九、發明說明： 【智^明戶斤^支系奸々頁4^】 技術領域 本發明係有關於-種組成物，其可於室溫硬化形成聚 石夕氧彈性體，詳而言之係提供-種室溫硬化性聚有機石夕氧 院組成物’其硬化後的物性優異且附著性獲得了改善，並 且相對基材附著面之剝離性亦十分優異。 ° L· ^ 背景技術 於室溫可硬化產生橡膠狀彈性體的聚有機石夕氧烧組成 物中’有-_會由於接觸料氣中的水分㈣生硬化反 應。該類型組成物不需要在使用前秤量本體（原料聚合 物）、交聯劑、催化劑或是混合料物質等煩雜手續，而不 會發生摻合上的失誤，並且且有值 、有優異的接著性，因此被廣 泛地用來作為電工業、電子工紫楚 菜荨之中的彈性接著劑、塗 層’及作為建築用密封材料等。 \種組成物，一船係於分 子末端以經基閉塞之石夕烧醇基的 '、 H t有機矽氧烷中，摻合分 子中具有超過兩個水解性基團 ^ m父聯劑等者，且依交聯劑 的種類，該組成物在硬化時會放 MA_ 出醋酸等有機酸、有機胺、 醯胺、有機搜基胺、杇化合物、 叫、或丙酮等。 其中，脫酵型者因具有作為 人聯劑之烷氧矽烷不只能 便宜取得，而且放出物質為如 r兀个 技 曰士包%、乙醇的醇類’容易揮 發’因此具有無臭氣的問題的優 p, Bg .. ^ 並且具有無金屬腐蝕 問碭寻優點，故被廣泛利用作為 ^电盗、電子機械的塗層等。 但是’上述脫醇型者有硬化遲缓及因保存時系統中存 在之微量水而使交聯劑水解’且由於產生的醇類會切斷原 料聚合物’因此造成安定性不佳等缺點，這些缺點仍有待 克服。為解決這些問題，於特公平5-72424號公報、特公平 5-88866號公報中，藉使用兩末端業已以二烷氧一有機甲矽 烷基封鎖住的聚有機矽氧烷或是兩末端業已以三烷氧曱矽 烷基封鎖的聚有機矽氧烷當作原料聚合物，再選擇經表面 處理以作為填料之二氧化矽、作為交聯劑的烷氧矽烷及鈦 螯合物催化劑組合於該原料聚合物中，以提高保存安定性 及硬化速度(表面皮膜形成速度）。 然而，依本發明人的再次試驗，根據特公平5-72424號 公報、特公平5-88866號公報的技術，在某種程度上，雖能 獲得保存安定性及硬化速度優異的組合物，但其接著性仍 未能令人滿意。 另一方面’在LCD電極塗層等領域中，在使硬化性聚 有機矽氧烷組成物硬化後，因修理等的理由，有時必須將 該硬化物從基材表面去除、剝離，此時該硬化物必須毫不 殘留地從基材表面進行介面剝離。 雖然於特開平4-293962號公報中已揭示了選擇組合兩 末端業已以三烷氧甲矽烷基封鎖住的聚有機矽氧烷與二官 能基烧氧石夕院及鈦螯合物催化劑來作成其有如此特性之硬 化性聚有機矽氧烷組成物，然而，依攄本發明人的再次試 驗，該組成物雖可能與基材表面產生介面剝離’但其對基 材的附著性低，無法作為令人滿意的密対材料。 【明内j 發明之揭示 本發明的目的，係解決前述先前技術的缺點，益提供 —種室溫魏絲有機魏馳祕，其硬化後的物性優 異且附著倾得改善’並且㈣基材附著面之獅性亦十 分優異。 本發明人為了得到能達成上述目標的室溫硬化性聚有 機石夕氧院組成物而進行研討，結果發現併用業已以三炫氧 甲石夕院基封鎖住兩末端的聚有機％氧烧及業已以二炫氧一 有機甲魏基封鎖住兩末端的聚有機⑦氧燒-起作為原料 聚合物’且組合與該原料聚合物不產生反應㈣氧油及二 官能基院氧魏交聯劑是極為有效的，並完成了本發明。 p本發明為-種室溫硬化性聚有機石夕氧烧組成物， 係相對於由 ()95重里％之聚有機矽氧烷，其25。(：時之黏度為 0.1〜lOOOPa · s，η a 士 b 兩末知1以三烷氧甲矽烷基封鎖；及 ()54ll：%之聚有機石夕氧烧，其25。(：時之黏度為 0.1~1000Pa· s » η ^ / λ末知以二烷氧一有機曱矽烷基封鎖 形成之100重量份的聚有機石夕氧烧並含有： ^ 里伤之聚有機矽氧烷，其分子中不含矽烷醇 土 ^氧基及—垸氧基，且在25°c時黏度比（Α)成分及/ 或(B)成分的黏度為低； (D)l〜50重量份少_ & 之二氧化矽粉，其比表面積有50m2/g以 上； (Ε)〇·5〜15重量份之二官能基烷氧矽烷或其部分水解缩 合物；及 (F)〇.l~15重量份之鈦螯合物催化劑。 本發明係藉併用（A)成分與(B)成分’即併用末端三官 能聚合物與末端二官能聚合物以顯現適當的橡膠強度，並 藉摻合與該等聚合物不產生反應的矽氧油（c)，以及二官能 基烷氧矽烷交聯劑(E)以表現高附著性，更藉該等物質的平 衡產生優異的剝離性者。 發明的詳細說明 以下詳細地說明本發明。於本發明使用的（A)、（B)成 分’聚有機石夕氧炫，係為本組成物的原料4合物，且係將 (A)業已以三烷氧曱矽烷基封鎖住兩末端的聚有機矽氣梭 及（B)業已以二烷氧一有機甲矽烷基封鎖住兩末端的聚有 機矽氧烷，以（A)成分5〜95重量％對@)成分95〜5重量％，且 以（A)成分1〇~90重量％對(B)成分9〇~1 〇重量％為佳的比例 摻合而成者。（A)成分若小於5重量％會使對基材之剝離性不 佳’若超過95重量％則會降低對基材之附著性。如此的聚 有機矽氧烷組成物之製造方法已廣為人知，例如：分子鏈 兩末端具有氫化甲矽烷基的聚有機矽氧烷與烯基三烷氧矽 烷或者與烯基烷基二烷氧矽烷一起進行加成反應的方法； 分子鏈兩末端具有烯基甲矽烷基的聚有機矽氧烷與三烷氧 矽烷或者與烷基二烷氧矽烷一起進行加成反應的方法；及 分子鏈兩末端具有氫氧化甲矽烷基的聚有機矽氧烷與四烷 氧矽烷或者與烷基三烷氧矽烷一起進行脫醇縮合反應的方 1354689. 法等。 關於(A)、（B)成分，除末端構造之外並無特別限定’ 可為通常的直鏈狀等的聚有機^夕氧炫，而作為與石夕原子結 合的取代基者’可舉例如烧基、環烧基、稀基、芳香基、 5 方香族烧基等一價煙基、氣甲基、三氟<曱基等鹵代煙基、 /5·氰乙基、γ-氰丙基等氰烷基。 又’（Α)成分的黏度宜為〇.l~l〇〇〇Pa · s ’且以 〇·2〜l〇〇pa · s更佳。若低於〇 1Pa · s則橡膠會變脆而使介面 剝離性變差。再者，若高於lOOOPa · s，則流動性會變差而 1〇 使密封性變差。 (B)成分的黏度宜為〇.1〜i〇〇〇pa · s，且以〇.2~l〇〇Pa · s 為佳。若低於O.lPa· s則橡膠會變脆而使介面剝離性變差。 再者’若高於lOOOPa · s，則流動性會變差而使密封性變差。 於本發明使用的（C)成分可增加聚有機矽氧烷對基材 15 之附著性’且在分子中不含矽烷醇基、三烷氧基、及二烷 氧基。又，其末端係三有機甲矽烷基為佳，且其支鏈係與 (A)及(B)成分相同種為佳。再者’（〇成分在25°C時的黏度 至少一定要比(A)成分、（B)成分任一者的黏度低，而以低於 (A)成分、（B)成分兩者之黏度者為佳。因（〇成分的黏度若 20 比（A)成分及(B)成分高就會從硬化物排出而降低附著性。 具體來說，較佳之(C)成分的黏度為〇.〇2~l〇Pa · s。 