CN110564340A - UV (ultraviolet) moisture dual-curing hot melt adhesive film and preparation method and application thereof - Google Patents
UV (ultraviolet) moisture dual-curing hot melt adhesive film and preparation method and application thereof Download PDFInfo
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- CN110564340A CN110564340A CN201910802991.8A CN201910802991A CN110564340A CN 110564340 A CN110564340 A CN 110564340A CN 201910802991 A CN201910802991 A CN 201910802991A CN 110564340 A CN110564340 A CN 110564340A
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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
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/002—Dendritic macromolecules
- C08G83/005—Hyperbranched macromolecules
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/04—Homopolymers or copolymers of ethene
- C09J123/08—Copolymers of ethene
- C09J123/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C09J123/0815—Copolymers of ethene with aliphatic 1-olefins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/04—Homopolymers or copolymers of ethene
- C09J123/08—Copolymers of ethene
- C09J123/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C09J123/0853—Vinylacetate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/35—Heat-activated
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
- G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F2203/00—Indexing scheme relating to G06F3/00 - G06F3/048
- G06F2203/041—Indexing scheme relating to G06F3/041 - G06F3/045
- G06F2203/04103—Manufacturing, i.e. details related to manufacturing processes specially suited for touch sensitive devices
Abstract
the invention belongs to the technical field of adhesive film preparation, and particularly relates to a UV (ultraviolet) moisture dual-curing hot melt adhesive film and a preparation method and application thereof. The hot melt adhesive film is prepared by taking a hyperbranched silicon-containing acrylate monomer as a main raw material and combining components such as resin, a photoinitiator, a silane coupling agent, a catalyst, an antioxidant and a light stabilizer, so that the adhesive film which can be cured by UV light irradiation and/or moisture is conveniently cured by continuous moist heat without UV light irradiation, the peel strength of the black edge part of the touch screen is improved, and the packaging problem of the touch screen is solved.
Description
Technical Field
The invention belongs to the technical field of adhesive film preparation, and particularly relates to a UV (ultraviolet) moisture dual-curing hot melt adhesive film and a preparation method and application thereof.
Background
Touch screen market demand is getting bigger and bigger, need use the laminating of optical cement in its production process. The optical cement in the current market is divided into three types: one is OCA, namely a transparent substrate-free double-sided adhesive tape, has a long application history, but has the defects of high initial adhesion, extremely low fluidity, difficult bubble discharge in the processing process, and mainly attachment to a mobile phone or a screen below 10 inches; the second type is LOCA, namely liquid optical cement, which is liquid in the processing process and solid after curing, has better elasticity and light transmittance, and can be suitable for large size. The third type is a hot-melt optical adhesive film, which has been developed in recent years, is suitable for attaching screens of various sizes, and has a simple processing process and easy reverse disassembly. The hot-melt optical adhesive film can reduce the bonding threshold of the touch screen and the liquid crystal module thereof, improve the bonding yield and develop very rapidly in two years.
the traditional optical packaging is difficult to be suitable for automatic packaging of 60-90 inch oversized display screens, the defect rate is high, and reworking is complex; the black edge area of the corner of the oversized screen can overflow glue or delaminate after long-term use. Along with the development of hot melt optical adhesive film and full-automatic laminating production line, for LOCA and traditional OCA glue, packaging process is simpler can realize doing over again simultaneously and reduce the defective products and produce.
Along with the popularization of outdoor advertisements, education whiteboards and business all-in-one machines, the size of a packaged touch display screen is larger and larger, and the requirement of 60-100 inches is gradually developed. Because the touch screen size is very big, current UV hot melt adhesive can not provide effective protection at the touch screen that has the black border field, and the film is incomplete at the shade part solidification that shelters from, causes the touch screen frame or has the marginal colored printing ink place UV irradiation intensity weak, brings the peel strength in black border field inadequately, can produce the delaminating after long-term the use. Therefore, how to realize the reliable stability of the full-size range of the large-screen display screen so as to solve the problem that the black edge field cannot be completely cured is a big problem in the field of optical packaging.
Disclosure of Invention
The invention aims to provide a UV moisture dual-curing hot melt adhesive film and a preparation method and application thereof.
In order to solve the technical problems, the invention provides a UV moisture dual-curing hot melt adhesive film which comprises the following raw materials in parts by weight: resin: 80-95 parts; photoinitiator (2): 1-4 parts; hyperbranched silicon-containing acrylate monomer: 2-5 parts; silane coupling agent: 0.5-1 part; catalyst: 0.001-0.01 portion; antioxidant: 0.1-0.5 part; and light stabilizers: 0.1 to 0.5 portion.
Further, the structural formula of the hyperbranched silicon-containing acrylate monomer is as follows:
Wherein R is1Is CH2-CH2-Si(OMe)3，R2Is H or CH3。
Further, the resin comprises at least one of EVA resin and POE resin; wherein the content of VA in the EVA resin is 20-30%, and the melt index is 15-30g/10 min; and the content of octene in the POE resin is 20-40%, and the melt index is 15-30g/10 min.
