TWI828020B - 聚酯膜、標籤膜、顯示器用擴散膜及顯示器用透鏡膜 - Google Patents
聚酯膜、標籤膜、顯示器用擴散膜及顯示器用透鏡膜 Download PDFInfo
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- TWI828020B TWI828020B TW110146888A TW110146888A TWI828020B TW I828020 B TWI828020 B TW I828020B TW 110146888 A TW110146888 A TW 110146888A TW 110146888 A TW110146888 A TW 110146888A TW I828020 B TWI828020 B TW I828020B
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- polyester
- polyester resin
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
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Landscapes
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Abstract
本發明提供一種硬挺感優異且透明性亦優異,適於生產成型體、標籤、光學膜等之聚酯膜。本發明之雙軸延伸聚酯膜係包含以對苯二甲酸及乙二醇作為主要的構成成分之聚酯樹脂(I),前述聚酯樹脂(I)係藉由DSC所得之再結晶溫度為160℃以上至193℃以下,相對於膜總體100質量%而包含60質量%之前述聚酯樹脂(I),拉伸彈性模數於長度方向、寬度方向均為3200MPa以上,拉伸彈性模數之長度方向與寬度方向之合計為7000MPa以上。
Description
本發明係關於一種雙軸延伸聚酯膜。進而,本發明係關於一種具有雙軸延伸聚酯膜之標籤膜、顯示器用擴散膜及顯示器用透鏡膜。
聚對苯二甲酸乙二酯(PET)膜所代表之雙軸延伸聚酯膜因該優異之透明性、尺寸穩定性、機械性質、電氣性質、耐藥品性等,而被用於磁帶、絕緣帶、照相軟片、描圖膠片(tracing film)、包裝材料、印刷標籤、電氣絕緣材料、資訊記錄材料、各種步驟用紙(processing paper)、光學材料等廣泛之領域(例如專利文獻1及專利文獻2)。這些用途中,強度或彈性等機械特性為非常受重視之性質。例如若強度不足,則於後續之加工步驟中引起斷裂等事故。若彈性模數不足,則硬挺感降低而膜撓曲,可想到搬運性劣化、印刷性降低等事故。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本特開2020-63399公報。
[專利文獻2]日本特開2018-28075公報。
作為提高機械特性中重要之彈性模數的對策,本案發明人著眼於調整延伸倍率、使結晶度增加等方法。然而,於只有增大延伸倍率之情形時,
雖然彈性模數提高,但由斷裂所致之製膜性降低之疑慮增加。另外,雖然亦有僅於雙軸中的其中一者增大倍率之方法,但另一者之彈性模數會降低,成為具有極端異向性之膜。
另一方面,為了使結晶度增加,必須充分進行熱處理。然而,若延長處理時間則產生生產所耗費之時間變長之缺點,若於高溫進行處理,則有產生寡聚物、白化、脆化之問題。
本發明係以該先前技術之課題作為背景而成。亦即,本發明之目的在於提供一種與先前相比較而硬挺感更優異且透明性更優異,適於生產成型體或標籤、光學膜等之聚酯膜。
本案發明人為了達成該目的而進行了潛心研究,結果以至完成了本發明。亦即,本發明提供以下之發明。
1.一種雙軸延伸聚酯膜,係包含以對苯二甲酸及乙二醇作為主要的構成成分之聚酯樹脂(I),聚酯樹脂係藉由DSC(Differential Scanning Calorimeter;差示掃描熱析儀)所得之再結晶溫度為160℃以上至193℃以下;相對於膜總體100質量%而包含60質量%以上之聚酯樹脂(I);拉伸彈性模數於長度方向、寬度方向均為3200MPa以上,拉伸彈性模數之長度方向與寬度方向之合計為7000MPa以上。
2.於一態樣中,本發明之雙軸延伸聚酯膜中,乙二醇或對苯二甲酸或者該對苯二甲酸之酯形成性衍生物係源自於生質資源。
3.於一態樣中,本發明提供一種雙軸延伸聚酯膜,係於上述雙軸延伸聚酯膜之至少單面具有易接著層。
4.於另一態樣中,本發明提供一種標籤膜,係於上述雙軸延伸聚酯膜之至少單面具有黏著層。
5.於一態樣中,本發明提供一種雙軸延伸聚酯膜,係於上述雙軸延伸聚酯膜之至少單面具有UV(Ultraviolet;紫外線)硬化樹脂之塗層。
