CN103242796A - Ultraviolet curing liquid state optical cement and preparation method thereof - Google Patents
Ultraviolet curing liquid state optical cement and preparation method thereof Download PDFInfo
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- CN103242796A CN103242796A CN2013101963825A CN201310196382A CN103242796A CN 103242796 A CN103242796 A CN 103242796A CN 2013101963825 A CN2013101963825 A CN 2013101963825A CN 201310196382 A CN201310196382 A CN 201310196382A CN 103242796 A CN103242796 A CN 103242796A
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Abstract
The invention relates to ultraviolet curing liquid state optical cement which is prepared from the components in parts by mass as follows: 40-70 parts of polyurethane acrylate oligomer, 20-40 parts of (methyl) acrylic ester, 0.1-5 parts of photoinitiator, 1-10 parts of silane coupling agent and 0-10 parts of assistant. The invention further provides a preparation method of the ultraviolet curing liquid state optical cement. Besides the characteristics of transparent appearance, stable viscosity, low energy required for curing, quick curing speed, high refractive index and the like, the ultraviolet curing liquid state optical cement provided by the invention further has the excellent characteristics of great bonding strength, low hardness after curing, good flexibility and excellent weather ability.
Description
Technical field
The present invention relates to tackiness agent, be specifically related to the liquid optical cement of a kind of ultraviolet light polymerization that mounts for touch-screen, and the preparation method of the liquid optical cement of this ultraviolet light polymerization.
Background technology
Touch-screen combines owing to good vision is presented with intuition system operation easily, obtains application more and more widely in recent years in electronic products such as mobile phone, panel computer, televisor, Vehicular guidance system.
At present, in touch-screen is made, use liquid optical cement (Liquid Optical Clear Adhesive mostly, LOCA) as tackiness agent bonding between each base material, existing liquid optical cement can satisfy some basic demands, as: transmitance is more than 90% in the water white transparency, specific light-wave band, and the specific refractory power of curing back specific refractory power and the sticking base material of quilt is close etc.But, crisp firmly, problems such as snappiness is poor, weathering resistance difference a little less than the existing liquid optical cement ubiquity cohesive strength, after the curing, the steady quality time limit of greatly having reduced touch-screen product self.
Summary of the invention
Technical problem to be solved by this invention provides the preparation method of the liquid optical cement of a kind of ultraviolet light polymerization that mounts for touch-screen and the liquid optical cement of this ultraviolet light polymerization, the liquid optical cement cohesive strength of this ultraviolet light polymerization is big, curing back hardness is low and snappiness good, and weathering resistance is splendid.The technical scheme that adopts is as follows:
The liquid optical cement of a kind of ultraviolet light polymerization, it is characterized in that being formed by following components in weight percentage: urethane acrylate oligomer 40-70 part, (methyl) acrylate 20-40 part, light trigger 0.1-5 part, silane coupling agent 1-10 part, auxiliary agent 0-10 part.
Preferred above-mentioned urethane acrylate oligomer is that average viscosity is that 20000-70000cps, molecular-weight average are that 10000-50000, functionality are the urethane acrylate of 1-3.Above-mentioned urethane acrylate oligomer is formed by monomer and the Acrylic Acid Monomer copolymerization of long-chain polyhydric alcohol, band isocyanide ester base.Low functionality makes degree of crosslinking reduce, thereby has reduced hardness; The polyol structure of overlength segment has improved the snappiness of colloid, thereby has reduced hardness; The effect of isocyanide ester base makes urethane acrylate itself have stronger force of cohesion, thereby improves the cohesive strength of colloid.
Above-mentioned (methyl) acrylate is being collectively referred to as of acrylate and methacrylic ester.Preferably above-mentioned (methyl) acrylate is (methyl) acrylate that contains the long-chain section, or (methyl) acrylate of hydroxyl structure, or (methyl) acrylate of band heterocycle structure, or (methyl) acrylate of the many rings of band benzene.The existence of long-chain section can improve the snappiness of colloid; The existence of hydroxyl because generating hydrogen bond, thereby improves colloid to the cohesive force of glass; The existence of heterocycle (including but not limited to naphthenic hydrocarbon, phenyl ring, epoxy etc.) helps to improve intensity and the cohesive force of colloid; The structure of many ring benzene can improve the specific refractory power of colloid; Long-chain section or alicyclic structure can also improve hydrophobicity, water boiling resistance performance, the high-temp resisting high-humidity resisting performance of colloid.
