JP3550198B2 - One-part room temperature curable adhesive composition - Google Patents
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Description
【０００１】
【産業上の利用分野】
本発明は、一液型室温硬化性接着剤組成物に関する。
【０００２】
【従来の技術】
従来より、タイル貼り工事にはセメントモルタルもしくはポリマーセメントモルタルが接合材料として広く用いられており、特に外装タイル貼り工事に関しては、現在でもセメントモルタルもしくはポリマーセメントモルタルが一般的に用いられている。しかし、上記セメントモルタルもしくはポリマーセメントモルタルを用いるタイル貼り工事には高度な専門的技能を有する技能工が必要であり、最近ではそのような技能工の確保が困難になりつつあるという問題点がある。
【０００３】
近年、硬化後にゴム弾性を有し、外力が加えられた場合の歪みを吸収し得る室温硬化性接着剤がタイル貼り工事用等として検討されており、例えば、分子中に少なくとも１つの反応性珪素基を含有するゴム系有機重合体、エポキシ樹脂、エポキシ基と反応しうる官能基と反応性珪素基とを分子中に含有するシリコン化合物及びエポキシ樹脂硬化剤を有効成分として含有し、上記各成分が特定の比率であることを特徴とする硬化性樹脂組成物（特公平３−３１７２６号公報）や、エポキシ樹脂と、１分子中にエポキシ樹脂と反応し得る官能基及び反応性珪素基を有するシリコン化合物とを含む接着剤組成物であって、上記各成分を特定の割合で配合することを特徴とする接着剤組成物（特開平５−１４８４６９号公報）等が提案されている。
【０００４】
しかし、上記提案による組成物は二液型であるため、塗布作業直前に二液を均一に混合する必要があり、混合作業が煩雑で作業性が悪かったり、混合不良や混合ミスに起因する接着性能の低下を来し易い等の問題点がある。又、二液を混合して得られる混合液の揺変性が不充分であるため、例えば垂直面にタイルのような建材等を接着する場合、混合液が硬化する前にタイルのような建材等にズレが生じ易く支障を来すという問題点もある。
【０００５】
【発明が解決しようとする課題】
本発明は、上記従来の問題点を解決するため、作業性が良好であり、垂直面にタイルのような建材等を接着する場合にもズレを生じ難いと共に、硬化後は優れた接着性、耐衝撃性、耐久性等を発揮する一液型室温硬化性接着剤組成物を提供することを目的とする。
【０００６】
【課題を解決するための手段】
一般に、垂直面にタイルのような建材等（以下、「被着体」と記す）を接着する場合、接着剤に無機質もしくは有機質の充填剤を含有させて接着剤の粘度や揺変性を高めることにより、接着剤が硬化する前に生じる被着体のズレを防止することが行われている。しかし、接着剤に含有させる充填剤の量を単純に増加させると、接着剤の粘度が高くなり過ぎて塗布作業性が悪くなると共に、硬化後の柔軟性が乏しくなって耐衝撃性や耐久性等が不充分となる傾向がある。又、単に１種類の充填剤のみを用いると、接着剤のベースポリマーに均一分散する量が制約されるため充分な粘度や揺変性を得られずズレ防止効果が乏しくなる傾向がある。
【０００７】
本発明者等は上記の点に鑑み鋭意検討した結果、主成分として分子中に少なくとも１個の反応性珪素基を含有する有機重合体を用い、該有機重合体に対し、揺変剤として４種類に分類される揺変剤、及び有機重合体の硬化促進触媒として有機錫触媒をそれぞれ特定量含有させることにより、上記目的を達成し得ることを見出し、本発明を完成するに至った。
【０００８】
即ち、本発明による一液型室温硬化性接着剤組成物は、分子中に少なくとも１個の反応性珪素基を有する有機重合体１００重量部に対し、コロイド炭酸カルシウム５０〜１００重量部、合成スメクタイト５〜１５重量部、疎水性微粉シリカ１〜１０重量部、有機揺変剤１〜５重量部、有機錫触媒０．５〜３重量部及び脱水剤１〜５重量部を含有して成ることを特徴とし、そのことにより上記目的が達成される。
【０００９】
本発明による一液型室温硬化性接着剤組成物には、主成分として分子中に少なくとも１個の反応性珪素基を有する有機重合体が用いられる。
【００１０】
ここで言う反応性珪素基とは、水酸基もしくは加水分解性基の結合した珪素原子を含む珪素原子含有基であって、シラノール縮合反応によりシロキサン結合を形成し得る基を意味する。
