CN117801676A - Organic silicon liquid optical cement and preparation method and application thereof - Google Patents
Organic silicon liquid optical cement and preparation method and application thereof Download PDFInfo
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- CN117801676A CN117801676A CN202311857596.2A CN202311857596A CN117801676A CN 117801676 A CN117801676 A CN 117801676A CN 202311857596 A CN202311857596 A CN 202311857596A CN 117801676 A CN117801676 A CN 117801676A
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- 230000003287 optical effect Effects 0.000 title claims abstract description 155
- 239000007788 liquid Substances 0.000 title claims abstract description 139
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 71
- 239000010703 silicon Substances 0.000 title claims abstract description 71
- 239000004568 cement Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 122
- -1 polysiloxane Polymers 0.000 claims abstract description 117
- 229920002050 silicone resin Polymers 0.000 claims abstract description 91
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 90
- 239000001257 hydrogen Substances 0.000 claims abstract description 88
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 88
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 86
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 86
- 230000001070 adhesive effect Effects 0.000 claims abstract description 85
- 239000000853 adhesive Substances 0.000 claims abstract description 83
- 239000004970 Chain extender Substances 0.000 claims abstract description 54
- 239000003054 catalyst Substances 0.000 claims abstract description 40
- 239000003112 inhibitor Substances 0.000 claims abstract description 24
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 229920002545 silicone oil Polymers 0.000 claims description 12
- 238000003475 lamination Methods 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- CEBKHWWANWSNTI-UHFFFAOYSA-N 2-methylbut-3-yn-2-ol Chemical compound CC(C)(O)C#C CEBKHWWANWSNTI-UHFFFAOYSA-N 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 239000004973 liquid crystal related substance Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 3
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 claims description 2
- NECRQCBKTGZNMH-UHFFFAOYSA-N 3,5-dimethylhex-1-yn-3-ol Chemical compound CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 claims description 2
- MQSZOZMNAJHVML-UHFFFAOYSA-N 3-phenylbut-1-yn-1-ol Chemical compound OC#CC(C)C1=CC=CC=C1 MQSZOZMNAJHVML-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 238000005538 encapsulation Methods 0.000 claims description 2
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- QXLPXWSKPNOQLE-UHFFFAOYSA-N methylpentynol Chemical compound CCC(C)(O)C#C QXLPXWSKPNOQLE-UHFFFAOYSA-N 0.000 claims description 2
- 238000002834 transmittance Methods 0.000 abstract description 33
- 230000032683 aging Effects 0.000 abstract description 25
- 238000004383 yellowing Methods 0.000 abstract description 14
- 230000000052 comparative effect Effects 0.000 description 23
- 239000002313 adhesive film Substances 0.000 description 13
- 230000006835 compression Effects 0.000 description 12
- 238000007906 compression Methods 0.000 description 12
- 239000011521 glass Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 238000004132 cross linking Methods 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 5
- 230000002159 abnormal effect Effects 0.000 description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 4
- 230000003247 decreasing effect Effects 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000003522 acrylic cement Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 239000013008 thixotropic agent Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/08—Printing inks based on natural resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides an organosilicon liquid optical cement, a preparation method and application thereof. The organic silicon liquid optical adhesive comprises the following components in parts by weight: 100 parts of vinyl polysiloxane, 0.5-10 parts of hydrogen polysiloxane, 1-30 parts of silicone resin, 0.5-5 parts of chain extender, 0.01-0.4 part of catalyst and 0.01-0.5 part of inhibitor. The organic silicon liquid optical adhesive provided by the technical scheme has the characteristics of high light transmittance, good transparency, good adhesive property, good wet heat aging resistance, good yellowing resistance and good weather resistance.
Description
Technical Field
The invention belongs to the technical field of optical cement, and particularly relates to an organic silicon liquid optical cement, and a preparation method and application thereof.
Background
Liquid optical adhesives (LOCA) are special adhesives (such as touch screens and liquid crystal displays) used for bonding transparent optical elements. With the rapid development of electronic information industry, communication technology and automobile industry, electronic touch screens are increasingly used in various aspects of people's production and life. The touch screen is sequentially provided with a protection panel, a touch screen and a display screen from outside to inside, and the touch screen is required to be sequentially attached through optical cement. The bonding of the liquid crystal display module and the touch screen protective panel requires that the liquid optical adhesive has high light transmittance, no yellowing, small shrinkage and good weather resistance, and also requires that the liquid optical adhesive has better 180-degree peeling force.
According to the difference of the used resin main bodies, the liquid optical cement is mainly classified into polyurethane optical cement, epoxy resin optical cement, acrylic ester optical cement and organic silicon optical cement. Polyurethane optical cement has a wide bonding surface, but has obviously insufficient moisture resistance. The epoxy optical adhesive has higher bonding strength, but has the defects of poor weather resistance, poor wet heat resistance and the like. The acrylic optical cement has high curing speed, but has large dimensional shrinkage after curing, poor weather resistance, and is easy to generate yellowing phenomenon and lower light transmittance when being used for a long time under the environment exceeding 80 ℃. The addition type organosilicon optical cement has better weather resistance and humidity and heat aging resistance, and the size shrinkage rate after curing is less than 0.5 percent, and the quick curing can be realized by adjusting a curing system.
CN107286901a discloses a full-lamination frame adhesive for a touch screen and a preparation method thereof, wherein the frame adhesive comprises the following components: 20 to 40 percent of vinyl silicone oil, 1 to 15 percent of hydrogen-containing silicone oil, 1 to 3 percent of coupling agent, 30 to 50 percent of 110 raw rubber, 5 to 10 percent of thixotropic agent, 1 to 3 percent of hardness regulator, 1 to 3 percent of construction auxiliary agent, 0.001 to 0.05 percent of catalyst and 0.001 to 0.05 percent of inhibitor. The touch screen full-lamination frame adhesive provided by the technical scheme is packaged and used in a single-component mode, meets the operation requirements of automatic equipment in the lamination process, and is not ideal in visible light transmittance.
