CN104327757B - A kind of near infrared ray barrier film and preparation method - Google Patents
A kind of near infrared ray barrier film and preparation method Download PDFInfo
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- CN104327757B CN104327757B CN201410492148.1A CN201410492148A CN104327757B CN 104327757 B CN104327757 B CN 104327757B CN 201410492148 A CN201410492148 A CN 201410492148A CN 104327757 B CN104327757 B CN 104327757B
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Abstract
The invention belongs to optical functional materials technical field.Use and there is the polyacrylate pressure-sensitive containing acrylic acid alkoxy ester of excellent compatibility as film forming system, special process ripening with Diimmonium salt dyestuff.The near infrared ray barrier film that the present invention relates to, for single layer structure, it is made up of base material, viscosity glued membrane and isolating membrane, viscosity film thickness is between 5～50 μm, the quality composition of viscosity glued membrane coating fluid at least includes: the acrylate pressure-sensitive adhesive 100 parts containing acrylic acid alkoxy ester 9%～50%, Diimmonium salt 0.5 10 parts；0.1 10 parts of firming agent.Its preparation method also includes maturing process, and cooking conditions is 40 70 DEG C, 30 60%RH, 24 168 hours.This infrared ray barrier film light transmission effect and good stability, preparation technology is simple, it is easy to operates and controls, and production efficiency and yields are high.It is applicable near infrared ray is had the fields such as the electronics of shielding requirements, optical instrument.
Description
Technical field
The invention belongs to optical functional materials technical field, relate to near-infrared interrupter technique, hinder particularly near infrared ray
Disconnected material, relates to its preparation method simultaneously.
Background technology
Near infrared ray barrier film is the core component of flat faced display, is mainly used in shielding, absorbs flat faced display
The near infrared ray (wave-length coverage 800 ~ 1100 nm) discharged, thus avoid household electrical appliance near-infrared remote control or infrared communication
The fault of port.Near infrared ray barrier film is broadly divided into single layer structure and double-decker according to the structure of functional layer at present.
The near infrared ray barrier film of single layer structure refers to that nearly IR absorbing dye is combined in polyacrylate pressure-sensitive
In the middle of itself, pressure sensitive adhesive had both played the effect of dye carrier, played again the effect of bonding, and its advantage is to shorten production week
Phase, the manufacture efficiency of barrier film can be improved.The major defect of the near infrared ray barrier film of single layer structure is near infrared ray
Dyestuff and pressure sensitive adhesive compatibility requirements between the two is higher.
Diimmonium salt is the near-infrared absorbing dyestuff that combination property is best, has that absorbing wavelength scope is wide, absorbability
By force, visible light transmissivity advantages of higher, but owing to Diimmonium salt dyestuff is very poor with the conventional acrylic ester pressure-sensitive adhesive compatibility,
Directly attach after can not mixing film, be difficult to be prepared as the near infrared ray barrier film of single layer structure the most at present.
The near infrared ray barrier film that CN 1910723A introduces is double-decker, uses SAN resin (styrene and acrylonitrile
Copolymer) be mixed with film material with Diimmonium salt dyestuff, then bond on display pannel with acrylate pressure-sensitive adhesive layer, its
There is good ruggedness, heat stability and the high-transmittance in visible-range, and can make in the preparation of this film
With Conventional solvents, decrease environmental pollution.
CN 102736155A is by various dope dyes (0.4415 ~ 0.8830 part), neon yellow light absorbing dye (0.02 ~ 0.05
Part) and Diimmonium salt dyestuff (0.2 ~ 0.5 part) and acrylic resin (16 ~ 35 parts), solvent (45 ~ 74 parts), auxiliary agent (0.2 ~ 2
Part) it is prepared as the barrier film of plasma display after mix homogeneously, there is preferable humidity resistance, heat-resisting quantity and light stability
Can, high in visible light wave range transmitance, maximum up to 67%, but acrylic resin no adhesion used by this barrier film, only as
Double-decker barrier film uses.
