TWI718244B - 熱可塑性樹脂層合延伸薄膜 - Google Patents
熱可塑性樹脂層合延伸薄膜 Download PDFInfo
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- TWI718244B TWI718244B TW106103502A TW106103502A TWI718244B TW I718244 B TWI718244 B TW I718244B TW 106103502 A TW106103502 A TW 106103502A TW 106103502 A TW106103502 A TW 106103502A TW I718244 B TWI718244 B TW I718244B
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Abstract
如藉由本發明,則可提供一種熱可塑性樹脂層合延伸薄膜,其係於包含甲基丙烯酸樹脂(A)之層的至少一面上層合包含熱可塑性樹脂(B)之層而成的熱可塑性樹脂層合延伸薄膜,其特徵為前述甲基丙烯酸樹脂(A)中之全部結構單位的90莫耳%以上為甲基丙烯酸甲酯,前述熱可塑性樹脂(B)之固有雙折射為-0.005~0.005,前述甲基丙烯酸樹脂(A)之玻璃轉移溫度TgA(℃)與前述熱可塑性樹脂(B)之玻璃轉移溫度TgB(℃)滿足式:5℃<(TgB-TgA)<50℃。
Description
本發明係有關適於偏光子保護薄膜等之光學用途的熱可塑性樹脂層合延伸薄膜。
於液晶顯示裝置係為了將透過光變換為直線偏光所以使用偏光板。一般而言,偏光板係以在偏光子之兩面貼合偏光子保護薄膜的3層所構成。
作為偏光子係通常,使用使碘或染料吸附、分散於聚乙烯醇(以下簡寫為「PVA」)的一軸配向薄膜,但如此的PVA系偏光子係因為機械上的特性低,又,因熱或水分而容易收縮、偏光機能容易下降,所以作為於該兩面接著有偏光子保護薄膜的層合體而使用。於此偏光子保護薄膜係被要求不顯現雙折射性、光線透過率高、防濕性‧耐熱性優異、機械上的特性優異、與PVA系偏光子之接著性良好等。又,在使用防濕性優異的偏光子保護薄膜的情況,於偏光子與偏光子保護薄膜之接著係一般而言使用UV硬化型之接著劑,但因為硬化時之UV照射而偏光子之偏光機能會下降,所以近年來係以防止UV硬化時之
偏光子之機能下降為目的,亦要求合於380nm以下之UV截止性的案例增加。
先前,作為偏光子保護薄膜係使用三醋酸纖維素(以下簡寫為「TAC」)薄膜。但是,TAC薄膜係因為防濕性不充分,所以例如在高溫高濕環境下係有產生由偏光子剝離、透明性低下、偏光子之偏光度低下等之問題。又,TAC係因為光彈性係數亦大,所以由外部應力容易產生相位差變化,例如因實際使用於偏光板時之扭曲或所貼合的PVA之尺寸變化,特別是在大型之液晶顯示裝置,有產生色不均、周邊部之對比低下等之問題。
在專利文獻1係開示有以作為主成分使用具有賦與正之相位差的內酯環構造單位與來自賦與負之相位差的芳香族單體之構造單位的丙烯酸系共聚物,可得到光彈性係數小、即使延伸而光學均向性亦高的偏光子保護薄膜。然而,為了得到專利文獻1之偏光子保護薄膜所要求的UV截止性係有添加大量UV吸收劑的必要,所以有因在製膜時UV吸收劑之滲出而產生輥髒污,缺乏連續生產性的情況。又,專利文獻1之丙烯酸系共聚物係因為吸水性高,所以在高溫高濕環境等之高濕度下係有產生尺寸變化或薄膜面之精度惡化的情況。
又,在專利文獻2係開示透過將相對於來自芳香族乙烯基單體之結構單元而言,來自(甲基)丙烯酸酯單體之結構單元之莫耳比為0.25~4的共聚物之芳香族雙鍵之70%以上被氫化而可得的熱可塑性透明樹脂予以延
伸,可得到耐熱性、機械強度、光學均向性優異的延伸薄膜。然而,在專利文獻2之延伸薄膜亦為了得到所要求的UV截止性係有添加大量紫外線吸收劑的必要,所以有因在製膜時紫外線吸收劑之滲出而產生輥髒污,有缺乏連續生產性的情況。
又,在先前之延伸薄膜係在延伸加工時,因為若延伸加工溫度低則配向度變高,所以容易得到充分的機械物性,但雙折射容易增大,在延伸溫度過低的情況係有在延伸加工時於薄膜會產生斷裂的情況。另一方面,若延伸加工溫度高則配向度被低地抑制,所以可抑制雙折射之增大,但難以得到充分的機械物性,在延伸加工溫度過高的情況係有於延伸加工時在薄膜會產生斷裂、外觀會惡化的情況。
[專利文獻1]日本專利第4878302號公報
[專利文獻2]日本特開2008-115314號公報
本發明係由如以上之狀況,其目的為提供一種熱可塑性樹脂層合延伸薄膜,該熱可塑性樹脂層合延伸薄膜係合適地使用於偏光子保護薄膜,兼具密著性、延伸
性、光學均向性、機械強度,連續生產性優異。
本發明者等係為了解決上述之課題而專心致力研討的結果,發現透過延伸滿足特定之特性的熱可塑性樹脂層合體,可得到兼具連續生產性、密著性、延伸性、光學均向性、機械強度的薄膜,進而達成本發明。本發明係提供以下之熱可塑性樹脂層合延伸薄膜者。
尚,在本說明書所謂「(甲基)丙烯酸」係設為意味著丙烯酸或甲基丙烯酸者。
[1]一種熱可塑性樹脂層合延伸薄膜,其係於包含甲基丙烯酸樹脂(A)之層的至少一面上具有包含熱可塑性樹脂(B)之層的熱可塑性樹脂層合延伸薄膜,其特徵為前述甲基丙烯酸樹脂(A)中之全部結構單位的90莫耳%以上為甲基丙烯酸甲酯,前述熱可塑性樹脂(B)之固有雙折射為-0.005~0.005,前述甲基丙烯酸樹脂(A)之玻璃轉移溫度TgA(℃)與前述熱可塑性樹脂(B)之玻璃轉移溫度TgB(℃)滿足式:5℃<(TgB-TgA)<50℃。
[2]如[1]之熱可塑性樹脂層合延伸薄膜,其中面內阻滯Re為0.0~3.0nm,且厚度方向阻滯Rth為-10.0~10.0nm之範圍。
[3]如[1]或[2]之熱可塑性樹脂層合延伸薄膜,其中前述熱可塑性樹脂(B)包含下述一般式(1)所示之(甲基)丙烯酸酯結構單元(a)、與下述一般式(2)所示之脂肪族乙烯
基結構單元(b),相對於前述熱可塑性樹脂(B)中之全部結構單元之合計而言,前述(甲基)丙烯酸酯結構單元(a)與前述脂肪族乙烯基結構單元(b)之合計比例為90~100莫耳%,前述(甲基)丙烯酸酯結構單元(a)與前述脂肪族乙烯基結構單元(b)之莫耳比為55:45~85:15。
[4]如[3]之熱可塑性樹脂層合延伸薄膜,其中前述一般式(1)之R1及R2為甲基。
[5]如[3]或[4]之熱可塑性樹脂層合延伸薄膜,其中前述一般式(2)之R4為環己基。
[6]如[1]~[5]中任一項之熱可塑性樹脂層合延伸薄膜,其中於前述包含甲基丙烯酸樹脂(A)之層的兩面具有
前述包含熱可塑性樹脂(B)之層。
[7]如[1]~[6]中任一項之熱可塑性樹脂層合延伸薄膜,其中前述延伸為二軸延伸。