CN109517574a discloses an ultraviolet light curing organic silicon liquid optical adhesive composition, a preparation method and application thereof, wherein the ultraviolet light curing organic silicon liquid optical adhesive composition comprises the following components: 30-80 parts of vinyl silicone oil containing terminal mercapto, 10-50 parts of copolymer of thioalkanol group and alkyl and/or aryl siloxane, 1-60 parts of vinyl silicone oil, 0.01-1 part of photoinitiator, 0.01-1 part of tackifier and 0.01-0.1 part of flame retardant. The ultraviolet light curing organic silicon liquid optical cement composition provided by the technical scheme can form good lamination with a glass cover plate and an LCD screen, can be used for full lamination of a touch screen, and has the advantages of high temperature resistance, high humidity resistance, cold and hot impact resistance and the like. However, the cohesive strength of the optical adhesive is low, and bubbles are generated at low pressure, reducing visual effect.
In addition, the organosilicon optical cement in the prior art still has the phenomenon of generating certain yellowing when working under high temperature, high humidity or direct sunlight, and the cohesiveness still needs to be further improved.
Therefore, it is necessary to develop an organosilicon liquid optical cement with high light transmittance, good transparency, good adhesion, good resistance to wet heat aging, good weather resistance and good yellowing resistance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an organic silicon liquid optical cement and a preparation method and application thereof. The organic silicon liquid optical adhesive has the characteristics of high light transmittance, good transparency, good adhesion performance, good resistance to humidity and heat aging, good yellowing resistance and good weather resistance.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides an organosilicon liquid optical cement, which comprises the following components in parts by weight: 100 parts of vinyl polysiloxane, 0.5-10 parts of hydrogen polysiloxane (e.g., 0.8 parts, 1 parts, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts or 9 parts, etc.), 1-30 parts of silicone (e.g., 2 parts, 5 parts, 8 parts, 11 parts, 14 parts, 17 parts, 20 parts, 23 parts, 26 parts or 29 parts, etc.), 0.5-5 parts of chain extender (e.g., 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts or 4.5 parts, etc.), 0.01-0.4 parts of catalyst (e.g., 0.05 parts, 0.1 parts, 0.15 parts, 0.2 parts, 0.25 parts, 0.3 parts or 0.35 parts, etc.), and 0.01-0.5 parts of inhibitor (e.g., 0.05 parts, 0.1 parts, 0.15 parts, 0.2 parts, 0.25 parts, 0.3 parts, 0.35 parts, 0.4 or 0.45, etc.).
In the invention, the vinyl polysiloxane has lower volatile components, and can enable the organic silicon liquid optical adhesive to have softness, brightness and weather resistance; the hydrogen-containing polysiloxane can be crosslinked with vinyl polysiloxane, so that the mechanical property of the organic silicon liquid optical adhesive is improved; the chain extender can prolong the molecular chain of vinyl polysiloxane, improve the breaking elongation of the organic silicon liquid optical adhesive, increase the toughness, and also has the functions of reducing the hardness of the organic silicon liquid optical adhesive and improving the weather resistance; the silicone resin can improve the viscosity of the organic silicon liquid optical adhesive and improve the bonding strength. The invention improves the yellowing problem of the organic silicon liquid optical adhesive by reducing the dosage of the catalyst, the collocation of the vinyl polysiloxane, the silicone resin, the hydrogen-containing polysiloxane and the chain extender effectively improves the bonding performance between the organic silicon liquid optical adhesive and glass, has good adhesive force on a display substrate, and the organic silicon liquid optical adhesive has better weather resistance, wet heat aging resistance, high transmittance, good transparency, no yellowing, layering, degradation, detachment with the adhered surface, bubble and other problems during long-time use, and has certain reworkability.
According to the invention, the prepared organic silicon liquid optical adhesive has good performance by controlling the weight parts of the components in the organic silicon liquid optical adhesive within a specific range. The weight part of the hydrogen-containing polysiloxane is 0.5-10 parts, and if the weight part of the hydrogen-containing polysiloxane is too small, the crosslinking degree of the organic silicon liquid optical adhesive for curing is insufficient, so that the compression strength and the viscosity are low; if the weight portion of the hydrogen-containing polysiloxane is too large, the hardness of the cured organosilicon liquid optical cement is high, the compression strength is high and the viscosity is low. The weight part of the silicone resin is 1-30 parts, and if the weight part of the silicone resin is too large, the hardness of the organic silicon liquid optical adhesive is obviously reduced, so that the compression strength is reduced; if the weight fraction of the silicone resin is too small, the silicone liquid optical adhesive has a low viscosity and a high hardness, and thus the shear strength is reduced, but the compression strength is increased. The weight part of the catalyst is 0.01-0.4 part, if the weight part of the catalyst is too small, the reaction activity of the organic silicon liquid optical adhesive is low, the crosslinking degree of curing is too low, and the organic silicon liquid optical adhesive is too soft after curing and even does not react for curing; if the weight part of the catalyst is too large, the organosilicon liquid optical cement can be obviously hardened and become brittle after being solidified, and the viscosity is lacking. The weight part of the chain extender is 0.5-5 parts, if the weight part of the chain extender is too large, the organic silicon liquid optical adhesive is softer after solidification, and the compression strength is reduced; if the weight part of the chain extender is too small, the toughness of the cured organosilicon liquid optical cement is reduced, the material is harder, and the compression strength is higher.