6.於另一態樣中,本發明提供一種顯示器用擴散膜,係具有上述雙軸延伸聚酯膜。
7.於另一態樣中,本發明提供一種顯示器用透鏡膜,係具有上述雙軸延伸聚酯膜。
本發明之雙軸延伸聚酯膜含有冷結晶溫度為特定範圍之聚酯樹脂,故而能夠保持透明性並且提高膜之機械特性。
根據本發明,可獲得一種較先前而硬挺感更優異且透明性亦更優異的適於生產成型體、標籤、光學膜等之聚酯膜。
以下,針對本發明加以詳細說明。根據本發明,提供一種硬挺感(彈性)優異且適於生產成型體或標籤、光學膜等之聚酯膜。另外,本發明係關於一種於原料中包含聚酯樹脂(I)之聚酯膜,該聚酯樹脂(I)係由源自於植物之乙二醇成分聚合而成。
本發明提供一種雙軸延伸聚酯膜,係包含以對苯二甲酸及乙二醇作為主要的構成成分之聚酯樹脂(I),聚酯樹脂係藉由DSC所得之再結晶溫度為160℃以上至193℃以下,相對於膜總體100質量%而包含60質量%以上之聚酯樹
脂;拉伸彈性模數於長度方向、寬度方向均為3200MPa以上,拉伸彈性模數之長度方向與寬度方向之合計為7000MPa以上。
具有此種特徵之本發明係能夠使機械特性中重要之彈性模數提高。而且,本發明能夠以良好之平衡具有先前被視為困難之下述效果:提高彈性模數,與避免由斷裂所致之製膜性之降低。而且,本發明能夠抑制異向性變得非常大。另外,能夠一併抑制熱處理後的寡聚物之產生、白化及脆化。
[聚酯膜]
本發明中之聚酯膜可為至少包含聚酯樹脂(I)之單層構成之膜,於使用兩種以上之聚酯樹脂之情形時,亦可為多層構成之膜。本態樣中,本發明係至少包含聚酯樹脂(I)。
本發明之聚酯膜係包含以對苯二甲酸及乙二醇作為主要的構成成分之聚酯樹脂(I),前述聚酯樹脂(I)係藉由DSC所得之再結晶溫度為160℃以上至193℃以下。
於一態樣中,本發明中之聚酯膜可除了上述聚酯樹脂(I)以外,包含至少一種聚酯樹脂(II),該聚酯樹脂(II)可藉由下述方式製造:使以芳香族二羧酸或其酯形成性衍生物作為主成分之二羧酸成分、與以乙二醇作為主成分之二醇成分經過酯化反應或轉酯反應,至少於銻化合物及磷化合物之存在下進行縮聚。
再者,於本發明中,聚酯樹脂(II)係指藉由DSC所得之再結晶溫度顯示與本發明之聚酯樹脂(I)不同之溫度,例如未達160℃或超過193℃之聚酯樹脂。
作為本發明之聚酯樹脂(I)中之芳香族二羧酸或其酯形成性衍生物,可列舉對苯二甲酸。
另外,聚酯樹脂(II)中,作為芳香族二羧酸或其酯形成性衍生物,可列舉以下之化合物。具體而言,例如可列舉:對苯二甲酸、鄰苯二甲酸、間苯二甲酸、二溴間苯二甲酸、磺基間苯二甲酸鈉、苯二氧基二羧酸、4,4’-二苯基二羧酸、4,4’-二苯基醚二羧酸、4,4’-二苯基酮二羧酸、4,4’-二苯氧基乙烷二羧酸、4,4’-二苯基碸二羧酸、2,6-萘二羧酸、以及對苯二甲酸二甲酯、2,6-萘二羧酸二甲酯等這些芳香族二羧酸之碳數1至4左右之烷基酯及鹵化物等,其中較佳為對苯二甲酸、2,6-萘二羧酸或這些之烷基酯,尤佳為對苯二甲酸。
另外,作為乙二醇以外之二醇成分,例如可列舉:丙二醇、丁二醇、戊二醇、己二醇、辛二醇、癸二醇、新戊二醇、2-乙基-2-丁基-1,3-丙二醇、二乙二醇、聚乙二醇、聚丁醚二醇等脂肪族二醇;1,2-環己二醇、1,4-環己二醇、1,1-環己烷二甲醇、1,4-環己烷二甲醇、2,5-降冰片烷二甲醇等脂環式二醇;以及二甲苯二醇、4,4’-二羥基聯苯、2,2-雙(4’-羥基苯基)丙烷、2,2-雙(4’-β-羥基乙氧基苯基)丙烷、雙(4-羥基苯基)碸、雙(4-β-羥基乙氧基苯基)磺酸等芳香族二醇;以及2,2-雙(4’-羥基苯基)丙烷之環氧乙烷加成物或環氧丙烷加成物等。
本發明之聚酯樹脂(I)可藉由使二羧酸成分與二醇成分經由酯化反應或轉酯反應進行縮聚而製造,前述二羧酸成分係使前述芳香族二羧酸或其酯形成性衍生物佔二羧酸成分之50莫耳%以上、較佳為90莫耳%以上、進而較佳為95莫耳%以上、尤佳為99莫耳%以上,前述二醇成分係使乙二醇佔二醇成分之50莫耳%以上、較佳為90莫耳%以上、進而較佳為95莫耳%以上、尤佳為97莫耳%以上。
再者,亦可使反應系統內生成的副產物之二乙二醇進行共聚,作為共聚成分較佳為亦包含自系統外添加之部分的二乙二醇之含量為5莫耳%以下。若二乙
二醇之含量多,則除了有作為聚酯樹脂(I)而銻之溶出量之抑制程度降低之傾向以外,還有作為樹脂之熔融熱穩定性、耐熱性及機械強度等降低之傾向。
本發明中之聚酯樹脂(I)係藉由DSC所得之自熔融狀態冷卻時所觀察之再結晶溫度處於特定之範圍內。以-10℃/分鐘自熔融狀態冷卻時所觀察之再結晶溫度為160℃以上,較佳為170℃以上,更佳為172℃以上,進而較佳為174℃以上。藉由滿足上述溫度條件,而能夠抑制結晶化之開始變遲,能夠獲得充分之結晶度。另外,本發明能夠一併抑制熱處理後之寡聚物之產生、白化及脆化。
