TWI834803B - 剝離紙或剝離薄膜用樹脂組成物,及剝離紙或剝離薄膜 - Google Patents
剝離紙或剝離薄膜用樹脂組成物,及剝離紙或剝離薄膜 Download PDFInfo
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- TWI834803B TWI834803B TW109102483A TW109102483A TWI834803B TW I834803 B TWI834803 B TW I834803B TW 109102483 A TW109102483 A TW 109102483A TW 109102483 A TW109102483 A TW 109102483A TW I834803 B TWI834803 B TW I834803B
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Abstract
本發明提供剝離性與重複耐久性良好,於低溫之硬化性優異,且保存安定性亦優異之胺基醇酸樹脂・胺基丙烯酸樹脂系剝離劑組成物。
本發明之剝離紙或剝離薄膜用樹脂組成物包含
(A)選自(A-1)含羥基之丙烯酸樹脂及(A-2)醇酸樹脂之樹脂,
(B)選自全醚型甲基化三聚氰胺樹脂、羥甲基型甲基化三聚氰胺樹脂及該等之多聚物之樹脂,及
(C)於1分子中具有2個以上之可與(A)成分及(B)成分中選出之1種以上樹脂化學鍵結之官能基之有機聚矽氧烷,
(D)碳數1~8之一元醇。
Description
本發明有關剝離紙或剝離薄膜用樹脂組成物,及使其硬化而成之剝離紙或剝離薄膜者。
以往,於紙或塑膠等之薄片狀基材表面塗佈剝離劑,形成硬化皮膜,藉此對接著性或黏著性物質賦與剝離特性。
剝離紙及剝離薄膜之用途有多樣,有對於如標籤或貼紙、膠帶之黏著性物質使用之情況,或使用於陶瓷層或胺基甲酸酯樹脂等之非黏著性物質之成形步驟中使用之情況,根據用途而要求不同性能。
作為非黏著性物質之形成步驟中使用之例,舉例為合成皮革製造用之製程紙。合成皮革之製造步驟中,於基材上使剝離劑硬化形成製程紙,於該製程紙上塗佈胺基甲酸酯樹脂、氯化乙烯樹脂、聚醯胺樹脂、聚胺基酸樹脂等,並使之乾燥。於該經乾燥之樹脂上形成接著層,貼合基布,自製程紙剝離樹脂而製造合成皮革。
合成皮革有霧面(消光)型與琺瑯(強光澤)型,琺瑯型之合成皮革製造時,為了於合成皮革反應剝離劑皮膜之表面狀態,而對硬化皮膜要求高光澤度。且,為了提高合成皮革之生產性,一般製程紙連續複數次使用。因此,期望剝離性(脫模性)於重複使用之際的變化較少。
作為用以使合成皮革用製程紙之表面作成剝離性之樹脂組成物,已知代表者為聚丙烯系、胺基醇酸樹脂・胺基丙烯酸樹脂系、聚矽氧系之3種。聚丙烯系者,重複使用之情況的剝離性持久性雖優異,但於比較高溫下之使用有界限,該情況剝離面容易損傷,且有不利於琺瑯型合成皮革用等之缺點。胺基醇酸樹脂・胺基丙烯酸樹脂系基者雖光澤優異,但缺乏剝離性。聚矽氧系者雖剝離性優異,但由於光澤差,不利於琺瑯型合成皮革用。
作為解決上述問題點者,於專利文獻1(日本特開昭56-14550號公報)中,揭示一種製程剝離紙用樹脂組成物,其係由聚矽氧改質丙烯酸樹脂與聚異氰酸酯化合物所成,該聚矽氧改質丙烯酸樹脂係經1分子中鍵結於矽原子之有機基的15~50mol%為苯基,其餘有機基中至少1個為羥基取代有機基的有機聚矽氧烷改質而成。而且,記載有「藉由使用羥基取代有機基,可獲得耐熱性優異、具有良好光澤且剝離性良好之製程剝離紙」。
又,專利文獻2(日本特開昭56-11980號公報)中,揭示一種製程剝離紙用樹脂組成物,其係由聚矽氧改質醇酸樹脂與聚異氰酸酯化合物所成,該聚矽氧改質醇酸樹脂係經1分子中鍵結於矽原子之有機基的15~50mol%為苯基,其餘有機基中至少1個為羥基取代有機基的有機聚矽氧烷改質而成。而且,記載有「於使用醇酸樹脂之製程剝離紙,耐熱性亦優異,可獲得具有良好光澤且剝離性良好之製程剝離紙」。
專利文獻3(日本特開昭56-14566號公報)中,揭示一種製程剝離紙用樹脂組成物,其係由聚矽氧改質丙烯酸樹脂、烷醇改質胺基樹脂與酸性觸媒所成,該聚矽氧改質丙烯酸樹脂係經1分子中鍵結於矽原子之有機基的15~50mol%為苯基,其餘有機基中至少1個為羥基取代有機基的有機聚矽氧烷改質而成。而且,記載有「藉由酸性觸媒,於同時包含丙烯酸樹脂及胺基樹脂之製程剝離紙之耐熱性亦優異,可獲得具有良好光澤且剝離性良好之製程剝離紙」。