Preferably, the vinyl polysiloxane comprises a linear or branched polysiloxane having vinyl groups at the chain ends and/or side chains, and illustratively, the vinyl polysiloxane comprises any one or a combination of at least two of a silicone oil having vinyl groups at the chain ends, or a silicone oil having vinyl groups at the chain ends and side chains.
Preferably, the vinyl polysiloxane further comprises at least one of the following features:
the vinyl polysiloxane comprises 0.1% -5% by mass of vinyl groups, such as 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4% or 4.5% by mass, etc.
The vinyl siloxane has a viscosity of 200-20000 mPas at 25 ℃, for example 500 mPas, 1000 mPas, 5000 mPas, 10000 mPas, 13000 mPas, 15000 mPas or 18000 mPas, etc.
The vinyl siloxane has a refractive index of 1.39-1.41, such as 1.392, 1.394, 1.396, 1.398, 1.400, 1.402, 1.404, 1.406, 1.408, etc.
Preferably, the hydrogen-containing polysiloxane contains three or more hydrogen atoms bonded to silicon atoms in the molecular chain.
In the present invention, the molecular chain of the hydrogen-containing polysiloxane contains more than three hydrogen atoms bonded with silicon atoms, and the positions of the hydrogen atoms are not limited and can be located at the chain end and/or the side chain of the molecular chain. Illustratively, the hydrogen-containing polysiloxane includes hydrogen-containing silicone oil having a hydrogen atom located in a side chain of a molecular chain and/or hydrogen-containing silicone oil having a hydrogen atom located in a chain end of a molecular chain and a side chain. The viscosity of the hydrogen-containing polysiloxane is not particularly limited, and the viscosity of the hydrogen-containing polysiloxane is preferably 20 to 100 mPas, for example, 30 mPas, 40 mPas, 50 mPas, 60 mPas, 70 mPas, 80 mPas, 90 mPas, or the like.
Preferably, the hydrogen atom content of the hydrogen-containing polysiloxane is 0.01% to 0.8% (e.g., 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, or 0.7%, etc.), and more preferably 0.02% to 0.3%.
In the invention, the mass percentage of hydrogen atoms in the hydrogen-containing polysiloxane is 0.01-0.8%, and if the mass percentage of hydrogen atoms is too large, the hardness of the cured material of the organosilicon liquid optical cement is large, and the viscosity is poor; if the mass percentage of the hydrogen atoms is too small, the material of the cured organosilicon liquid optical cement is softer, and the compression strength is poor.
Preferably, the hydrogen-containing polysiloxane comprises hydrogen-containing silicone oil.
Preferably, the silicone resin comprises vinyl silicone resin and/or hydrogen-containing silicone resin.
Preferably, the vinyl silicone resin comprises any one or a combination of at least two of vinyl MQ silicone resin, vinyl MT silicone resin, vinyl MDT silicone resin or vinyl MTQ silicone resin, and further preferably vinyl MQ silicone resin and/or vinyl MDT silicone resin. In the present invention, the "MQ silicone resin" means a silicone resin composed of monofunctional siloxane units and tetrafunctional siloxane units; the term "MT silicone resin" means a silicone resin composed of monofunctional siloxane units and trifunctional siloxane units; the "MDT silicone" means a silicone resin composed of monofunctional siloxane units, difunctional siloxane units, and trifunctional siloxane units; the "MTQ silicone resin" means a silicone resin composed of monofunctional siloxane units, trifunctional siloxane units, and tetrafunctional siloxane units. The following description refers to the same descriptions, all with the same meaning.
Preferably, the viscosity of the vinyl MQ silicone resin is 1000-50000 mPa-s (e.g. 5000 mPa-s, 10000 mPa-s, 15000 mPa-s, 20000 mPa-s, 25000 mPa-s, 30000 mPa-s, 35000 mPa-s, 40000 mPa-s or 45000 mPa-s, etc.), more preferably 3000-20000 mPa-s, the ratio of monofunctional siloxane links to tetrafunctional siloxane links in the vinyl MQ silicone resin is 0.5-1.2 (e.g. 0.6, 0.7, 0.8, 0.9, 1.0 or 1.1, etc.), still more preferably 0.7-0.8, the mass percentage of vinyl in the vinyl MQ silicone resin is 0.01% -5% (e.g. 0.05%, 0.1%, 1%, 2%, 3%, 4% or 4.5%, etc.).
In the invention, the vinyl silicone resin is preferably vinyl MQ resin, and when the M/Q ratio is 0.7-0.8, the prepared organosilicon liquid optical cement can obtain a material with balanced hardness and viscosity after being solidified, and has better performance.
Preferably, the hydrogen-containing silicone resin comprises any one or a combination of at least two of hydrogen-containing MQ silicone resin, hydrogen-containing MT silicone resin, hydrogen-containing MDT silicone resin or hydrogen-containing MTQ silicone resin, and more preferably hydrogen-containing MQ silicone resin and/or hydrogen-containing MDT silicone resin.
Preferably, the viscosity of the hydrogen-containing MQ silicone resin is 1000 to 10000 mPa-s (e.g., 2000 mPa-s, 3000 mPa-s, 4000 mPa-s, 5000 mPa-s, 6000 mPa-s, 7000 mPa-s, 8000 mPa-s, 9000 mPa-s, etc.), more preferably 3000 to 10000 mPa-s, the ratio of monofunctional siloxane links to tetrafunctional siloxane links in the hydrogen-containing MQ silicone resin is 0.5 to 1.2 (e.g., 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, etc.), more preferably 0.7 to 0.8, and the mass percentage of hydrogen in the hydrogen-containing MQ silicone resin is 0.01 to 1.0% (e.g., 0.02%, 0.05%, 0.1%, 0.3%, 0.5%, 0.7%, or 0.9%, etc.).