相對於(A)、（B)成分合計的100重量份，（C)成分使用 1〜50重量份。這是因為若其摻合量小於1重量份則無法得到 充分的附著性’而超過50重量份則會降低橡膠強度而降低 9 介面剝離性。又，3~30重量份則更佳。 於本發明使用之(D)成分 必叫 WDuni/g以 上的二乳化㈣，例如煙霧性質二氧化砂、培燒二氧化石夕' ，者是於該等二氧切表面以有機氯化魏類、聚有機石夕 钱類、有财氮錢等迄今眾所皆知的處賴進行表面 處理者》在此言及的比表面積係由BET法測定者。（d)成分 以用有機魏顏處理者為佳，尤以时機錢院類處理 成2%含碳量以上的煙霧性質二氧化碎為佳。 相對於(Α)、⑻成分合計的⑽重量份，⑼成分使用 1~50重量份。 其次，於树較狀(E)m讀纽氧碎烧或 其部分水解縮合物，其係作為交聯劑作用。 具體來說，（E)成分可舉例如：二甲基二甲氧矽烷、苯 基甲基二甲氧石夕烧、二苯二甲氧矽烷、乙烯甲基二甲氧石夕 烷、二甲基二乙氧矽烷、甲基丙基二甲氧矽烷、曱基乙烯 二乙氧矽烷等二官能基烷氧矽烷及其部分水解縮合物。以 二S旎烷氧矽烷、一官旎烷氧矽烷等作為交聯劑使用則無 法獲得充分的附著性及介面剝離性。 相對於(A)、（B)成分合計的1〇〇重量份，（e)成分使用 0.5~15重量份左右的量。小於〇.5重量份則保存安定性不 佳’且無法獲得充分的附著性’若超過15重量份則會降低 橡膠強度而降低介面剝離性。- 本發明使用的(F)成分，鈦螯合物催化劑可舉例如：二 異丙氧雙（乙醯醋酸乙醋）銳 '二異丙氧雙（乙醯醋酸甲醋） 欽、二異丙氧雙（乙酿丙酮）鈦、二丁氧雙（乙酿醋酸乙 鈦、二曱氧雙（乙醯醋酸乙酯）鈦等眾所皆知的各種鈦螯合化 合物。 相對於(A)、（B)成分合計的100重量份，（F)成分使用 0.1~15重量份左右的量。 只要無損於本發明之目的，本發明之紐成物除含有上 述(A)〜(F)成分之外’可再加入石英微粉末、碳黑、碳酸辦 等無機填料、該等無機填料經疏水化處理物、附與流動減 黏性劑、黏度調整劑、流動性調整劑、顏料、耐熱劑、難 燃劑、有機溶劑、防黴劑、抗菌劑、紫外光吸收劑、耐熱 性強化劑、難燃化劑、接著性強化劑等各種添加劑。‘”、 圖式簡單說明IX. Description of the invention: [Chi-Ming 明 斤 ^ 支 支 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 4 The room temperature-curable polyorganismite composition is excellent in physical properties after hardening, and the adhesion is improved, and the peeling property with respect to the substrate adhesion surface is also excellent. ° L· ^ Background Art In a polyorgano-oxygen-burning composition which can be hardened at room temperature to produce a rubber-like elastomer, '--- will be hardened by contact with moisture (iv) in the feed gas. This type of composition does not require any complicated procedures such as weighing the bulk (raw material polymer), crosslinking agent, catalyst or mixture material before use, without occurrence of blending errors, and has a value and excellent adhesion. It is widely used as an elastic adhesive, coating in the electric industry, electronics industry, and as a sealing material for construction. \A composition, a ship tied at the end of the molecule with a base occluded in the ', H t organic oxane, the blending molecule has more than two hydrolyzable groups ^ m parent agent, etc. Further, depending on the type of the crosslinking agent, the composition may be subjected to an organic acid such as acetic acid, an organic amine, a guanamine, an organic amine, an anthraquinone compound, or an acetone, etc., upon hardening. Among them, the de-fermented type has a problem that the alkoxysilane which is a human-linked agent is not only inexpensively obtained, but also the substance which is released is such that the alcohol of the technical formula is %, and the alcohol of the alcohol is 'evaporable' and thus has a problem of no odor. Excellent p, Bg .. ^ and has the advantage of no metal corrosion, so it is widely used as a coating for electric thieves and electronic machinery. However, the above-mentioned dealcoholic type has disadvantages such as retardation of hardening and