TWI725742B - 低收縮低寡聚物聚酯膜及其製造方法 - Google Patents
低收縮低寡聚物聚酯膜及其製造方法 Download PDFInfo
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Abstract
本發明公開一種低收縮低寡聚物聚酯膜及其製造方法,此製造方法包括:將至少一聚酯組合物形成一未延伸的聚酯厚片以及以2倍至6倍的延伸倍率對未延伸的聚酯厚片進行縱向(MD)與橫向(TD)延伸加工。聚酯組合物包含:94至99.974重量百分比的聚酯樹脂、0.01至1重量百分比的一級抗氧化劑、0.01至1重量百分比的二級抗氧化劑、0.003至2重量百分比的晶核劑以及0.003至2重量百分比的加工流動助劑,其中聚酯樹脂具有一介於0.60分升/克至0.80分升/克之間的固有黏度。
Description
本發明涉及一種聚酯膜,特別是涉及一種低收縮低寡聚物聚酯膜及其製造方法。
聚酯(如是聚對苯二甲酸乙二酯、聚2,6-萘二甲酸乙二酯等)在成型性、機械特性、熱特性、電氣特性及耐化學藥品性等方面都有不錯的表現,可作不同用途,例如光學膜、電氣絕緣膜、阻隔膜、離型膜、保護膜、農用地膜、包裝材料及隔熱膜。
然而,當聚酯膜作為裝置的一部分使用於高溫環境下,或於高溫環境下進行加工時,除了容易發生白化碎裂,以及發生明顯的熱收縮導致膜的尺寸不安定,甚至還會有大量寡聚物(oligomer)析出於膜的表面,這些情況都會造成聚酯膜在應用上受到限制。
本發明所要解決的技術問題在於,針對現有技術的不足提供一種低收縮低寡聚物聚酯膜,其能滿足在高溫環境下的應用需求;並且,提供一種製造方法用於製造此低收縮低寡聚物聚酯膜。
為了解決上述的技術問題,本發明所採用的其中一技術方案是,提供一種低收縮低寡聚物聚酯膜的製造方法,其包括將至少一聚酯組合物形成一未延伸的聚酯厚片以及以2倍至6倍的延伸倍率對所述未延伸的聚酯厚片進行縱向(MD)與橫向(TD)延伸加工。所述聚酯組合物包含:94至99.974重量百分比的聚酯樹脂、0.01至1重量百分比的一級抗氧化劑、0.01至1重量百分比的二級抗氧化劑、0.003至2重量百分比的晶核劑以及0.003至2重量百分比的加工流動助劑;其中聚酯樹脂具有一介於0.60分升/克至0.80分升/克之間的固有黏度。
在本發明的一實施例中,對所述雙軸延伸的聚酯膜進行橫向及/或縱向的預收縮。
在本發明的一實施例中,所述縱向(MD)延伸加工與所述橫向(TD)延伸加工是先後進行的,所述縱向(MD)延伸加工是在70
oC至145
oC的溫度下進行,且所述橫向(TD)延伸加工是在90
oC至160
oC的溫度下進行。
在本發明的一實施例中,所述縱向(MD)延伸加工與所述橫向(TD)延伸加工是在70
oC至160
oC的溫度下,使用2倍至6倍的延伸倍率同步進行的。
在本發明的一實施例中,所述低收縮低寡聚物聚酯膜的製造方法還包括在形成所述未延伸的聚酯厚片之前,以120
oC至180
oC的溫度對至少一所述聚酯組合物進行結晶乾燥處理。
在本發明的一實施例中,所述結晶乾燥處理的時間為3至8小時。
在本發明的一實施例中,所述聚酯組合物還進一步包含0.5至2重量百分比的滑劑粒子,其粒徑介於1微米至5微米之間。
在本發明的一實施例中,所述聚酯樹脂的固有黏度介於0.65分升/克至0.78分升/克之間。
為了解決上述的技術問題,本發明所採用的另外一技術方案是,提供一種低收縮低寡聚物聚酯膜,其包括一基底層以及至少一表皮層。至少一所述表皮層形成於所述基底層的至少一表面上,且所述基底層與至少一所述表皮層各為一聚酯組合物所形成;所述聚酯組合物包含:94至99.974重量百分比的聚酯樹脂、0.01至1重量百分比的一級抗氧化劑、0.01至1重量百分比的二級抗氧化劑、0.003至2重量百分比的晶核劑以及0.003至2重量百分比的加工流動助劑;其中聚酯樹脂具有一介於0.60分升/克至0.80分升/克之間的固有黏度。
在本發明的一實施例中,形成至少一所述表皮層的所述聚酯組合物還進一步包含0.02至0.5重量百分比的滑劑粒子,其粒徑介於1微米至5微米之間。