Preferably, the chain extender has a general structural formula of HRR 'SiO (RR' SiO) n SiRR 'H wherein R, R' are each independently an alkyl group having 1 to 8 (e.g., 2, 3, 4, 5, 6, or 7) carbon atoms and n is a natural number of 1 to 8 (e.g., 2, 3, 4, 5, 6, or 7), and the chain extender comprises 0.01% to 0.2% hydrogen by mass (e.g., 0.02%, 0.05%, 0.07%, 0.09%, 0.11%, 0.13%, 0.15%, 0.17%, or 0.19%, etc.).
Preferably, each of said R, R' is independently methyl.
In the invention, the chain extender is hydrogen-containing silicone oil with silicon-hydrogen bonds at two ends of a molecular chain, and the chain extender has the main function of reacting with vinyl groups to connect the molecular chains of vinyl polysiloxane together, so that the effective molecular weight and the distance between potential crosslinking points of the chain extender are increased. Because the chain extender has a difunctional structure, the chain extender can not cause crosslinking in the curing reaction, only the molecular weight of vinyl polysiloxane is prolonged, and the effects of reducing the crosslinking density and the hardness of the final colloid formed by the organosilicon liquid optical cement can be realized, so that the toughness of the organosilicon liquid optical cement is improved, and the ageing resistance is improved. The mass percentage of hydrogen in the chain extender is 0.01% -0.2%, and if the mass percentage of hydrogen is too large, the hardness of the cured material of the organosilicon liquid optical cement is increased, and the viscosity is reduced; if the mass percentage of hydrogen is too small, the material of the cured organosilicon liquid optical cement is softer, and the compression strength is poor.
The reason for the yellowing of the organic silicon liquid optical adhesive disclosed by the invention also comprises that a large number of aromatic groups such as phenyl groups or naphthyl groups are introduced into the organic silicon liquid optical adhesive, and the existence of the aromatic groups can easily cause the organic silicon liquid optical adhesive to yellow in the high-temperature and aging processes. In the invention, R, R' in the structural general formula of the chain extender is independently alkyl with 1-8 carbon atoms, and the problem of yellowing of the liquid optical organosilicon adhesive is improved by avoiding selection of the chain extender containing aromatic groups and avoiding selection of other components containing aromatic groups.
Preferably, the catalyst comprises any one or a combination of at least two of chloroplatinic acid, a platinum-vinyl siloxane complex, a Karstedt platinum catalyst or a Willing platinum catalyst.
Preferably, the inhibitor comprises any one or a combination of at least two of 2-methyl-3-butyn-2-ol, 3, 5-dimethyl-1-hexyn-3-ol, 3-methyl-1-butyn-3-ol, 3-methyl-1-pentyn-3-ol, 1-ethynyl-1-cyclohexanol, phenylbutynol, tetramethyl divinyl disiloxane, tetramethyl tetra vinyl cyclotetrasiloxane or polyvinyl silicone oil.
Preferably, the viscosity of the silicone liquid optical adhesive is 1000-40000 mPa-s, (e.g. 2000 mPa-s, 5000 mPa-s, 8000 mPa-s, 10000 mPa-s, 15000 mPa-s, 20000 mPa-s, 25000 mPa-s, 30000 mPa-s or 35000 mPa-s, etc.).
In a second aspect, the present invention provides a method for preparing the liquid silicone optical cement according to the first aspect, the method comprising the following steps: and mixing vinyl polysiloxane, hydrogen-containing polysiloxane, silicone resin, a chain extender, a catalyst and an inhibitor to obtain the organosilicon liquid optical cement.
Preferably, the preparation method specifically comprises the following steps:
(1) Preparing a component A: mixing vinyl polysiloxane, optionally vinyl silicone resin and catalyst to obtain the A component.
(2) And (3) preparing a component B: mixing vinyl polysiloxane, optionally hydrogen-containing silicone resin, chain extender, hydrogen-containing polysiloxane and inhibitor to obtain the component B.
(3) And mixing the component A and the component B to obtain the organosilicon liquid optical cement.
The step (1) and the step (2) are carried out step by step in no sequence or simultaneously.
The mixing in step (1) of the preparation method comprises adding vinyl silicone resin and/or the mixing in step (2) comprises adding hydrogen-containing silicone resin.
Preferably, the mass ratio of the A component and the B component in step (3) is 1:0.9-1.1, such as 1:0.92, 1:0.94, 1:0.96, 1:0.98, 1:1, 1:1.02, 1:1.04, 1:1.06 or 1:1.1, etc.
In a third aspect, the present invention provides an application of the silicone liquid optical adhesive according to the first aspect in the lamination or encapsulation of electronic equipment.
Preferably, the electronic device comprises a liquid crystal display or a touch screen.
Compared with the prior art, the invention has the following beneficial effects:
the invention effectively improves the bonding performance between the organic silicon liquid optical adhesive and glass through the matching of vinyl polysiloxane, hydrogen-containing polysiloxane, silicone resin, chain extender, catalyst and inhibitor, and improves the yellowing problem of the organic silicon liquid optical adhesive by reducing the dosage of the catalyst and preferably adding components without aromatic groups. The organic silicon liquid optical adhesive has the advantages of high light transmittance, good transparency, good adhesion performance, good humidity and heat aging resistance and yellowing resistanceThe weather resistance is good, yellowing, delamination, degradation, detachment from the adhered surface, bubbles and other problems can not occur after long-time use, and the weather resistance has certain reworkability. The initial light transmittance of the adhesive film prepared by the organic silicon liquid optical adhesive is more than or equal to 99.1 percent, the wet heat aging light transmittance is more than or equal to 92.5 percent, the high temperature aging light transmittance is more than or equal to 91.8 percent, and the compression strength is 7.6-9.5gf/mm 2 The tensile shear strength of the glass-to-glass lap joint of the organic silicon liquid optical cement is more than or equal to 0.2Mpa. Preferably, the initial light transmittance of the adhesive film prepared by the organic silicon liquid optical adhesive is more than or equal to 99.1%, the wet heat aging light transmittance is more than or equal to 98.2%, the high temperature aging light transmittance is more than or equal to 97.2%, and the compression strength is 8.3-8.6gf/mm 2 The tensile shear strength of the glass-to-glass lap joint of the organic silicon liquid optical cement is more than or equal to 0.24Mpa.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
The following examples of the invention and comparative examples are presented as follows:
(1) The specific types of vinyl polysiloxanes A are shown in Table 1.
