane, mixed at high speed uniformly obtains Mixture puts into mixture in double screw extruder, and extrusion temperature is 100 DEG C, and cooling, pelletizing obtains master batch;Master batch is thrown Enter to single screw rod extrudate through curtain coating, compacting, cooling, traction, winding, while the front and back of the extrudate in curtain coating section is each attached Upper one layer of PE and PET protection film, and through curtain coating, compacting, cooling, traction, winding, obtaining upper and lower layer is PE and PET protection film, Centre is the optical film of optical adhesive layer, and optical adhesive layer is with a thickness of 0.25mm.
Embodiment 3:
The positive octene copolymer of ethylene-by weight ratio, MI 15,60 DEG C 50 parts of fusing point, ethylene-n-butene copolymer, MI is 45,45 DEG C 50 parts of fusing point, 1.5 parts of photoinitiator 1- hydroxycyclohexyl phenyl ketone, and thermal initiator peroxidating 2- ethyl hexyl 0.5 part of base carbonic acid tert-pentyl ester, 2 parts of multi-group crosslink agent's trimethylol-propane trimethacrylate, light stabilizer 4- hydroxyl- 0.2 part of polymer, antioxidant β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid of 2,2,6,6- tetramethyl -1- piperidine alcohols Positive 0.2 part of octadecanol ester, 2 parts of tackifier 3- methacryloxypropyl trimethoxy silane, mixed at high speed uniformly obtains Mixture puts into mixture in double screw extruder, and extrusion temperature is 100 DEG C, and cooling, pelletizing obtains master batch;Master batch is thrown Enter to single screw rod extrudate through curtain coating, compacting, cooling, traction, winding, while the front and back of the extrudate in curtain coating section is each attached Upper one layer of PE and PET protection film, and through curtain coating, compacting, cooling, traction, winding, obtaining upper and lower layer is PE and PET protection film, Centre is the optical film of optical adhesive layer, and optical adhesive layer is with a thickness of 0.25mm.
Embodiment 4:
The positive octene copolymer of ethylene-by weight ratio, MI 15,60 DEG C 30 parts of fusing point, ethylene-n-butene copolymer, MI is 45,45 DEG C 70 parts of fusing point, 1.5 parts of photoinitiator 1- hydroxycyclohexyl phenyl ketone, and thermal initiator peroxidating 2- ethyl hexyl 0.5 part of base carbonic acid tert-pentyl ester, 2 parts of multi-group crosslink agent's trimethylol-propane trimethacrylate, light stabilizer 4- hydroxyl- 0.2 part of polymer, antioxidant β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid of 2,2,6,6- tetramethyl -1- piperidine alcohols Positive 0.2 part of octadecanol ester, 2 parts of tackifier 3- methacryloxypropyl trimethoxy silane, mixed at high speed uniformly obtains Mixture puts into mixture in double screw extruder, and extrusion temperature is 100 DEG C, and cooling, pelletizing obtains master batch;Master batch is thrown Enter to single screw rod extrudate through curtain coating, compacting, cooling, traction, winding, while the front and back of the extrudate in curtain coating section is each attached Upper one layer of PE and PET protection film, and through curtain coating, compacting, cooling, traction, winding, obtaining upper and lower layer is PE and PET protection film, Centre is the optical film of optical adhesive layer, and optical adhesive layer is with a thickness of 0.25mm.
Embodiment 5:
Ethylene-n-butene copolymer by weight ratio, MI 45,45 DEG C 100 parts of fusing point, photoinitiator 1- hydroxyl ring 1.5 parts of hexyl phenyl ketone, 0.5 part of multi-group crosslink agent of thermal initiator peroxidating 2- ethylhexyl carbonate tert-pentyl ester, three hydroxyl first 2 parts of base propane trimethyl acrylic ester, 0.2 part of the polymer of light stabilizer 4- hydroxyl -2,2,6,6- tetramethyl -1- piperidine alcohols, 0.2 part of antioxidant β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecyl alcohol ester, tackifier 3- methacryloxypropyl 2 parts of base propyl trimethoxy silicane, mixed at high speed uniformly obtains mixture, and mixture is put into double screw extruder, squeezes out Temperature is 100 DEG C, cooling, and pelletizing obtains master batch;By master batch put into single screw rod extrudate through curtain coating, compacting, cooling, traction, Winding, while one layer of PE and PET protection film are respectively enclosed in the front and back of the extrudate in curtain coating section, and through curtain coating, compacting, cooling, Traction, winding, obtain upper and lower layer be PE and PET protection film, centre be optical adhesive layer optical film, optical adhesive layer with a thickness of 0.25mm。
The optical adhesive film obtained through the foregoing embodiment with comparative example is assessed, assessment result through following test methods It is listed in table 1:
(1) degree of cross linking
Sample making: taking two panels 1mm heavy sheet glass, optical adhesive film, PET release film, according to lower glass-release film-optical cement The sequence that film-release film-goes up glass is placed, and after 80 DEG C of vacuum laminator precompressed are bonded, in light intensity 1200Mw, peak wavelength is The mercury lamp of 310-365nm irradiates 1 minute.Glue film after solidification is taken out to test from release film.
