TWI374173B - - Google Patents

Description

1374173 (1) 九、發明說明 【發明所屬之技術領域】 本發明係關於一種具有可被調節之黏著力的聚矽氧黏 * 著劑組成物。 【先前技術】 使用聚矽氧黏著劑之黏著膠帶或黏著標籤係因聚矽氧 φ 黏著劑層具有優異之耐熱性、耐寒性、耐候性、電絕緣性 及耐藥品性，故在亞克力系黏著劑、橡膠系黏著劑等之有 機系黏著劑係在如會變質、劣化之嚴格環境下被使用。即 • 使對於各種被黏體亦良好地黏著，故亞克力系黏著劑、橡 . 膠系黏著劑等之有機系黏著劑係對黏著困難之聚烯烴樹脂 、聚砂氧樹脂、氟樹脂、含有水分之表面被使用。 例如，電子、電氣零件製造時或加工時、組裝時可使 用一利用聚矽氧黏著劑之黏著膠帶。在此製造步驟中進行 φ 加熱處理時，有時必須全面或部分地保護或遮蔽或暫時固 定。如此之用途所使用之黏著膠帶，或曝露於高溫之電子 /電器零件的製品、固定、結束等使用的黏著膠帶中，即 使超過250°C之加熱後，使用一具有耐熱性之聚矽氧黏著 劑亦適宜。但，近年，製造電子/電氣零件、加工的步驟 '係呈多階段，有時亦反覆加熱、冷却、洗淨、照射等，高 度精密化、複雜化。進一步，以無塵化爲目的下，亦常在 無塵室、無塵屋等被密閉之空間內進行處理。 將一使用習知之聚矽氧黏著劑的黏著膠帶或黏著標籤 -4- (2) 1374173 貼在被黏體上或遮蔽，受到100~250°C之高溫履歷時，有 時殘留於黏著劑層之微量甲苯、二甲苯、乙基苯、苯等之 芳香族烴會揮發。此等芳香族烴係已含於聚矽氧黏著劑組 • 成物者。在如上述之電氣/電子零件的製造步驟中被封閉 .. 的空間，使用一利用聚矽氧黏著劑之黏著膠帶，會產生芳 香族烴的揮發物質，進一步在其後之步驟中，進行紫外線 照射時，紫外線會被芳香族烴吸收，有時招致不能有效率 φ 地照射之問題。 進一步，近年之電子零件係正進行小型化、微細化、 薄型化。以利用習知被廣泛使用之聚矽氧黏著劑的黏著膠 - 帶爲了保護進行遮蔽時，進行特定處理之後，於剝離遮蔽 . 膠帶時（再剝離），黏著力太強而被黏體之電子零件上的微 細構造或電子零件本身會變形、或破壞。又，遮蔽此等電 子零件時，亦有時於廣面積進行貼上膠帶之作業。剝離貼 於廣面積之遮蔽膠帶時，若黏著力太強，很難剝離，或被 φ 黏體會變形、或破壞。又，除黏著膠帶以外，被黏著加工 之膜貼在被黏體時，若黏著膜之黏著力太強，很難剝離， 或被黏體會變形、或破壞。此被黏體係可舉例各種之電子 零件、平面狀顯示器、玻璃窗、壁面等，被黏著加工之膜 係可舉例：防污膜、防刮傷膜、反射抑制膜、遮光膜、防 * 爆玻璃膜，用以裝飾或廣告之遮蔽膜等。 在建築、內裝等之黏著膠帶、黏著標籤的用途上，被 黏體之表面以撥水、撥油、防污等爲目的，有時含有聚矽 氧樹脂或氟樹脂，有時被聚矽氧處理、氟處理。在如此之 -5- (3) 1374173 表面上因以亞克力系黏著劑不會良好地黏著，故有時可使 用聚矽氧黏著劑。壁紙貼黏用黏著紙、家倶等之化粧板等 貼黏用黏著紙、防水/氣密用黏著膠帶、屋內內裝固定用 * 黏著膠帶、修補用膠帶、製飾固定用膠帶、防爆玻璃用黏 , 著膜、遮光用黏著膜、汽車內裝固定用膠帶等居住環境所 使用之黏著膠帶、黏著標籤中，係芳香族烴溶劑會殘留， 其揮發，滯留於室內空氣時，即使其爲極微量，亦恐成爲 Φ 化學物質過敏、疾病建物症候群、化學物質敏感症等之原 因。 進一步，在如貼藥或絆創膏、手術膠帶、運動用膠布 膠帶等直接貼在皮膚的用途，若有芳香族烴溶劑之殘留， . 會對皮膚造成刺激。 爲解決如此之問題，已知有一種無溶劑型聚矽氧感壓 接著劑組成物，其係由於直鏈狀分子鏈（不具有分枝）之兩 末端具有低級烯基的聚有機矽氧烷、含R3SiOQ.5單元及 φ Si02單元之聚有機矽氧烷，於1分子中至少具有2個SiH之 有機氫聚矽氧烷、鈾系觸媒所構成者（專利文獻1)。此物 有時係交聯密度變低，用於遮蔽膠帶係黏著力高達必要以 上，且再剝離性差。 (專利文獻1)特開平6-84494號公報 【發明內容】 發明欲解決之問題 本發明之目的在於提供一種聚矽氧黏著劑組成物，其 -6 - (4) 1374173 係不含有機溶劑，而可防止所殘留、揮發之物質造成的、 紫外線照射等之吸收、電子/電氣零件的污染、對人體之 影響、對皮膚之刺激，又且，不使被黏體變形或破壞而再 • 剝離容易、可調整黏著力者。 [用以解決課題之手段] 本發明人等經專心硏究之結果發現，使用一種無溶劑 φ 型聚矽氧黏著劑組成物作爲聚矽氧黏著劑組成物，可有效 達成下述目的。而該無溶劑型聚矽氧黏著劑組成物，其係 含有：（A)於一分子中至少具有2個含烯基的有機基，且具 • 有分枝之聚二有機矽氧烷；（B)於一分子中至少具有2個 、 SiH基的聚有機氫矽氧烷：（〇含有R^SiOo.s單元及Si02 單元且R^SiOo.s單元/Si02單元的莫耳比爲〇.6~1.7之聚有 機矽氧烷（R1係碳數1至10之一價烴基）；（D)鉑系觸媒。 進一步若使用一種無溶劑型聚矽氧黏著劑組成物，其 φ 係相對於上述之（A)、（B)、（C)成分之合計1〇〇質量份，（A) 、（B)成分之合計爲90~30質量份，但（B)成份中之SiH基 對（A)成分中之烯基的莫耳比成爲〇·5〜5之量，（C)成分爲 10~70質量份（D)成分之鉑觸媒含有5〜2000ppm作爲鉑成分 ;發現可有效達成下述目的》即不含有機溶劑，而可防止 所殘留、揮發之物質造成的、紫外線照射等之吸收、電子 /電氣零件的污染、對人體之影響、對皮膚之刺激，又且 ’可有效使用於一不使被黏體變形或破壞而再剝離容易、 可調整黏著力之黏著膠帶、黏著膜' 黏著片、黏著標鐵用 (5) 13741731374173 (1) Description of the Invention [Technical Field of the Invention] The present invention relates to a polyoxyxene adhesive composition having an adhesive property that can be adjusted. [Prior Art] Adhesive tape or adhesive label using a polyoxygenated adhesive is adhesive in the acrylic layer because of its excellent heat resistance, cold resistance, weather resistance, electrical insulation and chemical resistance. Organic adhesives such as agents and rubber-based adhesives are used in a strict environment where deterioration or deterioration occurs. That is, it is also good adhesion to various adherends, so the organic adhesives such as acrylic adhesives, rubber adhesives, etc. are difficult to adhere to polyolefin resin, polyoxyn resin, fluororesin, and moisture. The surface is used. For example, an adhesive tape using a polyoxygenated adhesive can be used in the manufacture of electronic or electrical parts, during processing, or during assembly. When the φ heat treatment is carried out in this manufacturing step, it is sometimes necessary to fully or partially protect or shield or temporarily fix. Adhesive tape used for such use, or adhesive tape exposed to high-temperature electronic/electrical parts, fixing, finishing, etc., even after heating at more than 250 ° C, using a heat-resistant polyoxygen adhesive The agent is also suitable. However, in recent years, the steps of manufacturing electronic/electrical parts and processing have been carried out in multiple stages, and sometimes repeated heating, cooling, washing, and irradiation have been highly sophisticated and complicated. Further, for the purpose of dust-free, it is often treated in a sealed space such as a clean room or a clean room. Adhesive tape or adhesive label -4- (2) 1374173 using a conventional polyoxygen adhesive is attached to the adherend or shielded. When subjected to a high temperature history of 100 to 250 ° C, it sometimes remains in the adhesive layer. A trace amount of aromatic hydrocarbons such as toluene, xylene, ethylbenzene, and benzene are volatilized. These aromatic hydrocarbons are already contained in the polyoxygen adhesive group. In the space where the electrical/electronic parts are manufactured as described above, using a sticky tape using a polyoxygen adhesive, a volatile substance of aromatic hydrocarbons is generated, and in the subsequent step, ultraviolet rays are irradiated. When irradiated, ultraviolet rays are absorbed by aromatic hydrocarbons, and there is a problem that illumination cannot be efficiently performed. Further, in recent years, electronic components are being miniaturized, miniaturized, and thinned. In order to protect the masking adhesive, the adhesive is used for the purpose of protection. After the specific treatment, the adhesive is peeled off. When the tape is removed (re-peeling), the adhesion is too strong and the electrons are adhered. The fine structure on the part or the electronic part itself may be deformed or destroyed. Moreover, when these electronic components are shielded, the tape may be attached to a wide area. When peeling off a masking tape of a wide area, if the adhesion is too strong, it is difficult to peel off, or the φ adhesive may be deformed or broken. Further, in addition to the adhesive tape, when the film to be adhered is attached to the adherend, if the adhesive force of the adhesive film is too strong, it is difficult to peel off, or the adherend may be deformed or broken. The adhered system can be exemplified by various electronic parts, flat displays, glass windows, wall surfaces, etc., and the film system to be adhered can be exemplified by an antifouling film, a scratch resistant film, a reflection suppressing film, a light shielding film, and an anti-explosive glass. Membrane, masking film for decoration or advertising, etc. In the use of adhesive tapes and adhesive labels for construction, interiors, etc., the surface of the adherend is intended to be water-repellent, oil-repellent, anti-fouling, etc., sometimes containing polyoxyn resin or fluororesin, sometimes being aggregated. Oxygen treatment, fluorine treatment. On such a surface of -5-(3) 1374173, since the acrylic adhesive does not adhere well, a polyoxygen adhesive can sometimes be used. Sticky adhesive tape for adhesives such as adhesive paper, home decoration, etc. Adhesive tape for waterproofing, airtight/adhesive adhesive tape, interior fixing for use* Adhesive tape, repair tape, decorative fixing tape, explosion-proof glass In an adhesive tape or an adhesive label used in a living environment such as a film for adhesion, film, light-shielding adhesive film, or automobile interior fixing tape, an aromatic hydrocarbon solvent remains, and when it is volatilized, it stays in indoor air, even if it is It is extremely rare, and it may become a cause of Φ chemical allergy, disease building syndrome, and chemical substance sensitivity. Further, if it is applied directly to the skin such as a patch or a plaster, a surgical tape, or a sports tape, if it is left with an aromatic hydrocarbon solvent, it may cause irritation to the skin. In order to solve such a problem, there is known a solvent-free polyfluorene-sensitive pressure-sensitive adhesive composition which is a polyorganosiloxane having a lower alkenyl group at both ends of a linear molecular chain (having no branching) A polyorganosiloxane containing R3SiOQ.5 unit and φSiO 2 unit, which is composed of an organic hydrogen polyoxyalkylene having at least two SiHs and a uranium-based catalyst in one molecule (Patent Document 1). This material sometimes has a low crosslink density, and is used for the masking tape to have an adhesive force as high as necessary, and the removability is poor. SUMMARY OF THE INVENTION PROBLEMS TO BE SOLVED BY THE INVENTION An object of the present invention is to provide a composition of a polyoxyxylene adhesive, which is free of organic solvents, -6 - (4) 1374173 It can prevent the absorption of ultraviolet rays and other substances caused by residual and volatilized substances, the contamination of electronic/electrical parts, the influence on the human body, the stimulation to the skin, and the deformation or destruction of the adherends. Easy, adjustable adhesion. [Means for Solving the Problem] As a result of intensive research, the present inventors have found that the use of a solvent-free φ-type polyoxyxide adhesive composition as a composition of a polyoxyxide adhesive can effectively achieve the following object. The solvent-free polyoxyxene adhesive composition comprises: (A) an organic group having at least two alkenyl groups in one molecule, and having a branched polydiorganotoxime; B) Polyorganohydroquinone having at least two, SiH groups in one molecule: (〇 contains R^SiOo.s unit and SiO 2 unit and the molar ratio of R^SiOo.s unit/SiO2 unit is 〇. a polyorganosiloxane of 6 to 1.7 (R1 is a monovalent hydrocarbon group having 1 to 10 carbon atoms); (D) a platinum-based catalyst. Further, if a solvent-free polyoxyxene adhesive composition is used, the φ system is relatively The total of the components (A), (B), and (C) is 1 part by mass, and the total of the components (A) and (B) is 90 to 30 parts by mass, but the SiH group in the component (B) The molar ratio of the alkenyl group in the component (A) is 〇·5 to 5, and the component (C) is 10 to 70 parts by mass. The platinum catalyst of the component (D) contains 5 to 2000 ppm as a platinum component; It achieves the following objectives: that is, it does not contain organic solvents, and it can prevent the absorption of ultraviolet rays and the like caused by substances remaining and volatilized, the contamination of electronic/electrical parts, the influence on the human body, and the skin. Stimulation, and it "can be used effectively without being sticky in a deformation or destruction readily removable, adjustable adhesive force of adhesive tape, adhesive film 'adhesive sheet, the adhesive with a standard iron (5) 1374173

