WO2021035910A1 - Organic silicone adhesive specifically used for display bonding and preparation method thereof - Google Patents
Organic silicone adhesive specifically used for display bonding and preparation method thereof Download PDFInfo
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- WO2021035910A1 WO2021035910A1 PCT/CN2019/112268 CN2019112268W WO2021035910A1 WO 2021035910 A1 WO2021035910 A1 WO 2021035910A1 CN 2019112268 W CN2019112268 W CN 2019112268W WO 2021035910 A1 WO2021035910 A1 WO 2021035910A1
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- Prior art keywords
- parts
- silicone oil
- adhesive
- vinyl
- acrylate
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- 239000013464 silicone adhesive Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 229920002545 silicone oil Polymers 0.000 claims abstract description 62
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 39
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 39
- -1 phenyl-vinyl Chemical group 0.000 claims abstract description 35
- 239000000853 adhesive Substances 0.000 claims abstract description 30
- 230000001070 adhesive effect Effects 0.000 claims abstract description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000001257 hydrogen Substances 0.000 claims abstract description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 22
- 229920002050 silicone resin Polymers 0.000 claims abstract description 20
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 17
- 238000010030 laminating Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000011261 inert gas Substances 0.000 claims description 13
- 239000000741 silica gel Substances 0.000 claims description 13
- 229910002027 silica gel Inorganic materials 0.000 claims description 13
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- BPCZRRZEJCLZEW-UHFFFAOYSA-N 4-tert-butyl-1-ethynylcyclohexan-1-ol Chemical compound CC(C)(C)C1CCC(O)(C#C)CC1 BPCZRRZEJCLZEW-UHFFFAOYSA-N 0.000 claims description 4
- KDSZHLCFSYQMCH-UHFFFAOYSA-N 1-ethynylcyclobutan-1-amine Chemical compound C#CC1(N)CCC1 KDSZHLCFSYQMCH-UHFFFAOYSA-N 0.000 claims description 3
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 3
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- KNVOCSQDAIHOPP-UHFFFAOYSA-N 2-ethynylcyclohexan-1-ol Chemical compound OC1CCCCC1C#C KNVOCSQDAIHOPP-UHFFFAOYSA-N 0.000 claims description 2
- JRZIIUSKYKGRDH-UHFFFAOYSA-N 2-ethynylcyclopentan-1-ol Chemical compound OC1CCCC1C#C JRZIIUSKYKGRDH-UHFFFAOYSA-N 0.000 claims description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 2
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 claims description 2
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 2
- GTTSNKDQDACYLV-UHFFFAOYSA-N Trihydroxybutane Chemical compound CCCC(O)(O)O GTTSNKDQDACYLV-UHFFFAOYSA-N 0.000 claims description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 229940125782 compound 2 Drugs 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 125000003944 tolyl group Chemical group 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- VDIHFNQRHGYISG-UHFFFAOYSA-N cyclopentylbenzene Chemical compound C1CCCC1C1=CC=CC=C1 VDIHFNQRHGYISG-UHFFFAOYSA-N 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 239000004973 liquid crystal related substance Substances 0.000 abstract description 10
- 239000000758 substrate Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 238000000465 moulding Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 18
- 239000011521 glass Substances 0.000 description 6
- 239000003292 glue Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000001960 triggered effect Effects 0.000 description 2
- WREBXCVYHWKUML-UHFFFAOYSA-N 1-cyclopropyl-4-ethynylbenzene Chemical compound C1=CC(C#C)=CC=C1C1CC1 WREBXCVYHWKUML-UHFFFAOYSA-N 0.000 description 1
- PZZDCCHJBAKHRD-UHFFFAOYSA-N 2-(trihydroxymethyl)prop-2-enoic acid Chemical compound OC(=O)C(=C)C(O)(O)O PZZDCCHJBAKHRD-UHFFFAOYSA-N 0.000 description 1
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- 206010025421 Macule Diseases 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- QPMJENKZJUFOON-PLNGDYQASA-N ethyl (z)-3-chloro-2-cyano-4,4,4-trifluorobut-2-enoate Chemical compound CCOC(=O)C(\C#N)=C(/Cl)C(F)(F)F QPMJENKZJUFOON-PLNGDYQASA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008855 peristalsis Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- 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
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Definitions
- the invention relates to the technical field of display laminating, in particular to a special organic silicone adhesive for display laminating and a preparation method thereof.
- Laminating means bonding the liquid crystal display to the touch screen or protective glass with optical glue.
- the different bonding methods it can be divided into frame bonding and full bonding.
- the so-called frame sticker is simply to fix the touch screen and the four sides of the liquid crystal display with double-sided tape, but there is an air layer in the middle of this bonding method, which causes the display effect to be greatly reduced after the light is refracted.
- Fully lamination and ready-to-use glue will completely glue the touch screen or protective glass with the LCD in a seamless way. Compared with frame fitting, it can provide better display effect. There is no air between the screens, which helps to reduce the reflection between the display and the glass, which can make the screen look more transparent and enhance the display effect of the screen.
- the touch module is closely integrated with the display to increase the strength.
- the full bonding can effectively reduce the interference of the display panel noise on the touch signal.
- the traditional method of laminating industry is to use OCA sheet optical glue, which is prone to produce some defects, such as bubbles, foreign objects, etc., and the production yield is low; it is difficult to rework unqualified products after laminating, or even cannot be reworked; in addition, traditional production
- the operation method mainly relies on manpower to transport between the stations, the low production efficiency, high manpower cost and other issues have greatly affected the production efficiency.
- Another bonding material is UV glue, which is cured by ultraviolet light, which is prone to macula, and the edge glue is not easy to dry. As a result, the above two adhesives cannot be applied to the full bonding of liquid crystal displays, especially for large and medium-sized displays.
- the purpose of the present invention is to provide a special organic silicone adhesive for display laminating and a preparation method thereof in order to solve the above-mentioned problems.
- a special organic silicone adhesive for display laminating which contains the following components in parts by weight:
- the vinyl-terminated silicone oil is divinyl-terminated polydimethylsiloxane with a viscosity of 400-2000 cps. The higher the viscosity, the lower the vinyl content. When the vinyl content is low, the cross-linking density will be small and the mechanical properties of the adhesive will deviate; and the high vinyl content will cause the cross-linking density to be too high. Elongation and heat resistance and aging resistance become worse.
- the ratio of vinyl-terminated silicone oil defined in the present invention has a suitable vinyl content, which not only ensures the mechanical properties of the adhesive, but also ensures the elongation and heat resistance. Anti-aging performance.
