JPWO2017065131A1 - Shock-absorbing screen protection film - Google Patents
Shock-absorbing screen protection film Download PDFInfo
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- JPWO2017065131A1 JPWO2017065131A1 JP2017545197A JP2017545197A JPWO2017065131A1 JP WO2017065131 A1 JPWO2017065131 A1 JP WO2017065131A1 JP 2017545197 A JP2017545197 A JP 2017545197A JP 2017545197 A JP2017545197 A JP 2017545197A JP WO2017065131 A1 JPWO2017065131 A1 JP WO2017065131A1
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- 239000000203 mixture Substances 0.000 claims abstract description 111
- 239000012790 adhesive layer Substances 0.000 claims abstract description 50
- 229920001971 elastomer Polymers 0.000 claims abstract description 34
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- 239000002985 plastic film Substances 0.000 claims abstract description 15
- 229920006255 plastic film Polymers 0.000 claims abstract description 15
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- 239000004820 Pressure-sensitive adhesive Substances 0.000 claims description 53
- 125000004432 carbon atom Chemical group C* 0.000 claims description 38
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- 239000000853 adhesive Substances 0.000 claims description 30
- 230000001070 adhesive effect Effects 0.000 claims description 30
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 28
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- 239000003054 catalyst Substances 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 13
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- 238000001879 gelation Methods 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 1
- WNLRTRBMVRJNCN-UHFFFAOYSA-N hexanedioic acid Natural products OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- GJRQTCIYDGXPES-UHFFFAOYSA-N iso-butyl acetate Natural products CC(C)COC(C)=O GJRQTCIYDGXPES-UHFFFAOYSA-N 0.000 description 1
- FGKJLKRYENPLQH-UHFFFAOYSA-M isocaproate Chemical compound CC(C)CCC([O-])=O FGKJLKRYENPLQH-UHFFFAOYSA-M 0.000 description 1
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 1
- 125000003253 isopropoxy group Chemical group [H]C([H])([H])C([H])(O*)C([H])([H])[H] 0.000 description 1
- 229940011051 isopropyl acetate Drugs 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
- OQAGVSWESNCJJT-UHFFFAOYSA-N isovaleric acid methyl ester Natural products COC(=O)CC(C)C OQAGVSWESNCJJT-UHFFFAOYSA-N 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- JPQBRSQJGWOTGC-UHFFFAOYSA-N methyl(silyloxysilyloxy)silane Chemical compound C[SiH2]O[SiH2]O[SiH3] JPQBRSQJGWOTGC-UHFFFAOYSA-N 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
- QXLPXWSKPNOQLE-UHFFFAOYSA-N methylpentynol Chemical compound CCC(C)(O)C#C QXLPXWSKPNOQLE-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- AHHWIHXENZJRFG-UHFFFAOYSA-N oxetane Chemical compound C1COC1 AHHWIHXENZJRFG-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920006289 polycarbonate film Polymers 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 229940086066 potassium hydrogencarbonate Drugs 0.000 description 1
- IALUUOKJPBOFJL-UHFFFAOYSA-N potassium oxidosilane Chemical class [K+].[SiH3][O-] IALUUOKJPBOFJL-UHFFFAOYSA-N 0.000 description 1
- CUQOHAYJWVTKDE-UHFFFAOYSA-N potassium;butan-1-olate Chemical compound [K+].CCCC[O-] CUQOHAYJWVTKDE-UHFFFAOYSA-N 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- VNRWTCZXQWOWIG-UHFFFAOYSA-N tetrakis(trimethylsilyl) silicate Chemical compound C[Si](C)(C)O[Si](O[Si](C)(C)C)(O[Si](C)(C)C)O[Si](C)(C)C VNRWTCZXQWOWIG-UHFFFAOYSA-N 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- JNRUXZIXAXHXTN-UHFFFAOYSA-N trimethyl(2-methylbut-3-yn-2-yloxy)silane Chemical compound C#CC(C)(C)O[Si](C)(C)C JNRUXZIXAXHXTN-UHFFFAOYSA-N 0.000 description 1
- NWMVPLQDJXJDEW-UHFFFAOYSA-N trimethyl(3-methylpent-1-yn-3-yloxy)silane Chemical compound CCC(C)(C#C)O[Si](C)(C)C NWMVPLQDJXJDEW-UHFFFAOYSA-N 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Adhesive Tapes (AREA)
- Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Laminated Bodies (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
従来よりも耐衝撃性に優れた衝撃吸収性画面保護フィルムを提供する。プラスチック製フィルムの少なくとも一方の面に、付加硬化型のシリコーン粘着剤組成物の硬化物からなる粘着層を有し、粘着層のゴム硬度がアスカーＣ型硬度計を用いて測定したときに４０〜７５である衝撃吸収性画面保護フィルム。Provided is an impact-absorbing screen protection film having superior impact resistance. When having an adhesive layer made of a cured product of an addition-curable silicone adhesive composition on at least one surface of the plastic film, the rubber hardness of the adhesive layer is 40 to 40 when measured using an Asker C-type hardness meter. 75, a shock-absorbing screen protection film.
Description
本発明は、貼り合わせる各種ディスプレイの耐衝撃性を向上させることが可能な衝撃吸収性画面保護フィルムに関する。 The present invention relates to an impact-absorbing screen protective film capable of improving the impact resistance of various displays to be bonded.
近年、携帯電話やノートパソコンなどの持ち運び可能な電子機器が広く普及している。その中でも、最近では特にタッチパネルを搭載したスマートフォンやタブレットＰＣの市場が拡大している。スマートフォンとタブレットＰＣの特徴としては、キーパッドやキーボードが無くなるため、大画面であり小型化を可能としている。 In recent years, portable electronic devices such as mobile phones and notebook computers have become widespread. Among them, the market for smartphones and tablet PCs equipped with a touch panel has recently been expanding. As a feature of smartphones and tablet PCs, since there is no keypad or keyboard, the screen is large and can be downsized.
これらの端末は、ディスプレイに直接手を触れることにより操作を行うものであるが、ディスプレイが露出しているためゴミなどが付着しやすく、指で操作を行うことから皮脂汚れでディスプレイを汚すなどにより、表面外観が悪化したり視認性が悪くなることがある。そこで、これらの端末には保護フィルムと呼ばれる透明な粘着性フィルムをディスプレイに貼り合わせることで表面の外観を維持することが一般的となっている。 These devices are operated by touching the display directly. However, because the display is exposed, dust and the like are likely to adhere to it. The surface appearance may deteriorate or the visibility may deteriorate. Therefore, it is common for these terminals to maintain the appearance of the surface by attaching a transparent adhesive film called a protective film to the display.
保護フィルムに用いられる粘着剤を構成するためのベース材料はいくつか種類があり、ゴム系の粘着剤、アクリル系の粘着剤、シリコーン系の粘着剤などに大別される。その中で、シリコーン粘着剤が画面保護フィルムとして多く用いられているのは、泡抜け性やリワーク性が他の材料と比較して優れているためである。泡抜け性が良好であれば、自然と粘着層がディスプレイに濡れていくため貼り合わせがしやすく、リワーク性が良いと貼り直しが容易である。 There are several types of base materials for constituting the pressure-sensitive adhesive used in the protective film, and they are roughly classified into rubber-based pressure-sensitive adhesives, acrylic-based pressure-sensitive adhesives, silicone-based pressure-sensitive adhesives, and the like. Among them, the silicone adhesive is often used as a screen protective film because it is superior in bubble removal properties and reworkability compared to other materials. If the defoaming property is good, the adhesive layer naturally gets wet with the display, so that it is easy to attach, and if the rework property is good, it is easy to reattach.
このようなシリコーン粘着剤を使用した画面保護フィルムには、最近新たに耐衝撃性を向上させたいという要求が高まっている。これは、スマートフォンやタブレットＰＣといったディスプレイが露出している端末が増えたことにより、ディスプレイ上にものを落とすなどして破損するというリスクが増えたため、保護フィルムにより破損を防ぐ、あるいは衝撃を緩和することを目的としている。 Recently, there is an increasing demand for a screen protection film using such a silicone adhesive to newly improve impact resistance. This is because the number of devices with exposed displays such as smartphones and tablet PCs has increased the risk of damage caused by dropping things on the display, etc., so protective films can prevent damage or reduce impact The purpose is that.
これまでのシリコーン粘着剤を用いたフィルムは、数十μｍ程度の薄層の粘着層を有するものが主流であり、耐衝撃性への配慮はなされていなかった（特許文献１〜４：特許第３０９５１７９号公報、特許第３１３０１７６号公報、特開２０００−３１３８５９号公報、特許第４６７８８４７号公報）。そこで、シリコーン粘着剤を用いて厚みのある粘着層を形成することで耐衝撃性の付与が可能になると考えられるが、厚膜の形成が可能としている特許文献５，６（特開平０５−０８６３５１号公報、特許第５２３４０６４号公報）において、これらの特許のいずれについても耐衝撃性に関してはまったく言及していない。 Conventionally, a film using a silicone adhesive has a thin adhesive layer of about several tens of μm, and no consideration has been given to impact resistance (Patent Documents 1 to 4: Patent No. 1). No. 3095179, Japanese Patent No. 3130176, Japanese Unexamined Patent Publication No. 2000-313859, Japanese Patent No. 4678847). Therefore, it is considered that a shock-resistant layer can be provided by forming a thick pressure-sensitive adhesive layer using a silicone pressure-sensitive adhesive. However, Patent Documents 5 and 6 (Japanese Patent Laid-Open No. 05-086351) that enable the formation of a thick film. No. 523464) makes no mention of impact resistance in any of these patents.
本発明は、上記事情に鑑みなされたもので、従来よりも耐衝撃性に優れた衝撃吸収性画面保護フィルムを提供することを目的とする。 The present invention has been made in view of the above circumstances, and an object thereof is to provide an impact-absorbing screen protection film that is more excellent in impact resistance than before.
本発明者は、上記目的を達成するため鋭意検討を重ねた結果、フィルムの耐衝撃性が粘着層のゴム硬度と相関があることを見出し、プラスチック製フィルムの少なくとも一方の面に、付加硬化型のシリコーン粘着剤組成物の硬化物からなる粘着層を有する画面保護フィルムにおいて、該粘着層のゴム硬度がアスカーＣ型硬度計を用いて測定したときに４０〜７５であると、従来よりも耐衝撃性に優れた画面保護フィルムとなり得ることを見出し、本発明をなすに至った。 As a result of intensive studies to achieve the above object, the present inventor has found that the impact resistance of the film has a correlation with the rubber hardness of the adhesive layer, and the addition-curing type is applied to at least one surface of the plastic film. When the rubber hardness of the adhesive layer is 40 to 75 when measured using an Asker C-type hardness meter, the screen protective film having an adhesive layer comprising a cured product of the silicone adhesive composition of It has been found that it can be a screen protective film excellent in impact properties, and has led to the present invention.
従って、本発明は、下記の衝撃吸収性画面保護フィルムを提供する。
［１］
プラスチック製フィルムの少なくとも一方の面に、付加硬化型のシリコーン粘着剤組成物の硬化物からなる粘着層を有し、粘着層のゴム硬度がアスカーＣ型硬度計を用いて測定したときに４０〜７５である衝撃吸収性画面保護フィルム。
［２］
前記粘着層の厚みが５０〜５００μｍであることを特徴とする［１］に記載の衝撃吸収性画面保護フィルム。
［３］
前記粘着層の厚みが１００〜４５０μｍであることを特徴とする［１］に記載の衝撃吸収性画面保護フィルム。
［４］
前記プラスチック製フィルムがポリエステルフィルムであることを特徴とする［１］乃至［３］のいずれかに記載の衝撃吸収性画面保護フィルム。
［５］
厚さ２５μｍのポリエステルフィルムの片面に、前記シリコーン粘着剤組成物の硬化物からなる厚さ２００μｍの粘着層を備える衝撃吸収性画面保護フィルムを、衝撃試験機のロードセル上にポリエステルフィルムを上面にした状態で貼り合わせて、２５０ｍｍの高さから１５０．８ｇの鋼球をポリエステルフィルム面に落下させたときの衝撃力が８．００ｋＮ以下であることを特徴とする［１］乃至［４］のいずれかに記載の衝撃吸収性画面保護フィルム。
［６］
幅２５ｍｍ、厚さ２５μｍのポリエステルフィルムの一方の面に、前記シリコーン粘着剤組成物の硬化物からなる厚さ３０μｍの粘着層を有する衝撃吸収性画面保護フィルムにおいて、該フィルムの粘着面をステンレススチール製の板に貼り合わせ、これを１８０°方向へ３００ｍｍ／分で剥離したときの粘着力が０．０１〜２．０Ｎ／２５ｍｍの範囲となることを特徴とする［１］乃至［５］のいずれかに記載の衝撃吸収性画面保護フィルム。
［７］
前記シリコーン粘着剤組成物が、
（Ａ）下記平均組成式（１）で表される、１分子中に少なくとも２個のアルケニル基含有有機基を有し、１００ｇ中にアルケニル基０．００１〜０．０５モルが含まれるオルガノポリシロキサン：１００〜６０質量部、
（Ｂ）Ｒ2 3ＳｉＯ1/2単位（式中、Ｒ2は独立に脂肪族不飽和結合を有さない炭素数１〜１０の１価炭化水素基又は炭素数２〜６のアルケニル基を示す。）とＳｉＯ4/2単位を主成分とし、（Ｒ2 3ＳｉＯ1/2単位）／（ＳｉＯ4/2単位）がモル比で０．５〜１．０であるオルガノポリシロキサン：０〜４０質量部、
（Ｃ）下記平均組成式（２）で表され、１分子中に少なくとも３個のＳｉ−Ｈ基を有するオルガノハイドロジェンポリシロキサン：（Ａ）、（Ｂ）成分の合計アルケニル基に対し、Ｓｉ−Ｈ基がモル比で０．２〜１５となる量、
Ｒ3 eＨfＳｉＯ(4-e-f)/2 （２）
（式中、Ｒ3は独立に非置換又は置換の炭素数１〜１０の１価炭化水素基を示し、ｅ＞０、ｆ＞０であり、さらに０＜ｅ＋ｆ≦３である。）
（Ｄ）（Ａ）、（Ｂ）成分のアルケニル基と（Ｃ）成分のＳｉ−Ｈ基をヒドロシリル化付加して硬化させるための白金族金属系触媒：上記（Ａ）〜（Ｃ）成分の総量に対し、金属質量が１〜５００ｐｐｍとなる量
を含むことを特徴とする［１］乃至［６］のいずれかに記載の衝撃吸収性画面保護フィルム。
［８］
前記シリコーン粘着剤組成物が、さらに（Ｅ）反応制御剤を、（Ａ）〜（Ｃ）成分の合計１００質量部に対し０．０１〜５質量部含むことを特徴とする［７］に記載の衝撃吸収性画面保護フィルム。
［９］
ガラス製又はプラスチック製のディスプレイに貼り合わせて使用することを特徴とする［１］乃至［８］のいずれかに記載の衝撃吸収性画面保護フィルム。Accordingly, the present invention provides the following shock-absorbing screen protection film.
