TWI833890B - 雙軸延伸聚酯膜及其製造方法、包裝袋、以及標籤 - Google Patents
雙軸延伸聚酯膜及其製造方法、包裝袋、以及標籤 Download PDFInfo
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- TWI833890B TWI833890B TW109103434A TW109103434A TWI833890B TW I833890 B TWI833890 B TW I833890B TW 109103434 A TW109103434 A TW 109103434A TW 109103434 A TW109103434 A TW 109103434A TW I833890 B TWI833890 B TW I833890B
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Abstract
本發明提供一種雙軸延伸聚酯膜,銻含量極少而衛生性優異,且異物亦少,具有優異的透明性、耐熱性,並且印刷性、加工性、生產性良好。本發明的雙軸延伸聚酯膜係膜中的銻的含量為10ppm以下,磷的含量為25ppm以上至75ppm以下,膜的極限黏度為0.51dl/g以上至0.70dl/g以下,且膜每1000平方米中1mm以上之缺點數為1.0個以下。
Description
本發明係關於一種雙軸延伸聚酯膜,衛生性優異,印刷性、加工性、生產性良好。
作為耐熱性、機械物性優異之熱塑性樹脂之聚對苯二甲酸乙二酯(PET;polyethylene terephthalate)或聚對苯二甲酸丁二酯(PBT;polybuthylene terephthalate)等聚酯樹脂被用於塑膠膜、電子設備、能源、包裝材料、汽車等非常多樣的領域中。塑膠膜中,雙軸延伸PET膜由於機械特性強度、耐熱性、尺寸穩定性、耐化學品性、光學特性等與成本之平衡優異,故而被廣泛地用於工業用領域、包裝用領域。
於工業用膜之領域中,由於具有優異的透明性,故而可用作適於液晶顯示器或電漿顯示器等平板顯示器(FPD;Flat Panel Display)之功能膜。另外,被賦予有耐水解性之PET膜亦被用作太陽電池背片(back sheet)用膜,作為功能性膜、基底膜以各種目的使用。
於包裝用膜之領域中,被用作食品包裝用途、氣體阻隔膜用途。尤其是,氣體阻隔性優異之膜被用作食品、醫藥品、電子零件等要求氣密性之包裝材料或氣體阻斷材料,近年來需求不斷高漲。
但是,包裝用膜中,由於與食品直接接觸,故而就衛生性之方面而言,較理想為聚酯膜的異物少。另外,將聚酯的原料進行生產(聚合)之步驟中所使用之銻觸媒有致癌性之可能性,因此較理想為對聚酯膜中所添加之銻儘可能少或不含。
先前,例如如專利文獻1、2中所記載,有不使用銻觸媒之聚酯原料。但是,關於使膜中的異物數減少之方法及所期望之膜特性並無記載。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本專利3461175號公報。
[專利文獻2]日本專利3506236號公報。
[發明所欲解決之課題]
本發明的課題在於提供一種雙軸延伸聚酯膜及將該膜捲取而成之膜輥之製造方法,該雙軸延伸聚酯膜係銻含量極少,且異物亦少,具有優異的透明性、耐熱性,並且印刷加工適性及印刷外觀亦優異。
[用以解決課題之手段]
解決上述之課題而成之本發明係由以下之構成所組成。
1.一種雙軸延伸聚酯膜,特徵在於:滿足下述要件(1)至要件(4):(1)膜中的銻的含量為10ppm以下;(2)膜中的磷的含量為25ppm以上至75ppm以下;(3)膜的極限黏度為0.51dl/g以上至0.70dl/g以下;(4)膜每1000平方米中1mm以上之缺點數為1.0個以下。
2.如1.所記載之聚酯膜,所使用之聚酯原料為:於聚酯樹脂中含有選自鋁化合物中的至少1種及選自磷化合物中的至少1種作為聚合觸媒。
3.如1.或2.所記載之聚酯膜,其中膜的霧度為1%以上至8%以下。
4.如1.至3.中任一項所記載之聚酯膜,特徵在於:於150℃、15分鐘之條件下所測定之縱向的熱收縮率為0.8%以上至3%以下。
5.如1.至4.中任一項所記載之聚酯膜,特徵在於:利用連續接觸式厚度計跨越1m長所測定之縱向及橫向的厚度不均的值均為1%以上至10%以下。
6.一種包裝袋,係使用1層以上之如前述1.至5.中任一項所記載之雙軸延伸聚酯膜而成。
7.一種標籤,係使用1層以上之如前述1.至5.中任一項所記載之雙軸延伸聚酯膜而成。
8.一種如1.至5.中任一項所記載之雙軸延伸聚酯膜之製造方法,特徵在於:係以原料聚酯樹脂的極限黏度與聚酯膜的極限黏度之差成為0.06dl/g以下之方式,將原料聚酯樹脂進行熔融擠出,繼而進行冷卻固化而獲得未延伸膜後,將該未延伸膜進行雙軸延伸,繼而進行熱固定處理。
[發明功效]