More preferably in the scheme, above-mentioned (methyl) acrylate is Hydroxyethyl acrylate, hydroxyethyl methylacrylate, 4-hydroxybutyl acrylate, vinylformic acid-2-hydroxypropyl acrylate, Rocryl 410,2-hydroxyl-2-butyl acrylate cores, 1,4-cyclohexanedimethanol mono acrylic ester, 1,4-cyclohexanedimethanol methacrylic ester, 1-chloro-2-hydroxypropyl acrylate, 1-chloro-2-hydroxypropylmethyl acrylate, diethylene glycol monoacrylate, the glycol ether methyl acrylate, 1, the 6-hexanediol monoacrylate, 1,6 hexanediol diacrylate, pentaerythritol triacrylate, dipentaerythritol five acrylate, the TriMethylolPropane(TMP) dimethacrylate, isobornyl acrylate, isobornyl methacrylate, the cyclopentyl acrylate, the cyclopentyl methyl acrylate, 2-vinylformic acid cyclohexyl ester, the 2-cyclohexyl methacrylate, dicyclo benzene oxygen ethyl propylene acid esters, methyl acrylate, ethyl propenoate, Jia Jibingxisuanyizhi, propyl acrylate, propyl group-2-methyl-2-acrylate, isopropyl acrylate, n-BMA, n-butyl acrylate, the methacrylic tert-butyl acrylate, isobutyl acrylate, Propenoic acid, 2-methyl, isobutyl ester, the vinylformic acid n-pentyl ester, the methacrylic acid pentyl ester, the vinylformic acid n-octyl, Isooctyl acrylate monomer, Isooctyl methacrylate, decyl acrylate, decyl-octyl methacrylate, methacrylic acid undecyl ester, the 2-dodecylacrylate, a kind of in lauryl acrylate and the lauryl methacrylate(LMA) or wherein multiple combination.
Above-mentioned light trigger mainly plays the absorption UV-light, thereby excites to provide free radical, the effect that reaction is carried out smoothly.Effective functional group of light trigger includes but not limited to bitter almond oil camphor class, acetophenones, a-hydroxyl ketone, acylphosphine oxide, a-aminoketones etc.Preferred above-mentioned light trigger is tetraethyl-michaelis ketone, benzophenone, 1-hydroxy-cyclohexyl phenyl ketone, acrylate benzophenone, phenyl benzophenone, dihydroxy benaophenonel, 4; 4'-two (N; the N-dimethylamino) benzophenone, 2; 2'-diethoxy acetophenone, 2-hydroxyl-2-phenyl methyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 2; 4; 6-Three methyl Benzene formyl-diphenyl phosphine oxide, two (2; 4,6-trimethylbenzoyl) a kind of in phenyl phosphine oxide, benzoin methyl ether, Benzoin ethyl ether and the cyanuric chloride or wherein multiple combination.
The hydrolysable group hydrolysis of above-mentioned silane coupling agent generates silanol, forms siloxanes with inorganic substance (as glass) combination; In addition, " molecule bridge " erected in the organo-functional group of silane coupling agent and Acrylic Acid Monomer copolymerization between inorganic substance and organic substance, makes the liquid optical cement of ultraviolet light polymerization have excellent cohesive force.Preferred above-mentioned silane coupling agent is trimethoxy silicomethane, vinyltriethoxysilane, 3-Trimethoxy silane vinylformic acid third fat, 3-methyl allyl acyloxypropyl trimethoxysilane, 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane, 3-[(2,3)-and epoxy third oxygen] a kind of in propyl group methyl dimethoxysilane, trimethoxy [2-(7-oxabicyclo [4.1.0] heptan-3-yl) ethyl] silane, 3-TSL 8330 (being coupling agent KH-540) and the 3-r-chloropropyl trimethoxyl silane or wherein multiple combination.
Above-mentioned auxiliary agent can be a kind of in softening agent, defoamer and the photostabilizer or combination that it is multiple.
Above-mentioned softening agent is used for increasing the flexibility of polymkeric substance, and its specific refractory power general requirement is more than 1.48.Preferred above-mentioned softening agent is a kind of in phthalic ester, phosphoric acid ester (as triphenylphosphate), alkyl sulfonic ester, fatty group dibasic acid (as the own ester of hexanodioic acid two (2-ethyl), the just own ester of sebacic acid two), benzene polyacid ester and the epoxy compounds or wherein multiple combination.
