TWI677433B - 具有改善模數性質之多層膜 - Google Patents
具有改善模數性質之多層膜 Download PDFInfo
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- TWI677433B TWI677433B TW107110198A TW107110198A TWI677433B TW I677433 B TWI677433 B TW I677433B TW 107110198 A TW107110198 A TW 107110198A TW 107110198 A TW107110198 A TW 107110198A TW I677433 B TWI677433 B TW I677433B
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- 238000004519 manufacturing process Methods 0.000 claims abstract description 24
- 239000010410 layer Substances 0.000 claims description 88
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- KKEYFWRCBNTPAC-UHFFFAOYSA-N terephthalic acid group Chemical group C(C1=CC=C(C(=O)O)C=C1)(=O)O KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 46
- -1 bis-hydroxyethyl Chemical group 0.000 claims description 44
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- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 4
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- 239000005058 Isophorone diisocyanate Substances 0.000 description 3
- SJRJJKPEHAURKC-UHFFFAOYSA-N N-Methylmorpholine Chemical compound CN1CCOCC1 SJRJJKPEHAURKC-UHFFFAOYSA-N 0.000 description 3
- RWRDLPDLKQPQOW-UHFFFAOYSA-N Pyrrolidine Chemical compound C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 description 3
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- ORLQHILJRHBSAY-UHFFFAOYSA-N [1-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1(CO)CCCCC1 ORLQHILJRHBSAY-UHFFFAOYSA-N 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C13/00—Dental prostheses; Making same
- A61C13/0003—Making bridge-work, inlays, implants or the like
- A61C13/0022—Blanks or green, unfinished dental restoration parts
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C5/00—Filling or capping teeth
- A61C5/007—Dental splints; teeth or jaw immobilisation devices; stabilizing retainers bonded to teeth after orthodontic treatments
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0011—Combinations of extrusion moulding with other shaping operations combined with compression moulding
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
本發明有關一種具有改善模數性質之多層(較佳為共擠壓)塑膠模,其特別適合於製造三維成型物件。
Description
本發明有關一種具有改善模數性質之多層(較佳為共擠壓)塑膠模,其特別適合於製造三維成型物件,例如藉由熱成型方法。