專利文獻4(日本特開平3-263475號公報)中,揭示一種製程剝離紙用樹脂組成物,其係由聚矽氧改質醇酸樹脂、烷醇改質胺基樹脂與酸性觸媒所成,該聚矽氧改質醇酸樹脂係於矽原子鍵結甲基、苯基及有機基,且該有機基之至少1個為羥基取代有機基,且鍵結於矽原子之全部取代基的15~50mol%為苯基的有機聚矽氧烷改質而成。而且,記載有「藉由酸性觸媒,於同時包含醇酸樹脂及胺基樹脂之製程剝離紙之耐熱性亦優異,可獲得具有良好光澤且剝離性良好之製程剝離紙」。
專利文獻5(日本特開平2-28242號公報)中,揭示一種製程剝離紙用樹脂組成物,其係由醇酸樹脂或丙烯酸樹脂、與有機聚矽氧烷、烷醇改質胺基樹脂與酸性觸媒所成,該有機聚矽氧烷係1分子中之矽原子鍵結有機基的15~50mol%為苯基,其餘有機基中之至少1個為羥基取代有機基者。而且,記載有「藉由該製程剝離紙用樹脂組成物所得之製程剝離紙,與迄今之製程剝離紙相比,剝離性、耐熱性優異,光澤亦良好,可抑制品質不均」。
專利文獻6(日本專利第5282083號公報)中,揭示一種剝離劑組成物,其係由含羥基之丙烯酸樹脂、胺基樹脂及聚矽氧樹脂所成,該含羥基之丙烯酸樹脂之羥基價為10~150mgKOH/g、玻璃轉移溫度為20~100℃且重量平均分子量為20,000~100,000,該聚矽氧樹脂具有可與前述含羥基之丙烯酸樹脂及前述胺基樹脂之至少一樹脂化學鍵結之官能基。而且記載有「於高溫之剝離性、光澤、表面狀態及重複耐久性優異」。
如上述,胺基醇酸樹脂・胺基丙烯酸樹脂系剝離劑可改良光澤、耐熱性及剝離性,可獲得一定效果。然而,胺基醇酸樹脂・胺基丙烯酸樹脂系剝離劑具有硬化較慢之缺點,針對硬化性之改良並未進行檢討。近幾年,為了提高製程紙之生產效率,而要求短時間或低溫之硬化性,而成為重要課題。
作為解決上述課題者,專利文獻7(日本特開2000-095929號公報)中,揭示一種製程剝離紙用剝離劑組成物,其係由醇酸樹脂、胺基樹脂、含有具有與前述醇酸樹脂及前述胺基樹脂之反應性的官能基之聚矽氧樹脂所成,前述胺基樹脂含有每一個三嗪核含有1個以上羥甲基之甲基化三聚氰胺作為主成分,且記載有「可用於製造於高溫之剝離性、光澤、表面狀態、重複使用性優異之製程剝離紙,且可於低溫乾燥硬化」。
然而,專利文獻7中記載之方法改良了低溫之硬化性之情況,有剝離劑組成物之保存安定性容易惡化之課題。
[先前技術文獻]
[專利文獻]
[專利文獻1] 日本特開昭56-14550號公報
[專利文獻2] 日本特開昭56-11980號公報
[專利文獻3] 日本特開昭56-14566號公報
[專利文獻4] 日本特開平3-263475號公報
[專利文獻5] 日本特開平2-28242號公報
[專利文獻6] 日本專利第5282083號公報
[專利文獻7] 日本特開2000-095929號公報
[發明欲解決之課題]
剝離劑組成物之保存安定性惡化之情況,由於根據時間變化而於組成物之硬化皮膜性能產生偏差,故基於品質管理面而言欠佳。又,組成物之黏度於保管經時變化之情況下,組成物黏度產生變化,有塗佈變難之情況。因此,對剝離劑組成物要求兼具硬化性與保存安定性。
本發明係鑒於上述情況而完成者,其目的在於提供剝離性與重複耐久性良好,於低溫之硬化性優異,且保存安定性亦優異之剝離紙或剝離薄膜用樹脂組成物。
[用以解決課題之手段]
本發明人等為達成上述目的而進行積極檢討之結果,發現藉由包含(A)選自(A-1)含羥基之丙烯酸樹脂及(A-2)醇酸樹脂之樹脂、(B)選自全醚型甲基化三聚氰胺樹脂、羥甲基型甲基化三聚氰胺樹脂及該等之多聚物之樹脂、及(C)具有可與(A)成分及(B)成分中選出之1種以上樹脂化學鍵結之官能基之有機聚矽氧烷、及(D)碳數1~8之一元醇之樹脂組成物,可提供剝離性與重複耐久性良好,於低溫之硬化性優異,且保存安定性亦優異之剝離紙或剝離薄膜用樹脂組成物。
因此,本發明提供下述發明。
1. 一種剝離紙或剝離薄膜用樹脂組成物,其包含
(A)選自(A-1)含羥基之丙烯酸樹脂及(A-2)醇酸樹脂之樹脂:100質量份,
(B)選自全醚型甲基化三聚氰胺樹脂、羥甲基型甲基化三聚氰胺樹脂及該等之多聚物之樹脂:10~120質量份,
(C)於1分子中具有2個以上之可與(A)成分及(B)成分中選出之1種以上的樹脂化學鍵結之官能基之有機聚矽氧烷:0.5~20質量份,及
(D)碳數1~8之一元醇:相對於(A)~(C)成分之合計100質量份,為5~300質量份。
2. 如1記載之剝離紙或剝離薄膜用樹脂組成物,其中(D)成分係碳數1~4之一元醇。
3. 如1或2記載之剝離紙或剝離薄膜用樹脂組成物,其中(D)成分之調配量,相對於(A)~(C)成分之合計100質量份,為10~200質量份。