hydrolysis of the crosslinking agent due to the trace amount of water present in the system during storage, and the alcohol produced by the cut off causes the raw material polymer to cause poor stability. These shortcomings still have to be overcome. In order to solve these problems, in the Japanese Patent Publication No. 5-72424 and Japanese Patent Publication No. Hei 5-88866, it is possible to use a polyorganosiloxane which has been blocked with a dialkyloxy-organosyl group at both ends or both ends. A polyorganosiloxane which is blocked with a trialkoxyalkylene group is used as a raw material polymer, and a ceria which is surface-treated as a filler, an alkoxysilane as a crosslinking agent, and a titanium chelate catalyst are combined. In the raw material polymer, the storage stability and the curing rate (surface film formation speed) are improved. However, according to the technique of Japanese Patent Publication No. Hei 5-72424 and Japanese Patent Publication No. Hei 5-88866, a composition excellent in storage stability and curing rate can be obtained to some extent. Its connectivity is still unsatisfactory. On the other hand, in the field of LCD electrode coating and the like, after the curable polyorganosiloxane composition is cured, it may be necessary to remove and peel the cured product from the surface of the substrate due to repair or the like. The cured product must be subjected to interfacial peeling from the surface of the substrate without any residue. It is disclosed in Japanese Laid-Open Patent Publication No. Hei-4-293962 that a combination of a polyorganosiloxane having a blocked terminal of a trialkoxymethyl sulfonyl group and a difunctional pyrithione and a titanium chelate catalyst is disclosed. It has a sclerosing polyorganosiloxane composition having such characteristics. However, according to the retest of the present inventors, the composition may be peeled off from the surface of the substrate, but its adhesion to the substrate is low. As a satisfactory secret material. [Explanation of the invention] The object of the present invention is to solve the above-mentioned shortcomings of the prior art, and to provide a room temperature Weisi organic Weichi secret, which has excellent physical properties after hardening and improved adhesion tilting' and (4) substrate adhesion The lion's face is also very good. The inventors of the present invention conducted research to obtain a room-temperature-curable polyorganismite composition which can achieve the above-mentioned object, and as a result, it has been found that a polyorgano% oxygen-burning which has been blocked at both ends by a trioxomethine The polyorgano 7oxygen is used as a raw material polymer to block the two ends of the dioxo-organic methyl group. The combination does not react with the base polymer. (IV) Oxygen oil and difunctional