藉由本發明,提供一種雙軸延伸聚酯膜及將該膜捲取而成之膜輥之製造方法,該雙軸延伸聚酯膜係銻含量極少,且異物亦少,具有優異的透明性、耐熱性,並且印刷加工適性及印刷外觀亦優異。
以下,對本發明的實施形態進行說明,但本發明並不限定於包含以下之實施例之實施形態而進行解釋,當然可在能夠達成發明的目的且不脫離發明的主旨之範圍內進行各種變更。
[原料聚酯樹脂]
本發明的雙軸延伸聚酯膜係以聚對苯二甲酸乙二酯系樹脂作為構成成分。此處,聚對苯二甲酸乙二酯系樹脂含有源自乙二醇之成分及源自對苯二甲酸之成分作為主要構成成分。所謂「主要構成成分」,係指於構成聚酯之二羧酸全部成分100莫耳%中,對苯二甲酸為80莫耳%以上,於二醇全部成分100莫耳%中,乙二醇為80莫耳%以上。
若為不阻礙本發明的目的之範圍,則亦可使其他二羧酸成分及二醇成分共聚。其他二羧酸成分及二醇成分的共聚量相對於全部二羧酸成分或全部二醇成分,分別為未達20莫耳%,較佳為10莫耳%以下,尤佳為5莫耳%以下。
作為上述之其他二羧酸成分,可列舉:間苯二甲酸、鄰苯二甲酸、萘二羧酸、4,4'-二羧基聯苯、間苯二甲酸-5-磺酸鈉等芳香族二羧酸、1,4-環己烷二羧酸、1,3-環己烷二羧酸、1,2-環己烷二羧酸、2,5-降莰烯二羧酸、四氫鄰苯二甲酸等脂環族二羧酸、及草酸、丙二酸、琥珀酸、己二酸、壬二酸、癸二酸、十一烷二酸、十二烷二酸、十八烷二酸、富馬酸、馬來酸、衣康酸、中康酸、檸康酸、二聚酸等脂肪族二羧酸等。
作為上述之其他二醇成分,可列舉:1,2-丙二醇、1,3-丙二醇、1,2-丁二醇、1,3-丁二醇、1,4-丁二醇、2-甲基-1,3-丙二醇、2-胺基-2-乙基-1,3-丙二醇、2-胺基-2-甲基-1,3-丙二醇、1,10-癸二醇、二羥甲基三環癸烷、二乙二醇、三乙二醇等脂肪族二醇、雙酚A、雙酚S、雙酚C、雙酚Z、雙酚AP、4,4'-聯苯酚之環氧乙烷加成物或環氧丙烷加成物、1,2-環己烷二甲醇、1,3-環己烷二甲醇、1,4-環己烷二甲醇等脂環族二醇、聚乙二醇、聚丙二醇等。
作為此種聚對苯二甲酸乙二酯系樹脂之聚合法,可利用以下之方法等任意的製造方法:直接聚合法,係使對苯二甲酸與乙二醇、以及視需要添加之其他二羧酸成分及二醇成分直接反應;以及酯交換法,係於使對苯二甲酸之二甲酯(視需要包含其他二羧酸之甲酯)與乙二醇(視需要包含其他二醇成分)進行酯交換反應後,進行縮聚反應。
作為聚酯樹脂,亦可使用將PET瓶進行再生利用所得之再利用樹脂或包含源自生質之單體成分之聚酯樹脂。
作為本發明的雙軸延伸聚酯膜的構成成分,亦可包含聚醯胺、聚苯乙烯、聚烯烴、及上述以外的聚酯等其他樹脂,但就雙軸延伸聚酯膜的機械特性、耐熱性之方面而言,其他樹脂的含量相對於聚酯膜的全部樹脂成分,較佳為30質量%以下,特佳為20質量%以下,進而更佳為10質量%以下,尤佳為5質量%以下,最佳為0質量%(構成聚酯膜之全部樹脂成分實質上為聚對苯二甲酸乙二酯系樹脂)。
另外,前述聚對苯二甲酸乙二酯系樹脂的固有黏度較佳為0.57dl/g至0.76dl/g之範圍,更佳為0.60dl/g至0.73dl/g,特佳為0.63dl/g至0.70dl/g。若固有黏度低於0.57dl/g,則於生產聚酯膜之中途,膜變得容易破裂(產生所謂斷裂),若高於0.76dl/g,則濾壓上升變大而高精度過濾變得困難,容易變得難以經由過濾器而將樹脂擠出。
另外,前述聚酯膜的樹脂的固有黏度較佳為0.51dl/g至0.70dl/g之範圍,更佳為0.56dl/g至0.68dl/g,特佳為0.59dl/g至0.65dl/g。若固有黏度低於0.51dl/g,則聚酯膜於印刷等加工步驟中變得容易破裂,若固有黏度高於0.76dl/g,則提高機械特性之效果容易成為飽和狀態。
[聚合觸媒]
其次,對製造本發明中所使用之原料聚酯樹脂時所使用之聚合觸媒進行說明。本發明中所使用之聚合觸媒係以具有促進酯化之能力為特徵之聚合觸媒。本發明中,較佳為如後述般儘可能不使用先前使用之三氧化銻等銻化合物之聚合觸媒。作為此種聚合觸媒,較佳為包含選自鋁化合物中的至少1種及選自磷系化合物中的至少1種之聚合觸媒。
於合成本發明中所使用之原料聚酯樹脂時,作為構成所使用之聚合觸媒之鋁化合物,可無限定地使用公知的鋁化合物。
作為鋁化合物,具體而言,可列舉:乙酸鋁、鹼性乙酸鋁、乳酸鋁、氯化鋁、氫氧化鋁、氫氧化氯化鋁及乙醯丙酮酸鋁、草酸鋁等有機鋁化合物及這些之部分水解物等。這些之中,較佳為羧酸鹽、無機酸鹽及螯合物化合物,當中更佳為乙酸鋁、鹼性乙酸鋁、乳酸鋁、氯化鋁、氫氧化鋁、氫氧化氯化鋁及乙醯丙酮酸鋁,特佳為乙酸鋁、鹼性乙酸鋁、氯化鋁、氫氧化鋁及氫氧化氯化鋁,最佳為乙酸鋁、鹼性乙酸鋁。
本發明的聚合觸媒中所使用之鋁化合物的使用量較佳為以鋁原子計,相對於所獲得之聚酯樹脂的總質量殘留1ppm至80ppm,更佳為2ppm至60ppm,特佳為3ppm至50ppm,尤佳為5ppm至40ppm,最佳為10ppm至30ppm。
若低於上述範圍,則有導致觸媒活性不良之可能性,若超過上述範圍,則有引起鋁系異物生成之可能性。