- the vinyl silicone resin is an active siloxane prepolymer with a high-strength cross-linked structure, which can effectively improve the mechanical properties of the adhesive, and its chain link structure is:
- the phenyl vinyl silicone oil is vinyl terminated methyl phenyl polysiloxane.
- the introduction of bulky phenyl side groups in the silicone adhesive will hinder the movement of macromolecules, and the friction in the molecular chain will increase with the increase of benzene.
- the tensile strength of the silicone adhesive is enhanced, so the introduction of a proper amount of phenyl in the silicone adhesive can effectively improve the mechanical properties such as tensile strength and tear strength, and it has a wider temperature range of use, as well as aging resistance. performance.
- the molecular formula of the hydrogen-containing silicone oil is:
- the active hydrogen atoms at both ends of the molecular chain of the hydrogen-containing silicone oil of the present invention can double the molecular chain during the gel forming process, and at the same time increase the bridge bonds between the molecular chains, resulting in the flexibility and physical machinery of the network structure of the adhesive
- the performance has been significantly improved, which can play a better role in reinforcement.
- the amount of hydrogen-containing silicone oil in different amounts has a greater impact on the properties of the adhesive.
- Too little hydrogen-containing silicone oil is not enough to fully crosslink with vinyl silicone oil, resulting in low tensile strength and elongation at break of the silicone adhesive, which cannot meet the actual use requirements; excessive hydrogen-containing silicone oil will cause excessive cross-linking , Which makes the adhesive too hard and too many cross-linking points, which restricts the peristalsis, transfer and rotation of the internal molecular chains and chain segments of the material, resulting in a decrease in the mechanical properties of the adhesive. Only when the amount of hydrogen-containing silicone oil is within a certain range can the adhesive have better performance, and the range defined by the present invention can ensure that the product has better performance.
- the ethynyl compound is selected from the group consisting of ethynyl cycloethanol, 1-ethynyl cyclobutylamine, 4-ethynyl cyclopropphenyl 1-ethynyl cyclopentyl benzene, 2-ethynyl cyclohexanol, 2-ethynyl cyclopentanol , One or more of 1-ethynylcyclohexanol or 4-tert-butyl-1-ethynylcyclohexanol.
- the platinum catalyst is a chloroplatinic acid-tetramethyldivinyldisiloxane complex.
- the acrylic compound is a (meth)acrylate compound, selected from methyl (meth)acrylate, ethyl (meth)acrylate, butyl (meth)acrylate, and glycidyl (meth)acrylate , Any one of ⁇ -methacryloxypropyl trimethoxysilane, hydroxyethyl (meth)acrylate or trihydroxymethacrylate.
- the organic silicone adhesive of the present invention has small shrinkage, excellent mechanical properties, and convenient molding. It is an excellent special material for modern liquid crystal displays and is widely used in the fields of electronics and electrical, automobiles, and medical treatment.
- the organic silicone adhesive of the present invention can recover the liquid crystal display and the substrate through a simple method, so that the adhesive can be applied to a large-size display device, and the cost is saved.
- 600cps-terminated vinyl silicone oil 25 parts, vinyl silicone resin 5 parts, hydrogen-containing silicone oil 25 parts, ethynyl cycloethanol 2 parts, (meth)ethyl acrylate 1 part add to the reaction device under the protection of inert gas, and heat to 60°C, 0.003 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 30 minutes, and cool to room temperature to obtain a colorless and transparent liquid, depress the air bubbles, and heat and solidify at 80°C Heating for 25 minutes, the organic silica gel adhesive is prepared.
- Comparative example 2 (containing 2 parts of phenyl vinyl silicone oil)
- 600cps-terminated vinyl silicone oil 25 parts, vinyl silicone resin 5 parts, hydrogen-containing silicone oil 25 parts, phenyl vinyl silicone oil 2 parts, ethynyl cycloethanol 2 parts, (meth)acrylate 1 part, under inert gas protection Add it to the reaction device, heat to 60°C, 0.003 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 30 minutes, and cool to room temperature to obtain a colorless and transparent liquid, which is removed under reduced pressure The air bubbles are heated and cured at 80° C. and heated for 25 minutes to obtain the organic silica gel adhesive.
- Comparative example 3 (containing 5 parts of phenyl vinyl silicone oil)
- 600cps-terminated vinyl silicone oil 25 parts, vinyl silicone resin 5 parts, hydrogen-containing silicone oil 25 parts, phenyl vinyl silicone oil 5 parts, ethynyl cycloethanol 2 parts, (meth)acrylate 1 part, under inert gas protection Add it to the reaction device, heat to 60°C, 0.003 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 30 minutes, and cool to room temperature to obtain a colorless and transparent liquid, which is removed under reduced pressure The air bubbles are heated and cured at 80° C. and heated for 25 minutes to obtain the organic silica gel adhesive.
- Performance comparison test example performance test of organic silicone adhesive after curing
- Example 1 no Colorless and transparent 2.715 294
- Example 2 no Colorless and transparent 3.497 335
- Example 3 no Colorless and transparent 2.89 345
- Example 4 no Colorless and transparent 3.578 330
- Example 5 no Colorless and transparent 3.411 367
- Example 6 no Colorless and transparent 2.917 354 Comparative example 1 no Colorless and transparent 0.618 211 Comparative example 2 no Colorless and transparent 1.212 232 Comparative example 3 no Colorless and transparent 1.578 200 Comparative example 4 no Colorless and transparent 3.32 234 Comparative example 5 no Colorless and transparent 3.222 245 Comparative example 6 no Colorless and transparent 3.342 219
- the colorless and transparent liquid obtained in the above example is reduced under reduced pressure to remove bubbles, and a small amount of colorless and transparent liquid is applied to a glass plate of 10cm in length, 5cm in width and 2mm in thickness.
- the thickness is 0.5mm, and then another glass plate of the same size is overlapped, then heated to 60°C, taken out after 20 minutes, cooled to room temperature to solidify, and tested by a tensile machine.
- Table 2 The test results are shown in Table 2 below:
- Example 2 Colorless and transparent 33 no Example 3 Colorless and transparent 35 no Example 4 Colorless and transparent 34 no Example 5 Colorless and transparent 32 no Example 6 Colorless and transparent 34 no Comparative example 1 Colorless and transparent 18 no Comparative example 2 Colorless and transparent 26 no Comparative example 3 Colorless and transparent 28 no Comparative example 4 Colorless and transparent 16 no Comparative example 5 Colorless and transparent 18 no Comparative example 6 Colorless and transparent 17 no
- phenyl vinyl silicone oil has a very obvious effect on its tensile strength and elongation at break.
- the bulky phenyl has high steric hindrance, and the friction between molecules also increases.
