JP6917097B2 - 高耐熱性ポリウレタンホットメルト接着剤の調製方法 - Google Patents
高耐熱性ポリウレタンホットメルト接着剤の調製方法 Download PDFInfo
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Description
高耐熱性ポリウレタンホットメルト接着剤の調製方法であって、重量部で計算すると、以下のステップを含む。
(1)平均官能価が2.5より大きいイソシアネートを10〜20部を反応釜に添加し、反応釜内に不活性雰囲気を維持したまま、60〜80℃まで昇温させてから、反応釜にシラン変性剤を0.3〜3.0部添加し、攪拌条件下で1〜3時間保温反応させることで、平均官能価が1.5〜2.0のイソシアネート誘導体を調製し得た後、反応釜に化学脱水剤を0.005〜0.04部添加して均一に混合する。
(2)ステップ(1)が終了後の反応釜に、脱水前処理を経た希釈剤を1〜5部、粘着付与樹脂を7〜20部添加し、反応釜内に不活性雰囲気を維持したまま、100〜120℃まで昇温させ、攪拌により材料を均一に混合してから、その中に脱水前処理を経た結晶性ポリエステルポリオールを25〜45部、ポリエーテルポリオールを6〜20部添加し、攪拌条件下で0.5〜2時間保温反応させる。
(3)ステップ(2)が終了後の反応釜に、脱水前処理を行ったポリエーテルアミンを15〜35部添加し、反応釜内に不活性雰囲気を維持し、攪拌条件下で115〜140℃で1〜2時間反応させる。
(4)ステップ(3)が終了後の反応釜に、触媒を0.01〜0.2部添加し、真空抽出によって気泡を除去し、取り出し、密閉パッケージングして完成する。
(1)利用されるイソシアネートは、高い芳香環含有量を有するため、耐熱性能が良い。利用されるイソシアネートは、官能価が2.5より大きく、シラン変性剤でそのNCO基の官能価を2.0ぐらいまで低下させると、二重官能基構成のNCO基を形成してポリオールの鎖延長反応に寄与する。接着硬化後、側鎖のシロキサンは、水解によりアルコール分を除き、硬化反応を三次元網目構造へ発展させることで高密度の架橋網目構造を形成し、耐熱性能が向上することができる。
(1)15部の多官能性イソシアネートPM−200を反応釜に入れて窒素ガス保護の条件下で80℃まで昇温させ、反応釜にシラン変性剤であるメルカプトプロピルトリメトキシシラン(KH−590)を3.0部添加してから、700回転/分の回転速度で攪拌し、1時間保温反応させることで、平均官能価が1.7のイソシアネート誘導体を調製し得た。反応終了後、反応釜に0.04部のオルトギ酸トリエチルを添加して均一に混合した。
(2)反応釜に脱水前処理を行ったジイソプロピルナフタレン(DI)を1部、2602キシレンホルムアルデヒド樹脂を13部添加し、窒素ガス保護の条件下で120℃まで昇温させ、攪拌により材料を均一に混合してから、その中に脱水前処理を行った結晶性ポリエステルポリオールPTMEG−300を25部、ポリエーテルポリオールPPG−204を20部添加し、400回転/分の回転速度で攪拌して1時間20分間保温反応させた。
(3)ステップ(2)が終了後の反応釜に、脱水前処理を行ったポリエーテルアミンVersalink P−250を35部添加し、反応釜内に窒素ガスを充填して保護し、900回転/分の回転速度で攪拌し、115℃で維持したまま1時間反応させた。
(4)ステップ(3)が終了後の反応釜に、触媒としてのトリエチルアミンを0.2部添加し、真空抽出によって気泡を除去し、取り出して密閉パッケージングして、高耐熱性ポリウレタンホットメルト接着剤を調製し得た。