TABLE 1
(2) The specific types of hydrogen-containing polysiloxane B are shown in Table 2.
TABLE 2
(3) The specific types of silicone C are as follows:
TABLE 3 Table 3
TABLE 4 Table 4
C5: the hydrogen-containing MT silicone resin has the viscosity of 5000 mPas, the mass percent of hydrogen of 0.1 percent, the ratio of monofunctional siloxane units to trifunctional siloxane units of 0.8, and the manufacturer: nanxiong Lichang New Material technology Co., ltd., model: HMT-0.4.
(4) The specific types of the chain extender D are shown in Table 5.
TABLE 5
(5) Catalyst E
E1: karstedt platinum catalyst
E2: willing platinum catalyst
(6) Inhibitor F
F1: 2-methyl-3-butyn-2-ol
F2: 1-ethynyl-1-cyclohexanol.
Example 1
The embodiment provides an organic silicon liquid optical adhesive and a preparation method thereof, wherein the organic silicon liquid optical adhesive comprises the following components in parts by weight: 100 parts of vinyl polysiloxane A1, 4 parts of hydrogen-containing polysiloxane B1, 5 parts of silicone resin C3, 1 part of chain extender D1, 0.1 part of catalyst E1 and 0.1 part of inhibitor F1.
The preparation method of the organic silicon liquid optical cement comprises the following steps:
(1) Preparing a component A: 55 parts of vinyl polysiloxane A1 and 0.1 part of catalyst E1 were mixed to obtain the A component.
(2) And (3) preparing a component B: 45 parts of vinyl polysiloxane A1, 4 parts of hydrogen-containing polysiloxane B1, 5 parts of silicone resin C3, 1 part of chain extender D1 and 0.1 part of inhibitor F1 are mixed to obtain the component B.
(3) Mixing the component A and the component B in a mass ratio of 1:1, and removing bubbles to obtain the organosilicon liquid optical cement.
And curing the organic silicon liquid optical adhesive to obtain the adhesive film.
Example 2
The embodiment provides an organic silicon liquid optical adhesive and a preparation method thereof, wherein the organic silicon liquid optical adhesive comprises the following components in parts by weight: 70 parts of vinyl polysiloxane A1, 30 parts of vinyl polysiloxane A2, 2 parts of hydrogen-containing polysiloxane B3, 20 parts of silicone resin C1, 2 parts of chain extender D1, 0.05 part of catalyst E1 and 0.03 part of inhibitor F2.
The preparation method of the organic silicon liquid optical cement comprises the following steps:
(1) Preparing a component A: 30 parts of vinyl polysiloxane A1, 12 parts of vinyl polysiloxane A2, 20 parts of silicone resin C1 and 0.05 part of catalyst E1 are mixed to obtain the component A.
(2) And (3) preparing a component B: the B component is obtained by mixing 40 parts of vinyl polysiloxane A1, 18 parts of vinyl polysiloxane A2, 2 parts of hydrogen-containing polysiloxane B3, 2 parts of chain extender D1 and 0.03 part of inhibitor F2.
(3) Mixing the component A and the component B in a mass ratio of 1:1, and removing bubbles to obtain the organosilicon liquid optical cement.
And curing the organic silicon liquid optical adhesive to obtain the adhesive film.
Example 3
The embodiment provides an organic silicon liquid optical adhesive and a preparation method thereof, wherein the organic silicon liquid optical adhesive comprises the following components in parts by weight: 100 parts of vinyl polysiloxane A1, 0.5 part of hydrogen-containing polysiloxane B1, 1 part of silicone resin C4, 2 parts of chain extender D1, 0.02 part of catalyst E1 and 0.1 part of inhibitor F2. The preparation method of the organic silicon liquid optical cement comprises the following steps:
(1) Preparing a component A: 51.3 parts of vinyl polysiloxane A1 and 0.02 part of catalyst E1 were mixed to give the A component.
(2) And (3) preparing a component B: 48.7 parts of vinyl polysiloxane A1, 0.5 part of hydrogen-containing polysiloxane B1, 1 part of silicone resin C4, 2 parts of chain extender D1 and 0.1 part of inhibitor F2 are mixed to obtain the component B.
(3) Mixing the component A and the component B in a mass ratio of 1:1, and removing bubbles to obtain the organosilicon liquid optical cement.
And curing the organic silicon liquid optical adhesive to obtain the adhesive film.
Example 4
The embodiment provides an organic silicon liquid optical adhesive and a preparation method thereof, wherein the organic silicon liquid optical adhesive comprises the following components in parts by weight: 100 parts of vinyl polysiloxane A1, 4 parts of hydrogen-containing polysiloxane B1, 15 parts of silicone resin C2, 4 parts of chain extender D1, 0.1 part of catalyst E1 and 0.2 part of inhibitor F1.
The preparation method of the organic silicon liquid optical cement comprises the following steps:
(1) Preparing a component A: 46.5 parts of vinyl polysiloxane A1, 15 parts of silicone resin C2 and 0.1 part of catalyst E1 were mixed to obtain the A component.