(2) light transmittance
Sample making: the same degree of cross linking of method.
Test method is with reference to light transmittance in national standard GB/T 2410-2008 " measurement of transparent plastic light transmittance and mist degree " Part.
(3) glass/packaging adhesive film adhesion strength
" 180 ° of peeling strength test method flexible materials of adhesive are to rigidity with reference to standard GB/T/T2790 for test method Material ".
Sample making: taking 1mm heavy sheet glass, optical adhesive film, 0.2mm transparent PET substrate, by glass-optical film-PET times Sequence is placed, and after 80 DEG C of vacuum laminator precompressed are bonded, in light intensity 1200Mw, the mercury lamp that peak wavelength is 310-365nm irradiates 1 Minute.It is tested on puller system, peeling rate 100mm/min, records tensile strength numerical value
(4) wet-heat resisting accelerated ageing is tested
Sample making: it takes two panels with a thickness of 1mm glass, clamps optical adhesive film, sample specification 100mm* above and below 100mm, after 80 DEG C of vacuum laminator precompressed are bonded, in light intensity 1200Mw, the mercury lamp that peak wavelength is 310-365nm irradiates 1 Minute.Carry out the accelerated hydrothermal aging experiment of following condition:
Temperature: whether 85 DEG C of 85% time of humidity 1000h, the sample after aging there is the phenomenon that delamination, bubble, xanthochromia.
Table 1
Test result: can find from the result of embodiment 1-5 sum: optical adhesive film of the present invention is in wet and heat ageing resistant Performance, has obviously superiority at water vapor rejection performance.The scheme of adopted proposition in the present invention, can fully meet touch Screen assembly is to the higher demand of optical cement performance.
Above the embodiments of the present invention are described in detail, but the present invention is not limited to described embodiments.It is right For those skilled in the art, in the case where not departing from the principle of the invention and spirit, these embodiments are carried out more Kind change, modification, replacement and modification, still fall in protection scope of the present invention.

Claims (10)

1. a kind of modified polyolefin optical glue film of UV crosslinking curing, which is characterized in that using the positive octene copolymer of ethylene-and second Alkene-n-butene copolymer polyolefin resin is base-material, and the positive octene copolymer of the ethylene-accounts for polyolefin blend resin The range of weight ratio is 0~100%;It is 100 parts according to polyolefin resin mixture base-material total weight, the UV crosslinking curing changes The polyolefin optical glue film of property further includes following raw material by weight:
2. the modified polyolefin optical glue film of UV crosslinking curing according to claim 1, which is characterized in that described light-initiated Agent can be by benzoin and its derivative, benzil ketals derivative, benzophenone and its derivative, acetophenone derivs, alkyl Benzophenone class and its derivative, aroyl phosphine oxide and its derivative, aroyl phosphate and its derivative, Sulfo-benzophenone Class compound, esterification oximinoketone compound, aryl peroxide ester compounds, halogenated methyl arone, benzoyl formiate, benzophenone and Its derivative, thioxanthone and its derivative, anthraquinone and its derivative, triaryl salt compounded of iodine and its derivative, alkyl salt compounded of iodine And its derivative, triaryl sulfonium salts and its derivative, one or more of isopropylbenzene cyclopentadienyl iron and its derivative it is mixed Close object.
3. the modified polyolefin optical glue film of UV crosslinking curing according to claim 1, which is characterized in that the heat causes Agent can be by bis- (tert-butyl peroxy base) hexanes of tert-butyl hydroperoxide propylene carbonate, 2,5- dimethyl -2,5-, bis- (the peroxidating uncles of 1- Butyl) -3,3,5- trimethyl-cyclohexanes, tert-butyl hydroperoxide carbonic acid -2- ethylhexyl, bis- (t-butyl peroxy) -3 1,1-, 3, Bis- (t-amyl peroxy) -3 5- trimethyl-cyclohexane, 1,1-, bis- (t-amyl peroxy) hexamethylenes of 3,5- trimethyl-cyclohexanes, 1,1- Bis- (t-butyl peroxy) hexamethylenes of alkane, 1,1-, bis- (t-butyl peroxy) butane of 2,2-, peroxidating 2- ethylhexyl carbonate uncle penta Ester, 2,5- dimethyl 2, bis- (benzoyl the peroxide)-hexanes of 5-, peroxidating carbonic acid tert-pentyl ester, 3,3,5 tri-methyl hexanoic acid uncle of peroxidating The one or more of butyl ester are formed by the mixing of any proportion.
