JP7218385B2 - 交互オリゴマーを介して光ファイバーをコーティングするための放射線硬化性組成物とそれから生成されたコーティング - Google Patents
交互オリゴマーを介して光ファイバーをコーティングするための放射線硬化性組成物とそれから生成されたコーティング Download PDFInfo
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- JP7218385B2 JP7218385B2 JP2020566819A JP2020566819A JP7218385B2 JP 7218385 B2 JP7218385 B2 JP 7218385B2 JP 2020566819 A JP2020566819 A JP 2020566819A JP 2020566819 A JP2020566819 A JP 2020566819A JP 7218385 B2 JP7218385 B2 JP 7218385B2
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- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 150000004654 triazenes Chemical class 0.000 description 1
- OACSUWPJZKGHHK-UHFFFAOYSA-N tribenzyl phosphate Chemical compound C=1C=CC=CC=1COP(OCC=1C=CC=CC=1)(=O)OCC1=CC=CC=C1 OACSUWPJZKGHHK-UHFFFAOYSA-N 0.000 description 1
- 229920000428 triblock copolymer Polymers 0.000 description 1
- TUQOTMZNTHZOKS-UHFFFAOYSA-N tributylphosphine Chemical compound CCCCP(CCCC)CCCC TUQOTMZNTHZOKS-UHFFFAOYSA-N 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 125000004953 trihalomethyl group Chemical group 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- XHGIFBQQEGRTPB-UHFFFAOYSA-N tris(prop-2-enyl) phosphate Chemical compound C=CCOP(=O)(OCC=C)OCC=C XHGIFBQQEGRTPB-UHFFFAOYSA-N 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
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- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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Description
この出願は、ここに完全に記載されているかのようにその全体が出典明示によりここに援用される、2018年6月1日出願の米国仮出願第62/679383号の優先権を主張する。
ここで、η(T)はT(℃)での組成物の粘度(Pa・s)である。
ここで、η(T)はT(℃)での組成物の粘度(Pa・s)である、コーティングされた光ファイバーを製造するための方法である。
少なくとも一種の重合性基を含む反応性オリゴマーであって、ポリプロピレングリコールから実質的に誘導されていない反応性オリゴマー;
反応性希釈モノマー;
光開始剤;及び
場合によっては、一又は複数種の添加剤
を含む、光ファイバーをコーティングするための放射線硬化性組成物であって、
放射線硬化性組成物が、液体ガラス転移温度(Tg,rheo)、摂氏25°(℃)での第一粘度(η25)、55℃での第二粘度(η55)、及び85℃での第三粘度(η85)を有し、
放射線硬化性組成物のTg,rheoが、-74℃未満、又は-80℃未満、又は-85℃未満、又は-90℃未満、又は-100℃未満、又は-105℃未満、又は-120から-83.6℃、又は-113から-83℃、又は-106から-83℃であり、ここで、Tg,rheoが式(8)を、放射線硬化性組成物の実験粘度対温度データへ適合させることによって決定され:
ここで、η(T)はT(℃)での組成物の粘度(Pa・s)である、放射線硬化性組成物である。