[1]
When having an adhesive layer made of a cured product of an addition-curable silicone adhesive composition on at least one surface of the plastic film, the rubber hardness of the adhesive layer is 40 to 40 when measured using an Asker C-type hardness meter. 75, a shock-absorbing screen protection film.
[2]
The shock-absorbing screen protection film according to [1], wherein the pressure-sensitive adhesive layer has a thickness of 50 to 500 μm.
[3]
The shock-absorbing screen protective film according to [1], wherein the adhesive layer has a thickness of 100 to 450 μm.
[4]
The impact-absorbing screen protection film according to any one of [1] to [3], wherein the plastic film is a polyester film.
[5]
A shock-absorbing screen protective film having a 200 μm thick adhesive layer made of a cured product of the silicone adhesive composition on one side of a 25 μm thick polyester film, and a polyester film on the top surface of a load cell of an impact tester. Any one of [1] to [4], wherein the impact force when a 150.8 g steel ball is dropped onto a polyester film surface from a height of 250 mm is 8.00 kN or less. The shock-absorbing screen protective film described in Crab.
[6]
In an impact-absorbing screen protection film having a 30 μm thick adhesive layer made of a cured product of the silicone adhesive composition on one side of a polyester film having a width of 25 mm and a thickness of 25 μm, the adhesive side of the film is made of stainless steel. [1] to [5], wherein the adhesive strength when bonded to a plate made of metal and peeled in a 180 ° direction at 300 mm / min is in the range of 0.01 to 2.0 N / 25 mm. The shock-absorbing screen protective film according to any one of the above.
[7]
The silicone pressure-sensitive adhesive composition is
(A) Organopoly having at least two alkenyl group-containing organic groups in one molecule and 0.001 to 0.05 mol of alkenyl groups in 100 g, represented by the following average composition formula (1) Siloxane: 100-60 parts by mass,
(B) R 2 3 SiO 1/2 unit (wherein R 2 independently represents a monovalent hydrocarbon group having 1 to 10 carbon atoms or an alkenyl group having 2 to 6 carbon atoms which does not have an aliphatic unsaturated bond). And an organopolysiloxane having a SiO 4/2 unit as a main component and (R 2 3 SiO 1/2 unit) / (SiO 4/2 unit) in a molar ratio of 0.5 to 1.0: 0 ~ 40 parts by mass,
(C) Organohydrogenpolysiloxane represented by the following average composition formula (2) and having at least 3 Si—H groups in one molecule: (A), Si (V) with respect to the total alkenyl groups of the components An amount such that the —H group has a molar ratio of 0.2 to 15;
R 3 e H f SiO (4-ef) / 2 (2)
(In the formula, R 3 independently represents an unsubstituted or substituted monovalent hydrocarbon group having 1 to 10 carbon atoms, e> 0, f> 0, and 0 <e + f ≦ 3.)
(D) Platinum group metal catalyst for hydrosilylation addition and curing of alkenyl group of components (A) and (B) and Si—H group of component (C): of components (A) to (C) above The impact-absorbing screen protection film according to any one of [1] to [6], wherein the metal mass includes an amount of 1 to 500 ppm relative to the total amount.
[8]
[7] The silicone pressure-sensitive adhesive composition further includes (E) a reaction control agent in an amount of 0.01 to 5 parts by mass with respect to a total of 100 parts by mass of the components (A) to (C). Shock absorbing screen protection film.
[9]
The impact-absorbing screen protection film according to any one of [1] to [8], which is used by being attached to a glass or plastic display.
本発明によれば、特定の硬度を有し、好ましくはさらに特定の厚みを有する、皮膜強度の強いシリコーン粘着剤組成物を硬化させて得られた粘着層を有することにより、外力を受けたときの衝撃吸収性が向上するため、耐衝撃性に優れた衝撃吸収性画面保護フィルムを製造することが可能である。 According to the present invention, when an external force is applied by having a pressure-sensitive adhesive layer obtained by curing a silicone pressure-sensitive adhesive composition having a specific hardness, preferably a specific thickness, and a high film strength. Therefore, it is possible to produce a shock-absorbing screen protection film excellent in impact resistance.
以下、本発明についての詳細を記す。
本発明の衝撃吸収性画面保護フィルムは、プラスチック製フィルムの少なくとも一方の面に、付加硬化型のシリコーン粘着剤組成物の硬化物からなる粘着層を有し、該粘着層のゴム硬度がアスカーＣ型硬度計を用いて測定したときに４０〜７５のものである。Details of the present invention will be described below.
The shock-absorbing screen protective film of the present invention has an adhesive layer made of a cured product of an addition-curable silicone adhesive composition on at least one surface of a plastic film, and the rubber hardness of the adhesive layer is Asker C. 40 to 75 when measured using a mold hardness meter.
［プラスチック製フィルム］
本発明の衝撃吸収性画面保護フィルムは、プラスチック製フィルムを有する。
プラスチック製フィルムとしては、ポリエチレンフィルム、ポリプロピレンフィルム、ポリエステルフィルム、ポリイミドフィルム、ポリ塩化ビニルフィルム、ポリ塩化ビニリデンフィルム、ポリビニルアルコールフィルム、ポリカーボネートフィルム、ポリテトラフルオロエチレンフィルム、ポリスチレンフィルム、エチレン−酢酸ビニル共重合体フィルム、エチレン−ビニルアルコール共重合体フィルム、トリアセチルセルロースフィルム、ポリエーテルエーテルケトンフィルム、ポリフェニレンサルファイドフィルムなどが挙げられ、ポリエステルフィルムが好ましい。
プラスチック製フィルムの厚みは３〜２００μｍとすればよいが、特に限定されるものではない。[Plastic film]
The shock-absorbing screen protective film of the present invention has a plastic film.
Plastic films include polyethylene film, polypropylene film, polyester film, polyimide film, polyvinyl chloride film, polyvinylidene chloride film, polyvinyl alcohol film, polycarbonate film, polytetrafluoroethylene film, polystyrene film, ethylene-vinyl acetate copolymer Examples include a coalesced film, an ethylene-vinyl alcohol copolymer film, a triacetyl cellulose film, a polyether ether ketone film, a polyphenylene sulfide film, and the like, and a polyester film is preferable.
The thickness of the plastic film may be 3 to 200 μm, but is not particularly limited.
［付加硬化型シリコーン粘着剤組成物］
本発明の衝撃吸収性画面保護フィルムは、プラスチック製フィルムの少なくとも一方の面に付加硬化型のシリコーン粘着剤組成物を硬化させて得られる粘着層を有する。[Addition-curing type silicone pressure-sensitive adhesive composition]
The impact-absorbing screen protective film of the present invention has an adhesive layer obtained by curing an addition-curable silicone adhesive composition on at least one surface of a plastic film.
シリコーン粘着剤組成物を硬化させて得られる粘着層（以下、粘着層とする）の厚みは５０〜５００μｍであることが好ましく、より好ましくは８０〜４８０μｍ、さらに好ましくは１００〜４５０μｍである。５０μｍよりも薄いと外力からの衝撃に対し弱くなる場合があり、５００μｍより厚いと加工が難しくなり、粘着層表面の平坦性が悪くなる場合がある。 The thickness of the pressure-sensitive adhesive layer (hereinafter referred to as pressure-sensitive adhesive layer) obtained by curing the silicone pressure-sensitive adhesive composition is preferably 50 to 500 μm, more preferably 80 to 480 μm, and still more preferably 100 to 450 μm. If it is thinner than 50 μm, it may be weak against an impact from an external force, and if it is thicker than 500 μm, the processing becomes difficult and the flatness of the adhesive layer surface may be deteriorated.
粘着層のゴム硬度は、アスカーＣ型硬度計を用いて測定したときに４０〜７５となるものであり、好ましくは４２〜７５、より好ましくは４４〜７５となるものがよい。本発明者は、シリコーン粘着剤組成物を硬化させて得られる粘着層のゴム硬度が耐衝撃性に相関があることを見出した。ゴム硬度が４０よりも小さいと粘着層が柔らかくなり、外部からの衝撃を吸収できずに被着体を傷つけてしまう。ゴム硬度が７５よりも大きいと粘着層が硬くなり、外部からの衝撃が直接被着体に伝わり、被着体を傷つけてしまう。 The rubber hardness of the adhesive layer is 40 to 75, preferably 42 to 75, more preferably 44 to 75 when measured using an Asker C-type hardness meter. The present inventor has found that the rubber hardness of the pressure-sensitive adhesive layer obtained by curing the silicone pressure-sensitive adhesive composition has a correlation with the impact resistance. When the rubber hardness is less than 40, the adhesive layer becomes soft, and the adherend is damaged without being able to absorb the impact from the outside. When the rubber hardness is greater than 75, the adhesive layer becomes hard, and external impacts are directly transmitted to the adherend, thereby damaging the adherend.
以下、付加硬化型シリコーン粘着剤組成物の詳細について説明する。
［（Ａ）成分］
（Ａ）成分は、下記平均組成式（１）で表され、１分子中に少なくとも２個のアルケニル基含有有機基を有し、１００ｇ中にアルケニル基０．００１〜０．０５モルが含まれるオルガノポリシロキサンである。
[(A) component]
The component (A) is represented by the following average composition formula (1) and has at least two alkenyl group-containing organic groups in one molecule, and 0.001 to 0.05 mol of alkenyl groups are contained in 100 g. Organopolysiloxane.
上記式（１）において、Ｒ1は同一又は異種の炭素数１〜１０の脂肪族不飽和結合を有さない１価炭化水素基又は炭素数２〜１０のアルケニル基含有有機基であり、Ｒ1のうち少なくとも２個は炭素数２〜１０のアルケニル基含有有機基である。
脂肪族不飽和結合を有さない１価炭化水素基としては、例えば、メチル基、エチル基、プロピル基、ブチル基等のアルキル基、シクロヘキシル基等のシクロアルキル基、フェニル基等のアリール基などが挙げられ、さらに、これらの基の炭素原子に結合した水素原子の一部又は全部がハロゲン原子又はその他の基で置換されていてもよく、置換基としては、トリフルオロメチル基、３，３，３−トリフルオロプロピル基等が例示される。中でも、飽和の脂肪族基又は芳香族基が好ましく、メチル基、フェニル基が好ましい。In the above formula (1), R 1 is the same or different monovalent hydrocarbon group having no aliphatic unsaturated bond having 1 to 10 carbon atoms or an alkenyl group-containing organic group having 2 to 10 carbon atoms, R At least two of 1 are alkenyl group-containing organic groups having 2 to 10 carbon atoms.
Examples of monovalent hydrocarbon groups having no aliphatic unsaturated bond include alkyl groups such as methyl, ethyl, propyl, and butyl groups, cycloalkyl groups such as cyclohexyl groups, and aryl groups such as phenyl groups. In addition, some or all of the hydrogen atoms bonded to the carbon atoms of these groups may be substituted with halogen atoms or other groups. Examples of the substituent include a trifluoromethyl group, 3, 3 , 3-trifluoropropyl group and the like. Among them, a saturated aliphatic group or an aromatic group is preferable, and a methyl group or a phenyl group is preferable.