[8]如[1]~[7]中任一項之熱可塑性樹脂層合延伸薄膜,其中至少1個延伸方向上的延伸倍率為1.1~3.0倍。
[9]如[1]~[8]中任一項之熱可塑性樹脂層合延伸薄膜,全體之厚度為10~1000μm。
[10]如[1]~[9]中任一項之熱可塑性樹脂層合延伸薄膜,其中相對於前述包含甲基丙烯酸樹脂(A)之層和前述包含熱可塑性樹脂(B)之層的合計厚度而言,前述包含熱可塑性樹脂(B)之層的厚度之比例為5~50%之範圍。
[11]如[1]~[10]中任一項之熱可塑性樹脂層合延伸薄膜,其中前述包含熱可塑性樹脂(B)之層包含選自紫外線吸收劑、抗氧化劑、抗著色劑、抗靜電劑、脫模劑、潤滑劑、染料、及顏料所成群組中之一種以上。
[12]一種光學薄膜,其特徵為包含如[1]~[11]中任一項之熱可塑性樹脂層合延伸薄膜。
[13]一種偏光子保護薄膜,其特徵為包含如[12]之光學薄膜。
[14]一種熱可塑性樹脂層合延伸薄膜之製造方法,其係如[1]~[11]中任一項之熱可塑性樹脂層合延伸薄膜之製造方法,其特徵為包含以TgB+25(℃)~TgB+65(℃)之範圍的延伸加工溫度進行延伸的步驟。
透過本發明而可得的熱可塑性樹脂層合延伸薄膜係因為具有密著性、延伸性、光學均向性、機械強度,所以可合適地使用於偏光子保護薄膜等之光學用途。進而本發明之熱可塑性樹脂層合延伸薄膜係即使添加紫外線吸收劑等之低分子添加劑,因為於製膜時因滲出所致的輥髒污亦為少產生或無產生,所以連續生產性優異。
以下,關於本發明加以詳細地說明。本發明之熱可塑性樹脂層合延伸薄膜係於包含甲基丙烯酸樹脂(A)的層之至少一面,層合包含熱可塑性樹脂(B)的層而成的熱可塑性樹脂層合延伸薄膜。該延伸薄膜係前述甲基丙烯酸樹脂(A)中之全部結構單位的90莫耳%以上為甲基丙烯酸甲酯,前述熱可塑性樹脂(B)之固有雙折射為-0.005~0.005,前述甲基丙烯酸樹脂(A)之玻璃轉移溫度TgA(℃)與前述熱可塑性樹脂(B)之玻璃轉移溫度TgB(℃)滿足式:5℃<(TgB-TgA)<50℃的熱可塑性樹脂層合體,可透過延伸該熱可塑性樹脂層合體而製造。尚,所謂在本發明的玻璃轉移溫度係使用示差掃描熱量測定裝置,以試料10mg、昇溫速度10℃/分測定,以在第二加熱之中點法算出時之溫度。
使用於本發明之熱可塑性樹脂層合延伸薄膜的甲基丙烯酸樹脂(A)係其特徵為甲基丙烯酸樹脂(A)中之
全部結構單元之90莫耳%以上為甲基丙烯酸甲酯。理想為甲基丙烯酸樹脂(A)中之全部結構單元之95~100莫耳%為甲基丙烯酸甲酯。透過使用上述之甲基丙烯酸樹脂(A),本發明之熱可塑性樹脂層合延伸薄膜係成為透明性優異者。
於包含使用於本發明之熱可塑性樹脂層合延伸薄膜的甲基丙烯酸樹脂(A)的層係除了甲基丙烯酸樹脂(A)以外,可在不損及透明性或光學均向性的範圍內混合其他樹脂及橡膠粒子。作為其他樹脂之例,例如可舉出聚苯乙烯、甲基丙烯酸甲酯-苯乙烯共聚樹脂、丙烯腈-苯乙烯共聚樹脂、聚甲基丙烯酸甲酯、甲基丙烯酸甲酯-苯乙烯-馬來酸酐共聚樹脂、苯乙烯-馬來酸酐共聚樹脂、環狀聚烯烴樹脂、馬來醯亞胺改質丙烯酸樹脂、聚碳酸酯、聚酯、丙烯酸橡膠粒子等。具體而言係可舉出RESISFY R-100(電氣化學工業公司製)、XIRAN SZ15170(Polyscope公司製)等。
使用於本發明之熱可塑性樹脂層合延伸薄膜的熱可塑性樹脂(B)係固有雙折射為-0.005~0.005,前述甲基丙烯酸樹脂(A)之玻璃轉移溫度TgA(℃)與前述熱可塑性樹脂(B)之玻璃轉移溫度TgB(℃)滿足式:5℃<(TgB-TgA)<50℃的熱可塑性樹脂。在熱可塑性樹脂(B)之固有雙折射為小於-0.005、或大於0.005的情況,因為於延伸加工時在包含熱可塑性樹脂(B)的層會顯現雙折射,所以不理想。又,熱可塑性樹脂(B)之光彈性係數係若為-1.0×10-11
~1.0×10-11m2/N之範圍則較理想。在熱可塑性樹脂(B)之光彈性係數為小於-1.0×10-11m2/N、或大於1.0×10-11m2/N的情況,於延伸加工時在包含熱可塑性樹脂(B)的層變得容易顯現雙折射、因為由外部應力所致的相位差變化變大,所以依用途係有不實用的情況。又,若(TgB-TgA)為5℃以下,則除了無法賦與充分的耐熱性於所得到的延伸薄膜以外,再加上必需降低延伸加工溫度,因為缺乏在包含甲基丙烯酸樹脂(A)的層之抑制雙折射顯現之效果,所以不理想。又,若(TgB-TgA)為50℃以上,則必需過度地提高延伸加工溫度,包含甲基丙烯酸樹脂(A)的層之配向度難以提高,因為難以得到充分的機械物性,所以不實用。透過熱可塑性樹脂(B)之固有雙折射為-0.005~0.005,前述甲基丙烯酸樹脂(A)之玻璃轉移溫度TgA(℃)與前述熱可塑性樹脂(B)之玻璃轉移溫度TgB(℃)滿足式:5℃<(TgB-TgA)<50℃,成為可將延伸加工時之延伸加工溫度延伸在熱可塑性樹脂(B)之玻璃轉移溫度TgB(℃)以上,TgB+25(℃)~TgB+65(℃)之範圍。然後,以降低在包含甲基丙烯酸樹脂(A)的層之配向度及應力,因為可抑制在包含甲基丙烯酸樹脂(A)的層之雙折射顯現,所以得到的延伸薄膜係成為耐熱性、光學均向性、機械強度優異者。作為滿足上述熱可塑性樹脂之例係例如可舉出乙烯基共聚樹脂(B1)、透過甲基丙烯酸或馬來酸酐等之結構單元而使耐熱性提高的耐熱甲基丙烯酸樹脂、含有內酯環構造與苯乙烯結構單元的丙烯酸系共聚物(例如記載於專利文獻1)、
環狀聚烯烴樹脂、甲基丙烯酸甲酯-苯基馬來醯亞胺-環己基馬來醯亞胺共聚物、含有具有戊二醯亞胺結構單元的丙烯酸系共聚物的樹脂組成物等,但由與包含甲基丙烯酸樹脂(A)的層之密著性優異,吸水‧吸濕時之尺寸變化亦小的觀點,乙烯基共聚樹脂(B1)為最理想。以下係關於乙烯基共聚樹脂(B1)而詳述。
作為在本發明的熱可塑性樹脂(B)合適地使用的乙烯基共聚樹脂(B1)係包含來自以下述一般式(1)所示的(甲基)丙烯酸酯單體之結構單元(a)、與來自以下述一般式(2’)所示的芳香族乙烯基單體之結構單元(b’)的熱可塑性樹脂,該熱可塑性樹脂係在相對於該結構單元(a)、結構單元(b’)之合計而言,結構單元(a)之比例為55~85莫耳%的乙烯基共聚樹脂(B1’),將來自芳香族乙烯基單體之結構單元(b’)中之芳香族雙鍵之70%以上進行氫化而可得。亦即,乙烯基共聚樹脂(B1’)係將乙烯基共聚樹脂(B1)之芳香族雙鍵進行氫化前之熱可塑性樹脂。
在乙烯基共聚樹脂(B1),以前述一般式(1)所示的(甲基)丙烯酸酯結構單元(a)、與以前述一般式(2)所示的脂肪族乙烯基結構單元(b)之莫耳比係55:45~85:15之範圍為理想,若為60:40~80:20之範圍為較理想。若相對於(甲基)丙烯酸酯結構單元(a)與脂肪族乙烯基結構單元(b)之合計而言,(甲基)丙烯酸酯結構單元(a)之莫耳比未達55%,則因為與包含甲基丙烯酸樹脂(A)的層之密著性變低所以不實用。又,若該莫耳比為超過85%,則除了在所得到的延伸薄膜之吸水、吸濕時之尺寸變化變大,再加上有產生薄膜面之精度惡化的情況,並不理想。