Further, the photoinitiator includes 2-hydroxy-2-methyl-1-phenyl acetone, 1-hydroxy-cyclohexyl phenyl ketone, 1' - (methylenebis-4, 1-phenylene) bis [ 2-hydroxy-2-methyl-1-propanone, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone, 2-methyl-1- (4-methylthiophenyl) -2-morpholinyl-1-acetone, (2,4, 6-trimethylbenzoyl) diphenyl phosphine oxide, phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide and one or more of 2, 2-dimethoxy-2-phenyl acetophenone.
Further, the silane coupling agent comprises one or more of vinyl trimethoxy silane, vinyl triacetoxy silane and vinyl tri (beta-methoxyethoxy) silane.
Further, the catalyst comprises one or more of cobalt naphthenate, cobalt stearate and stannous oxalate.
Further, the antioxidant comprises one or more of 2- [4, 6-bis (2, 4-dimethylphenyl) -1,3, 5-triazin-2-yl ] -5- (octyloxy) phenol, pentaerythritol tetrakis (3, 5-di-tert-butyl-4-hydroxy) phenylpropionate, and n-octadecyl 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate.
Further, the light stabilizer includes one or more of bis (1-octyloxy-2, 2,6, 6-tetramethyl-4-piperidyl) sebacate, bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate, and polysuccinic acid (4 hydroxy-2, 2,6, 6-tetramethyl-1-piperidylethanol ester).
In another aspect, the present invention further provides a method for preparing a UV moisture dual-curing hot melt adhesive film, including: preparing additive masterbatch; preparing a liquid auxiliary agent; adding resin and the additive master batch into a liquid auxiliary agent, and uniformly mixing by a mixer; extruding through a material extruder; and preparing the UV moisture dual-curing hot melt adhesive film through a casting die head.
Further, mixing an antioxidant, a light stabilizer, a photoinitiator and resin, and extruding the mixture through a co-rotating meshed double-screw extruder to obtain the additive masterbatch; wherein the twin-screw rotating speed of the co-rotating meshed twin-screw extruder is 40r/min-60r/min, and the temperature of each section is 100 ℃, 120 ℃, 130 ℃, 140 ℃ and 140 ℃ in sequence.
Further, adding a catalyst into the mixture of the hyperbranched silicon-containing acrylate monomer and the silane coupling agent, and uniformly dispersing to form the liquid auxiliary agent.
Further, the mixer is a vertical double-ribbon mixer, the driving power of the mixer is 3KW-120KW, the mixing temperature is 35-45 ℃, and the mixing time is 2-5 hours.
Further, the material extruder is a single screw extruder, the diameter of a screw is 130mm, the rotating speed of the screw is 30-60r/min, and the temperature of each section is 75 ℃, 80 ℃, 84 ℃, 85 ℃ and 85 ℃ in sequence.
on the other hand, the invention also provides application of the UV moisture dual-curing hot melt adhesive film in packaging the touch screen.
The UV moisture dual-curing hot melt adhesive film and the preparation method and application thereof have the advantages that the UV moisture dual-curing hot melt adhesive film is prepared by taking the hyperbranched silicon-containing acrylate monomer as a main raw material and combining the components such as resin, a photoinitiator, a silane coupling agent, a catalyst, an antioxidant, a light stabilizer and the like, and has simple synthesis process, no pollution and the like; by adjusting the content of the hyperbranched silicon-containing acrylate monomer and the catalyst, the UV and moisture curing rate can be improved to meet the packaging requirements of different types of touch screens, the defect that the shadow part or the bottom part of the hot melt adhesive film touch screen cannot be cured is avoided, and the problem of weak corner peeling strength in the field of black edges is solved.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
in order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a flow chart of the process for preparing the hot melt adhesive film of the present invention;
FIG. 2 is an infrared spectrum of a hyperbranched silicon-containing acrylate monomer of the invention;
FIG. 3 shows the CDCl of the hyperbranched silicon-containing acrylate monomer of the invention3Hydrogen spectra in solution;
FIG. 4 is a GPC chart of a hyperbranched silicon-containing acrylate monomer of the invention in THF solution.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
interpretation of custom nouns or English abbreviations:
UV: ultraviolet rays;
KH 550: KH550 type silane coupling agent with CAS number 919-30-2;
THF: tetrahydrofuran, a heterocyclic organic compound;
EVA resin: from nonpolar, crystalline vinyl monomers (C)2H4) And a strongly polar, noncrystalline vinyl acetate monomer (CH)3COOC2H3) A thermoplastic resin obtained by high-pressure bulk polymerization in the presence of an initiator;
POE resin: a polymer blend comprised of octene and a polyolefin resin, the continuous phase and the dispersed phase exhibiting two phase separation;
triacrylate: acrylates containing three functional groups, such as glycerol triacrylate, trimethylolpropane triacrylate (TMPTA), or mixtures of the two; and trimethylolpropane triacrylate of the formula (CH)2＝CHCOOCH2)3-CCH2CH3。
example 1
This embodiment 1 provides a UV moisture dual-curing hot melt adhesive film, which includes by weight: resin: 80-95 parts; photoinitiator (2): 1-4 parts; hyperbranched silicon-containing acrylate monomer: 2-5 parts; silane coupling agent: 0.5-1 part; catalyst: 0.001-0.01 portion; antioxidant: 0.1-0.5 part; and light stabilizers: 0.1 to 0.5 portion.