- the loss factor is increased, and the tensile strength of silicone is generally increased, and the elongation at break is long.
- Excessive phenyl vinyl silicone oil causes the molecules to become brittle, the tensile strength decreases, and the elongation at break becomes shorter.
- vinyl silicone resin has a significant effect on improving the adhesion of silicone adhesives.
Abstract
The invention relates to a organic silicone adhesive specifically used for display bonding and a preparation method thereof. The composition comprises the following components in parts by weight: 25-50 parts of a 400-2000 cps vinyl-terminated silicone oil; 5-10 parts of a vinyl silicone resin; 0.1 to 1 part of a phenyl-vinyl silicone oil; 25 to 35 parts of a hydrogen-containing silicone oil; 2 to 4 parts of an ethynyl compound; 0.001 to 0.005 parts of a platinum catalyst; and 1 to 5 parts of an acrylic compound. The organic silicone adhesive of the present invention has low shrinkage, excellent mechanical properties, and convenient molding, and serves as an excellent special-use bonding material for modern liquid crystal displays. The organic silicone adhesive can be widely used in the fields of electronics, automobiles, medical treatment, etc. The organic silicone adhesive allows the use of simple methods to recycle liquid crystal displays and substrates, making the application of the adhesive to large-size display devices possible, and also saving costs.
Description
本发明涉及显示器贴合技术领域，尤其是涉及一种显示器贴合专用有机硅胶黏剂及其制备方法。The invention relates to the technical field of display laminating, in particular to a special organic silicone adhesive for display laminating and a preparation method thereof.
进入21世纪以来，液晶显示器己全面取代阴极射线显像管，在显示界面越来越优质的情况下，液晶显示器本身重量大幅下降，体积亦大幅下降的情况下，使用者对于液晶显示器的使用要求也越也越高。特别是智能手机的兴起，苹果手机的创新掀起的触控潮，直接引发了贴合技术的发展。贴合意指将液晶显示器与触摸屏或是保护玻璃用光学胶贴合。Since the beginning of the 21st century, liquid crystal displays have completely replaced cathode-ray picture tubes. With the display interface becoming more and more high-quality, the weight of the liquid crystal display itself has been greatly reduced, and the size of the liquid crystal display has also been greatly reduced. Also higher. In particular, the rise of smart phones and the touch wave triggered by the innovation of Apple mobile phones directly triggered the development of bonding technology. Laminating means bonding the liquid crystal display to the touch screen or protective glass with optical glue.
按贴合方式的不同，可以分为框贴和全贴合。所谓框贴就是简单的以双面胶将触控屏和液晶显示器的四边固定，但是这种贴合方式中间存在着空气层，在光线折射后导致显示效果大打折扣。全贴合即用胶水将触摸屏或保护玻璃与液晶显示器无缝隙的方式完全黏在一起。较于框贴合，它可以提供更好的显示效果。屏幕之间无空气，这有助于减少显示器与玻璃之间的反光，可以让屏幕看起来更加通透，增强屏幕的显示效果。另外触控模块也因为与显示器紧密结合让强度有所提升，除此之外，全贴合更能有效降低显示面板噪声对触控讯号所造成的干扰。According to the different bonding methods, it can be divided into frame bonding and full bonding. The so-called frame sticker is simply to fix the touch screen and the four sides of the liquid crystal display with double-sided tape, but there is an air layer in the middle of this bonding method, which causes the display effect to be greatly reduced after the light is refracted. Fully lamination and ready-to-use glue will completely glue the touch screen or protective glass with the LCD in a seamless way. Compared with frame fitting, it can provide better display effect. There is no air between the screens, which helps to reduce the reflection between the display and the glass, which can make the screen look more transparent and enhance the display effect of the screen. In addition, the touch module is closely integrated with the display to increase the strength. In addition, the full bonding can effectively reduce the interference of the display panel noise on the touch signal.
传统的贴合作业方式是用OCA片材光学胶，易产生一些不良，如气泡，异物等，生产良率较低；贴合后的不合格品返工困难，甚至不能返工；另外，传统的生产作业方式主要靠人力在各工站间的搬运，生产效率低下，人力成本过高等问题己经极大地影响了生产效益。另一种贴合材料就是UV胶，它采用紫外光固化，容易出现黄斑，边缘胶水不易干燥等问题。这样就造成以上两种胶黏剂不能很好的应用在 液晶显示器的全贴合上，尤其是对于中大尺寸的显示器。The traditional method of laminating industry is to use OCA sheet optical glue, which is prone to produce some defects, such as bubbles, foreign objects, etc., and the production yield is low; it is difficult to rework unqualified products after laminating, or even cannot be reworked; in addition, traditional production The operation method mainly relies on manpower to transport between the stations, the low production efficiency, high manpower cost and other issues have greatly affected the production efficiency. Another bonding material is UV glue, which is cured by ultraviolet light, which is prone to macula, and the edge glue is not easy to dry. As a result, the above two adhesives cannot be applied to the full bonding of liquid crystal displays, especially for large and medium-sized displays.
因此，设计并研究出新的显示器贴合专用的胶黏剂不仅可以达到优化性能，降低成本，减少工艺等，而且对目前市场的最新需求具有重要的意义。Therefore, the design and research of a new special adhesive for display bonding can not only achieve optimized performance, reduce costs, and reduce processes, but also have important significance for the latest needs of the current market.
发明内容Summary of the invention
本发明的目的就是为了解决上述问题而提供一种显示器贴合专用有机硅胶黏剂及其制备方法。The purpose of the present invention is to provide a special organic silicone adhesive for display laminating and a preparation method thereof in order to solve the above-mentioned problems.
本发明的目的通过以下技术方案实现：The purpose of the present invention is achieved through the following technical solutions:
一种显示器贴合专用有机硅胶黏剂，以重量份计包含下述组分：A special organic silicone adhesive for display laminating, which contains the following components in parts by weight:
所述端乙烯基硅油为双乙烯基端封的聚二甲基硅氧烷，粘度为400～2000cps。粘度越大，乙烯基含量越低，参与的乙烯基含量较低时，会导致交联密度小，胶黏剂的机械性能偏差；而乙烯基含量偏高时，会导致交联密度过大，伸长率及耐热耐老化性能变差，本发明所限定的端乙烯基硅油的配比具有合适的乙烯基含量，即保证了胶黏剂的机械性能，又保证了伸长率及耐热耐老化性能。The vinyl-terminated silicone oil is divinyl-terminated polydimethylsiloxane with a viscosity of 400-2000 cps. The higher the viscosity, the lower the vinyl content. When the vinyl content is low, the cross-linking density will be small and the mechanical properties of the adhesive will deviate; and the high vinyl content will cause the cross-linking density to be too high. Elongation and heat resistance and aging resistance become worse. The ratio of vinyl-terminated silicone oil defined in the present invention has a suitable vinyl content, which not only ensures the mechanical properties of the adhesive, but also ensures the elongation and heat resistance. Anti-aging performance.