前述(甲基)丙烯酸酯結構單元(a)與前述脂肪族乙烯基結構單元(b)之合計比例係相對於前述熱可塑性樹脂(B)中之全部結構單元之合計而言,90~100莫耳%為理想,95~100莫耳%為較理想。
在構成乙烯基共聚樹脂(B1’)的來自以前述一般式(1)所示的(甲基)丙烯酸酯單體之結構單元(a),R1為氫原子或甲基,R2為碳數1~16之烴基。在結構單元(a)為複數存在的情況,複數存在的R1、R2係可各自相同或相
異。作為前述(甲基)丙烯酸酯單體係R2為由甲基、乙基、丁基、月桂基、硬脂醯基、環己基及異冰片基所選擇的至少1種的(甲基)丙烯酸酯單體為理想,具體而言係可舉出(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸硬脂醯酯、(甲基)丙烯酸環己酯、(甲基)丙烯酸異冰片酯等之(甲基)丙烯酸烷基酯類。結構單元(a)係較理想為來自由甲基丙烯酸甲酯及丙烯酸甲酯所選擇至少1種的結構單元。以將乙烯基共聚樹脂(B1’)之結構單元(a)設為來自由甲基丙烯酸甲酯及丙烯酸甲酯所選擇至少1種的結構單元,使用於本發明之熱可塑性樹脂層合延伸薄膜的乙烯基共聚樹脂(B1)係成為透明性優異者。
在來自以前述一般式(2’)所示的芳香族乙烯基單體之結構單元(b’),R3為氫原子或甲基,R4’為苯基或具有碳數1~4之烴取代基的苯基。在結構單元(b’)為複數存在的情況,複數存在的R3、R4’係可各自相同或相異。作為前述芳香族乙烯基單體係可舉出由苯乙烯、α-甲基苯乙烯、o-甲基苯乙烯及p-甲基苯乙烯中選擇至少1種。較理想為,R3為氫原子、R4’為苯基的來自苯乙烯之結構單元。以將結構單元(b’)設為來自苯乙烯的結構單元,使用於本發明之熱可塑性樹脂層合延伸薄膜的乙烯基共聚樹脂(B)係成為在吸水、吸濕時之尺寸安定性優異者。
作為在本發明的熱可塑性樹脂(B)合適地使用的乙烯基共聚樹脂(B1)係透過後述的方法,將乙烯基共聚
樹脂(B1’)的來自芳香族乙烯基單體之結構單元(b’)中之全芳香族雙鍵之70%以上進行氫化而可得。乙烯基共聚樹脂(B1)係可包含在結構單元(b’)的R4’(苯基或具有碳數1~4之烴取代基的苯基)之苯基之芳香族雙鍵之一部分被氫化的結構單元,亦可包含R4’為苯基的結構單元(亦即,苯基之芳香族雙鍵未氫化的結構單元)。作為R4’之苯基之芳香族雙鍵之一部分為已氫化的結構單元係具體而言,可舉出來自環己烷、環己烯、環己二烯、α-甲基環己烷、α-甲基環己烯、α-甲基環己二烯、o-甲基環己烷、o-甲基環己烯、o-甲基環己二烯、p-甲基環己烷、p-甲基環己烯、p-甲基環己二烯的結構單元,亦可包含來自此等所選擇的至少1種之結構單元。其中,尤其包含來自由環己烷及α-甲基環己烷中選擇至少1種的結構單元為理想。
作為在本發明的熱可塑性樹脂(B)合適地使用的乙烯基共聚樹脂(B1)之氫化前之乙烯基共聚樹脂(B1’)係可透過聚合前述(甲基)丙烯酸酯單體、與芳香族乙烯基單體而製造。於聚合係可使用一般周知之方法,但例如可透過塊狀聚合法、溶液聚合法而製造。塊狀聚合法係將包含上述單體及聚合起始劑的單體組成物連續地供給於完全混合槽,在100~180℃透過連續聚合的方法等進行。上述單體組成物係按照必要亦可包含鏈轉移劑。
聚合起始劑係無特別限定,但可舉出t-戊基過氧基-2-乙基己酸酯、t-丁基過氧基-2-乙基己酸酯、過氧化苯甲醯、1,1-二(t-己基過氧基)-3,3,5-三甲基環己
烷、1,1-二(t-己基過氧基)環己烷、1,1-二(t-丁基過氧基)環己烷、t-己基過氧基異丙基單碳酸酯、t-戊基過氧基正辛酸酯、t-丁基過氧異丙基單碳酸酯、二-t-丁基過氧化物等之有機過氧化物、2,2’-偶氮雙異丁腈、2,2’-偶氮雙(2-甲基丁腈)、2,2’-偶氮雙(2,4-二甲基戊腈)等之偶氮化合物。此等係可單獨或組合2種以上來使用。
鏈轉移劑係按照必要而使用,例如可舉出α-甲基苯乙烯二聚物。
作為使用於溶液聚合法的溶媒,例如可舉出甲苯、二甲苯、環己烷、甲基環己烷等之烴系溶媒、乙酸乙酯、異丁酸甲酯等之酯系溶媒、丙酮、甲基乙基酮等之酮系溶媒、四氫呋喃、二噁烷等之醚系溶媒、甲醇、異丙醇等之醇系溶媒。
作為在本發明的熱可塑性樹脂(B)合適地使用的乙烯基共聚樹脂(B1)係聚合(甲基)丙烯酸酯單體和芳香族乙烯基單體而得到乙烯基共聚樹脂(B1’)後,在該乙烯基共聚樹脂(B1’)的來自芳香族乙烯基單體之結構單元中之芳香族雙鍵之70%以上進行氫化而可得。使用於上述氫化反應的溶媒係可與前述之聚合溶媒相同,亦可為相異。例如,可舉出環己烷、甲基環己烷等之烴系溶媒、乙酸乙酯、異丁酸甲酯等之酯系溶媒、丙酮、甲基乙基酮等之酮系溶媒、四氫呋喃、二噁烷等之醚系溶媒、甲醇、異丙醇等之醇系溶媒。
氫化之方法係無特別限定,可使用一般周知
之方法。例如,可在氫氣壓力3~30MPa、反應溫度60~250℃,以批次式或連續流一般式進行。透過將溫度設為60℃以上而不過度花費反應時間,又透過設為250℃以下而會少產生分子鏈之切斷或酯部位之氫化之情事。
作為使用於氫化反應的觸媒係例如可舉出將鎳、鈀、鉑、鈷、釕、銠等之金屬或該等金屬之氧化物或鹽或錯合物化合物,擔載於碳、氧化鋁、二氧化矽、二氧化矽‧氧化鋁、矽藻土等之多孔性載體的固體觸媒等。
作為在本發明的熱可塑性樹脂(B)合適地使用的乙烯基共聚樹脂(B1)係在前述乙烯基共聚樹脂(B1’),將來自芳香族乙烯基單體之結構單元中之芳香族雙鍵之70%以上進行氫化而可得者。亦即,殘存於來自芳香族乙烯基單體之結構單元中的芳香族雙鍵之比例為30%以下。若超過30%的範圍,則乙烯基共聚樹脂(B1)之透明性低下,該結果,有本發明之熱可塑性樹脂層合延伸薄膜之透明性低下的情況。上述殘存於來自芳香族乙烯基單體之結構單元中的芳香族雙鍵之比例係理想為未達10%之範圍,較理想為未達5%之範圍。又,乙烯基共聚樹脂(B1)係亦可包含防氧化劑、防著色劑、紫外線吸收劑、光擴散劑、難燃劑、脫模劑、潤滑劑、防帶電劑、染顏料等之一般所使用的添加劑。
乙烯基共聚樹脂(B1)之重量平均分子量係無特別限制,但由強度及成形性之觀點視之,40,000~500,000為理想、50,000~300,000為較理想。上述
重量平均分子量係藉由凝膠滲透層析法(GPC)法而測定的標準聚苯乙烯換算之重量平均分子量。