在本發明的一實施例中,所述聚酯樹脂的固有黏度介於0.65分升/克至0.78分升/克之間。
在本發明的一實施例中,所述低收縮低寡聚物聚酯膜的厚度介於15微米至350微米之間,至少一所述表皮層的厚度佔所述低收縮低寡聚物聚酯膜總厚度的2%至30%。
在本發明的一實施例中,所述低收縮低寡聚物聚酯膜在210
oC下的縱向(MD)與橫向(TD)收縮率均小於1%。
在本發明的一實施例中,所述低收縮低寡聚物聚酯膜的厚度介於15微米至350微米之間,且至少一所述表皮層的厚度佔所述低收縮低寡聚物聚酯膜的厚度的2%至30%。
在本發明的一實施例中,至少一所述表皮層的厚度佔所述低收縮低寡聚物聚酯膜的厚度的3%至20%。
在本發明的一實施例中,至少一所述表皮層的厚度佔所述低收縮低寡聚物聚酯膜的厚度的4%至15%。
本發明的其中一有益效果在於,本發明的低收縮低寡聚物聚酯膜,其能通過“基底層與表皮層各為一聚酯組合物所形成,其中聚酯組合物包含特定用量的聚酯樹脂、一級抗氧化劑、二級抗氧化劑、晶核劑及加工流動助劑,且聚酯樹脂具有一介於0.60分升/克至0.80分升/克之間的固有黏度”的技術方案,以在高溫環境下防止寡聚物析出於膜的表面。
本發明的低收縮低寡聚物聚酯膜的製造方法,其採用特定的延伸加工條件,並在進行延伸加工之前,對聚酯膜進行縱向預收縮與橫向預收縮;因此,所製成的聚酯膜在高溫環境下可具有非常低的縱向熱收縮率和橫向熱收縮率,霧度變化量(rHaze)也小於1%。
為使能更進一步瞭解本發明的特徵及技術內容,請參閱以下有關本發明的詳細說明與圖式,然而所提供的圖式僅用於提供參考與說明,並非用來對本發明加以限制。
聚酯膜的用途十分廣泛,考量機械、電氣和熱特性等方面,可作為電池(如汽車電池、燃料電池及鋰電池)用阻隔膜、壓合模具用脫模膜、耐高溫離型膜及熱壓用膜。因此,本發明提供能改善聚酯膜的耐熱性和尺寸安定性,且能抑制聚酯寡聚物析出的技術方案。
以下是通過特定的具體實施例來說明本發明所公開有關“低收縮低寡聚物聚酯膜及其製造方法”的實施方式,本領域技術人員可由本說明書所公開的內容瞭解本發明的優點與效果。本發明可通過其他不同的具體實施例加以施行或應用,本說明書中的各項細節也可基於不同觀點與應用,在不悖離本發明的構思下進行各種修改與變更。另外,本發明的附圖僅為簡單示意說明,並非依實際尺寸的描繪,事先聲明。以下的實施方式將進一步詳細說明本發明的相關技術內容,但所公開的內容並非用以限制本發明的保護範圍。
應當可以理解的是,雖然本文中可能會使用到“第一”、“第二”、“第三”等術語來描述各種元件或者信號,但這些元件或者信號不應受這些術語的限制。這些術語主要是用以區分一元件與另一元件,或者一信號與另一信號。另外,本文中所使用的術語“或”,應視實際情況可能包括相關聯的列出項目中的任一個或者多個的組合。
除非另外定義,否則本文中使用的所有技術及科學術語,都具有與本領域技術人員通常所理解含義相同的含義。當術語以單數形式出現時,涵蓋此術語的複數形式。
除非另有指示,否則本文中提到的所有百分比都為重量百分比。當提供一系列上、下限範圍時,涵蓋所提到的範圍的所有組合,如同明確列出各組合。
參閱圖1所示,本發明實施例的低收縮低寡聚物聚酯膜的製造方法,其包括:步驟S1,為計量混合步驟,將所需成分計量混合,得到至少一種聚酯組合物;步驟S2,為結晶乾燥步驟,以120
oC至180
oC之溫度對聚酯原料進行結晶乾燥處理;步驟S3,為熔融押出及冷卻成型步驟,將聚酯原料熔融押出後,流延冷卻定型,得到未延伸的聚酯厚片;以及步驟S4,為延伸加工步驟,對未延伸的聚酯厚片進行預熱及延伸後,再進行橫向及/或縱向的熱收縮(或稱“預收縮”)。
值得一提的是,聚酯組合物的配方能直接產生抑制聚酯寡聚物析出的技術效果,聚酯組合物包含94至99.974重量百分比的聚酯樹脂、0.01至1重量百分比的一級抗氧化劑、0.01至1重量百分比的二級抗氧化劑、0.003至2重量百分比的晶核劑以及0.003至2重量百分比的加工流動助劑。