4. 如3記載之剝離紙或剝離薄膜用樹脂組成物,其中(D)成分之調配量,相對於(A)~(C)成分之合計100質量份,為20~100質量份。
5. 如1至4中任一項之剝離紙或剝離薄膜用樹脂組成物,其中(B)成分係選自全醚型甲基化三聚氰胺及其多聚物者。
6. 如1至5中任一項之剝離紙或剝離薄膜用樹脂組成物,其中進而包含(E)酸性觸媒。
7. 一種剝離紙或剝離薄膜,其具有將如1至5中任一項之剝離紙或剝離薄膜用樹脂組成物塗佈於基材後,藉加熱而形成之硬化皮膜。
[發明效果]
本發明之剝離紙或剝離薄膜用樹脂組成物係剝離性與重複耐久性良好,於低溫之硬化性優異,且保存安定性良好。
以下,針對本發明更詳細說明。以下,有時將「剝離紙或剝離薄膜用樹脂組成物」簡稱為「組成物」。
[(A)成分]
本發明之(A)成分係選自(A-1)含羥基之丙烯酸樹脂及(A-2)醇酸樹脂之樹脂,可單獨使用1種或適當組合2種以上使用。
作為(A-1)含羥基之丙烯酸樹脂若為1分子中具有1個以上羥基之丙烯酸樹脂,則未特別限定,但較佳為1分子中具有1個以上羥基、1分子中具有1個以上自由基聚合性基之自由基聚合性單體(A-1-a)與1分子中不具有羥基、1分子中具有1個以上自由基聚合性基之自由基聚合性單體(A-1-b)之共聚物。
作為本發明所用之(A-1-a)成分,若為1分子中具有1個以上羥基、1分子中具有1個以上自由基聚合性基之自由基聚合性單體,則未特別限定,可單獨使用1種亦可混合2種以上使用。作為自由基聚合性基舉例為丙烯酸基、甲基丙烯酸基、苯乙烯基、桂皮酸酯基、乙烯基、烯丙基等之自由基聚合性基。具體而言,可例示(甲基)丙烯酸2-羥基乙酯、(甲基)丙烯酸2-羥基丙酯、(甲基)丙烯酸2-羥基丁酯、(甲基)丙烯酸2-羥基-3-苯氧基丙酯、(甲基)丙烯酸1,4-環己烷二甲醇酯、(甲基)丙烯酸2-羥基乙酯、將該等以己內酯改質之PLACCEL F系列(DAICEL股份有限公司製)。
作為本發明所用之(A-1-b)成分,若為1分子中不具有羥基、1分子中具有1個以上自由基聚合性基之自由基聚合性單體,則未特別限定,可單獨使用1種亦可混合2種以上使用。具體而言可例示1分子中具有1個丙烯酸基、甲基丙烯酸基、苯乙烯基、桂皮酸酯基、乙烯基、烯丙基等之自由基聚合性基之化合物,更具體而言,可例示(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸硬脂酯、(甲基)丙烯酸環己酯、(甲基)丙烯酸苄酯、(甲基)丙烯酸異冰片酯、(甲基)丙烯酸三氟丙酯、(甲基)丙烯酸全氟丁基乙酯、(甲基)丙烯酸全氟辛基乙酯等之(甲基)丙烯酸之酯化合物類;(甲基)丙烯酸縮水甘油酯、(甲基)丙烯酸β-甲基縮水甘油酯、(甲基)丙烯酸3,4-環氧基環己基甲酯等之含環氧基之自由基聚合性單體;γ-甲基丙烯醯氧基丙基三甲氧基矽烷、γ-甲基丙烯醯氧基丙基甲基二甲氧基矽烷、γ-甲基丙烯醯氧基丙基二甲基甲氧基矽烷、γ-甲基丙烯醯氧基丙基三乙氧基矽烷、γ-甲基丙烯醯氧基丙基甲基二乙氧基矽烷、γ-甲基丙烯醯氧基丙基三丁氧基矽烷、γ-甲基丙烯醯氧基丙基三異丙氧基矽烷、γ-丙烯醯氧基丙基三甲氧基矽烷、丙烯醯氧基甲基三甲氧基矽烷、γ-丙烯醯氧基丙基三乙氧基矽烷、γ-丙烯醯氧基丙基甲基二乙氧基矽烷、苯乙烯基三甲氧基矽烷、苯乙烯基三乙氧基矽烷、α-甲基苯乙烯基三甲氧基矽烷等之自由基聚合性矽烷化合物;含有聚氧伸烷基之自由基聚合性單體;甘油(甲基)丙烯酸酯。
(A-1-a)成分與(A-1-b)成分之聚合比率係對應於含羥基之丙烯酸樹脂之羥基價而調整。藉由聚合所得之含羥基之丙烯酸樹脂之羥基價較佳為20~200mgKOH/g,更佳為30~190mgKOH/g,又更佳為40~180 mgKOH/g。羥基價若在上述範圍內,則硬化性優異,可容易地合成。又,本形態中,含羥基之丙烯酸樹脂之羥基價係採用依據中和滴定法(JIS K 0070)測定之值。
包含(A-1-a)成分與(A-1-b)成分之單體原料之共聚合亦可適用在過氧化苯甲醯、過氧化異丙苯、過氧化月桂醯、2-乙基過氧己酸第三丁酯等之過氧化物類、2,2’-偶氮雙(2-甲基丁腈)等之偶氮系化合物等之通常自由基聚合起始劑存在下進行之溶液聚合法、乳化聚合法、懸浮聚合法、塊狀聚合法之任一方法。
本發明中,該等聚合法中,為了可容易地將(A-1)含羥基之丙烯酸樹脂之重量平均分子量調整於最適範圍,較佳為溶液聚合法。作為該情況所用之溶劑舉例為苯、甲苯、二甲苯等之芳香族烴類;丙酮、甲基乙基酮、甲基異丁基酮等之酮類;乙酸乙酯、乙酸丁酯、乙酸異丁酯等之酯類;乙醇、異丙醇、正丁醇、異丁醇等之一元醇類等,可單獨使用1種或適當組合2種以上使用。