鋁化合物即便於聚酯聚合時置於減壓環境下,由於使用量之大致100%會殘留,因此可認為使用量成為殘留量。
聚合觸媒中所使用之磷化合物並無特別限定,若使用膦酸系化合物、次膦酸系化合物,則觸媒活性提高之效果大而較佳,這些之中,若使用膦酸系化合物,則觸媒活性提高之效果特別大而較佳。
這些磷化合物中,較佳為於同一分子內具有酚部之磷化合物。若為具有酚結構之磷化合物,則無特別限定,但若使用選自由於同一分子內具有酚部之膦酸系化合物、次膦酸系化合物所組成之群組中的一種或兩種以上之化合物,則觸媒活性提高之效果大而較佳。這些之中,若使用一種或兩種以上之於同一分子內具有酚部之膦酸系化合物,則觸媒活性提高之效果特別大而較佳。
另外,作為於同一分子內具有酚部之磷化合物,可列舉下述通式(化1)、(化2)所表示之化合物等。
[化1]
[化2]
(式(化1)至(化2)中,R1
表示包含酚部之碳數1至50之烴基、包含羥基或鹵基或烷氧基或胺基等取代基及酚部之碳數1至50之烴基。R4
表示氫、碳數1至50之烴基、包含羥基或鹵基或烷氧基或胺基等取代基之碳數1至50之烴基。R2
、R3
分別獨立地表示氫、碳數1至50之烴基、包含羥基或烷氧基等取代基之碳數1至50之烴基。其中,烴基亦可包含分支結構、或環己基等脂環結構、或者苯基或萘基等芳香環結構。R2
與R4
之末端彼此亦可鍵結)
作為前述之於同一分子內具有酚部之磷化合物,例如可列舉:對羥基苯基膦酸、對羥基苯基膦酸二甲酯、對羥基苯基膦酸二乙酯、對羥基苯基膦酸二苯酯、雙(對羥基苯基)次膦酸、雙(對羥基苯基)次膦酸甲酯、雙(對羥基苯基)次膦酸苯酯、對羥基苯基苯基次膦酸、對羥基苯基苯基次膦酸甲酯、對羥基苯基苯基次膦酸苯酯、對羥基苯基次膦酸、對羥基苯基次膦酸甲酯、對羥基苯基次膦酸苯酯等。此外,可列舉下述通式(化3)所表示之磷化合物。
[化3]
式(化3)中,X1
、X2
分別表示氫、碳數1至4之烷基、或1價以上之金屬。
另外,X1
中金屬為2價以上,且X2
亦可不存在。進而,亦可對磷化合物配置相當於金屬的剩餘價數之陰離子。
作為金屬,較佳為Li、Na、K、Ca、Mg、Al。
藉由於聚酯之聚合時添加這些於同一分子內具有酚部之磷化合物,則鋁化合物的觸媒活性提高,並且聚合而成之共聚聚酯樹脂的熱穩定性亦提高。
上述之中,作為縮聚觸媒使用較佳之磷化合物係選自化學式(化4)、化學式(化5)所表示之化合物中的至少一種磷化合物。
[化4]
[化5]
作為上述之化學式(化4)所表示之化合物,市售有Irganox1222(BASF公司製造)。另外,作為化學式(化5)所表示之化合物,市售有Irganox1425(BASF公司製造),均可使用。
本發明的聚合觸媒中所使用之磷化合物的使用量較佳為以磷原子計,相對於所獲得之原料聚酯樹脂的總質量殘留10ppm至100ppm,更佳為15ppm至90ppm,特佳為20ppm至80ppm,尤佳為25ppm至70ppm,最佳為30ppm至60ppm。
於殘存有超出上述之上下限之量的磷原子之情形時,有使聚合活性降低之可能性。
磷化合物於聚酯聚合時置於減壓環境下時,根據聚合條件,使用量之約10%至30%會被去除至系統外。因此,實際上必須進行多次試行實驗,充分掌握磷化合物於聚酯中的殘留率以決定使用量。
另外,藉由使用上述之磷化合物,能夠提高樹脂的耐熱性。原因雖不明確,但可認為藉由磷化合物中的受阻酚部分而提高了共聚聚酯樹脂的耐熱性。
若磷化合物的殘留量少於10ppm,則上述之耐熱性提高之效果減弱,結果有時無法獲得本發明的聚酯樹脂的耐熱性、著色改善效果。
在無損本發明的效果之範圍內,為了進一步提高觸媒活性,亦可併用銻化合物、鈦化合物、錫化合物、鍺化合物等含金屬之縮聚觸媒。該情形時,銻化合物相對於所獲得之共聚聚酯樹脂的質量以銻原子計較佳為10ppm以下,鍺化合物相對於所獲得之聚酯樹脂的質量以鍺原子計較佳為10ppm以下,鈦化合物相對於所獲得之聚酯樹脂的質量以鈦原子計較佳為3ppm以下,錫化合物相對於所獲得之聚酯樹脂的質量以錫原子計較佳為3ppm以下。就本發明的目的而言,較佳為儘可能不使用這些銻化合物、鈦化合物、錫化合物、鍺化合物等含金屬之縮聚觸媒。
本發明中,除鋁化合物以外,亦可使少量的選自鹼金屬、鹼土金屬以及其化合物中的至少1種作為第2金屬含有成分共存。使該第2金屬含有成分與觸媒系共存時,除抑制二乙二醇之生成之效果以外,亦提高觸媒活性,因此能獲得進一步提高了反應速度之觸媒成分,從而對生產性提高有效。於併用添加鹼金屬、鹼土金屬、或這些之化合物之情形時,這些成分的使用量(mol%)相對於構成聚酯樹脂之二羧酸成分的莫耳數,較佳為1×10-5
mol%至0.01mol%。鹼金屬、鹼土金屬、或這些之化合物即便於聚酯聚合時置於減壓環境下,由於使用量之大致100%會殘留,因此可認為使用量成為殘留量。
本發明的聚合觸媒不僅於縮聚反應中即使於酯化反應及酯交換反應中亦具有觸媒活性。對苯二甲酸二甲酯等二羧酸之烷基酯與乙二醇等二醇之酯交換反應通常於鋅等酯交換觸媒之存在下進行,但亦可使用本發明的觸媒代替這些觸媒。另外,本發明的聚合觸媒不僅於熔融聚合中即使於固相聚合或溶液聚合中亦具有觸媒活性。