進一步而言,聚酯樹脂可為一種以上的二元酸與一種以上的二元醇所形成。二元酸可為芳香族二元酸、脂環族二元酸或其組合;二元醇可為芳香族二元醇、脂肪族二元醇、脂環族二元醇或其組合。
芳香族二元酸的具體例包括:對苯二甲酸、間苯二甲酸、鄰苯二甲酸、萘二甲酸、二苯基碸二羧酸、二苯醚二羧酸、二苯基酮二羧酸、苯基茚滿二羧酸、間苯二甲酸磺酸鈉及二溴對苯二甲酸;脂環族二元酸的具體例包括:草酸、丁二酸、己二酸、壬二酸、癸二酸及二聚酸。二元醇可為芳香族二元醇、脂肪族二元醇、脂環族二元醇或其任意組合。
芳香族二元醇的具體例包括:萘二酚、2,2雙(4-羥基二苯基)丙烷、2,2-雙(4-羥基乙氧基苯基)丙烷、雙(4-羥基苯基)碸及對苯二酚;脂肪族二元醇的具體例包括:乙二醇、丙二醇、1,4-丁二醇、己二醇、新戊二醇及二乙二醇;脂環族二元醇的具體例包括:環己烷二甲醇及環己二醇。
在一些實施例中,聚酯樹脂可選自聚對苯二甲酸乙二酯(PET)、聚對苯二甲酸丙二醇酯(PPT)、聚對苯二甲酸丁二酯(PBT)、聚萘二甲酸乙二醇酯(PEN)、聚萘二甲酸丁二醇酯(PBN)、聚對苯二甲酸環己烷二甲醇酯(PCT)、聚碳酸酯(PC)或聚芳酯;優選的聚酯樹脂為PET。聚酯樹脂的固有黏度(intrinsic viscosity, IV)可介於0.60分升/克至0.80分升/克之間,優選為介於0.65分升/克至0.78分升/克之間,如此能減少聚酯樹脂於成型時受到的負荷(如環境負荷、外力負荷等),並且能減少剪切加工所產生的熱量,而避免樹脂發生熱分解。
一級抗氧化劑與二級抗氧化劑能很好地發揮協同作用,以提供更好的抗氧化效果。進一步而言,一級抗氧化劑能快速和過氧化自由基(peroxy radical, ROO•)發生反應,以終止自由基連鎖反應;二級抗氧化劑能與氫過氧化物(ROOH)反應,將其轉化為無自由基且無反應活性的產物。一級抗氧化劑可選自酚類化合物或胺類化合物,具體可舉出商標名為Irganox 1010、Irganox 1425、Irganox 245、Anox 1315、Anox PP18、Anox 20、Lowinox 1790、Lowinox TBM-68及Naugard 445的市售品;二級抗氧化劑可選自亞磷酸類化合物或硫酯類化合物,具體可舉出商標名為Sandostab P-EPQ、Irgafos 168及Naugard 412S的市售品。
晶核劑能提高總結晶度,使聚酯膜的耐熱性獲得改善;此外,晶核劑能促進結晶成長,使結晶大小微細化,減少大球晶產生,且可避免膜面脆化;晶核劑可為礦物材料、金屬氧化物、矽化合物、有機酸或無機酸的金屬鹽、芳香族磷酸酯金屬鹽、多元醇衍生物、磺醯亞胺化合物、玻璃粉末、金屬粉末或其任意組合。礦物材料的具體例包括:石墨、滑石及高嶺土;金屬氧化物的具體例包括:氧化鋅、氧化鋁及氧化鎂;矽化合物的具體例包括:氧化矽、矽酸鈣及矽酸鎂;有機酸或無機酸的金屬鹽的具體例包括:碳酸鎂、碳酸鈣、碳酸鈉、碳酸鉀等碳酸金屬鹽、硫酸鋇、硫酸鈣、苯甲酸鈉及對叔丁基苯甲酸鋁;磷酸酯金屬鹽可舉出芳香族磷酸酯金屬鹽;多元醇衍生物可舉出二亞苄基山梨醇;考量耐熱性,優選的晶核劑為無機材料。
加工流動助劑能有效降低熔融押出聚酯原料時的機械扭力,減少聚合物分子鏈斷鏈;加工流動助劑可為季戊四醇硬脂酸酯(PETS)或其類似物,其在高温下具有良好的熱稳定性、低揮發性和好的脱模和流動性能,且對部分結晶的聚酯有很好的成核作用。
聚酯組合物可進一步包含0.02至0.5重量百分比的滑劑粒子,滑劑粒子不僅能提高聚酯膜的耐熱性,還能阻礙寡聚物的流動性,進而防止寡聚物的析出於膜的表面;滑劑粒子的粒徑可介於1微米至5微米之間,優選為1.5微米。
以下,將進一步說明本發明的製造方法各步驟的實施細節。
步驟S1中,是將基底層與表皮層各自所需的一般聚酯粒與至少一種功能性改質劑(如晶核劑)聚酯粒計量並均勻混合,準備成基底層與表皮層的混合聚酯粒原料。此處功能性改質劑聚酯粒之功能性原料可由聚合製程中添加,也可/或由混練製程添加。
步驟S2為結晶乾燥步驟,是以120
oC至180
oC之溫度對聚酯原料(聚酯粒)進行結晶乾燥處理,使聚酯原料的含水量低於30 ppm;結晶乾燥處理的時間可為3至8小時,但不限於此。