アルケニル基含有有機基としては、炭素数２〜１０のもの、例えば、ビニル基、アリル基、ヘキセニル基、オクテニル基等のアルケニル基、アクリロイルプロピル基、アクリロイルメチル基、メタクリロイルプロピル基等のアクリロイルアルキル基、及びメタクリロイルアルキル基、シクロヘキセニルエチル基等のシクロアルケニルアルキル基、ビニルオキシプロピル基等のアルケニルオキシアルキル基などが挙げられる。中でもビニル基が好ましい。 Examples of the alkenyl group-containing organic group include those having 2 to 10 carbon atoms, for example, alkenyl groups such as vinyl group, allyl group, hexenyl group, octenyl group, acryloylpropyl group, acryloylmethyl group, methacryloylpropyl group, etc. And cycloalkenylalkyl groups such as a methacryloylalkyl group and a cyclohexenylethyl group, and alkenyloxyalkyl groups such as a vinyloxypropyl group. Of these, vinyl groups are preferred.
（Ａ）成分に含まれるアルケニル基の量は、オルガノポリシロキサン１００ｇ中０．００１〜０．０５モルであり、０．００２〜０．０４モルが好ましく、０．００３〜０．０３モルがより好ましい。０．００１モルよりも小さいと架橋密度が小さくなり、粘着層が十分な硬度を得られない場合があり、０．０５モルよりも大きいと粘着層が硬くなることで適切な耐衝撃性が得られない場合がある。 The amount of the alkenyl group contained in the component (A) is 0.001 to 0.05 mol in 100 g of the organopolysiloxane, preferably 0.002 to 0.04 mol, and more preferably 0.003 to 0.03 mol. preferable. If the amount is less than 0.001 mol, the crosslinking density may be reduced, and the adhesive layer may not have sufficient hardness. If the amount is more than 0.05 mol, the adhesive layer will be hard and appropriate impact resistance can be obtained. It may not be possible.
ａは２以上の整数、ｂは１以上の整数、ｃは０以上の整数、ｄは０以上の整数で、５０≦ａ＋ｂ＋ｃ＋ｄ≦１２，０００であり、１００≦ａ＋ｂ＋ｃ＋ｄ≦１０，０００であることが好ましく、２００≦ａ＋ｂ＋ｃ＋ｄ≦８，０００であることがより好ましい。ａ＋ｂ＋ｃ＋ｄが５０より小さいと、架橋点が多くなりすぎることで反応性が低下するおそれがあり、１２，０００より大きいと、組成物の粘度が非常に高くなるため撹拌混合しにくくなる等、作業性が悪くなるおそれがある。 a is an integer of 2 or more, b is an integer of 1 or more, c is an integer of 0 or more, d is an integer of 0 or more, 50 ≦ a + b + c + d ≦ 12,000, and 100 ≦ a + b + c + d ≦ 10,000 Preferably, 200 ≦ a + b + c + d ≦ 8,000 is more preferable. If a + b + c + d is less than 50, the reactivity may decrease due to excessive crosslinking points, and if it is greater than 12,000, the viscosity of the composition becomes very high, making it difficult to stir and mix. May get worse.
（Ａ）成分は、通常、オクタメチルシクロテトラシロキサン等の環状低分子シロキサンと、アルケニル基含有有機基を含む環状低分子シロキサンとを、触媒を用いて開環重合させて製造するが、重合後は原料である環状低分子シロキサンを含有しているため、これを加熱及び減圧下で、反応生成物中に不活性気体を通気させながら、留去したものを用いることが好ましい。 The component (A) is usually produced by ring-opening polymerization of a cyclic low molecular siloxane such as octamethylcyclotetrasiloxane and a cyclic low molecular siloxane containing an alkenyl group-containing organic group using a catalyst. Since it contains cyclic low-molecular siloxane that is a raw material, it is preferable to use a material obtained by distilling the reaction product through an inert gas while heating and reducing pressure.
（Ａ）成分としては、下記一般式で表されるものが挙げられるが、これらに限定されない。
Ｒ1-1Ｒ1-2 2ＳｉＯ（Ｒ1-2 2ＳｉＯ）pＳｉＲ1-2 2Ｒ1-1
Ｒ1-1Ｒ1-2 2ＳｉＯ（Ｒ1-2 2ＳｉＯ）p（Ｒ1-1Ｒ1-2ＳｉＯ）qＳｉＲ1-2 2Ｒ1-1
Ｒ1-2 3ＳｉＯ（Ｒ1-2 2ＳｉＯ）p（Ｒ1-1Ｒ1-2ＳｉＯ）qＳｉＲ1-2 3
Ｒ1-1 3ＳｉＯ（Ｒ1-2 2ＳｉＯ）p（Ｒ1-1Ｒ1-2ＳｉＯ）qＳｉＲ1-1 3
Ｒ1-1Ｒ1-2 2ＳｉＯ（Ｒ1-2 2ＳｉＯ）p（Ｒ1-1Ｒ1-2ＳｉＯ）qＳｉＲ1-2 2Ｒ1-1
（式中、Ｒ1-1は同一又は異種の炭素数２〜１０のアルケニル基含有有機基であり、Ｒ1-2は同一又は異種の炭素数１〜１０の脂肪族不飽和結合を有さない１価炭化水素基であり、ｐ≧５０、ｑ≧１である（但し、分子中に（Ｒ1-1Ｒ1-2ＳｉＯ）ｑ以外にＲ1-1を有しない場合はｑ≧２である。）。）(A) Although a component represented with the following general formula is mentioned as a component, It is not limited to these.
R 1-1 R 1-2 2 SiO (R 1-2 2 SiO) p SiR 1-2 2 R 1-1
R 1-1 R 1-2 2 SiO (R 1-2 2 SiO) p (R 1-1 R 1-2 SiO) q SiR 1-2 2 R 1-1
R 1-2 3 SiO (R 1-2 2 SiO) p (R 1-1 R 1-2 SiO) q SiR 1-2 3
R 1-1 3 SiO (R 1-2 2 SiO) p (R 1-1 R 1-2 SiO) q SiR 1-1 3
R 1-1 R 1-2 2 SiO (R 1-2 2 SiO) p (R 1-1 R 1-2 SiO) q SiR 1-2 2 R 1-1
(In the formula, R 1-1 is the same or different organic group having 2 to 10 carbon atoms, and R 1-2 has the same or different aliphatic unsaturated bond having 1 to 10 carbon atoms. A monovalent hydrocarbon group, and p ≧ 50 and q ≧ 1 (provided that q ≧ 2 when R 1-1 is not contained in the molecule other than (R 1-1 R 1-2 SiO) q) .).)
Ｒ1-1，Ｒ1-2としては、上記Ｒ1で例示されたものが挙げられる。なお、ｐは５０≦ｐ≦１０，０００が好ましく、１００≦ｐ≦８，０００がより好ましく、ｑは１≦ｑ≦１，０００が好ましく、２≦ｑ≦１，０００がより好ましい。Examples of R 1-1 and R 1-2 include those exemplified for R 1 above. Note that p is preferably 50 ≦ p ≦ 10,000, more preferably 100 ≦ p ≦ 8,000, and q is preferably 1 ≦ q ≦ 1,000, more preferably 2 ≦ q ≦ 1,000.
より具体的な（Ａ）成分としては、下記一般式で表されるものが挙げられるが、これらに限定されない。なお、下記式中のＭｅ，Ｖｉ，Ｐｈはそれぞれメチル基、ビニル基、フェニル基を示す。
［（Ｂ）成分］
（Ｂ）成分は、Ｒ2 3ＳｉＯ1/2単位（式中、Ｒ2は独立に脂肪族不飽和結合を有さない炭素数１〜１０の１価炭化水素基又は炭素数２〜６のアルケニル基を示す。）及びＳｉＯ4/2単位を主成分とし、（Ｒ2 3ＳｉＯ1/2単位）／（ＳｉＯ4/2単位）で表されるモル比が、０．５〜１．０であるオルガノポリシロキサンである。このモル比が０．５未満では、粘着力やタックが低下するおそれがあり、１．０を超える場合には、粘着力や保持力が低下するおそれがある。なお、上記モル比は０．６〜０．９が好ましい。[Component (B)]
The component (B) is an R 2 3 SiO 1/2 unit (wherein R 2 is independently a monovalent hydrocarbon group having 1 to 10 carbon atoms or 2 to 6 carbon atoms having no aliphatic unsaturated bond). An alkenyl group.) And a SiO 4/2 unit as a main component, and a molar ratio represented by (R 2 3 SiO 1/2 unit) / (SiO 4/2 unit) is 0.5 to 1.0. Is an organopolysiloxane. If this molar ratio is less than 0.5, the adhesive force and tack may be reduced, and if it exceeds 1.0, the adhesive force and holding force may be reduced. The molar ratio is preferably 0.6 to 0.9.
Ｒ2は独立に脂肪族不飽和結合を有さない炭素数１〜１０の１価炭化水素基又は炭素数２〜６のアルケニル基を示し、炭素数１〜１０の１価炭化水素基としては、例えば、メチル基、エチル基、プロピル基、ブチル基等のアルキル基、シクロヘキシル基等のシクロアルキル基、フェニル基等のアリール基等が挙げられる。中でも、メチル基、エチル基、プロピル基、ブチル基等の炭素数２〜６のアルキル基、フェニル基、トリル基等の炭素数６〜１０のアリール基が好ましい。
また、炭素数２〜６のアルケニル基としては、ビニル基、アリル基、ブテニル基等が好ましい。R 2 independently represents a monovalent hydrocarbon group having 1 to 10 carbon atoms or an alkenyl group having 2 to 6 carbon atoms that does not have an aliphatic unsaturated bond, and the monovalent hydrocarbon group having 1 to 10 carbon atoms is Examples thereof include alkyl groups such as methyl group, ethyl group, propyl group and butyl group, cycloalkyl groups such as cyclohexyl group, and aryl groups such as phenyl group. Among these, an alkyl group having 2 to 6 carbon atoms such as a methyl group, an ethyl group, a propyl group, and a butyl group, and an aryl group having 6 to 10 carbon atoms such as a phenyl group and a tolyl group are preferable.
Moreover, as a C2-C6 alkenyl group, a vinyl group, an allyl group, a butenyl group, etc. are preferable.
（Ｂ）成分は、Ｒ2以外にシラノール基や加水分解性のアルコキシ基を含んでいてもよく、アルコキシ基としては、メトキシ基、エトキシ基、イソプロポキシ基、ブトキシ基、フェノキシ基等を挙げることができ、使用する場合にはメトキシ基が好ましい。その含有量は、（Ｂ）成分の総質量の０．０１〜４．０質量％となるのが好ましく、０．０５〜３．５質量％となるのがより好ましい。上記含有量が０．０１質量％よりも少ないと粘着剤の凝集力が低くなるおそれがあり、４．０質量％よりも多いと粘着剤のタックが低下するおそれがある。The component (B) may contain a silanol group or a hydrolyzable alkoxy group in addition to R 2 , and examples of the alkoxy group include a methoxy group, an ethoxy group, an isopropoxy group, a butoxy group, and a phenoxy group. When used, a methoxy group is preferred. The content is preferably 0.01 to 4.0% by mass of the total mass of the component (B), more preferably 0.05 to 3.5% by mass. When the content is less than 0.01% by mass, the cohesive force of the pressure-sensitive adhesive may be lowered, and when it is more than 4.0% by mass, the tack of the pressure-sensitive adhesive may be reduced.
（Ｂ）成分は２種以上を併用してもよい。また、本発明の特性を損なわない範囲でＲ2ＳｉＯ3/2単位、Ｒ2 2ＳｉＯ2/2単位を（Ｂ）成分に含有させることも可能である。(B) 2 or more types of components may be used together. Further, R 2 SiO 3/2 units and R 2 2 SiO 2/2 units may be contained in the component (B) as long as the characteristics of the present invention are not impaired.
（Ｂ）成分は、触媒存在下において縮合反応させて得てもよい。これは、表面に存在する加水分解性基同士を反応させる作業であり、粘着力の向上等の効果が見込める。アルカリ性触媒を用い、室温（２５℃）〜還流下で反応させ、必要に応じて中和すればよい。
ここで、アルカリ性触媒としては、水酸化リチウム、水酸化ナトリウム、水酸化カリウム、水酸化カルシウム等の金属水酸化物；炭酸ナトリウム、炭酸カリウム等の炭酸塩；炭酸水素ナトリウム、炭酸水素カリウム等の炭酸水素塩；ナトリウムメトキシド、カリウムブトキシド等の金属アルコキシド；ブチルリチウム等の有機金属；カリウムシラノレート；アンモニアガス、アンモニア水、メチルアミン、トリメチルアミン、トリエチルアミン等の窒素化合物などが挙げられるが、アンモニアガス又はアンモニア水が好ましい。縮合反応の温度は、室温から有機溶剤の還流温度で行えばよい。反応時間は、特に限定されないが、０．５〜２０時間、好ましくは１〜１６時間とすればよい。さらに、反応終了後、必要に応じて、アルカリ性触媒を中和する中和剤を添加してもよい。中和剤としては、塩化水素、二酸化炭素等の酸性ガス；酢酸、オクチル酸、クエン酸等の有機酸；塩酸、硫酸、リン酸等の鉱酸等が挙げられる。アルカリ性触媒として、アンモニアガス又はアンモニア水、低沸点のアミン化合物を用いた場合は、窒素等の不活性ガスを通気し留去してもよい。The component (B) may be obtained by a condensation reaction in the presence of a catalyst. This is an operation for reacting hydrolyzable groups present on the surface, and an effect such as improvement in adhesive strength can be expected. What is necessary is just to make it react under room temperature (25 degreeC)-recirculation | reflux using an alkaline catalyst, and may neutralize as needed.