Optionally, the thickness of the prepared hot melt adhesive film is 0.1-0.5mm, preferably 0.2mm and 0.4mm, and can be freely adjusted based on the requirements of customers on the market.
Optionally, the UV moisture dual-curing hot melt adhesive film comprises the following raw materials in parts by weight: resin: 85 parts of a mixture; photoinitiator (2): 2 parts of (1); hyperbranched silicon-containing acrylate monomer: 3 parts of a mixture; silane coupling agent: 0.8 part; catalyst: 0.006 part of a lubricant; antioxidant: 0.3 part; and light stabilizers: 0.2 part.
Optionally, the UV moisture dual-curing hot melt adhesive film comprises the following raw materials in parts by weight: resin: 90 parts of a mixture; photoinitiator (2): 3 parts of a mixture; hyperbranched silicon-containing acrylate monomer: 4 parts of a mixture; silane coupling agent: 0.6 part; catalyst: 0.008 parts of; antioxidant: 0.2 part; and light stabilizers: 0.4 part.
FIG. 2 is an infrared spectrum of a hyperbranched silicon-containing acrylate monomer of the invention.
FIG. 3 shows the CDCl of the hyperbranched silicon-containing acrylate monomer of the invention3Hydrogen spectrum in solution.
FIG. 4 is a GPC chart of a hyperbranched silicon-containing acrylate monomer of the invention in THF solution.
As an alternative embodiment of the hyperbranched silicon-containing acrylate monomer.
The structural formula of the hyperbranched silicon-containing acrylate monomer is as follows:
Wherein R is1Is CH2-CH2-Si(OMe)3，R2Is H or CH3。
Optionally, the hyperbranched silicon-containing acrylate monomer can be synthesized from KH550, triacrylate and sodium alkoxide. And the triacrylate includes, but is not limited to, any one of glycerol triacrylate, trimethylolpropane triacrylate, or a mixture of both.
as shown in fig. 2 to 4, the hyperbranched silicon-containing acrylate monomer of the present embodiment is characterized by the following test by infrared spectroscopy (fig. 2), hydrogen spectroscopy (fig. 3), and GPC (fig. 4), respectively:
(1) Referring to FIG. 2, it can be seen from the infrared spectrum that 1270cm on the abscissa-1And 985cm-1respectively, the stretching vibration peaks of amido bond and acrylic ester C-O, and 1730cm-1、1630cm-1、1180cm-1And 800cm-1Are characteristic absorption peaks for acrylate functionality. Wherein the depth is 1080cm-1Is Si-O-C and an ester functionThe characteristic peaks of clusters overlap.
(2) referring to fig. 3, it can be found by hydrogen spectroscopy that three sets of characteristic absorption peaks with the abscissa of 5.80-6.56ppm verify the acrylate structure on the hyperbranched silicon-containing acrylate monomer. Peak 1(δ ═ 5.76 to 6.80ppm, CH2CHCOO-) and peak (2+3+4+5) [ delta ] 4.07-4.47ppm, OC (OCH)2CH2)3]by integrating the peak areas, it can be calculated that the ratio of the peak areas is 1.19/4, relative to the ratio of the formula () of the two monomers prior to reaction is 3/4, which means that 39.7% of the acrylate structure is reacted onto the hyperbranched silicon-containing acrylate monomer. Peak 9(δ 1.43-1.75ppm, NCH) is present2CH2CH2Si) and peak 10(δ 0.46-0.71ppm, CH)2CH2si) which indicates Si-O-C in the structural formula2H5There was a small amount of hydrolysis.
(3) Referring to FIG. 4, the average number average molecular weight of the hyperbranched silicon-containing acrylate is 3308g/mol, and the dispersity is 1.59, as seen from the GPC pattern of the hyperbranched silicon-containing acrylate in THF solution.
Therefore, the hyperbranched silicon-containing acrylate monomer of the embodiment can be used as a monomer to participate in the light curing reaction of the hot melt adhesive film in the early stage, and can also continue the crosslinking reaction under the moisture condition in the later stage, so that the adhesive strength of the adhesive film at the black edge of the display screen can be effectively improved.
Optionally, the resin includes, but is not limited to, at least one of EVA resin and POE resin; wherein the content of VA in the EVA resin is 20-30%, and the melt index is 15-30g/10 min; and the content of octene in the POE resin is 20-40%, and the melt index is 15-30g/10 min. By limiting the melt index of the resin, the bonding deaeration of the product is facilitated, and the yield can be improved; and the VA content and the octene content are limited, so that the resin has more excellent performance and the product is convenient to produce and process.
Optionally, the content of VA in the EVA resin is 25% and the melt index is 18g/10min, or the content of VA in the EVA resin is 28% and the melt index is 25g/10 min.
Optionally, the content of octene in the POE resin is 25% and the melt index is 25g/10min, or the content of octene in the POE resin is 35% and the melt index is 20g/10 min.