再結晶溫度為193℃以下,更佳為190℃以下,進而較佳為188℃以下。藉由滿足上述溫度條件,而能夠抑制結晶溫度與熔融溫度之差變得過小,變得能夠顯示優異之延伸性。另外,藉由再結晶溫度為上述範圍而製膜性亦良好,藉由短時間之加熱而可獲得充分之結晶度,故而成為具有充分之彈性模數之膜。另外,本發明能夠一併抑制熱處理後之寡聚物之產生、白化及脆化。
於本發明中,除了聚酯樹脂(I)具有預定之再結晶溫度以外,相對於膜總體100質量%而包含60質量%以上之聚酯樹脂(I)。於一態樣中,亦可相對於膜總體100質量%而包含70質量%以上之聚酯樹脂(I),例如亦可為75質量%以上。藉由聚酯樹脂(I)之含量為上述範圍內,而能夠提高彈性模數,且避免由斷裂所致之製膜性之降低。進而,能夠一併抑制熱處理後之寡聚物之產生、白化及脆化。
另外,亦可相對於膜總體100質量%而包含100質量%以下之聚酯樹脂(I),例如亦可包含98質量%以下之聚酯樹脂(I),於一態樣中,亦可包含95質量%以下之聚酯樹脂(I)。藉由聚酯樹脂(I)之含量為上述範圍內,而能夠提高彈
性模數,且避免由斷裂所致之製膜性之降低。進而,能夠一併抑制熱處理後之寡聚物之產生、白化及脆化。
本發明中之聚酯樹脂(I)可源自於石油,亦可源自於生質。於將源自於石油之聚酯樹脂與使用源自於生質之原料的聚酯樹脂混合使用之情形時,就降低環境負荷之觀點而言,生質度較佳為10%以上,更佳為13%以上。藉由生質度為上述範圍內,而能夠對降低環境負荷發揮效果。
另外,生質度較佳為100%,例如亦可為90%以下。於一態樣中,生質度為13%以上至30%以下,例如為13%以上至20%以下。
例如,聚對苯二甲酸乙二酯藉由僅將乙二醇設為源自於植物而生質度理論上成為20%,但為了設為20%以上,對苯二甲酸亦需要設為源自於植物,成本高漲。關於生質度,將依據ASTM(American Society of Testing Materials;美國材料與試驗學會)D6866所測定的源自於植物之碳佔總碳數之比率設為生質度。本發明中,例如乙二醇或對苯二甲酸或者其酯形成性衍生物係源自於生質資源。
本發明中之聚酯樹脂(I)亦可為將寶特瓶加以回收再利用之回收再利用聚酯樹脂。較佳為使用由含有間苯二甲酸成分作為酸成分之寶特瓶所構成的回收再利用聚酯樹脂。關於寶特瓶所使用之聚酯,為了使瓶外觀良好而進行結晶性之控制,結果有時使用包含10莫耳%以下之間苯二甲酸成分之聚酯。為了將回收再利用樹脂加以活用,有時使用包含間苯二甲酸成分之材料。
對苯二甲酸成分於構成膜中所含之聚酯樹脂的總二羧酸成分中所佔之量較佳為95莫耳%以上,更佳為96莫耳%以上,進而較佳為96.5莫耳%以上,尤佳為97莫耳%以上。若未達95莫耳%則有結晶性降低之傾向,有時熱收縮率會變高,故而不太佳。另一方面,本發明能夠解決此種問題。
另外,膜中所含之聚酯樹脂之對苯二甲酸成分之量較佳為99.5莫耳%以下,更佳為99莫耳%以下。由寶特瓶所構成之回收再利用聚酯樹脂係大多情況下含有間苯二甲酸所代表的對苯二甲酸以外之二羧酸成分,故而構成膜中之聚酯樹脂的對苯二甲酸成分超過99.5莫耳%之結果為,變得難以製造回收再利用樹脂之比率高的聚酯膜,不太佳。另一方面,本發明能夠解決此種問題。
間苯二甲酸成分於構成膜中所含之聚酯樹脂的總二羧酸成分中所佔之量為0.5莫耳%以上,更佳為0.7莫耳%以上,進而較佳為0.9莫耳%以上,尤佳為1莫耳%以上。
由寶特瓶所構成之回收再利用聚酯樹脂係有時大量包含間苯二甲酸成分,故而構成膜中之聚酯樹脂的間苯二甲酸成分未達0.5莫耳%之結果為,變得難以製造回收再利用樹脂之比率高的聚酯膜,不太佳。另一方面,本發明能夠解決此種問題。
間苯二甲酸成分於構成膜中所含之聚酯樹脂的總二羧酸成分中所佔之量較佳為5莫耳%以下,更佳為4莫耳%以下,進而較佳為3.5莫耳%以下,尤佳為3莫耳%以下。若超過5莫耳%則結晶性降低,故而不太佳。另一方面,本發明能夠解決此種問題。
另外,藉由將間苯二甲酸成分之含有率設為上述範圍,而變得容易製作層壓強度、收縮率、厚度不均優異之膜而較佳。
由寶特瓶所構成之回收再利用樹脂之極限黏度較佳為0.9dl/g以下,更佳為0.8dl/g以下,進而較佳為0.77dl/g以下,尤佳為0.75dl/g以下。若超過0.9dl/g則有時變得不易自擠出機吐出樹脂而生產性降低,不太佳。另一方面,本發明能夠解決此種問題。
於獲得膜之潤滑性之方面,較佳為於原料添加潤滑劑。關於潤滑劑,作為潤滑劑種類,除了二氧化矽、碳酸鈣、氧化鋁等無機系潤滑劑以外,較佳為有機系潤滑劑,更佳為二氧化矽、碳酸鈣。這些無機粒子能以單體使用,或亦可併用兩種以上。這些粒子可藉由預先添加於聚酯樹脂中而含有於膜內。添加有粒子之聚酯樹脂亦可用於膜總體也無妨,但亦可藉由僅用於表層而確保更高之透明性。潤滑劑添加層可僅設於單面,亦可設於兩面也無妨。為了兼具潤滑性與透明性,相對於膜總體之厚度,表層較佳為1%至30%之範圍。藉此能夠表現出透明性及潤滑性。