步驟S3為熔融押出及冷卻成型步驟,是將聚酯原料熔融押出後,流延冷卻定型,得到未延伸的聚酯厚片。進一步而言,聚酯原料可通過單層押出或多層共押出的方式形成具有流動性的熔融物,此步驟可用雙螺桿壓出機實現,熔融物再於流延輥之間流延為膜狀並冷卻固化。然而,這些細節只是本實施例所提供可行的實施方式,而並非用以限定本發明。
步驟S4為延伸加工步驟,是對未延伸的聚酯厚片進行預熱及延伸後,再進行橫向及/或縱向的熱收縮;延伸加工方式可為逐次雙軸延伸加工或同步雙軸延伸加工。值得一提的是,在特定的延伸加工條件下,可完成聚酯膜的結晶配向,且聚酯膜在高溫環境下可具有非常低的縱向熱收縮率和橫向熱收縮率。
進一步而言,未延伸的聚酯厚片可以先在70
oC至145
oC的溫度下,使用2倍至6倍的延伸倍率進行縱向(或稱“長度方向”,MD)延伸加工,以形成單軸延伸的聚酯膜,再在90
oC至160
oC的溫度下,使用2倍至6倍的延伸倍率進行橫向(或稱“寬度方向”,TD)延伸加工,以形成雙軸延伸的聚酯膜;根據實際需要,可將縱向延伸加工與橫向延伸加工的順序反過來。聚酯膜的延伸加工可用習知的拉幅延伸機實現,但不限於此。
此外,也可對未延伸的聚酯厚片進行同步雙軸延伸加工。進一步而言,未延伸的聚酯厚片可在70
oC至160
oC的溫度下,使用2倍至6倍的延伸倍率同時進行縱向延伸加工與橫向延伸加工,以直接形成雙軸延伸的聚酯膜。
值得一提的是,步驟S4中進一步對雙軸延伸的聚酯膜進行橫向及/或縱向的熱收縮,能提高聚酯膜的結晶度及改善聚酯膜的收縮應力。進一步而言,上述熱收縮處理可使用夾具夾持聚酯膜的寬度方向或長度方向的兩端部,將聚酯膜反覆地拉伸和鬆弛,拉伸幅度可為500%,鬆弛幅度可為10%。藉此,能有效抑制聚酯膜在高溫下的熱收縮,即提高聚酯膜的熱尺寸安定性,而不需要在延伸加工後實施額外的熱處理。
參閱圖2及圖3所示,利用本發明的製造方法所製成的聚酯膜(下稱“低收縮低寡聚物聚酯膜”) 1,其可包括一基底層11及一形成於基底層11的一表面(如上表面)上的第一表皮層12,如圖2所示;或者,低收縮低寡聚物聚酯膜1可包括一基底層11、一形成於基底層11的一表面(如上表面)上的第一表皮層12及一形成於基底層11的相對另一表面(如下表面)上的第二表皮層13,如圖3所示。在一未繪示的實施例中,低收縮低寡聚物聚酯膜1也可為單層結構。
進一步而言,基底層11含有94至99.974重量百分比的聚酯樹脂、0.01至1重量百分比的一級抗氧化劑、0.01至1重量百分比的二級抗氧化劑、0.003至2重量百分比的晶核劑及0.003至2重量百分比的加工流動助劑;其中聚酯樹脂的固有黏度可介於0.60分升/克至0.80分升/克之間,優選為介於0.65分升/克至0.78分升/克之間。考量耐熱性和抑制寡聚物析出等方面,第一表皮層12/第二表皮層13除了上述成分外,還進一步含有0.02至0.5重量百分比的滑劑粒子;滑劑粒子的粒徑可介於1微米至5微米之間,優選為1.5微米。
低收縮低寡聚物聚酯膜1的厚度可介於15微米至350微米之間,其中第一表皮層12與第二表皮層13的厚度分別佔聚酯膜總厚度的2%至30%,優選為聚酯膜總厚度的3%至20%,且更優選為聚酯膜總厚度的4%至15%,如此對限制寡聚物移動到其表面及膜霧度均會有非常好的效果。若第一表皮層12/第二表皮層13的厚度佔比未達2%,則寡聚物很容易移動到膜的表面;一旦聚酯膜受熱,環狀低聚物將會大量析出於膜的表面,影響膜的外觀。若第一表皮層12/第二表皮層13的厚度佔比超出30%,雖對抑制寡聚物移動到其膜表面會有良好效果,但膜霧度會上升,造成透明性不足。
[特性評價]
實驗例1至5與比較例1至5的聚酯膜可依上述步驟S1至步驟S4製成,各步驟的加工條件如表1所示。這些聚酯膜都具有圖3所示的A/B/A三層結構,A表示表皮層,B表示基底層;其中各層的厚度,以及各層所含聚酯粒的固有黏度和功能性添加劑的濃度也如表1所示。測試這些聚酯膜的關鍵物性,相關的測試方法說明如下,其結果也如表1所示。