エチレン性不飽和重合性化合物は、一又は一より多い反応性オレフィン二重結合を含みうる。それらは、低分子量(モノマー)又は高分子量(オリゴマー)化合物でありうる。
一つの二重結合を含む低分子量モノマーの典型的な例は、アルキル又はヒドロキシアルキルアクリレート又はメタクリレート、例えば、メチル、エチル、ブチル、2-フェノキシエチル、2-エチルヘキシル、及び2-ヒドロキシエチルアクリレート、イソボルニルアクリレート、メチル及びエチルメタクリレート、ラウリル-アクリレート、エトキシル化ノニル-フェノールアクリレート、及びジエチレン-グリコール-エチル-ヘキシルアシレート(DEGEHA)である。これらのモノマーの更なる例は、アクリロニトリル、アクリルアミド、メタクリルアミド、N-置換(メタ)アクリルアミド、ビニルエステル、例えば酢酸ビニル、スチレン、アルキルスチレン、ハロスチレン、N-ビニルピロリドン、N-ビニルカプロラクタム、塩化ビニル及び塩化ビニリデンである。一を超える二重結合を含むモノマーの例は、エチレングリコールジアクリレート、プロピレングリコールジアクリレート、トリプロピレングリコールジアクリレート、ネオペンチルグリコールジアクリレート、ヘキサメチレングリコールジアクリレート、ビスフェノールAジアクリレート、4,4’-ビス(2-アクリロイルオキシエトキシ)ジフェニルプロパン、トリメチロールプロパントリアクリレート、ペンタエリスリトールトリアクリレート及びテトラアクリレート、ビニルアクリレート、ジビニルベンゼン、ジビニルスクシネート、ジアリルフタレート、トリアリルホスフェート、トリアリルイソシアヌレート又はトリス(2-アクリロイルエチル)イソシアヌレートである。
一般に、光ファイバーコーティング材料は反応性オリゴマー成分を含む。オリゴマーは、中間の相対分子量の分子であり、その構造は、実際に又は概念的に、より低い相対分子量の分子に由来する複数の単位を含む。ここで使用される場合、「オリゴマー」は、テトラヒドロフラン中のポリスチレン標準で較正されたサイズ排除クロマトグラフィー(SEC)によって測定されて、600g/モルから20000g/モルの数平均分子量(Mn)を有する。
好ましい実施態様では、本発明の光ファイバーをコーティングするための液体放射線硬化性樹脂は、フリーラジカル光開始剤成分を含む。光開始剤は、光の作用又は光の作用と増感色素の電子励起との間の相乗効果によって化学的に変化して、ラジカル、酸、及び塩基のうちの少なくとも一つを生成する化合物である。
上式中、R50は、非置換であるか、1から4のハロゲン又はC1-C8アルキルで置換されている、C1-C12アルキル、シクロヘキシル又はフェニルであり;
R51及びR52は、それぞれ独立して他のC1-C8アルキル又はC1-C8アルコキシであり;
R53は水素又はC1-C8アルキルであり;及び
R54は水素又はメチルである。
上式中、
R1及びR2は、互いに独立して、非置換であるか、又はハロゲン、C1-C8アルキル及び/又はC1-C8アルコキシで1から4回置換されている、C1-C12アルキル、ベンジル、フェニルであり、又はシクロヘキシル又は基-COR3であり、あるいは
R1は-OR4であり;
R3は、非置換であるか、又はC1-C8アルキル、C1-C8アルコキシ、C1-C8アルキルチオ及び/又はハロゲンによって1から4回置換されているフェニルであり;かつ
R4はC1-C8アルキル、フェニル又はベンジルである。例えば、R1は-OR4である。例えば、R2は、非置換であるか、又はハロゲン、C1-C8アルキル及び/又はC1-C8アルコキシによって1から4回置換されているフェニルである。例えば、R3は、非置換であるか、又はC1-C8アルキルによって1から4回置換されているフェニルである。例えば、本発明のモノアシルホスフィンオキシドは、2,4,6-トリメチルベンゾイルエトキシフェニルホスフィンオキシド(CAS#84434-11-7)又は2,4,6-トリメチルベンゾイルジフェニルホスフィンオキシド(CAS#12790-72-6)である。
上式中
R11及びR12は、互いに独立して、水素、C1-C6アルキル、フェニル、C1-C6アルコキシ、OSiR16(R17)2又は-O(CH2CH2O)q-C1-C6アルキルであり、あるいは
R11及びR12は、それらが結合している炭素原子と共に、シクロヘキシル環を形成し;
qは1から20までの数であり;
R13は、OH、C1-C16アルコキシ又は-O(CH2CH2O)q-C1-C6アルキルであり;
R14は、水素、C1-C18アルキル、C1-C12ヒドロキシアルキル、C1-C18アルコキシ、-OCH2CH2-OR15、-CH=CH2、-C(CH3)=CH2であり、又は
であり、
nは2から10までの数字であり;
