TW202000812A - 一種水溶性塗液及塗佈這種水溶性塗液的聚酯光學薄膜 - Google Patents

一種水溶性塗液及塗佈這種水溶性塗液的聚酯光學薄膜 Download PDF

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TW202000812A
TW202000812A TW107121926A TW107121926A TW202000812A TW 202000812 A TW202000812 A TW 202000812A TW 107121926 A TW107121926 A TW 107121926A TW 107121926 A TW107121926 A TW 107121926A TW 202000812 A TW202000812 A TW 202000812A
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water
coating liquid
optical film
soluble coating
coating
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TW107121926A
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TWI698503B (zh
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廖德超
曹俊哲
鄭文瑞
陳政宏
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南亞塑膠工業股份有限公司
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Priority to TW107121926A priority Critical patent/TWI698503B/zh
Priority to CN201910371271.0A priority patent/CN110643250B/zh
Priority to US16/448,852 priority patent/US20190390082A1/en
Priority to JP2019116015A priority patent/JP6836627B2/ja
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Abstract

一種聚酯光學薄膜的表面，塗佈一塗層，其配方，依重量比，包含2-40wt%的丙烯酸酯接枝改質的聚氨酯樹脂、0.5-30wt%的交聯劑、0.05-30wt%的填充粒子溶液、0.05-10wt%的添加劑及50-85wt%的水溶媒；其中，填充粒子溶液的成分中，包含經過表面改質的無機粒子，使塗層達到提高抗沾黏性的效果；該聚酯光學薄膜塗佈塗層後的物性，具有高透明性、低霧度、優異抗沾黏性、優良接著性及滑性等特性，使用用途適合作為液晶顯示器的背光模組基材，例如，擴散膜或增亮膜等。

Description

一種水溶性塗液及塗佈這種水溶性塗液的聚酯光學薄膜
本發明涉及一種水溶性塗液，具塗佈於聚酯薄膜基材的表面上形成塗層之用途，特別是一種塗佈這種塗層的聚酯光學薄膜，具高透明性及低霧度外，其塗層還具優異抗沾黏性、接著性及滑性等特性。