(1)10部の多官能性イソシアネートDesmodur N3300を反応釜に入れて窒素ガス保護の条件下で70℃まで昇温させ、反応釜にシラン変性剤であるN−フェニル−γ−アミノプロピルトリメトキシシラン(Y−9669)を1.6部添加してから、550回転/分の回転速度で攪拌し、3時間保温反応させることで、平均官能価が1.85のイソシアネート誘導体を調製し得た。反応終了後、反応釜に脱水剤であるp−トルエンスルホニルイソシアネートPTSIを0.03部添加して均一に混合した。
(2)反応釜に脱水前処理を行ったジイソプロピルナフタレン(DI)を5部、フェノール樹脂TXN−203を7部添加し、窒素ガス保護の条件下で110℃まで昇温させ、攪拌により材料を均一に混合してから、その中に脱水前処理を行った結晶性ポリエステルポリオールXCP−3000Hを36部、ポリエーテルポリオールDL−400を14部添加し、600回転/分の回転速度で攪拌して2時間保温反応させた。
(3)ステップ(2)が終了後の反応釜に、脱水前処理を行ったポリエーテルアミンD230を25部添加し、反応釜内に窒素ガスを充填して保護し、700回転/分の回転速度で攪拌し、130℃で維持したまま1.5時間反応させた。
(4)ステップ(3)が終了後の反応釜に、触媒としてのジモルホリノジエチルエーテルDMDEEを0.11部添加し、真空抽出によって気泡を除去し、取り出して密閉パッケージングして、高耐熱性ポリウレタンホットメルト接着剤を調製し得た。
(1)20部の多官能性イソシアネートMR−200を反応釜に入れて窒素ガス保護の条件下で60℃まで昇温させ、反応釜にシラン変性剤であるエチレンジアミノプロピルトリメトキシシランKH−792を0.3部添加し、400回転/分の回転速度で攪拌し、2時間保温反応させることで、平均官能価が2.0のイソシアネート誘導体を調製し得た。反応終了後、反応釜にオキサゾリジン系脱水剤を0.005部添加して均一に混合した。
(2)反応釜に脱水前処理を行ったジイソプロピルナフタレン(DI)を3部、石油樹脂LA700Pを20部添加し、窒素ガス保護の条件下で100℃まで昇温させ、攪拌により材料を均一に混合してから、その中に脱水前処理を行った結晶性ポリエステルポリオールPOL−356Tを45部、ポリエーテルポリオールPPG−207を6部添加し、700回転/分の回転速度で攪拌して0.5時間保温反応させた。
(3)ステップ(2)が終了後の反応釜に、脱水前処理を行ったポリエーテルアミンEC−301を15部添加し、反応釜内に窒素ガスを充填して保護し、1100回転/分の回転速度で攪拌し、140℃で維持したまま2時間反応させた。
(4)ステップ(3)が終了後の反応釜に、触媒としてのジブチルスズジラウレートを0.01部添加し、真空抽出によって気泡を除去し、取り出して密閉パッケージングして、高耐熱性ポリウレタンホットメルト接着剤を調製し得た。
(1)15部の多官能性イソシアネートPM−200を反応釜に入れて窒素ガス保護の条件下で80℃まで昇温させ、反応釜にシラン変性剤であるメルカプトプロピルトリメトキシシラン(KH−590)を3.0部添加し、700回転/分の回転速度で攪拌し、1時間保温反応させることで、平均官能価が1.7のイソシアネート誘導体を調製し得た。反応終了後、反応釜にオルトギ酸トリエチルを0.04部添加して均一に混合した。
(2)反応釜に脱水前処理を行ったジイソプロピルナフタレン(DI)を1部、重合ロジンを13部添加し、窒素ガス保護の条件下で120℃まで昇温させ、攪拌により材料を均一に混合してから、その中に脱水前処理を行った結晶性ポリエステルポリオールPTMEG−300を25部、ポリエーテルポリオールPPG−204を20部添加し、400回転/分の回転速度で攪拌して1時間20分間保温反応させた。