Alternatively, the photoinitiator includes, but is not limited to, 2-hydroxy-2-methyl-1-phenylacetone, 1-hydroxy-cyclohexylphenyl ketone, 1' - (methylenebis-4, 1-phenylene) bis [ 2-hydroxy-2-methyl-1-propanone, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone, 2-methyl-1- (4-methylthiophenyl) -2-morpholinyl-1-acetone, (2,4, 6-trimethylbenzoyl) diphenyl phosphine oxide, phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide and one or more of 2, 2-dimethoxy-2-phenyl acetophenone. The photoinitiator can absorb energy with a certain wavelength in an ultraviolet region (250-420 nm) to generate free radicals, so that the hyperbranched silicon-containing acrylate monomer is initiated to be crosslinked and cured.
Optionally, the silane coupling agent includes, but is not limited to, one or more of vinyltrimethoxysilane, vinyltriacetoxysilane, vinyltris (. beta. -methoxyethoxy) silane. The silane coupling agent can greatly improve the bonding strength of the hot melt adhesive film and the glass, and prevent the hot melt adhesive film from peeling off the surface of the touch screen.
Optionally, the catalyst comprises one or more of cobalt naphthenate, cobalt stearate and stannous oxalate, and can accelerate the reaction of KH550 and triacrylate to synthesize the hyperbranched silicon-containing acrylate monomer.
Optionally, the antioxidant includes, but is not limited to, one or more of 2- [4, 6-bis (2, 4-dimethylphenyl) -1,3, 5-triazin-2-yl ] -5- (octyloxy) phenol, pentaerythritol tetrakis (3, 5-di-tert-butyl-4-hydroxy) phenylpropionate, and n-octadecyl 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate. The antioxidant can delay or inhibit the oxidation process of the adhesive film, thereby preventing the adhesive film from aging and prolonging the service life of the adhesive film.
Optionally, the light stabilizer includes, but is not limited to, one or more of bis (1-octyloxy-2, 2,6, 6-tetramethyl-4-piperidyl) sebacate, bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate, and polysuccinic acid (4 hydroxy-2, 2,6, 6-tetramethyl-1-piperidylethanol ester). The light stabilizer can prevent or delay the light aging process and prolong the service life of the hot melt adhesive film.
Example 2
FIG. 1 is a flow chart of the preparation process of the hot melt adhesive film of the present invention.
as shown in fig. 1, based on embodiment 1, this embodiment 2 provides a method for preparing a UV moisture dual-curing hot melt adhesive film, including: preparing additive masterbatch; preparing a liquid auxiliary agent; adding resin and the additive master batch into a liquid auxiliary agent, and uniformly mixing by a mixer; extruding through a material extruder; and preparing the UV moisture dual-curing hot melt adhesive film through a casting die head.
further, mixing an antioxidant, a light stabilizer, a photoinitiator and resin, and extruding the mixture through a co-rotating meshed double-screw extruder to obtain the additive masterbatch; wherein the twin-screw rotating speed of the co-rotating meshed twin-screw extruder is 40r/min-60r/min, and the temperature of each section is 100 ℃, 120 ℃, 130 ℃, 140 ℃ and 140 ℃ in sequence.
further, adding a catalyst into the mixture of the hyperbranched silicon-containing acrylate monomer and the silane coupling agent, and uniformly dispersing to form the liquid auxiliary agent.
Further, the mixer is a vertical double-ribbon mixer, the driving power of the mixer is 3KW-120KW, the mixing temperature is 35-45 ℃, and the mixing time is 2-5 hours.
Further, the material extruder is a single screw extruder, the diameter of a screw is 130mm, the rotating speed of the screw is 30-60r/min, and the temperature of each section is 75 ℃, 80 ℃, 84 ℃, 85 ℃ and 85 ℃ in sequence.
For the contents of the components and the specific implementation of the hot melt adhesive film, reference is made to the related discussion in example 1, which is not repeated herein.
Example 3
Based on embodiments 1-2, embodiment 3 further provides an application of the UV moisture dual-curing hot melt adhesive film in packaging a touch screen.
Specifically, the hot melt adhesive film can be used as a hot melt optical adhesive film, can be cured in the environment of UV light and/or moisture, is used for packaging an oversized touch screen, and effectively solves the problem that the black edge field cannot be completely cured.
For the component contents and the specific implementation of the hot melt adhesive film, reference is made to the relevant discussion in examples 1-2, which is not repeated herein.
In summary, the UV moisture dual-curing hot melt adhesive film, the preparation method thereof and the application thereof in the packaging of the touch screen in embodiments 1 to 3 are implemented by using a hyperbranched silicon-containing acrylate monomer as a main raw material, and combining with components such as resin, a photoinitiator, a silane coupling agent, a catalyst, an antioxidant, a light stabilizer and the like to prepare a UV light irradiation and/or moisture curable adhesive film, so that the adhesive film can be cured by heat and humidity continuously without UV light irradiation, the peel strength of the black edge portion of the touch screen is improved, and the packaging problem of the touch screen is solved; the hyperbranched silicon-containing acrylate monomer is added into EVA or POE elastomer resin, the prepared adhesive film still belongs to hot melt adhesive, the packaging process is simple and convenient, reworking can be realized, and the packaging method is suitable for ensuring the yield of large-size touch screen packaging; by adjusting the content of the hyperbranched silicon-containing acrylate monomer and the catalyst, the UV and moisture curing rate can be improved to meet the packaging requirements of different types of touch screens, the defect that the shadow part or the bottom part of the hot melt adhesive film touch screen cannot be cured is avoided, the problem of poor corner peeling strength in the black edge field is solved, and the packaging requirements of various types of touch screens with super-large sizes can be met. Has the characteristics of simple process, no pollution, convenient operation and control, stable quality and high production efficiency.