(A-2)醇酸樹脂係指多元醇及多元酸與脂肪酸或脂肪油之聚縮合及酯交換反應所得之合成樹脂。醇酸樹脂可使用市售者,亦可依據以往習知方法合成。
形成醇酸樹脂之單體中,作為多元醇之具體例,舉例為例如乙二醇、聚乙二醇、二乙二醇、三乙二醇、丙二醇、聚丙二醇、1,3-丁二醇、2,3-丁二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、1,4-環己烷二甲醇、2,2-二甲基-1,3-丙二醇(新戊二醇)、2,2-二烷基-1,3-丙二醇、2,4,4-三甲基-1,3-戊二醇、丁二醇、氫化雙酚A、雙酚A之環氧乙烷加成物、雙酚A之環氧丙烷加成物等之二元醇、甘油、三羥甲基乙烷、三羥甲基丙烷、季戊四醇、三(2-羥基乙基)異氰脲酸酯等之三元以上之多元醇等。該等多元醇可單獨使用1種或可適當組合2種以上使用。其中,較佳以二元醇作為必要多元醇成分,根據需要併用三元以上之多元醇。
形成醇酸樹脂之單體中,作為多元酸之具體例舉例為例如鄰苯二甲酸酐、對苯二甲酸、琥珀酸、己二酸、癸二酸等之飽和多元酸;馬來酸、馬來酸酐、富馬酸、依康酸、檸康酸酐、間苯二甲酸及均苯三甲酸酐等之不飽和多元酸;環戊二烯-馬來酸酐加成物、萜烯-馬來酸酐加成物及松香-馬來酸酐加成物等之迪爾仕-阿爾德反應(Diels–Alder reaction)之多元酸等。又,除上述多元酸以外,亦有併用一元酸的苯甲酸。
作為脂肪酸或脂肪油之具體例,舉例為辛酸、月桂酸、棕櫚酸、硬脂酸、油酸、亞油酸、亞麻油酸、十八碳三烯酸(eleostearic acid)、蓖麻酸、以及脫水蓖麻酸、亞麻仁油、大豆油、葵花油、中國桐油、麻籽油、荏胡麻油、妥爾油、米糠油、蓖麻油、脫水蓖麻油、菜籽油、棉籽油、椰子油、魚油、魚肝油等之動植物油及該等之脂肪酸等。
醇酸樹脂可使用習知者。例如可使用利用醇酸樹脂之油長0~65,較佳25~55的動植物油或動植物油脂肪酸、或各種飽和脂肪酸而製造者。又,該等醇酸樹脂亦可使丙烯酸樹脂、聚酯樹脂、環氧樹脂、酚樹脂等改質或混合而使用。
作為醇酸樹脂之市售品舉例為例如ALUKIDIR 1307-60-EL、ALUKIDIR 1308-E、ALUKIDIR ER-4005-60、ALUKIDIR EZ-3065-P、ALUKIDIR EZ-3509-60、ALUKIDIR EZ-3801-60、ALUKIDIR OD-E-198-50、ALUKIDIR OD-E-230-70、ALUKIDIR OD-E-230-70E、ALUKIDIR J-524-A(以上為DIC股份有限公司製)、ARAKYD IA-120-60L、ARAKYD 1782-60、ARAKYD 3101X-60(以上為荒川化學工業製)、HARIPHTHAL 732-60、HARIPHTHAL 915-60L、HARIPHTHAL COG40-50T、HARIPHTHAL SB-7150X、HARIPHTHAL SB-7540(以上為HARIMA化成集團股份有限公司)等。
(A)成分之重量平均分子量較佳為3,000~ 400,000,更佳為5,000~350,000,又更佳為7,000~ 300,000。重量平均分子量若為上述範圍內,則塗佈性與處理性良好。又,重量平均分子量係藉由以四氫呋喃作為展開溶劑之凝膠滲透層析儀(以下簡稱「GPC」)之聚苯乙烯換算值。
[(B)成分]
(B)成分係選自全醚型甲基化三聚氰胺樹脂、羥甲基型甲基化三聚氰胺樹脂及該等之多聚物之樹脂,可單獨使用1種或可適當組合2種以上使用。本發明中之(B)成分係包含於三嗪環周圍經由3個氮原子鍵結有官能基之構造者。(B)成分作為與(A)成分及/或(C)成分反應之交聯劑發揮作用。
三聚氰胺樹脂係使三聚氰胺與甲醛縮合而得之合成樹脂,係由單體或二聚物以上之多聚物所成之縮合物。於1分子中具有作為官能基之亞胺基、羥甲基或烷氧基甲基,依據官能基而分類為全醚型、羥甲基型、亞胺型、羥甲基/亞胺型。
又,三聚氰胺根據烷氧基甲基種類而區分,烷氧基甲基全部為甲氧基甲基之三聚氰胺樹脂為甲基化三聚氰胺樹脂,烷氧基甲基全部為正丁氧基甲基之三聚氰胺樹脂為正丁基化三聚氰胺樹脂,烷氧基甲基混合存在有甲氧基甲基及正丁氧基甲基之三聚氰胺樹脂為甲基化/正丁基化三聚氰胺樹脂。
本發明之(B)成分由於剝離性與重複耐久性、硬化性優異,故使用全醚型甲基化三聚氰胺樹脂、羥甲基型甲基化三聚氰胺樹脂及該等之多聚物,較佳為全醚型甲基化三聚氰胺樹脂及其多聚物。