Here, examples of the alkaline catalyst include metal hydroxides such as lithium hydroxide, sodium hydroxide, potassium hydroxide, and calcium hydroxide; carbonates such as sodium carbonate and potassium carbonate; carbonates such as sodium hydrogen carbonate and potassium hydrogen carbonate. Hydrogen salts; Metal alkoxides such as sodium methoxide and potassium butoxide; Organic metals such as butyl lithium; Potassium silanolates; Nitrogen compounds such as ammonia gas, aqueous ammonia, methylamine, trimethylamine, and triethylamine. Ammonia water is preferred. The temperature of the condensation reaction may be from room temperature to the reflux temperature of the organic solvent. The reaction time is not particularly limited, but may be 0.5 to 20 hours, preferably 1 to 16 hours. Furthermore, a neutralizing agent that neutralizes the alkaline catalyst may be added as necessary after completion of the reaction. Examples of the neutralizing agent include acidic gases such as hydrogen chloride and carbon dioxide; organic acids such as acetic acid, octylic acid and citric acid; and mineral acids such as hydrochloric acid, sulfuric acid and phosphoric acid. When ammonia gas or ammonia water or a low-boiling amine compound is used as the alkaline catalyst, an inert gas such as nitrogen may be vented and distilled off.
本発明にかかるシリコーン粘着剤組成物において、（Ａ）成分の配合量は１００〜６０質量部、（Ｂ）成分の配合量は０〜４０質量部であって、（Ｂ）成分が含まれない場合もある。（Ａ）、（Ｂ）成分の配合質量比は、（Ａ）／（Ｂ）＝１００／０〜６０／４０であり、フィルム又はテープ等で使用する際の再剥離性の点から、１００／０〜６５／３５が好ましく、１００／０〜７０／３０がより好ましい。（Ｂ）成分の割合が４０を超えると、再剥離性が悪くなる場合がある。 In the silicone pressure-sensitive adhesive composition according to the present invention, the compounding amount of the component (A) is 100 to 60 parts by mass, the compounding amount of the component (B) is 0 to 40 parts by mass, and the component (B) is not included. In some cases. The blending mass ratio of the components (A) and (B) is (A) / (B) = 100/0 to 60/40. From the viewpoint of removability when used in a film or tape, 100 / 0-65 / 35 is preferable and 100 / 0-70 / 30 is more preferable. When the ratio of (B) component exceeds 40, re-peelability may worsen.
［（Ｃ）成分］
（Ｃ）成分は、下記平均組成式（２）で表され、１分子中に少なくとも３個のＳｉ−Ｈ基を有するオルガノハイドロジェンポリシロキサンである。
Ｒ3 eＨfＳｉＯ(4-e-f)/2 （２）
（式中、Ｒ3は独立に非置換又は置換の炭素数１〜１０の１価炭化水素基を示し、ｅ＞０、ｆ＞０であり、さらに０＜ｅ＋ｆ≦３である。）[Component (C)]
The component (C) is an organohydrogenpolysiloxane represented by the following average composition formula (2) and having at least three Si—H groups in one molecule.
R 3 e H f SiO (4-ef) / 2 (2)
(In the formula, R 3 independently represents an unsubstituted or substituted monovalent hydrocarbon group having 1 to 10 carbon atoms, e> 0, f> 0, and 0 <e + f ≦ 3.)
上記式（２）において、Ｒ3の炭素数１〜１０の１価炭化水素基としては、例えば、メチル基、エチル基、プロピル基、ブチル基等のアルキル基、シクロヘキシル基等のシクロアルキル基、ビニル基、アリル基、ヘキセニル基、オクテニル基等のアルケニル基、フェニル基等のアリール基等が挙げられる。さらに、これらの基の炭素原子に結合した水素原子の一部又は全部がハロゲン原子又はその他の基で置換されていてもよく、トリフルオロメチル基、３，３，３−トリフルオロプロピル基等が例示される。中でも、飽和の脂肪族基又は芳香族基が好ましく、メチル基、フェニル基がより好ましい。上記平均組成式（２）中、ｅ＞０、ｆ＞０であり、０＜ｅ＋ｆ≦３である。In the above formula (2), examples of the monovalent hydrocarbon group having 1 to 10 carbon atoms of R 3 include an alkyl group such as a methyl group, an ethyl group, a propyl group, and a butyl group, a cycloalkyl group such as a cyclohexyl group, Examples thereof include alkenyl groups such as vinyl group, allyl group, hexenyl group and octenyl group, and aryl groups such as phenyl group. Furthermore, some or all of the hydrogen atoms bonded to the carbon atoms of these groups may be substituted with halogen atoms or other groups, such as trifluoromethyl group, 3,3,3-trifluoropropyl group, etc. Illustrated. Among them, a saturated aliphatic group or aromatic group is preferable, and a methyl group or a phenyl group is more preferable. In the average composition formula (2), e> 0, f> 0, and 0 <e + f ≦ 3.
（Ｃ）成分としては、下記一般式（３）のものを例示することができるが、これに限定されるものではない。
Ｒ4 3Ｓｉ−Ｏ−（Ｒ5 2Ｓｉ−Ｏ）g−（Ｒ6ＨＳｉ−Ｏ）h−ＳｉＲ7 3 （３）
（式中、Ｒ4，Ｒ7はそれぞれ独立に炭素数１〜１０の１価炭化水素基又は水素原子を示し、Ｒ5，Ｒ6はそれぞれ独立に炭素数１〜１０の１価炭化水素基を示し、ｇは０≦ｇ≦１００であり、ｈは３≦ｈ≦８０である。）(C) As a component, although the thing of the following general formula (3) can be illustrated, it is not limited to this.
R 4 3 Si—O— (R 5 2 Si—O) g — (R 6 HSi—O) h —SiR 7 3 (3)
(In the formula, R 4 and R 7 each independently represent a monovalent hydrocarbon group having 1 to 10 carbon atoms or a hydrogen atom, and R 5 and R 6 each independently represent a monovalent hydrocarbon group having 1 to 10 carbon atoms. Where g is 0 ≦ g ≦ 100 and h is 3 ≦ h ≦ 80.)
上記式（３）において、Ｒ5，Ｒ6の炭素数１〜１０の１価炭化水素基としては、例えば、メチル基、エチル基、プロピル基、ブチル基等のアルキル基、シクロヘキシル基等のシクロアルキル基、ビニル基、アリル基、ヘキセニル基、オクテニル基等のアルケニル基、フェニル基等のアリール基などが挙げられる。さらに、これらの基の炭素原子に結合した水素原子の一部又は全部がハロゲン原子又はその他の基で置換されていてもよく、置換基としては、トリフルオロメチル基、３，３，３−トリフルオロプロピル基等が挙げられる。Ｒ5，Ｒ6としては、飽和の脂肪族基又は芳香族基が好ましく、メチル基、フェニル基がより好ましい。Ｒ4，Ｒ7は炭素数１〜１０の１価炭化水素基又は水素原子である。Ｒ4，Ｒ7の炭素数１〜１０の１価炭化水素基としては、上記と同様のものが例示され、Ｒ4，Ｒ7としては、メチル基、フェニル基が好ましい。ｇは０≦ｇ≦１００であり、１≦ｇ≦８０が好ましく、ｈは３≦ｈ≦８０であり、５≦ｈ≦７０が好ましい。In the above formula (3), examples of the monovalent hydrocarbon group having 1 to 10 carbon atoms of R 5 and R 6 include an alkyl group such as a methyl group, an ethyl group, a propyl group, and a butyl group, and a cyclohexane such as a cyclohexyl group. Examples include alkyl groups, vinyl groups, allyl groups, hexenyl groups, alkenyl groups such as octenyl groups, and aryl groups such as phenyl groups. Furthermore, some or all of the hydrogen atoms bonded to the carbon atoms of these groups may be substituted with halogen atoms or other groups. Examples of the substituent include a trifluoromethyl group, 3,3,3-trimethyl group. A fluoropropyl group etc. are mentioned. R 5 and R 6 are preferably a saturated aliphatic group or an aromatic group, and more preferably a methyl group or a phenyl group. R 4 and R 7 are each a monovalent hydrocarbon group having 1 to 10 carbon atoms or a hydrogen atom. Examples of the monovalent hydrocarbon group having 1 to 10 carbon atoms of R 4 and R 7 are the same as those described above. R 4 and R 7 are preferably a methyl group or a phenyl group. g is 0 ≦ g ≦ 100, preferably 1 ≦ g ≦ 80, h is 3 ≦ h ≦ 80, and preferably 5 ≦ h ≦ 70.
（Ｃ）成分は、通常、オクタメチルシクロテトラシロキサン等の環状低分子シロキサンと、テトラメチルシクロテトラシロキサン等のＳｉ−Ｈ基を含有する環状低分子シロキサンを、酸触媒を用いて開環重合させて製造するが、重合後は原料である環状低分子シロキサンを含有しているため、これを加熱及び減圧下で、反応生成物中に不活性気体を通気させながら、留去したものを用いることが好ましい。 Component (C) is usually a ring-opening polymerization of a cyclic low-molecular siloxane such as octamethylcyclotetrasiloxane and a cyclic low-molecular siloxane containing a Si—H group such as tetramethylcyclotetrasiloxane using an acid catalyst. However, after polymerization, it contains cyclic low-molecular siloxane, which is a raw material, so use it by distilling it while heating and reducing the pressure while passing an inert gas through the reaction product. Is preferred.
（Ｃ）成分の具体的な構造を表したものとしては、以下に示すようなもの等が挙げられるが、これらに限定されない。なお、下記式中のＭｅはそれぞれメチル基を示す。
（Ｃ）成分の配合量は、（Ａ）、（Ｂ）成分の合計アルケニル基に対し、Ｓｉ−Ｈ基がモル比（Ｓｉ−Ｈ基／アルケニル基）で０．２〜１５となる量であり、０．５〜１０の範囲となるように配合することが好ましい。０．２未満では架橋密度が低くなり、これにより凝集力、保持力が低くなるおそれがある。一方、１５を超えると架橋密度が高くなり適度な粘着力及びタックが得られないことがある。 The amount of component (C) is such that the Si—H group is 0.2 to 15 in molar ratio (Si—H group / alkenyl group) with respect to the total alkenyl groups of components (A) and (B). Yes, it is preferable to blend so as to be in the range of 0.5-10. If it is less than 0.2, the crosslinking density becomes low, which may cause a decrease in cohesion and holding power. On the other hand, if it exceeds 15, the crosslinking density becomes high and appropriate adhesive strength and tack may not be obtained.
［（Ｄ）成分］
（Ｄ）成分は、（Ａ）、（Ｂ）成分のアルケニル基及び（Ｃ）成分のＳｉ−Ｈ基をヒドロシリル化付加して硬化させるための白金族金属系触媒である。この触媒の中心金属としては、白金、パラジウム、イリジウム、ロジウム、オスミウム、ルテニウム等が例として挙げられ、中でも白金が好適である。白金触媒としては、塩化白金酸、塩化白金酸のアルコール溶液、塩化白金酸とアルコールとの反応物、塩化白金酸とオレフィン化合物との反応物、塩化白金酸とビニル基含有シロキサンとの反応物等が挙げられる。[(D) component]
The component (D) is a platinum group metal catalyst for hydrosilylation addition and curing of the alkenyl groups of the components (A) and (B) and the Si—H group of the component (C). Examples of the central metal of the catalyst include platinum, palladium, iridium, rhodium, osmium, ruthenium and the like, and platinum is particularly preferable. Platinum catalysts include chloroplatinic acid, alcohol solution of chloroplatinic acid, reaction product of chloroplatinic acid and alcohol, reaction product of chloroplatinic acid and olefin compound, reaction product of chloroplatinic acid and vinyl group-containing siloxane, etc. Is mentioned.