Example 4
8 parts by mol of EVA resin, 2 parts by mol of 2-hydroxy-2-methyl-1-phenyl acetone, 0.2 part by mol of 2- [4, 6-bis (2, 4-dimethylphenyl) -1,3, 5-triazin-2-yl ] -5- (octyloxy) phenol and 0.2 part by mol of bis (1-octyloxy-2, 2,6, 6-tetramethyl-4-piperidyl) sebacate are mixed and extruded to prepare an additive master batch. 0.005 molar weight part of catalyst is dispersed in 2 molar weight parts of hyperbranched silicon-containing acrylate monomer and 0.5 molar weight part of vinyl trimethoxy silane to prepare the liquid auxiliary agent. Then, 80 molar parts by weight of EVA resin, the additive master batch and the dispersed liquid auxiliary agent are uniformly mixed in a slow mixing tank, a double-screw extruder is adopted to extrude the mixed material, and a film with the thickness of 0.2mm is prepared by tape casting. Wherein the VA content in the EVA resin is 28%.
Example 5
8 parts by mol of EVA resin, 3 parts by mol of 1-hydroxy-cyclohexylphenyl ketone, 0.25 part by mol of 2- [4, 6-bis (2, 4-dimethylphenyl) -1,3, 5-triazin-2-yl ] -5- (octyloxy) phenol, and 0.25 part by mol of bis (1-octyloxy-2, 2,6, 6-tetramethyl-4-piperidyl) sebacate were mixed and extruded to prepare an additive master batch. 0.005 molar weight part of catalyst is dispersed in 3 molar weight parts of hyperbranched silicon-containing acrylate monomer and 0.5 molar weight part of vinyl trimethoxy silane to prepare the liquid auxiliary agent. Then, 80 molar parts by weight of EVA resin, the additive master batch and the dispersed liquid auxiliary agent are uniformly mixed in a slow mixing tank, a double-screw extruder is adopted to extrude the mixed material, and a film with the thickness of 0.2mm is prepared by tape casting. Wherein the VA content in the EVA resin is 28%.
Example 6
8 parts by mol of EVA resin, 3 parts by mol of 2-methyl-1- (4-methylthiophenyl) -2-morpholinyl-1-propanone, 0.25 part by mol of 2- [4, 6-bis (2, 4-dimethylphenyl) -1,3, 5-triazin-2-yl ] -5- (octyloxy) phenol and 0.25 part by mol of bis (1-octyloxy-2, 2,6, 6-tetramethyl-4-piperidyl) sebacate are mixed and extruded to prepare the additive master batch. 0.005 molar part of catalyst is dispersed in 2 molar parts of hyperbranched silicon-containing acrylate monomer and 1 molar part of vinyl trimethoxy silane, and the liquid auxiliary agent is formed by uniform dispersion. Then, 85 parts by mol weight of EVA resin, the additive master batch and the dispersed liquid auxiliary agent are uniformly mixed in a slow mixing tank, a double-screw extruder is adopted to extrude the mixed material, and a film with the thickness of 0.2mm is prepared by tape casting. Wherein the VA content in the EVA resin is 30%.
Example 7
8 parts by mol of EVA resin, 3 parts by mol of (2,4, 6-trimethylbenzoyl) diphenylphosphine oxide, 0.25 part by mol of 2- [4, 6-bis (2, 4-dimethylphenyl) -1,3, 5-triazin-2-yl ] -5- (octyloxy) phenol, and 0.25 part by mol of bis (1-octyloxy-2, 2,6, 6-tetramethyl-4-piperidyl) sebacate were mixed and extruded to prepare an additive master batch. 0.005 molar weight part of catalyst is dispersed in 3 molar weight parts of hyperbranched silicon-containing acrylate monomer and 1 molar weight part of vinyl triacetoxysilane, and the liquid auxiliary agent is formed by uniform dispersion. Then, 85 parts by mol weight of EVA resin, the additive master batch and the dispersed liquid auxiliary agent are uniformly mixed in a slow mixing tank, a double-screw extruder is adopted to extrude the mixed material, and a film with the thickness of 0.2mm is prepared by tape casting. Wherein the VA content in the EVA resin is 30%.