針對數種應用,特別是醫學應用,主要興趣在於潮濕或濕氣環境存在中,已由形成塑膠模獲得之三維成型物件係穩定呈其三維形式。此外,大量需求於塑膠膜製作,特別有關其張力模數,因為成型物件再其使用期間必須運用充分張力。
過去,例如由多樣化熱塑性材料組成之單層膜已被用於潮濕或濕氣環境之應用,然而即使使用開始前之高張力模數,其在使用期間具有大幅降低此張力模數之缺點,以致未如計畫頻繁地獲得所欲使用成功,變得需要重做(reworking)三維成型物件。如此重做非常昂貴。
為了避免此缺點,因此存在需求製造三維成型物件之塑膠膜,該物件可減小在潮濕環境中使用期間張力模數之明顯下降。
構成本發明基礎之目的因此在於提供適合製造三維成型物件之塑膠膜,該物件可減小使用期間張力模數之明 顯下降。
驚人地,已發現多層(較佳為三層)塑膠膜消除上列缺點,其含有包括聚碳酸酯或共聚碳酸酯及/或聚酯或共聚酯之核心層,介於包括具有特殊性質的熱塑性聚胺基甲酸酯及/或聚酯或共聚酯之兩層。
本發明主題因此為一種多層塑膠膜,特徵在於-其具有核心層A,其含有具有玻璃轉移溫度Tg為80℃至200℃、較佳80℃至170℃、更佳80℃至150℃之至少一種聚碳酸酯或共聚碳酸酯及/或聚酯或共聚酯,-此核心層係座落介於兩個外層B間,其含有展現硬度為45蕭耳D至85蕭耳D之至少一種熱塑性聚胺基甲酸酯及/或聚酯或共聚酯。
玻璃轉移溫度Tg係根據標準DIN EN 61006藉助微差掃描熱量(DSC)於加熱速率20K/min測定,以Tg定義為中點溫度(正切方法)。
根據本發明較佳者,核心層A包括至少一種聚酯或共聚酯,其中聚酯或共聚酯之固有黏度總計為0.50dL/g至1.20dL/g且聚酯或共聚酯展現玻璃轉移溫度Tg為80℃至150℃。
固有黏度係在25℃下60/40(重量/重量)酚/四氯乙烷中於濃度0.5g/100ml測定。
根據本發明較佳者,兩個外層B包括展現硬度為45蕭耳D至85蕭耳D之至少一種熱塑性聚胺基甲酸酯。
在本發明較佳具體實例中,多層塑膠膜-具有核心層A,其含有具有固有黏度為0.50dL/g至1.20dL/g及玻璃轉移溫度Tg為80℃至150℃之至少一種聚酯或共聚酯,-此核心層係座落介於兩個外層B間,其含有展現硬度為 45蕭耳D至85蕭耳D之至少一種熱塑性聚胺基甲酸酯。
適合且較佳核心層A之聚酯或共聚酯為對酞酸或萘二羧酸之聚-或共聚縮合物,例如且較佳為聚-或共聚對酞酸乙二酯(PET或CoPET)、經乙二醇改質PET(PETG)或聚-或共聚對酞酸丁二酯(PBT或CoPBT)、聚-或共聚萘二甲酸乙二酯(PEN或CoPEN)。
適合且較佳核心層A之聚碳酸酯或共聚碳酸酯特別是具有平均分子量Mw為500至100,000、較佳10,000至80,000、特佳15,000至40,000之聚碳酸酯或共聚碳酸酯。
此外,含有至少一種如此聚碳酸酯或共聚碳酸酯之摻混物係對核心層A適合且較佳。上述聚碳酸酯或共聚碳酸酯與至少一種對酞酸之聚-或共聚縮合物的摻混物再者亦適合且較佳,特別是至少一種如此具有平均分子量Mw為10,000至200,000、較佳26,000至120,000的對酞酸之聚-或共聚縮合物。在發明特佳具體實例中,摻混物為聚碳酸酯或共聚碳酸酯與聚-或共聚對酞酸丁二酯之摻混物。如此聚碳酸酯或共聚碳酸酯與聚-或共聚對酞酸丁二酯之摻混物可較佳具有1至90重量%聚碳酸酯或共聚碳酸酯及99至10重量%聚-或共聚對酞酸丁二酯、較佳1至90重量%聚碳酸酯及99至10重量%聚對酞酸丁二酯,含量合計達100重量%。如此聚碳酸酯或共聚碳酸酯與聚-或共聚對酞酸丁二酯之摻混物可特佳具有20至85重量%聚碳酸酯或共聚碳酸酯及80至15重量%聚-或共聚對酞酸丁二酯、較佳20至85重量%聚碳酸酯及80至15重量%聚對酞酸丁二酯,含量合計達100重量%。如此聚碳酸酯或共聚碳酸酯與聚-或共聚對酞酸丁二酯之摻混物可非常特佳具有35至80重量%聚碳酸酯或共聚碳酸酯及65至20重量%聚-或共聚對酞酸丁二酯、較佳35至80重量%聚碳酸酯及65至20重量%聚對酞酸丁二酯,含量合計達100重量%。 在較佳具體實例中,特別適合聚碳酸酯或共聚碳酸酯為芳香族聚碳酸酯或共聚碳酸酯。
聚碳酸酯或共聚碳酸酯可為線型或以已知方式分支。
從二酚、碳酸衍生物、視情況鏈終止劑及視情況分支劑,可以已知方式進行製備此等聚碳酸酯。製備聚碳酸酯之細節已制定於許多專利說明書約40年。此處可參考舉例僅對Schnell,「Chemistry and Physics of Polycarbonates」,Polymer Reviews,第9卷,Interscience Publishers,紐約,倫敦,雪梨1964;對D.Freitag,U.Grigo,P.R.Müller,H.Nouvertne',BAYER AG,「Polycarbonates」於Encyclopedia of Polymer Science and Engineering,第11卷,第二版,1988,第648至718頁;及最後對Dres.U.Grigo,K.Kirchner與P.R.Müller「Polycarbonate」於Becker/Braun,Kunststoff-Handbuch,第3/1卷,Polycarbonate,Polyacetale,Polyester,Celluloseester,Carl Hanser Verlag慕尼黑,維也納1992,第117至299頁。