R15は水素、-COCH=CH2又は-COC(CH3)=CH2であり;
R16及びR17は、互いに独立して、C1-C8アルキル又はフェニルであり;かつ
G3及びG4は、互いに独立して、ポリマー構造の末端基、好ましくは水素又はメチルである。
又は
であるものである。
である化合物である。
α-ヒドロキシシクロヘキシルフェニルケトン、
2-ヒドロキシ-2-メチル-1-フェニルプロパノン、
2-ヒドロキシ-2-メチル-1-(4-イソプロピルフェニル)プロパノン、
2-ヒドロキシ-2-メチル-1-(4-ドデシルフェニル)プロパノン、
2-ヒドロキシ-1-{4-[4-(2-ヒドロキシ-2-メチル-プロピオニル)-ベンジル]-フェニル}-2-メチル-プロパン-1-オン及び
2-ヒドロキシ-2-メチル-1-[(2-ヒドロキシエトキシ)フェニル]プロパノン
である。
である。
のフェニルグリオキサレートであり、上式中、YはC1-C12アルキレン、シクロヘキスリエン、シクロヘキシレン、O、S、又はNR30によって一又は複数回中断されたC2-C40アルキレンであり、R30は水素、C1-C12アルキル又はフェニルであり、好ましくはYはCH2CH2-O-CH2CH2である。
添加剤は、典型的には、改善された保存期間、改善されたコーティングの酸化的及び加水分解的安定性などのような所定の望ましい特性を達成するために光ファイバーコーティングにまた添加される。多くの異なるタイプの望ましい添加剤があり、ここで検討される本発明は、これらによって限定されることは意図されないが、それらは望ましい効果を有するので、想定される実施態様に含められる。
光重合を加速するために、例えば、欧州特許出願公開第438123号及び英国特許出願公開第2180358号に記載されているように、チオール、チオエーテル、ジスルフィド及びホスフィンなどの促進剤、共開始剤及び自動酸化剤を添加することが可能である。
本発明者は、ここに記載のタイプの従来の放射線硬化性一次コーティング組成物、特にオリゴマー成分が、典型的には非ニュートンレオロジー挙動によって特徴付けられることを今発見した。つまり、それらはシアシニングであり、又は高せん断速度でせん断粘度の低下を示す。更に、そのような材料は温度に大きく依存する;つまり、組成物の粘度はその温度に大きく影響される。本発明者は、これらの特性の組み合わせが、高線引速度又は低ヘリウム光ファイバーコーティングプロセスにおいて経験されるもののような、高温、高せん断速度条件に特に敏感な材料をもたらすことを知見した。
ここで、τ(T)は温度Tにおける高分子材料のガラス転移の緩和時間であり、τ(Tref)は基準温度Trefにおける高分子材料のガラス転移の緩和時間、C1とC2は定数である。C1とC2の値は、選択された基準温度に依存する。C1=17.44及びC2=51.6の「普遍的な」値は、基準温度がガラス転移温度(Tg)に等しくなるように選択された場合、広範囲の高分子材料に使用できることが文献に記載されおり、ここで、TgはMcCrum, Read及びWilliams, Anelastic and Dielectric Effects in Polymeric Solids, John Wiley & Sons, New York, 1967に記載されている方法において動的走査熱量測定によって決定される。しかし、本発明者の知見では、未硬化の光ファイバーコーティング樹脂配合物の粘度は
で適切に記述することができる。
本発明に係る未硬化の液体光ファイバーコーティング樹脂配合物は、比率η(25℃)/η(55℃)及び/又はη(25℃)/η(85℃)から測定して、従来の樹脂配合物と比較して、樹脂粘度のより低い温度感度を有する。そのためには、基準温度としてTg,rheoから25℃の基準温度に式(3)を変換するのが有用である。
異なる基準温度へのWLF式の変換は、
と
を等しくすることによってなすことができる。
又は
ここで、η(T)はT(℃)での組成物の粘度(Pa・s)である、コーティングされた光ファイバーを製造するための方法である。
最初に、関連するポリオール(オリゴマー1ではPolycerin DCB-4000、オリゴマー2ではPTGL-4000)を、上の表2において特定された量を確保するように測定した後、乾燥空気ブランケット下で、清浄で乾燥したフラスコに加え、続いて特定量の阻害剤(BHT食品等級)を加えた。次に、特定量のイソシアネート成分Desmodur Wを加えた後、特定量のアクリル酸を加えた。これらの試薬を混合し、約10分間撹拌し、温度を監視して上昇が観察されないことを確認した。次に、特定量の関連する触媒DBTDLを同じフラスコに加え、更に約15分間混合した。次に、得られた混合物を、加熱マントル内で60℃において2時間反応させた。