[發明之效果] * 依本發明，可得到不含芳香族溶劑之無溶劑型聚矽氧 , 黏著劑組成物。無芳香族溶劑殘留於黏著膠帶造成之弊害 。再剝離時不使被黏體破壞、變形。 φ [用以實施發明之最佳形態] 以下，若更詳細述之，（A)成分爲具有：以下述平均 組成式（1)所示且在25°C之黏度爲5~1000mPa.s的分子中具 • 有分枝之含烯基的有機基之聚二有機矽氧烷。 (R3Si01/2)a-(R2Si0)b-(RSi03/2)c-(Si02)d (1) (其中，R可爲相同或相異之碳數1〜10的1價烴基，R φ 之中至少2個含有烯基之有機基；a爲2以上之整數，b爲3 以上之整數，c及d爲0以上之整數，ISc + d、a + b + c + dS 400) » R爲碳數1〜10之1價烴基，全R基之中2個以上爲含烯 基之有機基。具體上係亦可例示甲基、乙基、丙基、丁基 ' 等之烷基，環己基等的環烷基、苯基、甲苯基等之芳基等 ，進一步，以其他之基取代結合於此等之基的碳原子之氫 原子的一部分或全部，即3，3，3 -三氟丙基、3 -羥丙基 、3-胺基丙基等。尤其宜爲甲基、苯基。 -8- (6) (6)1374173 又，含有烯基之有機基宜爲碳數2〜10者，爲乙烯基、 烯丙基、己烯基、辛烯基、丙烯醯基丙基、丙燃醯基甲基 '甲基丙烯醯基丙基、環己烯基乙基、乙烯氧基丙基等， 尤其工業上宜爲乙烯基》 此處，a、b、c、d係使此聚有機矽氧烷之25 °C的黏度 爲5〜lOOOmPas之數，但具體上a爲2以上之整數，b爲3 以上之整數，c及d爲0以上之整數，lgc + d、a + b + c + dg 400，但較佳係a爲3以上之整數，b爲10以上之整數，c 及d爲0以上之整數，ISc + d、a + b + c + d$ 250。 (A)成分爲具有：以下述平均組成式（4)所示且在25°C 之黏度爲5~1〇0〇 mPa‘s的分子中具有分枝之含烯基的有機 基之聚亡有機矽氧烷。 (R3Si〇i/2)c + 2-(R2SiO)b-(RSi03/2)c (4) (其中，R表示與上述相同之基；b爲3以上之整數，c 爲1以上之整數，b + 2 + c + 2‘ 400) 進一步，（A)成分如以下述平均組成式所示般，更宜 爲於分子鏈之末端具有含有烯基之有機基者。 (XR2Si01/2)a-(R2Si0)b-(RSi03/2)c-(Si02)d (XR2Si〇i/2)c + 2-(R2SiO)b-(RSi03/2)c X爲前述含有烯基之有機基，R、a、b、c、d係與前 1374173 ⑺ 述相同* (Α)成分之烯基含量宜爲0·005~〇·25莫耳/l〇〇g ,更宜 爲〇.008~0.1莫耳/i〇〇g，0.005莫耳/100g以下時，黏著力 1 太高，〇·25莫耳/I00g以上時，黏著力或黏性會太低，不 ·. 適合。 (A) 成分之黏度宜在25°c下爲5~1000mPa.s，尤宜爲 5〇〜700mPai。在5mPa_s以下時硬化性降低，黏著力下降 φ ’故不適宜。若超過1〇〇〇 mPa.s，組成物成爲過高黏度而 製造時之攪拌或塗布變困難。進一步，（A)成分亦可併用2 種以上。 (A)成分一般係利用觸媒而使八甲基環四矽氧烷等之 . 單體、與具有二甲基乙烯基矽氧烷單元的矽烷化合物或矽 氧烷化合物、具有甲基矽氧單元之矽烷化合物或矽氧烷化 合物聚合來製造，但，聚合後含有環狀之低分子矽氧烷， 故宜使用此環狀低分子矽氧烷加熱及/或在減壓下通入惰 φ 性氣體同時並餾去者。 (B) 成分係交聯劑，且於1分子中至少具有2個結合於 矽原子之氫原子的聚有機氫矽氧烷，可使用直鏈狀、分枝 狀、環狀者。就（B)成分，具體上可例示下述式（2)及（3)者 ，但不限於此等者。 【化1】[Effect of the Invention] According to the present invention, a solvent-free polyfluorene-oxygen and an adhesive composition containing no aromatic solvent can be obtained. No aromatic solvents remain in the adhesive tape and cause the harm. When peeling again, the adherend is not broken or deformed. φ [Best Mode for Carrying Out the Invention] Hereinafter, as described in more detail, the component (A) has a viscosity of 5 to 1000 mPa·s as shown by the following average composition formula (1) and at 25 ° C. A polydiorganooxynonane having a branched alkenyl group-containing organic group in the molecule. (R3Si01/2)a-(R2Si0)b-(RSi03/2)c-(Si02)d (1) (wherein R may be the same or different monovalent hydrocarbon group having a carbon number of 1 to 10, R φ At least two organic groups having an alkenyl group; a is an integer of 2 or more, b is an integer of 3 or more, and c and d are integers of 0 or more, ISc + d, a + b + c + dS 400) » R is A monovalent hydrocarbon group having 1 to 10 carbon atoms, and two or more of the entire R groups are an alkenyl group-containing organic group. Specifically, an alkyl group such as a methyl group, an ethyl group, a propyl group or a butyl group, a cycloalkyl group such as a cyclohexyl group, an aryl group such as a phenyl group or a tolyl group, or the like may be exemplified, and further, the group may be substituted by another group. Some or all of the hydrogen atoms of the carbon atom of these groups, that is, 3,3,3-trifluoropropyl, 3-hydroxypropyl, 3-aminopropyl, and the like. It is especially preferably a methyl group or a phenyl group. -8- (6) (6) 1374173 Further, the organic group having an alkenyl group is preferably a carbon number of 2 to 10, and is a vinyl group, an allyl group, a hexenyl group, an octenyl group, an acryloyl propyl group, or a propylene group. A hydrazinyl methyl 'methacryl decyl propyl group, a cyclohexenyl ethyl group, a vinyl oxy propyl group, etc., especially industrially suitable as a vinyl group. Here, a, b, c, d system makes this poly The viscosity of the organic alkane at 25 ° C is 5 to 1000 mPas, but specifically a is an integer of 2 or more, b is an integer of 3 or more, and c and d are integers of 0 or more, lgc + d, a + b + c + dg 400, but preferably a is an integer of 3 or more, b is an integer of 10 or more, and c and d are integers of 0 or more, ISc + d, a + b + c + d$ 250. The component (A) has a group of organic groups having a branched alkenyl group in a molecule having an average composition formula (4) and having a viscosity of 5 to 1 〇 0 〇 mPa's at 25 ° C. Organic oxirane. (R3Si〇i/2)c + 2-(R2SiO)b-(RSi03/2)c (4) (wherein R represents the same group as above; b is an integer of 3 or more, and c is an integer of 1 or more, b + 2 + c + 2' 400) Further, the component (A) is preferably an organic group having an alkenyl group at the terminal of the molecular chain as shown by the following average composition formula. (XR2Si01/2)a-(R2Si0)b-(RSi03/2)c-(SiO2)d (XR2Si〇i/2)c + 2-(R2SiO)b-(RSi03/2)c X is the aforementioned alkene The organic group of the base, R, a, b, c, d is the same as the former 1374173 (7) * The alkenyl content of the * (Α) component is preferably 0·005~〇·25 mol/l〇〇g, more preferably 〇.008~0.1mol/i〇〇g, 0.005mol/100g or less, the adhesion force 1 is too high, when 〇·25mol/I00g or more, the adhesion or viscosity will be too low, not. . (A) The viscosity of the component should be 5 to 1000 mPa.s at 25 ° C, and particularly preferably 5 to 700 mPa. When the hardness is 5 mPa_s or less, the hardenability is lowered, and the adhesive force is lowered by φ', which is not preferable. If it exceeds 1 〇〇〇 mPa.s, the composition becomes too high in viscosity and it becomes difficult to stir or apply at the time of manufacture. Further, the component (A) may be used in combination of two or more kinds. The component (A) is generally obtained by using a catalyst such as octamethylcyclotetraoxane or the like. Monomer, a decane compound having a dimethylvinyl siloxane unit or a decane compound, having a methyl oxime The unit is produced by polymerizing a decane compound or a decane compound, but after polymerization, it contains a cyclic low molecular oxymethane, so it is preferred to use the cyclic low molecular siloxane to heat and/or to introduce inertia under reduced pressure. The gas is simultaneously distilled. (B) The component is a cross-linking agent, and a polyorganohydroquinone having at least two hydrogen atoms bonded to a halogen atom in one molecule can be used in a linear form, a branched form, or a ring shape. The component (B) is specifically exemplified by the following formulas (2) and (3), but is not limited thereto. 【化1】