(2) And (3) preparing a component B: 53.5 parts of vinyl polysiloxane A1, 4 parts of hydrogen-containing polysiloxane B1, 4 parts of chain extender D1 and 0.1 part of inhibitor F2 are mixed to obtain the component B.
(3) Mixing the component A and the component B in a mass ratio of 1:1, and removing bubbles to obtain the organosilicon liquid optical cement.
And curing the organic silicon liquid optical adhesive to obtain the adhesive film.
Example 5
The embodiment provides an organic silicon liquid optical adhesive and a preparation method thereof, wherein the organic silicon liquid optical adhesive comprises the following components in parts by weight: 90 parts of vinyl polysiloxane A1, 10 parts of vinyl polysiloxane A3, 1 part of hydrogen-containing polysiloxane B2, 30 parts of silicone resin C2, 1 part of chain extender D2, 0.02 part of catalyst E1 and 0.1 part of inhibitor F1;
the preparation method of the organic silicon liquid optical cement comprises the following steps:
(1) Preparing a component A: 32 parts of vinyl polysiloxane A1, 4 parts of vinyl polysiloxane A3, 30 parts of silicone resin C2 and 0.02 part of catalyst E1 are mixed to obtain the component A.
(2) And (3) preparing a component B: 58 parts of vinyl polysiloxane A1, 6 parts of vinyl polysiloxane A3, 1 part of hydrogen-containing polysiloxane B2, 1 part of chain extender D2 and 0.1 part of inhibitor F1 are mixed to obtain the component B.
(3) Mixing the component A and the component B in a mass ratio of 1:1, and removing bubbles to obtain the organosilicon liquid optical cement.
And curing the organic silicon liquid optical adhesive to obtain the adhesive film.
Example 6
The embodiment provides an organic silicon liquid optical adhesive and a preparation method thereof, wherein the organic silicon liquid optical adhesive comprises the following components in parts by weight: 100 parts of vinyl polysiloxane A3, 0.5 part of hydrogen-containing polysiloxane B4, 1 part of silicone resin C5, 5 parts of chain extender D1, 0.04 part of catalyst E2 and 0.1 part of inhibitor F1;
the preparation method of the organic silicon liquid optical cement comprises the following steps:
(1) Preparing a component A: 53.3 parts of vinyl polysiloxane A3 and 0.04 part of catalyst E2 were mixed to obtain the A component.
(2) And (3) preparing a component B: 46.7 parts of vinyl polysiloxane A3, 0.5 part of hydrogen-containing polysiloxane B4, 1 part of silicone resin C5, 5 parts of chain extender D1 and 0.1 part of inhibitor F1 are mixed to obtain the component B.
(3) Mixing the component A and the component B in a mass ratio of 1:1, and removing bubbles to obtain the organosilicon liquid optical cement.
And curing the organic silicon liquid optical adhesive to obtain the adhesive film.
Example 7
This example provides an organosilicon liquid optical cement and a preparation method thereof, which are different from example 1 only in that the chain extender D1 is replaced by a chain extender D3 with the same mass, and the other is the same as example 1.
Example 8
This example provides an organosilicon liquid optical cement and a preparation method thereof, which are different from example 1 only in that the chain extender D1 is replaced by a chain extender D4 with the same mass, and the other is the same as example 1.
Example 9
This example provides an organosilicon liquid optical cement and a preparation method thereof, which are different from example 1 only in that the chain extender D1 is replaced by a chain extender D5 with the same mass, and the other is the same as example 1.
Example 10
This example provides an organosilicon liquid optical cement and a preparation method thereof, which are different from example 1 only in that hydrogen-containing polysiloxane B1 is replaced by hydrogen-containing polysiloxane B2 of the same mass, and the other is the same as example 1.
Example 11
This example provides an organosilicon liquid optical cement and a preparation method thereof, which are different from example 1 only in that the weight part of the catalyst E1 is adjusted to 0.2 part, and the other is the same as example 1.
Comparative example 1
This comparative example provides an organosilicon liquid optical cement and a preparation method thereof, which are different from example 1 only in that the weight part of the catalyst E1 is adjusted to 0.5 part, and the other is the same as example 1.
Comparative example 2
This comparative example provides an organosilicon liquid optical cement and a preparation method thereof, which are different from example 1 only in that a chain extender D1 is not added, and the other is the same as example 1.
Comparative example 3
This comparative example provides an organosilicon liquid optical cement and a preparation method thereof, which are different from example 1 only in that the weight part of hydrogen-containing polysiloxane B1 is adjusted to 0.4 part, and the other is the same as example 1.
Comparative example 4
This comparative example provides an organosilicon liquid optical cement and a preparation method thereof, which are different from example 1 only in that the weight part of hydrogen-containing polysiloxane B1 is adjusted to 15 parts, and the other is the same as example 1.
Comparative example 5
This comparative example provides an organosilicon liquid optical cement and a preparation method thereof, which are different from example 1 only in that the weight part of silicone resin C3 is adjusted to 35 parts, and the other is the same as example 1.
Comparative example 6
This comparative example provides an organosilicon liquid optical cement and a preparation method thereof, which are different from example 1 only in that the weight part of silicone resin C3 is adjusted to 0.5 part, and otherwise the same as example 1.
Comparative example 7
This comparative example provides an organosilicon liquid optical cement and a preparation method thereof, which are different from example 1 only in that no silicone resin C3 is added, and the other is the same as example 1.
The silicone liquid optical gums provided in the examples and comparative examples were subjected to the following performance tests.
(1) Refractive index of light: the test was carried out using a WAY-2W Abbe refractometer from Shanghai electric physical optical instruments, inc. at a temperature of 23 ℃.