本發明中所使用之聚酯的聚合觸媒可於聚合反應的任意階段添加至反應系。例如,可於酯化反應或酯交換反應的開始前及反應中途的任意階段、縮聚反應的即將開始前或縮聚反應中途的任意階段中添加至反應系。尤其是,本發明的鋁化合物及磷化合物之添加較佳為於縮聚反應的即將開始前添加。
[雙軸延伸聚酯系膜的較佳的製造方法]
本發明的雙軸延伸聚酯膜可為1層、2層、3層、或4層以上之積層結構。於2層結構以上之情形時,雖各層為如上所述以聚對苯二甲酸乙二酯系樹脂、及無機粒子、進而聚對苯二甲酸乙二酯系樹脂以外的樹脂作為構成成分,但較佳為相互鄰接之各層的任意的構成成分的種類或含量不同。
於由A層所構成之單層結構之情形時,本發明中的A層成為雙軸延伸聚酯膜整體。
於包含A層之2層結構之情形時,本發明中的A層成為任一層或兩層。於包含A層之3層結構之情形時,本發明中的A層成為任一層或兩側表層之兩層。
尤其是,於3層結構之情形時,即便於內部層中不存在無機粒子,藉由僅就表層部的添加粒子量進行控制,亦能夠控制膜的表面粗糙度,能夠使膜中無機粒子的含量更少,故而較佳。原因在於,亦連帶改善以下之方面:香味成分經由在無機粒子與聚酯樹脂之交界所形成之孔隙(空隙)而逃逸,保香性降低。
進而,在不對膜表面的特性造成不良影響之範圍內,對於內層部適時混合將製膜步驟中所產生之邊緣部分進行整邊所得之回收原料、或其他製膜步驟的再利用原料等而使用會變得容易,於成本方面亦有優勢。
作為前述之無機粒子,例如可使用二氧化矽、氧化鋁、二氧化鈦、碳酸鈣、高嶺土、硫酸鋇等。無機粒子的平均粒徑較佳為於利用庫爾特計數器進行測定時為0.05μm至3.0μm之範圍內。膜中的無機粒子含有率的下限較佳為0.01重量%,更佳為0.015重量%,特佳為0.02重量%。若未達0.01重量%,則有滑動性降低之情況。上限較佳為1重量%,更佳為0.2重量%,特佳為0.1重量%。若超過1重量%,則有透明性降低之情況,故而不佳。
作為使聚酯中含有無機粒子之方法,例如可列舉:使無機粒子以預定的比例以漿料之形式分散於作為二醇成分之乙二醇中,於聚酯聚合結束前的任意階段添加該乙二醇漿料。
此處,於添加粒子時,例如若不使粒子之合成時所獲得之水溶膠或醇溶膠暫且乾燥即添加粒子,則粒子的分散性良好,能夠抑制粗大突起之產生,故而較佳。
另外,將粒子之水漿料直接與預定的聚酯顆粒混合,供給至排氣方式之雙軸混練擠出機而練入至聚酯之方法亦有效。
本發明中,較佳為使擠出機的樹脂溫度於(樹脂的熔點+2℃以上至樹脂的熔點+6℃以下進行擠出。若擠出溫度未達熔點+2℃,則樹脂不熔融而噴出未熔融物,該未熔融物成為異物,故而欠佳。另外,若於高於熔點+6℃之溫度進行擠出,則樹脂發生熱劣化而成為異物產生之原因,故而欠佳。
並且,將擠出後的片狀的熔融樹脂利用T字模擠出後進行急冷,藉此能夠獲得未延伸膜。此外,作為將熔融樹脂進行急冷之方法,可較佳地採用以下之方法:將熔融樹脂自T字模澆鑄於轉筒上而進行急冷固化,藉此獲得實質上未配向之樹脂片。
另外,於T字模容易附著上熔融樹脂的昇華物(低聚物等),若附著物掉落,則會附著於未延伸片,成為膜的異物,故而欠佳。因此,較佳為對於T字模以昇華物不易掉落之方式預先貼附具有黏著性之片,另外,以即便異物附著於冷卻輥亦不轉印至未延伸片之方式於運轉中亦利用清潔器來進行清潔。
進而,將所獲得之未延伸膜進行雙軸延伸,繼而進行熱固定處理及熱鬆弛處理。藉由將如下之長度方向及寬度方向的延伸條件、熱固定條件、熱鬆弛條件等製膜條件適宜組合,能夠達成後述之較佳的膜特性。以下詳細地進行說明。
延伸方法可為同步雙軸延伸,亦可為逐步雙軸延伸,但就製膜速度快而生產性高之方面而言,較佳為逐步雙軸延伸。以下,對利用首先實施縱延伸、其次實施橫延伸之縱延伸-橫延伸之逐步雙軸延伸法進行說明,但亦可為顛倒順序之橫延伸-縱延伸。
作為長度(縱)方向(以下,有時簡稱為MD)的延伸溫度,就彎曲(bowing)減少之方面而言,較佳為於(Tg+5)℃至(Tg+55)℃進行延伸,作為延伸倍率,較佳為以3.3倍至4.7倍進行延伸。於延伸溫度高於(Tg+55)℃或延伸倍率低於3.3倍之情形時,雖彎曲減少,但寬度方向的分子配向相較於長度方向變得過大,因此無法維持配向平衡,故而欠佳。另外,所獲得之雙軸延伸聚酯膜的平面性亦惡化,故而欠佳。另一方面,於低於(Tg+15)℃或延伸倍率高於4.7倍之情形時,收縮應力增加,彎曲增加,故而欠佳。
另外,於長度方向之延伸中,於多個輥間以多階段進行延伸而並非以一階段進行延伸之方法中,由於一邊控制延伸速度,一邊緩慢地沿長度方向進行延伸,因此能夠減少在膜寬度方向上的物性差。就效果或設備方面、成本方面而言,較佳為二階段至五階段延伸。
於沿寬度(橫)方向(以下,有時簡稱為TD)進行延伸之情形時,將未延伸膜導入至能夠用夾具把持膜的兩端而進行加熱之拉幅機裝置,藉由熱風將膜加熱至預定的溫度後,一邊沿長度方向進行搬送、一邊擴大夾具間的距離,藉此將膜沿寬度方向進行延伸。