液晶顯示器的背光模組基材，例如，擴散膜或增亮膜等，是由聚酯光學薄膜例如雙軸延伸的PET光學薄膜製成。聚酯光學薄膜的透明性、霧度與滑性，與聚酯光學薄膜的結晶程度，以及，與所添加的微米級滑劑的種類和含量有關外，另一個重要因素也與塗佈在聚酯薄膜基材上面的塗層的物性息息相關。塗層的成分中，除了聚酯樹脂外，還添加微細無機粒子來改善聚酯薄膜的滑性。除了塗層的折射率及表面平整性會影響聚酯光學薄膜的透明性外，塗層中的微細無機粒子的分散程度，也會影響聚酯光學薄膜的透明性。
現有技術中的聚氨酯樹脂，有機械強度低、不耐UV光、耐熱性、與耐水性差等缺點。尤其是，聚酯光學薄膜的塗層成分中，包含聚氨酯樹脂及微細無機粒子時，聚氨酯樹脂與無機粒子間的相容性差。如果無機粒子分散不均勻，會產生團聚的現象。例如，中國大陸專利公開號CN103171223 A1，提到一種高透明性及抗沾黏性佳的聚酯光學薄膜，其塗液配方包括水性聚氨酯樹脂及使用0.04-6μm微細無機粒子等，但無機粒子在聚氨酯樹脂間會分散不均勻易造成團聚。當聚酯光學薄膜經過延伸後， 塗層的這種團聚現象，會在團聚的無機粒子周圍產生空隙，從而導致塗層表面平整性不佳。這些不佳的因素都會影響到聚酯光學薄膜的透光率、霧度和滑性。
當用途作為液晶顯示器的背光模組基材使用時，聚酯光學薄膜的塗層，對供其塗佈的聚酯薄膜基材、以及，對液晶顯示材料(以下簡稱LCD材料)中經UV硬化的高折射率丙烯酸酯樹脂塗層，都必須同時具有優良的接著性。
但，聚酯光學薄膜的塗層，若純為丙烯酸酯樹脂，雖耐候性佳，不但對LCD材料中經UV硬化的高折射率丙烯酸酯樹脂的接著性不佳，對聚酯薄膜基材的接著性也不佳；同樣情形，聚酯光學薄膜的塗層，若純為聚酯樹脂，雖對聚酯薄膜基材的接著性甚佳，但對LCD材料中經UV硬化的丙烯酸酯樹脂的接著性仍不佳。
此外，聚酯光學薄膜的塗層，是塗佈在聚酯薄膜基材的一面或兩面，如果塗層不具備優異抗沾黏性，聚酯光學薄膜於收捲時易沾黏在一起，這種沾黏現象會影響聚酯光學薄膜的後續加工、剪裁或包裝。尤其是，聚酯光學薄膜的表面，受到沾黏後，會形成白霧、條紋及細微晶點，會影響及聚酯光學薄膜的外觀與應用。
更具體而言，聚酯光學薄膜作為液晶顯示器的背光模組基材使用時，聚酯光學薄膜的塗層，是需要具備優異抗沾黏性、優良接著性及滑性等特性。
為解決現有技術中的聚酯光學薄膜的塗層問題，本發明使用丙烯酸酯接枝改質的聚氨酯樹脂，以及表面經過改質的無機粒子，來改善聚氨酯樹脂與無機粒子間的相容性，使無機粒子均勻分散在改質的聚氨 酯樹脂間，從而聚酯光學薄膜的塗層具優異抗沾黏性、接著性及滑性等特性。
本發明的主要目的在於提供一種水溶性塗液，具塗佈於聚酯薄膜基材的表面上形成塗層之用途，依重量比，包含以下成分，且以下各成分的總和為100wt%：(1)2-40wt%的丙烯酸酯接枝改質的聚氨酯樹脂；(2)0.5-30wt%的交聯劑；(3)0.05-30wt%的填充粒子混合液；(4)0.05-10wt%的添加劑，選自助劑、觸媒或共溶劑中的一種或以上；及(5)50-85wt%的水。
作為優選實施例，所述水溶性塗液的成分(3)的填充粒子混合液的組成，包含：a)20-95wt%的無機粒子，選自氧化矽、氧化鈦、氧化鋁、碳酸鈣、磷酸鈣或硫酸鋇中的一種或以上；及b)0.5-30wt%的表面改質劑，對無機粒子表面改質。
作為優選實施例，所述水溶性塗液的成分(3)的填充粒子的粒徑，介於0.005-3μm。
作為優選實施例，所述水溶性塗液的固含量中，表面經過改質的填充粒子濃度，佔0.01-6%。
作為優選實施例，所述水溶性塗液的成分(1)的丙烯酸酯接枝改質的聚氨酯樹脂，是使用由下列成分組成的丙烯酸酯單體進行接枝改質，且以下各成分的總和為100wt%： (a)90-95wt%的含烷基之(甲基)丙烯酸酯；(b)4-9wt%的含羥基之(甲基)丙烯酸酯；(c)1-5wt%的含羧基的乙烯基單體，選自丙烯酸、甲基丙烯酸、衣康酸、丁烯酸、馬來酸、富馬酸或馬來酸酐中的一種或以上。