透光率及霧度測試:採用日商Tokyo Denshoku的霧度計(型號為TC-HIII DPK),依JIS K7705測試標準,測試實驗例1至5與比較例1至5的聚酯膜於加熱前後的透光率及霧度值,並計算這些聚酯膜的霧度變化量(rHaze);本測試使用烘箱進行加熱,加熱溫度為210
oC,加熱時間為3小時。
熱收縮性測試:將實驗例1至5與比較例1至5的聚酯膜裁成長寬15 cm Î 15 cm,置入210
oC烘箱3小時後,量測這些聚酯膜的長邊長度與寬邊長度,並計算這些聚酯膜於加熱前後的長邊長度與寬邊長度的變化量;將所得到的每一個長邊長度化量除以初始長度(即15 cm)再乘上100%,並將所得到的每一個寬邊長度化量除以初始寬度(即15 cm)再乘上100%,依此得到所有聚酯膜的縱向熱收縮率和橫向熱收縮率。
薄膜IV測試:以 SI Analytics AVSPRO3 IV測定儀分析。先將實驗例1至5與比較例1至5的聚酯膜,秤取樣品重量125 mg,置於100 ml的廣口瓶內。添加IV溶劑25 ml,於加熱板攪拌加熱,板溫溫度為122
oC,使聚酯膜完全溶解後量測。
表1
項目 | 比較例1 | 比較例2 | 比較例3 | 比較例4 | 比較例5 | |
薄膜 | 總厚度(μm) | 125 | 125 | 125 | 125 | 125 |
共押出結構 | A/B/A | A/B/A | A/B/A | A/B/A | A/B/A | |
各層厚度(μm) | 6/113/6 | 6/113/6 | 6/113/6 | 6/113/6 | 6/113/6 | |
A層 助劑用量 | 粒徑2 μm的 二氧化矽(ppm) | 1000 | 1000 | 1000 | 1000 | 1000 |
1級抗氧化劑(ppm) | - | 5000 | - | - | 5000 | |
2級抗氧化劑(ppm) | - | 5000 | - | - | 5000 | |
晶核劑(ppm) | - | - | 1500 | - | - | |
加工流動助劑(ppm) | - | - | - | 1500 | 1500 | |
B層 助劑用量 | 1級抗氧化劑(ppm) | - | 5000 | - | - | 5000 |
2級抗氧化劑(ppm) | - | 5000 | - | - | 5000 | |
晶核劑(ppm) | - | - | 1500 | - | - | |
加工流動助劑(ppm) | - | - | - | 1500 | 1500 | |
加工 條件 | 結晶乾燥溫度( oC)/時間(小時) | 140/4 | 140/4 | 140/4 | 140/4 | 140/4 |
押出機溫度( oC) | 295 | 295 | 295 | 295 | 295 | |
縱向延伸溫度( oC) | 94 | 94 | 94 | 94 | 94 | |
縱向延伸倍率 | 3.3 | 3.3 | 3.3 | 3.3 | 3.3 | |
橫向延伸溫度( oC) | 110 | 110 | 110 | 110 | 110 | |
橫向延伸倍率 | 4.0 | 4.0 | 4.0 | 4.0 | 4.0 | |
縱向預收縮(%) | - | - | - | - | - | |
橫向預收縮(%) | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | |
原料 | 聚酯粒平均IV | 0.8 | 0.8 | 0.8 | 0.8 | 0.8 |
薄膜 物性 | IV | 0.60 | 0.65 | 0.61 | 0.63 | 0.69 |
rIV | 0.2 | 0.15 | 0.19 | 0.17 | 0.11 | |
收縮率(MD)% | 2.0 | 1.98 | 1.99 | 2.00 | 1.58 | |
收縮率(TD)% | 1.02 | 1 | 1.01 | 1.01 | 0.92 | |
霧度(Haze)% | 1.65 | 1.55 | 1.55 | 1.62 | 1.55 | |
210 oC*3小時後的霧度(Haze%) | 15 | 12.5 | 10.21 | 14.2 | 8.92 | |