HH

R oR o

\J/ 2 i 2 R 丨 s — R ___' a \-/ *1 2 H 丨 s— R R — Η -10- (8) 1374173 及/或 【化2】\J/ 2 i 2 R 丨 s — R ___' a \-/ *1 2 H 丨 s — R R — Η -10- (8) 1374173 and/or [Chemical 2]

HIS— R 2 \)/HIS — R 2 \)/

〇 * X 2 2 R —SIR (其中R2爲不具有爲相同或相異之脂肪族不飽和鍵之 1價烴基，α爲0或l，p、g爲0以上之整數；α爲0之時， Ρ爲2以上，表示此有機氫聚矽氧烷之25 °C的黏度成爲 1〜1000mPa*s之數目；又，s爲2以上之整數，t表示0以上 之整數，且3彡s + t，宜爲3Ss + tS8之整數） 此處，R2係宜爲碳數1〜10者，若例示，爲甲基、乙基 、丙基'丁基等之烷基、環己基等之環烷基、苯基、甲苯 基等之芳基等，進一步，以鹵素、胺、羥、氰基等之其他 之基取代結合於此等之基的碳原子之氫原子的一部分或全 部，即3 -胺基丙基、3，3，3 -三氟丙基、3 -羥丙基、 3 -胺基丙基等。尤其宜爲甲基、苯基。 此有機氫聚矽氧烷在25°C的黏度宜爲1~1〇〇〇 mPa_s， 更宜爲1~700 mPa‘s »亦可爲2種以上之混合物。 (B)成分之使用量係（B)成分中之SiH基對（A)成分之 烯基的莫耳比宜成爲0.5 ~5，尤其成爲〇·8~3的範圍的方式 進行調配。不足〇·5時係交聯密度變低’隨此，有時保持 力會降低，若超過5，交聯密度會變高，有時無法得到充 -11 - 1374173 ⑼ 分的黏著力及黏性。 (C)成分係含有R^SiOo.s單元（R1係碳數1〜10之一價 烴基）及Si02單元，R^SiOo.s單元/5丨02單元的莫耳比爲 0·6~1·7之聚有機矽氧烷。R^SiOo.s單元/Si02單元之莫耳 比未達0.6時係有時黏著力或黏性會降低，若超過1.7，有 時黏著力或保持力會降低。 R1係可舉例甲基、乙基、丙基'丁基等之烷基，環烷 基、苯基、乙烯基、烯丙基、己烯基。宜爲甲基。 (C) 成份亦可含有OH基，OH基含量宜爲0.01-4.0質 量％者。OH者未達〇.〇1質量％時，有時黏著劑之凝集力變 低，超過4.0質量％者係因黏著劑之黏性的理由，故不佳。 又，在不.損及本發明之特性的範圍中，亦可使RkiOr5單 元、R^SiO單元含有於（B)成分中。又，（B)成分亦可倂用 2種以上。 (A)、（B)成分之合計與（C)成分之調配比就質量比爲 90/10-30/70，尤其宜形成 70/30~35/65。（A)、（B)成分之 聚二有機矽氧烷的合計之調配比若低於30/70，黏著力或 保持力會降低，組成物之黏度太高。有時塗布會變困難， 若超過90/10，黏著力或黏性降低。 (D) 成分係加成反應觸媒，可舉例：氯化鉑酸、氯化 鉑酸之醇溶液、氯化鉑酸與醇之反應物、氯化鉑酸與烯烴 化合物之反應物、氯化鈾酸與含有乙烯基之矽氧烷之反應 物、鉑-烯烴錯合物、錨與含有乙烯基之矽氧烷錯合物、 铑錯合物等。 -12- (10) 1374173 (D)成分之添加量相對於（A)、（B)、（C)成分之合計， 就銷成分宜爲5~2000ppm’尤宜爲l〇~500ppm。不足5 ppm 時，硬化性會降低，交聯密度變低，有時保持力降低，若 * 超過2000 ppm，有時處理浴之可使用時間變短。 ·. (E)成分爲控制劑，且係調配聚矽氧黏著劑組成物乃 至塗布基材時在加熱硬化以前處理液不產生增黏或凝膠化 的方式進行添加者。具體上係可舉例：3 -甲基-1- 丁 φ 炔-3-醇、3 -甲基-1-戊炔-3-醇、3，5 -二甲基-1-己炔-3-醇、1-乙炔基環己醇、3 -甲基-3-三甲 基矽氧-1- 丁炔、3_甲基-3-三甲基矽氧-1-戊炔， * 3、5 -二甲基-3-三甲基矽氧-1-己炔，1-乙炔基- • 1-三甲基矽氧基環己烷、雙（2，2 -二甲基-3- 丁氧基） 二甲基矽烷、1，3，5，7 -四甲基-1，3，5，7 -四乙烯 基環四矽氧烷、1，1，3’ 3 -四甲基-1，3 -二乙烯基二 矽氧烷等。 • (E)成分之調配量係只要相對於（A)、（B)、（C)成分之 合計100質量份爲〇~8.0質量份的範圍即可，尤宜爲 0· 05 ~2.0質量份。若超過8.0質量份，有時硬化性會降低。 本發明之組成物係藉由混合溶解（A)成分' (B)成份、 (C)成份及依需要之（E)成份來製造。以（C)成份被溶解於溶 劑之形態供給時，混合（A)、（B)、（C)成分後，只要在常 溫-加熱及/或減壓下除去溶劑即可。其後，只要添加（E) 成份即可。一般。以此狀態爲了保管、輸送而被塡充於容 器。製造黏著膠帶、黏著片、黏著標籤等時係將此依需要 -13- (11) 1374173 而添加、混合（D)成分，塗布於後所示之各種基材。 或，本發明之組成物係藉於鹼觸媒存在下混合（A)、 (C)成分所得到之生成物中添加（B)、（E)亦可製造。依需要 ^ ，亦可倂用後所示之溶劑。鹼觸媒係可舉例：氫氧化鋰、 . 氫氧化鈉、氫氧化鉀、氫氧化鈣等之金屬氫氧化物、碳酸 鈉、碳酸鉀等之碳酸鹽、碳酸氫鈉等之碳酸氫鹽、甲氧基 鈉、丁氧基鉀等之金屬烷氧化物、丁基鋰等之有機金屬、 φ 鉀矽氧基鹽、氨氣'氨水、甲胺'三甲基胺、三乙基胺等 之氮化合物等。宜爲氨氣、氨水。混合之溫度可爲2〇~ 15 0 °C，但一般係只要在室溫~有機溶劑之回流溫度下實施即 • 可。時間無特別限定，但只要爲0.5小時至1 0小時，宜爲1 小時至6小時即可》 進而’反應終了後，依需要，亦可添加中和鹼觸媒之 中和劑。中和劑係可舉例：氯化氫、二氧化碳等之酸性氣 體、醋酸、辛酸、檸檬酸等之有機酸、鹽酸、硫酸、磷酸 φ 等之無機酸等。 此生成物一般係使揮發成分之濃度調整至例如5質量 %以下，爲了保管、輸送而被塡充於容器。製造黏著膠帶 、黏著片、黏著標籤等時係生成物依需要而以有機溶劑稀 釋’添加、混合（D)成分，塗布於後所示之各種基材。 _ 本發明之聚矽氧黏著劑組成物係可於上述各種成分以 外添加任意成分。例如，可使用聚二甲基矽氧烷、聚二甲 基二苯基矽氧烷等之非反應性的聚有機矽氧烷，進而，酚 系 '酿系 '胺系 '磷系、亞磷酯系、硫系、硫醚系等之氧 -14- (13) 1374173 基材係可舉例··聚酯、聚四氟乙烯、聚醯亞胺、聚苯 硫醚、聚醯胺 '聚碳酸酯、聚苯乙烯、聚丙烯、聚乙烯、 聚氯乙烯等之塑膠膜、鋁膜、銅箔等之金屬箔、和紙合成 ^ 紙、聚乙烯層合紙等之紙、布、玻璃纖維，此等之中的複 ; 數層合而成的複合基材。 爲提昇此等基材與黏著層的密著性，亦可使用經過處 理劑處理’電暈處理、蝕刻處理、電漿處理、噴砂處理者 φ 。宜爲電暈處理及處理劑處理。 可使用的處理劑組成物係可舉例於末端含有一具有 SiOH基之聚二有機矽氧烷 '具有SiH基之聚矽氧烷及/或 • 具有烷氧基之聚矽氧烷、縮合反應觸媒之縮合型聚矽氧處 . 理劑組成物、或、含有一具有乙烯基等之烯基的聚二有機 矽氧烷 '具有SiH基之聚矽氧烷、加成反應觸媒之加成型 聚矽氧處理劑組成物。 塗布方法係只要使用公知之塗布方式而塗布即可，可 • 舉例：雙輥式塗布器、唇式塗布器、輥式塗布器、模頭式 塗布器、刮刀式塗布器、刮片式塗布器、桿式塗布器、吻 合式塗布器、凹版式塗布、網版塗布、浸漬塗布、濤鑄塗 布等。 塗布量就硬化後之黏著劑層的厚度可形成2〜ΙΟΟΟμηι ，尤其 3~500μηι 0 硬化條件係只要在80~130°C進行30秒~3分即可，但不 限於此β 亦可直接塗布於如上述之基材而製造黏著膠帶等，亦 -16- (14) 1374173 可塗布於已進行剝離塗覆之剝離膜或剝離紙，進行硬化後 ，藉由貼合於上述基材之轉印法以製造黏著膠帶等。 如上述調配之聚矽氧黏著劑組成物，係使用一以黏著 ， 劑層之厚度成爲4〇μηι之方式塗布於聚醯亞胺膜基材（厚度 ； 25μιη)之黏著膠帶，依JIS Ζ 0237所示之180。剝離黏著力 的測定方法進行測定時，宜成爲0.01-4.0N/25mm者，更 宜成爲 0.01~3.0N/25mm 者。 φ 在0·〇1Ν/2 5mm以下時，黏著力太低而無法得到充分 的遮蔽性，在4.0N/25mm以上時，黏著力太高而再剝離性 差，故不佳。 - 使用本發明之聚矽氧黏著劑組成物而製造的黏著膠帶 . 等俾可遮蔽的被黏體係無特別限定，但可例示如下者。在 電子零件製造等的用途中，可舉例：不銹剛、銅、鐵、鋁 、鉻、金等之金屬或合金，此等之表面被電鍍處理或防銹 處理、塗覆處理之金屬、玻璃、陶瓷器、陶瓷、聚四氟乙 φ 烯、聚醯亞胺、環氧樹脂'酚醛清漆樹脂等之樹脂等。在 建築等之用途中係除上述外尙有合板、木材、和紙、合成 紙等之紙，進一步此等之中的複數被複合而構成者。 【實施方式】 [實施例] 以下，表示實施例及比較例具體地說明本發明，但本 發明不受下述之實施例所限制。又，例中之份係表示質量 份，特性値係表示以下述之試驗方法所得到之測定値。又 -17- (15) 1374173 ，Me表示甲基、Vi表示乙烯基。 黏著力 ^ 使用塗藥器而將聚矽氧黏著劑組成物溶液塗布於厚 . 25μιη、幅2 5 m m之聚醯亞胺膜至硬化後之厚度爲4 Ο μ m後 ，以120°C、1分鐘之條件加熱、硬化，製成黏著膠帶。將 此黏著膠帶貼於不銹鋼板，藉由使以重2kg之橡膠層被覆 φ 之輥往返2次，進行壓接。在室溫下放置約20小時後，使 用抗拉試驗機而以300mm/分之速度、180°C的角度測定從 不銹鋼板剝離膠帶所需的力量（N/25mm)。 . 保持力 以與黏著力評估相同的方法製成黏著膠帶。以使黏著 面積成爲25x25mxn之方式將此黏著膠帶貼於不銹鋼板的 下端，於黏著膠帶之下端施加重1kg之荷重，讀取在250 φ °C下垂直放罝1小時後之偏移距離，以顯微鏡進行測定。 探針黏性 以與黏著力評估相同的方法製成黏著膠帶。使用 Poly ken公司製探針黏性測試器測定此黏著膠帶的黏性。 殘留甲苯量 以與黏著力評估相同的方法製成黏著膠帶。秤量約 10cm之此黏著膠帶後，封入管瓶內，在260°C加熱此管瓶 -18 - (16) 1374173 1小時後，藉氣體色層分析分析管瓶中之氣體而定量所產 生之單位黏著膠帶質量的甲苯量。 ^ 再剝離性 : 以與黏著力評估相同的方法製成黏著膠帶。將此黏著 膠帶貼於厚50μιη之銅箔上，在150°c下放置1小時後，剝 離黏著膠帶。銅箔不變形，又於被黏體之表面無黏著劑殘 φ 留，可剝離者則視爲良好，銅箔變形或於表面產生黏著劑 殘留者則視爲不良。 - (實施例1) . 使以如下之平均組成式所示且具分枝的含有乙烯基之聚 二甲基矽氧烷（A-1)(含烯基量0.025莫耳/ lOOg、250mPa’s)(36.1 份）、（ViM.e2Si〇i/2)3_ (Me2SiO)i6〇 - (MeSi〇3/2)i 下述式所示的具有SiH基之聚甲基氫矽氧烷（Β-1)(8·9 •份）.、 【化3】〇* X 2 2 R —SIR (wherein R 2 is a monovalent hydrocarbon group which does not have the same or different aliphatic unsaturated bond, α is 0 or 1, p, g is an integer of 0 or more; when α is 0 , Ρ is 2 or more, indicating that the viscosity of the organic hydrogen polyoxyalkylene at 25 ° C is 1 to 1000 mPa * s; further, s is an integer of 2 or more, t represents an integer of 0 or more, and 3 彡 s + t, preferably an integer of 3Ss + tS8) Here, R2 is preferably a carbon number of 1 to 10, and if exemplified, an alkyl group such as a methyl group, an ethyl group, a propyl 'butyl group or the like, a cyclohexane such as a cyclohexyl group. Further, an aryl group such as a phenyl group or a tolyl group, or the like, a part or all of a hydrogen atom of a carbon atom bonded to a group such as a halogen, an amine, a hydroxyl group or a cyano group, that is, 3 - Aminopropyl, 3,3,3-trifluoropropyl, 3-hydroxypropyl, 3-aminopropyl and the like. It is especially preferably a methyl group or a phenyl group. The viscosity of the organic hydrogen polyoxyalkylene at 25 ° C is preferably 1 to 1 〇〇〇 mPa_s, more preferably 1 to 700 mPa s » or a mixture of 2 or more types. The amount of the component (B) used is such that the molar ratio of the SiH group in the component (B) to the alkenyl group (A) is preferably 0.5 to 5, and particularly in the range of 〇·8 to 3. When the number is less than 〇5, the crosslink density becomes low. As a result, the holding power may decrease. If it exceeds 5, the crosslink density may become high, and the adhesion and viscosity of the charge may not be obtained at -11 - 1374173 (9). . The component (C) contains R^SiOo.s unit (R1 is a carbon number of 1 to 10 hydrocarbons) and a SiO2 unit, and the molar ratio of the R^SiOo.s unit/5丨02 unit is 0·6~1. · 7 polyorganosiloxane. When the molar ratio of the R^SiOo.s unit/Si02 unit is less than 0.6, the adhesion or viscosity may decrease. If it exceeds 1.7, the adhesion or retention may decrease. The R1 may, for example, be an alkyl group such as a methyl group, an ethyl group or a propyl 'butyl group, a cycloalkyl group, a phenyl group, a vinyl group, an allyl group or a hexenyl group. It should be a methyl group. (C) The component may also contain an OH group, and the OH group content is preferably 0.01 to 4.0% by mass. When the amount of OH is less than 质量1% by mass, the cohesive force of the adhesive may be lowered, and if it exceeds 4.0% by mass, the adhesion of the adhesive is not preferable. Further, in the range which does not impair the characteristics of the present invention, the RkiOr5 unit and the R^SiO unit may be contained in the component (B). Further, two or more kinds of the component (B) may be used. The ratio of the total of the components (A) and (B) to the ratio of the component (C) is 90/10-30/70, and particularly preferably 70/30 to 35/65. If the total blend ratio of the polydiorganosiloxanes of the components (A) and (B) is less than 30/70, the adhesion or holding force is lowered, and the viscosity of the composition is too high. Sometimes coating becomes difficult, and if it exceeds 90/10, the adhesion or viscosity is lowered. (D) Component addition reaction catalyst, for example: chloroplatinic acid, chloroplatinic acid alcohol solution, chloroplatinic acid and alcohol reactant, chlorinated platinum acid and olefin compound reactant, chlorination A reaction of uronic acid with a vinyl group-containing decane, a platinum-olefin complex, an anchor with a vinyl-containing alkane complex, a ruthenium complex, and the like. -12- (10) 1374173 The amount of the component (D) added is preferably from 5 to 2000 ppm', particularly preferably from 10 to 500 ppm, based on the total of the components (A), (B), and (C). When the amount is less than 5 ppm, the hardenability is lowered, the crosslinking density is lowered, and the holding power is sometimes lowered. If the amount exceeds 2000 ppm, the service life of the treatment bath may be shortened. The component (E) is a control agent, and is added in such a manner that the composition of the polyoxyxene adhesive is added to the substrate, and the treatment liquid is not thickened or gelled before heat curing. Specifically, it can be exemplified by 3-methyl-1-butyryn-3-ol, 3-methyl-1-pentyn-3-ol, 3,5-dimethyl-1-hexyne-3- Alcohol, 1-ethynylcyclohexanol, 3-methyl-3-trimethylphosphonium-1-butyne, 3-methyl-3-trimethylphosphonium-1-pentyne, *3,5 -Dimethyl-3-trimethyloxime-1-hexyne, 1-ethynyl- • 1-trimethyldecyloxycyclohexane, bis(2,2-dimethyl-3-butoxy) Dimethyl decane, 1,3,5,7-tetramethyl-1,3,5,7-tetravinylcyclotetraoxane, 1,1,3' 3-tetramethyl-1, 3-divinyldioxane and the like. The amount of the component (E) is preferably in the range