作為優選實施例，所述水溶性塗液的成分(2)的交聯劑，選自三聚氰胺交聯劑、羥甲基改質的三聚氰胺衍生物交聯劑、異氰酸酯系交聯劑、氮丙啶系交聯劑、噁唑啉系交聯劑或碳二亞胺系交聯劑中的一種或以上。
作為優選實施例，所述水溶性塗液的成分(3)的表面改質劑，選自乙烯基矽烷偶聯劑、環氧基矽烷偶聯劑、苯乙烯基矽烷偶聯劑、甲基丙烯醯氧基矽烷偶聯劑、丙烯醯氧基矽烷偶聯劑、氨基矽烷偶聯劑、異氰脲酸酯基矽烷偶聯劑、脲基矽烷偶聯劑或異氰酸鹽矽烷偶聯劑中的一種或以上。
作為優選實施例，所述水溶性塗液的成分(4)的助劑，選自含矽的添加劑、含氟的添加劑、或含矽/氟混合成分的添加劑。
作為優選實施例，所述水溶性塗液的成分(4)的共溶劑，選自甲醇、乙醇、正丙醇、異丙醇、丁醇、異丁醇、二甲基亞碸、丙酮或四氫呋喃溶劑中的一種或以上。
本發明的又一目的在於提供一種聚酯光學薄膜，具有一雙軸延伸的聚酯薄膜基材，且基材的表面，使用本發明的水溶性塗液塗佈其上構成塗層，可顯著改善聚酯光學薄膜的透明性、霧度、接著性、滑性及抗沾黏性等特性。
本發明的有益效果，包括：
1.聚酯光學薄膜的塗層具優異抗沾黏性、接著性及滑性等特性。
2.聚酯光學薄膜塗佈這種塗層後易收捲不沾黏，有利後續加工、剪裁或包裝。
3.聚酯光學薄膜具有高透明性及低霧度，用途適合作為液晶顯示器的背光模組基材使用，例如，可作為擴散膜、增亮膜、抗反射膜、保護膜使用。
本發明公開一種水溶性塗液，使用用途為供塗佈於聚酯薄膜基材的表面上，從而形成聚酯光學薄膜的塗層，該水溶性塗液(或塗層)的配方，依重量比，包含以下成分，且以下各成分的總和為100wt%：(1)2-40wt%的丙烯酸酯接枝改質的聚氨酯樹脂；(2)0.5-30wt%的交聯劑；優選用量為5-20wt%；(3)0.05-30wt%的填充粒子混合液；(4)0.05-10wt%的添加劑；及(5)50-85wt%的水，作為溶媒使用。
其中，成分(3)的填充粒子混合液，包含：a)20-95wt%的無機粒子；優選用量為20-90wt%，特優選用量為50-80wt%；且選自氧化矽、氧化鈦、氧化鋁、碳酸鈣、磷酸鈣或硫酸鋇中的一種以上；b)0.5-30wt%的表面改質劑；優選用量為5-20wt%。
本發明的水溶性塗液，其中，表面經過改質的填充粒子濃 度，佔水溶性塗液的固含量的0.01%-6%。
所述成分(1)的丙烯酸酯接枝改質的聚氨酯樹脂，其合成方法，包含以下步驟，基於包含去離子水的總反應原料量：
(1)預聚物的製備：
將15-25wt%的聚酯(醚)多元醇，真空脫水，加入裝有攪拌器、溫度計和冷凝管的反應器中，待油浴溫度達到70-80℃時，加入5-12wt%的脂肪族二異氰酸酯，進行合成反應。
(2)預聚物的稀釋及擴鏈：
預聚物反應2-3小時後，再加入10-30wt%的丙烯酸酯單體稀釋降低黏度，持溫85-90℃，直到NCO理論當量比值(NCO/OH)為1.1-2.3，再加入1.5-3.0wt%的乙二胺基乙磺酸鈉(AAS)，續反應25-40分鐘。
(3)水分散：
將步驟(2)反應製得的聚合物降溫至室溫，在轉速500rpm高速剪切力下，加入35-55wt%的去離子水，再加入0.1-0.5wt%的乙二胺，進行擴鏈反應約30分鐘，製得不含溶劑的磺酸鹽型水性聚氨酯分散液。
(4)丙烯酸酯合成：
對步驟(3)的磺酸鹽型水性聚氨酯分散液，加入0.3-1.0wt%的十二烷基硫酸鈉(SLS)乳化劑混合形成乳化液，升溫至50-70℃後，滴加0.01-0.10wt%的過硫酸銨水溶液(APS)起始劑，進行聚合丙烯酸酯，續升溫至75-85℃，在此溫度下恆溫1-3小時，降溫至50-70℃後，加入0.01-0.08wt%的還原劑， 製得所述丙烯酸酯接枝改質的聚氨酯樹脂。