所述乙烯基硅树脂为具有高强度交联结构的活性硅氧烷预聚体，能有效地提高胶黏剂的力学性能，其链节结构为：The vinyl silicone resin is an active siloxane prepolymer with a high-strength cross-linked structure, which can effectively improve the mechanical properties of the adhesive, and its chain link structure is:
所述苯基乙烯基硅油为乙烯基端封的甲基苯基聚硅氧烷，在有机硅胶黏剂中引入大体积的苯基侧基会阻碍大分子运动，分子链内磨擦加剧随着苯基含量的增大，在外力作用造成形变过程中分子链沿剪切方向运动时，大体积的苯基有更高的位阻，分子间的摩檫也随之增加，会导致损耗因子增大，有机硅胶黏剂的拉伸强度增强，因此在有机硅胶黏剂中引入适量的苯基能有效地提高拉伸强度、撕裂强度等力学性能和其具有更宽的使用温度范围，以及耐老化性能。The phenyl vinyl silicone oil is vinyl terminated methyl phenyl polysiloxane. The introduction of bulky phenyl side groups in the silicone adhesive will hinder the movement of macromolecules, and the friction in the molecular chain will increase with the increase of benzene. The increase of the base content, when the molecular chain moves in the shear direction during the deformation process caused by the external force, the bulky phenyl group has higher steric hindrance, and the friction between the molecules also increases, which will cause the loss factor to increase. , The tensile strength of the silicone adhesive is enhanced, so the introduction of a proper amount of phenyl in the silicone adhesive can effectively improve the mechanical properties such as tensile strength and tear strength, and it has a wider temperature range of use, as well as aging resistance. performance.
所述含氢硅油的分子式为：The molecular formula of the hydrogen-containing silicone oil is:
本发明含氢硅油分子链两端的活性氢原子在成胶过程中可以使分子链成倍增长，同时使分子链间的桥键得到增长，致使胶黏剂的网状结构的柔顺性和物理机械性能得到明显提高，因而能起到更好的补强作用。不同用量的含氢硅油的用量对胶黏剂性能有较大的影响。含氢硅油太少，则不足以与乙烯基硅油充分交联，导致有机硅胶黏剂的拉伸强度、断裂伸长率较小，不能满足实际使用需求；含氢硅油过量，则交联多度，使得胶黏剂过硬，交联结点过多，从而限制了材料内部分子链、链段的蠕动、转移和旋转，导致胶黏剂的力学性能有所降低。只有当含氢硅油的用量在一定的范围内，才能使胶黏剂具有较好的性能，本发明所限定的范围可保证产品具有较好的性能。The active hydrogen atoms at both ends of the molecular chain of the hydrogen-containing silicone oil of the present invention can double the molecular chain during the gel forming process, and at the same time increase the bridge bonds between the molecular chains, resulting in the flexibility and physical machinery of the network structure of the adhesive The performance has been significantly improved, which can play a better role in reinforcement. The amount of hydrogen-containing silicone oil in different amounts has a greater impact on the properties of the adhesive. Too little hydrogen-containing silicone oil is not enough to fully crosslink with vinyl silicone oil, resulting in low tensile strength and elongation at break of the silicone adhesive, which cannot meet the actual use requirements; excessive hydrogen-containing silicone oil will cause excessive cross-linking , Which makes the adhesive too hard and too many cross-linking points, which restricts the peristalsis, transfer and rotation of the internal molecular chains and chain segments of the material, resulting in a decrease in the mechanical properties of the adhesive. Only when the amount of hydrogen-containing silicone oil is within a certain range can the adhesive have better performance, and the range defined by the present invention can ensure that the product has better performance.
所述乙炔基化合物选自乙炔基环乙醇、1-乙炔基环丁胺、4-乙炔基环丙苯1-乙炔环戊基苯、2-乙炔基环己醇、2-乙炔基环戊醇、1-乙 炔基环己醇或4-叔丁基-1-乙炔基环己醇中的一种或几种。The ethynyl compound is selected from the group consisting of ethynyl cycloethanol, 1-ethynyl cyclobutylamine, 4-ethynyl cyclopropphenyl 1-ethynyl cyclopentyl benzene, 2-ethynyl cyclohexanol, 2-ethynyl cyclopentanol , One or more of 1-ethynylcyclohexanol or 4-tert-butyl-1-ethynylcyclohexanol.
所述铂催化剂为氯铂酸-四甲基二乙烯基二硅氧烷络合物。The platinum catalyst is a chloroplatinic acid-tetramethyldivinyldisiloxane complex.
所述丙烯酸酯类化合物为(甲基)丙烯酸酯类化合物，选自(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸缩水甘油酯、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、(甲基)丙烯酸羟乙酯或三羟基甲基丙烷烯酸酯的任一种。The acrylic compound is a (meth)acrylate compound, selected from methyl (meth)acrylate, ethyl (meth)acrylate, butyl (meth)acrylate, and glycidyl (meth)acrylate , Any one of γ-methacryloxypropyl trimethoxysilane, hydroxyethyl (meth)acrylate or trihydroxymethacrylate.
所述的显示器贴合专用有机硅胶黏剂的制备方法，步骤如下：The preparation method of the special organic silicone adhesive for display laminating, the steps are as follows:
以重量份计称取：400～2000cps的端乙烯基硅油25～50份，乙烯基硅树脂5～10份，苯基乙烯基硅油0.1～1份，含氢硅油25～35份，乙炔基化合物2～4份，丙烯酸酯类化合物1～5份，在惰性气体保护下加入反应装置中，加热至40～60℃，加入铂催化剂0.001～0.005份，继续搅拌20～30分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在40～80℃下加热固化加热20～40分钟，即制得有机硅胶黏剂。Weigh in parts by weight: 400-2000cps of 25-50 parts of vinyl-terminated silicone oil, 5-10 parts of vinyl silicone resin, 0.1-1 part of phenyl vinyl silicone oil, 25-35 parts of hydrogen-containing silicone oil, ethynyl compound 2 to 4 parts, 1 to 5 parts of acrylate compounds, add to the reaction device under the protection of inert gas, heat to 40-60°C, add 0.001 to 0.005 parts of platinum catalyst, continue to stir for 20-30 minutes, and cool to room temperature. The colorless transparent liquid is obtained, the bubbles are removed under reduced pressure, and the organic silica gel adhesive is prepared by heating and curing at 40-80 DEG C for 20-40 minutes.