【００１１】
上記加水分解性基の種類としては、特に限定されるものではないが、各種アルコキシ基が挙げられ、これらの１種もしくは２種以上が好適に用いられるが、なかでも反応性が穏やかなメトキシ基、エトキシ基等がより好適に用いられる。
【００１２】
上記分子中に少なくとも１個の反応性珪素基を有する有機重合体の具体例としては、例えば、下記一般式（１）に示されるようなポリプロピレンオキシドを主鎖骨格とし、メトキシ基を加水分解性基として含有する変成シリコン化合物が挙げられ、好適に用いられる。
【化１】
【００１３】
本発明による一液型室温硬化性接着剤組成物に揺変剤として用いられるコロイド炭酸カルシウムの種類としては、特に限定されるものではないが、脂肪酸系表面処理剤、珪酸系表面処理剤、スルホン酸系表面処理剤等により表面処理を施されたコロイド炭酸カルシウム等が挙げられ、これらの１種もしくは２種以上が好適に用いられるが、なかでも脂肪酸系表面処理剤で表面処理を施された平均粒子径が０．０５〜０．２μｍであるコロイド炭酸カルシウムが揺変性付与効果に優れるのでより好適に用いられる。
【００１４】
本発明においては、前記分子中に少なくとも１個の反応性珪素基を有する有機重合体１００重量部に対し、上記コロイド炭酸カルシウムが５０〜１００重量部含有されていることが必要である。
【００１５】
分子中に少なくとも１個の反応性珪素基を有する有機重合体１００重量部に対するコロイド炭酸カルシウムの含有量が５０重量部未満であると、充分な揺変性付与効果を得られず、逆に１００重量部を超えると、得られる接着剤硬化物の柔軟性が乏しくなり耐衝撃性や耐久性が低下する。
【００１６】
本発明による一液型室温硬化性接着剤組成物に揺変剤として用いられる合成スメクタイトの種類としては、特に限定されるものではないが、各種膨潤性層状珪酸塩が挙げられ、これらの１種もしくは２種以上が好適に用いられるが、なかでも親油化処理を施された合成スメクタイトがより好適に用いられる。
【００１７】
上記親油化処理を施された合成スメクタイトの具体例としては、コープケミカル社より市販されている商品名「ルーセンタイト」が挙げられ好適に用いられる。
【００１８】
本発明においては、前記分子中に少なくとも１個の反応性珪素基を有する有機重合体１００重量部に対し、上記合成スメクタイトが５〜１５重量部含有されていることが必要である。
【００１９】
分子中に少なくとも１個の反応性珪素基を有する有機重合体１００重量部に対する合成スメクタイトの含有量が５重量部未満であると、充分な揺変性付与効果を得られず、逆に１５重量部を超えると、得られる接着剤硬化物の柔軟性が乏しくなり耐衝撃性や耐久性が低下する。
【００２０】
本発明による一液型室温硬化性接着剤組成物に揺変剤として用いられる疎水性微粉シリカの種類としては、特に限定されるものではないが、親水性シリカ中のシラノール基がジメチルジクロロシラン等により変成された各種疎水性微粉シリカが挙げられ、これらの１種もしくは２種以上が好適に用いられが、なかでも一次粒子の平均粒子径が５〜１５ｎｍである疎水性微粉シリカが揺変性付与効果に優れるのでより好適に用いられる。
【００２１】
本発明においては、前記分子中に少なくとも１個の反応性珪素基を有する有機重合体１００重量部に対し、上記疎水性微粉シリカが１〜１０重量部含有されていることが必要である。
【００２２】
分子中に少なくとも１個の反応性珪素基を有する有機重合体１００重量部に対する疎水性微粉シリカの含有量が１重量部未満であると、揺変性付与効果を殆ど得られず、逆に１０重量部を超えると、得られる接着剤組成物の粘度が高くなり過ぎて塗布作業性が悪化する。
【００２３】
本発明による一液型室温硬化性接着剤組成物に揺変剤として用いられる有機揺変剤の種類としては、特に限定されるものではないが、植物重合油系揺変剤、水添ひまし油系揺変剤、脂肪酸アマイド系揺変剤等が挙げられ、これらの１種もしくは２種以上が好適に用いられが、なかでも脂肪酸アマイド系揺変剤が揺変性付与効果に優れるのでより好適に用いられる。
【００２４】
本発明においては、前記分子中に少なくとも１個の反応性珪素基を有する有機重合体１００重量部に対し、上記有機揺変剤が１〜５重量部含有されていることが必要である。
【００２５】
分子中に少なくとも１個の反応性珪素基を有する有機重合体１００重量部に対する有機揺変剤の含有量が１重量部未満であると、充分な揺変性付与効果を得られず、逆に５重量部を超えると、得られる接着剤硬化物の柔軟性が乏しくなり、耐衝撃性や耐久性が低下する。