4. the modified polyolefin optical glue film of UV crosslinking curing according to claim 1, which is characterized in that described multifunctional Group's crosslinking agent is cyanuric acid triacrylate, cyamelide triacrylate, trimethylolpropane trimethacrylate, season penta Tetrol triacrylate, tri (propylene glycol) diacrylate, hydroxyethyl meth acrylate, isobornyl methacrylate, And one or more kinds of mixtures of other acrylate derivatives.
As further technical solution of the present invention, the antioxidant is phosphoric acid ester, phosphorous acid esters, Hinered phenols antioxygen The mixture of one or more of agent.The hindered phenol anti-oxidants are four [β-(3,5- di-tert-butyl-phenyl) Propionic acid] Ji Shusi alcohol ester, three (2,4- di-tert-butyl-phenyl) phosphite esters, β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid Positive octadecanol ester, ethylene bis- (oxyethylene groups) is bis- [3- (5- tertiary butyl-4-hydroxy-tolyl) propionic ester], the phosphorus Esters of gallic acid antioxidant and phosphite antioxidant are triphenyl phosphite, triphenyl phosphate, and one benzene two of phosphorous acid is different pungent Ester, the different monooctyl ester of phosphorous acid hexichol one, phosphorous acid 4,4- bis- isodigeranyl phenol (12-14) carbon Arrcostab, (2,4 '-two special fourths of phosphorous acid three Base phenyl) ester it is one or more kinds of according to any than mixing composition.
5. the modified polyolefin optical glue film of UV crosslinking curing according to claim 1, which is characterized in that the light is stablized Agent is hindered amine light stabilizer, by 3,5- di-t-butyl -4- hydroxy-benzoic acid cetyl ester, three (1,2,2,6,6- five first Base -4- piperidyl) phosphite ester, decanedioic acid double -2,2,6,6- tetramethyl piperidine alcohol esters, double -1- decane oxygroups -2,2,6,6- tetra- Methyl piperidine -4- alcohol sebacate, succinic acid and 4- hydroxyl -2,2, polymer, the N of 6,6- tetramethyl -1- piperidine alcohols, N '-are bis- (2,2,6,6- tetramethyl -4- piperidyl) -1,6- hexamethylene diamine and 2,4- bis- chloro- 6- (1,1,3,3- tetramethyl butyl) amino -1, Bis- (2,2,6,6- tetramethyl 4- piperidyl) -1, the 6- hexamethylene diamines of polymer, the N of 3,5- triazines, N '-and morpholine -2,4,6- tri- is chloro- The one or more of the polymer of 1,3,5-triazines are formed by the mixing of any proportion.
6. the modified polyolefin optical glue film of UV crosslinking curing according to claim 1, which is characterized in that the tackifier For for gamma-aminopropyl-triethoxy-silane, 3- glycidyl ether oxypropyltrimethoxysilane, γ-methacryloxy Propyl trimethoxy silicane, N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silane, vinyltrimethoxysilane, vinyl Three ('beta '-methoxy ethyoxyl) silane, gamma-mercaptopropyltriethoxysilane, 3- piperazinopropyl methyl dimethoxysilane, benzene Amine methyltriethoxysilane, the mixing of one or more of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane Object.
7. the modified polyolefin optical glue film of UV crosslinking curing according to claim 1, which is characterized in that the thickening tree Rouge is to be made of the oligomeric resin of acrylic resin or derivatives thereof, and the oligomeric resin of described acrylic resin or derivatives thereof is Unsaturated polyester (UP), epoxy acrylate, urethane acrylate, polyester acrylate, polyethers acrylic ester, pure acrylic resin, Epoxy resin, the mixture of one or more of organic siliconresin.