用於接枝改質的丙烯酸酯(單體)的組成，依重量比，包含以下成分，且以下各成分的總和為100wt%：(a)含烷基之(甲基)丙烯酸酯 90-95wt%；(b)含羥基之(甲基)丙烯酸酯 4-9wt%；及(c)含羧基的乙烯基單體 1-5wt%。
所述含烷基之(甲基)丙烯酸酯選自(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸異丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸異辛酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸十八酯、(甲基)丙烯酸環己酯、(甲基)丙烯酸甲氧基乙酯或(甲基)丙烯酸乙氧基甲酯中的一種單獨使用或一種以上混合並用。
所述含羥基之(甲基)丙烯酸選自(甲基)丙烯酸2-羥基乙酯、(甲基)丙烯酸4-羥基丁酯、丙烯酸氯2-羥基丙酯、二乙二醇單(甲基)丙烯酸酯或烯丙醇中的一種單獨使用或一種以上混合並用。
所述含羧基的乙烯基單體選自由丙烯酸、甲基丙烯酸、衣康酸、丁烯酸、馬來酸、富馬酸或馬來酸酐中的一種單獨使用或一種以上混合並用。
成述成分(2)之交聯劑，選自三聚氰胺交聯劑、三聚氰胺與甲醛縮合之羥甲基改質的三聚氰胺衍生物交聯劑、異氰酸酯系交聯劑、氮丙啶系交聯劑、噁唑啉系交聯劑或碳二亞胺系交聯劑中的一種單獨使用或一種以上混合並用。
所述填充粒子混合液中的無機粒子，粒徑介於0.005-3μm。 視聚酯光學薄膜的物性需求，例如透明度、霧度、滑性或抗沾黏性等特性的需求，所述填充粒子混合液中的無機粒子，可搭配組合不同大小粒徑的無機粒子。當無機粒子的粒徑愈大，聚酯光學薄膜的塗層，在高溫下的抗沾效果愈好。當無機粒子的分散性愈佳，無機粒子愈不易團聚，聚酯光學薄膜及其塗層愈透明，霧度愈低。
所述填充粒子混合液中的表面改質劑，選自乙烯基矽烷偶聯劑、環氧基矽烷偶聯劑、苯乙烯基矽烷偶聯劑、甲基丙烯醯氧基矽烷偶聯劑、丙烯醯氧基矽烷偶聯劑、氨基矽烷偶聯劑、異氰脲酸酯基矽烷偶聯劑、脲基矽烷偶聯劑或異氰酸鹽矽烷偶聯劑中的一種單獨使用或一種以上混合並用。
無機粒子經過表面改質劑的改質後，可改善粒子團聚、分散性不佳、相容性低、接著性低等缺點，尤其是，無機粒子可以在塗層中形成微球，且稍微凸起於塗層表面，有效改善了聚酯光學薄膜的塗層的抗沾黏性問題。收捲時，借助無機粒子稍微凸起於塗層表面，聚酯光學薄膜其處於收捲狀態的薄膜與薄膜之間會形成空氣層，而空氣層的存在能降低薄膜與薄膜之間的摩擦係數，也降低了彼此相互間的沾黏性，從而避免薄膜間發生沾黏現象，解決了往昔聚酯光學薄膜收捲易出現沾黏的問題。
所述成分(4)之添加劑，包括助劑、觸媒或共溶劑中的一種單獨使用或一種以上混合並用。其中，添加助劑可以調整塗液的表面張力，提升聚酯光學薄膜的塗層(或塗佈膜)的平坦度以及與聚酯基材間的潤濕性。添加觸媒可以控制塗液的架橋反應速率。添加共溶劑可以控制塗液中的液態成份的揮發速率。
所述觸媒為無機物質、鹽類、有機物質、鹼性物質或酸性物質。所述共溶劑為甲醇、乙醇、正丙醇、異丙醇、丁醇、異丁醇、二甲 基亞碸、丙酮或四氫呋喃溶劑中的一種或以上。
所述助劑包括含矽的添加劑、含氟的添加劑、或含矽/氟混合成分的添加劑。所述含矽的添加劑，選自BYK公司的BYK307、BYK325、BYK331、BYK380N或BYK381中的一種單獨使用或一種以上混合並用。
所述含氟的添加劑，選自3M公司的FC-4430、FC-4432、美國杜邦公司的Zonyl FSN-100或日本大金公司的DSX中的一種單獨使用或一種以上混合並用。