of 〇 to 8.0 parts by mass based on 100 parts by mass of the total of the components (A), (B), and (C), and particularly preferably from 0.05 to 2.0 parts by mass. . When it exceeds 8.0 parts by mass, the hardenability may be lowered. The composition of the present invention is produced by mixing and dissolving the component (B) (B), the component (C) and the component (E) as needed. When the component (C) is dissolved in the form of a solvent, the components (A), (B) and (C) may be mixed, and the solvent may be removed under normal temperature-heating and/or reduced pressure. Then, just add the (E) ingredient. general. In this state, it is filled in the container for storage and transportation. When an adhesive tape, an adhesive sheet, an adhesive label, or the like is produced, the component (D) is added and mixed as needed -13-(11) 1374173, and applied to various substrates shown later. Alternatively, the composition of the present invention may be produced by adding (B) or (E) to the product obtained by mixing the components (A) and (C) in the presence of a base catalyst. The solvent shown after use can also be used as needed. Examples of the alkali catalyst system include lithium hydroxide, metal hydroxides such as sodium hydroxide, potassium hydroxide, and calcium hydroxide; carbonates such as sodium carbonate and potassium carbonate; and hydrogencarbonates such as sodium hydrogencarbonate; a metal alkoxide such as sodium oxyhydroxide or potassium butoxide, an organic metal such as butyl lithium, a potassium sulfonium oxide salt, an ammonia gas, an ammonia water, a methylamine 'trimethylamine, a triethylamine or the like. Compounds, etc. It should be ammonia gas or ammonia water. The mixing temperature can be from 2 〇 to 150 ° C, but it is generally carried out at room temperature to the reflux temperature of the organic solvent. The time is not particularly limited, but it is preferably from 1 hour to 6 hours as long as it is from 0.5 hours to 10 hours. Further, after the reaction is completed, a neutralizing agent for neutralizing the alkali catalyst may be added as needed. The neutralizing agent may, for example, be an acid gas such as hydrogen chloride or carbon dioxide, an organic acid such as acetic acid, caprylic acid or citric acid, or an inorganic acid such as hydrochloric acid, sulfuric acid or phosphoric acid φ. In the product, the concentration of the volatile component is adjusted to, for example, 5% by mass or less, and is filled in the container for storage and transportation. When an adhesive tape, an adhesive sheet, an adhesive label, or the like is produced, the product is diluted with an organic solvent as needed. The component (D) is added and mixed, and applied to various substrates shown later. The polyoxyxylene adhesive composition of the present invention may contain an optional component in addition to the above various components. For example, a non-reactive polyorganosiloxane such as polydimethylsiloxane or polydimethyldiphenyloxane can be used, and further, a phenolic system can be used as a phosphorus-based or phosphorous-phosphorus. Oxygen-14-(13) 1374173 substrate of ester, sulfur or thioether system, etc. · Polyester, polytetrafluoroethylene, polyimine, polyphenylene sulfide, polyamine Plastic film of ester, polystyrene, polypropylene, polyethylene, polyvinyl chloride, metal foil such as aluminum film, copper foil, paper, cloth, glass fiber, etc. a composite substrate that is laminated in several layers. In order to improve the adhesion between these substrates and the adhesive layer, it is also possible to use a treatment agent to treat 'corona treatment, etching treatment, plasma treatment, sand blasting φ . It should be treated with corona treatment and treatment agent. The treating agent composition which can be used is exemplified by a polydioxanthene having a SiOH group at the terminal, a polyoxyalkylene having an SiH group, and/or a polyoxyalkylene having an alkoxy group, and a condensation reaction. a condensed polyoxyl group of a medium, a physicochemical composition, or a polydiorganosiloxane having an alkenyl group such as a vinyl group, a polyoxyalkylene having a SiH group, and an addition reaction of an addition reaction catalyst Polyoxygen treatment composition. The coating method can be applied by using a known coating method, and can be exemplified by: a two-roll coater, a lip coater, a roll coater, a die coater, a blade coater, and a blade coater. , rod coater, staple applicator, gravure coating, screen coating, dip coating, Tao casting coating, and the like. The coating amount is such that the thickness of the adhesive layer after hardening can be formed into 2~ΙΟΟΟμηι, especially 3~500μηι 0. The curing condition can be carried out at 80 to 130 ° C for 30 seconds to 3 minutes, but is not limited to this β and can be directly coated. An adhesive tape or the like is produced on the substrate as described above, and -16-(14) 1374173 can be applied to a release film or release paper which has been subjected to release coating, and after hardening, transfer by bonding to the substrate The method is to manufacture adhesive tape and the like. The polyadone oxygen adhesive composition as described above is applied to an adhesive tape of a polyimide film substrate (thickness; 25 μm) by means of adhesion, and the thickness of the layer is 4 〇μηι, according to JIS Ζ 0237 180 shown. When the measurement method of the peeling adhesive force is measured, it is preferably 0.01 to 4.0 N/25 mm, and more preferably 0.01 to 3.0 N/25 mm. When φ is 0·〇1Ν/2 5 mm or less, the adhesion is too low to provide sufficient shielding properties. When the thickness is 4.0 N/25 mm or more, the adhesion is too high and the removability is poor, which is not preferable. - Adhesive tape produced by using the polyoxyxene adhesive composition of the present invention. The adhesive system to be shielded is not particularly limited, and the following may be exemplified. In the use of electronic parts manufacturing, etc., metals or alloys such as stainless steel, copper, iron, aluminum, chromium, gold, etc., such as metal or glass, which are surface-plated or rust-proof treated, coated, and coated, may be exemplified. , ceramics, ceramics, polytetrafluoroethylene phthalene, polyimine, epoxy resin, such as novolac resin. In the use of construction or the like, papers such as plywood, wood, paper, synthetic paper, and the like are used in addition to the above-mentioned outer layer, and the plurals among these are composited. [Embodiment] [Examples] Hereinafter, the present invention will be specifically described by way of examples and comparative examples, but the present invention is not limited by the following examples. Further, the parts in the examples represent the parts by mass, and the characteristics are the measured enthalpy obtained by the following test method. Further -17-(15) 1374173, Me represents a methyl group, and Vi represents a vinyl group. Adhesive force ^ Apply the solution of the polyoxyxide adhesive composition to a thick film of 25 μm and 2 mm of polyimine film to a thickness of 4 μm after hardening at 120 ° C using an applicator. Heated and hardened for 1 minute to form an adhesive tape. The adhesive tape was attached to a stainless steel plate, and the roller was coated twice with a rubber layer having a weight of 2 kg to be crimped twice. After standing at room temperature for about 20 hours, the force required to peel the tape from the stainless steel sheet (N/25 mm) was measured at a speed of 300 °C at a speed of 300 °C using a tensile tester. Retention The adhesive tape is made in the same way as the adhesion evaluation. Apply the adhesive tape to the lower end of the stainless steel plate so that the adhesive area is 25x25mxn, apply a load of 1kg at the lower end of the adhesive tape, and read the offset distance after vertical immersion for 1 hour at 250 φ °C. The measurement was performed by a microscope. Probe Viscosity Adhesive tape was prepared in the same manner as adhesion evaluation. The adhesiveness of the adhesive tape was measured using a probe viscous tester manufactured by Polyken. Amount of residual toluene Adhesive tape was prepared in the same manner as the adhesion evaluation. After weighing the adhesive tape of about 10 cm, seal it into the vial and heat the vial at 260 °C for -18 - (16) 1374173. After 1 hour, analyze the gas in the vial by gas chromatography to quantify the unit produced. Adhesive tape mass of toluene. ^ Re-peelability: Adhesive tape is prepared in the same manner as adhesion evaluation. The adhesive tape was stuck on a copper foil having a thickness of 50 μm, and after standing at 150 ° C for 1 hour, the adhesive tape was peeled off. The copper foil is not deformed, and no adhesive residue φ remains on the surface of the adherend, and the peelable one is considered to be good, and the copper foil is deformed or the adhesive residue on the surface is considered to be bad. - (Example 1). A vinyl group-containing polydimethyl methoxy oxane (A-1) having an average composition formula as follows (alkenyl group content: 0.025 mol/lOOg, 250 mPa's) (36.1 parts), (ViM.e2Si〇i/2)3_(Me2SiO)i6〇-(MeSi〇3/2)i A polymethylhydroquinone (Si-1) having a SiH group represented by the following formula ) (8·9 • copies)., [Chemical 3]