（Ｄ）成分の配合量は、上記（Ａ）〜（Ｃ）成分の総量に対し、金属質量として１〜５００ｐｐｍであり、２〜４５０ｐｐｍが好ましい。１ｐｐｍ未満だと、反応が遅く、硬化不十分となることにより粘着力や保持力の各種特性が発揮されないおそれがあり、５００ｐｐｍを超えると、硬化物の柔軟性が乏しくなる場合がある。 (D) The compounding quantity of a component is 1-500 ppm as a metal mass with respect to the total amount of the said (A)-(C) component, and 2-450 ppm is preferable. If it is less than 1 ppm, the reaction is slow and curing may be insufficient, and thus various properties such as adhesive strength and holding power may not be exhibited. If it exceeds 500 ppm, flexibility of the cured product may be poor.
［（Ｅ）成分］
（Ｅ）成分は反応制御剤であり、シリコーン粘着剤組成物を調合乃至基材上に硬化させて粘着層を形成する際に、加熱硬化の以前に付加反応が開始して処理液が増粘やゲル化を起こさないようにするために任意に添加する成分である。反応制御剤は付加反応触媒である白金族金属に配位して付加反応を抑制し、加熱硬化させるときには配位がはずれて触媒活性が発現する。付加反応硬化型シリコーン組成物に従来使用されている反応制御剤はいずれも使用することができる。具体例としては、３−メチル−１−ブチン−３−オール、３−メチル−１−ペンチン−３−オール、３，５−ジメチル−１−ヘキシン−３−オール、１−エチニルシクロヘキサノール、３−メチル−３−トリメチルシロキシ−１−ブチン、３−メチル−３−トリメチルシロキシ−１−ペンチン、３，５−ジメチル−３−トリメチルシロキシ−１−ヘキシン、１−エチニル−１−トリメチルシロキシシクロヘキサン、ビス（２，２−ジメチル−３−ブチノキシ）ジメチルシラン、１，３，５，７−テトラメチル−１，３，５，７−テトラビニルシクロテトラシロキサン、１，１，３，３−テトラメチル−１，３−ジビニルジシロキサン、マレイン酸エステル、アジピン酸エステル等が挙げられる。[(E) component]
Component (E) is a reaction control agent. When a silicone pressure-sensitive adhesive composition is prepared or cured on a substrate to form a pressure-sensitive adhesive layer, an addition reaction starts before heat curing to increase the viscosity of the treatment liquid. Or a component that is optionally added to prevent gelation. The reaction control agent coordinates to the platinum group metal which is an addition reaction catalyst to suppress the addition reaction, and when heated and cured, the coordination is lost and the catalytic activity is exhibited. Any reaction control agent conventionally used in addition reaction curable silicone compositions can be used. Specific examples include 3-methyl-1-butyn-3-ol, 3-methyl-1-pentyn-3-ol, 3,5-dimethyl-1-hexyn-3-ol, 1-ethynylcyclohexanol, 3 -Methyl-3-trimethylsiloxy-1-butyne, 3-methyl-3-trimethylsiloxy-1-pentyne, 3,5-dimethyl-3-trimethylsiloxy-1-hexyne, 1-ethynyl-1-trimethylsiloxycyclohexane, Bis (2,2-dimethyl-3-butynoxy) dimethylsilane, 1,3,5,7-tetramethyl-1,3,5,7-tetravinylcyclotetrasiloxane, 1,1,3,3-tetramethyl Examples include -1,3-divinyldisiloxane, maleic acid ester, and adipic acid ester.
（Ｅ）成分の配合量は、（Ａ）〜（Ｃ）成分の合計１００質量部に対し０．０１〜５質量部が好ましく、０．０５〜２質量部がより好ましい。 (E) As for the compounding quantity of a component, 0.01-5 mass parts is preferable with respect to a total of 100 mass parts of (A)-(C) component, and 0.05-2 mass parts is more preferable.
［その他］
（溶剤）
以上の成分を混合して得られたシリコーン粘着剤組成物において、粘度が高くハンドリングが困難な場合には、希釈するために溶剤を任意で加えてもよい。溶剤としては、トルエン、キシレン等の芳香族炭化水素系溶剤、ヘキサン、ヘプタン、オクタン、イソオクタン、デカン、シクロヘキサン、メチルシクロヘキサン、イソパラフィン等の脂肪族炭化水素系溶剤、工業用ガソリン、石油ベンジン、ソルベントナフサ等の炭化水素系溶剤、アセトン、メチルエチルケトン、２−ペンタノン、３−ペンタノン、２−ヘキサノン、２−ヘプタノン、４−ヘプタノン、メチルイソブチルケトン、ジイソブチルケトン、アセトニルアセトン、シクロヘキサノン等のケトン系溶剤、酢酸エチル、酢酸プロピル、酢酸イソプロピル、酢酸ブチル、酢酸イソブチル等のエステル系溶剤、ジエチルエーテル、ジプロピルエーテル、ジイソプロピルエーテル、ジブチルエーテル、１，２−ジメトキシエタン、１，４−ジオキサン等のエーテル系溶剤、２−メトキシエチルアセタート、２−エトキシエチルアセタート、プロピレングリコールモノメチルエーテルアセタート、２−ブトキシエチルアセタート等のエステルとエーテル部分を有する溶剤、ヘキサメチルジシロキサン、オクタメチルトリシロキサン、オクタメチルシクロテトラシロキサン、デカメチルシクロペンタシロキサン、トリス（トリメチルシロキシ）メチルシラン、テトラキス（トリメチルシロキシ）シラン等のシロキサン系溶剤、又はこれらの混合溶剤等が挙げられる。これらは１種単独で又は２種以上を適宜組み合わせて用いることができる。
溶剤の配合量は、（Ａ）〜（Ｃ）成分の合計１００質量部に対し、０〜１，０００質量部であり、好ましくは０〜８００質量部、より好ましくは０〜５００質量部である。１，０００質量部より多くなると、塗工性が悪くなる場合がある。[Others]
(solvent)
In the silicone pressure-sensitive adhesive composition obtained by mixing the above components, if the viscosity is high and handling is difficult, a solvent may be optionally added for dilution. Solvents include aromatic hydrocarbon solvents such as toluene and xylene, aliphatic hydrocarbon solvents such as hexane, heptane, octane, isooctane, decane, cyclohexane, methylcyclohexane, and isoparaffin, industrial gasoline, petroleum benzine, and solvent naphtha. Hydrocarbon solvents such as acetone, methyl ethyl ketone, 2-pentanone, 3-pentanone, 2-hexanone, 2-heptanone, 4-heptanone, methyl isobutyl ketone, diisobutyl ketone, acetonylacetone, cyclohexanone, and other ketone solvents, acetic acid Ester solvents such as ethyl, propyl acetate, isopropyl acetate, butyl acetate, isobutyl acetate, diethyl ether, dipropyl ether, diisopropyl ether, dibutyl ether, 1,2-dimethoxyethane, 1,4- Ether solvents such as oxane, 2-methoxyethyl acetate, 2-ethoxyethyl acetate, propylene glycol monomethyl ether acetate, 2-butoxyethyl acetate and other solvents having an ester and ether moiety, hexamethyldisiloxane, octa Examples thereof include siloxane solvents such as methyltrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, tris (trimethylsiloxy) methylsilane, tetrakis (trimethylsiloxy) silane, and mixed solvents thereof. These can be used individually by 1 type or in combination of 2 or more types.
The compounding amount of the solvent is 0 to 1,000 parts by mass, preferably 0 to 800 parts by mass, more preferably 0 to 500 parts by mass with respect to 100 parts by mass of the total of the components (A) to (C). . If the amount is more than 1,000 parts by mass, the coatability may be deteriorated.
［シリコーン粘着剤組成物の使用方法］
シリコーン粘着剤組成物は、上記各成分を均一に混合することにより調製できる。一般的に、シリコーン粘着剤組成物は、使用する直前に触媒を均一に混合して使用する。
硬化条件としては、８０〜１５０℃で２０秒〜１０分とすればよいがこの限りではない。
触媒を混合したシリコーン粘着剤組成物を加熱硬化して粘着層を形成する方法としては、ポッティング成型や塗工などがある。塗工方法は、公知の塗工方式を用いて塗工すればよく、例えば、コンマコーター、リップコーター、ロールコーター、ダイコーター、ナイフコーター、ブレードコーター、ロッドコーター、キスコーター、グラビアコーター、スクリーン塗工、浸漬塗工、キャスト塗工等が挙げられる。[Method of using silicone pressure-sensitive adhesive composition]
The silicone pressure-sensitive adhesive composition can be prepared by uniformly mixing the above components. Generally, a silicone pressure-sensitive adhesive composition is used by uniformly mixing a catalyst immediately before use.
The curing conditions may be 20 seconds to 10 minutes at 80 to 150 ° C., but are not limited thereto.
Examples of a method for forming a pressure-sensitive adhesive layer by heating and curing a silicone pressure-sensitive adhesive composition mixed with a catalyst include potting molding and coating. The coating method may be applied using a known coating method, for example, comma coater, lip coater, roll coater, die coater, knife coater, blade coater, rod coater, kiss coater, gravure coater, screen coating. , Dip coating, cast coating and the like.
なお、プラスチック製フィルムと粘着層の密着性を向上させるために、プラスチック製フィルムは、プライマー処理、コロナ処理、エッチング処理、プラズマ処理、サンドブラスト処理したものを用いてもよい。好ましくはコロナ処理がよい。プライマー処理はなくてもよく、プライマー層のない構成とし得る。 In order to improve the adhesion between the plastic film and the adhesive layer, the plastic film may be a primer-treated, corona-treated, etching-treated, plasma-treated or sand-blasted one. Corona treatment is preferable. There is no need for primer treatment, and a structure without a primer layer may be employed.
本発明においては、厚さ２５μｍのポリエステルフィルムの片面に、前記シリコーン粘着剤組成物の硬化物からなる粘着層が２００μｍの厚さで形成された衝撃吸収性画面保護フィルムを、衝撃試験機のロードセル上にポリエステルフィルムを上面にした状態で貼り合わせて、２５０ｍｍの高さから１５０．８ｇの鋼球をポリエステルフィルム面に落下させたときの衝撃力が、８．００ｋＮ以下であることがよく、好ましくは７．８０ｋＮ以下、より好ましくは７．５０ｋＮ以下である。衝撃力が８．００ｋＮよりも大きくなると、被着体を傷つけてしまう場合がある。 In the present invention, a shock-absorbing screen protective film in which a pressure-sensitive adhesive layer made of a cured product of the silicone pressure-sensitive adhesive composition is formed on one side of a polyester film having a thickness of 25 μm with a thickness of 200 μm is used as a load cell of an impact tester. The impact force when the polyester film is laminated on the top surface and a steel ball of 150.8 g from a height of 250 mm is dropped on the polyester film surface is preferably 8.00 kN or less, preferably Is 7.80 kN or less, more preferably 7.50 kN or less. If the impact force is greater than 8.00 kN, the adherend may be damaged.
また、本発明においては、幅２５ｍｍ、厚さ２５μｍのポリエステルフィルムの一方の面に、前記シリコーン粘着剤組成物の硬化物からなる粘着層を３０μｍの厚みで形成した粘着性フィルム（衝撃吸収性画面保護フィルム）について、該フィルムの粘着面をステンレススチール製の板に貼り合わせ、これを１８０°方向へ３００ｍｍ／分で剥離したときの粘着力が、０．０１〜２．０Ｎ／２５ｍｍの範囲であることがよく、好ましくは０．０１〜１．８Ｎ／２５ｍｍ、より好ましくは０．０１〜１．５Ｎ／２５ｍｍである。粘着力が０．０１Ｎ／２５ｍｍよりも小さいと粘着力が弱く被着体にうまく貼りつかない場合があり、２．０Ｎ／２５ｍｍよりも大きいとリワークが難しくなる場合がある。 In the present invention, a pressure-sensitive adhesive film (shock absorbing screen) in which a pressure-sensitive adhesive layer made of a cured product of the silicone pressure-sensitive adhesive composition is formed on one surface of a polyester film having a width of 25 mm and a thickness of 25 μm. For the protective film), the adhesive surface of the film is bonded to a stainless steel plate, and the adhesive strength when peeled in the direction of 180 ° at 300 mm / min is in the range of 0.01 to 2.0 N / 25 mm. It is often 0.01 to 1.8 N / 25 mm, more preferably 0.01 to 1.5 N / 25 mm. If the adhesive strength is less than 0.01 N / 25 mm, the adhesive strength is weak and may not stick well to the adherend. If it is greater than 2.0 N / 25 mm, rework may be difficult.
プラスチック製フィルムの粘着層面との反対面には、傷つき防止、汚れ防止、指紋付着防止、防眩、反射防止、帯電防止等の処理等の表面処理されたものが好ましい。粘着層を塗工してから上記の各表面処理をしてもよいし、表面処理してから粘着層を塗工してもよい。
傷つき防止処理（ハードコート処理）としては、アクリレート系、シリコーン系、オキセタン系、無機系、有機無機ハイブリッド系等のハードコート剤による処理が挙げられる。防汚処理としては、フッ素系、シリコーン系、セラミック系、光触媒系等の防汚処理剤による処理が挙げられる。反射防止処理としては、フッ素系、シリコーン系等の反射防止剤の塗工によるウェット処理や、蒸着やスパッタリングによるドライ処理が挙げられる。帯電防止処理としては、界面活性剤系、シリコーン系、有機ホウ素系、導電性高分子系、金属酸化物系、蒸着金属系等の帯電防止剤による処理が挙げられる。The surface opposite to the adhesive layer surface of the plastic film is preferably subjected to surface treatment such as scratch prevention, stain prevention, fingerprint adhesion prevention, antiglare, antireflection, antistatic treatment or the like. Each surface treatment described above may be performed after the adhesive layer is applied, or the adhesive layer may be applied after the surface treatment.