Example 8
8 parts by mol of EVA resin, 3 parts by mol of (2,4, 6-trimethylbenzoyl) diphenylphosphine oxide, 0.25 part by mol of 2- [4, 6-bis (2, 4-dimethylphenyl) -1,3, 5-triazin-2-yl ] -5- (octyloxy) phenol and 0.25 part by mol of bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate were mixed and extruded to prepare an additive master batch. 0.005 molar part of catalyst is dispersed in 2 molar parts of hyperbranched silicon-containing acrylate monomer and 1 molar part of vinyl tri (beta-methoxyethoxy) silane, and the mixture is uniformly dispersed to form the liquid assistant. Then, 85 parts by mol weight of EVA resin, the additive master batch and the dispersed liquid auxiliary agent are uniformly mixed in a slow mixing tank, a double-screw extruder is adopted to extrude the mixed material, and a film with the thickness of 0.2mm is prepared by tape casting. Wherein the VA content in the EVA resin is 33%.
example 9
8 parts by mol of EVA resin, 3 parts by mol of phenylbis (2,4, 6-trimethylbenzoyl) phosphine oxide, 0.25 part by mol of 2- [4, 6-bis (2, 4-dimethylphenyl) -1,3, 5-triazin-2-yl ] -5- (octyloxy) phenol and 0.25 part by mol of bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate were mixed and extruded to prepare an additive master batch. 0.005 molar parts by weight of catalyst was dispersed in 3 molar parts by weight of hyperbranched silicon-containing acrylate monomer and 1 molar part by weight of vinyltris (. beta. -methoxyethoxy) silane to form a liquid adjuvant. Then, 85 parts by mol weight of EVA resin, the additive master batch and the dispersed liquid auxiliary agent are uniformly mixed in a slow mixing tank, a double-screw extruder is adopted to extrude the mixed material, and a film with the thickness of 0.2mm is prepared by tape casting. Wherein the VA content in the EVA resin is 33%.
example 10
Mixing and extruding 8 molar parts of EVA resin, 1 molar part of phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide, 0.1 molar part of 2 tetra (3, 5-di-tert-butyl-4-hydroxy) benzenepropanoic acid pentaerythritol ester and 0.5 molar part of polysuccinic acid (4 hydroxy-2, 2,6, 6-tetramethyl-1 piperidine ethanol ester) to prepare the additive master batch. 0.001 molar weight part of catalyst is dispersed in 2 molar weight parts of hyperbranched silicon-containing acrylate monomer and 0.5 molar weight part of vinyltris (beta-methoxyethoxy) silane to form the liquid assistant. Then, 72 molar parts by weight of EVA resin, the additive master batch and the dispersed liquid auxiliary agent are uniformly mixed in a slow mixing tank, a double-screw extruder is adopted to extrude the mixed material, and a film with the thickness of 0.1mm is prepared by tape casting.
Example 11
Mixing and extruding 8 molar parts of POE resin, 1 molar part of phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide, 3 molar parts of 2-hydroxy-2-methyl-1-phenyl acetone, 0.5 molar part of 2 tetra (3, 5-di-tert-butyl-4-hydroxy) pentaerythritol phenylpropionate and 0.1 molar part of polysuccinic acid (4-hydroxy-2, 2,6, 6-tetramethyl-1 piperidine ethanol ester) to prepare the additive master batch. 0.01 molar weight part of catalyst is dispersed in 5 molar weight parts of hyperbranched silicon-containing acrylate monomer and 1 molar weight part of vinyl tri (beta-methoxyethoxy) silane to form the liquid assistant. Then, 87 molar parts by weight of POE resin, the additive master batch and the dispersed liquid auxiliary agent are uniformly mixed in a slow mixing tank, a double-screw extruder is adopted to extrude the mixed material, and a film with the thickness of 0.5mm is prepared by tape casting.
Example 12
Mixing and extruding 8 molar parts of POE resin, 2.5 molar parts of 2-hydroxy-2-methyl-1-phenyl acetone, 0.4 molar part of 2 tetra (3, 5-di-tert-butyl-4-hydroxy) benzenepropanoic acid pentaerythritol ester and 0.3 molar part of polysuccinic acid (4 hydroxy-2, 2,6, 6-tetramethyl-1 piperidine ethanol ester) to prepare the additive master batch. 0.006 molar parts of catalyst was dispersed in 3.5 molar parts of hyperbranched silicon-containing acrylate monomer and 0.75 molar parts of vinyltris (. beta. -methoxyethoxy) silane to form a liquid adjuvant. Then, 60 parts by mol of POE resin, 20 parts by mol of EVA resin, the additive masterbatch and the dispersed liquid auxiliary agent are uniformly mixed in a slow mixing tank, the mixed material is extruded by a double-screw extruder, and a film with the thickness of 0.4mm is prepared by tape casting.
Example 13
mixing and extruding 8 molar parts of POE resin, 3.5 molar parts of 2-hydroxy-2-methyl-1-phenyl acetone, 0.2 molar part of 2 tetra (3, 5-di-tert-butyl-4-hydroxy) benzenepropanoic acid pentaerythritol ester and 0.2 molar part of polysuccinic acid (4 hydroxy-2, 2,6, 6-tetramethyl-1 piperidine ethanol ester) to prepare the additive master batch. 0.007 parts by mole of catalyst was dispersed in 2.5 parts by mole of hyperbranched silicon-containing acrylate monomer and 0.6 parts by mole of vinyltris (. beta. -methoxyethoxy) silane to form a liquid adjuvant. Then, 50 parts by mol of POE resin, 25 parts by mol of EVA resin, the additive masterbatch and the dispersed liquid auxiliary agent are uniformly mixed in a slow mixing tank, the mixed material is extruded by a double-screw extruder, and a film with the thickness of 0.2mm is prepared by tape casting.