oxy-trans-crosslinking agent It is extremely effective and has completed the present invention. The present invention is a room temperature curable polyorgano oxy-oxygen composition having a ratio of 95% by weight of polyorganosiloxane. (: viscosity at the time of 0.1~lOOOPa · s, η a 士b two ends know that 1 is blocked with a trialkoxymethyl sulfonyl group; and () 54ll:% of the polyorganic oxy-oxygen, 25 of them. Viscosity of 0.1~1000Pa·s » η ^ / λ is known as 100 parts by weight of polyorganooxime formed by blocking with dialkyloxy-organoalkylene and contains: ^ Polyorganosiloxane The molecule does not contain decyl alcohol oxy and oxime, and the viscosity at 25 ° C is lower than the viscosity of (Α) component and / or (B) component; (D) l~50 parts by weight less _ & cerium oxide powder having a specific surface area of 50 m 2 /g or more; (Ε) 5 5 to 15 parts by weight of a difunctional alkoxy decane or a partially hydrolyzed condensate thereof; and (F) 〇.l~15 Parts by weight of titanium chelate catalyst. The invention combines (A) component and (B) component together, that is, a terminal trifunctional polymer and a terminal difunctional polymer are used together to exhibit appropriate rubber strength, and by blending with The helium oxide oil (c) in which the polymer does not react, and the difunctional alkoxysilane crosslinker (E) exhibit high adhesion, and further excellent balance is produced by the balance of the substances. DETAILED DESCRIPTION OF THE INVENTION The present invention will be described in detail below. The components (A) and (B) used in the present invention are polyorganisms, which are the starting materials of the composition and are (A) The polyorganofluorene shuttle at both ends has been blocked with a trialkoxyalkylene group and (B) the polyorganosiloxane has been blocked with a dialkoxy-organosylalkyl group at both ends, with (A) component 5~ 95% by weight of the @) component is 95 to 5% by weight, and is blended in a ratio of (A) component of 1% to 90% by weight to (B) component of 9% to 1% by weight. (A) When the content is less than 5% by weight, the peeling property to the substrate is not good. If it exceeds 95% by weight, the adhesion to the substrate is lowered. Such a method for producing a polyorganosiloxane composition is widely known, for example, a molecule. a method of performing an addition reaction of a polyorganooxyalkylene having a hydrogenated methylation group with an alkenyl trialkoxide or an alkenylalkyldoxantane at both ends of the chain; having an alkenylmethyl group at both ends of the molecular chain Polyorganosilating alkane with a trialkoxy alkane or an alkyldialkyloxane And a method of performing a dealcoholization condensation reaction between a polyorganooxynonane having a methyl hydrazinyl group at both ends of the molecular chain and a tetraalkoxy decane or an alkyltrial