適合二酚可為例如通式(III)之二羥芳基化合物,HO-Z-OH (III)其中Z為具有6至34個C原子之芳香族基團,其可含有一或多個視情況經取代之芳香族核及脂族或環脂族基團或烷芳基或雜原子作為橋聯成員。
特佳二羥芳基化合物為間苯二酚、4,4’-二羥聯苯、雙-(4-羥苯基)-二苯基甲烷、1,1-雙-(4-羥苯基)-1-苯基乙烷、雙-(4-羥苯基)-1-(1-萘基)-乙烷、雙-(4-羥苯基)-1-(2-萘基)-乙烷、2,2-雙-(4-羥苯基)-丙烷、2,2-雙-(3,5-二甲基-4-羥苯基)-丙烷、1,1-雙-(4-羥苯基)-環己烷、1,1-雙-(3,5-二甲基-4-羥苯基)-環己烷、1,1-雙-(4-羥苯基)-3,3,5-三甲基-環己烷、1,1’-雙-(4-羥苯基)-3-二異丙基苯及1,1’-雙-(4-羥苯基)-4-二異丙基苯。
非常特佳二羥芳基化合物為4,4’-二羥聯苯、2,2-雙-(4-羥苯基)-丙烷及雙-(4-羥苯基)-3,3,5-三甲基環己烷。
非常特佳共聚碳酸酯可使用1,1-雙-(4-羥苯基)-3,3,5-三甲基環己烷及2,2-雙-(4-羥苯基)-丙烷製備。
適合碳酸衍生物可為例如光氣或通式(IV)之碳酸二芳酯
其中R、R’及R” 互相獨立為相同或不同且表示氫、線型或分支C1-C34-烷基、C7-C34-烷芳基或C6-C34-芳基,R可另外亦代表-COO-R’’’,其中R’’’表示氫、線型或分支C1-C34-烷基、C7-C34-烷芳基或C6-C34-芳基。
特佳二芳基化合物為碳酸二苯酯、碳酸4-第三丁苯-苯酯、碳酸二-(4-第三丁苯)酯、碳酸聯苯-4-基-苯酯、碳酸二-(聯苯-4-基)酯、碳酸4-(1-甲基-1-苯乙基)-苯-苯酯、碳酸二-[4-(1-甲基-1-苯乙基)-苯]酯及碳酸二-(柳酸甲酯)酯。
碳酸二苯酯為非常特別佳。
可使用一種碳酸二芳酯或不同碳酸二芳酯。
可額外地利用一或多種尚未用於製備所用碳酸二芳酯之單羥芳基化合物,例如作為鏈終止劑以控制或改變端基。此等可為通式(V)者
其中RA 表示線型或分支C1-C34-烷基、C7-C34-烷芳基、C6-C34-芳基或-COO-RD,其中RD表示氫、線型或分支C1-C34-烷基、C7-C34-烷芳基或C6-C34-芳基,且RB、RC 互相獨立為相同或不同且表示氫、線型或分支C1-C34-烷基、C7-C34-烷芳基或C6-C34-芳基。
4-第三丁酚、4-異辛酚及3-十五烷基酚為較佳。
適合分支劑可為具有三或多個官能基之化合物,較佳為具有三或多個羥基者。
較佳分支劑為3,3-雙-(3-甲基-4-羥苯基)-2-氧-2,3-二氫吲哚及1,1,1-參(4-羥苯基)-乙烷。
針對核心層A,聚-或共聚對酞酸烷二酯或聚-或共聚萘二甲酸烷二酯係適合於發明較佳具體實例中為對酞酸或萘二羧酸之聚-或共聚縮合物。適合聚-或共聚對酞酸烷二酯或聚-或共聚萘二甲酸烷二酯為例如芳香族二羧酸或其反應性衍生物(例如二甲酯或酐)與脂族、環脂族或芳脂族二醇之反應產物及此等反應產物之混合物。
如本文所用,術語「對酞酸」意欲包含與二醇有用於製作聚酯反應方法之對酞酸本身與其殘基以及對酞酸之任何衍生物,包含其關聯的醯鹵化物、酯、半酯、鹽、半鹽、酐、混合酐、或其混合物或殘基。在一項具體實例中,酯係選自至少一種下列:甲基、乙基、丙基、異丙基、及苯酯。在一項具體實例中,可使用對酞酸作為起始材料。在另外具體實例中,可使用對酞酸二甲酯作為起始材料。 在另外具體實例中,可使用對酞酸與對酞酸二甲酯之混合物作為起始材料及/或作為中間材料。
如本文所用,術語「萘二羧酸」意欲包含與二醇有用於製作聚酯反應方法之萘二羧酸本身與其殘基以及萘二羧酸之任何衍生物,包含其關聯的醯鹵化物、酯、半酯、鹽、半鹽、酐、混合酐、或其混合物或殘基。在一項具體實例中,酯係選自至少一種下列:甲基、乙基、丙基、異丙基、及苯酯。在一項具體實例中,可使用萘二羧酸作為起始材料。在另外具體實例中,可使用萘二羧酸的二甲酯作為起始材料。在另外具體實例中,可使用萘二羧酸與萘二羧酸的二甲酯之混合物作為起始材料及/或作為中間材料。
除了對酞酸或萘二羧酸外,有用於發明的聚-或共聚酯之二羧酸成分可視情況包括高至30莫耳%、較佳高至20莫耳%、更佳高至10莫耳%、最佳高至5莫耳%一或多種改質芳香族二羧酸。在較佳具體實例中,有用於發明的聚-或共聚酯之二羧酸成分包括高至1莫耳%一或多種改質芳香族二羧酸。又於另外較佳具體實例中,有用於發明的聚-或共聚酯之二羧酸成分包括0莫耳%改質芳香族二羧酸。因而,若存在,思忖一或多種改質芳香族二羧酸用量範圍可為任何此等先前端點數值,包含例如0.01至30莫耳%、較佳0.01至20莫耳%、更佳0.01至10莫耳%、最佳0.01至5莫耳%及在較佳具體實例中0.01至1莫耳%。在一項具體實例中,可用於本發明之改質芳香族二羧酸包含(但不限於)具有高至20個碳原子、較佳具有8至14個碳原子且可呈線型、對位定向(para-oriented)、或對稱者。可用於本發明之改質芳香族二羧酸實例包含(但不限於)酞酸、異酞酸、4,4’-聯苯基二羧酸、1,4-、1,5-、2,6-、2,7-萘二羧酸(於聚-或共聚對酞酸烷二酯情況)、對酞酸(於聚-或共聚萘二甲酸烷二酯情況)及反-4,4’-茋 二羧酸、及其酯。