Comparative example
100 parts by mole of an EVA resin, 3 parts by mole of phenylbis (2,4, 6-trimethylbenzoyl) phosphine oxide, 1 part by mole of vinyltris (. beta. -methoxyethoxy) silane, 3 parts by mole of trimethylolpropane triacrylate, 0.25 parts by mole of 2- [4, 6-bis (2, 4-dimethylphenyl) -1,3, 5-triazin-2-yl ] -5- (octyloxy) phenol, and 0.25 parts by mole of bis (2,2,6, 6-tetramethyl-4-piperidinyl) sebacate were mixed uniformly in a slow mixing tank, and the above mixed materials were extruded by a twin-screw extruder to prepare a film having a thickness of 0.2mm by casting. Wherein the VA content in the EVA resin is 33%.
Example 14
In this example 14, the hot melt adhesive films (cast films) obtained in examples 4 to 9 and comparative example were respectively subjected to the following performance tests:
(1) And (5) testing the bonding strength.
The sample preparation method comprises the following steps: laminating according to the mode of ultrawhite glass/hot melt adhesive film/polyethylene glycol terephthalate film, wherein half area is shielded by black adhesive tape, and vacuumizing is carried out in a laminator at the temperature of 80 ℃ to finish prepressing lamination. One sample was cured under irradiation with a UV mercury lamp. After the other sample was cured by irradiation of a UV mercury lamp, the moisture curing was continued at a temperature of 23. + -. 1 ℃ and a relative humidity of 50. + -. 5% RH.
And (3) testing conditions are as follows: the temperature is 23 +/-5 ℃, and the relative humidity is 50 +/-20% RH.
And (3) performance characterization: the test was carried out according to GB/T2790-1995 test method for 180 ℃ peel strength of adhesives for Flexible versus rigid materials.
(2) and (5) performing constant temperature and humidity test.
The sample preparation method comprises the following steps: the hot melt adhesive film is clamped by two pieces of ultra-white glass with black frames, the laminating machine with 80 ℃ is vacuumized to complete prepressing and laminating, and UV curing and moisture curing are carried out firstly.
And (3) testing conditions are as follows: the temperature is 85 ℃, the humidity is 85 percent, and the time is 500 h.
And (3) performance characterization: the yellowing index (Delta YI) is tested according to GB 2409-80 national standard 'test method for yellow index of plastics'.
(3) And (4) performing a cold and hot impact test.
The sample preparation method comprises the following steps: laminating according to the mode of a glass cover plate/a hot melt adhesive film/a sensor, vacuumizing a laminating machine at the temperature of 80 ℃ to finish prepressing and laminating, and performing UV curing and then moisture curing.
And (3) testing conditions are as follows: 30min/90 ℃ at-40 ℃ and 30min X200 cycles.
and (3) performance characterization: the appearance was observed.
(4) Ultraviolet aging yellowing test.
The sample preparation method comprises the following steps: laminating according to the mode of a glass cover plate/a hot melt adhesive film/a sensor, vacuumizing a laminating machine at the temperature of 80 ℃ to finish prepressing and laminating, and performing UV curing and then moisture curing.
And (3) testing conditions are as follows: UVA-340nm, UVB-313nm, 60 +/-5 ℃ and 15kwh/m2。
And (3) performance characterization: the yellowing index (Delta YI) is tested according to GB 2409-80 national standard 'test method for yellow index of plastics'.
the test results are shown in table 1: from the test results of examples 4 to 9 and comparative example, it can be seen that the UV moisture dual-curable hot melt adhesive film prepared according to the present invention can be adjusted in curing energy and moisture curing time, can be cured by moisture in the shaded shadow portion, and is excellent in adhesive strength, resistance to wet and heat aging, resistance to thermal shock, and resistance to ultraviolet aging.
TABLE 1 Performance test and comparison results of Hot melt adhesive films
In conclusion, the UV moisture dual-curing hot melt adhesive film and the preparation method and application thereof provided by the invention have the advantages that the hyper-branched silicon-containing acrylate monomer is used as a raw material, and the hot melt adhesive film suitable for UV and/or moisture dual curing is prepared by combining with other components such as resin and the like, so that the adhesive film can be continuously cured by moisture and heat without UV light irradiation, the peeling strength of the black edge part of the touch screen is improved, effective protection can be provided for the touch screen in the field with the black edge, the adhesive film is completely cured in the shielded shadow part, and the packaging problem of the touch screen is solved; the resin is EVA (ethylene vinyl acetate) elastomer resin or POE (polyolefin elastomer) elastomer resin, so that the prepared adhesive film still belongs to hot melt adhesive, the packaging process is simple and convenient, reworking can be realized, and the yield of large-size touch screen packaging is ensured; by adjusting the content of the hyperbranched silicon-containing acrylate monomer and the catalyst, the UV and moisture curing rate can be improved to meet the packaging requirements of different types of touch screens, the defect that the shadow part or the bottom part of the hot melt adhesive film touch screen cannot be cured is avoided, the problem of weak corner peeling strength in the black edge field is solved, the packaging requirements of various types of touch screens can be met, and the packaging requirements of the touch screens with the ultra-large sizes are particularly suitable for. Therefore, the UV and moisture dual-curing hot melt adhesive film can be cured by UV and/or moisture, and has excellent performances in the aspects of bonding strength, resistance to damp-heat aging, cold and hot shock, ultraviolet aging and the like.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (14)
1. The UV moisture dual-curing hot melt adhesive film is characterized by comprising the following raw materials in parts by weight:
Resin: 80-95 parts;
photoinitiator (2): 1-4 parts;
Hyperbranched silicon-containing acrylate monomer: 2-5 parts;
Silane coupling agent: 0.5-1 part;
catalyst: 0.001-0.01 portion;
Antioxidant: 0.1-0.5 part; and
Light stabilizer: 0.1 to 0.5 portion.