(3)ステップ(2)が終了後の反応釜に、脱水前処理を行ったポリエーテルアミンVersalink P−250を35部添加し、反応釜内に窒素ガスを充填して保護し、900回転/分の回転速度で攪拌し、115℃で維持したまま1時間反応させた。
(4)ステップ(3)が終了後の反応釜に、触媒としてのオクタン酸鉛を0.2部添加し、真空抽出によって気泡を除去し、取り出して密閉パッケージングして、高耐熱性ポリウレタンホットメルト接着剤を調製し得た。
(1)10部の多官能性イソシアネートDesmodur N3300を反応釜に入れて窒素ガス保護の条件下で70℃まで昇温させ、反応釜にシラン変性剤であるN−フェニル−γ−アミノプロピルトリメトキシシラン(Y−9669)を1.6部添加してから、550回転/分の回転速度で攪拌し、3時間保温反応させることで、平均官能価が1.85のイソシアネート誘導体を調製し得た。反応終了後、反応釜に脱水剤であるp−トルエンスルホニルイソシアネートPTSIを0.03部添加して均一に混合した。
(2)反応釜に脱水前処理を行ったジイソプロピルナフタレン(DI)を5部、アクリル樹脂を7部添加し、窒素ガス保護の条件下で110℃まで昇温させ、攪拌により材料を均一に混合してから、その中に脱水前処理を行った結晶性ポリエステルポリオールXCP−3000Hを36部、ポリエーテルポリオールDL−400を14部添加し、600回転/分の回転速度で攪拌して2時間保温反応させた。
(3)ステップ(2)が終了後の反応釜に、脱水前処理を行ったポリエーテルアミンD230を25部添加し、反応釜内に窒素ガスを充填して保護し、700回転/分の回転速度で攪拌し、130℃で維持したまま1.5時間反応させた。
(4)ステップ(3)が終了後の反応釜に、触媒としてのチタン酸テトライソブチルを0.11部添加し、真空抽出によって気泡を除去し、取り出して密閉パッケージングして、高耐熱性ポリウレタンホットメルト接着剤を調製し得た。
従来の湿気硬化型PUR接着剤の調合方法及び生産プロセスは、以下のとおりである。20部のポリエーテルポリオールPPG210、45部のポリエステルポリオールPOL−356Tを反応釜に入れて500回転/分の回転速度で攪拌し、120℃での真空で2時間脱水させ、真空度を−0.09MPaに維持している。その後、80℃になるまで冷却し、攪拌しながら4,4’ジフェニルメタンジイソシアネート MDIを15部添加した後、徐々に昇温させて80℃で維持するように温度を制御すると共に、窒素ガスを充填して保護し、2.5時間反応させる。NCO%含有量をサンプリングして分析し、設計値に達した後、さらにテルペン粘着付与樹脂を15部、触媒としてのジブチルスズジラウレートを0.1部、トリエチレンジアミンを0.4部添加する。温度が110℃の条件下で気泡がないように真空抽出してから,取り出して密閉パッケージングして、使用されるまで置いておく。この接着剤をプロセスで使用されるとき、まずは、加熱システムをオンにして、温度を100〜130℃に設定し、接着剤ガンで接着剤を塗布し、接着剤塗布プロセスがオープンタイム内に完了するのを確保する。その後、規定に従ってテストを行う。高耐熱性能、耐冷熱衝撃性能、耐落下靱性、接着強度及び耐湿熱老化性能に関するテストは、いずれも接着剤塗布してから室温で7日間放置した後で行われる。一般的に、室温で7日間硬化したら最高強度になれるからである。
Claims (10)
- 重量部で計算すると、