所述含矽/氟混合成分的添加劑，選自BYK公司的BYK346、BYK347或BYK348中的一種單獨使用或一種以上混合並用。
本發明的水溶性塗液(或塗層)，可以採用線外(off-line)或線上(in-line)塗佈方式，塗佈在聚酯薄膜基材的表面上形成聚酯光學薄膜的塗層。而且，所製得的聚酯光學薄膜，具有高透明性、低霧度、優良的抗黏層性、接著性及滑性等特性，適合應用於如LCD或CRT用的擴散膜、增亮膜、保護膜等。
以下各實施例與各比較例的聚酯光學薄膜(簡稱光學膜)，是依照以下評估方法進行評估。
(1) 光透過率及霧度測試：
採用Tokyo Denshoku Co.,Ltd.Haze Meter，型號為TC-HⅢ，測試光學膜樣品的光透過率及霧度值，其方法符合JIS K7705規範。光透過率越高、霧度值越低代表光學膜的光學性質越佳。
(2) 對光學膠密著性測試 ：
採用量宏公司曝光機，型號為Model F300S+AJ-6-UVL，測試光學膜樣品塗佈面對擴散膜或增亮膜用之丙烯酸酯UV膠的接著性，其方法符合ASTM D3359規範。以12號塗佈棒，將國內生產擴散膜或增亮膜用之光學膠塗佈於光學膜樣品之塗佈面後，經UV曝光機曝光乾燥，以百格刀劃百格後，再將3M 600型膠帶貼於百格試樣上，密著後撕離膠帶進行接著性評估。
(3) UV光照射後對光學膠密著性測試 ：
光學膜樣品的塗佈面，先以UV光曝光，經曝光能量500mJ/cm2後，續以前述測試方法(2)進行對光學膠密著性測試，評估光學膠密著性。
(4) 塗層的填充粒子分散性測試 ：
光學膜樣品的塗佈面，使用Hitachi S5000型掃描式電子顯微鏡測試其填充粒子的分散性，首先將樣品固定於碳膠上，再利用鍍金機，鍍上金或白金薄膜，並以10000倍的測試倍率進行觀察。
(5) 塗層抗沾黏性的溫度 ：
以崴鐿公司熱封試驗機，型號HST-H3，測試光學膜樣品的塗層抗沾黏性的溫度。測試條件：取兩片光學膜樣品，將樣品的塗佈膜表面相對，熱封壓力2MPa、熱封時間2分鐘，進行不同溫度的抗沾黏性測試。熱封後，兩片樣品可輕易分開，且表面無痕跡，記錄此溫度即為光學膜樣品的塗層抗沾黏性的極限溫度。
預製丙烯酸酯接枝改質的聚氨酯樹脂 (1)預聚物的製備：
將100g的PTMG2000(聚醚二元醇，分子量2000)、6.5g的1,4-BG(1,4-丁二醇，分子量90)依次加入反應器中，勻速攪拌下升溫至80℃，之後加入43g異佛爾酮二異氰酸酯，升溫至85-90℃，並在此溫度下反應2-3小時。
(2)預聚物的稀釋及擴鏈：
接著，批次加入140g的甲基丙烯酸甲酯(MMA)、8g的丙烯酸2羥乙酯(2-HEA)、4.8g的丙烯酸乙酯(EA)稀釋降黏，對預聚物再加入10g的乙二胺基乙磺酸鈉(AAS)，續反應25-40分鐘。
(3)水分散：
完成反應後，將步驟(2)所得的預聚物降溫至室溫，在500rpm轉速下加入300g的去離子水，再加入1g的乙二胺進行擴鏈反應約30分鐘，製得磺酸鹽型水性聚氨酯乳液。
(4)丙烯酸酯合成：
在快速攪拌下，將4.8g的乳化劑十二烷基硫酸鈉(SLS)加入步驟(3)的磺酸鹽型水性聚氨酯乳液，升溫至50-70℃，之後滴加0.40g的過硫酸銨水溶液(APS)，續升溫至75-85℃，於此溫度恆溫1-3小時，降溫至50-70℃後，加入0.12g的叔丁基過氧化氫水溶液(TBHP)及0.12g的甲醛合次硫酸氫鈉(SFS)，反應30分鐘，得到丙烯酸酯接枝改質的聚氨酯樹脂。
【實施例1】
將PET粒充分乾燥後，送料至擠出機熔融押出，並經過表面溫度為25℃之冷卻筒冷卻及固化，得到未延伸的PET片(Sheet)，經加熱後，在拉伸比為4倍下進行縱向單軸延伸，製得單軸延伸PET膜。