The near infrared ray barrier film with diimmonium salt-dye as absorbent that above-mentioned document is introduced, the defect of its maximum is just
Be resin used by the functional layer no matter carrying dyestuff be SAN resin or acrylic resin, itself all there is no cementitiousness,
Must be coated one layer of pressure sensitive adhesive in actual applications, add technological process, production efficiency is low, affects yield rate.
Summary of the invention
It is an object of the invention to provide a kind of Diimmonium salt single layer structure near infrared ray barrier film, this blocking-up is provided simultaneously
The preparation method of film, improves production efficiency and yields.
The object of the present invention is achieved like this, use with Diimmonium salt dyestuff have excellent compatibility containing alkyl acrylate
The polyacrylate pressure-sensitive adhesive of epoxide ester and Diimmonium salt dyestuff mixed system, use conventional coating process to prepare glued membrane,
The near-infrared barrier film of the single layer structure that the present invention relates to is obtained after ripening.
The near infrared ray barrier film that the present invention relates to, for single layer structure, is made up of base material, viscosity glued membrane and isolating membrane, viscous
Property film thickness between 5 ~ 50 μm, the quality of viscosity glued membrane coating fluid composition at least includes:
Acrylate pressure-sensitive adhesive 100 parts
Diimmonium salt 0.5-10 part
Firming agent 0.1-10 part
Wherein；Described acrylate pressure-sensitive adhesive contains acrylic acid alkoxy ester 9%～50%；
Firming agent is toluene di-isocyanate(TDI), hexamethylene diisocyanate, N, the m-benzene of N, N ', N '-four glycidyl group two
Methylamine, N, the one in N, N ', N '-four glycidyl group ethylenediamine；
Diimmonium salt is hexafluorophosphoric acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-and to phenylene two
Imonium, hexafluoro-antimonic acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-to phenylene diimmonium or double (trifluoro
Methane sulfonyl) imidic acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-in phenylene diimmonium
Kind or the most several mixed systems.
The near infrared ray barrier film that the present invention relates to, for single layer structure, is made up of base material, viscosity glued membrane and isolating membrane, viscous
Property film thickness is between 10 ~ 30 μm.
The near infrared ray barrier film that the present invention relates to, for single layer structure, is made up of base material, viscosity glued membrane and isolating membrane, viscous
Property film thickness is between 5 ~ 20 μm.
The near infrared ray barrier film that the present invention relates to, described acrylate pressure-sensitive adhesive containing acrylic acid alkoxy ester 25%～
45%。
The near infrared ray barrier film that the present invention relates to, the quality composition of described viscosity glued membrane coating fluid at least includes:
Containing alkyl acrylate epoxide ester pressure-sensitive adhesive 100 parts
Diimmonium salt 1-4 part
Firming agent 1-5 part.
The near infrared ray barrier film that the present invention relates to, the quality composition of described viscosity glued membrane coating fluid at least includes:
Containing alkyl acrylate epoxide ester pressure-sensitive adhesive 100 parts
Diimmonium salt dyestuff 3-6 part
Firming agent 4-10 part.
The near infrared ray barrier film preparation method that the present invention relates to, release including coating fluid preparation, coating film forming and attaching
Membrane process and maturing process, cooking conditions is 40-70 DEG C, 30-60%RH, 24-168 hour.
The near infrared ray barrier film preparation method that the present invention relates to, release including coating fluid preparation, coating film forming and attaching
Film and maturing process, described coating fluid uses solwution method preparation, and Diimmonium salt concentration is between 0.5-5%.
The near infrared ray barrier film preparation method that the present invention relates to, release including coating fluid preparation, coating film forming and attaching
Membrane process and maturing process, described coating fluid preparation solvent is in ethyl acetate, butyl acetate, butanone, dimethylbenzene
Kind or the most several mixed systems.