2. The hot melt adhesive film according to claim 1,
The structural formula of the hyperbranched silicon-containing acrylate monomer is as follows:
Wherein
R1Is CH2-CH2-Si(OMe)3，R2is H or CH3。
3. The hot melt adhesive film according to claim 1,
the resin comprises at least one of EVA resin and POE resin; wherein
The content of VA in the EVA resin is 20-30%, and the melt index is 15-30g/10 min; and
The content of octene in the POE resin is 20-40%, and the melt index is 15-30g/10 min.
4. The hot melt adhesive film according to claim 1,
the photoinitiator comprises 2-hydroxy-2-methyl-1-phenyl acetone, 1-hydroxy-cyclohexyl phenyl ketone, 1' - (methylene di-4, 1-phenylene) bis [ 2-hydroxy-2-methyl-1-acetone, 2-benzyl-2-dimethylamino-1- (4-morpholine phenyl) butanone, 2-methyl-1- (4-methylthiophenyl) -2-morpholinyl-1-acetone, (2,4, 6-trimethylbenzoyl) diphenyl phosphine oxide, phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide and one or more of 2, 2-dimethoxy-2-phenyl acetophenone.
5. The hot melt adhesive film according to claim 1,
The silane coupling agent comprises one or more of vinyl trimethoxy silane, vinyl triacetoxy silane and vinyl tri (beta-methoxyethoxy) silane.
6. The hot melt adhesive film according to claim 1,
The catalyst comprises one or more of cobalt naphthenate, cobalt stearate and stannous oxalate.
7. The hot melt adhesive film according to claim 1,
The antioxidant comprises one or more of 2- [4, 6-bis (2, 4-dimethylphenyl) -1,3, 5-triazine-2-yl ] -5- (octyloxy) phenol, pentaerythritol tetrakis (3, 5-di-tert-butyl-4-hydroxy) phenylpropionate and n-octadecyl 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate.
8. The hot melt adhesive film according to claim 1,
The light stabilizer comprises one or more of bis (1-octyloxy-2, 2,6, 6-tetramethyl-4-piperidyl) sebacate, bis (2,2,6, 6-tetramethyl-4-piperidyl) sebacate and polysuccinic acid (4-hydroxy-2, 2,6, 6-tetramethyl-1-piperidyl ethanol ester).
9. A preparation method of a hot melt adhesive film is characterized by comprising the following steps:
Preparing additive masterbatch;
Preparing a liquid auxiliary agent;
Adding resin and the additive master batch into a liquid auxiliary agent, and uniformly mixing by a mixer;
Extruding through a material extruder; and
Preparing the UV moisture dual-curing hot melt adhesive film through a casting die head.
10. The production method according to claim 9,
Mixing an antioxidant, a light stabilizer, a photoinitiator and resin, and extruding the mixture through a co-rotating meshed double-screw extruder to obtain additive masterbatch; wherein
The rotating speed of the twin-screw of the co-rotating meshed twin-screw extruder is 40r/min-60r/min, and the temperature of each section is 100 ℃, 120 ℃, 130 ℃, 140 ℃ and 140 ℃ in sequence.
11. the production method according to claim 9,
And adding a catalyst into the mixture of the hyperbranched silicon-containing acrylate monomer and the silane coupling agent, and uniformly dispersing to form the liquid auxiliary agent.
12. The production method according to claim 9,
The mixer is a vertical double-ribbon mixer, the driving power of the mixer is 3KW-120KW, the mixing temperature is 35-45 ℃, and the mixing time is 2-5 hours.
13. The production method according to claim 9,
the material extruder is a single-screw extruder, the diameter of a screw is 130mm, the rotating speed of the screw is 30-60r/min, and the temperatures of all sections are 75 ℃, 80 ℃, 84 ℃, 85 ℃ and 85 ℃ in sequence.
14. an application of a UV moisture dual-curing hot melt adhesive film in packaging a touch screen.
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| CN113528064A (en) * | 2021-07-09 | 2021-10-22 | 江苏惠沣环保科技有限公司 | Hot melt adhesive film for bonding proton exchange membrane of hydrogen energy battery |
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