Examples of the scratch prevention treatment (hard coat treatment) include treatment with hard coat agents such as acrylate, silicone, oxetane, inorganic, and organic-inorganic hybrid. Examples of the antifouling treatment include treatment with an antifouling treatment agent such as fluorine, silicone, ceramic, and photocatalyst. Examples of the antireflection treatment include a wet treatment by applying an antireflective agent such as a fluorine type or a silicone type, and a dry treatment by vapor deposition or sputtering. Examples of the antistatic treatment include treatment with an antistatic agent such as a surfactant, silicone, organic boron, conductive polymer, metal oxide, or vapor deposition metal.
得られた衝撃吸収性画面保護フィルムは、各種ディスプレイの保護フィルム、電気絶縁フィルム、マスキングフィルム、スプライシングテープ、皮膚への貼り付けなどに用いられる。ディスプレイはガラス製あるいはプラスチック製であり、具体的には、テレビ受像機、コンピューター用モニター、携帯情報端末用モニター、監視用モニター、ビデオカメラ、デジタルカメラ、携帯電話、携帯情報端末、自動車等の計器盤用ディスプレイ、種々の設備・装置・機器の計器盤用ディスプレイ、液晶ディスプレイ、有機ＥＬディスプレイ、自動券売機、現金自動預け払い機等の文字や記号、画像を表示するための種々のタッチパネルやフラットパネルディスプレイ（ＦＰＤ）などが挙げられる。 The obtained impact-absorbing screen protective film is used for protective films for various displays, electrical insulating films, masking films, splicing tapes, affixing to skin, and the like. The display is made of glass or plastic. Specifically, TV receivers, computer monitors, monitors for personal digital assistants, monitors for monitoring, video cameras, digital cameras, mobile phones, personal digital assistants, automobiles, etc. Various touch panels and flats for displaying characters, symbols and images on panel displays, instrument panel displays for various facilities, devices and equipment, liquid crystal displays, organic EL displays, automatic ticket vending machines, automatic teller machines, etc. A panel display (FPD) is exemplified.
以下、実施例及び比較例を示し、本発明を具体的に説明するが、本発明は下記の実施例に制限されるものではない。また、Ｍｅはメチル基、Ｖｉはビニル基を表す。 EXAMPLES Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example. Me represents a methyl group and Vi represents a vinyl group.
＜ゴム硬度＞
本発明に従い作製した以下の実施例及び比較例に示すシリコーン粘着剤組成物を、アルミニウム製の容器に流し込んだ後に脱泡し、１０５℃の乾燥機で３０分乾燥させて、厚みが３ｍｍ以上の硬化物を得た。この硬化物のゴム硬度を、アスカーゴム硬度計Ｃ型を用いて測定した。<Rubber hardness>
The silicone pressure-sensitive adhesive compositions shown in the following examples and comparative examples prepared according to the present invention were defoamed after pouring into an aluminum container, dried in a dryer at 105 ° C. for 30 minutes, and the thickness was 3 mm or more. A cured product was obtained. The rubber hardness of the cured product was measured using an Asker rubber hardness meter C type.
＜衝撃力及び耐衝撃性＞
シリコーン粘着剤組成物を厚み２５μｍ、幅２５ｍｍのポリエチレンテレフタラート（ＰＥＴ）フィルムに、アプリケーターを用いて硬化後の粘着層の厚みが１５０〜４００μｍとなるよう設定して塗工した。これを１３０℃の乾燥機で２〜８分間風乾させて作製した。この粘着性フィルムを厚さ３ｍｍのガラス板に貼り合わせ、ガラスを下側に、フィルムを上側にした状態で、２５０ｍｍの高さから、直径３３．３ｍｍ、重さ１５０．８ｇの金属製の鋼球をフィルム上に落下させることにより衝撃力を測定し、ガラスが割れる（ひびが入るも含める）かガラスが割れないかで耐衝撃性を評価した。同様の試験を３回行い、ガラスが割れなかった回数で評価した（３〜０で表され数値が大きいほうが耐衝撃性が高い）。なお、試験は株式会社前川試験機製作所製の計装化鋼球落下衝撃試験システムＴＩＴ−０１−Ｉを用いた。<Impact force and impact resistance>
The silicone adhesive composition was applied to a polyethylene terephthalate (PET) film having a thickness of 25 μm and a width of 25 mm using an applicator so that the thickness of the adhesive layer after curing was 150 to 400 μm. This was produced by air drying for 2 to 8 minutes with a dryer at 130 ° C. This adhesive film is bonded to a glass plate with a thickness of 3 mm, and a metal steel with a diameter of 33.3 mm and a weight of 150.8 g from a height of 250 mm with the glass facing down and the film facing up. The impact force was measured by dropping a sphere onto the film, and the impact resistance was evaluated based on whether the glass was broken (including cracks) or not broken. The same test was performed 3 times and evaluated by the number of times that the glass did not break (the higher the numerical value expressed by 3 to 0, the higher the impact resistance). For the test, an instrumented steel ball drop impact test system TIT-01-I manufactured by Maekawa Test Co., Ltd. was used.
＜粘着力＞
シリコーン粘着剤組成物を、厚み２５μｍ、幅２５ｍｍのＰＥＴフィルムに硬化後の厚みが３０μｍとなるようにアプリケーターを用いて塗工した後、１３０℃／１分の条件で加熱し硬化させ、粘着性フィルムを作製した。この粘着性フィルムをステンレススチール板に貼りつけ、重さ２ｋｇのゴム層で被覆されたローラーを２往復させることにより圧着した。室温（２５℃）で約２０時間静置した後、引っ張り試験機を用いて３００ｍｍ／分の速度で１８０゜の角度でフィルムをステンレススチール板から引き剥がすのに要する力（Ｎ／２５ｍｍ）を測定した。<Adhesive strength>
The silicone pressure-sensitive adhesive composition is applied to a PET film having a thickness of 25 μm and a width of 25 mm using an applicator so that the thickness after curing is 30 μm, and then heated and cured under the conditions of 130 ° C./1 min, A film was prepared. This adhesive film was attached to a stainless steel plate and pressed by reciprocating a roller covered with a rubber layer having a weight of 2 kg. After standing at room temperature (25 ° C) for about 20 hours, using a tensile tester, measure the force (N / 25mm) required to peel the film from the stainless steel plate at an angle of 180 ° at a speed of 300mm / min. did.
＜シリコーン粘着剤組成物＞
［実施例１］
以下の平均組成式（Ａ−１）で表されるビニル基を有するジメチルポリシロキサン１００質量部（１００ｇあたりビニル基０．００３６モル含有）、
以下の平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン０．４７質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）、
エチニルシクロヘキサノール０．１０質量部を混合した。上記（Ａ）、（Ｃ）成分を合計１００質量部有する混合物に、１，３−ジビニル−１，１，３，３−テトラメチルジシロキサン白金（０）錯体の白金分を０．５質量％含むシリコーン溶液０．５質量部を添加し、シリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが４００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。<Silicone adhesive composition>
[Example 1]
100 parts by mass of dimethylpolysiloxane having a vinyl group represented by the following average composition formula (A-1) (containing 0.0036 mol of vinyl group per 100 g),
0.47 parts by mass of an organohydrogenpolysiloxane represented by the following average composition formula (C-1) (the Si—H group in the component (C) is moles relative to the vinyl group contained in the component (A): Ratio is 2.0)
0.10 parts by mass of ethynylcyclohexanol was mixed. In a mixture having a total of 100 parts by mass of the components (A) and (C), the platinum content of the 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum (0) complex is 0.5% by mass. A silicone pressure-sensitive adhesive composition was prepared by adding 0.5 parts by mass of the silicone solution. Using this, rubber hardness and adhesive force were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 400 μm.
［実施例２］
耐衝撃性を評価するフィルムの粘着層の厚さが２００μｍのフィルムを用いたこと以外は実施例１と同様にして評価した。[Example 2]
Evaluation was conducted in the same manner as in Example 1 except that a film having an adhesive layer thickness of 200 μm was evaluated.
［実施例３］
耐衝撃性を評価するフィルムの粘着層の厚さが１５０μｍのフィルムを用いたこと以外は実施例１と同様にして評価した。[Example 3]
Evaluation was conducted in the same manner as in Example 1 except that a film having an adhesive layer thickness of 150 μm was used to evaluate impact resistance.
［実施例４］
平均組成式（Ａ−１）で表されるビニル基を有するジメチルポリシロキサン９５質量部（１００ｇあたりビニル基０．００３６モル含有）、Ｍｅ3ＳｉＯ1/2単位及びＳｉＯ2単位を含有し、（Ｍｅ3ＳｉＯ1/2単位）／（ＳｉＯ2単位）のモル比が０．８５であるオルガノポリシロキサン（Ｂ）の６０質量％トルエン溶液を不揮発分として５質量部を混合し、減圧留去によりトルエンを除去した。そこへ、平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン０．４４質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）、エチニルシクロヘキサノール０．１０質量部を混合した。上記（Ａ）、（Ｂ）、（Ｃ）成分を合計１００質量部有する混合物に、１，３−ジビニル−１，１，３，３−テトラメチルジシロキサン白金（０）錯体の白金分を０．５質量％含むシリコーン溶液０．５質量部を添加し、シリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Example 4]
95 parts by mass of dimethylpolysiloxane having a vinyl group represented by the average composition formula (A-1) (containing 0.0036 mol of vinyl group per 100 g), Me 3 SiO 1/2 unit and SiO 2 unit ( Mixing 5 parts by mass with a 60 mass% toluene solution of organopolysiloxane (B) having a molar ratio of Me 3 SiO 1/2 unit / (SiO 2 unit) of 0.85 as a nonvolatile component, Toluene was removed. Then, 0.44 parts by mass of the organohydrogenpolysiloxane represented by the average composition formula (C-1) (the Si-H group in the component (C) is based on the vinyl group contained in the component (A)). 2.0 times in molar ratio) and 0.10 parts by mass of ethynylcyclohexanol were mixed. The platinum content of the 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum (0) complex is reduced to 0 in a mixture having a total of 100 parts by mass of the components (A), (B), and (C). 0.5 parts by mass of a silicone solution containing 5% by mass was added to prepare a silicone pressure-sensitive adhesive composition. Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［実施例５］
平均組成式（Ａ−１）で表されるビニル基を有するジメチルポリシロキサンを９０質量部（１００ｇあたりビニル基０．００３６モル含有）、Ｍｅ3ＳｉＯ1/2単位及びＳｉＯ2単位を含有し、（Ｍｅ3ＳｉＯ1/2単位）／（ＳｉＯ2単位）のモル比が０．８５であるオルガノポリシロキサン（Ｂ）の６０質量％トルエン溶液を不揮発分として１０質量部、平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン０．４２質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）としたこと以外は、実施例４と同様にして試験に用いるシリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Example 5]
90 parts by mass of dimethylpolysiloxane having a vinyl group represented by the average composition formula (A-1) (containing 0.0036 mol of vinyl group per 100 g), Me 3 SiO 1/2 unit and SiO 2 unit, Non-volatile content of 60 mass% toluene solution of organopolysiloxane (B) having a (Me 3 SiO 1/2 unit) / (SiO 2 unit) molar ratio of 0.85, an average composition formula (C— 0.42 parts by mass of the organohydrogenpolysiloxane represented by 1) (the Si—H group in the component (C) is 2.0 times in molar ratio to the vinyl group contained in the component (A)) A silicone pressure-sensitive adhesive composition used for the test was prepared in the same manner as in Example 4 except that. Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［実施例６］
以下の平均組成式（Ａ−２）で表されるビニル基を有するジメチルポリシロキサン１００質量部（１００ｇあたりビニル基０．００５３モル含有）、
平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン０．６８質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）、エチニルシクロヘキサノール０．１０質量部を混合した。上記（Ａ）、（Ｃ）成分を合計１００質量部有する混合物に、１，３−ジビニル−１，１，３，３−テトラメチルジシロキサン白金（０）錯体の白金分を０．５質量％含むシリコーン溶液０．５質量部を添加し、シリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Example 6]
100 parts by mass of dimethylpolysiloxane having a vinyl group represented by the following average composition formula (A-2) (containing 0.0053 mol of vinyl group per 100 g),
0.68 parts by mass of the organohydrogenpolysiloxane represented by the average composition formula (C-1) (Si—H groups in the component (C) are in a molar ratio with respect to the vinyl groups contained in the component (A). 2.0 times) and 0.10 parts by mass of ethinylcyclohexanol were mixed. In a mixture having a total of 100 parts by mass of the components (A) and (C), the platinum content of the 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum (0) complex is 0.5% by mass. A silicone pressure-sensitive adhesive composition was prepared by adding 0.5 parts by mass of the silicone solution. Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［実施例７］