有用於發明的共聚酯之羧酸成分可視情況以高至10莫耳%、例如高至5莫耳%或較佳高至1莫耳%一或多種含有2至16個碳原子之脂族二羧酸進一步改質,例如丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、栓酸、壬二酸、癸二酸、環己烷二乙酸及十二烷二酸二羧酸。又另外具體實例含有0莫耳%改質脂族二羧酸。因而,若存在,思忖一或多種改質脂族二羧酸用量範圍可為任何此等先前端點數值,包含例如0.01至10莫耳%及較佳0.1至10莫耳%。
較佳聚-或共聚對酞酸烷二酯或聚-或共聚萘二甲酸烷二酯含有至少70莫耳%、較佳至少80莫耳%乙二醇、丁烷二醇-1,4、2,2,4,4-四甲基-1,3-環丁烷二醇及/或1,4-環己烷二甲醇殘基,相對於二醇成分。
除了乙二醇、丁烷二醇-1,4、2,2,4,4-四甲基-1,3-環丁烷二醇及/或1,4-環己烷二甲醇殘基外,較佳聚-或共聚對酞酸烷二酯或聚-或共聚萘二甲酸烷二酯可含有高至30莫耳%、較佳高至20莫耳%具有3至12個C原子之其他脂族二醇基團或具有6至21個C原子之環脂族二醇基團,例如丙烷二醇-1,3、2-乙基丙烷二醇-1,3、新戊二醇、戊烷二醇-1,5、己烷二醇-1,6、環己烷二甲醇-1,4、3-甲基戊烷二醇-2,4、2-甲基戊烷二醇-2,4、2,2,4-三甲基戊烷二醇-1,3與2-乙基己烷二醇-1,6、2,2-二乙基丙烷二醇-1,3、己烷二醇-2,5、1,4-二-(β-羥乙氧基)-苯、2,2-雙-(4-羥環己基)-丙烷、2,4-二羥基-1,1,3,3-四甲基環丁烷、2,2-雙-(3-β-羥乙氧基苯基)-丙烷及2,2-雙-(4-羥丙氧基苯基)-丙烷之基團(參見DE-OS 24 07 674、24 07 776、27 15 932)。
本發明聚-或共聚酯可包括0至10莫耳%、例如0.01至5莫耳%(分別以二醇或二酸殘基之總莫耳百分率為基準)一或多種具有3或多個羧取代基、羥取代基、或其組 合之分支單體(本文亦稱為分支劑)殘基。在某些具體實例中,在聚-或共聚酯聚合之前及/或期間及/或之後可添加分支單體或分支劑。有用於發明的聚-或共聚酯因而可呈線型或分支。在較佳具體實例中,有用於發明的聚-或共聚酯呈線型且因而不含有如此分支劑。
若存在,分支單體實例包含(但不限於)多官能酸或多官能醇,例如苯偏三酸、苯偏三酸酐、焦蜜石酸二酐、三羥甲基丙烷、甘油、新戊四醇、檸檬酸、酒石酸、3-羥戊二酸及類似者。在一項具體實例中,分支單體殘基可包括0.1至0.7莫耳%一或多種選自至少一種下列殘基:苯偏三酸酐、焦蜜石酸二酐、甘油、山梨醇、1,2,6-己烷三醇、新戊四醇、三羥甲基乙烷、及/或1,3,5-苯三甲酸。分支單體可與共聚酯呈敘述例如於U.S.專利號5,654,347及5,696,176的濃縮物形式而被添加於共聚酯反應混合物或摻混物。
較佳聚-或共聚對酞酸烷二酯或聚-或共聚萘二甲酸烷二酯含有至少70莫耳%、較佳至少80莫耳%對酞酸或萘二羧酸殘基(相對於二羧酸成分),及至少70莫耳%、較佳至少80莫耳%乙二醇、丁烷二醇-1,4、2,2,4,4-四甲基-1,3-環丁烷二醇及/或1,4-環己烷二甲醇殘基(相對於二醇成分)。
在特佳具體實例中,核心層A包括僅從對酞酸及其反應性衍生物(例如其二烷酯)與乙二醇及/或丁烷二醇-1,4製造之至少一種共聚酯。
在另外特佳具體實例中,核心層A包括聚碳酸酯或共聚碳酸酯與聚-或共聚對酞酸丁二酯之至少一種摻混物,具1至90重量%聚碳酸酯或共聚碳酸酯及99至10重量%聚-或共聚對酞酸丁二酯,較佳具35至80重量%聚碳酸酯及65至20重量%聚對酞酸丁二酯,含量總計達100重量%。
在本發明另外特佳具體實例中,核心層A包括至少 一種展現來自以下殘基之共聚酯(a)二羧酸成分,包括i)70莫耳%至100莫耳%對酞酸殘基,ii)0莫耳%至30莫耳%具有高至20個碳原子之芳香族二羧酸殘基,及iii)0莫耳%至10莫耳%具有高至16個碳原子之脂族二羧酸殘基,及(b)二醇成分,包括i)5莫耳%至50莫耳%2,2,4,4-四甲基-1,3-環丁烷二醇殘基,及ii)50莫耳%至95莫耳%1,4-環己烷二甲醇殘基,其中二羧酸成分殘基i)至iii)之莫耳%總合總計為100莫耳%,且二醇成分殘基i)及ii)之莫耳%總合總計為100莫耳%。
兩個外層B較佳包括展現硬度為45蕭耳D至85蕭耳D之至少一種熱塑性聚胺基甲酸酯。
特佳如此至少一種熱塑性聚胺基甲酸酯係從以下可獲得a)一或多種線型聚醚二醇,其具有平均分子量500g/mol至10,000g/mol、較佳500g/mol至6000g/mol,且各情況中平均至少1.8及至多3.0、較佳1.8至2.2Tserevitinov活性氫原子,b)一或多種有機二異氰酸酯,c)一或多種二醇鏈伸長劑,其具有分子量60g/mol至500g/mol且具有平均1.8至3.0 Tserevitinov活性氫原子,於以下存在d)視情況一或多種觸媒,添加以下 e)視情況輔助物質及添加劑,其中b)中NCO基團與a)及c)中對異氰酸酯呈反應性的基團之莫耳比率總計為0.85:1至1.2:1、較佳0.9:1至1.1:1。