本發明之(B)成分可使用市售者,亦可依據以往習知方法合成。作為市售品舉例為例如CYMEL 300、CYMEL 303LF、CYMEL 350、CYMEL 370N(以上為ALLNEX JAPAN股份有限公司製)、NIKALAC MW-30M、NIKALAC MW-30(以上為NIPPON CARBIDE工業股份有限公司製)等。
(B)成分之調配量相對於(A)成分100質量份,為10~120質量份,較佳為12~110質量份,更佳為14~100質量份。若為上述範圍內,則剝離性及硬化性良好,重複耐久性優異。
[(C)成分]
本發明之(C)成分係1分子中具有2個以上之可與(A)成分及(B)成分中選出之1種以上樹脂化學鍵結之官能基之有機聚矽氧烷,可單獨使用1種或適當組合2種以上使用。(C)1分子中必須具有2個以上之可與(A)成分及(B)成分中選出之1種以上樹脂化學鍵結之官能基。藉由如此,藉由構成剝離層之(A)樹脂及(B)樹脂與剝離成分的聚矽氧樹脂於剝離層中成為經化學鍵結之構造,而可抑制聚矽氧樹脂朝黏著劑層之移行,可防止膠帶保存時之重剝離化或使用時之黏著力降低。作為此等官能基舉例為羥基、胺基、羧基、環氧基、異氰酸酯基等,較佳為羥基、環氧基,更佳為羥基。
有機聚矽氧烷於能發揮本發明作用效果之範圍內,可為直鏈狀或分支鏈狀之任一種構造,較佳為以下述平均組成式(1)表示者。
(式中,R1
可為相同亦可不同,且為碳數1~20之非取代或取代之有機基,1分子中具有2個以上之具有羥基、胺基、羧基、環氧基或異氰酸酯基之可於雜原子上取代之碳數1~20之有機基,a為2以上,b為1以上,c為0以上,d為0以上之整數,5≦a+b+c+d≦500)。
作為上述碳數1~20之有機基之較佳者,具體舉例為甲基、乙基、丙基、丁基等之碳數1~6之烷基、環己基等之碳數5~8之環烷基、苯基、甲苯基等之碳數6~10之芳基、苄基等之碳數7~10之芳烷基。或自該等基之鍵結於碳原子之氫原子之一部分或全部經聚醚基、烷氧基烷基、鹵原子等取代之羥基丙基、1-氯丙基、3,3,3-三氟丙基等選出之碳數1~10之烷基。其中,基於剝離性之觀點,更佳為甲基、苯基。
作為上述具有羥基、胺基、羧基、環氧基或異氰酸酯基之可於雜原子上取代之碳數1~20之有機基舉例為羥甲基、羥乙基、羥丙基、羥丁基、羥戊基、羥己基、羥庚基、羥辛基等之羥烷基、以-(CH2
)3
-(OCH2
CH2
)n
-OH表示之聚乙二醇基、以-(CH2
)3
-(OCH2
CH2
CH2
)n
-OH表示之聚丙二醇基、3-胺基丙基、N-2-(胺基乙基)-3-胺基丙基、羧基辛基、3-縮水甘油氧基丙基、2-(3,4-環氧基環己基)乙基、3-異氰酸酯基丙基。其中,基於硬化性之觀點,更佳為羥基烷基、聚乙二醇基、聚丙二醇基。
上述官能基R1
中,較佳5~50mol%為芳基、芳烷基,更佳10~40 mol%為芳基、芳烷基。若為上述範圍內,則剝離性更良好。
上述式(1)中之a、b、c、d係a為2以上,較佳為2~30,b為1以上,較佳1~500之整數,c為0以上,較佳0~10之整數,d為0以上,較佳0~10之整數,5≦a+b+c+d≦500,較佳10≦a+b+c+d≦400。
(C)成分之調配量相對於(A)成分100質量份,為0.5~20質量份,較佳為0.5~10質量份,更佳為1~8質量份。若為上述範圍內,則剝離性優異,可抑制聚矽氧之移行性。
[(D)成分]
本發明之(D)成分係碳數1~8之一元醇,可單獨使用1種或適當組合2種以上使用。藉由調配(D)成分,組成物之保存安定性提高。
作為碳數1~8之一元醇舉例為例如甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-1-丙醇、2-甲基-2-丙醇、1-戊醇、2-戊醇、3-戊醇、2-甲基-2-丁醇、3-甲基-2-丁醇、2-甲基-1-丁醇、3-甲基-1-丁醇、3-甲氧基丁醇、3-甲基-3-甲氧基丁醇、1-己醇、2-己醇、3-己醇、環己醇、2-甲基-1-戊醇、2-甲基-2-戊醇、2-甲基-3-戊醇、3-甲基-1-戊醇、3-甲基-2-戊醇、3-甲基-3-戊醇、4-甲基-1-戊醇、4-甲基-2-戊醇、2-甲基-1-丁醇、2,2-二甲基-3-戊醇、2,3-二甲基-3-戊醇、2,4-二甲基-3-戊醇、4,4-二甲基-2-戊醇、3-乙基-3-戊醇、1-庚醇、2-庚醇、3-庚醇、2-甲基-2-己醇、2-甲基-3-己醇、5-甲基-1-己醇、5-甲基-2-己醇、2-乙基-1-己醇、甲基環己醇、三甲基環己醇、4-甲基-3-庚醇、6-甲基-2-庚醇、1-辛醇、2-辛醇、3-辛醇、2-丙基-1-戊醇、2,4,4-三甲基-1-戊醇、2,6-二甲基-4-戊醇、3-乙基-2,2-二甲基-戊醇,較佳為碳數1~6之一元醇,更佳為碳數1~4之一元醇。碳數若為上述範圍內,則保存安定性優異。