Above-mentioned defoamer is used for suppressing, reduce or eliminates the bubble in the polymkeric substance.Preferred above-mentioned defoamer is a kind of in tributyl phosphate, polydimethylsiloxane, polyacrylic ester and the polyethers or wherein multiple combination.
Above-mentioned photostabilizer is used for suppressing or slowing down polymkeric substance photooxidation resistance process.Preferred above-mentioned photostabilizer is two (1,2,2,6,6-pentamethyl--4-piperidines) sebate, 1-methyl-8-(1,2,2,6,6-pentamethyl--4-piperidines) sebate, 4-hydroxyl-2,2,6,6-tetramethyl--1-piperidines alcohol, two (3,5-di-tert-butyl-4-hydroxyl benzyl monoethyl phosphate) nickel, 2-(2 '-hydroxyl-3 ', 5-di-tert-butyl-phenyl) a kind of in benzotriazole and 2-hydroxyl-two ketones of 4-n-octyloxy or wherein multiple combination.
The present invention also provides a kind of preparation method of the liquid optical cement of above-mentioned ultraviolet light polymerization, it is characterized in that comprising the steps: successively
(1) by weight, get 40-70 part urethane acrylate oligomer, 20-40 part (methyl) acrylate, 0.1-5 part light trigger, 1-10 part silane coupling agent and 0-10 part auxiliary agent, and join in the reaction vessel of cleaning, drying, be to be stirred under 1000-1500 rev/min the condition to mix (preferred churning time is 30-60 minute) then with the material low whipping speed in the reaction vessel, obtain sizing material;
(2) sizing material that step (1) is obtained with the vacuum defoamation machine carries out deaeration (the preferred deaeration time is 20-30 minute), obtains the liquid optical cement of ultraviolet light polymerization.
For guaranteeing the purity of the liquid optical cement of ultraviolet light polymerization, before step (2) was carried out deaeration, the sizing material that step (1) is obtained filtered, and removed wherein impurity (impurity is that materials such as dust on production unit are infected with in neutralization from environment).The filter membrane aperture that is preferred for filtering is 1-20um.
The liquid optical cement of ultraviolet light polymerization of the present invention needs the characteristics such as energy is low, curing speed is fast, specific refractory power height except having appearance transparent, stable viscosity, curing, also have following good characteristic: cohesive strength is big, curing back hardness is low and snappiness good, and weathering resistance is splendid.
Embodiment
Embodiment 1
In the present embodiment, the preparation method of the liquid optical cement of ultraviolet light polymerization comprises the steps: successively
(1) by weight, (being average viscosity is 50000cps to get 67 gram urethane acrylate oligomer, molecular-weight average is 50000, functionality is 2 urethane acrylate, this urethane acrylate is by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), 20 gram (methyl) acrylate (are 1,4-cyclohexanedimethanol methacrylic ester), 5 gram light triggers (being phenyl benzophenone), 6 gram silane coupling agents (being vinyltriethoxysilane) and 2 gram auxiliary agents (being the own ester of softening agent hexanodioic acid two (2-ethyl)), and join cleaning, in the dry reaction vessel, be to be stirred under 1200 rev/mins the condition to mix (churning time is 50 minutes) then with the material low whipping speed in the reaction vessel, obtain sizing material;
(2) sizing material that step (1) is obtained with the vacuum defoamation machine carries out deaeration (the deaeration time is 25 minutes), obtains the liquid optical cement of ultraviolet light polymerization.
Consisting of of the liquid optical cement of the ultraviolet light polymerization that makes: (be average viscosity is 50000cps to urethane acrylate oligomer 67 grams, molecular-weight average is 50000, functionality is 2 urethane acrylate, this urethane acrylate is by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), (methyl) acrylate 20 grams (being the 1,4 cyclohexane dimethanol methacrylic ester), light trigger 5 grams (being phenyl benzophenone), silane coupling agent 6 grams (being vinyltriethoxysilane) and auxiliary agent 2 grams (being the own ester of softening agent hexanodioic acid two (2-ethyl)).
Being equipped with raw material during batch process according to the above ratio gets final product.