在本申請案特佳具體實例中,多層塑膠膜特徵在於-其具有核心層A,其含有至少一種展現來自以下殘基之共聚酯(a)二羧酸成分,包括i)70莫耳%至100莫耳%對酞酸殘基,ii)0莫耳%至30莫耳%具有高至20個碳原子之芳香族二羧酸殘基,及iii)0莫耳%至10莫耳%具有高至16個碳原子之脂族二羧酸殘基,及(b)二醇成分,包括i)5莫耳%至50莫耳%2,2,4,4-四甲基-1,3-環丁烷二醇殘基,及ii)50莫耳%至95莫耳%1,4-環己烷二甲醇殘基,其中二羧酸成分殘基i)至iii)之莫耳%總合總計為100莫耳%,且二醇成分殘基i)及ii)之莫耳%總合總計為100莫耳%,且其中共聚酯之固有黏度總計為0.50dL/g至1.20dL/g且共聚酯展現玻璃轉移溫度Tg為80℃至150℃,-此核心層係座落介於含有至少一種熱塑性聚胺基甲酸酯之兩個外層B間,熱塑性聚胺基甲酸酯展現硬度為45蕭耳D至85蕭耳D,且從以下可獲得a)一或多種線型聚醚二醇,其具有平均分子量500g/mol至10,000g/mol、較佳500g/mol至6000g/mol,且各情況中平均至少1.8及至多3.0、較佳1.8至2.2 Tserevitinov活性氫原子, b)一或多種有機二異氰酸酯,c)一或多種二醇鏈伸長劑,其具有分子量60g/mol至500g/mol且具有平均1.8至3.0 Tserevitinov活性氫原子,於以下存在d)視情況一或多種觸媒,添加以下e)視情況輔助物質及添加劑,其中b)中NCO基團與a)及c)中對異氰酸酯呈反應性的基團之莫耳比率總計為0.85:1至1.2:1、較佳0.9:1至1.1:1。
根據本發明膜驚人地在潮濕或濕氣條件下展現清楚較小的張力模數降低。再者,由如此根據本發明膜製成之三維成型物件係在如此條件下穩定呈其三維外形。
熱塑性聚胺基甲酸酯(TPU)多數從線型多元醇(巨二醇)如聚酯二醇、聚醚二醇或聚碳酸酯二醇、有機二異氰酸酯及短鏈多數二官能醇(鏈伸長劑)構成。其等可被連續或不連續製造。多數熟知製造方法為帶方法(GB-A 1,057,018)及擠壓機方法(DE-A 1 964 834)。
根據發明較佳利用之熱塑性聚胺基甲酸酯為由前述之下者形成之反應產物
a)聚醚二醇
b)有機二異氰酸酯
c)鏈伸長劑。
作為二異氰酸酯b),可使用芳香族、脂族、芳脂族、雜環及環脂族二異氰酸酯或此等二異氰酸酯的混合物(參見HOUBEN-WEYL「Methoden der organischen Chemie」,第E20卷「Makromolekulare Stoffe」,Georg Thieme Verlag,Stuttgart,New York 1987,第1587至1593頁或「Justus Liebigs Annalen der Chemie」,562,第75至136頁)。
詳言之,下列以示範方式提及:脂族二異氰酸酯,例如六亞甲基二異氰酸酯;環脂族二異氰酸酯,例如異佛酮二異氰酸酯、1,4-環己烷二異氰酸酯、1-甲基-2,4-環己烷二異氰酸酯與1-甲基-2,6-環己烷二異氰酸酯及亦對應異構物混合物、4,4’-二環己基甲烷二異氰酸酯、2,4’-二環己基甲烷二異氰酸酯與2,2’-二環己基甲烷二異氰酸酯及亦對應異構物混合物;芳香族二異氰酸酯,例如2,4-甲苯二異氰酸酯、由2,4-甲苯二異氰酸酯與2,6-甲苯二異氰酸酯組成之混合物、4,4’-二苯基甲烷二異氰酸酯、2,4’-二苯基甲烷二異氰酸酯與2,2’-二苯基甲烷二異氰酸酯、由2,4’-二苯基甲烷二異氰酸酯與4,4’-二苯基甲烷二異氰酸酯組成之混合物、經胺基甲酸酯改質液體4,4’-二苯基甲烷二異氰酸酯與2,4’-二苯基甲烷二異氰酸酯、4,4’-二異氰酸基二苯基乙烷-(1,2)及1,5-伸萘基二異氰酸酯。優先使用1,6-六亞甲基二異氰酸酯、異佛酮二異氰酸酯、二環己基甲烷-4,4’-二異氰酸酯、具4,4’-二苯基甲烷二異氰酸酯含量超過96重量%之二苯基甲烷二異氰酸酯異構物混合物,特別是4,4’-二苯基甲烷二異氰酸酯及1,5-伸萘基二異氰酸酯。陳述的二異氰酸酯可個別或互相呈混合物形式而找到應用。其等亦可與高至15重量%(就二異氰酸酯總量而言計算)聚異氰酸酯一起使用,例如三苯基甲烷-4,4’,4”-三異氰酸酯或聚苯基-聚亞甲基聚異氰酸酯。
在有機二異氰酸酯b)情況中,較佳討論一或多種選自含有4,4’-二苯基甲烷二異氰酸酯、異佛酮二異氰酸酯、二環己基甲烷-4,4’-二異氰酸酯及1,6-六亞甲基二異氰酸酯群組之異氰酸酯。
Tserevitinov活性聚醚二醇a)為具有平均至少1.8及至多3.0、較佳1.8至2.2 Tserevitinov活性氫原子者。
根據Tserevitinov發現之方法,以甲基鎂鹵化物轉化生成甲烷且鍵結至N、O或S之所有氫原子被定名為 Tserevitinov活性氫原子。在Tserevitinov反應後舉行測定,藉以將甲基碘化鎂用欲調查的化合物轉化,且與酸性氫反應形成鎂鹽及對應烴。藉由氣體容量分析測定產生的甲烷。
由一或多種在伸烷殘基具有2至4個碳原子之環氧烷用含有兩個活性氫原子呈鍵結形式之起始物分子轉化,可製造適合如此聚醚二醇。作為環氧烷,下列提及例如:環氧乙烷、1,2-環氧丙烷、表氯醇、1,2-環氧丁烷及2,3-環氧丁烷。環氧烷可個別、替代呈接續或呈混合物使用。作為起始物分子,考慮例如:水,胺基醇例如N-烷基二乙醇胺(例如N-甲基二乙醇胺),及二醇例如乙二醇、1,3-丙二醇、1,4-丁烷二醇與1,6-己烷二醇。視情況,亦可利用起始物分子之混合物。適合聚醚二醇再者為四氫呋喃及/或1,3-丙二醇之含羥基聚合產物。亦可利用呈比例0重量%至30重量%的三官能聚醚(相對於雙官能聚醚),但至多呈產生的產物仍為熱塑性可工作之如此量。
聚醚二醇優先擁有數量平均分子量Mn為500g/mol至8000g/mol、特佳500g/mol至6000g/mol。其等可個別或互相呈混合物形式兩者而找到應用。