The near infrared ray barrier film that the present invention relates to, it is seen that light district light transmission is good, and near infrared region light transmittance is low, spectrum is overall
Barrier effect good stability, meets pressure sensitive adhesive for adhesion strength and the composite request of cohesive strength, it is adaptable to the reddest simultaneously
Outside line has fields such as blocking the electronics of requirement, optical instrument, is particularly useful for making the key of plasma display display module
Assembly.
The preparation method of the near infrared ray barrier film that the present invention relates to, technique is simple, it is easy to operates and controls, production efficiency
High with yields, it is adaptable to prepared by the batch of single layer structure near infrared ray barrier film.
Detailed description of the invention
Below by embodiment, the technical scheme that the present invention relates to is described further, but protects not as to the present invention
Protect the restriction of scope.In addition to special instruction, material therefor proportioning is all in terms of mass parts.
Embodiment one
(1) adhesive synthesis: be passed through N2In the case of, by 200 parts of n-butyl acrylates, 100 parts of ethioxy
Ethyl ester, 200 parts of cyclohexyl acrylates, 1 part of (the 0.2% of monomer total amount) dibenzoyl peroxide and 300 parts of ethyl acetate mixing,
In disposable addition reaction flask.Start stirring and heating in water bath is warming up to 75 DEG C, back flow reaction 2h.Under constantly backflow at the uniform velocity
Dropping accounts for 0.5 part of (the 0.1% of monomer total amount) dibenzoyl peroxide and the initiator solution of 150 parts of ethyl acetate compositions, continues
Back flow reaction 4h.Under constantly backflow, at the uniform velocity dropping accounts for the dibenzoyl peroxide of monomer total amount 0.1% and 150 parts of acetic acid second again
The initiator solution of ester composition, liter high-temperature, to 80 DEG C, is further continued for back flow reaction 4h.The lower cooling reactant liquor of stirring goes out to room temperature
It is the polyacrylate pressure-sensitive adhesive of 20% that material obtains alkyl acrylate epoxide ester content.
(2) preparation coating fluid: by 0.5 part of hexafluorophosphoric acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-
Phenylene diimmonium is dissolved in 99.5 parts of ethyl acetate, obtains the dye solution that concentration is 0.5%；
By the polyacrylate pressure-sensitive adhesive and 2 that alkyl acrylate epoxide ester content is 20% of the 100 above-mentioned synthesis of solid part
Part toluene di-isocyanate(TDI) mix homogeneously, the dye solution mix homogeneously adding 100 part 0.5% obtains coating fluid；
(3) coating: technique coating machine spins in Japan of PET(Japan routinely, A4100,100 μm) it is coated with on base material
Cloth, controls film thickness 20 μm, dry out solvent under the conditions of 80 DEG C；
(4) mould release membrance is attached: viscosity film surface after the drying attaches mould release membrance, obtains barrier film semi-finished product；
(5) ripening: by barrier film semi-finished product temperature 52 DEG C, humidity 33%RH environment in ripening 102 h, obtain this
The bright near infrared ray barrier film with single layer structure related to.
This barrier film visible light wave range (380 ~ 780 nm) transmitance is 79%, and near infrared band 850 nm transmitance is
9.7%, 950 nm transmitances are 8.9%, and transmitted spectrum rate of change 0.8% after 3 months, peel strength 4.5N/25mm(is relative to light
Learn glass, 180 ° of strippings), more not cull when peeling off.
Embodiment two
During adhesive synthesis, acrylic acid alkoxy ester accounts for whole content of monomer and becomes 9%, alkyl acrylate and acrylic acid ring
Arrcostab usage ratio is 2:1, and remaining synthesis step is with embodiment one.
Dyestuff selection 1 part of hexafluoro-antimonic acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-to phenylene two
Imonium, solvent selects butyl acetate and dimethylbenzene press 2:1 and compounds, dyes concentration 1%, firming agent selection 0.1 part 1,6-oneself two
Isocyanates, viscosity film thickness is 30 μm, and cooking conditions elects temperature 43 DEG C, humidity 51%RH, ripening 87 h, preparation method as
With embodiment one.