6 i 8 MISIM 5 2 V}/ ο e i 6 M-SIM /IV 3 \—/ i e H — SIM /l\ 0 e·1e MISIM 1 e M e Μ 含有 Me3S iO〇.5單元及 Si〇2單兀且 Me3SiO〇.5單兀 /Si02單元的莫耳比爲0.85之聚有機矽氧烷（C)之60 %甲苯 溶液（9 1.7份）混合，在90 °C、減壓下豳去甲苯。冷却後， -19- (17) (17)1374173 於此生成物（100份）中，添加乙炔基環己醇（0.20份）、含有 鉑成分0.5質量％之含鉑-乙烯基的矽氧烷錯合物之聚矽氧 溶液（1.0份），並混合，調製聚矽氧黏著劑組成物^ 測定此聚矽氧黏著劑的糊殘留性、黏著力、保持力、 探針黏性、再剝離性。結果表示於表1中》 (實施例2) 使具分枝的含有乙烯基之聚二甲基矽氧烷（A· 1)(3 2.1 份）、具有SiH基的聚甲基氫矽氧烷（Β_1)(7·9份）、含有 Me3Si〇Q.5單元及Si02單元且Me3SiO〇.5單元/Si〇2單元的莫 耳比爲0.85之聚有機矽氧烷（C)之60%甲苯溶液（1〇〇份）混 合’在90 °C、減壓下餾去甲苯。冷却後，於此生成物（1〇〇 份）中，添加乙炔基環己醇（0.20份）、含有鉛成分〇.5質量％ 之含鉑-乙烯基的矽氧烷錯合物之聚矽氧溶液（1〇份），並 混合，調製聚矽氧黏著劑組成物。 測定此聚矽氧黏著劑的糊殘留性、黏著力、保持力、 探針黏性、再剝離性。結果表示於表1中。 (實施例3) 使具分枝的含有乙嫌基之聚二甲基矽氧烷0-2)(72.2 份）、具有SiH基的聚甲基氫矽氧烷（B_1)(178份）、含有 Me3Si〇Q.5單元及Si〇2單元且Me3Si〇()5單元/Si〇2單元的莫 耳比爲0.85之聚有機矽氧烷（C)之60%甲苯溶液（16 7份）混 合，在9(TC、減壓下餾去甲苯。冷却後，於此生成物（1〇〇 -20- (18) 1374173 份）中，添加乙炔基環己醇（0.20份）、含有鉑成分0.5質量％ 之含鉑-乙烯基的矽氧烷錯合物之聚矽氧溶液（1.0份）’並 混合，調製聚矽氧黏著劑組成物。 .. 測定此聚矽氧黏著劑的糊殘留性、黏著力、保持力、 探針黏性、再剝離性。結果表示於表1中。 (實施例4) ^ 使以如下之平均組成式所示且具分枝的含有乙烯基之聚 二甲基矽氧烷（A-2)(含烯基量0.048莫耳/l〇〇g、llOmPa· s)(30.6份）、 . (V i Me 2 S i Ο 1 /2) 3 - (M e 2 S i Ο)8〇 - (M e S i 0 3/2) 1 具有 SiH基的聚甲基氫矽氧烷（B-l)(14·4份）、含有 Me3SiO〇.5單元及Si02單元且Me3SiO〇.5單元/Si02單元的莫 耳比爲0.85之聚有機矽氧烷（C)之60 %甲苯溶液（91.7份）混 φ 合，在90 °C、減壓下餾去甲苯。冷却後，於此生成物（100 份）中，添加乙炔基環己醇（0.20份）、含有鉑成分〇.5質量％ 之含鉑-乙烯基的矽氧烷錯合物之聚矽氧溶液（1.0份），並 混合，調製聚矽氧黏著劑組成物。 測定此聚矽氧黏著劑的糊殘留性、黏著力 '保持力、 ' 探針黏性、再剝離性。結果表示於表1中。 (實施例5) 使具分枝的含有乙烯基之聚二甲基矽氧烷1.0 -21 - (19) 1374173 份）、以如下所示之具有SiH基的聚甲基氫矽氧烷（B-2)(3.7份）、 【化4】6 i 8 MISIM 5 2 V}/ ο ei 6 M-SIM /IV 3 \—/ ie H — SIM /l\ 0 e·1e MISIM 1 e M e Μ Contains Me3S iO〇.5 unit and Si〇2 single Further, a Me3SiO〇.5 monofluorene/SiO 2 unit was mixed with a 60% toluene solution (9 1.7 parts) of a polyorganosiloxane (C) having a molar ratio of 0.85, and toluene was removed at 90 ° C under reduced pressure. After cooling, -19-(17) (17)1374173 Add ethynylcyclohexanol (0.20 parts) to the product (100 parts), and a platinum-vinyl group-containing oxirane containing 0.5% by mass of a platinum component. The polyoxyl solution (1.0 parts) of the complex compound is mixed and prepared to prepare a composition of the polyoxyxide adhesive. The paste residue, adhesion, retention, probe viscosity, and peeling of the polyoxygen adhesive are measured. Sex. The results are shown in Table 1 (Example 2) A branched vinyl-containing polydimethyl methoxyane (A·1) (3 2.1 parts), a polymethylhydroquinone having a SiH group. (Β_1) (7·9 parts), 60% toluene of polyorganosiloxane (C) having a molar ratio of 0.85 with Me3SiO〇Q.5 unit and SiO2 unit and Me3SiO〇.5 unit/Si〇2 unit The solution (1 part) was mixed' toluene at 90 ° C under reduced pressure. After cooling, acetylene cyclohexanol (0.20 parts) and a platinum-vinyl-containing oxime complex having a lead component of 5% by mass were added to the product (1 part). An oxygen solution (1 part) was added and mixed to prepare a polyoxyxene adhesive composition. The paste residue, adhesion, retention, probe stickiness, and re-peelability of the polyoxyxylene adhesive were measured. The results are shown in Table 1. (Example 3) A branched polydimethyl methoxy oxane 0-2) (72.2 parts), a polymethylhydroquinone (B_1) having an SiH group (178 parts), Mixing 60% toluene solution (16 7 parts) containing a Me3Si〇Q.5 unit and a Si〇2 unit and a Me3Si〇()5 unit/Si〇2 unit with a molar ratio of 0.85 of polyorganosiloxane (C) Toluene was distilled off under reduced pressure at 9 (TC). After cooling, ethynylcyclohexanol (0.20 parts) and a platinum component were added to the product (1 〇〇-20-(18) 1374173 parts). Mass% of a platinum-vinyl oxirane complex of a polyoxo-oxygen solution (1.0 parts)' is mixed and prepared to form a polyoxyxene adhesive composition. . . . Determination of the paste residue of the polyoxyxene adhesive , adhesion, retention, probe tack, re-peelability. The results are shown in Table 1. (Example 4) ^ A vinyl-containing polydimethylene having the following average composition formula and branched Alkoxyoxane (A-2) (alkenyl group content: 0.048 mol/l〇〇g, llOmPa·s) (30.6 parts), . (V i Me 2 S i Ο 1 /2) 3 - (M e 2 S i Ο)8〇- (M e S i 0 3/2) 1 Polymethylhydroquinone with SiH group Alkane (Bl) (14·4 parts), a 60% toluene solution containing a Me3SiO〇.5 unit and a SiO 2 unit and a Me3SiO〇.5 unit/SiO 2 unit having a molar ratio of 0.85 polyorganosiloxane (C) ( 91.7 parts) were mixed, and toluene was distilled off under reduced pressure at 90 ° C. After cooling, acetylene cyclohexanol (0.20 parts) and platinum component 〇.5 mass were added to the product (100 parts). % of a platinum-vinyl oxirane complex polyoxyl solution (1.0 part), and mixed to prepare a polyoxyxene adhesive composition. The paste residue and adhesion of the polyoxygen adhesive are measured. 'Retention force, 'Probe viscosity, re-peelability. The results are shown in Table 1. (Example 5) Branched vinyl-containing polydimethyl methoxy alkane 1.0 - 21 - (19) 1374173 (Part 4), polymethylhydroquinone (B-2) having a SiH group as shown below (3.7 parts), [Chemical 4]