在使用过程中按照一定的质量比混合均匀后，脱泡，涂覆于基材上面，然后在60～80℃下加热固化30～40分钟，然后将涂覆了胶黏剂的基材通过正压将基材和液晶显示屏贴合在一起。In the process of use, after mixing uniformly according to a certain mass ratio, defoaming, coating on the substrate, and then heating and curing at 60 ~ 80 ℃ for 30 ~ 40 minutes, and then the adhesive coated substrate through the positive Press to bond the substrate and the LCD screen together.
与现有技术相比，本发明的有机硅胶黏剂具有收缩率小、机械性能优异、成型方便，是现代液晶显示器优良的贴合专用材料，在电子电气、汽车、医疗等领域广泛使用。本发明的有机硅胶黏剂能够通过简便的方法便得以回收液晶显示器和基材，使得这种胶黏剂能够应用于大尺寸的显示设备上成为可能，节约成本。Compared with the prior art, the organic silicone adhesive of the present invention has small shrinkage, excellent mechanical properties, and convenient molding. It is an excellent special material for modern liquid crystal displays and is widely used in the fields of electronics and electrical, automobiles, and medical treatment. The organic silicone adhesive of the present invention can recover the liquid crystal display and the substrate through a simple method, so that the adhesive can be applied to a large-size display device, and the cost is saved.
下面结合具体实施例对本发明进行详细说明，但绝不是对本发明的限制(以下各实施例中，各种原料每质量份均为1克)。The present invention will be described in detail below in conjunction with specific examples, but it is by no means a limitation of the present invention (in the following examples, each part of various raw materials is 1 gram).
实施例1Example 1
2000cps端乙烯基硅油25份，乙烯基硅树脂5份，苯基乙烯基硅油0.1份，含氢硅油25份，乙炔基环乙醇2份，(甲基)丙烯酸乙酯 1份，在惰性气体保护下加入反应装置中，加热至40℃，氯铂酸-四甲基二乙烯基二硅氧烷络合物0.001份，继续搅拌30分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在60℃下加热固化加热30分钟，即制得所述有机硅胶黏剂。2000cps 25 parts of vinyl silicone oil, 5 parts of vinyl silicone resin, 0.1 part of phenyl vinyl silicone oil, 25 parts of hydrogen-containing silicone oil, 2 parts of ethynyl cycloethanol, 1 part of ethyl (meth)acrylate, under inert gas protection Add it to the reaction device, heat to 40°C, 0.001 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 30 minutes, and cool to room temperature to obtain a colorless and transparent liquid, which is removed under reduced pressure The air bubbles are heated and cured at 60° C. for 30 minutes to prepare the organic silicone adhesive.
实施例2Example 2
980cps端乙烯基硅油30份，乙烯基硅树脂8份，苯基乙烯基硅油0.6份，含氢硅油34份，1-乙炔基环丁胺3份，(甲基)丙烯酸缩水甘油酯2份，在惰性气体保护下加入反应装置中，加热至40℃，氯铂酸-四甲基二乙烯基二硅氧烷络合物0.003份，继续搅拌20分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在60℃下加热固化加热30分钟，即制得所述有机硅胶黏剂。30 parts of 980cps terminal vinyl silicone oil, 8 parts of vinyl silicone resin, 0.6 parts of phenyl vinyl silicone oil, 34 parts of hydrogen-containing silicone oil, 3 parts of 1-ethynylcyclobutylamine, 2 parts of glycidyl (meth)acrylate, Add to the reaction device under the protection of inert gas, heat to 40°C, 0.003 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 20 minutes, and cool to room temperature to obtain a colorless and transparent liquid. The air bubbles are removed under reduced pressure, and the organic silica gel adhesive is prepared by heating and curing at 60° C. for 30 minutes.
实施例3Example 3
800cps端乙烯基硅油45份，乙烯基硅树脂8份，苯基乙烯基硅油0.8份，含氢硅油34份，4-乙炔基环丙苯4份，γ-甲基丙烯酰氧基丙基三甲氧基硅烷3份，在惰性气体保护下加入反应装置中，加热至40～60℃，氯铂酸-四甲基二乙烯基二硅氧烷络合物0.002份，继续搅拌25分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在40℃下加热固化加热20分钟，即制得所述有机硅胶黏剂。800cps terminal vinyl silicone oil 45 parts, vinyl silicone resin 8 parts, phenyl vinyl silicone oil 0.8 parts, hydrogen-containing silicone oil 34 parts, 4-ethynyl cyclopropylbenzene 4 parts, γ-methacryloxypropyl trimethyl Add 3 parts of oxysilane to the reaction device under the protection of inert gas, heat to 40～60℃, 0.002 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 25 minutes, and cool to At room temperature, a colorless and transparent liquid is obtained, the bubbles are removed under reduced pressure, and the organic silica gel adhesive is prepared by heating and curing at 40° C. for 20 minutes.
实施例4Example 4
400cps端乙烯基硅油25份，乙烯基硅树脂8份，苯基乙烯基硅油0.9份，含氢硅油32份，1-乙炔环戊基苯3份，(甲基)丙烯酸羟乙酯4份，在惰性气体保护下加入反应装置中，加热至50℃，氯铂酸-四甲基二乙烯基二硅氧烷络合物0.005份，继续搅拌20分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在60℃下加热固化加热40分钟，即制得所述有机硅胶黏剂。400cps terminal vinyl silicone oil 25 parts, vinyl silicone resin 8 parts, phenyl vinyl silicone oil 0.9 parts, hydrogen-containing silicone oil 32 parts, 1-acetylene cyclopentyl benzene 3 parts, (meth) hydroxyethyl acrylate 4 parts, Add to the reaction device under the protection of inert gas, heat to 50°C, 0.005 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 20 minutes, and cool to room temperature to obtain a colorless and transparent liquid. The air bubbles are removed under reduced pressure, and the organic silica gel adhesive is prepared by heating and curing at 60° C. for 40 minutes.
实施例5Example 5
600cps端乙烯基硅油30份，乙烯基硅树脂6份，苯基乙烯基硅油0.4份，含氢硅油30份，1-乙炔基环己醇3份，三羟基甲基丙烷烯 酸酯3份，在惰性气体保护下加入反应装置中，加热至60℃，氯铂酸-四甲基二乙烯基二硅氧烷络合物0.005份，继续搅拌30分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在80℃下加热固化加热20分钟，即制得所述有机硅胶黏剂。600cps terminal vinyl silicone oil 30 parts, vinyl silicone resin 6 parts, phenyl vinyl silicone oil 0.4 parts, hydrogen-containing silicone oil 30 parts, 1-ethynyl cyclohexanol 3 parts, trihydroxymethyl propane enoate 3 parts, Add it to the reaction device under the protection of inert gas, heat to 60°C, 0.005 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 30 minutes, and cool to room temperature to obtain a colorless and transparent liquid. The air bubbles are removed under reduced pressure, and the organic silica gel adhesive is prepared by heating and curing at 80° C. for 20 minutes.