膜中之潤滑劑之含有濃度之下限較佳為10ppm,更佳為30ppm,進而較佳為50ppm。若未達上述下限,則有時於潤滑性之方面而言實用性降低。潤滑劑濃度之上限較佳為10000ppm,更佳為9000ppm,進而較佳為8000ppm。若超過上述上限則有時透明性降低。另一方面,本發明能夠解決此種問題。
關於膜中之潤滑劑之粒徑,一次粒徑之下限為0.005μm,較佳為0.010μm,進而較佳為0.015μm。若小於0.005μm則可見熔融時之黏度上升,故而欠佳。關於潤滑劑之粒徑,一次粒徑之上限為50μm,較佳為40μm,進而較佳為30μm。若超過50μm則可見透明性之降低或脫落而欠佳。另一方面,本發明能夠解決此種問題。
於本發明中,聚酯膜於溫度285℃之熔融電阻率較佳為1.0×108Ω.cm以下。因此,所使用之聚酯系樹脂組成物較佳為由後述測定法所得之於285℃之熔融電阻率值以成為1.0×108Ω.cm以下、較佳為以成為0.5×108Ω.cm、進而較佳為以成為0.25×108Ω.cm之方式調整。於僅使用285℃之熔融電阻率值超過1.0×108Ω.cm之聚酯系樹脂來避免前述異常放電之生產條件下
欲向冷卻滾筒密接之情形時,於熔融樹脂片材與冷卻滾筒之間以局部夾入有空氣之狀態冷卻,故而於片材表面產生條狀氣泡(pinner bubble)而欠佳。另外,為了抑制條狀氣泡之產生,需要使生產速度下降至所吐出之熔融樹脂能夠於冷卻滾筒充分密接之程度為止,因此生產成本增大。下限值並無特別既定,若考慮色調等,則較佳為0.01×108Ω.cm以上。
本發明中所使用之聚酯系樹脂中,為了將熔融電阻率值控制於上述範圍,只要使該樹脂中含有鹼土金屬化合物及磷化合物即可。作為含有方法,藉由對由寶特瓶所再生之聚酯混合經含有鹼土金屬化合物及磷化合物之聚酯系樹脂等則無妨。鹼土金屬化合物中之鹼土金屬原子(M2)具有使樹脂之熔融電阻率值降低之作用。鹼土金屬化合物通常被用作由多元羧酸類與多元醇類生成酯時之觸媒,藉由積極添加至作為觸媒之需要量以上,而能夠發揮熔融電阻率值降低作用。具體而言,推薦將鹼土金屬化合物之含量設為以M2基準計而較佳為20ppm(質量基準,以下相同)以上,進而較佳為22ppm以上,尤佳為24ppm以上。另一方面,鹼土金屬化合物之含量推薦設為以M2基準計而為400ppm以下,較佳為350ppm以下,進而較佳為300ppm以下,即便使用超過該含量亦無法獲得與該量相應之效果,反而由該化合物所引起的異物之生成或著色等弊端變大,因而不太佳。
作為較佳之鹼土金屬化合物之具體例,可列舉:鹼土金屬之氫氧化物、脂肪族二羧酸鹽(乙酸鹽、丁酸鹽等,較佳為乙酸鹽)、芳香族二羧酸鹽、與具有酚性羥基之化合物之鹽(與苯酚之鹽等)等。另外,作為鹼土金屬,可列舉鎂、鈣、鍶、鋇等(較佳為鎂)。更具體而言,可列舉氫氧化鎂、乙酸鎂、乙酸鈣、乙酸鍶、乙酸鋇等,其中可較佳地使用乙酸鎂。上述鹼土金屬化合物可單獨使
用或組合使用兩種以上。如今,亦有於鹼土金屬中不包含鎂之定義,但本發明中,意指以往的包含鎂之定義之鹼土金屬。換言之,意指元素週期表IIa族之元素。
磷化合物係自身不具有使膜之熔融電阻率值降低之作用,但藉由與鹼土金屬化合物、及後述之鹼金屬化合物組合,而可有助於熔融電阻率值之降低。原因雖不明,但認為或許是藉由含有磷化合物,而能夠抑制異物之生成,使電荷載體之量增大。磷化合物之含量推薦設為以磷原子(P)基準計而較佳為10ppm(質量基準,以下相同)以上,進而較佳為11ppm以上,尤佳為12ppm以上。若磷化合物之含量低於上述範圍,則熔融電阻率值之降低效果不充分,進而有異物生成量增加之傾向,因而不太佳。
另一方面,磷化合物之含量推薦設為以P基準計而較佳為600ppm以下,進而較佳為550ppm以下,尤佳為500ppm以下,即便使用超過該含量亦無法獲得與該量相應之效果,熔融電阻率值之降低效果飽和。進而,促進二乙二醇之生成而引起膜之物性降低,因而不太佳。
作為上述磷化合物,可列舉:磷酸類(磷酸、亞磷酸、次磷酸等)及其酯(烷基酯、芳基酯等)、以及烷基膦酸、芳基膦酸及這些膦酸之酯(烷基酯、芳基酯等)。作為較佳之磷化合物,可例示:磷酸、磷酸之脂肪族酯(磷酸之烷基酯等;例如磷酸單甲酯、磷酸單乙酯、磷酸單丁酯等磷酸單C1-6烷基酯;磷酸二甲酯、磷酸二乙酯、磷酸二丁酯等磷酸二C1-6烷基酯;磷酸三甲酯、磷酸三乙酯、磷酸三丁酯等磷酸三C1-6烷基酯等)、磷酸之芳香族酯(磷酸三苯酯、磷酸三甲苯酯等磷酸之單、二或三C6-9芳基酯等)、亞磷酸之脂肪族酯(亞磷酸之烷基酯等;例如亞磷酸三甲酯、亞磷酸三丁酯等亞磷酸之單、二或三C1-6烷基酯等)、