r霧度(rHaze%) | 13.35 | 10.95 | 8.66 | 12.58 | 7.37 | |
透光率(TT%) | 87 | 87.2 | 87.2 | 87.2 | 87.1 |
表2
項目 | 實驗例1 | 實驗例2 | 實驗例3 | 實驗例4 | 實驗例5 | |
薄膜 | 總厚度(μm) | 15 | 50 | 125 | 250 | 350 |
共押出結構 | A/B/A | A/B/A | A/B/A | A/B/A | A/B/A | |
各層厚度(μm) | 2/11/2 | 2/46/2 | 6/113/6 | 12/226/12 | 18/314/18 | |
A層 助劑用量 | 粒徑2 μm的 二氧化矽(ppm) | 1000 | 500 | 500 | 600 | 500 |
1級抗氧化劑(ppm) | 3000 | 8000 | 5000 | 1500 | 200 | |
2級抗氧化劑(ppm) | 3000 | 8000 | 5000 | 1500 | 200 | |
晶核劑(ppm) | 30 | 500 | 1500 | 3000 | 3000 | |
加工流動助劑(ppm) | 30 | 500 | 1500 | 3000 | 3000 | |
B層 助劑用量 | 1級抗氧化劑(ppm) | 3000 | 8000 | 5000 | 1500 | 200 |
2級抗氧化劑(ppm) | 3000 | 8000 | 5000 | 1500 | 200 | |
晶核劑(ppm) | 30 | 500 | 1500 | 3000 | 3000 | |
加工流動助劑(ppm) | 30 | 500 | 1500 | 3000 | 3000 | |
加工 條件 | 結晶乾燥溫度( oC)/時間(小時) | 140/4 | 140/4 | 140/4 | 140/4 | 140/4 |
押出機溫度( oC) | 295 | 295 | 295 | 295 | 295 | |
縱向延伸溫度( oC) | 90 | 92 | 94 | 95 | 95 | |
縱向延伸倍率 | 3.8 | 3.5 | 3.3 | 3.1 | 2.9 | |
橫向延伸溫度( oC) | 110 | 110 | 110 | 115 | 115 | |
橫向延伸倍率 | 4.5 | 4.3 | 4.0 | 3.5 | 3.3 | |
縱向預收縮(%) | 1.8 | 1.8 | 1.8 | 1.8 | 1.8 | |
橫向預收縮(%) | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | |
原料 | 聚酯粒平均IV | 0.75 | 0.73 | 0.74 | 0.78 | 0.79 |
薄膜 物性 | IV | 0.68 | 0.68 | 0.68 | 0.68 | 0.68 |
rIV | 0.07 | 0.05 | 0.06 | 0.1 | 0.11 | |
收縮率(MD)% | 0.75 | 0.85 | 0.82 | 0.45 | 0.42 | |
收縮率(TD)% | 0.65 | 0.68 | 0.72 | 0.42 | 0.36 | |
霧度(Haze%) | 0.42 | 0.6 | 1.5 | 2.65 | 3.25 | |
210 oC加熱3小時後的霧度(Haze%) | 0.85 | 1.05 | 2.1 | 3.2 | 3.9 | |
r霧度(rHaze%) | 0.43 | 0.45 | 0.6 | 0.55 | 0.65 | |
透光率(TT%) | 89.5 | 89.2 | 89.1 | 89.5 | 89 |
由上可知,實驗例1至5的聚酯膜配方包含一級抗氧化劑、二級抗氧化劑、晶核劑及加工流動助劑,可達到低寡聚物製品的最佳綜合相乘效果。