【００２６】
本発明による一液型室温硬化性接着剤組成物に硬化促進触媒として用いられる有機錫触媒の種類としては、特に限定されるものではないが、ジブチル錫ジラウレイト、ジブチル錫ジマレート、ジブチル錫フタレイト、オクチル酸錫等のカルボン酸塩等が挙げられ、これらの１種もしくは２種以上が好適に用いられる。
【００２７】
本発明においては、前記分子中に少なくとも１個の反応性珪素基を有する有機重合体１００重量部に対し、上記有機錫触媒が０．５〜３重量部含有されていることが必要である。
【００２８】
分子中に少なくとも１個の反応性珪素基を有する有機重合体１００重量部に対する有機錫触媒の含有量が０．５重量部未満であると、充分な硬化促進効果を得られず、逆に３重量部を超えると、もはや硬化促進効果は向上しないにもかかわらず希釈作用が出て得られる接着剤組成物に好ましくない影響を与える。
【００２９】
本発明においては、前記分子中に少なくとも１個の反応性珪素基を有する有機重合体１００重量部に対し、上記脱水剤が１〜５重量部含有されていることが必要である。
本発明による一液型室温硬化性接着剤組成物に主成分として用いられる分子中に少なくとも１個の反応性珪素基を有する有機重合体は水分により硬化反応が進行するので、接着剤組成物中の微量水分により貯蔵中に接着剤組成物が増粘もしくはゲル化するのを防止するためである。
上記脱水剤の種類としては、特に限定されるものではないが、ビニルトリメトキシシラン等のビニルシラン類が挙げられ、これらの１種もしくは２種以上が好適に用いられる。
【００３０】
本発明による一液型室温硬化性接着剤組成物には、上述の各成分以外に、本発明の目的を阻害しない範囲で必要に応じ、接着性付与剤、粘度調整剤、着色剤、酸化防止剤、紫外線吸収剤、軟化剤、界面活性剤、難燃剤、消泡剤等の各種添加剤が含有されていても良い。
【００３１】
上記接着性付与剤の種類としては、特に限定されるものではないが、γ−（２−アミノエチル）アミノプロピルトリメトキシシラン、γ−アミノプロピルトリエトキシシラン等のアミノシラン類、γ−メルカプトプロピルトリメトキシシラン等のメルカプトシラン類、γ−グリシドキシプロピルトリメトキシシラン等のエポキシシラン類等のシランカップリング剤が挙げられ、これらの１種もしくは２種以上が好適に用いられる。
【００３２】
上記粘度調整剤の種類としては、特に限定されるものではないが、炭酸カルシウム、タルク、クレー等の充填剤やジブチルフタレート、ジオクチルフタレート等の可塑剤等が挙げられ、これらの１種もしくは２種以上が好適に用いられる。
【００３３】
上記着色剤の種類としては、特に限定されるものではないが、カーボンブラック、酸化チタン、弁柄等が挙げられ、これらの１種もしくは２種以上が好適に用いられる。
【００３４】
上記酸化防止剤の種類としては、特に限定されるものではないが、ヒンダードアミン系酸化防止剤やヒンダードフェノール系酸化防止剤等が挙げられ、これらの１種もしくは２種以上が好適に用いられる。
【００３５】
本発明による一液型室温硬化性接着剤組成物の製造方法は、特別なものではなく、所定量の各成分を秤量し、ミキサーやニーダー等の混合機で予備混合を行った後、例えば三本ロール等を用いて均一に混練りすることにより所望の一液型室温硬化性接着剤組成物を得ることが出来る。
【００３６】
【作用】
本発明による一液型室温硬化性接着剤組成物は、分子中に少なくとも１個の反応性珪素基を有する有機重合体を主成分とし、４種類に分類される揺変剤をそれぞれ特定量併用して含有するので、適正な粘度と揺変性を有し、作業性が良好であると共に、垂直面にタイルのような建材等を接着する場合にもズレを生じ難い。又、該接着剤組成物の硬化皮膜は柔軟性に富むので、優れた接着性、耐衝撃性、耐久性等を発揮する。
【００３７】
【実施例】
本発明をさらに詳しく説明するため、以下に実施例をあげる。尚、実施例中の「部」は「重量部」を意味する。
【００３８】
（実施例１）
【００３９】
（１）一液型室温硬化性接着剤組成物の作製