烷基膦酸(甲基膦酸、乙基膦酸等C1-6烷基膦酸)、烷基膦酸烷基酯(甲基膦酸二甲酯、乙基膦酸二甲酯等C1-6烷基膦酸之單或二C1-6烷基酯等)、芳基膦酸烷基酯(苯基膦酸二甲酯、苯基膦酸二乙酯等C6-9芳基膦酸之單或二C1-6烷基酯等)、芳基膦酸芳基酯(苯基膦酸二苯酯等C6-9芳基膦酸之單或二C6-9芳基酯等)等。尤佳之磷化合物中,包含磷酸、磷酸三烷基酯(磷酸三甲酯等)。這些磷化合物可單獨使用或組合使用兩種以上。
進而,鹼土金屬化合物與磷化合物較佳為以鹼土金屬原子(M2)與磷原子(P)之質量比(M2/P)計為1.2以上至5.0以下而含有於膜中。若M2/P值為1.2以下,則熔融電阻率值之降低效果明顯減少。更佳為1.3以上,進而較佳為1.4以上。另一方面,若M2/P值超過5.0,則相較於熔融電阻率值之降低效果,異物生成更受到促進,或膜著色等弊端變大而欠佳。更佳為4.5以下,進而較佳為4.0以下。
另外,於本發明之聚酯膜,為了改良印刷用油墨及/或塗劑等之塗佈性及/或接著性,亦可於至少單面設置塗佈層也無妨。作為構成該塗佈層之化合物,較佳為聚酯系樹脂。除此以外,可應用作為提高聚胺基甲酸酯樹脂、聚酯胺基甲酸酯樹脂、丙烯酸系樹脂、聚醚系樹脂等通常的聚酯系膜之接著性的手段(易接著層)而揭示之化合物。另外,為了提高這些易接著層之密接耐久性,亦可形成交聯結構。藉由含有交聯劑,可使高溫高濕下之密接性進一步提高。作為具體之交聯劑,可列舉:脲系、環氧系、三聚氰胺系、異氰酸酯系、噁唑啉系、碳二醯亞胺系等。另外,為了促進交聯反應,可根據需要而適當使用觸媒等。
於塗佈層,為了對表面賦予潤滑性或消光性、油墨吸收性等,亦可含有潤滑劑粒子。粒子可為無機粒子,亦可為有機粒子,並無特別限定。例如可列舉:(1)二氧化矽、高嶺土、滑石、輕質碳酸鈣、重質碳酸鈣、沸石、氧化鋁、硫酸鋇、碳黑、氧化鋅、硫酸鋅、碳酸鋅、氧化鋯、二氧化鈦、矽酸鋁、矽藻土、矽酸鈣、氫氧化鋁、碳酸鈣、碳酸鎂、磷酸鈣、氫氧化鎂、硫酸鋇等無機粒子;(2)丙烯酸或甲基丙烯酸系、氯乙烯系、乙酸乙烯酯系、尼龍、苯乙烯/丙烯酸系、苯乙烯/丁二烯系、聚苯乙烯/丙烯酸系、聚苯乙烯/異戊二烯系、聚苯乙烯/異戊二烯系、甲基丙烯酸甲酯/甲基丙烯酸丁酯系、三聚氰胺系、聚碳酸酯系、脲系、環氧系、胺基甲酸酯系、酚系、鄰苯二甲酸二烯丙酯系、聚酯系等之有機粒子。為了對塗佈層給予適度之潤滑性,可尤佳地使用二氧化矽。
作為設置塗佈層之方法,可應用凹版塗佈方式、輕觸式塗佈方式、浸漬方式、噴霧塗佈方式、簾幕式塗佈方式、氣刀塗佈方式、刮刀塗佈方式、反向輥塗佈方式等通常所用之方法。作為塗佈之階段,亦可為於膜之延伸前塗佈之方法、於縱向延伸後塗佈之方法、塗佈於延伸處理結束之膜表面之方法等任意方法。
繼而,對本發明中之聚酯膜之製膜方法加以說明,但不特別限定於此。例如,利用通常之方法將由前述組成物所構成之混合物加以乾燥後,自T字之模口以片狀熔融擠出,藉由靜電施加法等密接於澆鑄滾筒而冷卻固化,獲得未延伸膜。繼而,將該未延伸膜進行延伸、配向處理,以下以最普遍地使用之逐步雙軸延伸方法、尤其係將未延伸膜於長度方向進行縱向延伸繼而於寬度方向進行橫向延伸之方法為例進行說明。首先,於沿長度方向之縱向延伸步驟
中,將膜加熱,於周速不同之兩根或多數根輥間延伸至1.0倍至5.0倍。作為此時之加熱手段,可為使用加熱輥之方法,亦可為使用非接觸之加熱媒體之方法,亦可將這些方法併用,較佳為將膜之溫度設為(Tg-10℃)至(Tg+50℃)之範圍。
繼而將單軸延伸膜導入至拉幅機,於寬度方向以(Tg-10℃)至Tm-10℃以下之溫度延伸至1.0倍至6.0倍,藉此獲得雙軸延伸膜。其中,Tg為聚酯系樹脂之玻璃轉移溫度,Tm為聚酯之融點。另外,較佳為對藉由上述方式所得之膜根據需要實施熱處理,作為處理溫度,較佳為於(Tm-60℃)至Tm之範圍進行處理。
[膜之特性]
本發明中之雙軸延伸聚酯膜之拉伸彈性模數係長度方向與寬度方向之合計為7000MPa以上,更佳為7200MPa以上,進而較佳為7500MPa以上。於一態樣中,雙軸延伸聚酯膜之拉伸彈性模數係長度方向與寬度方向之合計為12000MPa以下,例如為11000MPa以下。
進而,雙軸延伸聚酯膜之拉伸彈性模數係於長度方向、寬度方向均為3200MPa以上,例如為3300MPa以上,亦可為3400MPa以上。於一態樣中,雙軸延伸聚酯膜之拉伸彈性模數係於長度方向、寬度方向均可為3500MPa以上,進而較佳為3700MPa以上。藉此,成為等向性而不限定使用方向,具有硬挺感而於搬運時撓曲少,亦適於加工之膜。
於一態樣中,於雙軸延伸聚酯膜之長度方向、寬度方向的至少一方向,拉伸彈性模數為4000MPa以上,例如為4200MPa以上,亦可為4300MPa以上。藉此,成為可進一步提高硬挺感,於搬運時撓曲少,亦更適於加工之膜。