H I eie Ml SIM 8 \ϊ/ e i e MISIM /V 0 e i e Ml SIM -· H 以如下所示之具有SiH基的聚甲基氫矽氧烷（B-3)(0 份） 化H I eie Ml SIM 8 \ϊ/ e i e MISIM /V 0 e i e Ml SIM -· H Polymethylhydroquinone (B-3) with SiH group as shown below (0 parts)

eΜ ι e i e Μ I SIM 5 2 \1/ i e H —SIM -i\o Θ i e ]M 丨 s —M 5 | e M 含有 Me3Si〇0.5單元及 Si02單元且 Me3Si〇c.5單元 φ /Si〇2單元的莫耳比爲0.85之聚有機矽氧烷（C)之60 %甲苯 溶液（9 1.7份）混合，在90 °C '減壓下餾去甲苯。冷却後， 於此生成物（100份）中，添加乙炔基環己醇（0.20份）、含有 鉑成分0.5質量％之含鉑-乙烯基的矽氧烷錯合物之聚矽氧 溶液（1.0份），並混合，調製聚矽氧黏著劑組成物" " 測定此聚矽氧黏著劑的糊殘留性、黏著力、保持力、 探針黏性、再剝離性。結果表示於表1中。 (實施例6) -22- (20) (20)1374173 使以如下之平均組成式所示且具分枝的含有乙烯基 之聚二甲基矽氧烷（A-3)(含烯基量0.026莫耳/100g、 360mPa· s)(35.8份）、 (ViMe2Si〇i/2)4_ (Me2SiO)2〇〇- (MeSi〇4/2)i 具有 SiH基的聚甲基氫矽氧烷（Β·1)(9.2份）、含有 Me3SiO〇.5單元及Si02單元且Me3SiO〇.5單元/Si02單元的莫 耳比爲0.85之聚有機矽氧烷（C)之60 %甲苯溶液（9 1.7份）混 合，在90 °C、Μ壓下餾去甲苯。冷却後，於此生成物（1〇〇 份）中，添加乙炔基環己醇（0.20份）、含有鉑成分0.5質量％ 之含鉑-乙烯基的矽氧烷錯合物之聚矽氧溶液（1.0份），並 混合，調製聚矽氧黏著劑組成物》 測定此聚矽氧黏著劑的糊殘留性、黏著力、保持力、 探針黏性、再剝離性。結果表示於表1中。 (實施例7) 使以如下之平均組成式所示且具分枝的含有乙烯基 之聚二甲基矽氧烷（Α-4)(含烯基量0.047莫耳/I00g、 220mPa s)(30.8份）、 (V i M e 2 S i Ο 1 / 2) 3 - (M e 2 S i Ο) 8 〇 - (M e S i Ο 3 / 2) 2 具有SiH基的聚甲基氫矽氧烷（B-l)(14.2份）、含有 -23- (21) (21)1374173EΜ ι eie Μ I SIM 5 2 \1/ ie H —SIM -i\o Θ ie ]M 丨s —M 5 | e M Contains Me3Si〇0.5 unit and SiO 2 unit and Me3Si〇c.5 unit φ /Si〇 The 2-unit molar ratio of 0.85 polyorganosiloxane (C) in 60% toluene (9 1.7 parts) was mixed, and toluene was distilled off under reduced pressure at 90 °C. After cooling, acetylene cyclohexanol (0.20 parts) and a platinum-vinyl-containing oxime complex having a platinum component of 0.5% by mass were added to the product (100 parts). (Parts), and mix, modulate the composition of the polyoxygen adhesive composition "" Determine the paste residue, adhesion, retention, probe adhesion, re-peelability of the polyoxygenated adhesive. The results are shown in Table 1. (Example 6) -22- (20) (20) 1374173 A vinyl group-containing polydimethyl methoxy oxane (A-3) having an average composition formula as follows (alkenyl group-containing amount) 0.026 mol/100 g, 360 mPa·s) (35.8 parts), (ViMe2Si〇i/2)4_(Me2SiO)2〇〇-(MeSi〇4/2)i polymethylhydroquinone having SiH group ( Β·1) (9.2 parts), a 60% toluene solution containing a Me3SiO〇.5 unit and a SiO 2 unit and a Me3SiO〇.5 unit/SiO 2 unit having a molar ratio of 0.85 of a polyorganosiloxane (C) (9 1.7) The mixture was mixed and the toluene was distilled off under a pressure of 90 °C. After cooling, acetylene cyclohexanol (0.20 parts) and a platinum-vinyl-containing oxirane complex containing polyfluorinated oxygen solution containing 0.5% by mass of a platinum component were added to the product (1 part). (1.0 part), and mixed, modulating the composition of the polyoxygen adhesive agent. The paste residue, adhesion, retention, probe stickiness, and re-peelability of the polyoxygen oxide adhesive were measured. The results are shown in Table 1. (Example 7) A vinyl group-containing polydimethyl methoxy oxane (Α-4) having an average composition formula and having a branching group (containing an alkenyl group of 0.047 mol/I00 g, 220 mPa s) 30.8 parts), (V i M e 2 S i Ο 1 / 2) 3 - (M e 2 S i Ο) 8 〇- (M e S i Ο 3 / 2) 2 Polymethylhydroquinone with SiH group Oxytomane (Bl) (14.2 parts), containing -23- (21) (21) 1374173