取由下列成分均勻攪拌而成的水溶性塗液：(1)8.5克的丙烯酸酯接枝改質的聚氨酯樹脂；(2)1.0克的三聚氰胺系交聯劑；(3)2.1克的填充粒子混合液；取0.05克的陰離子介面活性劑A、0.45克的非離子介面活性劑B、0.05克的含矽化合物及1.05克的高分子聚合物(聚酯樹脂)為處理劑；對0.10克的100nm氧化矽粒子A及0.40克的30nm氧化矽粒子B進行改質；(4)0.1克的觸媒、5克的異丙醇、1.4克的丁基纖維素及0.01克的含矽或氟助劑化合物；及(5)81.89克的水溶媒。
對預製的單軸延伸PET膜進行單面塗佈處理，將預製的水溶性塗液均勻塗佈在單軸延伸PET膜上，然後，塗佈完成的單軸延伸PET膜，以固定夾引導到105℃的加熱區，經乾燥及去除塗層的水分後，再送入125℃的加熱區；經過3.5倍的橫向延伸後，製得具有單面塗層的雙軸延伸的PET膜，接著，再經過235℃處理8秒鐘，製得膜厚50μm且具有單面塗層的聚酯光學薄膜。
測試聚酯光學薄膜的物理性能，測試結果如表1所示。
【實施例2】
同實施例1的製法，製得膜厚50μm且具有單面塗層的聚酯光學薄膜。但水溶性塗液改為使用由下列成分均勻攪拌而成：(1)8.75克的丙烯酸酯接枝改質的聚氨酯樹脂；(2)0.8克的三聚氰胺系交聯劑及0.5克的噁唑啉系交聯劑；(3)1.95克的填充粒子混合液；取0.25克的陰離子介面活性劑A、0.25克的非離子介面活性劑B、0.05克的含矽化合物及1.05克的高分子聚合物(聚酯樹脂)為處理劑；對0.10克的100nm氧化矽粒子A及0.25克的30nm氧化矽粒子B進行改質；(4)0.1克的觸媒、5克的異丙醇、1.4克的丁基纖維素及0.01克的含矽或氟助劑化合物；及(5)81.49克的水溶媒。
測試聚酯光學薄膜的物理性能，測試結果如表1所示。
【實施例3】
同實施例1的製法，製得膜厚50μm且具有單面塗層的聚酯光學薄膜。但水溶性塗液改為使用由下列成分均勻攪拌而成：(1)8.0克的丙烯酸酯接枝改質的聚氨酯樹脂；(2)1.0克的三聚氰胺系交聯劑及0.5克的噁唑啉系交聯劑；(3)2.0克的填充粒子混合液；取0.45克的陰離子介面活性劑A、0.05克的非離子介面活性劑B、0.05克的含矽化合物及1.05克的高分子聚合物(聚酯樹脂)為處理劑；對0.30克的100nm氧化矽粒子A及0.10克的30nm氧化矽粒子B進行改質； (4)0.1克的觸媒、5克的異丙醇、1.4克的丁基纖維素及0.01克的含矽或氟助劑化合物；及(5)81.99克的水溶媒。
測試聚酯光學薄膜的物理性能，測試結果如表1所示。
【實施例4】
同實施例1的製法，製得膜厚50μm且具有單面塗層的聚酯光學薄膜。但水溶性塗液改為使用由下列成分均勻攪拌而成：(1)8.5克的丙烯酸酯接枝改質的聚氨酯樹脂；(2)1.0克的噁唑啉系交聯劑；(3)2.1克的填充粒子混合液；取0.45克的陰離子介面活性劑A、0.05克的非離子介面活性劑B、0.1克的含矽化合物及1.0克的高分子聚合物(聚酯樹脂)為處理劑；對0.40克的100nm氧化矽粒子A及0.10克的30nm氧化矽粒子B進行改質；(4)0.1克的觸媒、5克的異丙醇、1.4克的丁基纖維素及0.01克的含矽或氟助劑化合物；及(5)81.89克的水溶媒。
測試聚酯光學薄膜的物理性能，測試結果如表1所示。
【實施例5】
同實施例1的製法，製得膜厚50μm且具有單面塗層的聚酯光學薄膜。但水溶性塗液改為使用由下列成分均勻攪拌而成： (1)8.75克的丙烯酸酯接枝改質的聚氨酯樹脂；(2)0.5克的三聚氰胺系交聯劑及0.8克的噁唑啉系交聯劑；(3)2.1克的填充粒子混合液；取0.05克的陰離子介面活性劑A、0.45克的非離子介面活性劑B、0.1克的含矽化合物及1.0克的高分子聚合物(聚酯樹脂)為處理劑；對0.10克的100nm氧化矽粒子A及0.40克的30nm氧化矽粒子B進行改質；(4)0.1克的觸媒、5克的異丙醇、1.4克的丁基纖維素及0.01克的含矽或氟助劑化合物；及(5)81.34克的水溶媒。