Embodiment 2
In the present embodiment, the preparation method of the liquid optical cement of ultraviolet light polymerization comprises the steps: successively
(1) by weight, (being average viscosity is 40000cps to get 55 gram urethane acrylate oligomer, molecular-weight average is 35000, functionality is 1 urethane acrylate, this urethane acrylate is by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), 32 gram (methyl) acrylate (being isobornyl methacrylate), 2 gram light triggers (are 2,2 '-diethoxy acetophenone), 1 gram silane coupling agent (being the 3-methyl allyl acyloxypropyl trimethoxysilane) and 10 gram auxiliary agents (being the just own ester of softening agent sebacic acid two), and join cleaning, in the dry reaction vessel, be to be stirred under 1500 rev/mins the condition to mix (churning time is 30 minutes) then with the material low whipping speed in the reaction vessel, obtain sizing material;
(2) sizing material that step (1) is obtained with the vacuum defoamation machine carries out deaeration (the deaeration time is 20 minutes), obtains the liquid optical cement of ultraviolet light polymerization.
Consisting of of the liquid optical cement of the ultraviolet light polymerization that makes: (be average viscosity is 40000cps to urethane acrylate oligomer 55 grams, molecular-weight average is 35000, functionality is 1 urethane acrylate, this urethane acrylate is by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), (methyl) acrylate 32 grams (being isobornyl methacrylate), light trigger 2 grams (being 2,2 '-diethoxy acetophenone), silane coupling agent 1 gram (being the 3-methyl allyl acyloxypropyl trimethoxysilane) and auxiliary agent 10 grams (being the just own ester of softening agent sebacic acid two).
Being equipped with raw material during batch process according to the above ratio gets final product.
Embodiment 3
In the present embodiment, the preparation method of the liquid optical cement of ultraviolet light polymerization comprises the steps: successively
(1) by weight, (being average viscosity is 45000cps to get 60 gram urethane acrylate oligomer, molecular-weight average is 40000, functionality is 1.5 urethane methacrylate, this urethane acrylate is by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), (wherein Isooctyl methacrylate 20 restrains 33 gram (methyl) acrylate, isobornyl methacrylate 13 grams), 0.2 gram light trigger (being 2-hydroxyl-2-phenyl methyl phenyl ketone), 3 gram silane coupling agents (are 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane) and 3.8 gram auxiliary agents (wherein photostabilizer two (3,5-di-tert-butyl-4-hydroxyl benzyl monoethyl phosphate) nickel 0.3 gram, softening agent triphenylphosphate 3.5 grams), and join cleaning, in the dry reaction vessel, be to be stirred under 1000 rev/mins the condition to mix (churning time is 60 minutes) then with the material low whipping speed in the reaction vessel, obtain sizing material;
(2) sizing material that step (1) is obtained with the vacuum defoamation machine carries out deaeration (the deaeration time is 30 minutes), obtains the liquid optical cement of ultraviolet light polymerization.
Consisting of of the liquid optical cement of the ultraviolet light polymerization that makes: (be average viscosity is 45000cps to urethane acrylate oligomer 60 grams, molecular-weight average is 40000, functionality is 1.5 urethane methacrylate, this urethane acrylate is by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), (wherein Isooctyl methacrylate 20 restrains (methyl) acrylate 33 grams, isobornyl methacrylate 13 grams), light trigger 0.2 gram (being 2-hydroxyl-2-phenyl methyl phenyl ketone), silane coupling agent 3 grams (are 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane) and auxiliary agent 3.8 gram (wherein photostabilizer two (3,5-di-tert-butyl-4-hydroxyl benzyl monoethyl phosphate) nickel 0.3 gram, softening agent triphenylphosphate 3.5 grams).
Being equipped with raw material during batch process according to the above ratio gets final product.
Embodiment 4
In the present embodiment, the preparation method of the liquid optical cement of ultraviolet light polymerization comprises the steps: successively
(1) by weight, (wherein average viscosity is 50000cps to get 65 gram urethane acrylate oligomer, molecular-weight average is 50000, functionality is 2 urethane acrylate 35 grams, average viscosity is 40000cps, molecular-weight average is 35000, functionality is 1.5 urethane acrylate 30 grams, these two kinds of urethane acrylates are by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), (wherein dicyclo benzene oxygen ethyl propylene acid esters 10 restrains 30 gram (methyl) acrylate, isobornyl methacrylate 20 grams), 3 gram light triggers (being Benzoin ethyl ether) and 2 gram silane coupling agents (being vinyltriethoxysilane), and join cleaning, in the dry reaction vessel, be to be stirred under 1400 rev/mins the condition to mix (churning time is 40 minutes) then with the material low whipping speed in the reaction vessel, obtain sizing material;
(2) sizing material that step (1) is obtained with the vacuum defoamation machine carries out deaeration (the deaeration time is 28 minutes), obtains the liquid optical cement of ultraviolet light polymerization.