alkane decane. About (A), The component (B) is not particularly limited as long as it is a terminal structure, and may be a polyorganosiloxane such as a normal linear chain, and a substituent which is bonded to a cerium atom may be, for example, a burnt group or a ring. a halogenated nicotine group such as a mercapto group, a dilute base, an aromatic group, a 5-party fragrant burn group, a halogenated nicotine group such as a gas methyl group, a trifluoro < fluorenyl group, a /5-cyanoethyl group, a γ-cyanopropyl group, etc. The viscosity of the '(Α) component is preferably 〇.l~l〇〇〇Pa · s ' and is preferably 〇·2~l〇〇pa · s. If it is less than Pa 1 Pa · s, the rubber becomes brittle and the interfacial peelability deteriorates. Further, if it is higher than 100 OPa·s, the fluidity may be deteriorated and the sealing property may be deteriorated. The viscosity of the component (B) is preferably 〇.1~i〇〇〇pa · s, and preferably 〇.2~l〇〇Pa · s. If it is less than 0.1 Pa·s, the rubber becomes brittle and the interface peelability is deteriorated. Further, if it is higher than 100 OOPa · s, the fluidity is deteriorated and the sealing property is deteriorated. The component (C) used in the present invention can increase the adhesion of the polyorganosiloxane to the substrate 15 and does not contain a stanol group, a trialkoxy group, and a dialkoxy group in the molecule. Further, the terminal is preferably a triorganosylalkyl group, and the branched chain is preferably the same as the components (A) and (B). Furthermore, '(the viscosity of the bismuth component at 25 ° C must be at least lower than the viscosity of either (A) component or (B) component, and lower than the viscosity of both (A) component and (B) component. It is preferable that (the viscosity of the bismuth component is 20% higher than the components (A) and (B), and the adhesion is lowered from the cured product. Specifically, the viscosity of the component (C) is preferably 〇.〇. 2~l〇Pa · s. The component (C) is used in an amount of 1 to 50 parts by weight based on 100 parts by weight of the total of the components (A) and (B). This is because if the blending amount is less than 1 part by weight, the product cannot be obtained. If the amount is more than 50 parts by weight, the rubber strength is lowered to reduce the 9-layer peeling property. Further, 3 to 30 parts by weight is more preferable. The component (D) used in the present invention must be WDuni/g or more. Emulsification (4), such as smog-type silica sand, sinter-burning sulphur dioxide sap, is on the surface of these dioxometers, organic chlorinated Wei, poly-organic stone, money, money, etc. The specific surface area mentioned here is determined by the BET method. (d) The composition is preferably treated with organic Wei Yan, especially when It is preferable to treat the smog-like oxidized granules with a carbon