实施例6Example 6
500cps端乙烯基硅油45份，乙烯基硅树脂7份，苯基乙烯基硅油0.3份，含氢硅油30份，4-叔丁基-1-乙炔基环己醇4份，(甲基)丙烯酸甲酯5份，在惰性气体保护下加入反应装置中，加热至40℃，氯铂酸-四甲基二乙烯基二硅氧烷络合物0.004份，继续搅拌20分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在40℃下加热固化加热30分钟，即制得所述有机硅胶黏剂。500cps terminal vinyl silicone oil 45 parts, vinyl silicone resin 7 parts, phenyl vinyl silicone oil 0.3 parts, hydrogen-containing silicone oil 30 parts, 4-tert-butyl-1-ethynyl cyclohexanol 4 parts, (meth)acrylic acid Add 5 parts of methyl ester to the reaction device under the protection of inert gas, heat to 40°C, 0.004 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 20 minutes, and cool to room temperature to obtain Colorless and transparent liquid, depressurize to remove bubbles, heat for curing at 40°C for 30 minutes to prepare the organic silica gel adhesive.
对比例1(不含苯基乙烯基硅油)Comparative example 1 (without phenyl vinyl silicone oil)
600cps端乙烯基硅油25份，乙烯基硅树脂5份，含氢硅油25份，乙炔基环乙醇2份，(甲基)丙烯酸乙酯1份，在惰性气体保护下加入反应装置中，加热至60℃，氯铂酸-四甲基二乙烯基二硅氧烷络合物0.003份，继续搅拌30分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在80℃下加热固化加热25分钟，即制得所述有机硅胶黏剂。600cps-terminated vinyl silicone oil 25 parts, vinyl silicone resin 5 parts, hydrogen-containing silicone oil 25 parts, ethynyl cycloethanol 2 parts, (meth)ethyl acrylate 1 part, add to the reaction device under the protection of inert gas, and heat to 60℃, 0.003 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 30 minutes, and cool to room temperature to obtain a colorless and transparent liquid, depress the air bubbles, and heat and solidify at 80℃ Heating for 25 minutes, the organic silica gel adhesive is prepared.
对比例2(含苯基乙烯基硅油2份)Comparative example 2 (containing 2 parts of phenyl vinyl silicone oil)
600cps端乙烯基硅油25份，乙烯基硅树脂5份，含氢硅油25份，苯基乙烯基硅油2份，乙炔基环乙醇2份，(甲基)丙烯酸乙酯1份，在惰性气体保护下加入反应装置中，加热至60℃，氯铂酸-四甲基二乙烯基二硅氧烷络合物0.003份，继续搅拌30分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在80℃下加热固化加热25分钟，即制得所述有机硅胶黏剂。600cps-terminated vinyl silicone oil 25 parts, vinyl silicone resin 5 parts, hydrogen-containing silicone oil 25 parts, phenyl vinyl silicone oil 2 parts, ethynyl cycloethanol 2 parts, (meth)acrylate 1 part, under inert gas protection Add it to the reaction device, heat to 60°C, 0.003 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 30 minutes, and cool to room temperature to obtain a colorless and transparent liquid, which is removed under reduced pressure The air bubbles are heated and cured at 80° C. and heated for 25 minutes to obtain the organic silica gel adhesive.
对比例3(含苯基乙烯基硅油5份)Comparative example 3 (containing 5 parts of phenyl vinyl silicone oil)
600cps端乙烯基硅油25份，乙烯基硅树脂5份，含氢硅油25份，苯基乙烯基硅油5份，乙炔基环乙醇2份，(甲基)丙烯酸乙酯1 份，在惰性气体保护下加入反应装置中，加热至60℃，氯铂酸-四甲基二乙烯基二硅氧烷络合物0.003份，继续搅拌30分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在80℃下加热固化加热25分钟，即制得所述有机硅胶黏剂。600cps-terminated vinyl silicone oil 25 parts, vinyl silicone resin 5 parts, hydrogen-containing silicone oil 25 parts, phenyl vinyl silicone oil 5 parts, ethynyl cycloethanol 2 parts, (meth)acrylate 1 part, under inert gas protection Add it to the reaction device, heat to 60°C, 0.003 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 30 minutes, and cool to room temperature to obtain a colorless and transparent liquid, which is removed under reduced pressure The air bubbles are heated and cured at 80° C. and heated for 25 minutes to obtain the organic silica gel adhesive.
对比例4(不含乙烯基硅树脂)Comparative example 4 (without vinyl silicone resin)
500cps端乙烯基硅油45份，苯基乙烯基硅油0.3份，含氢硅油30份，4-叔丁基-1-乙炔基环己醇4份，(甲基)丙烯酸甲酯5份，在惰性气体保护下加入反应装置中，加热至40℃，氯铂酸-四甲基二乙烯基二硅氧烷络合物0.004份，继续搅拌20分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在40℃下加热固化加热30分钟，即制得所述有机硅胶黏剂。500cps terminal vinyl silicone oil 45 parts, phenyl vinyl silicone oil 0.3 parts, hydrogen-containing silicone oil 30 parts, 4-tert-butyl-1-ethynyl cyclohexanol 4 parts, (meth)acrylate 5 parts, inert Add to the reaction device under gas protection, heat to 40°C, 0.004 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 20 minutes, and cool to room temperature to obtain a colorless and transparent liquid. The air bubbles are removed, and the organic silica gel adhesive is prepared by heating and curing at 40° C. for 30 minutes.
对比例5(乙烯基硅树脂3份)Comparative Example 5 (3 parts of vinyl silicone resin)
500cps端乙烯基硅油25份，乙烯基硅树脂3份，苯基乙烯基硅油0.8份，含氢硅油25份，乙炔基环乙醇2份，(甲基)丙烯酸乙酯1份，在惰性气体保护下加入反应装置中，加热至60℃，氯铂酸-四甲基二乙烯基二硅氧烷络合物0.003份，继续搅拌30分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在80℃下加热固化加热25分钟，即制得所述有机硅胶黏剂。500cps-terminated vinyl silicone oil 25 parts, vinyl silicone resin 3 parts, phenyl vinyl silicone oil 0.8 parts, hydrogen-containing silicone oil 25 parts, ethynyl cycloethanol 2 parts, (meth)acrylate 1 part, under inert gas protection Add it to the reaction device, heat to 60°C, 0.003 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 30 minutes, and cool to room temperature to obtain a colorless and transparent liquid, which is removed under reduced pressure The air bubbles are heated and cured at 80° C. and heated for 25 minutes to obtain the organic silica gel adhesive.