Consisting of of the liquid optical cement of the ultraviolet light polymerization that makes: (wherein average viscosity is 50000cps to urethane acrylate oligomer 65 grams, molecular-weight average is 50000, functionality is 2 urethane acrylate 35 grams, average viscosity is 40000cps, molecular-weight average is 35000, functionality is 1.5 urethane acrylate 30 grams, and these two kinds of urethane acrylates are by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), (wherein dicyclo benzene oxygen ethyl propylene acid esters 10 restrains (methyl) acrylate 30 grams, isobornyl methacrylate 20 grams), light trigger 3 grams (being Benzoin ethyl ether) and silane coupling agent 2 grams (being vinyltriethoxysilane).
Being equipped with raw material during batch process according to the above ratio gets final product.
Embodiment 5
In the present embodiment, the preparation method of the liquid optical cement of ultraviolet light polymerization comprises the steps: successively
(1) by weight, (being average viscosity is 50000cps to get 55 gram urethane acrylate oligomer, molecular-weight average is 50000, functionality is 1.5 urethane acrylate, this urethane acrylate is by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), (wherein dicyclo benzene oxygen ethyl propylene acid esters 10 restrains 40 gram (methyl) acrylate, isobornyl methacrylate 10 grams, hydroxyethyl methylacrylate 10 grams, Jia Jibingxisuanyizhi 10 grams), 2 gram light triggers (being Benzoin ethyl ether), 2 gram silane coupling agents (being vinyltriethoxysilane) and 1 gram auxiliary agent (are photostabilizer 2-(2 '-hydroxyl-3 ', the 5-di-tert-butyl-phenyl) benzotriazole), and join cleaning, in the dry reaction vessel, be to be stirred under 1200 rev/mins the condition to mix (churning time is 55 minutes) then with the material low whipping speed in the reaction vessel, obtain sizing material;
(2) sizing material that step (1) is obtained with the vacuum defoamation machine carries out deaeration (the deaeration time is 30 minutes), obtains the liquid optical cement of ultraviolet light polymerization.
Consisting of of the liquid optical cement of the ultraviolet light polymerization that makes: (be average viscosity is 50000cps to urethane acrylate oligomer 55 grams, molecular-weight average is 50000, functionality is 1.5 urethane acrylate), (wherein dicyclo benzene oxygen ethyl propylene acid esters 10 restrains (methyl) acrylate 40 grams, isobornyl methacrylate 10 grams, hydroxyethyl methylacrylate 10 grams, Jia Jibingxisuanyizhi 10 grams), light trigger 2 grams (being Benzoin ethyl ether), silane coupling agent 2 grams (being vinyltriethoxysilane) and auxiliary agent 1 gram (being photostabilizer 2-(2 '-hydroxyl-3 ', the 5-di-tert-butyl-phenyl) benzotriazole).
Being equipped with raw material during batch process according to the above ratio gets final product.
Embodiment 6
In the present embodiment, the preparation method of the liquid optical cement of ultraviolet light polymerization comprises the steps: successively
(1) by weight, (being average viscosity is 20000cps to get 40 gram urethane acrylate oligomer, molecular-weight average is 10000, functionality is 1.5 urethane acrylate, this urethane acrylate is by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), (wherein Isooctyl methacrylate 20 restrains 40 gram (methyl) acrylate, diethylene glycol monoacrylate 10 grams, lauryl acrylate 5 grams, pentaerythritol triacrylate 5 grams), 3 gram light triggers (are 2,4,6-Three methyl Benzene formyl-diphenyl phosphine oxide), 10 gram silane coupling agents (being trimethoxy [2-(7-oxabicyclo [4.1.0] heptan-3-yl) ethyl] silane) and 7 restrain auxiliary agents (being plasticizer phthalic acid ester), and join cleaning, in the dry reaction vessel, be to be stirred under 1500 rev/mins the condition to mix (churning time is 35 minutes) then with the material low whipping speed in the reaction vessel, obtain sizing material;
(2) sizing material that step (1) is obtained with the vacuum defoamation machine carries out deaeration (the deaeration time is 22 minutes), obtains the liquid optical cement of ultraviolet light polymerization.
Consisting of of the liquid optical cement of the ultraviolet light polymerization that makes: (be average viscosity is 20000cps to urethane acrylate oligomer 40 grams, molecular-weight average is 10000, functionality is 1.5 urethane acrylate, this urethane acrylate is by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), (wherein Isooctyl methacrylate 20 restrains (methyl) acrylate 40 grams, diethylene glycol monoacrylate 10 grams, lauryl acrylate 5 grams, pentaerythritol triacrylate 5 grams), light trigger 3 grams (are 2,4,6-Three methyl Benzene formyl-diphenyl phosphine oxide), silane coupling agent 10 gram (being trimethoxy [2-(7-oxabicyclo [4.1.0] heptan-3-yl) ethyl] silane) and auxiliary agent 7 restrain (being plasticizer phthalic acid ester).