另外,若寬度方向的延伸溫度未達(Tg+5)℃,則於延伸時容易產生斷裂,故而欠佳。另外,若高於(Tg+40)℃,則無法實現均勻的寬度方向的延伸,寬度方向的厚度不均變大,因此膜輥的硬度的偏差變大,故而欠佳。更佳為(Tg+8)℃以上至(Tg+37)℃以下,特佳為(Tg+11)℃以上至(Tg+34)℃以下。
寬度方向的延伸倍率並無特別規定,較佳為2倍以上至6倍以下。若延伸倍率未達2倍,則於物質收支方面不易獲得高產率,並且力學強度降低,此外會因寬度方向的厚度不均而產生膜輥的硬度的偏差,故而欠佳。另外,若延伸倍率超過6倍,則於延伸製膜時變得容易斷裂,故而欠佳。
作為TD延伸後的熱固定溫度(熱處理溫度),較佳為220℃至245℃。於熱固定溫度高於245℃之情形時,彎曲增加,故而欠佳。另一方面,於小於220℃之情形時,長度方向及寬度方向的熱收縮率均變高,蒸鍍加工時的熱尺寸穩定性變差,故而欠佳。另外,於TD延伸後的熱固定溫度超過245℃之情形時,彎曲增加,故而欠佳。
熱鬆弛處理步驟中,於膜藉由熱緩和而至收縮為止之期間,有時寬度方向的約束力減少而會因自重而鬆弛,另外,膜有時因伴隨氣流而膨脹,因此膜處於非常容易上下變動之狀況下。因此,該熱鬆弛步驟中,所獲得之雙軸延伸聚酯膜的配向角或斜向熱收縮率差的變化量會因為膜的搬送狀態而大幅變動。作為減輕該變動之方法,例如可列舉:藉由適宜調整自上下部的噴嘴吹出之風速,而將膜保持為平行。作為寬度方向的熱鬆弛率,較佳為4%至8%。於熱緩和率未達4%之情形時,所獲得之雙軸延伸聚酯膜的寬度方向的熱收縮率變高,蒸鍍加工時的尺寸穩定性變差,故而欠佳。另一方面,於熱緩和率大於8%之情形時,會產生彎曲之增加或鬆弛等,寬度方向的厚度不均變大,因此膜輥的硬度的偏差變大,故而欠佳。
利用上述之方法進行延伸製膜而成之膜係藉由捲繞機裝置而捲取,製作母輥。關於該母輥,於後續的分切步驟中,一邊對膜長度方向施加張力,進而自輥上施加利用接觸輥之壓力(以下稱為面壓),一邊分切成任意的寬度,捲取成製品膜輥。
[雙軸延伸聚酯膜的構成及特性]
本發明的雙軸延伸聚酯膜較佳為膜中的銻的含量為10ppm以下。銻係有致癌性疑慮之物質,因此量越少越佳,較佳為5ppm,更佳為0ppm。本發明中所使用之原料樹脂的銻雖較佳為0ppm,但有於生產時混入之可能性,故而設為10ppm以下。
本發明的雙軸延伸聚酯膜較佳為每1000平方米(例如每膜寬度500mm、膜捲長2000m)中1mm以上之尺寸之缺點數為1個以下。如此,藉由將每1000平方米(m2
)之大面積中1mm以上之尺寸之缺點數減少至1個以下,印刷性變得非常良好。若因異物所致之缺點數多,則於印刷中產生漏印,故而欠佳。1mm以上之尺寸之缺點數越少越佳,更佳為0.5個以下,特佳為0.3個以下,尤佳為0.1個以下,最佳為0個。本發明中,有於預料外故障時混入異物之可能性,故而設為1個以下。
本發明的雙軸延伸聚酯膜較佳為聚酯樹脂的極限黏度與聚酯膜的極限黏度之差為0.06dl/g以下。前述之極限黏度之差成為將聚酯樹脂進行熔融擠出時的劣化的程度的指標。若高於0.06dl/g,則樹脂於擠出機內劣化而成為異物之原因,故而欠佳。另外,極限黏度差較佳為0dl/g,但實質上因熔融而難以成為0dl/g。較佳為0.05dl/g以下,更佳為0.04dl/g以下。
為了如上所述般控制極限黏度之差,本發明中較佳為使擠出機的樹脂溫度於樹脂的熔點+2℃以上至樹脂的熔點+6℃以下進行擠出。若擠出溫度未達熔點+2℃,則樹脂不會熔融而噴出未熔融物,該未熔融物成為異物,故而欠佳。另外,若於高於熔點+6℃之溫度進行擠出,則樹脂發生熱劣化而成為異物,故而欠佳。
本發明的雙軸延伸聚酯膜較佳為霧度為1%以上至8%以下。若高於8%,則膜的透明性受損,故而欠佳。霧度以低為佳,但本發明中,為了賦予滑動性,且由於霧度的下限為1%,故而設為上述範圍。霧度較佳為7%以下,更佳為6%以下。
本發明的雙軸延伸聚酯膜較佳為於150℃、15分鐘之條件下所測定之熱收縮率在縱向為0.8%以上至3%以下。若熱收縮率在縱向高於3%,則於印刷後的步驟中進行乾燥時,膜會收縮而產生印刷圖案之偏移等,故而欠佳。若未達0.8%,則無問題,但由於本發明的生產方法中以0.8%為下限,故而設為0.8%以上。熱收縮率的縱向的上限較佳為2.5%以下,更佳為2%以下。再者,該熱收縮率的值係利用後述之式(3)所算出之值。
本發明的雙軸延伸聚酯膜跨越1m長進行測定時的縱向及橫向的厚度不均較佳為膜縱向及橫向的厚度不均均為1%以上至10%以下。若厚度不均大於10%,則於印刷等加工時產生因褶皺所致之漏印或蜿蜒,故而欠佳。膜縱向及橫向的厚度不均以低為佳,但本發明中1%左右為厚度不均的下限。再者,縱向及橫向的厚度不均更佳為8%以下,特佳為6%以下。