对比例6(乙烯基硅树脂15份)Comparative Example 6 (15 parts of vinyl silicone resin)
500cps端乙烯基硅油25份，乙烯基硅树脂15份，苯基乙烯基硅油0.8份，含氢硅油25份，乙炔基环乙醇2份，(甲基)丙烯酸乙酯1份，在惰性气体保护下加入反应装置中，加热至60℃，氯铂酸-四甲基二乙烯基二硅氧烷络合物0.003份，继续搅拌30分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在80℃下加热固化加热25分钟，即制得所述有机硅胶黏剂。500cps terminal vinyl silicone oil 25 parts, vinyl silicone resin 15 parts, phenyl vinyl silicone oil 0.8 parts, hydrogen-containing silicone oil 25 parts, ethynyl cycloethanol 2 parts, (meth)acrylate 1 part, under inert gas protection Add it to the reaction device, heat to 60°C, 0.003 parts of chloroplatinic acid-tetramethyldivinyldisiloxane complex, continue to stir for 30 minutes, and cool to room temperature to obtain a colorless and transparent liquid, which is removed under reduced pressure The air bubbles are heated and cured at 80° C. and heated for 25 minutes to obtain the organic silica gel adhesive.
性能对比试验例：固化后的有机硅胶黏剂性能测试Performance comparison test example: performance test of organic silicone adhesive after curing
拉伸强度、断裂伸长率测定Determination of tensile strength and elongation at break
将上述实施示例中所得到的无色透明液体，减压脱除气泡，取少 量的无色透明液体平铺在玻璃板上，厚度为0.5mm，然后加热至60℃，20分钟后取出，冷却至室温固化，然后用模具制备哑铃状的测试条，进行拉伸强度和断裂伸长率的测试，所采用仪器为万能测试机。Take the colorless and transparent liquid obtained in the above implementation example, remove the bubbles under reduced pressure, take a small amount of colorless and transparent liquid and spread it on a glass plate with a thickness of 0.5mm, then heat it to 60°C, take it out after 20 minutes, and cool it. It is cured at room temperature, and then a dumbbell-shaped test strip is prepared with a mold to test the tensile strength and elongation at break. The instrument used is a universal testing machine.
测试结果如下表1所示：The test results are shown in Table 1 below:
表1固化后的有机硅胶黏剂拉伸强度、断裂伸长率测定Table 1 Determination of tensile strength and elongation at break of organic silicone adhesive after curing
| 样品sample | 有无气泡Whether there are bubbles | 颜色colour | 拉伸强度MPaTensile strength MPa | 断裂伸长率％Elongation at break% |
| 实施例1Example 1 | 无no | 无色透明Colorless and transparent | 2.7152.715 | 294294 |
| 实施例2Example 2 | 无no | 无色透明Colorless and transparent | 3.4973.497 | 335335 |
| 实施例3Example 3 | 无no | 无色透明Colorless and transparent | 2.892.89 | 345345 |
| 实施例4Example 4 | 无no | 无色透明Colorless and transparent | 3.5783.578 | 330330 |
| 实施例5Example 5 | 无no | 无色透明Colorless and transparent | 3.4113.411 | 367367 |
| 实施例6Example 6 | 无no | 无色透明Colorless and transparent | 2.9172.917 | 354354 |
| 对比例1Comparative example 1 | 无no | 无色透明Colorless and transparent | 0.6180.618 | 211211 |
| 对比例2Comparative example 2 | 无no | 无色透明Colorless and transparent | 1.2121.212 | 232232 |
| 对比例3Comparative example 3 | 无no | 无色透明Colorless and transparent | 1.5781.578 | 200200 |
| 对比例4Comparative example 4 | 无no | 无色透明Colorless and transparent | 3.323.32 | 234234 |
| 对比例5Comparative example 5 | 无no | 无色透明Colorless and transparent | 3.2223.222 | 245245 |
| 对比例6Comparative example 6 | 无no | 无色透明Colorless and transparent | 3.3423.342 | 219219 |
胶黏强度测定Adhesive strength determination
将上述实施示例中所得到的无色透明液体，减压脱除气泡，取少量的无色透明液体分别涂覆于长10cm，宽5cm，厚2mm的玻璃板上，涂覆的有机硅胶黏剂的厚度为0.5mm,然后将另外一同样大小的玻璃板进行交叠，然后加热至60℃，20分钟后取出，冷却至室温固化，通过拉力机进行测试。测试结果如下表2所示：The colorless and transparent liquid obtained in the above example is reduced under reduced pressure to remove bubbles, and a small amount of colorless and transparent liquid is applied to a glass plate of 10cm in length, 5cm in width and 2mm in thickness. The thickness is 0.5mm, and then another glass plate of the same size is overlapped, then heated to 60°C, taken out after 20 minutes, cooled to room temperature to solidify, and tested by a tensile machine. The test results are shown in Table 2 below:
表2固化后的有机硅胶黏剂胶黏强度测定Table 2 Determination of adhesive strength of organic silicone adhesive after curing
| 样品sample | 颜色colour | 粘结强度(N/cm)Bond strength (N/cm) | 固化后的胶黏剂/有无气泡Adhesive after curing/with or without bubbles |
| 实施例1Example 1 | 无色透明Colorless and transparent | 3636 | 无no |
| 实施例2Example 2 | 无色透明Colorless and transparent | 3333 | 无no |
| 实施例3Example 3 | 无色透明Colorless and transparent | 3535 | 无no |
| 实施例4Example 4 | 无色透明Colorless and transparent | 3434 | 无no |
| 实施例5Example 5 | 无色透明Colorless and transparent | 3232 | 无no |
| 实施例6Example 6 | 无色透明Colorless and transparent | 3434 | 无no |
| 对比例1Comparative example 1 | 无色透明Colorless and transparent | 1818 | 无no |
| 对比例2Comparative example 2 | 无色透明Colorless and transparent | 2626 | 无no |
| 对比例3Comparative example 3 | 无色透明Colorless and transparent | 2828 | 无no |
| 对比例4Comparative example 4 | 无色透明Colorless and transparent | 1616 | 无no |
| 对比例5Comparative example 5 | 无色透明Colorless and transparent | 1818 | 无no |
| 对比例6Comparative example 6 | 无色透明Colorless and transparent | 1717 | 无no |
由此可以看出，不加苯基乙烯基硅油对其拉伸强度和断裂伸长率有非常明显的影响，大体积的苯基有很高的位阻，分子间的摩擦也随之增加，导致耗损因子增大，从而大致有机硅的拉伸强度增大，断裂伸长率长；而过量的苯基乙烯基硅油导致分子容易发脆，拉伸强度降低，断裂伸长率变短。It can be seen that the absence of phenyl vinyl silicone oil has a very obvious effect on its tensile strength and elongation at break. The bulky phenyl has high steric hindrance, and the friction between molecules also increases. As a result, the loss factor is increased, and the tensile strength of silicone is generally increased, and the elongation at break is long. Excessive phenyl vinyl silicone oil causes the molecules to become brittle, the tensile strength decreases, and the elongation at break becomes shorter.