(D)成分之調配量相對於(A)~(C)成分之合計100質量份,為5~300質量份,更佳為10~200質量份,又更佳為20~100質量份。若為上述範圍內,則保存安定性優異。
本發明中,發現藉由添加碳數1~8之一元醇,可兼具硬化性與保存安定性。雖不欲受理論限制,但三聚氰胺與羥基等官能基反應,藉由縮合反應與其他成分反應。認為藉由添加酸性觸媒而促進該反應,但與一分子中具有2個以上反應基之化合物反應時,形成交聯構造。因此組成物黏度上升,剝離強度亦產生變化。認為藉由相對於(A)~(C)成分之合計量,調配特定量之碳數1~8之一元醇,由於抑制了與一分子中具有2個以上反應基之化合物之反應,而提高保存安定性。
[(E)成分]
本發明之組成物中,基於促進(A)成分、(B)成分與(C)成分之交聯反應之觀點,可使用(E)酸性觸媒。作為酸性觸媒舉例為例如自鹽酸、硫酸、磷酸、硼酸等之無機酸類、乙酸、單氯乙酸、二氯乙酸、丁酸等之羧酸、苯磺酸、對-甲苯磺酸、二甲苯磺酸、對-苯酚磺酸、甲烷磺酸、乙烷磺酸等之有機磺酸等選出之有機酸。該等酸性觸媒可單獨使用1種或適當組合2種以上使用。
調配(E)成分時之調配量,為能促進反應之觸媒量即可,例如相對於(A)~(C)成分之合計100質量份,較佳為0.1~10質量份,更佳為0.5~5質量份。若為上述範圍內,則硬化性優異,皮膜之耐久性亦良好。
[(F)成分]
本發明之組成物可調配單獨1種或適當組合2種以上之任意量的溶劑(但(D)成分除外)作為(F)成分。亦可作為根據需要以溶劑稀釋之溶劑型組成物而使用。藉由以溶劑稀釋,獲得塗佈作業性改善、塗佈皮膜之厚度或表面精加工狀態等之塗佈皮膜狀態之改善等之實用上之優點。
作為可使用之溶劑舉例為甲苯、二甲苯等之芳香族烴系化合物;己烷、庚烷、異鏈烷等之脂肪族烴系化合物;丙酮、甲基乙基酮、甲基異丁基酮等之酮化合物;乙酸乙酯、乙酸丁酯等之酯化合物;二異丙醚、1,4-二噁烷等之醚化合物等,但若為可使溶解之化合物則亦可為任意。
調配(F)成分時之調配量,相對於(A)成分100質量份,較佳為100 ~20,000質量份,更佳為200~10,000質量份。
[剝離紙或剝離薄膜用樹脂組成物]
本發明之剝離紙或剝離薄膜用樹脂組成物於25℃之黏度較佳為0.1mPa・s~10Pa・s,更佳為0.2mPa・s~5Pa・s,又更佳為1mPa・s~ 3Pa・s。又,黏度若為1mPa以上則藉由B型黏度計測定,若未達1mPa,則以奧氏黏度計測定。
[製造方法]
本發明之組成物之調製只要將(A)~(D)成分、根據需要之(E)成分、(F)成分及任意成分混合即可,但將(A)、(B)、(C)、(D)、(F)及任意成分預先均一混合後,於即將使用前添加(E)成分之方法,就保存安定性方面而言較佳。混合方法等並未特別限定,可使用習知方法。
[剝離紙或剝離薄膜(塗佈物)]
本發明提供剝離紙或剝離薄膜,其具有將上述剝離紙或剝離薄膜用樹脂組成物塗佈於基材後,藉加熱而形成之硬化皮膜。
上述剝離紙或剝離薄膜用樹脂組成物可直接使用或進而以上述稀釋用溶劑稀釋為上述範圍後,藉由缺角輪塗佈器、唇模塗佈器、輥塗佈器、模嘴塗佈器、刮刀塗佈器、刮板塗佈器、狹縫塗佈器、接觸塗佈器、凹版塗佈器、線棒塗佈器等之塗佈、網版塗佈、浸漬塗佈、澆鑄塗佈等之塗佈方法,於紙、薄膜等之薄片狀基材之單面或兩面上塗佈0.01~100g/m2
後,於50~200℃加熱1~120秒,而可於基材上形成硬化皮膜。塗佈量較佳為0.01~100g/m2
,更佳為0.03~20g/m2
,乾燥時之溫度較佳為50~200℃,更佳為70~180℃。乾燥時之時間較佳為1~120秒,更佳為5~90秒。於基材兩面形成剝離層時,較佳對基材逐面進行硬化皮膜之形成操作。
作為基材之例舉例為聚乙烯層合紙、玻璃紙、上等紙、牛皮紙、灰銅紙、亮面紙等各種塗佈紙、YUPO等合成紙、聚乙烯薄膜、CPP或OPP等之聚丙烯薄膜、聚對苯二甲酸乙二酯薄膜等之聚酯薄膜、聚醯胺薄膜、聚醯亞胺薄膜、聚乳酸薄膜、聚苯酚薄膜、聚碳酸酯薄膜等。為了提高該等基材與剝離層之密著性,亦可使用於基材面進行電暈處理、蝕刻處理或電漿處理者。
[實施例]
以下顯示實施例及比較例,具體說明本發明,但本發明不限定於下述實施例。