先ず、合成スメクタイト（商品名「ルーセンタイトＳＰＮ」、コープケミカル社製）８部及びトルエン８部をポリエチレン容器中に秤取し、ヘラを用いて手練りし合成スメクタイトの塊をつぶした。次いで、上記ポリエチレン容器中に、分子中に少なくとも１個の反応性珪素基を有する有機重合体として変成シリコン化合物（商品名「サイリルＳＡＴ２００」、鐘淵化学工業社製）１００部、コロイド炭酸カルシウム（商品名「ＣＣＲ」、白石工業社製）６０部、疎水性微粉シリカ（商品名「アエロジルＲ−２０２」、日本アエロジル社製）５部、有機揺変剤として脂肪酸ビスアマイド（商品名「ディスパロン＃６５００」、楠本化成社製）２部及び脱水剤としてビニルトリメトキシシラン（商品名「ＫＢＭ１００３」、信越シリコーン社製）３部を秤取し、ヘラを用いて手練りした後、三本ロールに３回通して均一な混練物を得た。得られた混練物をガラス瓶に入れて１２０℃のギヤーオーブン中で３時間加熱した後、室温まで冷却し、有機錫触媒としてジブチル錫ジラウレイトとジブチル錫オキサイドの混合物（商品名「ＳＢ−６５」、三共有機合成社製）２部を添加混合して、一液型室温硬化性接着剤組成物を得た。
【００４０】
（２）評価
上記で得られた一液型室温硬化性接着剤組成物の各種性能を以下の方法で評価した。その結果は表１に示すとおりであった。
【００４１】
▲１▼垂直面でのズレ性：垂直に保持されたボードに、４ｍｍ角の櫛目ごてを用いて、上記接着剤組成物を塗布量が１．２ｋｇ／ｍ２ となるように塗布した。次いで直ちに、幅５０ｍｍ、長さ５０ｍｍ、厚み４ｍｍの２枚の板ガラス間の中心線上に先端がフック状に加工された針金を挟んで接着して予め作製しておいた重量６０ｇの被着体を、上記ボードの塗布面に針金のフック状部が下部となるように貼り付け、針金のフック状部に１５０ｇから１０ｇきざみで重くした荷重を掛け、被着体がズレ始める時の最小荷重（ｇ）を測定した。
【００４２】
▲２▼硬化物の物性：上記接着剤組成物を厚み２ｍｍのシート状に展延し、２３℃−６５％ＲＨの恒温恒湿室で７日間養生硬化させた後、ＪＩＳ Ｋ−６３０１「加硫ゴム物理試験方法」に準拠して、３号ダンベルで打ち抜き、最大点抗張力（ｋｇ／ｃｍ２ ）及び最大点伸び率（％）を測定した。
【００４３】
（実施例２〜５）
【００４４】
一液型室温硬化性接着剤組成物の作製において、表１に示す配合組成としたこと以外は実施例１と同様にして４種類の一液型室温硬化性接着剤組成物を得た。
【００４５】
（比較例１〜３）
【００４６】
一液型室温硬化性接着剤組成物の作製において、合成スメクタイト及びトルエンを用いることなく、表１に示す配合組成としたこと以外は実施例１と同様にして３種類の一液型室温硬化性接着剤組成物を得た。
【００４７】
（比較例４）
【００４８】
一液型室温硬化性接着剤組成物の作製において、表１に示す配合組成としたこと以外は実施例１と同様にして一液型室温硬化性接着剤組成物を得た。
【００４９】
実施例２〜５及び比較例１〜４で得られた８種類の一液型室温硬化性接着剤組成物の各種性能を実施例１と同様にして評価した結果は表１に示すとおりであった。
【００５０】
【表１】
【発明の効果】
以上述べたように、本発明による一液型室温硬化性接着剤組成物は、良好な作業性を有し、垂直面にタイルのような建材等を接着する場合にもズレを生じ難いと共に、硬化物は柔軟性に富み、優れた接着性、耐衝撃性、耐久性等を発揮するので、垂直面に建材等を接着する用途にも好適に用いられる。[0001]
[Industrial applications]
The present invention relates to a one-part room temperature-curable adhesive composition.
[0002]
[Prior art]
Conventionally, cement mortars or polymer cement mortars have been widely used as joining materials in tile work, and cement mortars or polymer cement mortars are generally still used today, particularly for exterior tile work. However, the tiling work using the cement mortar or the polymer cement mortar requires a skilled worker having a high level of specialized skill, and there is a problem that it is becoming difficult to secure such a skilled worker recently. .