乙烯基共聚樹脂(B1)之玻璃轉移溫度係110~160℃之範圍為理想。較理想係120~145℃。若乙烯基共聚樹脂(B1)之玻璃轉移溫度為未達110℃,則在本發明所提供的熱可塑性樹脂層合延伸薄膜為有在高溫環境或高濕環境下產生尺寸變化或彎曲的情況。又,若乙烯基共聚樹脂(B1)之玻璃轉移溫度為超過160℃,則因為在延伸加工時必需將延伸加工溫度作為180℃以上,所以包含甲基丙烯酸樹脂(A)的層之配向度難以提高,有無法得到充分的機械物性的情況。
於包含作為在本發明的熱可塑性樹脂(B)合適地使用的乙烯基共聚樹脂(B1)的層係除了乙烯基共聚樹脂(B1)以外,可在不損及透明性的範圍內混合其他樹脂。作為其他樹脂之例,例如可舉出聚苯乙烯、甲基丙烯酸甲酯-苯乙烯共聚樹脂、丙烯腈-苯乙烯共聚樹脂、聚甲基丙烯酸甲酯、聚碳酸酯、聚酯等。具體而言係可舉出商品名:ESTYREN MS200(新日鐵住金化學公司製)、RESISFY R-100(電氣化學工業公司製)、XIRAN SZ15170(Polyscope公司製)、Toyo Styrene T080(東洋苯乙烯公司製)等。又,乙烯基共聚樹脂(B1)係亦可包含防氧化劑、防著色劑、紫外線吸收劑、光擴散劑、難燃劑、脫模劑、潤滑劑、防帶電劑、染顏料等之一般所使用的各種添加劑。
本發明之熱可塑性樹脂層合延伸薄膜係於包
含甲基丙烯酸樹脂(A)之層的至少一面上層合包含熱可塑性樹脂(B)之層而成的多層延伸薄膜,其特徵為前述甲基丙烯酸樹脂(A)中之全部結構單位的90莫耳%以上為甲基丙烯酸甲酯,前述熱可塑性樹脂(B)之固有雙折射為-0.005~0.005,前述甲基丙烯酸樹脂(A)之玻璃轉移溫度TgA(℃)與前述熱可塑性樹脂(B)之玻璃轉移溫度TgB(℃)滿足式:5℃<(TgB-TgA)<50℃。以滿足上述式,將延伸加工溫度設為熱可塑性樹脂(B)之玻璃轉移溫度TgB(℃)以上,因為在TgB+25(℃)~TgB+65(℃)之範圍成為可延伸,所以可抑制因延伸加工所致的在包含甲基丙烯酸樹脂(A)的層之雙折射顯現,本發明之熱可塑性樹脂層合延伸薄膜係成為光學均向性優異者。較理想為10℃<(TgB-TgA)<40℃,更理想為12℃<(TgB-TgA)<36℃。若(TgB-TgA)低於5℃則難以得到本發明之效果,若高於50℃,則因為延伸加工溫度之容許寬度變窄,所以在實用上不理想。
以下,有將包含甲基丙烯酸樹脂(A)的層稱為「甲基丙烯酸樹脂(A)層」,將包含熱可塑性樹脂(B)的層,稱為「熱可塑性樹脂(B)層」之情事。作為層構成之例,例如可例示如甲基丙烯酸樹脂(A)層/熱可塑性樹脂(B)層之2種2層、熱可塑性樹脂(B)層/甲基丙烯酸樹脂(A)層/熱可塑性樹脂(B)層之2種3層之方式的層構成,但由所得的熱可塑性樹脂層合延伸薄膜之耐熱性、機械強度、吸水‧吸濕時之尺寸變化或薄膜面精度之惡化之觀點視之,熱可塑性樹脂(B)層/甲基丙烯酸樹脂(A)層/熱可塑性樹
脂(B)層之2種3層之構成為理想。以於如上述般的甲基丙烯酸樹脂(A)層之至少一面,設為層合熱可塑性樹脂(B)層之情事,本發明之熱可塑性樹脂層合延伸薄膜係成為在耐熱性、光學均向性、機械強度優異者。
本發明之熱可塑性樹脂層合延伸薄膜之甲基丙烯酸樹脂(A)層以及/或是熱可塑性樹脂(B)層係亦可含有紫外線吸收劑。在有添加大量之紫外線吸收劑的必要的情況係設為熱可塑性樹脂(B)層/甲基丙烯酸樹脂(A)層/熱可塑性樹脂(B)層之2種3層之層構成,僅於甲基丙烯酸樹脂(A)層添加紫外線吸收劑為理想。以如上述之方式設為熱可塑性樹脂(B)層/甲基丙烯酸樹脂(A)層/熱可塑性樹脂(B)層之2種3層之層構成,僅於甲基丙烯酸樹脂(A)層添加紫外線吸收劑之情事,於製膜時因紫外線吸收劑之滲出所致的輥髒污不產生,成為連續生產性優異者。作為添加的紫外線吸收劑係例如可舉出2,4-二羥基二苯甲酮、2-羥基-4-甲氧基二苯甲酮、2-羥基-4-n-辛氧基二苯酮、2-羥基-4-十二烷氧基二苯甲酮、2-羥基-4-十八烷氧基二苯甲酮、2,2’-二羥基-4-甲氧基二苯甲酮、2,2’-二羥基-4,4’-二甲氧基二苯甲酮、2,2’,4,4’-四羥基二苯甲酮等之二苯甲酮系紫外線吸收劑、2-(2-羥基-5-甲基苯基)苯并三唑、2-(2-羥基-3,5-二-t-丁基-苯基)苯并三唑、2-(2-羥基-3-t-丁基-5-甲基苯基)苯并三唑、(2H-苯并三唑-2-基)-4,6-雙(1-甲基-1-苯基乙基)苯酚等之苯并三唑系紫外線吸收劑、水楊酸苯酯、2,4-二-t-丁基苯基-3,5-
二-t-丁基-4-羥基苯甲酸酯等之苯甲酸酯系紫外線吸收劑、雙(2,2,6,6-四甲基哌啶-4-基)癸二酸酯等之受阻胺系紫外線吸收劑、2,4-二苯基-6-(2-羥基-4-甲氧基苯基)-1,3,5-三嗪、2,4-二苯基-6-(2-羥基-4-乙氧基苯基)-1,3,5-三嗪、2,4-二苯基-(2-羥基-4-丙氧基苯基)-1,3,5-三嗪、2,4-二苯基-(2-羥基-4-丁氧基苯基)-1,3,5-三嗪、2,4-二苯基-6-(2-羥基-4-丁氧基苯基)-1,3,5-三嗪、2,4-二苯基-6-(2-羥基-4-己氧基苯基)-1,3,5-三嗪、2,4-二苯基-6-(2-羥基-4-辛氧基苯基)-1,3,5-三嗪、2,4-二苯基-6-(2-羥基-4-十二烷氧基苯基)-1,3,5-三嗪、2,4-二苯基-6-(2-羥基-4-芐氧基苯基)-1,3,5-三嗪等之三嗪系紫外線吸收劑等。混合之方法係無特別限定,可使用全量合成方法、將母料進行乾混合的方法等。
又,本發明之熱可塑性樹脂層合延伸薄膜之甲基丙烯酸樹脂(A)層以及/或是熱可塑性樹脂(B)層係亦可混合紫外線吸收劑以外之各種添加劑而使用。作為紫外線吸收劑以外之添加劑之例係例如可舉出抗氧化劑或抗著色劑、抗靜電劑、脫模劑、潤滑劑、染料、顏料等。混合之方法係無特別限定,可使用全量合成方法、將母料進行乾混合的方法、全量乾混合的方法等。
作為本發明之熱可塑性樹脂層合延伸薄膜之製造方法係可將透過一般周知之多色射出成形法、薄膜插入法、熔融擠出法、擠出層合法、熱壓法、溶液澆鑄法等而成形的熱可塑性樹脂層合體,設為延伸薄膜用之原材薄
膜(以下,僅稱為「原材」)。由生產性之觀點,特別是熔融擠出法可合適地使用。在使用熔融擠出法的情況係有作為中間體之面狀成形體,不取出原材而連續地供給於延伸步驟之情事。在此情況,在本發明係將薄膜實際上被延伸之前之狀態定義為原材。
關於熔融擠出法所致的原材之製作更進一步進行詳述。本發明所使用的熱可塑性透明樹脂之原材係可使用一般周知之熔融擠出法的T型模頭擠出法、膨脹法等,但由得到厚度不均少的原材的觀點,選擇T型模頭擠出法為最佳。作為使樹脂熔融的裝置係如使用一般上所使用的擠出機即可,可為單軸擠出機亦可為多軸擠出機。擠出機係亦可具有一個以上之排氣口,亦可在排氣口進行減壓而由樹脂除去水分或低分子物質等。又,於擠出機之前端或下流側係按照必要而亦可設置金屬網過濾器或燒結過濾器、齒輪泵等。作為使樹脂層合的方法係可使用供料頭法或多歧管法等一般周知之方法。於T型模頭係有衣架模頭、魚尾模頭、堆疊板模頭等之種類,亦可選擇任一者。