This barrier film visible light wave range (380 ~ 780 nm) transmitance is 75%, and near infrared band 850 nm transmitance is
8.8%, 950 nm transmitances are 8.1%, and transmitted spectrum rate of change 0.5% after 5 months, peel strength 6.2N/25mm(is relative to light
Learn glass, 180 ° of strippings), more not cull when peeling off.
Embodiment three
During adhesive synthesis, acrylic acid alkoxy ester accounts for whole content of monomer and becomes 25%, alkyl acrylate and acrylic acid
Cycloalkyl ester usage ratio is 1:1, and remaining synthesis step is with embodiment one.
Dyestuff selection 3 parts of hexafluoro-antimonic acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-to phenylene two
Imonium, solvent selects butanone, dyes concentration 3%, firming agent 4 parts of N of selection, the m-second of N, N ', N '-four glycidyl group two
Amine, viscosity film thickness is 15 μm, and cooking conditions elects temperature 47 DEG C, humidity 42%RH, ripening 168 h as, and preparation method is with real
Execute example one.
This barrier film visible light wave range (380 ~ 780 nm) transmitance is 68%, and near infrared band 850 nm transmitance is
3.3%, 950 nm transmitances are 2.1%, and transmitted spectrum rate of change 0.5% after 1 year, peel strength 3.5N/25mm(is relative to optics
Glass, 180 ° of strippings), more not cull when peeling off.
Embodiment four
During adhesive synthesis, acrylic acid alkoxy ester accounts for whole content of monomer and becomes 40%, alkyl acrylate and acrylic acid
Cycloalkyl ester usage ratio is 2:1, and remaining synthesis step is with embodiment one.
Dyestuff selection 2.5 parts of hexafluoro-antimonic acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-to phenylene
Diimmonium and 2.5 parts double (trifluoromethane sulfonyl group) imidic acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-
To phenylene diimmonium, solvent selects dimethylbenzene, dyes concentration 5%, and firming agent selects 3 parts of N, N, N ', N '-four to shrink sweet
Oil base m-xylylenediamine, PET base material selects SKC company's T H-46T(100 μm), viscosity film thickness is 10 μm, and cooking conditions selects
For temperature 55 DEG C, humidity 60%RH, ripening 48 h, preparation method is with embodiment one.
This barrier film visible light wave range (380 ~ 780 nm) transmitance is 62%, and near infrared band 850 nm transmitance is
3.0%, 950 nm transmitances are 1.6%, and transmitted spectrum rate of change 0.6% after 5 months, peel strength 4.5N/25mm(is relative to light
Learn glass, 180 ° of strippings), more not cull when peeling off.
Embodiment five
During adhesive synthesis, acrylic acid alkoxy ester accounts for whole content of monomer and becomes 35%, alkyl acrylate and acrylic acid
Cycloalkyl ester usage ratio is 1:1, and remaining synthesis step is with embodiment one.
Dyestuff selection 6 parts of hexafluorophosphoric acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-to phenylene two
Imonium, solvent selects ethyl acetate and butanone press 1:1 and compounds, dyes concentration 3%, firming agent selection 5 part 1, and oneself is two different for 6-
Cyanate, viscosity film thickness is 12 μm, and cooking conditions elects temperature 40 DEG C, humidity 56%RH, ripening 144 h as, and preparation method is same
Embodiment one.
This barrier film visible light wave range (380 ~ 780 nm) transmitance is 69%, and near infrared band 850 nm transmitance is
5.2%, 950 nm transmitances are 4.0%, and transmitted spectrum rate of change 0.8% after 6 months, peel strength 4.2N/25mm(is relative to light
Learn glass, 180 ° of strippings), more not cull when peeling off.