先ず、表1Cに列挙されている試薬を使用して「ポリエステル樹脂」を作製した。ポリエステル樹脂の合成では、温度計、撹拌機、及び合成中に生成された水を除去するための蒸留装置を備えた2Lの反応容器に、591.3gの二量体脂肪ジオール(1.04モル)及び436.8gの二量体脂肪酸(0.78モル)を満たした。次に、温度を220℃に上昇させながら、撹拌を行い、反応混合物に軽い窒素流を流した。更なる水が放出されなくなるまで、温度を220℃に維持した。次に、0.3gのチタン酸テトライソプロピルを加え、2.0mgKOH/g未満の酸価が達成されるまで減圧下で反応を行った。酸価は、ISO2114に従って滴定測定で測定したが、1グラムの試験物質を中和するのに必要とされる水酸化カリウム(KOH)の質量(ミリグラム)として与えられ、存在するカルボン酸基の濃度の尺度として使用される。得られたポリエステルの特性は、AV=0.1mgKOH/g、OHV=33.9mgKOH/g、Mn=3323Da、Mw=8000Daであった。OHT、又はヒドロキシル値は、ISO4629に従って滴定測定で測定したが、1グラムの試験物質を中和するために必要とされる水酸化カリウム(KOH)のミリグラムでの質量であり、存在するヒドロキシル基の濃度の尺度として使用される。
最後に、比較のためにPPG含有オリゴマーを合成した。このオリゴマーを作製するために、関連するポリオール(Arcol Polyol PPG2000)を、測定して、上の表2において特定された量を確認した後、最初に乾燥空気ブランケット下で、清浄で乾燥したフラスコに加え、続いて特定量の阻害剤(BHT食品等級)を加えた。次に、特定量のイソシアネート成分(Mondur TDS 等級II)を加えた後、特定量のアクリル酸と2-エチルヘキサノールをついで加えた。これらの試薬を混合し、約15分間撹拌した。次に、特定量のDBTDL触媒を同じフラスコに加え、更に約15分間混合した。次に、得られた混合物を、加熱マントル内で60℃において1時間反応させた。
次に、オリゴマー、モノマー及び光開始剤の混合物を、不透明のポリプロピレンカップに10-20gスケールで秤量した。混合は、いわゆるスピードミキサー(ブランドHauschildタイプDAC150FVZ)において、室温で5分間、3000-3500rpmで実施した。混合中の温度は最大10℃上昇した。(固体)光開始剤が視覚的に完全に溶解しなかった場合、混合手順を繰り返した。サンプルは同じカップに保管した。
一般的な説明:樹脂の定常状態せん断粘度の測定の一般的説明は、ISO3219「プラスチック-液状又は乳液もしくは分散状態のポリマー/樹脂-せん断速度が一定の回転粘度計を用いた粘度の測定」に見出すことができる。本発明に係る未硬化光ファイバーコーティング配合物の定常状態せん断粘度の分析では、回転粘度計には、少なくとも20℃と90℃の間の温度における10s-1の変形速度での粘度の決定に対して感度が十分である測定ジオメトリーを備えるべきである。実験手順の過程で、典型的な実験精度の+/-5%を超えて測定結果に影響を及ぼすレベルまで、調査中のサンプルの成分が蒸発しないように注意する必要がある。限定するものではないが、そのような測定を実施するための次の好ましい設定をここで以下に記載する。
1. サンプルとジオメトリーの温度平衡を可能にするために、せん断やデータ収集を行わずに、温度を15分間20℃に設定した。
2. 5℃の温度間隔と10s-1のせん断速度を使用して、20から90℃のステップ温度定常せん断試験シーケンスを実施する。せん断なしに次の温度平衡に10分間加熱した後、せん断速度10s-1を使用して定常せん断測定を開始し、その後、6秒のデータポイント当たりの測定期間を使用して15個のデータポイントを取得した。次に、これらのデータポイントの平均を、特定の測定温度における粘度の値として採用した。このシーケンスは、90℃の測定温度まで繰り返した。最後に、これらの結果からのデータポイントを、25、55、及び85℃での粘度に対して抽出した。
ステップ温度測定シーケンスから得られた粘度データの整合性チェックのために、次の(任意選択的)測定シーケンスをまた追加した。このようなステップは、例えば測定中の蒸発による液体粘度の変化を無視できることをチェックするために特に組み込んだ:
3. ステップ温度シーケンスが完了したところで、サンプルとジオメトリーの温度平衡を可能にするために、せん断やデータ収集を行わずに、温度を10分間85℃に設定した。
4. 次に、せん断速度10s-1を使用した定常せん断測定を開始し、その後、6秒のデータポイント当たりの測定期間を使用して15個のデータポイントを取得した。取得したデータポイントの平均を取り、ついで10%の精度で以前に実施したステップ温度定常せん断測定によって決定された85℃での粘度とそれらが一致することを確認した。