平均組成式（Ａ−２）で表されるビニル基を有するジメチルポリシロキサン９５質量部（１００ｇあたりビニル基０．００５３モル含有）、Ｍｅ3ＳｉＯ1/2単位及びＳｉＯ2単位を含有し、（Ｍｅ3ＳｉＯ1/2単位）／（ＳｉＯ2単位）のモル比が０．８５であるオルガノポリシロキサン（Ｂ）の６０質量％トルエン溶液を不揮発分として５質量部を混合し、減圧留去によりトルエンを除去した。そこへ、平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン０．６４質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）、エチニルシクロヘキサノール０．１０質量部を混合した。上記（Ａ）、（Ｂ）、（Ｃ）成分を合計１００質量部有する混合物に、１，３−ジビニル−１，１，３，３−テトラメチルジシロキサン白金（０）錯体の白金分を０．５質量％含むシリコーン溶液０．５質量部を添加し、シリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Example 7]
95 parts by mass of dimethylpolysiloxane having a vinyl group represented by the average composition formula (A-2) (containing 0.0053 mol of vinyl group per 100 g), Me 3 SiO 1/2 unit and SiO 2 unit ( Mixing 5 parts by mass with a 60 mass% toluene solution of organopolysiloxane (B) having a molar ratio of Me 3 SiO 1/2 unit / (SiO 2 unit) of 0.85 as a nonvolatile component, Toluene was removed. Then, 0.64 parts by mass of the organohydrogenpolysiloxane represented by the average composition formula (C-1) (the Si—H group in the component (C) is based on the vinyl group contained in the component (A). 2.0 times in molar ratio) and 0.10 parts by mass of ethynylcyclohexanol were mixed. The platinum content of the 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum (0) complex is reduced to 0 in a mixture having a total of 100 parts by mass of the components (A), (B), and (C). 0.5 parts by mass of a silicone solution containing 5% by mass was added to prepare a silicone pressure-sensitive adhesive composition. Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［実施例８］
平均組成式（Ａ−２）で表されるビニル基を有するジメチルポリシロキサンを９０質量部（１００ｇあたりビニル基０．００５３モル含有）、Ｍｅ3ＳｉＯ1/2単位及びＳｉＯ2単位を含有し、（Ｍｅ3ＳｉＯ1/2単位）／（ＳｉＯ2単位）のモル比が０．８５であるオルガノポリシロキサン（Ｂ）の６０質量％トルエン溶液を不揮発分として１０質量部、平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン０．６１質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）としたこと以外は、実施例７と同様にして試験に用いるシリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Example 8]
90 parts by mass of dimethylpolysiloxane having a vinyl group represented by the average composition formula (A-2) (containing 0.0053 mol of vinyl group per 100 g), Me 3 SiO 1/2 unit and SiO 2 unit, Non-volatile content of 60 mass% toluene solution of organopolysiloxane (B) having a (Me 3 SiO 1/2 unit) / (SiO 2 unit) molar ratio of 0.85, an average composition formula (C— 1) 0.61 part by mass of the organohydrogenpolysiloxane represented by (the Si-H group in the component (C) is 2.0 times in molar ratio to the vinyl group contained in the component (A)) A silicone pressure-sensitive adhesive composition used for the test was prepared in the same manner as in Example 7 except that. Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［実施例９］
平均組成式（Ａ−２）で表されるビニル基を有するジメチルポリシロキサンを８０質量部（１００ｇあたりビニル基０．００５３モル含有）、Ｍｅ3ＳｉＯ1/2単位及びＳｉＯ2単位を含有し、（Ｍｅ3ＳｉＯ1/2単位）／（ＳｉＯ2単位）のモル比が０．８５であるオルガノポリシロキサン（Ｂ）の６０質量％トルエン溶液を不揮発分として２０質量部、平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン０．５４質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）としたこと以外は、実施例７と同様にして試験に用いるシリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Example 9]
80 parts by mass of dimethylpolysiloxane having a vinyl group represented by the average composition formula (A-2) (containing 0.0053 mol of vinyl group per 100 g), Me 3 SiO 1/2 unit and SiO 2 unit, Non-volatile content of 60 mass% toluene solution of organopolysiloxane (B) having a (Me 3 SiO 1/2 unit) / (SiO 2 unit) molar ratio of 0.85, an average composition formula (C— 1) 0.54 parts by mass of the organohydrogenpolysiloxane (the Si—H group in the component (C) is 2.0 times in molar ratio to the vinyl group contained in the component (A)) A silicone pressure-sensitive adhesive composition used for the test was prepared in the same manner as in Example 7 except that. Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［実施例１０］
平均組成式（Ａ−２）で表されるビニル基を有するジメチルポリシロキサンを６０質量部（１００ｇあたりビニル基０．００５３モル含有）、Ｍｅ3ＳｉＯ1/2単位及びＳｉＯ2単位を含有し、（Ｍｅ3ＳｉＯ1/2単位）／（ＳｉＯ2単位）のモル比が０．８５であるオルガノポリシロキサン（Ｂ）の６０質量％トルエン溶液を不揮発分として４０質量部、平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン０．４１質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）としたこと以外は、実施例７と同様にして試験に用いるシリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Example 10]
60 parts by mass of dimethylpolysiloxane having a vinyl group represented by the average composition formula (A-2) (containing 0.0053 mol of vinyl group per 100 g), Me 3 SiO 1/2 unit and SiO 2 unit, 40 parts by mass of a 60 mass% toluene solution of an organopolysiloxane (B) having a (Me 3 SiO 1/2 unit) / (SiO 2 unit) molar ratio of 0.85 as a non-volatile component, an average composition formula (C— 0.41 parts by mass of the organohydrogenpolysiloxane represented by 1) (the Si—H group in the component (C) is 2.0 times in molar ratio to the vinyl group contained in the component (A)) A silicone pressure-sensitive adhesive composition used for the test was prepared in the same manner as in Example 7 except that. Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［実施例１１］
以下の平均組成式（Ａ−３）で表されるビニル基を有するジメチルポリシロキサン６０質量部（１００ｇあたりビニル基０．００６０モル含有）、
Ｍｅ3ＳｉＯ1/2単位及びＳｉＯ2単位を含有し、（Ｍｅ3ＳｉＯ1/2単位）／（ＳｉＯ2単位）のモル比が０．８５であるオルガノポリシロキサン（Ｂ）の６０質量％トルエン溶液を不揮発分として４０質量部を混合し、減圧留去によりトルエンを除去した。そこへ、平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン０．４６質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）、エチニルシクロヘキサノール０．１０質量部を混合した。上記（Ａ）、（Ｂ）、（Ｃ）成分を合計１００質量部有する混合物に、１，３−ジビニル−１，１，３，３−テトラメチルジシロキサン白金（０）錯体の白金分を０．５質量％含むシリコーン溶液０．５質量部を添加し、シリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Example 11]
60 parts by mass of dimethylpolysiloxane having a vinyl group represented by the following average composition formula (A-3) (containing 0.0060 mol of vinyl group per 100 g),
60 mass% toluene of organopolysiloxane (B) containing Me 3 SiO 1/2 units and SiO 2 units and having a (Me 3 SiO 1/2 units) / (SiO 2 unit) molar ratio of 0.85 40 parts by mass of the solution was mixed as a nonvolatile component, and toluene was removed by distillation under reduced pressure. Then, 0.46 parts by mass of the organohydrogenpolysiloxane represented by the average composition formula (C-1) (the Si—H group in the component (C) is based on the vinyl group contained in the component (A)). 2.0 times in molar ratio) and 0.10 parts by mass of ethynylcyclohexanol were mixed. The platinum content of the 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum (0) complex is reduced to 0 in a mixture having a total of 100 parts by mass of the components (A), (B), and (C). 0.5 parts by mass of a silicone solution containing 5% by mass was added to prepare a silicone pressure-sensitive adhesive composition. Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［実施例１２］
平均組成式（Ａ−１）で表されるビニル基を有するジメチルポリシロキサン８０質量部（１００ｇあたりビニル基０．００３６モル含有）、以下の平均組成式（Ａ−４）で表されるビニル基を有するジメチルポリシロキサン２０質量部（１００ｇあたりビニル基０．０２７３モル含有）、
平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン１．０７質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）、エチニルシクロヘキサノール０．１０質量部を混合した。上記（Ａ）、（Ｃ）成分を合計１００質量部有する混合物に、１，３−ジビニル−１，１，３，３−テトラメチルジシロキサン白金（０）錯体の白金分を０．５質量％含むシリコーン溶液０．５質量部を添加し、シリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Example 12]
80 parts by mass of dimethylpolysiloxane having a vinyl group represented by the average composition formula (A-1) (containing 0.0036 mol of vinyl groups per 100 g), a vinyl group represented by the following average composition formula (A-4) 20 parts by mass of dimethylpolysiloxane having a vinyl group content of 0.0273 mol per 100 g,
1.07 parts by mass of the organohydrogenpolysiloxane represented by the average composition formula (C-1) (Si-H groups in the component (C) are in a molar ratio to the vinyl groups contained in the component (A). 2.0 times) and 0.10 parts by mass of ethinylcyclohexanol were mixed. In a mixture having a total of 100 parts by mass of the components (A) and (C), the platinum content of the 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum (0) complex is 0.5% by mass. A silicone pressure-sensitive adhesive composition was prepared by adding 0.5 parts by mass of the silicone solution. Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［実施例１３］
平均組成式（Ａ−１）で表されるビニル基を有するジメチルポリシロキサン６０質量部（１００ｇあたりビニル基０．００３６モル含有）、平均組成式（Ａ−４）で表されるビニル基を有するジメチルポリシロキサン４０質量部（１００ｇあたりビニル基０．０２７３モル含有）、平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン１．６８質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）としたこと以外は、実施例１２と同様にして試験に用いるシリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Example 13]
60 parts by mass of dimethylpolysiloxane having a vinyl group represented by the average composition formula (A-1) (containing 0.0036 mol of vinyl groups per 100 g), and having a vinyl group represented by the average composition formula (A-4) 40 parts by mass of dimethylpolysiloxane (containing 0.0273 mol of vinyl group per 100 g), 1.68 parts by mass of organohydrogenpolysiloxane represented by average composition formula (C-1) (Si—H in component (C)) A silicone pressure-sensitive adhesive composition used for the test was prepared in the same manner as in Example 12 except that the group was 2.0 times in molar ratio to the vinyl group contained in the component (A). Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［実施例１４］
平均組成式（Ａ−１）で表されるビニル基を有するジメチルポリシロキサン４０質量部（１００ｇあたりビニル基０．００３６モル含有）、平均組成式（Ａ−４）で表されるビニル基を有するジメチルポリシロキサン６０質量部（１００ｇあたりビニル基０．０２７３モル含有）、平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン２．２９質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）としたこと以外は、実施例１２と同様にして試験に用いるシリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Example 14]
40 parts by mass of dimethylpolysiloxane having a vinyl group represented by the average composition formula (A-1) (containing 0.0036 mol of vinyl groups per 100 g), and having a vinyl group represented by the average composition formula (A-4) 60 parts by mass of dimethylpolysiloxane (containing 0.0273 mol of vinyl group per 100 g), 2.29 parts by mass of organohydrogenpolysiloxane represented by the average composition formula (C-1) (Si-H in component (C)) A silicone pressure-sensitive adhesive composition used for the test was prepared in the same manner as in Example 12 except that the group was 2.0 times in molar ratio to the vinyl group contained in the component (A). Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［実施例１５］
平均組成式（Ａ−１）で表されるビニル基を有するジメチルポリシロキサン２０質量部（１００ｇあたりビニル基０．００３６モル含有）、平均組成式（Ａ−４）で表されるビニル基を有するジメチルポリシロキサン８０質量部（１００ｇあたりビニル基０．０２７３モル含有）、平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン２．８９質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）としたこと以外は、実施例１２と同様にして試験に用いるシリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Example 15]