另外,若為本發明,則藉由包含本發明之聚酯樹脂A的膜具有此種拉伸彈性模數,使本發明能夠以良好之平衡具有先前被視為困難之下述效果:提高彈性
模數,與避免由斷裂所致之製膜性之降低。而且,本發明能夠抑制異向性變得非常大。
上述彈性模數可藉由延伸倍率及結晶度而有效地調整。例如於包含本發明之聚酯樹脂(I)之情形時,延伸倍率較佳為於長度方向、寬度方向均為2.0倍以上至5.5倍以下,進而較佳為2.8倍以上至5.5倍以下,更佳為2.9倍以上至5.2倍以下,進而較佳為3.0倍以上至5.0倍以下。若為上述範圍內,則能夠獲得充分之彈性模數,能夠具有良好之製膜性。另外,為了獲得於長度方向、寬度方向均為3200MPa以上之雙軸延伸聚酯膜,寬度方向之延伸倍率相對於長度方向之延伸倍率較佳為1.0以上至1.8倍以下。
另外,關於結晶度,較佳為30%以上,更佳為35%以上,進而較佳為40%以上。該情況可藉由再結晶溫度為上述範圍而達成。
本發明之雙軸延伸聚酯膜之厚度為任意,較佳為5μm以上至500μm以下,進而較佳為30μm以上至300μm以下。藉由為上述範圍內,而能夠避免作業性降低。另外,能夠抑制折痕、厚度不均等,能夠獲得良好之外觀。
本發明之雙軸延伸聚酯膜之霧度較佳為5以下,更佳為4以下,進而較佳為3以下。例如,霧度為0.2以上,亦可為0.5以上。
總透光率較佳為80%以上,更佳為85%以上,進而較佳為88%以上。若成為上述範圍外,則有透明性降低之傾向。
於另一態樣中,本發明提供一種雙軸延伸聚酯膜,係於上述雙軸延伸聚酯膜之至少單面具有易接著層。
於一態樣中,本發明提供一種標籤膜,係於上述雙軸延伸聚酯膜之至少單面具有黏著層。
於一態樣中,本發明提供一種雙軸延伸聚酯膜,係於上述雙軸延伸聚酯膜之至少單面具有UV硬化樹脂之塗層。
易接著層、黏著層及UV硬化樹脂之塗層亦可為公知之層。
於另一態樣中,本發明提供一種顯示器用擴散膜,係具有上述雙軸延伸聚酯膜。
於另一態樣中,本發明提供一種顯示器用透鏡膜,係具有上述雙軸延伸聚酯膜。
[實施例]
繼而,藉由實施例對本發明加以更詳細說明,但本發明不限定於以下之例。膜之評價係藉由下述測定法進行。
[聚酯之融點、再結晶溫度]
使用SII製差示掃描式熱析儀(DSC),以樣本量10mg、升溫-降溫速度20℃/分鐘進行測定。將此處探測之融解吸熱波峰作為融點,將於降溫時檢測出之放熱波峰作為再結晶溫度。
[厚度]
使用測微計以有效數字4位測定三點,將平均值四捨五入成有效數字3位作為平均厚度(μm)。
[拉伸彈性模數]
依據JIS(Japanese Industrial Standards;日本工業標準)K 7113。使用剃刀於膜之長度方向及寬度方向切出寬度10mm、長度180mm之試樣作為試樣。以夾頭間距離100mm、拉伸速度200mm/分鐘之條件進行,使用3次測定結果之平均值。使用島津製作所公司製造之Autograph AG5000A作為測定裝置。
[霧度、總透光率]
使用霧度計(日本電色工業公司製造,NDH5000)進行測定。
[生質度]
將依據ASTM D6866測定的源自於植物之碳於總碳數中所佔之比率設為生質度。
[油墨密接性]
依據JIS-K5400所記載之棋盤格評價,於膜之易接著面印刷油墨後,使用交叉切割導引器以切割刀製作100個1mm網格後,使用膠帶(米其邦(Nichiban)公司製造,賽璐玢膠帶)評價網格部分之密接力。
評價結果
○:油墨殘留之網格為80格至100格。
△:油墨殘留之網格為60格至79格。
×:油墨殘留之網格未達60格。
[厚度不均評價]
測定膜1m之連續厚度,將最大厚度設為Tmax,將最小厚度設為Tmin,將平均厚度設為Tave,藉由下述式求出厚度不均。
厚度不均={(Tmax-Tmin)/Tave}×100(%)。
評價結果
○:厚度不均未達12%。
△:厚度不均為12%以上至未達20%。
×:厚度不均為20%以上。
[聚酯樹脂A之製造例]
於由源自於石油之原料所純化之對苯二甲酸與由源自於植物之原料所純化之乙二醇的混合物中,以於聚酯中以Mg原子計成為70ppm之方式添加乙酸鎂四水合物,於常壓下於溫度255℃進行酯化反應。然後,添加以Sb原子計於聚酯中成為280ppm般之量的三氧化銻、及以P原子計於聚酯中成為40ppm般之量的磷酸三甲酯,於溫度260℃進行反應。
繼而,將反應產物移至縮聚反應槽,一邊加熱升溫一邊將反應系統緩緩減壓,於133Pa(1mmHg)之減壓下於280℃藉由常規方法進行縮聚,獲得IV(intrinsic viscosity;固有黏度)=0.62之聚酯碎片。將該聚酯碎片作為聚酯A。再結晶溫度為180℃。藉由ASTM D6866測定該聚酯A之生質度,結果生質度為17%。
[聚酯樹脂B之製造例]