[0003]
In recent years, room-temperature-curable adhesives that have rubber elasticity after curing and can absorb distortion when an external force is applied have been studied for use in tiling work. For example, at least one reactive silicon A rubber-based organic polymer containing a group, an epoxy resin, a silicon compound containing a functional group capable of reacting with an epoxy group and a reactive silicon group in a molecule and an epoxy resin curing agent as active ingredients, and each of the above components Has a specific ratio, a curable resin composition (Japanese Patent Publication No. 3-31726), an epoxy resin, and a functional group and a reactive silicon group capable of reacting with the epoxy resin in one molecule. There has been proposed an adhesive composition containing a silicon compound, wherein the above components are blended in a specific ratio (Japanese Patent Application Laid-Open No. 5-148469).
[0004]
However, since the composition according to the above proposal is a two-part type, it is necessary to uniformly mix the two parts immediately before the coating operation, and the mixing operation is complicated and the workability is poor, or the adhesion due to poor mixing or mixing error is caused. There is a problem that the performance tends to decrease. In addition, since the thixotropic properties of the mixture obtained by mixing the two liquids are insufficient, for example, when a building material such as a tile is bonded to a vertical surface, the building material such as a tile before the mixture hardens. In addition, there is also a problem that deviation occurs easily and causes trouble.
[0005]
[Problems to be solved by the invention]
The present invention solves the above-mentioned conventional problems, the workability is good, and even when bonding a building material such as a tile on a vertical surface, it is unlikely that a gap will occur, and after curing, excellent adhesion, An object of the present invention is to provide a one-part room temperature curable adhesive composition exhibiting impact resistance, durability and the like.
[0006]
[Means for Solving the Problems]
Generally, when building materials such as tiles (hereinafter referred to as "adherend") are bonded to a vertical surface, an inorganic or organic filler is included in the adhesive to increase the viscosity and thixotropic properties of the adhesive. Thus, the displacement of the adherend before the adhesive is cured is prevented. However, simply increasing the amount of filler contained in the adhesive causes the viscosity of the adhesive to become too high, resulting in poor application workability and poor flexibility after curing, resulting in impact resistance and durability. Tend to be insufficient. Further, when only one kind of filler is used, the amount of the adhesive uniformly dispersed in the base polymer is restricted, so that sufficient viscosity and thixotropic property cannot be obtained, and the effect of preventing displacement is poor.
[0007]
The present inventors have conducted intensive studies in view of the above points, and as a result, have found that an organic polymer containing at least one reactive silicon group in the molecule is used as a main component, and 4% as a thixotropic agent is used for the organic polymer. The present inventors have found that the above objects can be achieved by adding a specific amount of a thixotropic agent classified as a type and an organotin catalyst as a catalyst for accelerating the curing of an organic polymer, thereby completing the present invention.
[0008]
That is, the one-part room temperature curable adhesive composition according to the present invention comprises 50 to 100 parts by weight of colloidal calcium carbonate, 100 parts by weight of an organic polymer having at least one reactive silicon group in a molecule, and synthetic smectite. 5-15 parts by weight, it comprising from 1 to 10 parts by weight of hydrophobic fine silica powder, organic thixotropic agents 1-5 parts by weight, 0.5 to 3 parts by weight organotin catalyst and a dehydrating agent 1-5 parts by weight Which achieves the above object.
[0009]
The one-part room temperature curable adhesive composition according to the present invention uses an organic polymer having at least one reactive silicon group in a molecule as a main component.
[0010]
The reactive silicon group mentioned here is a silicon atom-containing group containing a silicon atom to which a hydroxyl group or a hydrolyzable group is bonded, and means a group capable of forming a siloxane bond by a silanol condensation reaction.
[0011]
The type of the hydrolyzable group is not particularly limited, and examples thereof include various alkoxy groups. One or more of these are preferably used, and among them, a methoxy group having a mild reactivity is preferred. And ethoxy groups are more preferably used.
[0012]
Specific examples of the organic polymer having at least one reactive silicon group in the molecule include, for example, a polypropylene oxide represented by the following general formula (1) having a main chain skeleton and a methoxy group having a hydrolyzable group. A modified silicon compound contained as a group is exemplified, and is preferably used.
Embedded image
[0013]
The type of the colloidal calcium carbonate used as a thixotropic agent in the one-part room temperature curable adhesive composition according to the present invention is not particularly limited, but includes fatty acid-based surface treatment agents, silicic acid-based surface treatment agents, and sulfones. Colloidal calcium carbonate surface-treated with an acid-based surface treatment agent or the like can be mentioned, and one or more of these are suitably used, and among them, the surface treatment is performed with a fatty acid-based surface treatment agent. Colloidal calcium carbonate having an average particle size of 0.05 to 0.2 μm is more preferably used because of its excellent thixotropic effect.