數量平均分子量Mn可用端基測定,例如根據ASTM D4274測定羥基數目。
Tserevitinov活性鏈伸長劑c)係所謂鏈伸長試劑,且擁有平均1.8至3.0 Tserevitinov活性氫原子,並具有數量平均分子量60g/mol至500g/mol。除了展現胺基、硫醇基或羧基外,如此試劑可理解為具有二至三個(較佳二個)羥基者。具有二至三個(較佳二個)羥基之羥基化合物係特佳作為鏈伸長劑。
經由鏈伸長試劑利用者為例如且較佳具有分子量60g/mol至500g/mol之二醇或二胺,優先具有2至14個碳原子之脂族二醇,例如乙烷二醇、1,2-丙烷二醇、1,3- 丙烷二醇、1,4-丁烷二醇、2,3-丁烷二醇、1,5-戊烷二醇、1,6-己烷二醇、二乙二醇及二丙二醇。然而,亦適合者為對酞酸與具2至4個碳原子的二醇之二酯,例如對酞酸-雙-乙二醇或對酞酸-雙-1,4-丁烷二醇;氫醌之羥伸烷醚,例如1,4-二(β-羥乙基)氫醌;乙氧基化雙酚,例如1,4-二(β-羥乙基)雙酚A;(環)脂族二胺,例如異佛酮二胺、伸乙二胺、1,2-伸丙二胺、1,3-伸丙二胺、N-甲基伸丙基-1,3-二胺、N,N’-二甲基伸乙二胺;及芳香族二胺,例如2,4-甲苯二胺、2,6-甲苯二胺、3,5-二乙基-2,4-甲苯二胺或3,5-二乙基-2,6-甲苯二胺或一級經單-、二-、三-或四烷基取代的4,4’-二胺基二苯基甲烷。作為鏈伸長劑,特佳使用1,2-乙二醇、1,2-丙烷二醇、1,3-丙烷二醇、1,4-丁烷二醇、1,6-己烷二醇、1,4-二(β-羥乙基)氫醌或1,4-二(β-羥乙基)雙酚A。亦可利用前述鏈伸長劑之混合物。此外,亦可添加相當小量的三醇。
數量平均分子量Mn可用端基測定,例如根據ASTM D4274測定羥基數目。
在鏈伸長劑c)情況中,較佳討論一或多種選自含有1,4-丁烷二醇、1,3-丙烷二醇、1,2-丙烷二醇、1,2-乙二醇、1,6-己烷二醇、1,4-二(β-羥乙基)氫醌及1,4-二(β-羥乙基)雙酚A群組者。
a)及c)中對異氰酸酯呈反應性基團特別為含Tserevitinov活性氫原子的基團。
較佳如此選擇化合物a)及c)之相對量以致b)中異氰酸酯基總和與a)及c)中Tserevitinov活性氫原子總和之比率總計為0.85:1至1.2:1、特佳0.9:1至1.1:1。
根據發明利用之熱塑性聚胺基甲酸酯可視情況含有觸媒d)。適合觸媒係根據技藝發展水平已知且傳統之三級胺例如三乙胺、二甲基環己胺、N-甲基嗎啉、N,N’-二甲基哌、2-(二甲胺基乙氧基)乙醇、二吖雙環[2,2,2]辛烷與 相似者,及亦特別是有機金屬化合物例如鈦酸酯、鐵化合物或錫化合物,例如二乙酸錫、二辛酸錫、二月桂酸錫、或脂族羧酸的二烷基錫鹽,例如二乙酸二丁基錫或二月桂酸二丁基錫或相似者。較佳觸媒為有機金屬化合物,特別是鈦酸酯、鐵化合物及錫化合物。熱塑性聚胺基甲酸酯中觸媒總量通常總計約0重量%至5重量%、較佳0重量%至2重量%,相對於TPU總重。
根據發明利用之熱塑性聚胺基甲酸酯(TPU)可視情況含有0重量%高達至多20重量%、較佳0重量%至10重量%作為輔助物質及添加劑e)(相對於TPU總重)之傳統輔助物質及添加劑。典型輔助物質及添加劑為顏料、染料、阻燃劑、抗老化與天候影響的穩定劑、塑化劑、滑動添加劑、脫模劑、鏈終止劑、抑真菌與抑菌作用的物質及亦填料及其混合物。
作為如此添加劑,尤其是與異氰酸酯有關之單官能化合物可較佳以比例高至2重量%利用(相對於熱塑性聚胺基甲酸酯總重),如所謂鏈終止劑或脫模助劑。適合者為例如單胺如丁胺與二丁胺、辛胺、硬脂胺、N-甲基硬脂胺、吡咯啶、哌啶或環己胺,單醇如丁醇、2-乙基己醇、辛醇、十二烷醇、硬脂醇、各種戊醇、環己醇及乙二醇單甲醚。
進一步添加劑實例為滑動添加劑(例如脂肪酸酯、其金屬皂、脂肪酸醯胺、脂肪酸酯醯胺及聚氧氧化合物)、抗結塊劑、抑制劑、抗水解、光、熱與變色的穩定劑、阻燃劑、染料、顏料、無機及/或有機填料(例如聚碳酸酯)、及亦塑化劑及增強劑。增強劑特別為纖維增強物質,例如根據技藝發展水平製造且亦可已經受篩分材料之無機纖維。有關陳述輔助物質及添加劑之進一步特點可從專家文獻收集,例如從J.H.Saunders與K.C.Frisch以「High Polymers」為標題之專題論文,第XVI卷,Polyurethanes:Chemistry and Technology,Parts 1 and 2,Interscience Publishers 1962與1964;從R.Gächter u.H.Müller之Taschenbuch der Kunststoff-Additive(Hauser Verlag Munich 1990);或從DE-A 29 01 774。
根據發明利用之熱塑性聚胺基甲酸酯較佳展現硬度為50蕭耳D至80蕭耳D。根據DIN EN ISO 868測定蕭耳硬度。
根據發明利用之熱塑性聚胺基甲酸酯可於所謂擠壓機方法中(例如於多軸擠壓機)或於所謂帶方法中連續製造。進行計量供給TPU成分a)、b)及c)可為同時(亦即於單發(one-shot)方法中)或接續(亦即藉助預聚物方法)。預聚物方法為特別佳。關於此點,製造預聚物可藉由批次及連續兩者裝填於部分擠壓機中或於分開的上游預聚物組件中,例如於靜態混合器反應器,例如Sulzer混合器。
較佳聚酯或共聚酯(特別是根據發明利用之共聚酯)較佳展現玻璃轉移溫度Tg為85℃至130℃、特佳90℃至120℃。