5. 次に、サンプルとジオメトリーの温度平衡を可能にするために、せん断やデータ収集を行わずに、温度を15分間55℃に設定した。
6. この後、せん断速度10s-1を使用して追加の定常せん断測定を開始し、各6秒のデータポイント当たりの測定期間を使用して15個のデータポイントを取得した。次に、取得したデータポイントの平均を確立し、この値が、10%の精度で以前に実施されたステップ温度定常せん断測定で決定された55℃での粘度と一致することを確認した。
7. 加えて、サンプルとジオメトリーの温度平衡を可能にするために、せん断やデータ収集を行わずに、温度を15分間25℃に設定した。
8. 最後に、せん断速度10s-1を使用して追加の定常せん断測定を開始し、その後、各6秒のデータポイント当たりの測定期間を使用して15個のデータポイントを取得した。次に、これらの取得したデータポイントの平均を取って、取得してチェックし、10%の精度で以前に実施されたステップ温度定常せん断測定によって決定された25℃での粘度とそれらが一致することを確認した。
「Tg,rheo」という見出しの下で報告された値は、表3に報告された実際のレオロジーデータ(上で説明した取得方法)にウイリアムズ・ランデル・フェリー式の式(1)から(8)の一又は複数を適用した結果であるカーブフィッティング計算値である。好ましくは、簡略化された式(8)を使用できる:
ここで、η(T)は温度Tでの組成物の粘度であり、η25は第一粘度である。
表3のデータから分かるように、本発明の様々な態様に係る組成物は、粘度比(η25/η55及びη25/η85)によって、あるいは材料の液体Tg(Tg,rheo)によって決定して、望ましい熱感度値を示す。全ての実施例が、光ファイバーの市販の一次コーティング組成物に一般的な光開始剤又は商業的に知られている添加剤を有しているわけではないが、ここにおけるそれらの性能は、光開始剤と添加剤が温度感度に大きな影響を与えるとは予想されないため、塗布されたコーティング上に増加した熱応力量が配される光ファイバーコーティング用途で使用するための少なくとも前駆体組成物としてのそれらの適合性を示している。そのような増加した熱応力は、例えば、商業的な標準値に対して増加したライン速度によって、又はコーティングプロセス中に組成物に適用される冷却(ヘリウム流又は他の方法による)流体の量の低減又は排除によって誘発されうる。
本発明を詳細にかつその特定の実施態様を参照して説明したが、請求項記載の発明の精神及び範囲から逸脱することなく、それらに様々な変化及び変形を行うことができることは当業者には明らかであろう。
Claims (19)
- 少なくとも一種の重合性基を含む反応性オリゴマーであって、アクリレート基、ウレタン基、及び骨格を含み、骨格は、イソシアネート及びヒドロキシアルキルアクリレートと反応したポリオールから誘導され、ポリオールは、少なくとも一つのポリエステル又はポリテトラメチレンエーテルブロックを含み、
前記反応性オリゴマーを作成するために使用される反応物は、オリゴマーを合成するために使用される全ての反応物の重量に対して、1重量%未満のポリプロピレングリコールを含み、
反応性オリゴマーは、ポリスチレン標準に対して較正されたサイズ排除クロマトグラフィー法によって測定されて、6000g/モルから25000g/モルの数平均分子量を有する、
反応性オリゴマー;
反応性希釈モノマー;
光開始剤;及び
場合によっては、一又は複数種の添加剤
を含む、光ファイバーをコーティングするための放射線硬化性組成物であって、
放射線硬化性組成物が、液体ガラス転移温度(Tg,rheo)、摂氏25°(℃)での第一粘度(η25)、55℃での第二粘度(η55)、及び85℃での第三粘度(η85)を有し;
放射線硬化性組成物のTg,rheoが、-74℃未満、又は-80℃未満、又は-85℃未満、又は-90℃未満、又は-100℃未満、又は-105℃未満、又は-120から-83.6℃、又は-113から-83℃、又は-106から-83℃であり、ここで、Tg,rheoが式(8)を、放射線硬化性組成物の実験粘度対温度データへ適合させることによって決定され、
ここで、η(T)はT(℃)での組成物の粘度(Pa・s)である、放射線硬化性組成物。 - 少なくとも一種の重合性基と骨格を含む反応性オリゴマーであって、イソシアネート、ポリオール、及びアクリレートモノマーを含む反応物の生成物であるウレタンアクリレートオリゴマーを含み、骨格は、イソシアネート及びヒドロキシアルキルアクリレートと反応したポリオールから誘導され、ポリオールは、少なくとも一つのポリエステル又はポリテトラメチレンエーテルブロックを含み、