[0014]
In the present invention, it is necessary that the above-mentioned colloidal calcium carbonate is contained in an amount of 50 to 100 parts by weight based on 100 parts by weight of the organic polymer having at least one reactive silicon group in the molecule.
[0015]
If the content of the colloidal calcium carbonate is less than 50 parts by weight per 100 parts by weight of the organic polymer having at least one reactive silicon group in the molecule, a sufficient thixotropic effect cannot be obtained, and conversely 100 parts by weight If the amount exceeds the above range, the flexibility of the obtained cured adhesive becomes poor, and the impact resistance and durability are reduced.
[0016]
The type of synthetic smectite used as a thixotropic agent in the one-part room temperature-curable adhesive composition according to the present invention is not particularly limited, and includes various swellable layered silicates. Alternatively, two or more kinds are preferably used, and among them, a synthetic smectite subjected to a lipophilic treatment is more preferably used.
[0017]
Specific examples of the synthetic smectite that has been subjected to the lipophilic treatment include “Lucentite” (trade name) commercially available from Corp Chemical Co., Ltd., and are preferably used.
[0018]
In the present invention, it is necessary that the synthetic smectite is contained in an amount of 5 to 15 parts by weight based on 100 parts by weight of the organic polymer having at least one reactive silicon group in the molecule.
[0019]
If the content of the synthetic smectite is less than 5 parts by weight per 100 parts by weight of the organic polymer having at least one reactive silicon group in the molecule, a sufficient thixotropic effect cannot be obtained, and conversely, 15 parts by weight If it exceeds, the flexibility of the obtained cured adhesive becomes poor, and the impact resistance and durability are reduced.
[0020]
The type of the hydrophobic finely divided silica used as a thixotropic agent in the one-part room temperature-curable adhesive composition according to the present invention is not particularly limited, but the silanol group in the hydrophilic silica may be dimethyldichlorosilane or the like. Various types of finely divided hydrophobic silica may be used, and one or more of these may be suitably used, and among them, the finely divided hydrophobic silica having an average primary particle size of 5 to 15 nm is thixotropic. It is more preferably used because of its excellent effect.
[0021]
In the present invention, the hydrophobic finely divided silica needs to be contained in an amount of 1 to 10 parts by weight based on 100 parts by weight of the organic polymer having at least one reactive silicon group in the molecule.
[0022]
If the content of the hydrophobic finely divided silica is less than 1 part by weight based on 100 parts by weight of the organic polymer having at least one reactive silicon group in the molecule, the effect of imparting thixotropic property is hardly obtained, and conversely, 10 parts by weight If the amount exceeds the above range, the viscosity of the obtained adhesive composition becomes too high, and the coating workability deteriorates.
[0023]
The type of organic thixotropic agent used as a thixotropic agent in the one-part room temperature-curable adhesive composition according to the present invention is not particularly limited, but includes a vegetable polymerization oil-based thixotropic agent, a hydrogenated castor oil-based agent. Thixotropic agents, fatty acid amide-based thixotropic agents and the like are mentioned, and one or more of these are preferably used. Among them, fatty acid amide-based thixotropic agents are more preferably used because of their excellent thixotropic effect. Can be
[0024]
In the present invention, it is necessary that the organic thixotropic agent is contained in an amount of 1 to 5 parts by weight based on 100 parts by weight of the organic polymer having at least one reactive silicon group in the molecule.
[0025]
If the content of the organic thixotropic agent is less than 1 part by weight based on 100 parts by weight of the organic polymer having at least one reactive silicon group in the molecule, a sufficient thixotropic effect cannot be obtained. If the amount is more than 10 parts by weight, the obtained cured product of the adhesive becomes poor in flexibility, and the impact resistance and durability are reduced.
[0026]
The type of the organotin catalyst used as a curing acceleration catalyst in the one-part room temperature curable adhesive composition according to the present invention is not particularly limited, but is dibutyltin dilaurate, dibutyltin dimaleate, dibutyltin phthalate, octyl. Carboxylates such as tin acid are exemplified, and one or more of these are suitably used.
[0027]
In the present invention, the organic tin catalyst needs to be contained in an amount of 0.5 to 3 parts by weight based on 100 parts by weight of the organic polymer having at least one reactive silicon group in the molecule.
[0028]
If the content of the organotin catalyst is less than 0.5 part by weight based on 100 parts by weight of the organic polymer having at least one reactive silicon group in the molecule, a sufficient curing promoting effect cannot be obtained. If the amount is more than 10 parts by weight, the effect of diluting the adhesive composition will be undesirably exerted even though the effect of promoting the curing is no longer improved.