20 parts by mass of dimethylpolysiloxane having a vinyl group represented by the average composition formula (A-1) (containing 0.0036 mol of vinyl groups per 100 g), and having a vinyl group represented by the average composition formula (A-4) 80 parts by mass of dimethylpolysiloxane (containing 0.0273 mol of vinyl group per 100 g), 2.89 parts by mass of organohydrogenpolysiloxane represented by the average composition formula (C-1) (Si—H in component (C)) A silicone pressure-sensitive adhesive composition used for the test was prepared in the same manner as in Example 12 except that the group was 2.0 times in molar ratio to the vinyl group contained in the component (A). Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［比較例１］
特許第５２３４０６４号公報に記載の実施例１に従いシリコーン組成物を得た。すなわち、平均組成式（Ａ−１）で表わされるビニル基を有するジメチルポリシロキサン４５質量部（１００ｇあたりビニル基０．００３６モル含有）、以下の平均組成式（Ａ−５）で表わされる末端がシラノール基であるジメチルポリシロキサン１５質量部、
Ｍｅ3ＳｉＯ1/2単位及びＳｉＯ2単位を含有し、（Ｍｅ3ＳｉＯ1/2単位）／（ＳｉＯ2単位）のモル比が０．８５であるオルガノポリシロキサン（Ｂ）の６０質量％トルエン溶液を不揮発分として４０質量部を混合し、そこへアンモニア水０．５質量部を加え、室温にて１２時間混合撹拌した。その後、１００〜１３０℃でアンモニア水を除去し、減圧留去によりトルエンを除去した。そこへ、以下の平均組成式（Ｃ−２）で表されるオルガノハイドロジェンポリシロキサン０．１８質量部、
以下の平均組成式（Ｃ−３）で表されるオルガノハイドロジェンポリシロキサン１．１７質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で１．５倍）、
エチニルシクロヘキサノール０．１０質量部を混合した。上記（Ａ）、（Ｂ）、（Ｃ）成分を合計１００質量部有する混合物に、１，３−ジビニル−１，１，３，３−テトラメチルジシロキサン白金（０）錯体の白金分を０．５質量％含むシリコーン溶液０．５質量部を添加し、シリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Comparative Example 1]
A silicone composition was obtained according to Example 1 described in Japanese Patent No. 5234064. That is, 45 parts by mass of dimethylpolysiloxane having a vinyl group represented by the average composition formula (A-1) (containing 0.0036 mol of vinyl groups per 100 g), and the terminal represented by the following average composition formula (A-5) 15 parts by mass of dimethylpolysiloxane which is a silanol group,
60 mass% toluene of organopolysiloxane (B) containing Me 3 SiO 1/2 units and SiO 2 units and having a (Me 3 SiO 1/2 units) / (SiO 2 unit) molar ratio of 0.85 40 parts by mass of the solution as a nonvolatile content was mixed, 0.5 parts by mass of aqueous ammonia was added thereto, and the mixture was stirred at room temperature for 12 hours. Thereafter, aqueous ammonia was removed at 100 to 130 ° C., and toluene was removed by distillation under reduced pressure. There, 0.18 parts by mass of an organohydrogenpolysiloxane represented by the following average composition formula (C-2):
1.17 parts by mass of an organohydrogenpolysiloxane represented by the following average composition formula (C-3) (the Si—H group in the component (C) is moles relative to the vinyl group contained in the component (A): Ratio 1.5 times)
0.10 parts by mass of ethynylcyclohexanol was mixed. The platinum content of the 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum (0) complex is reduced to 0 in a mixture having a total of 100 parts by mass of the components (A), (B), and (C). 0.5 parts by mass of a silicone solution containing 5% by mass was added to prepare a silicone pressure-sensitive adhesive composition. Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［比較例２］
特許第５２３４０６４号公報に記載の実施例４に従いシリコーン組成物を得た。すなわち、平均組成式（Ａ−１）で表わされるビニル基を有するジメチルポリシロキサン８５質量部（１００ｇあたりビニル基０．００３６モル含有）、以下の平均組成式（Ａ−６）で表わされる末端がシラノール基であるジメチルポリシロキサン１０質量部、
Ｍｅ3ＳｉＯ1/2単位及びＳｉＯ2単位を含有し、（Ｍｅ3ＳｉＯ1/2単位）／（ＳｉＯ2単位）のモル比が０．８５であるオルガノポリシロキサン（Ｂ）の６０質量％トルエン溶液を不揮発分として５質量部を混合し、そこへアンモニア水０．５質量部を加え、室温にて１２時間混合撹拌した。その後、１００〜１３０℃でアンモニア水を除去し、減圧留去によりトルエンを除去した。そこへ、平均組成式（Ｃ−２）で表されるオルガノハイドロジェンポリシロキサン０．５８質量部、平均組成式（Ｃ−３）で表されるオルガノハイドロジェンポリシロキサン２．２２質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で１．９倍）、エチニルシクロヘキサノール０．１０質量部を混合した。上記（Ａ）、（Ｂ）、（Ｃ）成分を合計１００質量部有する混合物に、１，３−ジビニル−１，１，３，３−テトラメチルジシロキサン白金（０）錯体の白金分を０．５質量％含むシリコーン溶液０．５質量部を添加し、シリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Comparative Example 2]
A silicone composition was obtained according to Example 4 described in Japanese Patent No. 5234064. That is, 85 parts by mass of dimethylpolysiloxane having a vinyl group represented by the average composition formula (A-1) (containing 0.0036 mol of vinyl groups per 100 g), and the terminal represented by the following average composition formula (A-6) 10 parts by mass of dimethylpolysiloxane which is a silanol group,
60 mass% toluene of organopolysiloxane (B) containing Me 3 SiO 1/2 units and SiO 2 units and having a (Me 3 SiO 1/2 units) / (SiO 2 unit) molar ratio of 0.85 5 parts by mass was mixed with the solution as a non-volatile component, 0.5 parts by mass of aqueous ammonia was added thereto, and the mixture was stirred at room temperature for 12 hours. Thereafter, aqueous ammonia was removed at 100 to 130 ° C., and toluene was removed by distillation under reduced pressure. There, 0.58 parts by mass of the organohydrogenpolysiloxane represented by the average composition formula (C-2) and 2.22 parts by mass of the organohydrogenpolysiloxane represented by the average composition formula (C-3) (( C) Si—H group in component (1.9 times in molar ratio with respect to vinyl group contained in component (A)) was mixed with 0.10 parts by mass of ethynylcyclohexanol. The platinum content of the 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum (0) complex is reduced to 0 in a mixture having a total of 100 parts by mass of the components (A), (B), and (C). 0.5 parts by mass of a silicone solution containing 5% by mass was added to prepare a silicone pressure-sensitive adhesive composition. Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
［比較例３］
平均組成式（Ａ−４）で表されるビニル基を有するジメチルポリシロキサン１００質量部（１００ｇあたりビニル基０．０２７３モル含有）、平均組成式（Ｃ−１）で表されるオルガノハイドロジェンポリシロキサン３．５０質量部（（Ｃ）成分中のＳｉ−Ｈ基は、（Ａ）成分中に含まれるビニル基に対しモル比で２．０倍）、エチニルシクロヘキサノール０．１０質量部を混合した。上記（Ａ）、（Ｃ）成分を合計１００質量部有する混合物に、１，３−ジビニル−１，１，３，３−テトラメチルジシロキサン白金（０）錯体の白金分を０．５質量％含むシリコーン溶液０．５質量部を添加し、シリコーン粘着剤組成物を作製した。これを用い、ゴム硬度と粘着力を測定し、粘着層の厚さが２００μｍのフィルムを用いて衝撃力及び耐衝撃性を評価した。[Comparative Example 3]
100 parts by mass of dimethylpolysiloxane having a vinyl group represented by an average composition formula (A-4) (containing 0.0273 mol of vinyl groups per 100 g), an organohydrogen poly represented by an average composition formula (C-1) 3.50 parts by mass of siloxane (Si-H group in component (C) is 2.0 times in molar ratio to vinyl group in component (A)) and 0.10 parts by mass of ethynylcyclohexanol are mixed. did. In a mixture having a total of 100 parts by mass of the components (A) and (C), the platinum content of the 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum (0) complex is 0.5% by mass. A silicone pressure-sensitive adhesive composition was prepared by adding 0.5 parts by mass of the silicone solution. Using this, rubber hardness and adhesive strength were measured, and impact force and impact resistance were evaluated using a film having an adhesive layer thickness of 200 μm.
実施例１〜１５においては、いずれの硬化物のゴム硬度も４０〜７５であり、フィルムの耐衝撃性は良好なものであった。しかし、比較例１，２では、硬化物のゴム硬度が４０未満であることから強度が弱く、鋼球落下試験における耐衝撃性は劣る結果であった。比較例１，２は、末端がシラノール基のオルガノポリシロキサンをアンモニアにより縮合させる、架橋剤に末端ヒドロシリル基を有するものを併用するなどして、硬化物に柔軟性をもたせていることから、無溶剤型で厚塗りが可能となるが、耐衝撃性は本発明に及ばないことがわかる。また比較例３では、ゴム硬度が７６と高くなっており、衝撃を十分に吸収できなかったために耐衝撃性が悪くなったものと考えられる。 In Examples 1 to 15, the rubber hardness of any cured product was 40 to 75, and the impact resistance of the film was good. However, in Comparative Examples 1 and 2, since the rubber hardness of the cured product was less than 40, the strength was weak, and the impact resistance in the steel ball drop test was inferior. In Comparative Examples 1 and 2, the cured product is made flexible by condensing organopolysiloxane having a terminal silanol group with ammonia, or using a crosslinking agent having a terminal hydrosilyl group. It can be seen that thick coating is possible with a solvent type, but the impact resistance does not reach the present invention. In Comparative Example 3, the rubber hardness was as high as 76, and it was considered that the impact resistance deteriorated because the impact could not be sufficiently absorbed.
Claims (9)
（Ａ）下記平均組成式（１）で表される、１分子中に少なくとも２個のアルケニル基含有有機基を有し、１００ｇ中にアルケニル基０．００１〜０．０５モルが含まれるオルガノポリシロキサン：１００〜６０質量部、
（Ｂ）Ｒ2 3ＳｉＯ1/2単位（式中、Ｒ2は独立に脂肪族不飽和結合を有さない炭素数１〜１０の１価炭化水素基又は炭素数２〜６のアルケニル基を示す。）とＳｉＯ4/2単位を主成分とし、（Ｒ2 3ＳｉＯ1/2単位）／（ＳｉＯ4/2単位）がモル比で０．５〜１．０であるオルガノポリシロキサン：０〜４０質量部、
（Ｃ）下記平均組成式（２）で表され、１分子中に少なくとも３個のＳｉ−Ｈ基を有するオルガノハイドロジェンポリシロキサン：（Ａ）、（Ｂ）成分の合計アルケニル基に対し、Ｓｉ−Ｈ基がモル比で０．２〜１５となる量、
Ｒ3 eＨfＳｉＯ(4-e-f)/2 （２）
（式中、Ｒ3は独立に非置換又は置換の炭素数１〜１０の１価炭化水素基を示し、ｅ＞０、ｆ＞０であり、さらに０＜ｅ＋ｆ≦３である。）
（Ｄ）（Ａ）、（Ｂ）成分のアルケニル基と（Ｃ）成分のＳｉ−Ｈ基をヒドロシリル化付加して硬化させるための白金族金属系触媒：上記（Ａ）〜（Ｃ）成分の総量に対し、金属質量が１〜５００ｐｐｍとなる量
を含むことを特徴とする請求項１乃至６のいずれか１項に記載の衝撃吸収性画面保護フィルム。The silicone pressure-sensitive adhesive composition is
(A) Organopoly having at least two alkenyl group-containing organic groups in one molecule and 0.001 to 0.05 mol of alkenyl groups in 100 g, represented by the following average composition formula (1) Siloxane: 100-60 parts by mass,
(B) R 2 3 SiO 1/2 unit (wherein R 2 independently represents a monovalent hydrocarbon group having 1 to 10 carbon atoms or an alkenyl group having 2 to 6 carbon atoms which does not have an aliphatic unsaturated bond). And an organopolysiloxane having a SiO 4/2 unit as a main component and (R 2 3 SiO 1/2 unit) / (SiO 4/2 unit) in a molar ratio of 0.5 to 1.0: 0 ~ 40 parts by mass,
(C) Organohydrogenpolysiloxane represented by the following average composition formula (2) and having at least 3 Si—H groups in one molecule: (A), Si (V) with respect to the total alkenyl groups of the components An amount such that the —H group has a molar ratio of 0.2 to 15;
R 3 e H f SiO (4-ef) / 2 (2)
(In the formula, R 3 independently represents an unsubstituted or substituted monovalent hydrocarbon group having 1 to 10 carbon atoms, e> 0, f> 0, and 0 <e + f ≦ 3.)
(D) Platinum group metal catalyst for hydrosilylation addition and curing of alkenyl group of components (A) and (B) and Si—H group of component (C): of components (A) to (C) above The impact-absorbing screen protection film according to any one of claims 1 to 6, comprising an amount such that the metal mass is 1 to 500 ppm relative to the total amount.
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| EP3645651B1 (en) | 2017-10-19 | 2023-09-06 | Dow Silicones Corporation | A method for fabricating a flexible organic light emitting diode using a pressure sensitive adhesive composition |
| WO2020158640A1 (en) * | 2019-01-29 | 2020-08-06 | パナソニックＩｐマネジメント株式会社 | Shock absorbing material |
| WO2022019285A1 (en) * | 2020-07-21 | 2022-01-27 | パナソニック株式会社 | Shock absorbing material |
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- 2016-10-11 WO PCT/JP2016/080096 patent/WO2017065131A1/en active Application Filing
- 2016-10-11 JP JP2017545197A patent/JPWO2017065131A1/en active Pending
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