(2) Initial light transmittance: and testing a glue film prepared from the organic silicon liquid optical glue according to ASTM D1003-2013, wherein the adopted equipment is a spectrocolorimeter (Hunterlab Ultra Scan Vis), the thickness of the glue film is 0.3mm, and the light transmittance is more than or equal to 90 percent.
(3) Wet heat aged light transmittance: and (3) placing the adhesive film prepared by the organic silicon liquid optical adhesive into a constant temperature and humidity box with the temperature of 85 ℃ and the humidity of 85% for 1000 hours, then observing whether the surface is abnormal or not, and if the surface is abnormal, carrying out a light transmittance test, wherein the light transmittance is more than or equal to 90% and is qualified.
(4) High temperature aged light transmittance: and (3) placing the adhesive film prepared by the organic silicon liquid optical adhesive into an incubator with the temperature of 125 ℃ for 1000 hours, then observing whether the surface is abnormal or not, and if the surface is abnormal, carrying out a light transmittance test, wherein the light transmittance is more than or equal to 90 percent.
(5) Tensile shear strength: testing is carried out according to GB/T7124-1986, and the tensile shear strength of the glass of the organosilicon liquid optical cement to the lap joint of the glass is tested, and the tensile shear strength is required to be more than or equal to 0.2MPa and is qualified.
(6) Compressive strength: the test is carried out by adopting a texture analyzer (a Paul technology texture analyzer TA.XTC-20), the test sample is a sample with the diameter of 50mm and the thickness of 10mm, which is prepared by curing organosilicon liquid optical cement, and the compression strength is 7.5-9.5gf/mm 2 And the interval is qualified.
The test results are shown in Table 1.
TABLE 1
As can be seen from the test results in Table 1, the initial transmittance of the adhesive films prepared from the silicone liquid optical adhesives provided in examples 1 to 11 is not less than 99.1%, the wet heat aging transmittance is not less than 92.5%, the high temperature aging transmittance is not less than 91.8%, and the compressive strength is 7.6 to 9.5gf/mm 2 The tensile shear strength of the glass-to-glass lap joint of the organic silicon liquid optical cement is more than or equal to 0.2Mpa. The initial transmittance of the adhesive film prepared by the organic silicon liquid optical adhesive provided in examples 1-4 is more than or equal to 99.1%, the wet heat aging transmittance is more than or equal to 98.2%, the high temperature aging transmittance is more than or equal to 97.2%, and the compression strength is 8.3-8.6gf/mm 2 The tensile shear strength of the glass-to-glass lap joint of the organic silicon liquid optical cement is more than or equal to 0.24Mpa. The organic silicon liquid optical adhesive provided by the invention has high light transmittance and good transparency; the high light transmittance is still maintained after the wet heat aging and the high temperature aging, the wet heat aging resistance is good, the yellowing resistance is good, and the weather resistance is good; high tensile shear strength and good adhesive property.
In comparison with example 1, if the chain extender D1 is replaced with a chain extender D3 of the same mass (example 7), both the tensile shear strength of the silicone liquid optical adhesive and the compressive strength of the produced adhesive film are reduced; if the chain extender D1 is replaced by a chain extender D4 (example 8) with the same mass, the compressive strength of the cured silicone liquid optical adhesive material is higher. From the above, the mass percentage of hydrogen in the chain extender is 0.01% -0.2%, and the prepared organosilicon liquid optical cement has better performance.
In comparison with example 1, when the chain extender D1 was replaced with a chain extender D5 of the same mass (example 9), the transmittance after the wet heat aging and the high temperature aging was significantly lowered. It can be seen that the chain extender has the general structural formula of HRR 'SiO (RR' SiO) n SiRR 'H, wherein R, R' is alkyl with 1-8 carbon atoms independently, and the prepared organosilicon liquid optical cement has better performance.
In contrast to example 1, when the hydrogen-containing polysiloxane B1 was replaced with the hydrogen-containing polysiloxane B2 of the same mass (example 10), the tensile shear strength of the silicone liquid optical adhesive was reduced and the compressive strength after curing was increased. Therefore, when the mass percentage of hydrogen atoms in the hydrogen-containing polysiloxane is 0.02% -0.3%, the prepared organic silicon liquid optical adhesive has better performance.
In comparison with example 1, the increase in the weight fraction of the catalyst (example 11) reduced the optical transmittance after humid heat aging and high temperature aging.
In comparison with example 1, when the mass fraction of the catalyst E1 is too high (comparative example 1), the optical transmittance after the wet heat aging and the high temperature aging is significantly deteriorated, and it is understood that the performance of the silicone liquid optical adhesive prepared by the weight fraction of the catalyst within a specific range is better.
In contrast to example 1, without the addition of chain extender B1 (comparative example 2), the compressive strength is significantly increased, the stiffness is decreased, the tackiness is decreased, and the tensile shear strength is decreased.
Compared with the example 1, if the weight part of the hydrogen-containing polysiloxane B1 is too low (comparative example 3), the crosslinking curing degree of the organic silicon liquid optical adhesive after curing is too low, the tensile shear strength and the compressive strength are lower, and the viscosity is greatly reduced; if the weight fraction of the hydrogen-containing polysiloxane B1 is too high (comparative example 4), the silicone liquid optical adhesive becomes significantly hard after curing, and the tackiness is poor, so that the compressive strength is high and the shear strength is low. From the above, it is apparent that the weight portion of the hydrogen polysiloxane is within a specific range, and the prepared organosilicon liquid optical cement has better performance.
In contrast to example 1, if the weight fraction of silicone resin C3 is too high (comparative example 5), the compressive strength of the silicone liquid optical adhesive after curing is reduced; if the weight fraction of silicone resin C3 is too low (comparative example 6), the compressive strength increases but the shear strength decreases after the silicone liquid optical adhesive is cured. Therefore, the weight part of the silicone resin is in a specific range, and the prepared organic silicon liquid optical adhesive has better performance.