擠出時之樹脂溫度係200~300℃為理想。在未達200℃係樹脂之流動性不足,因為轉印輥表面之形狀無法轉印,所以會成為缺乏平滑性者。另一方面,若超過300℃,則因為成為樹脂分解、外觀不良、著色、耐熱變形性低下、因臭氣所致的作業環境之惡化等之原因所以不理想。較理想係擠出時之樹脂溫度為220~280℃。在擠出溫度於上述範圍的情況,所得到的原材之光學均向性、平
滑性或透明性係成為優異者。
由T型模頭擠出的熔融樹脂之冷卻方法係可使用先前一般周知之方法,但一般上係以冷卻輥進行冷卻。本發明所使用的甲基丙烯酸樹脂(A)及熱可塑性樹脂(B)係因為實質上為非晶性之樹脂,所以冷卻輥之溫度係可廣泛地設定。於得到光學均向性的光學薄膜係冷卻輥之溫度係設為熱可塑性樹脂(B)之玻璃轉移溫度之上下30℃為理想,更理想係設為熱可塑性樹脂(B)之玻璃轉移溫度之上下20℃。於得到光學均向性高的原材係以無實質上延伸之方式,依照裝置而控制吐出速度和放捲速度和冷卻輥之溫度為理想。
本發明之熱可塑性樹脂層合延伸薄膜係以延伸加工原材而得。透過延伸加工,機械上的強度提高,雖以產生破裂或斷裂,可得到操作性優異的熱可塑性樹脂層合延伸薄膜。延伸方法係無特別限定,可使用一般周知之方法。例如,可舉出自由端單軸延伸法或固定端單軸延伸法等之單軸延伸、同時二軸延伸法或逐次二軸延伸法等之二軸延伸。以可抑制機械強度之不均之觀點,二軸延伸為理想。
在進行二軸延伸的情況,向延伸方向之延伸倍率係1.1~3.0倍之範圍者為理想,1.2~2.0倍者為較理想。若為1.2~2.0倍之範圍內,則機械強度之提高效果高。若為1.1~3.0倍之範圍外,則有不能充分地得到機械強度提高之效果的情況。又,二軸方向各自之延伸倍率係
等倍亦可,倍率為相異亦可。延伸加工溫度係通常為熱可塑性樹脂(B)之玻璃轉移溫度TgB(℃)以上,TgB+25(℃)~TgB+65(℃)之範圍為理想,TgB+30(℃)~TgB+60(℃)為較理想。若延伸加工溫度低於TgB+25(℃),則除了有於薄膜產生斷裂的情況以外,再加上因為無法抑制在包含甲基丙烯酸樹脂(A)的層之雙折射顯現,所以不理想。又,若高於TgB+65(℃),則除了有因樹脂之流動而外觀惡化的情況以外,再加上因為包含甲基丙烯酸樹脂(A)的層之配向度難以提高而不能得到充分的機械物性,所以不實用。向延伸方向之延伸速度係0.1~3.0m/min之範圍為理想。若慢於0.1m/min,則除了延伸強度難以變高以外,再加上為了得到充分的延伸倍率而花費時間,在生產性之點上亦不充分。若快於3.0m/minm,則有於薄膜產生斷裂或厚度偏差的情況。
本發明之熱可塑性樹脂層合延伸薄膜之厚度係在10~1000μm之範圍為理想,較理想為20~200μm。在未達10μm係在以擠出成形製造的情況,厚度精度不良產生之情事多,因為於延伸加工時容易產生斷裂等,所以生產不適當之產生機率變高。又,若超過1000μm,則除了於延伸加工花費時間以外,再加上機械物性之提高效果小,並不實際。本發明之熱可塑性樹脂層合延伸薄膜之厚度係透過於原材製膜時調整製膜速度、T型模頭之吐出口厚度、輥間隙等、或於延伸加工時調節延伸倍率,而可調整。
相對於在本發明之熱可塑性樹脂層合延伸薄膜的包含甲基丙烯酸樹脂(A)的層和包含熱可塑性樹脂(B)的層之厚度之合計而言,包含熱可塑性樹脂(B)的層之厚度之比例係5~50%之範圍為理想。若包含熱可塑性樹脂(B)的層之厚度未達5%,則除了所得到的熱可塑性樹脂層合延伸薄膜之吸水‧吸濕時之尺寸變化變大以外,再加上於吸水、吸濕時包含熱可塑性樹脂(B)的層之機械強度經不起包含甲基丙烯酸樹脂(A)的層之尺寸變化,有於包含熱可塑性樹脂(B)的層會產生龜裂的情況。又,若包含熱可塑性樹脂(B)的層之厚度超過50%,則除了抑制尺寸變化之效果小以外,再加上在熱可塑性樹脂(B)層/甲基丙烯酸樹脂(A)層/熱可塑性樹脂(B)層之2種3層之層構成中僅於包含甲基丙烯酸樹脂(A)的層添加紫外線吸收劑的情況,UV截止性係容易受到包含甲基丙烯酸樹脂(A)的層之厚度不均之影響,有難以控制所得到的熱可塑性樹脂層合延伸薄膜之UV截止性的情況。
於本發明之熱可塑性樹脂層合延伸薄膜係可於該單面或兩面施與硬塗覆處理、防反射處理、防污處理、防帶電處理、耐侯性處理及防眩處理之任一者以上。該等之處理之方法係無特別限定,可使用一般周知之方法。例如,可舉出塗布熱硬化性或光硬化性皮膜的方法、塗布降低反射之塗料的方法、蒸鍍介電質薄膜的方法、塗布防帶電塗料的方法等。塗覆劑係可使用一般周知者,例如可舉出三聚氰胺樹脂、胺基甲酸酯樹脂、丙烯酸樹脂、
紫外線硬化型丙烯酸樹脂等之有機系塗覆劑、矽烷化合物等之矽系塗覆劑、金屬氧化物等之無機系塗覆劑、有機無機混合系塗覆劑。
本發明之熱可塑性樹脂層合延伸薄膜之面內阻滯Re係在0.0~3.0之範圍為理想,0.0~1.0為較理想。又,本發明之熱可塑性樹脂層合延伸薄膜之厚度方向阻滯Rth係在-10.0~10.0之範圍為理想,-6.0~6.0為較理想。Re及Rth係測定薄膜面內之主折射率nx、ny(但是,nx>ny)及厚度方向之主折射率nz,透過下述式而可算出。
Re=(nx-ny)×d(d:薄膜厚度)
Rth=((nx+ny)/2-nz)×d
以下,藉由實施例而具體地說明本發明。但是,本發明係不因此等之實施例及比較例而受到任何限制。在實施例及比較例所得到的熱可塑性樹脂層合延伸薄膜之評估係如以下之方式進行。
關於用以下之合成例所得的熱可塑性樹脂,透過氫化反應前後之UV光譜測定的260nm之吸收之減少率而求出。由在氫化反應前之樹脂之濃度C1的吸光度A1、在氫化反應後之樹脂之濃度C2的吸光度A2,透過以下之式算
出。
氫化率=100×[1-(A2×C1)/(A1×C2)]
關於用以下之合成例所得到的熱可塑性樹脂,透過分子軌道法,計算在結構單元各自之鍵結單位的介電極化差,作為該體積平均透過下述洛倫茲-洛倫茨方程式(Lorentz-Lorenz equation)而算出固有雙折射值。
△n0=2/9π×(n2+2)2/n×△P‧d‧N/M(△n0:固有雙折射值、△P:分子鏈軸方向之介電極化率與於分子鏈直角方向之介電極化率之差、n:折射率、d:密度、N:亞佛加厥常數、M:分子量)
在以下之實施例、比較例之原材薄膜之製作,在連續成形6小時後以目視觀察鏡面輥表面,於鏡面輥表面未產生來自添加劑之滲出的髒污者設為合格(○),以外設為不合格(×)。
關於在以下之實施例、比較例所得到的熱可塑性樹脂層合延伸薄膜,使用數位測微計(Sony Magnescale公司製:M-30)而測定,將取得的熱可塑性樹脂層合延伸薄膜之測定點10點之平均設為薄膜之厚度。