Being equipped with raw material during batch process according to the above ratio gets final product.
Embodiment 7
In the present embodiment, the preparation method of the liquid optical cement of ultraviolet light polymerization comprises the steps: successively
(1) by weight, (wherein average viscosity is 60000cps to get 50 gram urethane acrylate oligomer, molecular-weight average is 50000, functionality is 3 urethane acrylate 20 grams, average viscosity is 40000cps, molecular-weight average is 35000, functionality is 1.5 urethane acrylate 30 grams, these two kinds of urethane acrylates are by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), (wherein methacrylic acid undecyl ester 15 restrains 40 gram (methyl) acrylate, 2-cyclohexyl methacrylate 10 grams, dicyclo benzene oxygen ethyl propylene acid esters 10 grams, isobornyl methacrylate 5 grams), (wherein 2-hydroxyl-2-phenyl methyl phenyl ketone 2 restrains 3 gram light triggers, 2,4,6-Three methyl Benzene formyl-diphenyl phosphine oxide 1 gram), 1.8 gram silane coupling agent (being vinyltriethoxysilane) and 0.2 gram auxiliary agent (being the defoamer polydimethylsiloxane), and join cleaning, in the dry reaction vessel, be to be stirred under 1500 rev/mins the condition to mix (churning time is 35 minutes) then with the material low whipping speed in the reaction vessel, obtain sizing material;
(2) sizing material that step (1) is obtained with the vacuum defoamation machine carries out deaeration (the deaeration time is 30 minutes), obtains the liquid optical cement of ultraviolet light polymerization.
Consisting of of the liquid optical cement of the ultraviolet light polymerization that makes: (wherein average viscosity is 60000cps to urethane acrylate oligomer 50 grams, molecular-weight average is 50000, functionality is 3 urethane acrylate 20 grams, average viscosity is 40000cps, molecular-weight average is 35000, functionality is 1.5 urethane acrylate 30 grams, these two kinds of urethane acrylates are by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), (wherein methacrylic acid undecyl ester 15 restrains (methyl) acrylate 40 grams, 2-cyclohexyl methacrylate 10 grams, dicyclo benzene oxygen ethyl propylene acid esters 10 grams, isobornyl methacrylate 5 grams), (wherein 2-hydroxyl-2-phenyl methyl phenyl ketone 2 restrains light trigger 3 grams, 2,4,6-Three methyl Benzene formyl-diphenyl phosphine oxide, 1 gram), silane coupling agent 1.8 grams (being vinyltriethoxysilane) and auxiliary agent 0.2 gram (being the defoamer polydimethylsiloxane).
Being equipped with raw material during batch process according to the above ratio gets final product.
Embodiment 8
In the present embodiment, the preparation method of the liquid optical cement of ultraviolet light polymerization comprises the steps: successively
(1) by weight, (being average viscosity is 50000cps to get 50 gram urethane acrylate oligomer, molecular-weight average is 50000, functionality is 1.5 urethane acrylate, this urethane acrylate is by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), (wherein lauryl methacrylate(LMA) 20 restrains 40 gram (methyl) acrylate, hydroxyethyl methylacrylate 15 grams, 1,6-glycol diacrylate 5 grams), 2 gram light triggers (being Benzoin ethyl ether), 2 gram silane coupling agents (being vinyltriethoxysilane) and 1 restrain auxiliary agent (photostabilizer 1-methyl-8-(1 wherein, 2,2,6,6-pentamethyl--4-piperidines) sebate 0.5 gram, plasticizer phthalic acid ester 0.5 gram), and join cleaning, in the dry reaction vessel, be to be stirred under 1400 rev/mins the condition to mix (churning time is 45 minutes) then with the material low whipping speed in the reaction vessel, obtain sizing material;
(2) sizing material that step (1) is obtained with the vacuum defoamation machine carries out deaeration (the deaeration time is 20-30 minute), obtains the liquid optical cement of ultraviolet light polymerization.