In contrast to example 1, if silicone C3 (comparative example 7) was not added, the silicone liquid optical adhesive had lower tensile shear strength and significantly reduced tackiness.
The applicant states that the present invention is described by the above examples as an organosilicon liquid optical cement, and a preparation method and application thereof, but the present invention is not limited to the above examples, i.e. it does not mean that the present invention must be implemented by the above examples. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (10)
1. The organic silicon liquid optical adhesive is characterized by comprising the following components in parts by weight: 100 parts of vinyl polysiloxane, 0.5-10 parts of hydrogen polysiloxane, 1-30 parts of silicone resin, 0.5-5 parts of chain extender, 0.01-0.4 part of catalyst and 0.01-0.5 part of inhibitor.
2. The liquid silicone optical adhesive of claim 1, wherein the vinyl polysiloxane comprises a linear or branched polysiloxane having vinyl groups at the chain ends and/or side chains.
3. The silicone liquid optical adhesive of claim 1 or 2, wherein the vinyl polysiloxane further comprises at least one of the following features:
the mass percentage of vinyl in the vinyl polysiloxane is 0.1% -5%;
the viscosity of the vinyl siloxane at 25 ℃ is 200-20000 mPa.s;
the refractive index of the vinyl siloxane is 1.39-1.41.
4. A silicone liquid optical adhesive according to any one of claims 1 to 3, wherein the hydrogen-containing polysiloxane has three or more hydrogen atoms bonded to silicon atoms in a molecular chain;
preferably, the hydrogen atom content of the hydrogen-containing polysiloxane is 0.01-0.8%, and more preferably 0.02-0.3%;
preferably, the silicone resin comprises vinyl silicone resin and/or hydrogen-containing silicone resin;
preferably, the vinyl silicone resin comprises any one or a combination of at least two of vinyl MQ silicone resin, vinyl MT silicone resin, vinyl MDT silicone resin or vinyl MTQ silicone resin, and further preferably vinyl MQ silicone resin and/or vinyl MDT silicone resin;
preferably, the viscosity of the vinyl MQ silicone resin is 1000-50000 mPa.s at 25 ℃, the ratio of monofunctional siloxane chain units to tetrafunctional siloxane chain units in the vinyl MQ silicone resin is 0.5-1.2, and the mass percent of vinyl in the vinyl MQ silicone resin is 0.01-5%;
preferably, the hydrogen-containing silicone resin comprises any one or a combination of at least two of hydrogen-containing MQ silicone resin, hydrogen-containing MT silicone resin, hydrogen-containing MDT silicone resin or hydrogen-containing MTQ silicone resin, and more preferably hydrogen-containing MQ silicone resin and/or hydrogen-containing MDT silicone resin;
preferably, the viscosity of the hydrogen-containing MQ silicone resin is 1000-10000 mPa.s at 25 ℃, the ratio of monofunctional siloxane chain units to tetrafunctional siloxane chain units in the hydrogen-containing MQ silicone resin is 0.5-1.2, and the mass percentage of hydrogen in the hydrogen-containing MQ silicone resin is 0.01% -1.0%.
5. The liquid silicone optical cement according to any one of claims 1 to 4, wherein the chain extender has a general structural formula of HRR 'SiO (RR' SiO) n SiRR 'H, wherein R, R' is independently alkyl with 1-8 carbon atoms, n is a natural number of 1-8, and the mass percentage of hydrogen in the chain extender is 0.01% -0.2%;
preferably, each of said R, R' is independently methyl.
6. The silicone liquid optical adhesive of any one of claims 1-5 wherein the catalyst comprises any one or a combination of at least two of chloroplatinic acid, a platinum-vinyl siloxane complex, a Karstedt platinum catalyst, or a Willing platinum catalyst.
7. The silicone liquid optical adhesive of any one of claims 1-6 wherein the inhibitor comprises any one or a combination of at least two of 2-methyl-3-butyn-2-ol, 3, 5-dimethyl-1-hexyn-3-ol, 3-methyl-1-butyn-3-ol, 3-methyl-1-pentyn-3-ol, 1-ethynyl-1-cyclohexanol, phenylbutynol, tetramethyl divinyl disiloxane, tetramethyl tetravinyl cyclotetrasiloxane, or polyvinyl silicone oil;
preferably, the viscosity of the organosilicon liquid optical cement is 1000-40000 mPa.s.
8. A method for preparing the liquid silicone optical cement according to any one of claims 1 to 7, comprising the steps of: and mixing vinyl polysiloxane, hydrogen-containing polysiloxane, silicone resin, a chain extender, a catalyst and an inhibitor to obtain the organosilicon liquid optical cement.
9. The preparation method according to claim 8, characterized in that it comprises the following steps:
(1) Preparing a component A: mixing vinyl polysiloxane, optionally vinyl silicone resin, and catalyst to obtain the a component;
(2) And (3) preparing a component B: mixing vinyl polysiloxane, optionally hydrogen-containing silicone resin, chain extender, hydrogen-containing polysiloxane and inhibitor to obtain the component B;
(3) Mixing the component A and the component B to obtain the organosilicon liquid optical cement;
the step (1) and the step (2) are carried out step by step in no sequence or simultaneously;
the mixing in step (1) of the preparation method comprises adding vinyl silicone resin and/or the mixing in step (2) comprises adding hydrogen-containing silicone resin;
preferably, the mass ratio of the component A to the component B in the step (3) is 1:0.9-1.1.
10. Use of the silicone liquid optical adhesive of any one of claims 1-7 in the lamination or encapsulation of electronic devices;
preferably, the electronic device comprises a liquid crystal display or a touch screen.
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