使用由具有攪拌裝置、分凝器、原料饋入口及產物取出口之三段之完全混合槽所構成的連續酯化反應裝置來作為酯化反應裝置,將TPA(terephthalic acid;對苯二甲酸)設為2噸/hr,將EG(ethylene glycol;乙二醇)設為相對於1莫耳TPA為2莫耳,將三氧化銻設為相對於生成PET而Sb原子成為160ppm之量,將這些之漿料連續供給於酯化反應裝置之第一酯化反應罐,於常壓以平均滯留時間4小時於255℃反應。繼而,將上述第一酯化反應罐內之反應產物連續取出至系統外並供給於第二酯化反應罐,向第二酯化反應罐內供給相對於生成聚合物(生成PET)為8質量%的自第一酯化反應罐蒸餾去除之EG,進而添加包含相對於生成PET而Mg原子成為65ppm之量的乙酸鎂之EG溶液、及包含相對於生成PET而P原子成為20ppm之量的TMPA(trimethyl phosphate;磷酸三甲酯)之EG溶液,於常壓以平均滯留時間1.5小時於260℃反應。繼而,將上述第二酯化反應罐內之反應產物連續取出至系統外並供給於第三酯化反應罐,進而添加包含相對於生成PET而P原子
成為20ppm之量的TMPA之EG溶液,於常壓以平均滯留時間0.5小時於260℃反應。將上述第三酯化反應罐內所生成之酯化反應產物連續供給於三段之連續縮聚反應裝置進行縮聚,進而以不銹鋼燒結體之濾材(標稱過濾精度為阻隔90%之5μm粒子)進行過濾,獲得聚對苯二甲酸乙二酯樹脂。將該樹脂作為聚酯B。再結晶溫度為165℃。
[聚酯樹脂C之製造例]
將自飲料用寶特瓶沖洗殘留之飲料等異物後利用擠出機將經粉碎而得之薄片熔融,依序以網眼尺寸細者變更過濾器,將更細之異物過濾分離兩次,第三次以50μm之最小網眼尺寸之過濾器進行過濾分離,獲得聚酯再生原料。將該聚酯再生原料作為聚酯C。再結晶溫度為192℃。
[聚酯樹脂D之製造例]
將作為芳香族二羧酸成分之對苯二甲酸單元100莫耳%、作為二醇成分之乙二醇單元40莫耳%及新戊二醇單元60莫耳%作為構成成分,與聚酯樹脂B同樣地進行聚合。將所得之產物作為聚酯D。從熔融狀態至160℃為止之間未見到再結晶波峰。
[聚酯樹脂E之製造例]
使用聚對苯二甲酸丁二酯樹脂1100-211XG(CHANG CHUN PLASTICS CO.,LTD.,固有黏度1.28dl/g)。將該樹脂作為聚酯E。再結晶溫度為196℃。
[聚酯樹脂F之製造例]
於將酯化反應罐升溫而到達200℃之時間點,饋入由對苯二甲酸86.4質量份及乙二醇64.4質量份所構成之漿料,一邊攪拌一邊添加作為觸媒之三氧化銻0.025質量份及三乙胺0.16質量份。繼而進行加熱升溫,以計示壓0.34MPa、240
℃之條件進行加壓酯化反應。然後,使酯化反應罐內回到常壓,添加乙酸鎂四水合物0.34質量份,繼而添加磷酸三甲酯0.042質量份。進而,用15分鐘升溫至260℃後,添加磷酸三甲酯0.036質量份,繼而添加乙酸鈉0.0036質量份。將所得之酯化反應產物移動至縮聚反應罐,於減壓下自260℃朝向280℃緩緩升溫後,於285℃進行縮聚反應。縮聚反應結束後,以孔徑5μm(初始過濾效率95%)之不銹鋼燒結體製過濾器進行過濾處理,將所得之縮聚反應產物加以顆粒化。將該顆粒作為聚酯F。
[潤滑劑母料之製造例]
製作出設為於聚酯樹脂C含有0.3%之平均粒徑1.5μm之非晶形二氧化矽的母料來作為潤滑劑母料。
[膜之製作]
[實施例1]
將聚酯a層之原料設為聚酯樹脂A/聚酯樹脂F=95.0質量份/5.0質量份,另外,將聚酯b層之原料設為聚酯樹脂A/聚酯樹脂F/潤滑劑母料=90.8質量份/5.0質量份/4.2質量份。
將這些原料供給於各個擠出機並於280℃熔融,以聚酯A層與聚酯B層成為B/A/B之順序之方式積層,以該層之厚度比率成為8.5/83/8.5之方式以進料塊接合後,自T字模擠出至經調節為30℃之冷卻滾筒上,進行靜電密接而製造2種3層構成之未延伸膜。
使用加熱輥將未延伸膜a均勻加熱至80℃,於周速不同之兩對軋輥間縱向延伸至3.4倍。此時,作為膜之輔助加熱裝置,於軋輥中間部設置具備金反射膜之紅外線加熱器進行加熱。將以此方式獲得之單軸延伸膜引導至拉幅機,加熱至
160℃並橫向延伸至4.0倍,將寬度固定而於250℃實施熱固定處理,進而於210℃於寬度方向鬆弛2.3%,藉此獲得厚度50μm之聚酯膜。製膜性良好,彈性模數、霧度等亦良好。將各種條件、評價結果顯示於表1。
[實施例2]
除了將聚酯b層之原料設為聚酯樹脂A/聚酯樹脂F=95.0質量份/5.0質量份以外,與實施例1同樣地進行而獲得厚度50μm之聚酯膜。將各種條件、評價結果同樣地顯示於表1。
[實施例3]
除了將長度方向之延伸倍率設為3.0倍以外,與實施例1同樣地進行而獲得厚度50μm之聚酯膜。
[實施例4]
除了將長度方向之延伸倍率設為2.8倍以外,與實施例1同樣地進行而獲得厚度50μm之聚酯膜。