Consisting of of the liquid optical cement of the ultraviolet light polymerization that makes: (be average viscosity is 50000cps to urethane acrylate oligomer 50 grams, molecular-weight average is 50000, functionality is 1.5 urethane acrylate, this urethane acrylate is by long-chain polyhydric alcohol, monomer and the Acrylic Acid Monomer copolymerization of band isocyanide ester base form), (wherein lauryl methacrylate(LMA) 20 restrains (methyl) acrylate 40 grams, hydroxyethyl methylacrylate 15 grams, 1,6-glycol diacrylate 5 grams), light trigger 2 grams (being Benzoin ethyl ether), silane coupling agent 2 gram (being vinyltriethoxysilane) and auxiliary agent 1 restrain (photostabilizer 1-methyl-8-(1 wherein, 2,2,6,6-pentamethyl--4-piperidines) sebate 0.5 gram, plasticizer phthalic acid ester 0.5 gram).
Being equipped with raw material during batch process according to the above ratio gets final product.
The performance of the liquid optical cement of the ultraviolet light polymerization that above-described embodiment 1-8 is obtained is tested, and wherein: refraction index test uses Abbe refractometer, specific refractory power before and after test is solidified; Shao Shi A type hardness tester meter is used in hardness test, the test cured glue water hardness; Tension testing machine is used in cohesive strength test (comprise glass to glass, glass to polaroid), and concrete grammar is according to ISO 4587; Transmission measurement uses spectrophotometer, and the test wavelength is the transmitance of the light of 380nm-780nm; Young's modulus uses dynamic mechanical analysis instrument (DMA) to test; The weather resisteant test is placed 500h and is observed performance variation ((sign *) represents that namely weather resisteant is poor if mist is sent out in water inlet, if good weatherability is namely represented in no considerable change (indicating zero)) under 85 ℃/90%RH condition.Test performance is as shown in table 1:
Table 1
As can be seen from the above table, the liquid optical cement of the ultraviolet light polymerization of embodiment 1-8 has good weathering resistance, lower Young's modulus, and its optical property (specific refractory power, transmitance) all satisfies touch-screen and mounts service requirements.Embodiment 1,4,6, the liquid optical cement of 7 ultraviolet light polymerization, cohesive strength 〉=1.8MPa, hardness lower (≤25) between glass can satisfy the bonding of touch-screen cover plate camera lens well.Embodiment 2,3,5, the liquid optical cement of 8 ultraviolet light polymerization, cohesive strength＞0.2MPa, hardness extremely low (≤15) between glass and polaroid meet the direct bonding requirement of touch-screen display module and glass.
In sum, ultraviolet photo-curing cementing agent provided by the invention has characteristics such as viscosity is adjustable, specific refractory power is high, hardness is low, internal stress is little, cohesiveness is good, weathering resistance is good, can satisfy the bonding of touch-screen cover plate camera lens and two kinds of service requirementss of direct bonding of display module.Simultaneously, the rete of having avoided present liquid optical cement to exist is crisp firmly, cohesive strength weak, pliability is low, and problems such as weathering resistance difference have certain market competition advantage.
Claims (10)
1. the liquid optical cement of a ultraviolet light polymerization, it is characterized in that being formed by following components in weight percentage: urethane acrylate oligomer 40-70 part, (methyl) acrylate 20-40 part, light trigger 0.1-5 part, silane coupling agent 1-10 part, auxiliary agent 0-10 part.
2. the liquid optical cement of ultraviolet light polymerization according to claim 1, it is characterized in that: described urethane acrylate oligomer is that average viscosity is that 20000-70000cps, molecular-weight average are that 10000-50000, functionality are the urethane acrylate of 1-3.
3. the liquid optical cement of ultraviolet light polymerization according to claim 1, it is characterized in that: described (methyl) acrylate is Hydroxyethyl acrylate, hydroxyethyl methylacrylate, 4-hydroxybutyl acrylate, vinylformic acid-2-hydroxypropyl acrylate, Rocryl 410,2-hydroxyl-2-butyl acrylate cores, 1,4-cyclohexanedimethanol mono acrylic ester, 1,4-cyclohexanedimethanol methacrylic ester, 1-chloro-2-hydroxypropyl acrylate, 1-chloro-2-hydroxypropylmethyl acrylate, diethylene glycol monoacrylate, the glycol ether methyl acrylate, 1, the 6-hexanediol monoacrylate, 1,6 hexanediol diacrylate, pentaerythritol triacrylate, dipentaerythritol five acrylate, the TriMethylolPropane(TMP) dimethacrylate, isobornyl acrylate, isobornyl methacrylate, the cyclopentyl acrylate, the cyclopentyl methyl acrylate, 2-vinylformic acid cyclohexyl ester, the 2-cyclohexyl methacrylate, dicyclo benzene oxygen ethyl propylene acid esters, methyl acrylate, ethyl propenoate, Jia Jibingxisuanyizhi, propyl acrylate, propyl group-2-methyl-2-acrylate, isopropyl acrylate, n-BMA, n-butyl acrylate, the methacrylic tert-butyl acrylate, isobutyl acrylate, Propenoic acid, 2-methyl, isobutyl ester, the vinylformic acid n-pentyl ester, the methacrylic acid pentyl ester, the vinylformic acid n-octyl, Isooctyl acrylate monomer, Isooctyl methacrylate, decyl acrylate, decyl-octyl methacrylate, methacrylic acid undecyl ester, the 2-dodecylacrylate, a kind of in lauryl acrylate and the lauryl methacrylate(LMA) or wherein multiple combination.