[0029]
In the present invention, it is necessary that the dehydrating agent is contained in an amount of 1 to 5 parts by weight based on 100 parts by weight of the organic polymer having at least one reactive silicon group in the molecule.
The organic polymer having at least one reactive silicon group in the molecule used as a main component in the one-part room temperature curable adhesive composition according to the present invention has a curing reaction that proceeds with moisture. This is to prevent the adhesive composition from being thickened or gelled during storage due to the trace amount of water.
The type of the dehydrating agent is not particularly limited, but includes vinylsilanes such as vinyltrimethoxysilane, and one or two or more of these are suitably used.
[0030]
The one-part room temperature curable adhesive composition according to the present invention may further include, in addition to the components described above, an adhesiveness-imparting agent, a viscosity modifier, a coloring agent, and an antioxidant, as long as the object of the present invention is not impaired. Various additives such as an agent, an ultraviolet absorber, a softener, a surfactant, a flame retardant, and an antifoaming agent may be contained.
[0031]
The type of the adhesion-imparting agent is not particularly limited, but aminosilanes such as γ- (2-aminoethyl) aminopropyltrimethoxysilane and γ-aminopropyltriethoxysilane, and γ-mercaptopropyltrimethoxysilane Examples include silane coupling agents such as mercaptosilanes such as methoxysilane and epoxysilanes such as γ-glycidoxypropyltrimethoxysilane, and one or more of these are suitably used.
[0032]
Examples of the type of the viscosity modifier include, but are not particularly limited to, fillers such as calcium carbonate, talc, and clay, and plasticizers such as dibutyl phthalate and dioctyl phthalate. The above is preferably used.
[0033]
The type of the colorant is not particularly limited, and examples thereof include carbon black, titanium oxide, and red iron oxide. One or more of these are suitably used.
[0034]
The type of the antioxidant is not particularly limited, and examples thereof include a hindered amine antioxidant and a hindered phenol antioxidant. One or more of these are preferably used.
[0035]
The method for producing the one-part room-temperature-curable adhesive composition according to the present invention is not particularly limited, and a predetermined amount of each component is weighed and premixed by a mixer such as a mixer or a kneader. The desired one-part room temperature curable adhesive composition can be obtained by uniformly kneading using the present roll or the like.
[0036]
[Action]
The one-part room temperature curable adhesive composition according to the present invention is mainly composed of an organic polymer having at least one reactive silicon group in a molecule, and is used in combination with a thixotropic agent classified into four types, respectively. Since it has an appropriate viscosity and thixotropic properties, it has good workability, and does not easily shift even when a building material such as a tile is adhered to a vertical surface. Further, since the cured film of the adhesive composition is rich in flexibility, it exhibits excellent adhesiveness, impact resistance, durability and the like.
[0037]
【Example】
In order to explain the present invention in more detail, examples are given below. In the examples, “parts” means “parts by weight”.
[0038]
(Example 1)
[0039]
(1) Preparation of One-Part Room-Temperature Curable Adhesive Composition First, 8 parts of synthetic smectite (trade name “Lucentite SPN”, manufactured by Corp Chemical Co., Ltd.) and 8 parts of toluene were weighed in a polyethylene container, and the spatula was removed. The mixture was hand-mixed to crush a synthetic smectite mass. Next, in the polyethylene container, 100 parts of a modified silicon compound (trade name “Silyl SAT200”, manufactured by Kaneka Chemical Co., Ltd.) as an organic polymer having at least one reactive silicon group in a molecule, and colloidal calcium carbonate ( 60 parts of trade name "CCR" (manufactured by Shiraishi Industry Co., Ltd.), 5 parts of hydrophobic finely divided silica (trade name "Aerosil R-202", manufactured by Nippon Aerosil Co., Ltd.), and fatty acid bisamide (trade name "Disparon # 6500") as an organic thixotropic agent 2 parts) and 3 parts of vinyltrimethoxysilane (trade name "KBM1003", manufactured by Shin-Etsu Silicone Co., Ltd.) as a dehydrating agent, and after hand-mixing with a spatula, 3 parts on a three roll. The mixture was passed to obtain a uniform kneaded material. The obtained kneaded material was placed in a glass bottle, heated in a gear oven at 120 ° C. for 3 hours, cooled to room temperature, and a mixture of dibutyltin dilaurate and dibutyltin oxide (trade name “SB-65”) as an organotin catalyst. 2 parts (manufactured by Sankyoki Gosei Co., Ltd.) were added and mixed to obtain a one-part room temperature curable adhesive composition.