實驗例1至5的聚酯膜中,表皮層的組成能產生以下技術效果。聚酯樹脂原料具有一介於0.60dl/g至0.80dl/g之間的固有黏度;一級抗氧化劑與二級抗氧化劑的存在量各為0.01至1重量百分比,其能產生抗氧化協同效果,減少聚合物分子鏈斷鏈,以及減少寡聚物產生;晶核劑的存在量為0.003至2重量百分比,其能提高總結晶度,使聚酯膜的耐熱性獲得改善,以及阻礙寡聚物的流動,防止寡聚物的析出於膜的表面;此外,晶核劑也能促進結晶成長,使結晶大小微細化,減少大球晶產生,且可避免膜面脆化;加工流動助劑的存在量為0.003至2重量百分比,其能有效降低熔融押出聚酯原料時的機械扭力,減少聚合物分子鏈斷鏈。
實驗例的製品經縱向(MD)與橫向(TD)預收縮處理後,能提高結晶度,並釋放收縮應力。從實驗例可以看出,聚酯膜配方中添加有一級抗氧化劑、二級抗氧化劑、晶核劑及加工流動助劑四種添加劑,能有效防止聚酯膜寡聚物產生。搭配前述預收縮處理,所製得的膜經210
oC加熱3小時後,縱向(MD)與橫向(TD)收縮率均小於1%,霧度變化量(rHaze)也小於1%,實現了低收縮低寡聚物的效果。
實驗例1至5的聚酯膜含有晶核劑,其縱向熱收縮率和橫向熱收縮率明顯低於比較例的聚酯膜;並且,晶核劑的濃度愈高,聚酯膜的熱收縮率有愈低的趨勢。
比較例1的聚酯膜,未進行縱向預收縮處理,所製得的膜縱向(MD)收縮率與橫向(TD)收縮率明顯偏高(MD收縮率2.0%,TD收縮率1.02%)。此外,比較例1的聚酯膜配方無添加一級抗氧化劑、二級抗氧化劑、晶核劑及加工流動助劑等四種添加劑,所製得的膜經210
oC加熱3小時後,膜霧度變化量(rHaze)達13.35%,膜面明顯變霧。此外,聚酯膜製品耐熱性明顯不良,受熱後尺寸安定性差,無法利用。
比較例2的聚酯膜,未進行縱向預收縮處理,所製得的膜縱向(MD)收縮率與橫向(TD)收縮率明顯偏高(縱向收縮率1.98%、橫向收縮率1.0%)。此外,比較例2的聚酯膜配方僅添加一級抗氧化劑、二級抗氧化劑添加劑各5000 ppm,對耐熱效果改善幅度不明顯,所製得的膜經210
oC加熱3小時後,霧度變化量(rHaze)達10.95%,膜面明顯變霧。此外,聚酯膜製品耐熱性明顯不良,受熱後尺寸安定性差,應用範圍受限。
比較例3的聚酯膜,未進行縱向預收縮處理,所製得的膜縱向(MD)收縮率與橫向(TD)收縮率明顯偏高(縱向收縮率1.99%、橫向收縮率1.01%)。此外,比較例3的聚酯膜配方僅添加晶核劑1500 ppm,對耐熱效果改善幅度不明顯,所製得的膜經210
oC加熱3小時後,霧度變化量(rHaze)達8.66%,膜面明顯變霧。此外,聚酯膜製品耐熱性明顯不良,受熱後尺寸安定性差,應用範圍受限。
比較例4的聚酯膜,未進行縱向預收縮處理,所製得的膜縱向(MD)收縮率與橫向(TD)收縮率明顯偏高(縱向收縮率2.00%、橫向收縮率1.01%)。此外,比較例4的聚酯膜配方僅添加流動助劑1500 ppm,對耐熱效果改善幅度不明顯,所製得的膜經210
oC加熱3小時後,霧度變化量(rHaze)達12.58%,膜面明顯變霧。此外,聚酯膜製品耐熱性明顯不良,受熱後尺寸安定性差,應用範圍受限。
比較例5的聚酯膜,未進行縱向預收縮處理,所製得的膜縱向(MD)收縮率與橫向(TD)收縮率明顯偏高(縱向收縮率1.58%、橫向收縮率0.92%)。此外,比較例5的聚酯膜配方添加一級抗氧化劑、二級抗氧化劑添加劑各5000 ppm及加工流動助劑1500 ppm,對耐熱效果雖有改善,但仍不符生產需求,所製得的膜經210
oC加熱3小時後,霧度變化量(rHaze)達7.37%,膜面變霧情形略有改善。此外,聚酯膜製品耐熱性明顯不良,受熱後尺寸安定性差,應用範圍受限。
[實施例的有益效果]
本發明的其中一有益效果在於,本發明的低收縮低寡聚物聚酯膜,其能通過“基底層與表皮層各為一聚酯組合物所形成,其中聚酯組合物包含特定用量的聚酯樹脂、一級抗氧化劑、二級抗氧化劑、晶核劑及加工流動助劑,且聚酯樹脂具有一介於0.60分升/克至0.80分升/克之間的固有黏度”的技術方案,以在高溫環境下防止寡聚物析出於膜的表面。