聚酯或共聚酯(特別是根據發明利用之共聚酯)較佳展現固有黏度為0.50dL/g至0.80dL/g。
本發明使用之較佳共聚酯典型可藉由對酞酸及視情況一或多種額外二官能羧酸及/或多官能羧酸(下文稱為二羧酸成分)與至少兩種二官能羥基化合物2,2,4,4-四甲基-1,3-環丁烷二醇及1,4-環己烷二甲醇及視情況額外二官能羥基化合物及/或多官能羥基化合物(下文稱為二醇成分)之反應而製備。典型二羧酸成分可為一或多種二羧酸,二醇成分可為二或多種二元醇/二醇。二羧酸與二元醇/二醇較佳呈大體相等比例反應,且被併入共聚酯聚合物作為其等對應殘基。根據本發明使用之共聚酯因此可含有大體相等莫耳比例的酸殘基與二醇殘基。
如本文所用,術語「殘基」意指透過聚縮合及/或酯 化反應從對應單體併入聚合物之任何有機結構。
二羧酸殘基可衍生自二羧酸單體或其關聯的醯鹵化物、酯、鹽、酐、或其混合物。因此如本文所用,術語「二羧酸」意欲包含與二醇有用於製作(共)聚酯反應方法之二羧酸及二羧酸之任何衍生物,包含其關聯的醯鹵化物、酯、半酯、鹽、半鹽、酐、混合酐、或其混合物。
在特佳具體實例中,二羧酸成分包括70至100莫耳%對酞酸殘基、較佳80至100莫耳%對酞酸殘基、更佳90至100莫耳%對酞酸殘基、最佳95至100莫耳%對酞酸殘基。在特佳具體實例中,二羧酸成分包括98至100莫耳%對酞酸殘基。在另外特佳具體實例中,二羧酸成分包括100莫耳%對酞酸殘基。
二羧酸成分之總莫耳%為100莫耳%。
可使用改質二羧酸之酯及/或鹽以取代二羧酸。二羧酸酯之適合實例包含(但不限於)二甲基、二乙基、二丙基、二異丙基、二丁基、及二苯基酯。在一項具體實例中,酯係選自至少一種下列:甲基、乙基、丙基、異丙基、及苯基酯。
來自共聚酯二醇成分的2,2,4,4-四甲基-1,3-環丁烷二醇殘基與1,4-環己烷二甲醇殘基之比率總計為10莫耳%至35莫耳%2,2,4,4-四甲基-1,3-環丁烷二醇殘基與65莫耳%至90莫耳%1,4-環己烷二甲醇殘基、特佳15莫耳%至35莫耳%2,2,4,4-四甲基-1,3-環丁烷二醇殘基與65莫耳%至85莫耳%1,4-環己烷二甲醇殘基、相當特佳15莫耳%至30莫耳%2,2,4,4-四甲基-1,3-環丁烷二醇殘基與70莫耳%至85莫耳%1,4-環己烷二甲醇殘基,藉以此等二醇成分的兩種成分之莫耳%總和總計為100莫耳%。
在特佳具體實例中,共聚酯之二醇成分可含有25莫耳%或更少並非2,2,4,4-四甲基-1,3-環丁烷二醇或1,4-環己烷二甲醇之一或多種改質二醇。在一項具體實例中,有 用於發明之共聚酯可含有15莫耳%或更少一或多種改質二醇。在另外具體實例中,有用於發明之共聚酯可含有10莫耳%或更少一或多種改質二醇。在另外具體實例中,有用於發明之共聚酯可含有5莫耳%或更少一或多種改質二醇。在另外具體實例中,有用於發明之共聚酯可含有3莫耳%或更少一或多種改質二醇。在另外具體實例中,有用於發明之共聚酯可含有0莫耳%或更少一或多種改質二醇。某些具體實例亦可含有0.01或更多莫耳%、例如0.1或更多莫耳%、1或更多莫耳%、5或更多莫耳%、或10或更多莫耳%一或多種改質二醇。因而,若存在,思忖一或多種改質二醇用量範圍可為任何此等先前端點數值,包含例如0.01至15莫耳%及較佳0.1至10莫耳%。
有用於發明共聚酯之改質二醇涉及異於2,2,4,4-四甲基-1,3-環丁烷二醇及1,4-環己烷二甲醇之二醇且可含有2至16個碳原子。適合改質二醇實例包含(但不限於)乙二醇、1,2-丙烷二醇、1,3-丙烷二醇、新戊二醇、1,4-丁烷二醇、1,5-戊烷二醇、1,6-己烷二醇、對-二甲苯二醇、或其混合物。較佳改質二醇(若存在)為乙二醇、1,3-丙烷二醇及/或1,4-丁烷二醇。
各二醇2,2,4,4-四甲基-1,3-環丁烷二醇或1,4-環己烷二甲醇可為順式、反式、或其混合物。
針對所欲共聚酯,順式/反式2,2,4,4-四甲基-1,3-環丁烷二醇之莫耳比率可從各自純的形式或其混合物改變。在某些具體實例中,順式及/或反式2,2,4,4-四甲基-1,3-環丁烷二醇之莫耳百分率係大於50莫耳%順式及小於50莫耳%反式,或大於55莫耳%順式及小於45莫耳%反式,或30至70莫耳%順式及70至30莫耳%反式,或40至60莫耳%順式及60至40莫耳%反式,其中順-及反-2,2,4,4-四甲基-1,3-環丁烷二醇之莫耳百分率總和係等於100莫耳%。
針對所欲共聚酯,1,4-環己烷二甲醇之莫耳比率可從各自純的形式或其混合物改變。藉由使用順式及反式之混合物,順/反1,4-環己烷二甲醇之莫耳比率範圍可於50/50至0/100內改變,例如介於40/60至20/80。
有用於發明之聚-或共聚酯可藉由文獻已知之方法製作,例如藉由在均質溶液中之方法、藉由在熔融中之轉酯化方法、及藉由兩相介面方法。適合方法包含(但不限於)使一或多種二羧酸與一或多種二醇於溫度100℃至315℃及壓力0.13mbar至1011mbar(0.1至760mmHg)下反應足夠形成聚酯之時間的步驟。針對製造(共)聚酯之方法,參見U.S.專利號3,772,405或Kunststoff-Handbuch,第VIII卷,p.695 ff,Karl-Hanser-Verlag,Munich 1973。