平均官能価が2.5より大きいイソシアネートを10〜20部を反応釜に添加し、反応釜内に不活性雰囲気を維持したまま、60〜80℃まで昇温させてから、反応釜にシラン変性剤を0.3〜3.0部添加し、攪拌条件下で1〜3時間保温反応させることで、平均官能価が1.5〜2.0のイソシアネート誘導体を調製し得た後、反応釜に化学脱水剤を0.005〜0.04部添加して均一に混合するステップ(1)と、
ステップ(1)が終了後の反応釜に、脱水前処理を経た希釈剤を1〜5部、粘着付与樹脂を7〜20部添加し、反応釜内に不活性雰囲気を維持したまま、100〜120℃まで昇温させ、攪拌により材料を均一に混合してから、その中に脱水前処理を経た結晶性ポリエステルポリオールを25〜45部、ポリエーテルポリオールを6〜20部添加し、攪拌条件下で0.5〜2時間保温反応させるステップ(2)と、
ステップ(2)が終了後の反応釜に、脱水前処理を行ったポリエーテルアミンを15〜35部添加し、反応釜内に不活性雰囲気を維持し、攪拌条件下で115〜140℃で1〜2時間反応させるステップ(3)と、
ステップ(3)が終了後の反応釜に、触媒を0.01〜0.2部添加し、真空抽出によって気泡を除去し、取り出し、密閉パッケージングして完成するステップ(4)と、を含む、ことを特徴とする高耐熱性ポリウレタンホットメルト接着剤の調製方法。 - 前記イソシアネートは、ポリメチレンポリフェニルポリイソシアネート、トリフェニルメタントリイソシアネート、2,4−トルエンジイソシアネート三量体、ヘキサメチレンジイソシアネート三量体のうちいずれか一種であることを特徴とする請求項1に記載の調製方法。
- 前記シラン変性剤は、メルカプトプロピルトリエトキシシラン、メルカプトプロピルトリメトキシシラン、エチレンジアミノプロピルトリメトキシシラン、N−フェニル−γ−アミノプロピルトリメトキシシランのうちの1つ又は複数の組み合わせであることを特徴とする請求項1に記載の調製方法。
- 前記ポリエーテルアミンは、末端アミノ基含有のコポリエーテルジアミン、ポリテトラメチレンエーテルグリコールPTMEGを主鎖とするアリールアミノ末端基のポリエーテルジアミンのうちいずれか一種であることを特徴とする請求項1に記載の調製方法。
- 前記結晶性ポリエステルポリオールは、ポリテトラヒドロフランジオールまたはアジピン酸と、1,4−ブタンジオール、エチレングリコール、ジエチレングリコール、1,6−ヘキサンジオールのうち少なくとも1種のグリコールとを重合してなる生成物のうちの1種であることを特徴とする請求項1に記載の調製方法。
- 前記ポリエーテルポリオールは、分子量が400〜700g/molの範囲にあるポリオキシプロピレングリコール、ポリオキシプロピレン−エチレンオキシドグリコールのうちの1種であることを特徴とする請求項1に記載の調製方法。
- 前記触媒は、ジブチルスズジラウレート、オクタン酸第一すず、オクタン酸鉛、トリエチルアミン、トリエチレンジアミン、オクタン酸コバルト、ナフテン酸亜鉛、チタン酸テトライソブチル、又はジモルホリノジエチルエーテルのうちの1種であることを特徴とする請求項1に記載の調製方法。
- 前記化学脱水剤は、p−トルエンスルホニルイソシアネート、オルトギ酸トリエチル、オキサゾリジン化合物のうちの1つ又は複数の組み合わせであることを特徴とする請求項1〜7のいずれか一項に記載の調製方法。
- 前記希釈剤は、ジイソプロピルナフタレンであることを特徴とする請求項1〜7のいずれか一項に記載の調製方法。
- 前記粘着付与樹脂は、フェノール樹脂、テルペン樹脂、重合ロジン、アクリル樹脂、石油樹脂のうちの1つ又は複数の組み合わせであることを特徴とする請求項1〜7のいずれか一項に記載の調製方法。
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