本發明的低收縮低寡聚物聚酯膜的製造方法,其採用特定的延伸加工條件,並在進行延伸加工之前,對聚酯膜進行縱向預收縮與橫向預收縮;因此,所製成的聚酯膜在高溫環境下可具有非常低的縱向熱收縮率和橫向熱收縮率,霧度變化量(rHaze)也小於1%。
以上所公開的內容僅為本發明的優選可行實施例,並非因此侷限本發明的申請專利範圍,所以凡是運用本發明說明書及圖式內容所做的等效技術變化,均包含於本發明的申請專利範圍內。
1:低收縮低寡聚物聚酯膜
11:基底層
12:第一表皮層
13:第二表皮層
S1至S4:製造方法步驟
圖1為本發明的低收縮低寡聚物聚酯膜的製造方法的流程圖。
圖2為本發明的低收縮低寡聚物聚酯膜的其中一結構示意圖。
圖3為本發明的低收縮低寡聚物聚酯膜的另外一結構示意圖。
S1至S4:製造方法步驟
Claims (15)
- 一種低收縮低寡聚物聚酯膜的製造方法,其包括:將至少一聚酯組合物形成一未延伸的聚酯厚片,其中所述聚酯組合物包含:94至99.974重量百分比的聚酯樹脂,其具有一介於0.60分升/克至0.80分升/克之間的固有黏度;0.01至1重量百分比的一級抗氧化劑;0.01至1重量百分比的二級抗氧化劑;0.003至2重量百分比的晶核劑;以及0.003至2重量百分比的加工流動助劑;以及以2倍至6倍的延伸倍率對所述未延伸的聚酯厚片進行縱向(MD)與橫向(TD)延伸加工,形成一雙軸延伸的聚酯膜。
- 如請求項1所述的低收縮低寡聚物聚酯膜的製造方法,其還包括對所述雙軸延伸的聚酯膜進行橫向及/或縱向的預收縮。
- 如請求項1所述的低收縮低寡聚物聚酯膜的製造方法,其中,所述縱向(MD)延伸加工與所述橫向(TD)延伸加工是先後進行的,所述縱向(MD)延伸加工是在70℃至145℃的溫度下進行,且所述橫向(TD)延伸加工是在90℃至160℃的溫度下進行。
- 如請求項1所述的低收縮低寡聚物聚酯膜的製造方法,其中,所述縱向(MD)延伸加工與所述橫向(TD)延伸加工是在70℃至160℃的溫度下,使用2倍至6倍的延伸倍率同步進行的。
- 如請求項2所述的低收縮低寡聚物聚酯膜的製造方法,其還包括在形成所述未延伸的聚酯厚片之前,以120℃至180℃的溫度對至少一所述聚酯組合物進行結晶乾燥處理。
- 如請求項5所述的低收縮低寡聚物聚酯膜的製造方法,其中,所述結晶乾燥處理的時間為3至8小時。
- 如請求項1所述的低收縮低寡聚物聚酯膜的製造方法,其中,所述聚酯組合物還進一步包含滑劑粒子,其粒徑介於1微米至5微米之間。
- 如請求項1所述的低收縮低寡聚物聚酯膜的製造方法,其中,所述聚酯樹脂的固有黏度介於0.65分升/克至0.78分升/克之間。
- 一種低收縮低寡聚物聚酯膜,其包括:一基底層;以及至少一表皮層,形成於所述基底層的至少一表面上;其中,所述基底層與至少一所述表皮層各為一聚酯組合物所形成,所述聚酯組合物包含:94至99.974重量百分比的聚酯樹脂,其具有一介於0.60分升/克至0.80分升/克之間的固有黏度;0.01至1重量百分比的一級抗氧化劑;0.01至1重量百分比的二級抗氧化劑;0.003至2重量百分比的晶核劑;以及0.003至2重量百分比的加工流動助劑。
- 如請求項9所述的低收縮低寡聚物聚酯膜,其中,形成至少一所述表皮層的所述聚酯組合物還進一步包含滑劑粒子,其粒徑介於1微米至5微米之間。
- 如請求項9所述的低收縮低寡聚物聚酯膜,其中,所述聚酯樹脂的固有黏度介於0.65分升/克至0.78分升/克之間。
- 如請求項9所述的低收縮低寡聚物聚酯膜,其中,所述低收縮低寡聚物聚酯膜在210℃下的縱向(MD)與橫向(TD)收縮率均小於1%。
- 如請求項9所述的低收縮低寡聚物聚酯膜,其中,所述低收縮低寡聚物聚酯膜的厚度介於15微米至350微米之間,且至少一所述表皮層的厚度佔所述低收縮低寡聚物聚酯膜的厚度的2%至30%。
- 如請求項13所述的低收縮低寡聚物聚酯膜,其中,至少一所述表皮層的厚度佔所述低收縮低寡聚物聚酯膜的厚度的3%至20%。
- 如請求項14所述的低收縮低寡聚物聚酯膜,其中,至少一所述表皮層的厚度佔所述低收縮低寡聚物聚酯膜的厚度的4%至15%。
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