測試聚酯光學薄膜的物理性能，測試結果如表1所示。
【實施例6】
同實施例1的製法，製得膜厚50μm且具有雙面塗層的聚酯光學薄膜。但水溶性塗液改為使用由下列成分均勻攪拌而成：(1)8.0克的丙烯酸酯接枝改質的聚氨酯樹脂；(2)0.5克的三聚氰胺系交聯劑及1.0克的噁唑啉系交聯劑；(3)2.05克的填充粒子混合液；取0.25克的陰離子介面活性劑A、0.25克的非離子介面活性劑B、0.1克的含矽化合物及1.0克的高分子聚合物(聚酯樹脂)為處理劑；對0.15克的100nm氧化矽粒子A及0.30克的30nm氧化矽粒子B進行改質；(4)0.1克的觸媒、5克的異丙醇、1.4克的丁基纖維素及0.01克的含矽或氟助劑化合物；及(5)81.94克的水溶媒。
測試聚酯光學薄膜的物理性能，測試結果如表1所示。
【比較例1】
同實施例1的製法，製得膜厚50μm且具有單面塗層的聚酯光學薄膜。但水溶性塗液改為使用由下列成分均勻攪拌而成，且填充粒子未經過改質：(1)8.5克的丙烯酸酯接枝改質的聚氨酯樹脂；(2)1.0克的三聚氰胺系交聯劑；(3)0.4克的30nm氧化矽粒子B；(4)0.1克的觸媒、5克的異丙醇、1.4克的丁基纖維素及0.01克的含矽或氟助劑化合物；及(5)83.59克的水溶媒。
測試聚酯光學薄膜的物理性能，測試結果如表1所示。
【比較例2】
同實施例1的製法，製得膜厚50μm且具有單面塗層的聚酯光學薄膜。但水溶性塗液改為使用由下列成分均勻攪拌而成，且填充粒子未經過改質：(1)8.5克的丙烯酸酯接枝改質的聚氨酯樹脂；(2)1.0克的三聚氰胺系交聯劑；(3)0.10克的100nm氧化矽粒子A及0.3克的30nm氧化矽粒子B；(4)0.1克的觸媒、5克的異丙醇、1.4克的丁基纖維素及0.01克的含矽或氟助 劑化合物；及(5)83.59克的水溶媒。
測試聚酯光學薄膜的物理性能，測試結果如表1所示。
【比較例3】
同實施例1的製法，製得膜厚50μm且具有單面塗層的聚酯光學薄膜。但水溶性塗液改為使用由下列成分均勻攪拌而成：(1)8.50克的丙烯酸酯接枝改質的聚氨酯樹脂；(2)0.1克的三聚氰胺系交聯劑；(3)2.1克的填充粒子混合液；取0.05克的陰離子介面活性劑A、0.45克的非離子介面活性劑B、0.05克的含矽化合物及1.05克的高分子聚合物(聚酯樹脂)為處理劑；對0.10克的100nm氧化矽粒子A及0.40克的30nm氧化矽粒子B進行改質；(4)0.1克的觸媒、5克的異丙醇、1.4克的丁基纖維素及0.01克的含矽或氟助劑化合物；及(5)82.79克的水溶媒。
測試聚酯光學薄膜的物理性能，測試結果如表1所示。
Figure 107121926-A0101-12-0018-1
結果討論：
1.實施例1-6製得的聚酯光學薄膜的塗層成分中，有添加丙烯酸酯接枝改質的聚氨酯樹脂，作為液晶顯示器的背光模組基材使用時，聚酯光學薄膜的塗層，對光學膠的密著性及經UV光照射後對光學膠的密著性均佳。另外，塗層成分中的無機粒子，經表面改質劑後，在塗層中的分散性良好，所以，聚酯光學薄膜製品的光透過率佳、霧度佳；而且，塗層成分中的無機粒子，是使用混摻不同粒徑的無機粒子，可以改善PET基材的滑性，同時使聚酯光學薄膜的塗層提高了抗沾黏性的溫度比較例1-2製得的聚酯光學薄膜的塗層成分中，無機粒子沒有經過表面改質，聚酯光學薄膜製品的光透過率較差，霧度也較差。