關於在以下之實施例、比較例所得到的原材薄膜,將試驗片裁成110mm×110mm,以固定端同時二軸延伸機,以特定之延伸溫度、預熱時間40秒、延伸速度設為300mm/分、延伸倍率設為縱1.85倍、橫1.85倍,進行二軸延伸,將在延伸加工時不產生斷裂或厚度偏差的片數為10片中9片以上者設為合格(○),以外設為不合格(×)。
關於在以下之實施例、比較例所得到的熱可塑性樹脂層合延伸薄膜,將試驗片裁成100mm×300mm,將試驗片以在直徑80mm之圓筒上長邊成為圓周方向之方式按壓,評估層合樹脂之界面有無剝離。產生剝離的片數為10片中2片以下者設為合格(○),以外設為不合格(×)。
關於在以下之實施例、比較例所得到的熱可塑性樹脂層合延伸薄膜,以分光橢圓偏光計(日本分光公司製:M-
220),以測定波長590nm偵測慢軸,以3維折射率測定模式(擺動角-8~8°),測定薄膜面內之主折射率nx、ny(但是,nx>ny)及厚度方向之主折射率nz,透過下述式,算出面內阻滯Re及厚度方向阻滯Rth。將面內阻滯Re為0.0~3.0nm者設為合格(○),以外設為不合格(×)。又,將厚度方向阻滯Rth為-10.0~10.0nm者設為合格(○),以外設為不合格(×)。
Re=(nx-ny)×d(d:薄膜厚度)
Rth=((nx+ny)/2-nz)×d
關於在以下之實施例、比較例所得到的熱可塑性樹脂層合延伸薄膜,依照JIS P 8115,透過MIT型耐折疲勞試驗機(東洋精機製作所公司製),將折彎角度設為由中心起左右135°、以荷重500g、180次/分之速度測定至斷裂之折彎次數。將至斷裂之折彎次數為50次以上者設為合格(○),以外設為不合格(×)。
將由已純化的甲基丙烯酸甲酯(三菱氣體化學公司製)77.0莫耳%、和已純化的苯乙烯(和光純藥工業公司製)23.0莫耳%、和作為聚合起始劑之t-戊基過氧基-2-乙基己
酸酯(Arkema吉富公司製,商品名:LUPEROX575)0.002莫耳%所構成的單體組成物,以1kg/h連續地供給於附螺旋帶翼之10L完全混合槽,以平均滯留時間2.5小時、聚合溫度150℃進行連續聚合。以聚合槽之液面成為一定之方式由底部連續地抽出,導入溶劑除去裝置而得到顆粒狀之乙烯基共聚樹脂(B1’)。
將所得到的乙烯基共聚樹脂(B1’)溶解於異丁酸甲酯(關東化學公司製),調製10重量%異丁酸甲酯溶液。於1000mL高壓釜裝置將(B1’)之10重量%異丁酸甲酯溶液裝入500重量份、10重量%Pd/C(NE CHEMCAT公司製)裝入1重量份,以氫氣壓9MPa、200℃保持15小時而氫化苯環部位。透過過濾器除去觸媒,導入溶劑除去裝置而得到顆粒狀之乙烯基共聚樹脂(B1)。透過1H-NMR所測定之結果,甲基丙烯酸甲酯結構單元之比例係75莫耳%,又,在波長範圍260nm的吸光度測定之結果,苯環部位之氫化反應率為99%。所得到的乙烯基共聚樹脂(B1)之玻璃轉移溫度係120℃。又,所得到的乙烯基共聚樹脂(B1)之固有雙折射係-0.0003。
除了將在合成例1使用的甲基丙烯酸甲酯之使用量設為62.0莫耳%,又苯乙烯之使用量設為38.0莫耳%以外係與合成例1同樣地進行而得到乙烯基共聚樹脂(B2)。透過1H-NMR所測定之結果,甲基丙烯酸甲酯結構單元之比例
係60莫耳%,在波長範圍260nm的吸光度測定之結果,苯環部位之氫化反應率為99%。所得到的乙烯基共聚樹脂(B2)之玻璃轉移溫度係120℃。又,所得到的乙烯基共聚樹脂(B2)之固有雙折射係+0.0021。
除了將在合成例1使用的甲基丙烯酸甲酯之使用量設為32.000莫耳%,又苯乙烯之使用量設為68.0莫耳%以外係與合成例1同樣地進行而得到乙烯基共聚樹脂(B3)。透過1H-NMR所測定之結果,甲基丙烯酸甲酯結構單元之比例係30莫耳%,在波長範圍260nm的吸光度測定之結果,苯環部位之氫化反應率為99%。所得到的乙烯基共聚樹脂(B3)之玻璃轉移溫度係123℃。又,所得到的乙烯基共聚樹脂(B3)之固有雙折射係+0.0073。
除了將在合成例1苯環部位之氫化反應時間設為5小時以外係與合成例1同樣地進行而得到乙烯基共聚樹脂(B4)。透過1H-NMR所測定之結果,甲基丙烯酸甲酯結構單元之比例係75莫耳%,在波長範圍260nm的吸光度測定之結果,苯環部位之氫化反應率為82%。所得到的乙烯基共聚樹脂(B4)之玻璃轉移溫度係116℃。又,所得到的乙烯基共聚樹脂(B4)之固有雙折射係-0.0055。
將甲基丙烯酸甲酯(住友化學公司製SUMIPEX MG5(固有雙折射:-0.0043、玻璃轉移溫度:105℃))100重量份、和1.2重量份之三嗪系紫外線吸收劑(ADEKA公司製ADK STAB LA-F70),連續地導入軸徑30mm之二軸擠出機,以汽缸溫度250℃、吐出速度25kg/h之條件擠出,得到於甲基丙烯酸甲酯添加紫外線吸收劑的甲基丙烯酸樹脂(A1)。
使用具有軸徑32mm之單軸擠出機、與軸徑65mm之單軸擠出機、與連結於全擠出機的供料頭、與連結於供料頭的T型模頭的多層擠出裝置而成形層合體。於軸徑32mm之單軸擠出機連續地導入在合成例1得到的乙烯基共聚樹脂(B1),以汽缸溫度250℃、吐出速度24.0kg/h之條件擠出。又,於軸徑65mm之單軸擠出機連續地導入在製造例1得到的甲基丙烯酸樹脂(A1),以汽缸溫度250℃、吐出速度36.0kg/h擠出。連結於全擠出機的供料頭係具備2種3層之分配管腳,導入作為溫度250℃之甲基丙烯酸樹脂(A1)和乙烯基共聚樹脂(B1)而層合。在之前已連結的溫度250℃之T型模頭擠出為薄片狀,由上流側以溫度設為110℃、95℃、90℃的3支鏡面輥冷卻,得到於甲基丙烯酸樹脂(A1)之兩側層合乙烯基共聚樹脂(B1)的原
材。得到的原材之厚度係140μm,在連續成形時並無產生輥髒污。將得到的原材以固定端同時二軸延伸機,進行二軸延伸。延伸溫度係設為相較於乙烯基共聚樹脂(B1)之玻璃轉移溫度更高30℃的150℃、預熱時間係設為充分、將延伸速度設為300mm/分、延伸倍率設為縱1.85倍、橫1.85倍,製作熱可塑性樹脂層合延伸薄膜。得到的熱可塑性樹脂層合延伸薄膜之厚度係40μm,各層之厚度係在中央附近為(B1)/(A1)/(B1)=8μm/24μm/8μm,相對於乙烯基共聚樹脂(B1)和甲基丙烯酸樹脂(A1)之合計厚度而言,乙烯基共聚樹脂(B1)之厚度之比例係40%。又,甲基丙烯酸樹脂(A1)與乙烯基共聚樹脂(B1)之玻璃轉移溫度之差係15℃。連續生產性評估、密著性評估、延伸性評估、光學均向性評估、機械強度評估之結果均為良好,綜合判定為合格(○)。