content of 2% or more. For the total (10) parts by weight of the (Α) and (8) components, the component (9) is used in an amount of 1 to 50 parts by weight. (E) m read neochased or partially hydrolyzed condensate thereof, which acts as a crosslinking agent. Specifically, the component (E) may, for example, be dimethyldimethoxydecane or phenylmethyldimethyl a difunctional group such as oxysulfuric acid, benzophenone, ethylene methyl dimethoxide, dimethyl diethoxy decane, methyl propyl dimethoxy decane, decyl ethylene diethoxy decane Alkoxy oxane and a partially hydrolyzed condensate thereof. When used as a crosslinking agent such as di S-decane oxy decane or mono- sulfoxane oxane, sufficient adhesion and interfacial peelability cannot be obtained. Relative to (A), (B) The total amount of the component is 1 part by weight, and the component (e) is used in an amount of about 0.5 to 15 parts by weight. When the amount is less than 5% by weight, the stability is poorly stored and sufficient adhesion is not obtained. The rubber strength is lowered to lower the interface peelability. - The component (F) used in the present invention, the titanium chelate catalyst For example: diisopropyloxybis(acetonitrileacetate) acetra-diisopropyloxybis(acetamidineacetate), diisopropyloxybis(ethyl acetate) titanium, dibutoxy double (B Various titanium chelate compounds, such as titanium acetate, dioxane bis(acetate ethyl acetate), etc., are used, and (F) is used in combination with 100 parts by weight of the total of the components (A) and (B). An amount of about 0.1 to 15 parts by weight. The core of the present invention may be further added with quartz fine powder, carbon black, carbonic acid, etc., in addition to the above components (A) to (F), as long as the object of the present invention is not impaired. Inorganic filler, hydrophobized material of such inorganic filler, attached flow reducing agent, viscosity adjuster, fluidity regulator, pigment, heat-resistant agent, flame retardant, organic solvent, anti-fungal agent, antibacterial agent, ultraviolet Various additives such as a light absorber, a heat resistance enhancer, a flame retardant, and an adhesion enhancer. ‘”, simple description
第1圖係顯示在實施例中介面剝離率及剝離力 狀況之圖。 【實施冷式】 實施例 但本發明絕不 ’’都表示，，重量 雖於以下舉實施例具體地說明本發明， 限定於以下實施例。再者，實施例中的，，份 份”。 實施例1 合物⑷(使分子鏈兩末端具有氫氧化甲 而得之二氣;广T行脫醇縮合反應 乳甲夕烷基封鎖住兩末端的聚有 ⑽的黏㈣a.s))、5G__)(⑻鍵兩^ 1354689. 具有氫氧化甲矽烷基的聚二甲基矽氧烷與曱基三甲氧矽烷 一起做脫醇缩合反應而得之以曱基二曱氧甲矽炫基封鎖住 兩末端的聚有機矽氧烷(乃^的黏度為3Pa· s))、10份的矽 氧油（c)(以三曱基曱矽烷基封鎖住兩末端的二曱基矽氧烷 5 (25C的黏度為0.lPa· s))、及15份由BET法所測得之比表面 積為170m2/g且以六曱基二矽氮烷進行過表面處理的乾式 一氧化矽（含碳量3.0% :二氧化矽A)，並於室溫混合30分 鐘，再於150。(：與在40mmHg的減壓狀況下一邊加熱一邊混 合2小時。 10 冷卻至室溫之後’於該混合物加入了 2份的（F)二異丙 氧雙（乙酿醋酸乙酯）欽及3份的（E)二曱基二甲氧石夕烧，在隔 絕濕氣之情形下混合至均一狀。 於長80mm，寬25mm ’厚5mm的玻璃板上，將所得到 的組成物塗布至2mm的厚度，且於23。(：、50%RH的狀況下 15 硬化三天。接下來’如第1圖所示地藉自動紀錄器使橡膠及 玻璃進行剝離，並評定當時的介面剝離率及剝離力。 