<使用原料>
(A成分)
(A-1)
於具備攪拌機、溫度計、回流冷卻器、滴加裝置之玻璃製反應裝置中,饋入甲苯40.0質量份,於90~100℃加熱後,於氮氣通氣下歷時4小時滴加甲基丙烯酸2-羥基乙酯26.0質量份(0.20mol)、甲基丙烯酸甲酯10.0質量份(0.10mol)、甲基丙烯酸硬脂酯67.7質量份(0.20mol)、2-乙基過氧己酸第三丁酯2.5質量份(0.01mol)及甲苯29.1質量份之混合物。進而於90~100℃聚合2小時後,加入2-乙基過氧己酸第三丁酯2.5質量份(0.0012mol)進行2小時聚合,獲得含羥基之丙烯酸樹脂的60質量%甲苯溶液。所得含羥基之丙烯酸樹脂之羥基價為100mgKOH/g。利用GPC之聚苯乙烯換算之重量平均分子量為40,000。
(A-2)
ALUKIDIR J-524-A(DIC製:椰子油改質醇酸樹脂之60質量%二甲苯溶液)
(B成分)
(B-1)
CYMEL 303LF(ALLNEX JAPAN製:全醚型甲基化三聚氰胺樹脂)
(B-2)
CYMEL 370N(ALLNEX JAPAN製:羥甲基型甲基化三聚氰胺樹脂之88質量%異丙醇/異丁醇溶液)
(B-3)比較品
CYMEL 235(ALLNEX JAPAN製:全醚型甲基化正丁基化三聚氰胺樹脂)
(B-4)比較品
MYCOTE 506(ALLNEX JAPAN製:全醚型正丁基化三聚氰胺樹脂)
(B-5)比較品
CYMEL 325(ALLNEX JAPAN製:亞胺型甲基化三聚氰胺樹脂之80質量%異丁醇溶液)
(C成分)
(C-1)
以通式(2)表示之聚有機矽氧烷:各矽氧烷單位之鍵結順序並未限定於下述者,Me為甲基,Ph為苯基。
(C-2)
以通式(3)表示之聚有機矽氧烷:各矽氧烷單位之鍵結順序並未限定於下述者。
(D1)
甲醇
(D2)
1-丁醇
(E1)
對-甲苯磺酸
(F1)
甲苯
[實施例1~8、比較例1~8]
使用上述所示(A)~(F)成分作為原料,藉以下順序調製塗佈用組成物。
(A)、(B)、(C)、(D)、(F)成分依據表1~3的調配比取入燒瓶中,均一混合。於所得溶液中,依據表1~3之調配比,添加(E)成分,攪拌並混合,獲得塗佈用組成物。使用該組成物,藉後述方法製作塗佈品並評價。
[評價]
針對塗佈用組成物,藉由下述方法評價或測定「剝離強度」、「硬化性」、「重複耐久性」、「保存安定性」。結果示於表1。均為「○」者為合格。
[剝離強度]
於厚165μm之亮面紙上,藉由棒塗佈器以塗佈量成為5.0g/m2
之方式塗佈所得塗佈組成物,於120℃之熱風式乾燥機中加熱60秒及120秒形成剝離劑層後,於該硬化皮膜表面以塗膜厚成為30μm之方式塗佈一液型聚胺基甲酸酯溶液[CRISVON 5516S(大日本墨水化學工業(股)製)],於130℃熱處理2分鐘。其次,於該處理面貼合NITTO 31B膠帶並以2kg輥往返壓著1次,於25℃老化20小時後,將試料切斷為5cm寬,使用拉伸試驗機以180°之角度剝離速度0.3m/分鐘,拉動所貼合之膠帶,測定剝離所需之力(gf/ 50mm)。又,加熱60秒之際的剝離力設為RA,加熱120秒之際的剝離力設為RB。
且於加熱60秒所得之剝離劑層上,藉上述條件重複10次之聚胺基甲酸酯之剝離進行評價,第3次之剝離力設為RC。
[硬化性]
比較由上述剝離強度試驗所測定之剝離力,評價硬化性。
由(RA/RB)×100(%)之式,求出因加熱時間差異所致之剝離力變化率。於硬化性良好時,因加熱時間差異所致之剝離力的變化率變低。因此變化率以下述指標進行評價,變化率越少判斷為硬化性越良好。
○:變化率為120以下
△:變化率超過120~150以下
×:變化率超過150
[重複耐久性]
比較由上述剝離強度試驗所測定之剝離力,評價硬化性。
由(RC/RA)×100(%)之式,求出重複使用時之剝離力變化率。變化率越少,表示重複耐久性越優異。因此變化率以下述指標進行評價,變化率越少判斷為耐久操作性越良好。
○:變化率為120以下
△:變化率超過120~150以下
×:變化率超過150
[保存安定性]
・剝離強度
上述剝離強度評價中,除了將熱風式乾燥機中之硬化時間僅設為60秒以外,同樣進行剝離強度試驗。調製塗佈組成物,於25℃保存12小時後,以同樣方法測定剝離強度。將塗佈組成物剛調製後評價之際的剝離力設為RA,塗佈組成物調製後12小時後評價之剝離力設為RD時,由(RD/RA)×100(%)之式,求出調製塗佈組成物後隨保存時間之剝離力變化率。隨保存時間差異之變化率數值較高,表示保存安定性差。因此變化率以下述指標進行評價,變化率越少判斷為保存越良好。