Embodiment six
During adhesive synthesis, acrylic acid alkoxy ester accounts for whole content of monomer and becomes 50%, alkyl acrylate and acrylic acid
Cycloalkyl ester usage ratio is 3:1, and remaining synthesis step is with embodiment one.
4 parts of (trifluoromethane sulfonyl group) imidic acid-N selected by dyestuff, and N, N ', N '-four is [to two (cyclohexyl methyl) aminobenzene
Base]-to phenylene diimmonium and 6 parts of hexafluoro-antimonic acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-to sub-benzene
Base diimmonium, solvent selects butanone, dyes concentration 5%, firming agent 1.5 parts of toluene di-isocyanate(TDI)s of selection, viscosity glued membrane
Thickness is 5 μm, and cooking conditions elects temperature 66 DEG C, humidity 30%RH as, and ripening 24 h, preparation method is with embodiment one.
This barrier film visible light wave range (380 ~ 780 nm) transmitance is 61%, and near infrared band 850 nm transmitance is
2.2%, 950 nm transmitances are 1.5%, and transmitted spectrum rate of change 0.3% after 1 year, peel strength 5.5N/25mm(is relative to optics
Glass, 180 ° of strippings), more not cull when peeling off.
Embodiment seven
During adhesive synthesis, acrylic acid alkoxy ester accounts for whole content of monomer and becomes 45%, alkyl acrylate and acrylic acid
Cycloalkyl ester usage ratio is 2:1, and remaining synthesis step is with embodiment one.
4 parts of double (trifluoromethane sulfonyl group) imidic acid-N selected by dyestuff, and N, N ', N '-four is [to two (cyclohexyl methyl) amino
Phenyl]-to phenylene diimmonium, solvent selects dimethylbenzene, dyes concentration 4%, and firming agent selects 1 part of N, N, N ', N '-four
The m-ethylenediamine of glycidyl, PET base material selects Japan to spin company's A-4300(100 μm) viscosity film thickness is 40 μm, ripening
Condition elects temperature 70 C, humidity 46%RH as, and ripening 55 h, preparation method is with embodiment one.
This barrier film visible light wave range (380 ~ 780 nm) transmitance is 63%, and near infrared band 850 nm transmitance is
3.2%, 950 nm transmitances are 2.5%, and transmitted spectrum rate of change 0.6% after 9 months, peel strength 3.7N/25mm(is relative to light
Learn glass, 180 ° of strippings), more not cull when peeling off.
Embodiment eight
During adhesive synthesis, acrylic acid alkoxy ester accounts for whole content of monomer and becomes 10%, alkyl acrylate and acrylic acid
Cycloalkyl ester usage ratio is 1:2, and remaining synthesis step is with embodiment one.
Dyestuff selection 2 parts of hexafluoro-antimonic acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-to phenylene two
Imonium, solvent selects butanone, dyes concentration 2%, firming agent 10 parts of N of selection, the m-benzene of N, N ', N '-four glycidyl group
Dimethylamine, viscosity film thickness is 50 μm, and cooking conditions elects temperature 62 DEG C, humidity 37%RH, ripening 67 h as, and preparation method is same
Embodiment one.
This barrier film visible light wave range (380 ~ 780 nm) transmitance is 65%, and near infrared band 850 nm transmitance is
8.2%, 950 nm transmitances are 6.9%, and transmitted spectrum rate of change 0.7% after 6 months, peel strength 5.1N/25mm(is relative to light
Learn glass, 180 ° of strippings), more not cull when peeling off.