前記反応性オリゴマーを作成するために使用される反応物は、オリゴマーを合成するために使用される全ての反応物の重量に対して、1重量%未満のポリプロピレングリコールを含み、
反応性オリゴマーは、ポリスチレン標準に対して較正されたサイズ排除クロマトグラフィー法によって測定されて、6000g/モルから25000g/モルの数平均分子量を有する、
反応性オリゴマー;
反応性希釈モノマー;
光開始剤;及び
場合によっては、一又は複数種の添加剤
を含む、光ファイバーをコーティングするための放射線硬化性組成物であって、
ポリオールが、17.2モル/kg未満、又は15モル/kg未満、又は12モル/kg未満、又は5モル/kgから15モル/kg、又は6モル/kgから15モル/kg、又は7モル/kgから12モル/kgの第三級炭素含有量を含み;
放射線硬化性組成物が、液体ガラス転移温度(Tg,rheo)、摂氏25°(℃)での第一粘度(η25)、55℃での第二粘度(η55)、及び85℃での第三粘度(η85)を有し;
放射線硬化性組成物のTg,rheoが、-74℃未満、又は-80℃未満、又は-85℃未満、又は-90℃未満、又は-100℃未満、又は-105℃未満、又は-120から-83.6℃、又は-113から-83℃、又は-106から-83℃であり、ここで、Tg,rheoが式(8)を、放射線硬化性組成物の実験粘度対温度データへ適合させることによって決定され:
ここで、η(T)はT(℃)での組成物の粘度(Pa・s)である、放射線硬化性組成物。 - 組成物が二官能性反応性オリゴマーを含み、二官能性がオリゴマー当たり平均1.5から2.5の反応性基を有すると定義される、請求項1又は2に記載の放射線硬化性組成物。
- 反応性希釈モノマーが、2-エチルヘキシルアクリレート、2-フェノキシエチルアクリレート、2-(2-エトキシエトキシ)エチルアクリレート、n-ビニルピロリドン、ジメチルアクリル-アミド、n-ビニルカプロラクタム、エトキシル化2-フェノキシエチルアクリレート、4-ヒドロキシブチルアクリレート、ラウリルアクリレート、イソボルニルアクリレート、カプロラクトンアクリレート、エトキシル化ノニルフェノールアクリレート、又はイソデシルアクリレート、又はそれらの組み合わせを含む、請求項1から3の何れか一項に記載の放射線硬化性組成物。
- 反応性オリゴマーがブロックコポリマーを含み、反応性オリゴマーがモノブロック構造、ジブロック構造、又はトリブロック構造を有し、
ここで、モノブロック構造は、未反応オリゴマー当たり0.9から1.5未満の平均数のポリエーテルブロックとして定義され、
ジブロック構造は、未反応オリゴマー当たり1.5から2.5未満の平均数のポリエーテルブロックとして定義され、
トリブロック構造は、未反応のオリゴマー当たり2.5から3.5未満の平均数のポリエーテルブロックとして定義される、請求項1から4の何れか一項に記載の放射線硬化性組成物。 - オリゴマーがジブロック構造を有する、請求項5に記載の放射線硬化性組成物。
- 反応性オリゴマーが、ポリスチレン標準に対して較正されたサイズ排除クロマトグラフィー法によって測定されて、7000から20000g/モル、又は7000から15000g/モル、又は7000から10000g/モルの数平均分子量を有する、請求項1から6の何れか一項に記載の放射線硬化性組成物。
- 反応性オリゴマーが、放射線硬化性組成物全体の重量に対して、少なくとも55重量%、又は少なくとも60重量%、又は少なくとも65重量%、又は50から80重量%、存在する、請求項1から7の何れか一項に記載の放射線硬化性組成物。
- 放射線硬化性組成物が、第一粘度、第二粘度、及び第三粘度のそれぞれにおいて液体であり、第一粘度と第三粘度の比が18未満、又は13未満、又は12未満、又は11未満、又は5から20、又は7から18、又は7から15、又は7から13、又は7から12である、請求項1から8の何れか一項に記載の放射線硬化性組成物。
- 第一粘度と第二粘度の比が3から5.5、又は3.1から5、又は3.2から5、又は3.2から4.5である、請求項9に記載の放射線硬化性組成物。
- 第三粘度が0.10Pa・sより大きく、又は1Pa・s未満であり、又は0.01Pa・sから2Pa・sの間である、請求項1から10の何れか一項に記載の放射線硬化性組成物。
- 第二反応性希釈モノマーを含む、請求項1から11の何れか一項に記載の放射線硬化性組成物。
- 反応物が、ポリオール基とイソシアネート基のモル比で1:4から1:1、かつイソシアネート基とアクリレート基のモル比で1.5:1から5:1の量で存在する、請求項1から12の何れか一項に記載の放射線硬化性組成物。