此外，乙烯基硅树脂对提高有机硅胶黏剂的粘附性具有很明显的作用。In addition, vinyl silicone resin has a significant effect on improving the adhesion of silicone adhesives.
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和使用发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此，本发明不限于上述实施例，本领域技术人员根据本发明的揭示，不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。The above description of the embodiments is to facilitate those of ordinary skill in the technical field to understand and use the invention. It is obvious that those skilled in the art can easily make various modifications to these embodiments, and apply the general principles described here to other embodiments without creative work. Therefore, the present invention is not limited to the above-mentioned embodiments. According to the disclosure of the present invention by those skilled in the art, all improvements and modifications made without departing from the scope of the present invention should fall within the protection scope of the present invention.
Claims (9)
- 一种显示器贴合专用有机硅胶黏剂，其特征在于，以重量份计包含下述组分：A special organic silicone adhesive for display laminating, which is characterized in that it contains the following components in parts by weight:
- 根据权利要求1所述的显示器贴合专用有机硅胶黏剂，其特征在于，所述端乙烯基硅油为双乙烯基端封的聚二甲基硅氧烷，粘度为400～2000cps。The special organic silicone adhesive for display laminating according to claim 1, wherein the vinyl-terminated silicone oil is divinyl-terminated polydimethylsiloxane with a viscosity of 400-2000 cps.
- 根据权利要求1所述的显示器贴合专用有机硅胶黏剂，其特征在于，所述乙烯基硅树脂为具有高强度交联结构的活性硅氧烷预聚体，其链节结构为：The special organosilicone adhesive for display laminating according to claim 1, wherein the vinyl silicone resin is a reactive siloxane prepolymer with a high-strength cross-linked structure, and its chain link structure is:
- 根据权利要求1所述的显示器贴合专用有机硅胶黏剂，其特征在于，所述苯基乙烯基硅油为乙烯基端封的甲基苯基聚硅氧烷。The special organic silicone adhesive for display laminating according to claim 1, wherein the phenyl vinyl silicone oil is vinyl terminated methyl phenyl polysiloxane.
- 根据权利要求1所述的显示器贴合专用有机硅胶黏剂，其特征在于，所述含氢硅油的分子式为：The special organic silicone adhesive for display laminating according to claim 1, wherein the molecular formula of the hydrogen-containing silicone oil is:
- 根据权利要求1所述的显示器贴合专用有机硅胶黏剂，其特征在于，所述乙炔基化合物选自乙炔基环乙醇、1-乙炔基环丁胺、4-乙炔基环丙苯1-乙炔环戊基苯、2-乙炔基环己醇、2-乙炔基环戊醇、1-乙炔基环己醇或4-叔丁基-1-乙炔基环己醇中的一种或几种。The organic silicone adhesive for display laminating according to claim 1, wherein the ethynyl compound is selected from the group consisting of ethynyl cycloethanol, 1-ethynyl cyclobutylamine, 4-ethynyl cyclopropene 1-acetylene One or more of cyclopentylbenzene, 2-ethynylcyclohexanol, 2-ethynylcyclopentanol, 1-ethynylcyclohexanol, or 4-tert-butyl-1-ethynylcyclohexanol.
- 根据权利要求1所述的显示器贴合专用有机硅胶黏剂，其特征在于，所述铂催化剂为氯铂酸-四甲基二乙烯基二硅氧烷络合物。The special organic silicone adhesive for display laminating according to claim 1, wherein the platinum catalyst is a chloroplatinic acid-tetramethyldivinyldisiloxane complex.
- 根据权利要求1所述的显示器贴合专用有机硅胶黏剂，其特征在于，所述丙烯酸酯类化合物为(甲基)丙烯酸酯类化合物，选自(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸缩水甘油酯、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、(甲基)丙烯酸羟乙酯或三羟基甲基丙烷烯酸酯的任一种。The organic silicone adhesive for display laminating according to claim 1, wherein the acrylic compound is a (meth)acrylate compound selected from the group consisting of methyl (meth)acrylate and (meth)acrylate. Ethyl acrylate, butyl (meth)acrylate, glycidyl (meth)acrylate, γ-methacryloxypropyltrimethoxysilane, hydroxyethyl (meth)acrylate or trihydroxymethylpropane Any of enoic acid esters.
- 如权利要求1所述的显示器贴合专用有机硅胶黏剂的制备方法，其特征在于，步骤如下：3. The method for preparing a special organic silicone adhesive for display laminating according to claim 1, wherein the steps are as follows:以重量份计称取：400～2000cps的端乙烯基硅油25～50份，乙烯基硅树脂5～10份，苯基乙烯基硅油0.1～1份，含氢硅油25～35份，乙炔基化合物2～4份，丙烯酸酯类化合物1～5份，在惰性气体保护下加入反应装置中，加热至40～60℃，加入铂催化剂0.001～0.005份，继续搅拌20～30分钟，冷却至室温，得到无色透明液体，减压脱去气泡，在40～80℃下加热固化加热20～40分钟，即制得有机硅胶黏剂。Weigh in parts by weight: 400-2000cps of 25-50 parts of vinyl-terminated silicone oil, 5-10 parts of vinyl silicone resin, 0.1-1 part of phenyl vinyl silicone oil, 25-35 parts of hydrogen-containing silicone oil, ethynyl compound 2 to 4 parts, 1 to 5 parts of acrylate compounds, add to the reaction device under the protection of inert gas, heat to 40-60°C, add 0.001 to 0.005 parts of platinum catalyst, continue to stir for 20-30 minutes, and cool to room temperature. The colorless transparent liquid is obtained, the bubbles are removed under reduced pressure, and the organic silica gel adhesive is prepared by heating and curing at 40-80 DEG C for 20-40 minutes.
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