Me3SiO〇_5單元及Si02單元且Me3SiO0.5單元/si〇2單元的莫 耳比爲0.85之聚有機矽氧烷（C)之60%甲苯溶液（9 l7份）混 合，在90°C、減壓下餾去甲苯。冷却後，於此生成物（1〇〇 份）中，添加乙炔基環己醇（〇·20份）、含有鉛成分〇.5質量％ 之含鉑-乙烯基的矽氧烷錯合物之聚矽氧溶液（1.0份），並 混合，調製聚矽氧黏著劑組成物。 測定此聚矽氧黏著劑的糊殘留性、黏著力、保持力、 探針黏性、再剝離性。結果表示於表1中。 (實施例8) 使以如下之平均組成式所示且具分枝的含有乙烯基 之聚二甲基矽氧烷（A-5)(含烯基量〇.〇31莫耳/100g、 80mPa-s)(34.2份）、 (ViMe2Si01/2)2 - (M e 3 S i Ο ι/2) 2 - (M e 2 S i Ο) 8 〇 - (M e S i 03/2)2 具有SiH基的聚甲基氫矽氧烷（B-l)(l〇.8份）、含有 Me3Si〇〇.5單元及Si〇2單元且Me3Si〇Q5單元/Si〇2單元的莫 耳比爲0.85之聚有機矽氧烷（C)之60%甲苯溶液（91·7份）混 合，在9〇°C '減壓下餾去甲苯。冷却後，於此生成物（1〇〇 份）中，添加乙炔基環己醇（〇.2〇份）、含有鉑成分〇.5質量％ 之含鉑-乙烯基的矽氧烷錯合物之聚矽氧溶液（10份），並 混合，調製聚矽氧黏著劑組成物。 測定此聚矽氧黏著劑的糊殘留性、黏著力、保持力、 -24 - (22) 1374173 探針黏性、再剝離性。結果表示於表1中。 (實施例9) 使以如下之平均組成式所示且具分枝的含有乙烯基 之聚二甲基矽氧烷（A-6)(含烯基量0.020莫耳/l〇〇g、 950mPa.s)(3 7.6份）、 • (ViMe2Si01/2)3 - (ViMeSiO)2- (Me2SiO)33〇-(MeSi〇3/2)i 具有 SiH基的聚甲基氫矽氧烷（B-l)(7·4份）、含有 - Me3SiO〇.5單元及Si02單元且Me3SiO〇.5單元/Si02單元的莫 . 耳比爲〇·85之聚有機矽氧烷（C)之60 %甲苯溶液（91.7份）混 合，在90 °C、減壓下餾去甲苯。冷却後，於此生成物（100 份）中，添加乙炔基環己醇（〇·2〇份）、含有鉑成分〇·5質量％ 之含鉑-乙烯基的矽氧烷錯合物之聚矽氧溶液（1.0份），並 φ 混合，調製聚矽氧黏著劑組成物。 (比較例1) 使以下式所示且不具分枝的含有乙烯基之聚二甲基矽 氧烷（含烯基量〇.〇20莫耳/10(^、40〇11^38)(八-7)(37_6份） (ViMe2Si01/2)2 - (Me2SiO)13〇 具有SiH基的聚甲基氫矽氧烷（B-l)(7.4份）、含有 Me3SiO0.5單元及Si02單元且Me3SiO〇.5單元/Si02單元的莫 -25 - (23) 1374173 耳比爲0.85之聚有機矽氧烷之60%甲苯溶液（917份）混 合，在9〇。(：、減壓下餾去甲苯。冷却後，於此生成物（1()〇 份）中’添加乙炔基環己醇（0.20份）、含有鉑成分0.5質量％ ' 之含轴-乙烯基的矽氧烷錯合物之聚矽氧溶液（1.〇份），並 ： 混合’調製聚砂氧黏著劑組成物。 測定此聚砂氧黏著劑的糊殘留性'黏著力'保持力、 探針黏性、再剝離性。結果表示於表1中。 (比較例2) 使以下式所示且不具分枝的含有乙烯基之聚二甲基矽 ' 氧烷（含烯基量0.007莫耳/100g、於甲苯中溶解成濃度30 % ^ 者爲 2200mPa.s)(A-8)(44.0份）、 (ViMe2Si01/2)2- (ViMeSiO)14- (Me2SiO)2985 φ 使以下式所示且具有SiH基的聚甲基氫矽氧烷（Β- 4)(1.0份）、 化a Me3SiO〇_5 unit and a SiO2 unit and a Me3SiO0.5 unit/si〇2 unit having a molar ratio of 0.85 of a polyorganosiloxane (C) in a 60% toluene solution (9 l7 parts), at 90 ° C, The toluene was distilled off under reduced pressure. After cooling, acetylene cyclohexanol (20 parts) and a platinum-vinyl group-containing oxirane complex containing a lead component of 5% by mass were added to the product (1 part). A polyoxygenated solution (1.0 part) was mixed and mixed to prepare a polyoxyxene adhesive composition. The paste residue, adhesion, retention, probe stickiness, and re-peelability of the polyoxyxylene adhesive were measured. The results are shown in Table 1. (Example 8) A vinyl group-containing polydimethyl methoxy oxane (A-5) having an average composition formula as follows (alkenyl group-containing amount 〇. 31 mol/100 g, 80 mPa) -s) (34.2 parts), (ViMe2Si01/2)2 - (M e 3 S i Ο ι/2) 2 - (M e 2 S i Ο) 8 〇- (M e S i 03/2) 2 The SiH-based polymethylhydroquinone (Bl) (10 parts), the Me3Si〇〇.5 unit and the Si〇2 unit, and the Me3Si〇Q5 unit/Si〇2 unit have a molar ratio of 0.85. A 60% toluene solution (91·7 parts) of polyorganosiloxane (C) was mixed, and toluene was distilled off under reduced pressure of 9 °C. After cooling, acetylene cyclohexanol (〇2 parts) and a platinum-vinyl-containing oxime complex having a platinum component of 5% by mass were added to the product (1 part). The polyoxygenated solution (10 parts) was mixed and mixed to prepare a polyoxyxene adhesive composition. The paste residue, adhesion, and holding power of the polyoxygen adhesive were measured, and the tackiness and removability of the probe were -24 - (22) 1374173. The results are shown in Table 1. (Example 9) A vinyl group-containing polydimethyl methoxy oxane (A-6) having an average composition formula and having a branching ratio of 0.020 mol/l 〇〇g, 950 mPa .s) (3 7.6 parts), • (ViMe2Si01/2)3 - (ViMeSiO)2-(Me2SiO)33〇-(MeSi〇3/2)i Polymethylhydroquinone (Bl) with SiH group (7·4 parts), a 60% toluene solution containing -Me3SiO〇.5 unit and SiO 2 unit and Me3SiO〇.5 unit/SiO 2 unit in a molar ratio of 矽·85 polyorganosiloxane (C) 91.7 parts) were mixed, and toluene was distilled off at 90 ° C under reduced pressure. After cooling, the product (100 parts) was added with acetylene cyclohexanol (〇 2 parts), and a platinum-vinyl-containing oxirane complex containing platinum content of 5% by mass. An oxygen solution (1.0 part) was added and φ mixed to prepare a polyoxyxene adhesive composition. (Comparative Example 1) A vinyl-containing polydimethyl methoxy oxane having an alkyl group represented by the following formula and having no branching (alkenyl group-containing amount 〇. 20 mol / 10 (^, 40 〇 11 ^ 38) (eight -7) (37_6 parts) (ViMe2Si01/2) 2 - (Me2SiO) 13 聚 polymethylhydroquinone (Bl) (7.4 parts) having SiH group, containing Me3SiO0.5 unit and SiO2 unit and Me3SiO〇. 5-unit/SiO2 unit Mo-25 - (23) 1374173 A 60% toluene solution (917 parts) of a polyorganosiloxane having an ear ratio of 0.85 was mixed at 9 Torr. (:, toluene was distilled off under reduced pressure. Then, in the product (1 () aliquot), 'addition of acetylene cyclohexanol (0.20 parts), a platinum-containing oxime complex containing a platinum component of 0.5% by mass' Solution (1. 〇), and: Mixing 'Modified Sand Oxygen Adhesive Composition. Determine the paste residual 'adhesion' retention, probe viscosity, and re-peelability of the polyoxygen adhesive. In Table 1. (Comparative Example 2) A vinyl group-containing polydimethylhydrazine oxane having an alkyl group represented by the following formula (having an alkenyl group content of 0.007 mol/100 g, dissolved in toluene to a concentration of 30) % ^ is 2200mPa.s) (A- 8) (44.0 parts), (ViMe2Si01/2)2-(ViMeSiO)14-(Me2SiO)2985 φ A polymethylhydroquinone (Β-4) having a SiH group and having a SiH group (1.0 part) And

e Me M

1 M —S-M e o1 M —S-M e o

H —SIM o eΜ I e i MIS, e 含有Me3SiO〇.5單元及Si02單元且 Me3SiO〇.5單元 /Si02單元的莫耳比爲〇·85之聚有機矽氧烷（C)之60%甲苯 •26- (24) (24)1374173 溶液（91.7份）、甲苯（30·0份）混合，形成聚矽氧成分爲約 60%。於此生成物（1〇〇份）中，添加乙炔基環己醇（012份） '含有鈾成分0.5質量％之含鉑-乙烯基的矽氧烷錯合物之 聚矽氧溶液（〇·6份），並混合，調製聚矽氧黏著劑組成物。 測定此聚矽氧黏著劑的糊殘留性、黏著力、保持力、 探針黏性、再剝離性。結果表示於表1中。H —SIM o eΜ I ei MIS, e 60% toluene containing a Me3SiO〇.5 unit and a SiO 2 unit and a Me3SiO〇.5 unit/SiO 2 unit with a molar ratio of 〇·85 polyorganosiloxane (C) 26-(24) (24) 1374173 A solution (91.7 parts) and toluene (30·0 parts) were mixed to form a polyfluorene component of about 60%. To the product (1 part), ethynylcyclohexanol (012 parts) was added, and a polyfluorene-oxygen solution containing a platinum-vinyl oxime complex having a uranium content of 0.5% by mass was added. 6 parts), and mixed, to modulate the composition of the polyoxygen adhesive. The paste residue, adhesion, retention, probe stickiness, and re-peelability of the polyoxyxylene adhesive were measured. The results are shown in Table 1.