○:變化率為120以下
△:變化率超過120~150以下
×:變化率超過150
・溶液黏度
將塗佈用組成物之黏度設為VA(mPa・s),塗佈組成物調製後24小時後測定之黏度設為VB(mPa・s),由(VB/VA)×100(%)之式,求出塗佈組成物調製後隨保存時間之黏度變化率。隨保存時間差異之變化率數值較高,表示保存安定性差。因此變化率以下述指標進行評價,變化率越少判斷為保存越良好。
○:變化率為120以下
△:變化率超過120~150以下
×:變化率超過150
又,黏度之測定均於25℃使用B型旋轉黏度計測定之值。
表中之數值,關於調配量,針對(A)成分、(B)成分係劑載包含溶劑或溶液之量,( )內記載(A)成分、(B)成分之純成分量。又,「(B)/(A)100質量份」、「(C)/(A)100質量份」、「(D)/(A)~(C)合計100質量份」、「(E)/(A)100質量份」、「(F)/(A)100質量份」係以各成分之純成分換算量加以記載,(B)成分中相當於(D)成分之醇成分、(A)成分中相當於(F)成分之溶劑液包含於計算值。
Claims (8)
- 一種剝離紙或剝離薄膜用樹脂組成物,其包含(A)選自(A-1)含羥基之丙烯酸樹脂及(A-2)醇酸樹脂之樹脂:100質量份,(B)選自全醚型甲基化三聚氰胺樹脂、羥甲基型甲基化三聚氰胺樹脂及該等之多聚物之樹脂:10~120質量份,(C)於1分子中具有2個以上之可與(A)成分及(B)成分中選出之1種以上的樹脂化學鍵結之官能基之有機聚矽氧烷:0.5~20質量份,及(D)碳數1~8之一元醇:相對於(A)~(C)成分之合計100質量份,為5~300質量份;前述(A-1)含羥基之丙烯酸樹脂為1分子中具有1個以上羥基、1分子中具有1個以上自由基聚合性基之自由基聚合性單體(A-1-a)與1分子中不具有羥基、1分子中具有1個以上自由基聚合性基之自由基聚合性單體(A-1-b)之共聚物;前述(C)成分為以下述平均組成式(1)表示者,
- 如請求項1之剝離紙或剝離薄膜用樹脂組成物,其中(D)成分係碳數1~4之一元醇。
- 如請求項1或2之剝離紙或剝離薄膜用樹脂組成物,其中(D)成分之調配量,相對於(A)~(C)成分之合計100質量份,為10~200質量份。
- 如請求項3之剝離紙或剝離薄膜用樹脂組成物,其中(D)成分之調配量,相對於(A)~(C)成分之合計100質量份,為20~100質量份。
- 如請求項1或2之剝離紙或剝離薄膜用樹脂組成物,其中(B)成分係選自全醚型甲基化三聚氰胺及其多聚物者。
- 如請求項1或2之剝離紙或剝離薄膜用樹脂組成物,其中進而包含(E)酸性觸媒。
- 一種剝離紙,其具有將如請求項1至6中任一項之剝離紙或剝離薄膜用樹脂組成物塗佈於基材後,藉加熱而形成之硬化皮膜。
- 一種剝離薄膜,其具有將如請求項1至6中任一項之剝離紙或剝離薄膜用樹脂組成物塗佈於基材後,藉加熱而形成之硬化皮膜。
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KR102457454B1 (ko) * | 2021-09-07 | 2022-10-21 | 도레이첨단소재 주식회사 | 이형 코팅 조성물 |
CN115895268B (zh) * | 2022-07-14 | 2023-11-10 | 江门市澳卓实业有限公司 | 一种抗撕拉硅胶皮革及其制备工艺和应用 |
WO2024034362A1 (ja) * | 2022-08-08 | 2024-02-15 | 信越化学工業株式会社 | 剥離剤組成物、ならびに硬剥離紙及び剥離フィルム |
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JPH03263475A (ja) | 1979-07-09 | 1991-11-22 | Shin Etsu Chem Co Ltd | 工程剥離紙用樹脂組成物 |
JP2000095929A (ja) * | 1998-09-24 | 2000-04-04 | Hitachi Kasei Polymer Co Ltd | 工程剥離紙用剥離剤組成物 |
JP4827282B2 (ja) * | 2000-07-31 | 2011-11-30 | 日立化成ポリマー株式会社 | 剥離剤組成物及び剥離材 |
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