4. the liquid optical cement of ultraviolet light polymerization according to claim 1; it is characterized in that: described light trigger is the tetraethyl-michaelis ketone; benzophenone; 1-hydroxy-cyclohexyl phenyl ketone; the acrylate benzophenone; phenyl benzophenone; dihydroxy benaophenonel; 4; 4'-two (N; the N-dimethylamino) benzophenone; 2; the 2'-diethoxy acetophenone; 2-hydroxyl-2-phenyl methyl phenyl ketone; 2-hydroxy-2-methyl-1-phenyl-1-acetone; 2; 4; 6-Three methyl Benzene formyl-diphenyl phosphine oxide; two (2; 4,6-trimethylbenzoyl) phenyl phosphine oxide; benzoin methyl ether; a kind of in Benzoin ethyl ether and the cyanuric chloride or wherein multiple combination.
5. the liquid optical cement of ultraviolet light polymerization according to claim 1, it is characterized in that: described silane coupling agent is the trimethoxy silicomethane, vinyltriethoxysilane, 3-Trimethoxy silane vinylformic acid third fat, the 3-methyl allyl acyloxypropyl trimethoxysilane, 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane, 3-[(2,3)-epoxy third oxygen] the propyl group methyl dimethoxysilane, trimethoxy [2-(7-oxabicyclo [4.1.0] heptan-3-yl) ethyl] silane, a kind of in 3-TSL 8330 and the 3-r-chloropropyl trimethoxyl silane or wherein multiple combination.
6. the liquid optical cement of ultraviolet light polymerization according to claim 1 is characterized in that: described auxiliary agent is a kind of in softening agent, defoamer and the photostabilizer or combination that it is multiple.
7. the liquid optical cement of ultraviolet light polymerization according to claim 6 is characterized in that: described softening agent is a kind of in phthalic ester, phosphoric acid ester, alkyl sulfonic ester, fatty group dibasic acid, benzene polyacid ester and the epoxy compounds or wherein multiple combination.
8. the liquid optical cement of ultraviolet light polymerization according to claim 6 is characterized in that: described defoamer is a kind of in tributyl phosphate, polydimethylsiloxane, polyacrylic ester and the polyethers or wherein multiple combination.
9. the liquid optical cement of ultraviolet light polymerization according to claim 6, it is characterized in that: described photostabilizer is two (1,2,2,6,6-pentamethyl--4-piperidines) sebate, 1-methyl-8-(1,2,2,6,6-pentamethyl--4-piperidines) sebate, 4-hydroxyl-2,2,6,6-tetramethyl--1-piperidines alcohol, two (3,5-di-tert-butyl-4-hydroxyl benzyl monoethyl phosphate) nickel, 2-(2 '-hydroxyl-3 ', 5-di-tert-butyl-phenyl) a kind of in benzotriazole and 2-hydroxyl-two ketones of 4-n-octyloxy or wherein multiple combination.
10. the preparation method of the liquid optical cement of each described ultraviolet light polymerization of claim 1-9 is characterized in that comprising the steps: successively
(1) by weight, get 40-70 part urethane acrylate oligomer, 20-40 part (methyl) acrylate, 0.1-5 part light trigger, 1-10 part silane coupling agent and 0-10 part auxiliary agent, and join in the reaction vessel of cleaning, drying, be to be stirred under 1000-1500 rev/min the condition to mix then with the material low whipping speed in the reaction vessel, obtain sizing material;
(2) with the vacuum defoamation machine sizing material that step (1) obtains is carried out deaeration, obtain the liquid optical cement of ultraviolet light polymerization.
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