除了將實施例1之延伸溫度設為160℃以外,與實施例1同樣地進行而得到於甲基丙烯酸樹脂(A1)之兩側層合乙烯基共聚樹脂(B1)而延伸的熱可塑性樹脂層合延伸薄膜。原材之連續成形時,並無產生輥髒污。得到的熱可塑性樹脂層合延伸薄膜之厚度係40μm,各層之厚度係在中央附近為(B1)/(A1)/(B1)=8μm/24μm/8μm,相對於乙烯基共聚樹脂(B1)和甲基丙烯酸樹脂(A1)之合計厚度而言,乙
烯基共聚樹脂(B1)之厚度之比例係40%。又,甲基丙烯酸樹脂(A1)與乙烯基共聚樹脂(B1)之玻璃轉移溫度之差係15℃。連續生產性評估、密著性評估、延伸性評估、光學均向性評估、機械強度評估之結果均為良好,綜合判定為合格(○)。
除了將實施例1之延伸溫度設為170℃以外,與實施例1同樣地進行而得到於甲基丙烯酸樹脂(A1)之兩側層合乙烯基共聚樹脂(B1)而延伸的熱可塑性樹脂層合延伸薄膜。原材之連續成形時,並無產生輥髒污。得到的熱可塑性樹脂層合延伸薄膜之厚度係40μm,各層之厚度係在中央附近為(B1)/(A1)/(B1)=8μm/24μm/8μm,相對於乙烯基共聚樹脂(B1)和甲基丙烯酸樹脂(A1)之合計厚度而言,乙烯基共聚樹脂(B1)之厚度之比例係40%。又,甲基丙烯酸樹脂(A1)與乙烯基共聚樹脂(B1)之玻璃轉移溫度之差係15℃。連續生產性評估、密著性評估、延伸性評估、光學均向性評估、機械強度評估之結果均為良好,綜合判定為合格(○)。
將實施例2之軸徑32mm之單軸擠出機之吐出速度以
20.0kg/h之條件擠出。又除了設為軸徑65mm之單軸擠出機之吐出速度40.0kg/h以外,與實施例2同樣地進行而得到於甲基丙烯酸樹脂(A1)之兩側層合乙烯基共聚樹脂(B1)而延伸的熱可塑性樹脂層合延伸薄膜。原材之連續成形時,並無產生輥髒污。得到的熱可塑性樹脂層合延伸薄膜之厚度係40μm,各層之厚度係在中央附近為(B1)/(A1)/(B1)=6.5μm/27μm/6.5μm,相對於乙烯基共聚樹脂(B1)和甲基丙烯酸樹脂(A1)之合計厚度而言,乙烯基共聚樹脂(B1)之厚度之比例係33%。又,甲基丙烯酸樹脂(A1)與乙烯基共聚樹脂(B1)之玻璃轉移溫度之差係15℃。連續生產性評估、密著性評估、延伸性評估、光學均向性評估、機械強度評估之結果均為良好,綜合判定為合格(○)。
將實施例2之軸徑32mm之單軸擠出機之吐出速度以17.0kg/h之條件擠出。又除了設為軸徑65mm之單軸擠出機之吐出速度43.0kg/h以外,與實施例2同樣地進行而得到於甲基丙烯酸樹脂(A1)之兩側層合乙烯基共聚樹脂(B1)而延伸的熱可塑性樹脂層合延伸薄膜。原材之連續成形時,並無產生輥髒污。得到的熱可塑性樹脂層合延伸薄膜之厚度係40μm,各層之厚度係在中央附近為(B1)/(A1)/(B1)=5.5μm/29μm/5.5μm,相對於乙烯基共聚樹
脂(B1)和甲基丙烯酸樹脂(A1)之合計厚度而言,乙烯基共聚樹脂(B1)之厚度之比例係28%。又,甲基丙烯酸樹脂(A1)與乙烯基共聚樹脂(B1)之玻璃轉移溫度之差係15℃。連續生產性評估、密著性評估、延伸性評估、光學均向性評估、機械強度評估之結果均為良好,綜合判定為合格(○)。
除了取代在實施例2使用的乙烯基共聚樹脂(B1)而導入在合成例2得到的乙烯基共聚樹脂(B2)以外係與實施例2同樣地進行而得到於甲基丙烯酸樹脂(A1)之兩側層合乙烯基共聚樹脂(B2)而延伸的熱可塑性樹脂層合延伸薄膜。原材之連續成形時,並無產生輥髒污。得到的熱可塑性樹脂層合延伸薄膜之厚度係40μm,各層之厚度係在中央附近為(B2)/(A1)/(B2)=8μm/24μm/8μm,相對於乙烯基共聚樹脂(B2)和甲基丙烯酸樹脂(A1)之合計厚度而言,乙烯基共聚樹脂(B2)之厚度之比例係40%。又,甲基丙烯酸樹脂(A1)與乙烯基共聚樹脂(B2)之玻璃轉移溫度之差係15℃。連續生產性評估、密著性評估、延伸性評估、光學均向性評估、機械強度評估之結果均為良好,綜合判定為合格(○)。
除了將實施例1之延伸溫度設為130℃以外,與實施例1同樣地進行而得到於甲基丙烯酸樹脂(A1)之兩側層合乙烯基共聚樹脂(B1)而得到原材。得到的原材之厚度係140μm,在連續成形時並無產生輥髒污。又,甲基丙烯酸樹脂(A1)與乙烯基共聚樹脂(B1)之玻璃轉移溫度之差係15℃。雖然連續生產性評估及密著性評估之結果為良好,但是因為延伸性評估為不良所以無法取得延伸薄膜,其他之評估係無法實施。綜合判定為不合格(×)。
除了取代在實施例2使用的乙烯基共聚樹脂(B1)而導入在合成例3得到的乙烯基共聚樹脂(B3)以外係與實施例2同樣地進行而得到於甲基丙烯酸樹脂(A1)之兩側層合乙烯基共聚樹脂(B3)而延伸的熱可塑性樹脂層合延伸薄膜。原材之連續成形時,並無產生輥髒污。得到的熱可塑性樹脂層合延伸薄膜之厚度係40μm,各層之厚度係在中央附近為(B3)/(A1)/(B3)=8μm/24μm/8μm,相對於乙烯基共聚樹脂(B3)和甲基丙烯酸樹脂(A1)之合計厚度而言,乙烯基共聚樹脂(B3)之厚度之比例係40%。又,甲基丙烯酸樹脂(A1)與乙烯基共聚樹脂(B3)之玻璃轉移溫度之差係18℃。雖然連續生產性評估、光學均向性評估之結果為良好,但是延伸性評估、密著性評估為不良,其他之評估係無法實
施。綜合判定為不合格(×)。
除了取代在實施例2使用的乙烯基共聚樹脂(B1)而導入乙烯基共聚樹脂(B4)以外係與實施例2同樣地進行而得到於甲基丙烯酸樹脂(A1)之兩側層合乙烯基共聚樹脂(B4)而延伸的熱可塑性樹脂層合延伸薄膜。原材之連續成形時,並無產生輥髒污。得到的熱可塑性樹脂層合延伸薄膜之厚度係40μm,各層之厚度係在中央附近為(B4)/(A1)/(B4)=8μm/24μm/8μm,相對於乙烯基共聚樹脂(B4)和甲基丙烯酸樹脂(A1)之合計厚度而言,乙烯基共聚樹脂(B4)之厚度之比例係40%。又,甲基丙烯酸樹脂(A1)與乙烯基共聚樹脂(B4)之玻璃轉移溫度之差係11℃。雖然連續生產性評估、密著性評估、延伸性評估、機械強度評估之結果均為良好,但光學均向性評估係不良,綜合判定為不合格(×)。
使用具有軸徑65mm之單軸擠出機、與連結於擠出機的T型模頭的單層擠出裝置而成形單層體。於單軸擠出機連續地導入在製造例1得到的甲基丙烯酸樹脂(A1),以汽缸溫度250℃、吐出速度50.0kg/h擠出。在之前已連結的溫度250℃之T型模頭擠出為薄片狀,由上流側以溫度
設為90℃、82℃、105℃的3支鏡面輥冷卻,得到於甲基丙烯酸樹脂(A1)之原材。得到的原材之厚度係140μm。原材之連續成形時,產生輥髒污。將得到的原材以固定端同時二軸延伸機,進行二軸延伸。設為相較於甲基丙烯酸樹脂(A1)之玻璃轉移溫度更高45℃的150℃、預熱時間係設為充分、將延伸速度設為300mm/分、延伸倍率設為縱1.85倍、橫1.85倍,製作甲基丙烯酸樹脂(A1)延伸薄膜。得到的甲基丙烯酸樹脂(A1)延伸薄膜之厚度係40μm。雖然延伸性評估、機械強度評估均為良好,但連續生產性評估、光學均向性評估係不良,綜合判定為不合格(×)。