[0040]
(2) Evaluation Various properties of the one-part room temperature curable adhesive composition obtained above were evaluated by the following methods. The results were as shown in Table 1.
[0041]
(1) Displacement on a vertical surface: The above adhesive composition was applied to a board held vertically using a 4 mm square comb iron so that the application amount was 1.2 kg / m 2 . Immediately thereafter, an adherend having a weight of 60 g, which had been prepared in advance, was bonded to a center line between two sheet glasses having a width of 50 mm, a length of 50 mm, and a thickness of 4 mm by sandwiching a wire whose tip was processed into a hook shape. The wire is attached to the application surface of the board such that the hook portion of the wire faces downward, and a load of 150 g to 10 g is applied to the hook portion of the wire, and the minimum load (g) when the adherend starts to shift. ) Was measured.
[0042]
{Circle around (2)} Physical properties of cured product: The above adhesive composition was spread into a sheet having a thickness of 2 mm, cured and cured for 7 days in a constant temperature and humidity room at 23 ° C. and 65% RH, and then cured according to JIS K-6301. In accordance with the “vulcanized rubber physical test method”, punching was performed with a No. 3 dumbbell, and the maximum point tensile strength (kg / cm 2 ) and the maximum point elongation (%) were measured.
[0043]
(Examples 2 to 5)
[0044]
Four kinds of one-part room-temperature-curable adhesive compositions were obtained in the same manner as in Example 1 except that the composition shown in Table 1 was used to prepare the one-part room-temperature-curable adhesive composition.
[0045]
(Comparative Examples 1 to 3)
[0046]
In the preparation of the one-part room-temperature-curable adhesive composition, three kinds of one-part room-temperature-curable adhesive compositions were prepared in the same manner as in Example 1 except that the composition shown in Table 1 was used without using synthetic smectite and toluene. An adhesive composition was obtained.
[0047]
(Comparative Example 4)
[0048]
A one-part room-temperature-curable adhesive composition was obtained in the same manner as in Example 1 except that the composition shown in Table 1 was used to prepare the one-part room-temperature-curable adhesive composition.
[0049]
Various performances of the eight one-part room temperature curable adhesive compositions obtained in Examples 2 to 5 and Comparative Examples 1 to 4 were evaluated in the same manner as in Example 1, and the results are shown in Table 1. Was.
[0050]
[Table 1]
【The invention's effect】
As described above, the one-part room temperature-curable adhesive composition according to the present invention has good workability, and hardly causes a gap even when a building material such as a tile is bonded to a vertical surface, The cured product is rich in flexibility and exhibits excellent adhesiveness, impact resistance, durability and the like, and thus is suitably used for applications such as bonding a building material to a vertical surface.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28322994A JP3550198B2 (en) | 1994-11-17 | 1994-11-17 | One-part room temperature curable adhesive composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28322994A JP3550198B2 (en) | 1994-11-17 | 1994-11-17 | One-part room temperature curable adhesive composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08143850A JPH08143850A (en) | 1996-06-04 |
| JP3550198B2 true JP3550198B2 (en) | 2004-08-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28322994A Expired - Lifetime JP3550198B2 (en) | 1994-11-17 | 1994-11-17 | One-part room temperature curable adhesive composition |
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| Country | Link |
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| JP (1) | JP3550198B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962798B (en) * | 2005-11-08 | 2012-07-18 | 住友金属矿山株式会社 | Epoxy resin adhesive composition and optical semiconductor adhesive adopting same |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1210346C (en) * | 2000-06-28 | 2005-07-13 | 株式会社三键 | Cold-setting composition |
| CN104087029B (en) * | 2014-06-19 | 2016-03-30 | 广西华纳新材料科技有限公司 | A kind of preparation method of silicone sealant special active calcium carbonate |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0772250B2 (en) * | 1991-08-15 | 1995-08-02 | 鈴木産業株式会社 | Solvent-free room temperature curable organosiloxane composition, method for producing the same, and use thereof |
| JPH05287256A (en) * | 1992-04-13 | 1993-11-02 | Sekisui Chem Co Ltd | Adhesive composition |
| JPH06287530A (en) * | 1993-03-31 | 1994-10-11 | Sekisui Chem Co Ltd | Adhesive composition |
-
1994
- 1994-11-17 JP JP28322994A patent/JP3550198B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962798B (en) * | 2005-11-08 | 2012-07-18 | 住友金属矿山株式会社 | Epoxy resin adhesive composition and optical semiconductor adhesive adopting same |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH08143850A (en) | 1996-06-04 |
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