Claims (9)
1. a near infrared ray barrier film, for single layer structure, is made up of base material, viscosity glued membrane and isolating membrane, viscosity film thickness
Between 5～50 μm, the quality composition of viscosity glued membrane coating fluid at least includes:
Acrylate pressure-sensitive adhesive 100 parts
Diimmonium salt 0.5-10 part
Firming agent 0.1-10 part
Wherein；Described acrylate pressure-sensitive adhesive contains acrylic acid alkoxy ester 9%～50%；
Firming agent is toluene di-isocyanate(TDI), hexamethylene diisocyanate, N, N, N ', N '-four glycidyl group m-benzene diformazan
Amine, N, the one in N, N ', N '-four glycidyl group ethylenediamine；
Diimmonium salt is hexafluorophosphoric acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-to phenylene diimmonium,
Hexafluoro-antimonic acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-to phenylene diimmonium or double (fluoroform sulphur
Acyl group) imidic acid-N, N, N ', N '-four [to two (cyclohexyl methyl) aminophenyl]-to the one in phenylene diimmonium or its
In several mixed system；
Above-mentioned coating fluid is formulated, is coated with, attaches mould release membrance and maturing process formation near infrared ray barrier film, and cooking conditions is
40-70 DEG C, 30-60%RH, 24-168 hour.
Near infrared ray barrier film the most according to claim 1, described viscosity film thickness is between 10～30 μm.
Near infrared ray barrier film the most according to claim 1, described viscosity film thickness is between 5～20 μm.
Near infrared ray barrier film the most according to claim 1, described acrylate pressure-sensitive adhesive alkoxy ester in acrylic acid
25%～45%.
5. according to the near infrared ray barrier film described in Claims 1 to 4 any one, the quality of described viscosity glued membrane coating fluid
Composition at least includes:
Containing alkyl acrylate epoxide ester pressure-sensitive adhesive 100 parts
Diimmonium salt 1-4 part
Firming agent 1-5 part.
6. according to the near infrared ray barrier film described in Claims 1 to 4 any one, the quality of described viscosity glued membrane coating fluid
Composition at least includes:
Containing alkyl acrylate epoxide ester pressure-sensitive adhesive 100 parts
Diimmonium salt 3-6 part
Firming agent 4-10 part.
7., according to the near infrared ray barrier film preparation method described in Claims 1 to 4 any one, including coating fluid preparation, it is coated with
Cloth film forming and attaching mould release membrance process and maturing process, cooking conditions is 40-70 DEG C, 30-60%RH, 24-168 hour.
Near infrared ray barrier film preparation method the most according to claim 7, described coating fluid uses solwution method preparation, and two is sub-
Ammonium salt concentration is between 0.5-5%.
Near infrared ray barrier film preparation method the most according to claim 8, coating fluid preparation solvent is ethyl acetate, second
A kind of or the most several mixed system in acid butyl ester, butanone, dimethylbenzene.
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| CN111269666B (en) * | 2020-01-19 | 2021-11-19 | 成都立鑫新技术科技有限公司 | Preparation method of infrared laser protective film |
| CN111262646B (en) * | 2020-01-19 | 2021-11-19 | 成都立鑫新技术科技有限公司 | Infrared laser invasion protective film |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805566A (en) * | 2009-02-18 | 2010-08-18 | 日东电工株式会社 | Double-faced pressure-sensitive sheet adhesive and pressure-sensitive adhesive type optical element |
| CN102199406A (en) * | 2010-03-09 | 2011-09-28 | 株式会社巴川制纸所 | Bonding type optical film and adhesive composition |
| CN102778716A (en) * | 2011-05-10 | 2012-11-14 | 株式会社巴川制纸所 | Adhesive type optical film and plasma display panel |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009084400A (en) * | 2007-09-28 | 2009-04-23 | Gunze Ltd | Near-infrared absorbing pressure-sensitive adhesive composition and multilayer optical film |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805566A (en) * | 2009-02-18 | 2010-08-18 | 日东电工株式会社 | Double-faced pressure-sensitive sheet adhesive and pressure-sensitive adhesive type optical element |
| CN102199406A (en) * | 2010-03-09 | 2011-09-28 | 株式会社巴川制纸所 | Bonding type optical film and adhesive composition |
| CN102778716A (en) * | 2011-05-10 | 2012-11-14 | 株式会社巴川制纸所 | Adhesive type optical film and plasma display panel |
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