8. a kind of preparation method of UV crosslinking curing improved polyalkene optical adhesive film is prepared such as claim 1-7 any one institute The modified polyolefin optical glue film of the UV crosslinking curing stated, which is characterized in that the described method comprises the following steps:
S101, by weight ratio by the positive octene polymer of ethylene-or ethylene-resin of n-butene polymer, photoinitiator, heat Initiator, multi-group crosslink agent, antioxidant, light stabilizer, tackifier and the tackifying resin mixed at high speed in high-speed mixer Stirring obtains being uniformly mixed mixture;
S102, the mixture of step S101 is uniformly mixed and is squeezed out by double screw extruder, extrusion temperature is 80~120 DEG C, extrudate is through supercooling, and traction, pelletizing is at particle master batch;
S103, master batch investment single screw rod is cast in extruder, repressed, cooling, traction, winding obtains UV crosslinking curing and changes Property polyolefin optical glue film, the UV crosslinking curing improved polyalkene optical adhesive film with a thickness of 0.1~0.9mm.
9. the preparation method of UV crosslinking curing improved polyalkene optical adhesive film according to claim 8, which is characterized in that In In step S103, one layer of PE and PET protection film are respectively enclosed simultaneously in the front and back of the extrudate of single screw rod curtain coating extruding zone, and Through curtain coating, compacting, cooling, traction, winding, obtaining upper and lower level is PE and PET protection film, and centre is the polyolefin light of optical adhesive layer Learn glue film, the polyolefin optical glue film with a thickness of 0.1-0.9mm.
10. the preparation method of UV crosslinking curing improved polyalkene optical adhesive film according to claim 8, which is characterized in that The UV crosslinking curing improved polyalkene optical adhesive film 50-80 DEG C vacuum laminator precompressed fitting after, light intensity 400~ It is irradiated 10 seconds~5 minutes under the mercury lamp or LED lamp source of 4000Mw, 200~500nm of wavelength, crosslinking curing.
CN201910587096.9A 2019-07-01 2019-07-01 A kind of polyolefin optical glue film and preparation method thereof that UV crosslinking curing is modified Pending CN110499111A (en)

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CN111320936A (en) * 2019-12-31 2020-06-23 深圳市立昕光学材料科技有限公司 Full-lamination optical adhesive applied to touch screen and preparation method thereof
CN111410918A (en) * 2020-05-28 2020-07-14 广州市隆创新材料有限公司 Hot-melt optical adhesive with dark-edge cohesiveness and preparation method thereof
CN111440545A (en) * 2020-04-10 2020-07-24 嘉兴市海睿新材料有限公司 Full-lamination reactive hot-melt optical adhesive and preparation method thereof
CN111500206A (en) * 2020-04-27 2020-08-07 广东硕成科技有限公司 Wafer cutting film easy to pick up and preparation method thereof
CN111534237A (en) * 2020-04-14 2020-08-14 中山大学 Photo-thermal dual-curing polyolefin packaging adhesive film and preparation method thereof
CN115011283A (en) * 2022-07-13 2022-09-06 新纶电子材料(常州)有限公司 Hot melt adhesive particle, laminated busbar insulation adhesive film and preparation method thereof
CN115368831A (en) * 2021-05-18 2022-11-22 杭州福斯特应用材料股份有限公司 Packaging adhesive film and preparation method thereof

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CN111117498B (en) * 2019-12-26 2022-04-29 江苏鹿山新材料有限公司 Photo-thermal dual-curing POE (polyolefin elastomer) packaging adhesive film for photovoltaic and preparation method thereof
CN111320936A (en) * 2019-12-31 2020-06-23 深圳市立昕光学材料科技有限公司 Full-lamination optical adhesive applied to touch screen and preparation method thereof
CN111440545A (en) * 2020-04-10 2020-07-24 嘉兴市海睿新材料有限公司 Full-lamination reactive hot-melt optical adhesive and preparation method thereof
CN111534237A (en) * 2020-04-14 2020-08-14 中山大学 Photo-thermal dual-curing polyolefin packaging adhesive film and preparation method thereof
CN111534237B (en) * 2020-04-14 2021-10-08 中山大学 Photo-thermal dual-curing polyolefin packaging adhesive film and preparation method thereof
CN111500206A (en) * 2020-04-27 2020-08-07 广东硕成科技有限公司 Wafer cutting film easy to pick up and preparation method thereof
CN111410918A (en) * 2020-05-28 2020-07-14 广州市隆创新材料有限公司 Hot-melt optical adhesive with dark-edge cohesiveness and preparation method thereof
CN115368831A (en) * 2021-05-18 2022-11-22 杭州福斯特应用材料股份有限公司 Packaging adhesive film and preparation method thereof
CN115368831B (en) * 2021-05-18 2024-02-20 杭州福斯特应用材料股份有限公司 Packaging adhesive film and preparation method thereof
CN115011283A (en) * 2022-07-13 2022-09-06 新纶电子材料(常州)有限公司 Hot melt adhesive particle, laminated busbar insulation adhesive film and preparation method thereof

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Application publication date: 20191126