2.填充粒子混合液中的無機粒子的粒徑愈大，聚酯光學薄膜製品的塗層的抗沾黏性的溫度愈高，實施例3及4的聚酯光學薄膜製品，塗層使用大粒徑的無機粒子，塗層的抗沾黏性的溫度，高達100℃以上。相對地，比較例1的聚酯光學薄膜製品，塗層不使用大粒徑的無機粒子，也不添加表面改質劑進行改質，塗層的抗沾黏性的溫度較差，只達70℃，是本發明主要改善的項目之一。
3.比較例3的製得的聚酯光學薄膜，塗層的成分中，雖使用混摻不同粒徑的無機粒子，也添加表面改質劑進行改質，收到塗層分散性良好的效果，但交聯劑的添加量不足，導致塗層反應不完全，塗層的抗沾黏性的溫度仍較差。
綜上所述，本發明的聚酯光學薄膜製品的塗層成分中，由 丙烯酸酯接枝改質的聚氨酯樹脂、交聯劑、經過表面改質的無機粒子溶液及其它添加劑等組成，塗佈於聚酯光學基材上形成聚酯光學薄膜的塗層，可顯著改善聚酯光學薄膜的透明性、霧度、接著性、滑性及抗沾黏性等特性。

Claims (10)

  1. 一種水溶性塗液，具塗佈於聚酯薄膜基材的表面上形成塗層之用途，其特徵在於，依重量比，包含以下成分，且以下各成分的總和為100wt%：(1)2-40wt%的丙烯酸酯接枝改質的聚氨酯樹脂；(2)0.5-30wt%的交聯劑；(3)0.05-30wt%的填充粒子混合液；(4)0.05-10wt%的添加劑，選自助劑、觸媒或共溶劑中的一種或以上；及(5)50-85wt%的水；其中，成分(3)之填充粒子混合液的組成，包含：a)20-95wt%的無機粒子，選自氧化矽、氧化鈦、氧化鋁、碳酸鈣、磷酸鈣或硫酸鋇中的一種或以上；及b)0.5-30wt%的表面改質劑，對無機粒子表面改質。
  2. 如申請專利範圍第1項所述的水溶性塗液，其中，成分(3)的填充粒子的粒徑，介於0.005-3μm。
  3. 如申請專利範圍第1項所述的水溶性塗液，其中，表面經過改質的填充粒子濃度，佔水溶性塗液的固含量的0.01%-6%。
  4. 如申請專利範圍第1項、第2項或第3項所述的水溶性塗液，其中，所述丙烯酸酯接枝改質的聚氨酯樹脂，是使用由下列成分組成的丙烯酸酯單體進行接枝改質，且以下各成分的總和為100wt%： (a)含烷基之(甲基)丙烯酸酯 90-95wt%；(b)含羥基之(甲基)丙烯酸酯 4-9wt%；(c)含羧基的乙烯基單體 1-5wt%。
  5. 如申請專利範圍第4項所述的水溶性塗液，其中，所述含羧基的乙烯基單體選自丙烯酸、甲基丙烯酸、衣康酸、丁烯酸、馬來酸、富馬酸或馬來酸酐中的一種或以上。
  6. 如申請專利範圍第4項所述的水溶性塗液，其中，成分(2)的交聯劑，選自三聚氰胺交聯劑、羥甲基改質的三聚氰胺衍生物交聯劑、異氰酸酯系交聯劑、氮丙啶系交聯劑、噁唑啉系交聯劑或碳二亞胺系交聯劑中的一種或以上。
  7. 如申請專利範圍第4項所述的水溶性塗液，其中，成分(3)的表面改質劑，選自乙烯基矽烷偶聯劑、環氧基矽烷偶聯劑、苯乙烯基矽烷偶聯劑、甲基丙烯醯氧基矽烷偶聯劑、丙烯醯氧基矽烷偶聯劑、氨基矽烷偶聯劑、異氰脲酸酯基矽烷偶聯劑、脲基矽烷偶聯劑或異氰酸鹽矽烷偶聯劑中的一種或以上。
  8. 如申請專利範圍第4項所述的水溶性塗液，其中，成分(4)的助劑，選自含矽的添加劑、含氟的添加劑、或含矽/氟混合成分的添加劑。
  9. 如申請專利範圍第4項所述的水溶性塗液，其中，成分(4)的共溶劑，選自甲醇、乙醇、正丙醇、異丙醇、丁醇、異丁醇、二甲基亞碸、丙酮或四氫呋喃溶劑中的一種或以上。
  10. 一種聚酯光學薄膜，具有一雙軸延伸的聚酯薄膜基材，且其中的一表面，使用申請專利範圍第1項的水溶性塗液塗佈其上構成塗層。
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