實施例2 於實施例1中使用的聚合物(A)30份、聚合物(b)7〇份、 石夕氣油（C)5份中摻合10份的二氧化石夕A，並於室溫下混合3〇 20 分鐘’進一步在150。(：與在40mmHg的減壓狀況下一邊加熱 一邊混合了 2小時。 冷卻至室溫之後，於該混合物中加入了 2份的（F)二異 丙氧雙（乙醯醋酸乙酯）鈦及3份的（E)乙烯甲基二甲氧石夕 燒’並在隔絕濕氣之情形下混合至均一狀。對所得到的組 12 1354689. 成物進行與實施例1同樣的評定。 實施例3 於實施例1中使用的聚合物(A)50份、聚合物(B)50份、 石夕氧油（C)15份中摻合了 15份以BET法測得之比表面積為 5 170m2/g且以二甲基二氣矽烷進行過表面處理的乾式二氧 化石夕（含碳量1.0% :二氧化矽B)，並於室溫下混合30分鐘， 再於150°C與在4〇mrnHg的減壓狀況下一邊加熱—邊混合2 小時。 冷卻至室溫之後，於該混合物加入了 2份的（F)二異丙 1〇氧雙（乙醯醋酸乙酯）鈦及3份的（E)二甲基二曱氧矽烷，並在 隔絕濕氣之情形下混合至均一狀。對所得到的組成物進行 與實施例1同樣的評定。 丁 比較例1 於實施例1中不摻合矽氧油（c)，再者，（E)以甲基三甲 15 ^㈣取代二甲基二甲氧械。除此以外，以同樣方法調 製組成物，並進行同上述的評定。其結果顯示於表i中。 比較例2 於實施例1中不使用聚合物（B)而使用1〇〇份的聚合物 扣（A)，再者，不摻合石夕氧油(c)。除此以外，以同樣方法調製 組成物，並進行同上述的評定。其結果顯示於表丨中。 比較例3 於實施例1中不摻合矽氧油（C)。除此之外，以同樣方 法調製組成物，並進行同上述的収。其結果顯示於表！ 中。 & 13 1354689 表1 貫施 例1 實施 例2 實施 例3 比較 例1 比較 例2 比較 例3 聚合物A 50 30 50 50 100 50 聚合物B 50 70 50 50 50 矽氧油C 10 5 10 二氧化矽A 15 10 15 15 15 二氧化矽B 15 二甲基二曱氧矽烷 3 3 3 3 乙烯曱基二曱氧矽烷 2 甲基三甲氧矽烷 3 二異丙氧雙（乙醯醋酸乙酯）鈦 2 2 2 2 2 2 介面剝離率（％) 100 100 100 10 100 100 剝離力（附著性)(N/m) 60 55 50 70 30 35Fig. 1 is a graph showing the peeling rate and peeling force of the interposer in the examples. [Implementation of the cold type] The present invention is not limited to the present invention, and the present invention is specifically described by the following examples, and is limited to the following examples. Further, in the examples, the parts are "Examples" (4) (the two ends of the molecular chain have a hydrogen peroxide obtained by two molecules; the broad T-decoholization condensation reaction of the lactine alkyl blockade two The end of the poly (10) is viscous (4) a.s)), 5G__) ((8) bond two ^ 1354689. Polydimethyl methoxy oxane with carbaryl alkyl group and decyl trimethoxy decane are used together for the dealcoholization condensation reaction The polyorganooxynonane (the viscosity of 3 Pa·s) of the two ends is blocked by fluorenyl dioxin, and 10 parts of the oxime oil (c) (trialkyl sulfonyl group) Blocking the dimercapto oxane 5 at both ends (25C viscosity is 0.1 Pa·s), and 15 parts of the specific surface area measured by the BET method is 170 m 2 /g and hexamethylene diazoxide The surface-treated dry cerium oxide (containing 3.0% carbon: cerium oxide A) was mixed at room temperature for 30 minutes and then at 150. (: mixed with heating under a reduced pressure of 40 mmHg for 2 hours while heating 10 After cooling to room temperature, add 2 parts of (F) diisopropoxy bis(ethyl acetate) and 3 parts of (E) dimercapto dimethyl sulphate to the mixture. Isolated In the case of gas, it is mixed to a uniform shape. The obtained composition is applied to a thickness of 2 mm on a glass plate having a length of 80 mm and a width of 25 mm and a thickness of 5 mm, and is cured at a condition of 23% (in the case of 50% RH). Three days. Next, the rubber and glass were peeled off by an automatic recorder as shown in Fig. 1, and the interface peeling rate and peeling force at that time were