本發明的雙軸延伸聚酯膜的厚度並無特別規定,較佳為2μm以上至300μm以下。若厚度未達2μm,則膜的韌性不足,於印刷等加工時容易產生褶皺,另外,因韌性不足而於製成袋或標籤時的步驟中容易產生不良情況,故而欠佳。厚度厚一些並無問題,但此與因應於環境或成本而採行薄化所致減容化背道而馳,因此若厚過300μm則欠佳。厚度更佳為4μm以上至250μm以下,特佳為6μm以上至200μm以下。
本發明的雙軸延伸聚酯膜的製品輥的寬度並無特別規定,較佳為300mm以上至5000mm以下。若寬度未達300mm,則印刷或加工中的效率下降,故而欠佳。寬度寬一些並無問題,但於印刷或加工步驟中,若寬度過寬,則操作規模變大,因此若寬度長於5000mm則欠佳。膜輥的寬度更佳為400mm以上至4500mm以下,特佳為500mm以上至4000mm以下。
[實施例]
以下,藉由實施例更詳細地說明本發明,但本發明完全不受限於這些實施例之態樣,可在不脫離本發明的主旨之範圍內適宜變更。實施例、比較例中所使用之原料的組成、實施例、比較例中的膜的延伸方式、製造條件分別示於表中。
另外,膜的評價方法如下所述。
[Tg(玻璃轉移點)、Tm(熔點)]
使用示差掃描熱量分析裝置(精工電子工業股份有限公司製造,DSC220),將未延伸膜5mg放入至樣品鍋中,蓋上鍋蓋,於氮氣氛圍下以10℃/分鐘之升溫速度自-40℃升溫至300℃而測定。Tg(℃)及Tm(℃)係基於JIS-K7121-1987而求出。
[極限黏度(IV)]
將聚酯0.2g溶解於苯酚/1,1,2,2-四氯乙烷(60/40(重量比))之混合溶媒50ml中,於30℃使用奧士華黏度計而測定。單位為dl/g。
[聚酯膜中的各種原子的含量]
利用以下所示之方法進行定量。
(a)銻原子
利用硫酸/過氧化氫水之混合液使試樣1g進行濕式分解。繼而,添加亞硝酸鈉而使Sb原子成為Sb5+
,添加孔雀綠而與Sb生成藍色錯合物。利用甲苯將該錯合物進行萃取後,使用吸光光度計(島津製作所製造,UV-150-02),測定在波長625nm之吸光度,根據預先製成之校準曲線,將試樣中的Sb原子的量進行比色定量。
(b)磷原子
藉由以下之方法使磷化合物成為正磷酸:使試樣1g於碳酸鈉共存下進行乾式灰化分解之方法、或者利用硫酸/硝酸/過氯酸之混合液或硫酸/過氧化氫水之混合液進行濕式分解之方法。繼而,於1莫耳/L之硫酸溶液中使鉬酸鹽反應而製成磷鉬酸,將該磷鉬酸利用硫酸肼進行還原而生成藍色矽鉬藍雜多酸(Heteropoly blue)。藉由吸光光度計(島津製作所製造,UV-150-02),測定在波長830nm之吸光度。根據預先製成之校準曲線,將試樣中的磷原子的量進行定量。
(c)鋁原子
使試樣0.1g溶解於6M鹽酸溶液並放置一天後,利用純水進行稀釋,製成1.2M鹽酸測定溶液。將所製備之溶液試樣藉由高頻電漿發光分析而求出。
[缺點數]
使用退捲機,將寬度800mm、捲長10000m(8000平方米)之膜輥進行退捲。退捲時,使用FUTEC公司製造的缺點檢測機(型號 F MAX MR)調查缺點數。然後,於縱向或橫向之任一方向求出1mm以上之尺寸之缺點數。由全部之缺點數,藉由式(1),求出每1000平方米之缺點數。
每1000平方米之缺點數=全部之缺點數÷8 (式1)
[印刷]
將進行過缺點檢查之800mm、捲長10000m(8000平方米)之膜輥,使用凹版印刷機(東谷鐵工所公司製造)以速度100m/min且以網點5%實施凹版印刷。此時的油墨係凹版印刷油墨(東洋油墨公司製造:商品名Fine Star R92墨),係使用利用稀釋溶劑(東洋油墨公司製造:商品名SL302)以77:23之比率混合而成之油墨。使用退捲機將所獲得之印刷樣品進行退捲。退捲時,使用FUTEC公司製造的缺點檢測機(型號 F MAX MR)調查漏印數。然後,於縱向或橫向之任一方向求出1mm以上之尺寸之漏印數。由全部之漏印數,藉由式(2),求出每1000平方米之缺點數。
每1000平方米之漏印數=全部之缺點數÷8 (式2)
[熱收縮率]
以沿橫向為寬度10mm、沿縱向為220mm之尺寸進行取樣,沿縱向以200mm之間隔標記標線,測定標線的間隔(L0)後,將該膜夾於紙間,放入溫度控制為150℃之熱風烘箱,處理15分鐘後取出,然後測定標線的間隔(L),由式(3)求出熱收縮率。此外,依據JIS-C-2318進行。
熱收縮率(%)={(L0-L)/L0}×100 (式3)
[霧度]
依據JIS K 7105於23℃測定。使用霧度計(日本電色工業股份有限公司製造,300A)而測定。再者,測定係進行2次,求出2次的平均值。
[厚度不均]
將膜取樣成測定方向1m×寬度方向40mm之短條狀,使用Micron測定器股份有限公司製造的連續接觸式厚度計,以5(m/分鐘)之速度連續地測定膜試樣的厚度。由下式4算出膜的厚度不均。
厚度不均=(最大厚度-最小厚度)÷平均厚度×100(%) (式4)
[聚合觸媒溶液之製備]
[磷化合物之乙二醇溶液]