除了將比較例4之延伸溫度設為160℃以外係與比較例4同樣地進行而得到於甲基丙烯酸樹脂(A1)之原材。原材之連續成形時,產生輥髒污。得到的原材之厚度係140μm。因為連續生產性評估、延伸性評估為不良所以無法取得延伸薄膜,其他之評估係無法實施。綜合判定為不合格(×)。
Claims (14)
- 一種熱可塑性樹脂層合延伸薄膜,其係於包含甲基丙烯酸樹脂(A)之層的至少一面上具有包含熱可塑性樹脂(B)之層的熱可塑性樹脂層合延伸薄膜,其特徵為前述甲基丙烯酸樹脂(A)中之全部結構單元的90莫耳%以上為甲基丙烯酸甲酯,前述熱可塑性樹脂(B)之固有雙折射為-0.005~0.005,前述甲基丙烯酸樹脂(A)之玻璃轉移溫度TgA(℃)與前述熱可塑性樹脂(B)之玻璃轉移溫度TgB(℃)滿足式:5℃<(TgB-TgA)<50℃。
- 如請求項1之熱可塑性樹脂層合延伸薄膜,其中面內阻滯Re為0.0~3.0nm,且厚度方向阻滯Rth為-10.0~10.0nm之範圍。
- 如請求項3之熱可塑性樹脂層合延伸薄膜,其中前述一般式(1)之R1及R2為甲基。
- 如請求項3之熱可塑性樹脂層合延伸薄膜,其中前述一般式(2)之R4為環己基。
- 如請求項1或2之熱可塑性樹脂層合延伸薄膜,其中於前述包含甲基丙烯酸樹脂(A)之層的兩面具有前述包含熱可塑性樹脂(B)之層。
- 如請求項1或2之熱可塑性樹脂層合延伸薄膜,其中前述延伸為二軸延伸。
- 如請求項1或2之熱可塑性樹脂層合延伸薄膜,其中至少1個延伸方向上的延伸倍率為1.1~3.0倍。
- 如請求項1或2之熱可塑性樹脂層合延伸薄膜,其中全體之厚度為10~1000μm。
- 如請求項1或2之熱可塑性樹脂層合延伸薄膜,其中相對於前述包含甲基丙烯酸樹脂(A)之層與前述包含熱可塑性樹脂(B)之層的合計厚度而言,前述包含熱可塑性樹脂(B)之層的厚度之比例為5~50%之範圍。
- 如請求項1或2之熱可塑性樹脂層合延伸薄膜,其中前述包含熱可塑性樹脂(B)之層包含選自紫外線吸收 劑、抗氧化劑、抗著色劑、抗靜電劑、脫模劑、潤滑劑、染料、及顏料所成群組中之一種以上。
- 一種光學薄膜,其特徵為包含如請求項1~11中任一項之熱可塑性樹脂層合延伸薄膜。
- 一種偏光子保護薄膜,其特徵為包含如請求項12之光學薄膜。
- 一種熱可塑性樹脂層合延伸薄膜之製造方法,其係如請求項1~11中任一項之熱可塑性樹脂層合延伸薄膜之製造方法,其特徵為包含:製造在包含甲基丙烯酸樹脂(A)之層的至少一面上具有包含熱可塑性樹脂(B)之層之熱可塑性樹脂層合體的步驟,及,將前述熱可塑性樹脂層合體以TgB+25(℃)~TgB+65(℃)之範圍的延伸加工溫度進行延伸的步驟;其中,前述甲基丙烯酸樹脂(A)中之全部結構單元的90莫耳%以上為甲基丙烯酸甲酯,前述熱可塑性樹脂(B)之固有雙折射為-0.005~0.005,前述甲基丙烯酸樹脂(A)之玻璃轉移溫度TgA(℃)與前述熱可塑性樹脂(B)之玻璃轉移溫度TgB(℃)滿足式:5℃<(TgB-TgA)<50℃。
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US20130095337A1 (en) * | 2010-06-21 | 2013-04-18 | Mitsubishi Gas Chemical Company, Inc. | Thermoplastic resin laminate |
US20120161345A1 (en) * | 2010-12-27 | 2012-06-28 | Skc Haas Display Films Co., Ltd. | Method of manufacturing a diffusely-reflecting polarizer having a substantially amorphous nano-composite continuous phase |
JP2013114198A (ja) * | 2011-11-30 | 2013-06-10 | Keio Gijuku | 光学フィルム、光学フィルム用樹脂材料及び画像表示装置 |
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US20110069257A1 (en) * | 2004-03-23 | 2011-03-24 | Shunsuke Yamanaka | Optical laminate, optical element and liquid crystal display device |
US20150062702A1 (en) * | 2012-03-15 | 2015-03-05 | Zeon Corporation | Phase difference film laminate, method for producing phase difference film laminate, and method for producing phase difference film |
US20150378079A1 (en) * | 2013-02-04 | 2015-12-31 | Zeon Corporation | Multilayer retardation film and method for producing same |
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US20190339420A1 (en) | 2019-11-07 |
TW201800229A (zh) | 2018-01-01 |
JP6834992B2 (ja) | 2021-02-24 |
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CN108602335B (zh) | 2020-05-08 |
EP3412452B1 (en) | 2021-12-08 |
WO2017135336A1 (ja) | 2017-08-10 |
CN108602335A (zh) | 2018-09-28 |
EP3412452A1 (en) | 2018-12-12 |
KR20180104318A (ko) | 2018-09-20 |
JPWO2017135336A1 (ja) | 2018-12-06 |
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