-27- 1374173-27- 1374173

【i】 比較例 CS | 44.0 I q I 91.7 I I 66.7 I |一—4.1 —l I 0.02 I 00 寸 in ri X 1 37.6 | 1 7.4 J 1 91.7 | iTi I 36.7 I σ\ | 0.05 1 7.2 I O X 實施例 ON 37.6 | 寸 卜 σ\ 们 36.7 1 2.2 1 | 0.03 00 »n o 〇 00 1 34.2 I I 10.8 | \ 91.7 1 »n I 36.7 I α\ d | 0.04 | 寸 VO o 〇 卜 I 30.8 | 1. 14.2 | 1 91.7 1 m to | 36.7 | 00 d | 0.02 vn CN o 〇 35.8 (N σ\ 91.7 1 m m | 36.7 ] d | 0.02 1 2.0 o 〇 41.0 | Γ- γο CO d 1 91.7 1 m | 36.7 I | 0.05 | 1 4·7 o 〇 寸 | 30.6 | 14.4 1 1 91.7 1 in »〇 | 36.7 I o | 0.02 I m o 〇 m 72.2 | 17.8 ! 丨 16.7 1 O 卜 d | o.oi \q d o 〇 (N 32.1 | G\ 一 100 o v〇 o 对 ON (S | 0.02 I \6 o 〇 36.1 On 〇6 1 91.7 1 *n | 36.7 I ^o· | 0.02 o vn o 〇 調配 (質量份） A-l 1 A-2 A-3 对 1 < in 1 < 1 A-6 I A-7 1 A-8 1 tH ώ CN m ΓΟ m 寸 m u MQ 1甲苯1 黏著力(N/25mm) 保持力(mm) 黏性(N/5mm ·) 殘留甲苯量(ppm) 再剝離性 S g (C) 的內容 實驗結身 -28-[i] Comparative Example CS | 44.0 I q I 91.7 II 66.7 I | I—4.1 —l I 0.02 I 00 in ri X 1 37.6 | 1 7.4 J 1 91.7 | iTi I 36.7 I σ\ | 0.05 1 7.2 IOX Implementation Example ON 37.6 | Inch σ\36.7 1 2.2 1 | 0.03 00 »no 〇00 1 34.2 II 10.8 | \ 91.7 1 »n I 36.7 I α\ d | 0.04 | Inch VO o I I 30.8 | 1. 14.2 1 91.7 1 m to | 36.7 | 00 d | 0.02 vn CN o 〇35.8 (N σ\ 91.7 1 mm | 36.7 ] d | 0.02 1 2.0 o 〇41.0 | Γ- γο CO d 1 91.7 1 m | 36.7 I | 0.05 | 1 4·7 o 〇 inch | 30.6 | 14.4 1 1 91.7 1 in »〇| 36.7 I o | 0.02 I mo 〇m 72.2 | 17.8 ! 丨16.7 1 O 卜d | o.oi \qdo 〇(N 32.1 G\ 一100 ov〇o 对 ON (S | 0.02 I \6 o 〇36.1 On 〇6 1 91.7 1 *n | 36.7 I ^o· | 0.02 o vn o 〇配配(质量份) Al 1 A-2 A-3 to 1 < in 1 < 1 A-6 I A-7 1 A-8 1 tH ώ CN m ΓΟ m inch mu MQ 1 Toluene 1 Adhesion (N/25mm) Retention (mm) Resistance (N / 5mm ·) the residual amount of toluene (ppm) removability S g (C) content of experimental results body -28-

Claims (1)

1374173 (1) 十、申請專利範圍 第94 143 1 84號專利申請案 中文申請專利範圍修正本 民國9*7年8月5日修正 1. 一種無溶劑型聚矽氧黏著劑組成物，其係含有： (A) 於一分子中至少具有2個含烯基的有機基，且具有 分枝之聚二有機矽氧烷；1374173 (1) X. Patent Application No. 94 143 1 84 Patent Application Revision of Chinese Patent Application Revision Amendment to the Republic of China on August 5, 9*7 1. A solvent-free polyadhesive adhesive composition, Containing: (A) a polydiorganooxynonane having at least two alkenyl-containing organic groups in one molecule and having a branch; (B) 於一分子中至少具有2個SiH基的聚有機氫矽氧烷 (C) 含有R^SiOo」單元及Si02單元且R^SiOo.s單元 - /Si02單元的莫耳比爲0.6〜1.7之聚有機矽氧烷（R1係碳數1 . 至1 〇之一價烴基）： (D) 鉑系觸媒。 2 .如申請專利範圍第1項之無溶劑型聚矽氧黏著劑組 成物，其中相對於（A)、（B)、（C)成分之合計100質量份， ^ (A)、（B)成分之合計爲90〜30質量份，但（B)成份中之SiH 基對（A)成分中之烯基的莫耳比成爲0.5〜5之量，（C)成分 爲10〜70質量份，（D)成分之鉑觸媒含有5~2000PPm鉑成分 3 .如申請專利範圍第1或2項之無溶劑型聚矽氧黏著劑 組成物，其中（A)成分爲具有：以下述平均組成式（1)所示 且在25°C之黏度爲5~1000mPa，s的分子中具有分枝之含烯 基的有機基之聚二有機矽氧烷， (R3SiO,/2)a-(R2SiO)b-(RSi03/2)c-(Si〇2)d ⑴ (2) 1374173 (其中，R可爲相同或相異之碳數1〜10的1價烴基，R 之中至少2個含有烯基；a爲2以上之整數，b爲3以上之整 數，c及d爲0以上之整數，ISc + d、a + b + c + dS 400)。 4.如申請專利範圍第1或2項之無溶劑型聚矽氧黏著劑 組成物，其中（B)成分爲具有：以下述平均組成式（2)及/或 (3)所示且在25°C之黏度爲1〜lOOOmPai的1分子中至少具 有2個SiH基之聚有機氫矽氧烷， 【化1】 H H丨s丨R /l\ a-o 3 2 *1 R丨s o • 1 R丨s丨R .a I 3 H 2(B) a polyorganohydroquinone (C) having at least two SiH groups in one molecule containing a R^SiOo unit and a SiO 2 unit and a molar ratio of 0.6 to the R^SiOo.s unit-/SiO 2 unit. Polyorganotoxime of 1.7 (R1 is a carbon number of 1 to 1 fluorene hydrocarbon): (D) Platinum-based catalyst. 2. The solvent-free polyadhesive adhesive composition of claim 1, wherein 100 parts by mass of the components (A), (B), and (C), ^ (A), (B) The total amount of the components is 90 to 30 parts by mass, but the molar ratio of the alkenyl group in the component (B) to the SiH group in the component (B) is 0.5 to 5, and the component (C) is 10 to 70 parts by mass. The platinum catalyst of the component (D) contains 5 to 2000 ppm of a platinum component. The solvent-free polyoxyxide adhesive composition of claim 1 or 2, wherein the component (A) has the following average composition. (1) Polydiorganosiloxane having a branched alkenyl group-containing organic group in the molecule of 5 to 1000 mPa at 25 ° C, (R3SiO, /2) a-(R2SiO) B-(RSi03/2)c-(Si〇2)d (1) (2) 1374173 (wherein R may be the same or different monovalent hydrocarbon group having 1 to 10 carbon atoms, and at least 2 of R may have an alkenyl group ; a is an integer of 2 or more, b is an integer of 3 or more, and c and d are integers of 0 or more, ISc + d, a + b + c + dS 400). 4. The solvent-free polyoxyxene adhesive composition according to claim 1 or 2, wherein the component (B) has: an average composition formula (2) and/or (3) and at 25 The polyorganohydroquinone having at least two SiH groups in one molecule of 1 to 100 mPai at a viscosity of °C, [H1]HH丨s丨R /l\ ao 3 2 *1 R丨so • 1 R丨s丨R .a I 3 H 2 及/或 .【化2】 \ly 2 i 2 R I S 丨 R /fix s \ϊ/ 0 1 2 HIS— R 3 (R2爲不具有爲相同或相異之脂肪族不飽和鍵之1價烴 基，α爲0或1，P、g爲〇以上之整數；α爲0之時，p爲2 以上，表示此有機氫聚矽氧烷之25 °C的黏度成爲 l~1000mPa s之數目；又，s爲2以上之整數，t表示0以上 之整數，且3Ss + t，宜爲3Ss + tS8之整數）。 -2- (3) 1374173 5 _如申請專利範圍第1或2項之無溶劑型聚矽氧黏著劑 組成物，其中（A)成分爲具有：以下述平均組成式（4)所示 且在25 °C之黏度爲5〜1000 mPa.s的分子中具有分枝之含燦 基的有機基之聚二有機氫矽氧烷， (R3Si01/2)c + 2-(R2Si0)b-(RSi03/2)c (4) (其中，R表示與上述相同之基；b爲3以上之整數 爲1以上之整數，b + 2c + 2S 400)。And/or. [Chemical 2] \ly 2 i 2 RIS 丨R /fix s \ϊ/ 0 1 2 HIS- R 3 (R2 is a monovalent hydrocarbon group which does not have the same or different aliphatic unsaturated bonds, α is 0 or 1, P and g are integers above 〇; when α is 0, p is 2 or more, indicating that the viscosity of the organic hydrogen polyoxyalkylene at 25 ° C becomes 1 to 1000 mPa s; s is an integer of 2 or more, t represents an integer of 0 or more, and 3Ss + t is preferably an integer of 3Ss + tS8). -2- (3) 1374173 5 The solvent-free polyadhesive adhesive composition according to claim 1 or 2, wherein the component (A) has: an average composition formula (4) shown below and A polydiorganohydroquinone having a branching organic group containing a ke group in a molecule having a viscosity of 5 to 1000 mPa·s at 25 ° C, (R3Si01/2)c + 2-(R2Si0)b-(RSi03) /2) c (4) (wherein R represents the same base as described above; b is an integer of 3 or more and is an integer of 1 or more, and b + 2c + 2S 400). 6.如申請專利範圍第1或2項之無溶劑型聚矽氧黏著劑 組成物，其中相對於（A)、（B)、（C)成分之合計1〇〇質量份 含有控制劑〇〜8.0質量份作爲（E)成分。 7 ·如申請專利範圍第1或2項之聚矽氧黏著劑組成物 ，其黏著力係使用一以黏著劑層之厚度成爲40μιη之方式 塗布於聚醯亞胺膜基材（厚度25μιη)之黏著膠帶，依JIS Ζ 0237所示之180°剝離黏著力的測定方法進行測定時，成 爲 0·01~4·0 N/25mm 者。6. The solvent-free polyadhesive adhesive composition according to claim 1 or 2, wherein the total amount of the components (A), (B), and (C) is 1 part by mass of the control agent 〇~ 8.0 parts by mass as the component (E). 7. The adhesive composition according to claim 1 or 2, wherein the adhesive force is applied to the polyimide film substrate (thickness 25 μm) by using a thickness of the adhesive layer of 40 μm. When the adhesive tape is measured according to the measurement method of the 180° peeling adhesive force shown in JIS Ζ 0237, it is 0·01 to 4·0 N/25 mm.