於具備氮氣導入管、冷卻管之燒瓶中,於常溫常壓下添加乙二醇2.0升後,一邊於氮氣氛圍下以200rpm進行攪拌,一邊添加作為磷化合物之以化學式(4)所表示之Irganox1222(BASF公司製造)200g。進而,追加2.0升之乙二醇後,將套管溫度之設定變更為196℃而進行升溫,自內部溫度成為185℃以上之時間點起於回流下攪拌60分鐘。然後,停止加熱,立即將溶液自熱源取出,以保持氮氣氛圍下之狀態,在30分鐘以內冷卻至120℃以下。
[鋁化合物之乙二醇溶液]
於具備冷卻管之燒瓶中,於常溫常壓下添加純水5.0升後,一邊以200rpm進行攪拌,一邊以與純水成為漿料之形式添加鹼性乙酸鋁(羥基二乙酸鋁)200g。進而,以整體成為10.0升之方式追加純水,於常溫常壓下攪拌12小時。然後,將套管溫度之設定變更為100.5℃而進行升溫,自內部溫度成為95℃以上之時間點起於回流下攪拌3小時。停止攪拌,放置冷卻至室溫。此時,於可見未溶解粒子之情形時,利用玻璃過濾器(3G)將溶液進行過濾而獲得鋁化合物之水溶液。
繼而,於具備蒸餾裝置之燒瓶中,於常溫常壓下添加前述鋁化合物之水溶液2.0升及乙二醇2.0升,以200rpm攪拌30分鐘後,獲得均勻的水/乙二醇混合溶液。繼而,將套管溫度之設定變更為110℃而進行升溫,將水自該溶液餾除。於所餾出之水的量成為2.0升之時間點停止加熱,放置冷卻至室溫,藉此獲得鋁化合物之乙二醇溶液。
以下,「份」表示「質量份」。
於裝備有攪拌機、溫度計、餾出用冷凝機之反應罐中,添加對苯二甲酸2130份、乙二醇1955份、三乙基胺0.7份,於0.35MPa之加壓下,緩慢地從220℃升溫至250℃,一邊將所餾出之水去除至系統外,一邊進行酯化反應。繼而,以相對於聚酯樹脂中的二羧酸成分,磷原子成為0.047莫耳%、鋁原子成為0.021莫耳%之方式,添加作為前述聚合觸媒溶液之磷化合物之乙二醇溶液及鋁化合物之乙二醇混合溶液後,歷時1小時減壓至1.3kPa進行初期聚合,並且上升至270℃,進而以0.13kPa以下進行後期聚合,從而獲得聚酯1。
於前述之聚酯1之製造方法中,如下所述般變更一部分而製造聚酯2及聚酯3。各聚酯的組成及物性示於表1。
實施例及比較例中所使用之聚酯如以下所述。
・聚酯1:聚對苯二甲酸乙二酯(IV 0.73dl/g)
・聚酯2:於上述聚酯1之製造時,相對於聚酯以8,000ppm之比例添加有作為滑劑之SiO2
(FUJI SILYSIA公司製造的SYLYSIA 266)之聚對苯二甲酸乙二酯(IV 0.73dl/g)
・聚酯3:於上述聚酯1之製造時,以成為0.084莫耳%之方式添加銻觸媒代替鋁(IV 0.73dl/g)
[表1]
聚酯的原料組成(莫耳%) | 銻觸媒 | ||||
二羧酸成分 | 多元醇成分 | 滑劑添加量 | IV | ||
(ppm) | (dl/g) | (mol%) | |||
DMT | EG | ||||
聚酯1 | 100 | 100 | 0 | 0.73 | 0 |
聚酯2 | 100 | 100 | 8000 | 0.73 | 0 |
聚酯3 | 98 | 100 | 0 | 0.73 | 0.084 |
DMT:對苯二甲酸二甲酯 | |||||
EG:乙二醇 |
[實施例1]
將上述之聚酯1與聚酯2以重量比97:3混合並投入至擠出機。然後,使該混合樹脂於270℃熔融,冷卻至260℃並自T字模擠出,捲繞於表面溫度冷卻至30℃之旋轉金屬輥而進行急冷,藉此獲得厚度為220μm之未延伸膜。此時的未延伸膜的拉取速度(金屬輥的旋轉速度)為約80m/min。未延伸膜的Tg為75℃,Tm為256℃。另外,於T字模貼附由高熔點聚醯亞胺所製作之黏著片,以避免掉落熔融樹脂的揮發物。另外,為了將掉落至冷卻輥上之異物去除,而使用UV照射型之清潔器。
將所獲得之未延伸片加熱至115℃,利用將第一階段設為1.24倍、第二階段設為1.4倍、第三階段設為2.6倍之三階段延伸,以總延伸倍率4.5倍沿長度方向進行延伸。繼而,以溫度140℃、延伸倍率4.3倍沿寬度方向進行延伸,於243℃進行熱固定,沿寬度方向進行5%熱鬆弛處理。繼而,將該延伸後的膜的兩端部裁斷去除後,經過電暈放電處理,利用捲繞機捲取成輥狀,藉此製作厚度12μm、寬度8m之雙軸延伸聚酯膜之母輥。
藉由上述之方法將所獲得之膜的特性進行評價。另外,缺點數之評價係利用分切成寬度800mm、捲長10000m而獲得之輥,藉由上述之方法進行評價。膜的製造方法示於表2,評價結果示於表3。結果為能夠確保衛生性之足夠低之銻量,為缺點數少而印刷外觀優異之良好之膜。
[實施例2]
將聚酯1與聚酯2以重量比99.5:0.5混合並投入至擠出機,除此以外,利用與實施例1相同的方法獲得雙軸延伸聚酯膜輥。膜的製造方法示於表2,評價結果示於表3。結果為透明性較實施例1優異之良好品質之膜。另外,漏印亦少而良好。
[實施例3]
將聚酯1、聚酯2、及聚酯3以重量比96.5:3:0.5進行混合並投入至擠出機,除此以外,利用與實施例1相同的方法獲得雙軸延伸聚酯膜輥。膜的製造方法示於表2,評價結果示於表3。相較於實施例1,銻量略微增加,缺點數略微增加,但為足夠少之缺點數,為良好品質之膜。
[比較例1]