[實施例5]
除了將寬度方向之延伸倍率設為4.5倍以外,與實施例4同樣地進行而獲得厚度50μm之聚酯膜。
[實施例6]
除了將聚酯a層之原料設為聚酯樹脂B=100質量份,將聚酯b層之原料設為聚酯樹脂B/潤滑劑母料=95.8質量份/4.2質量份以外,與實施例1同樣地進行而獲得厚度50μm之聚酯膜。
[實施例7]
除了將聚酯a層之原料設為聚酯樹脂C/聚酯樹脂F=95.0質量份/5.0質量份,將聚酯b層之原料設為聚酯樹脂C/聚酯樹脂F/潤滑劑母料=90.8質量份/5.0質量份/4.2質量份以外,與實施例1同樣地進行而獲得厚度50μm之聚酯膜。
[實施例8]
除了將聚酯b層之原料設為聚酯樹脂C/聚酯樹脂F=95.0/5.0質量份以外,與實施例7同樣地進行而獲得厚度50μm之聚酯膜。
[實施例9]
將聚酯a層及聚酯b層之原料均設為聚酯樹脂A=100質量份,與實施例1同樣地進行而獲得厚度50μm之聚酯膜。
[比較例1]
除了將長度方向之延伸倍率設為1.0倍以外,與實施例1同樣地進行而獲得厚度50μm之聚酯膜。將各種條件、評價結果顯示於表1。
[比較例2]
除了將長度方向之延伸倍率設為1.0倍以外,與實施例6同樣地進行而獲得厚度50μm之聚酯膜。
[比較例3]
除了將聚酯a層之原料設為聚酯樹脂B/聚酯樹脂D=50.0質量份/50.0質量份,將聚酯b層之原料設為聚酯樹脂B/聚酯樹脂D/潤滑劑母料=45.8質量份/50.0質量份/4.2質量份以外,與實施例1同樣地進行而獲得厚度50μm之聚酯膜。
[比較例4]
除了將聚酯a層之原料設為聚酯樹脂B/聚酯樹脂E=50.0質量份/50.0質量份,將聚酯b層之原料設為聚酯樹脂B/聚酯樹脂E/潤滑劑母料=55.8質量份/40.0質量份/4.2質量份以外,與實施例1同樣地進行而獲得厚度50μm之聚酯膜。
如上述表所示,實施例1至實施例8中所得之膜係製膜性亦佳,厚度不均亦良好,透明性優異,且顯示充分之彈性模數。根據本發明,可獲得較先前而硬挺感更優異且透明性亦更優異的適於生產成型體、標籤、光學膜等之聚酯膜。
更詳細而言,能夠使機械特性中重要之彈性模數提高。而且,本發明能夠以良好之平衡具有下述效果:提高彈性模數、與避免由斷裂所致之製膜性之降低。另外,本發明能夠抑制異向性變得非常大,能夠一併抑制熱處理後之寡聚物之產生、白化及脆化。
另一方面,比較例1、比較例2雖然製膜性穩定,但為異向性非常強之膜。比較例1、比較例2之膜係長度方向之彈性模數不充分,未滿足拉伸彈性模數於長度方向、寬度方向均為3200MPa以上的本發明之條件。
比較例3、比較例4以未達60%之量包含再結晶溫度為本發明之範圍內之樹脂,故而延伸步驟中未產生充分之應力,而且在熱固定未充分結晶化,無法獲得具有充分之彈性模數的膜。
[產業可利用性]
根據本發明,可獲得一種較先前而硬挺感更優異且透明性亦更優異的適於生產成型體、標籤、光學膜等的聚酯膜。
Claims (7)
- 一種聚酯膜,係由聚酯a層與聚酯b層所積層而成;前述聚酯a層包含2種類之聚酯樹脂(I)以及聚酯樹脂(II);前述聚酯b層包含前述聚酯樹脂(I)以及前述聚酯樹脂(II);前述聚酯樹脂(I)之再結晶化溫度與前述聚酯樹脂(II)之再結晶化溫度不同;前述聚酯樹脂(I)係以對苯二甲酸及乙二醇作為主要的構成成分,乙二醇或對苯二甲酸或者對苯二甲酸之酯形成性衍生物係源自於生質資源;依據ASTM D6866測定的前述聚酯樹脂(I)之生質度為10%以上;前述聚酯樹脂(I)係藉由差示掃描熱析儀所得之以-10℃/分鐘自熔融狀態冷卻時之再結晶溫度為160℃以上至193℃以下;拉伸彈性模數於長度方向、寬度方向均為3200MPa以上;拉伸彈性模數之長度方向與寬度方向之合計為7000MPa以上。
- 如請求項1所記載之聚酯膜,其中結晶度為30%以上,厚度為5μm以上至500μm以下,霧度為5以下,總透光率為80%以上。
- 一種聚酯膜,係於如前述請求項1或2所記載之聚酯膜之至少單面具有易接著層。
- 一種標籤膜,係於如前述請求項1至3中任一項所記載之聚酯膜之至少單面具有黏著層。
- 一種聚酯膜,係於如前述請求項1至3中任一項所記載之聚酯膜之至少單面具有紫外線硬化樹脂之塗層。
- 一種顯示器用擴散膜,係具有如前述請求項1至3或5中任一項所記載之聚酯膜。
- 一種顯示器用透鏡膜,係具有如前述請求項1至3或5中任一項所記載之聚酯膜。
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JP2005288996A (ja) * | 2004-04-05 | 2005-10-20 | Toray Ind Inc | 積層フィルム |
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