- 反応性オリゴマーが、複数のポリオールを含む反応物の反応生成物であるコポリマーであり、使用される複数のポリオール全ての平均第三級炭素含有量が、重量分率で17.2モル/kg未満、又は15モル/kg未満、又は12モル/kg未満、又は5モル/kgから15モル/kg、又は6モル/kgから15モル/kg、又は7モル/kgから12モル/kgである、請求項1から13の何れか一項に記載の放射線硬化性組成物。
- ポリオールが、ポリエステル、ポリテトラメチレンエーテル、又はポリオキシプロピレングリコールブロック、又はそれらの組み合わせからなるか、あるいはそれらから本質的になる、請求項1から14の何れか一項に記載の放射線硬化性組成物。
- イソシアネートが、イソホロンジイソシアネート、2,4-異性体トルエンジイソシアネート、4,4’-メチレンジシクロヘキシルジイソシアネート、1,5-ペンタンジイソシアネート、2,2,4-トリメチル-ヘキサメチレンジイソシアネート、2,4,4-トリメチル-ヘキサメチレンジイソシアネート、又はヘキサメチレンジイソシアネート、又はそれらの組み合わせを含む、請求項1から15の何れか一項に記載の放射線硬化性組成物。
- アクリレートモノマーが、2-ヒドロキシエチルアクリレート、カプロラクトンアクリレート、又はエトキシル化ノニル-フェノールアクリレートを含む、請求項1から16の何れか一項に記載の放射線硬化性組成物。
- 反応性オリゴマーがポリプロピレングリコールを実質的に含まない、請求項1から17の何れか一項に記載の放射線硬化性組成物。
- 組成物が、組成物の全重量に対して、
50重量%から82重量%の反応性オリゴマー;
10重量%から50重量%の反応性希釈モノマー;
1重量%から5重量%の光開始剤;
及び1重量%から5重量%の添加剤
を含む、請求項1から18の何れか一項に記載の放射線硬化性組成物。
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2018
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Patent Citations (4)
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JP2003277453A (ja) | 2002-03-27 | 2003-10-02 | Jsr Corp | 液状硬化性樹脂組成物 |
JP2005524094A (ja) | 2002-04-24 | 2005-08-11 | ディーエスエム アイピー アセッツ ビー.ブイ. | コートされた光ファイバー |
JP2004217823A (ja) | 2003-01-16 | 2004-08-05 | Shin Etsu Chem Co Ltd | 液状放射線硬化型樹脂組成物、光ファイバ用被覆組成物及び光ファイバ |
JP2012056823A (ja) | 2010-09-13 | 2012-03-22 | Jsr Corp | 光ファイバ素線の最外層被覆用液状硬化性樹脂組成物及び光ファイバ素線 |
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US11952453B2 (en) | 2024-04-09 |
JP2021526174A (ja) | 2021-09-30 |
CN112437761A (zh) | 2021-03-02 |
JP7295887B2 (ja) | 2023-06-21 |
EP3802452A1 (en) | 2021-04-14 |
KR20210018338A (ko) | 2021-02-17 |
CN112437761B (zh) | 2023-01-20 |
CN116239949A (zh) | 2023-06-09 |
US20210208333A1 (en) | 2021-07-08 |
CN112203995A (zh) | 2021-01-08 |
EP3802453A1 (en) | 2021-04-14 |
KR20210018337A (ko) | 2021-02-17 |
WO2019231492A1 (en) | 2019-12-05 |
WO2019231491A1 (en) | 2019-12-05 |
US20210208334A1 (en) | 2021-07-08 |
CN112203995B (zh) | 2023-02-21 |
BR112020024440A2 (pt) | 2021-03-23 |
JP2021525817A (ja) | 2021-09-27 |
BR112020024462A2 (pt) | 2021-03-16 |
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