evaluated. Example 2 Polymer used in Example 1 (A) 30 parts, 7 parts of polymer (b), 7 parts of Shixia gas oil (C), 10 parts of silica magnetite A were blended, and mixed at room temperature for 3 〇 20 minutes 'further at 150. (: It was mixed with heating under reduced pressure of 40 mmHg for 2 hours. After cooling to room temperature, 2 parts of (F) diisopropyloxybis(ethyl acetate) titanium and 3 parts were added to the mixture. (E) Ethylene methyl dimethyl methoxide was burned and homogenized in the presence of moisture. The obtained group 12 1354689. The same composition was evaluated as in Example 1. Example 3 50 parts of the polymer (A) used in Example 1, 50 parts of the polymer (B), and 15 parts of the Oxime oil (C) were blended in 15 parts by the BET method. a dry-type silica dioxide having a specific surface area of 5 170 m 2 /g and surface-treated with dimethyl dioxane (containing 1.0% carbon: cerium oxide B), and mixing at room temperature for 30 minutes, and then While heating at 150 ° C under a reduced pressure of 4 〇 mrnHg for 2 hours. After cooling to room temperature, 2 parts of (F) diisopropyl 1 oxirane double (acetonitrile acetate B) was added to the mixture. Ester) titanium and 3 parts of (E) dimethyldioxane, and mixed to a uniform state in the absence of moisture. The composition obtained was evaluated in the same manner as in Example 1. Comparative Example 1 In the first embodiment, the oxygenated oil (c) was not blended, and further, (E) was substituted with methyltrimethyl 15 ^ (tetra). Except for this, the composition was adjusted in the same manner and evaluated as above. The results are shown in Table i. Comparative Example 2 In Example 1, a polymer (B) was used without using the polymer (B), and further, the alumite oil (c) was not blended. Except for this, the composition was prepared in the same manner and evaluated as above. The results are shown in the table. Comparative Example 3 In the example 1, the oxime oil (C) was not blended. In addition to this, the composition was prepared in the same manner and subjected to the above-mentioned collection. The results are shown in the table! in. & 13 1354689 Table 1 Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Polymer A 50 30 50 50 100 50 Polymer B 50 70 50 50 50 Oxygenated oil C 10 5 10 II Cerium oxide A 15 10 15 15 15 cerium oxide B 15 dimethyl dioxa oxy decane 3 3 3 3 ethylene decyl dioxane 2 methyl methoxy decane 3 diisopropyl oxy bis (ethyl acetate) Titanium 2 2 2 2 2 2 Interfacial peeling rate (%) 100 100 100 10 100 100 Peeling force (adhesion) (N/m) 60 55 50 70 30 35
14 1354689·14 1354689·
【圖式簡單說明】 第1圖係顯示在實施例中介面剝離率及剝離力的評定 狀況之圖。 【主要元件符號說明】 無 15BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a view showing the evaluation of the peeling rate and the peeling force of the interposer in the examples. [Main component symbol description] None 15