將聚酯3與聚酯2以重量比97:3混合並投入至擠出機。除此以外,利用與實施例1相同的方法獲得雙軸延伸聚酯膜輥。膜的製造方法示於表2,評價結果示於表3。相較於實施例1,銻量增加,缺點數增加,為品質較差之膜。另外,漏印亦多於實施例1而成為較差之結果。
[比較例2]
將聚酯1、聚酯2、及聚酯3以重量比48.5:3:48.5混合並投入至擠出機。然後,使該混合樹脂於280℃熔融,冷卻至270℃而自T字模擠出,除此以外,藉由與實施例1相同的方法獲得雙軸延伸聚酯膜。藉由與實施例1相同的方法將所獲得之膜的特性進行評價。膜的製造方法示於表2,評價結果示於表3。評價之結果為,極限黏度之降低大,缺點數亦增加,為品質差之雙軸延伸聚酯膜。
[表2]
樹脂組成 (重量比) | 原料的玻璃 轉移溫度 (℃) | 原料的熔點 (℃) | 擠出步驟 | 縱延伸步驟 | 橫延伸步驟 | ||||
擠出溫度 (℃) | 延伸溫度 (℃) | 延伸倍率 | 熱處理 溫度 (℃) | 鬆弛率 (%) | |||||
延伸倍率 | |||||||||
實施例1 | 聚酯1:聚酯2=97:3 | 75 | 256 | 260 | 4.5 | 140 | 4.3 | 243 | 5 |
實施例2 | 聚酯1:聚酯2=99.5:0.5 | 75 | 256 | 260 | 4.5 | 140 | 4.3 | 243 | 5 |
實施例3 | 聚酯1:聚酯2:聚酯3=96.5:3:0.5 | 75 | 256 | 260 | 4.5 | 140 | 4.3 | 243 | 5 |
比較例1 | 聚酯2:聚酯3=3:97 | 75 | 256 | 260 | 4.5 | 140 | 4.3 | 243 | 5 |
比較例2 | 聚酯1:聚酯2:聚酯3=48.5:3:48.5 | 75 | 256 | 270 | 4.5 | 140 | 4.3 | 243 | 5 |
[表3]
厚度 (μm) | 銻含量 (ppm) | 磷含量 (ppm) | IV (dl/g) | IV差 (原料- 膜) (dl/g) | 缺點數 (個/1000平方米) | 漏印數 (個/1000平方米) | 霧度 (%) | 150℃、15分鐘 熱收縮率(%) | 厚度不均 (%) | |||
縱向 | 橫向 | 縱向 | 橫向 | |||||||||
實施例1 | 12 | 0 | 36 | 0.69 | 0.04 | 0.1 | 0.1 | 2.2 | 1.6 | 0.1 | 3 | 3 |
實施例2 | 12 | 0 | 36 | 0.69 | 0.04 | 0.1 | 0.1 | 1.1 | 1.6 | 0.1 | 3 | 3 |
實施例3 | 12 | 1 | 36 | 0.69 | 0.04 | 0.3 | 0.2 | 2.2 | 1.6 | 0.1 | 3 | 3 |
比較例1 | 12 | 145 | 36 | 0.69 | 0.04 | 1.1 | 1 | 2.4 | 1.6 | 0.1 | 3 | 3 |
比較例2 | 12 | 71 | 36 | 0.65 | 0.08 | 1.5 | 1.2 | 2.3 | 1.6 | 0.1 | 3 | 3 |
[產業可利用性]
本發明的雙軸延伸聚酯膜係銻的量極少,且印刷性、加工性、生產性良好之雙軸延伸聚酯膜,係適於衛生性優異之食品包裝袋、標籤之膜。
Claims (8)
- 一種雙軸延伸聚酯膜,滿足下述要件(1)至要件(5):(1)膜中的銻的含量為10ppm以下;(2)膜中的磷的含量為25ppm以上至75ppm以下;(3)膜的極限黏度為0.51dl/g以上至0.70dl/g以下;(4)膜每1000平方米中1mm以上之缺點數為1.0個以下;(5)膜中不含有鈦元素。
- 如請求項1所記載之雙軸延伸聚酯膜,所使用之聚酯原料為:於聚酯樹脂中含有選自鋁化合物中的至少1種及選自磷化合物中的至少1種作為聚合觸媒。
- 如請求項1或2所記載之雙軸延伸聚酯膜,其中膜的霧度為1%以上至8%以下。
- 如請求項1或2所記載之雙軸延伸聚酯膜,於150℃、15分鐘之條件下所測定之縱向的熱收縮率為0.8%以上至3%以下。
- 如請求項1或2所記載之雙軸延伸聚酯膜,利用連續接觸式厚度計跨越1m長所測定之縱向及橫向的厚度不均的值均為1%以上至10%以下。
- 一種包裝袋,係使用1層以上之如請求項1至5中任一項所記載之雙軸延伸聚酯膜而成。
- 一種標籤,係使用1層以上之如請求項1至5中任一項所記載之雙軸延伸聚酯膜而成。
- 一種雙軸延伸聚酯膜之製造方法,係用以製造如請求項1至5中任一項所記載之雙軸延伸聚酯膜;係以原料聚酯樹脂的極限黏度與聚酯膜的極 限黏度之差成為0.06dl/g以下之方式,將原料聚酯樹脂進行熔融擠出,繼而進行冷卻固化而獲得未延伸膜後,將前述未延伸膜進行雙軸延伸,繼而進行熱固定處理。
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