有用於發明之適合聚碳酸酯或共聚碳酸酯係商業可得,例如商標名來自Bayer MaterialScience AG之Makrolon®。有用於發明之適合聚酯或共聚酯亦係商業可得,例如商標名來自SK Chemical之Skygreen或來自Eastman Chemical Company之TritanTM。有用於發明之適合熱塑性聚胺基甲酸酯亦係商業可得,如來自Bayer MaterialScience AG。
根據本發明塑膠膜較佳展現總厚度為300μm至2000μm、特佳400μm至1500μm、相當特佳500μm至1200μm。
根據本發明塑膠膜情況下,在較佳具體實例中,討論由核心層A介於兩個外層B間組成之三層膜。
此根據本發明塑膠膜之較佳具體實例顯露介於核心層A(特佳為共聚酯核心層A)與外層B(特佳為TPU外層B)間之優異黏著性。此等層間之良好黏著性係特別有利且必要,因為塑膠膜於其潮濕或濕氣環境使用期間之剝層係不受歡迎。再者,於製造三維成型物件後,例如使根據本發明膜熱成形並修整切割邊緣,必須碾磨物件。而且 在此碾磨方法期間,個別層之剝層係不受歡迎。
介於核心層A與外層B間之黏著力較佳總計超過0.3N/mm、較佳超過0.5N/mm。黏著力可根據ASTM D 903 98測定。
根據本發明塑膠膜之核心層A較佳展現層厚250μm至1600μm、特佳350μm至1400μm、相當特佳400μm至1000μm。根據本發明塑膠膜之外層B較佳於各情況中展現層厚25μm至500μm、特佳30μm至300μm、相當特佳50μm至200μm。
針對若干應用,如針對醫學應用,尤其亦想要製造成型物件之膜於使用期間儘可能地不顯眼。因此若塑膠膜儘可能地透明,則更為有利。此需求同樣由根據本發明膜而滿足。
根據本發明塑膠膜較佳展現可見光於波長範圍380nm至780nm之穿透率超過70%、特佳超過80%。穿透率可根據ASTM D 1003測定,例如用Hunter Associates Laboratory Inc製造之Ultra Scan XE。
根據本發明塑膠膜可藉助共擠壓或雙層合製造。藉助共擠壓製造為較佳。
藉助共擠壓製造多層塑膠膜為熟習技藝人士已知。關於此點,針對分別塑膠層,將分別塑膠(例如且較佳呈粒狀材料形式)熔化於混練擠壓機中,透過噴嘴擠壓成膜。
在雙層合期間,首先製造兩個膜成兩個外層B,優先藉助擠壓,然後藉由滲流熔體介於此等兩個塑膠膜間而製造核心層A。
由於其等傑出性質-例如張力模數輕微下降、其三維外形的穩定性及良好透明性-根據本發明塑膠膜特別充分適合於製造三維成型物件之目的。針對製造如此3D-成型物件之目的,從根據本發明塑膠膜,藉助熱成形實現塑型成適當外形,後者隨後切割及拋光塑膠膜。
因此,本發明進一步目的係從根據本發明多層膜獲得之三維成型物件,特別是藉助熱成形。
根據本發明塑膠膜特別充分適合於製造三維成型物件之目的,特別針對用於醫學應用,例如骨科設備(如骨科支架)、牙科設備(如牙科夾板或保持器)、或夾板(如穩定扭傷關節或骨折用)。此外,根據本發明塑膠膜特別充分適合於製造非醫學應用的三維成型物件之目的,例如光伏打或(地板下)加熱應用。再者,根據本發明塑膠膜特別充分適合於防彈玻璃層體。
以下實施例適用於示範說明發明,並非解釋成限制。
ISOPLAST 2530:醫學應用之商業芳香族透明熱塑性聚胺基甲酸酯,根據DIN EN ISO 868具有蕭耳硬度82D(Lubrizol Corp.)。
DESMOPAN DP 9365 D:商業芳香族透明熱塑性聚醚聚胺基甲酸酯,根據DIN EN ISO 868具有蕭耳硬度65D(Bayer MaterialScience AG)。
共聚酯I:由48.4重量%對酞酸、11.9重量%(23莫耳%相對於二醇成分)2,2,4,4-四甲基-1,3-環丁烷二醇及39.7重量%(77莫耳%相對於二醇成分)環己烷二甲醇組成之對酞酸共聚縮合物,具有固有黏度0.72dl/g(在25℃由酚及四氯乙烷組成的1:1混合物中測量)(Eastman Chemical)、玻璃轉移溫度110℃(由DSC測定)。
共聚酯II:由48.3重量%對酞酸、11.7重量%(23莫耳%相對於二醇成分)2,2,4,4-四甲基-1,3-環丁烷二醇及40.0重量%(77莫耳%相對於二醇成分)環己烷二甲醇組成之對酞酸共聚縮合物,具有固有黏度0.63dl/g(在25℃由酚及四氯乙烷組成的1:1混合物中測量)、玻璃轉移 溫度105℃(由DSC測定)。
TEXIN 970U:商業芳香族透明熱塑性聚醚聚胺基甲酸酯,根據DIN EN ISO 868具有蕭耳硬度70D(Bayer MaterialScience AG)。
MAKROLON 3108:來自Bayer MaterialScience AG之商業高黏度非晶質熱塑性雙酚A-聚碳酸酯,根據ISO 1133於300℃及1.2kg具有熔體容積速率(MVR)6g/10min,玻璃轉移溫度149℃(由DSC測定)。
HYTREL 7246:來自Dupont Company,Wilmington之商業高模數熱塑性聚酯彈性體級,根據DIN EN ISO 868具有標稱蕭耳硬度72D。
POCAN B 1600:來自Lanxess AG之商業熱塑性對酞酸丁二酯,根據ISO 1133於260℃及2.16kg具有熔體容積速率(MVR)14g/10min。
用於製造共擠壓膜之膜擠壓線包括:■擠壓機,具有螺桿60mm直徑(D)及具有長度33D;螺桿展現除氣區域;■熔體泵;■十字頭;■平板鑄模,具有寬度450mm;■三輥軋光機,具有水平滾輪排列,第三個滾輪就水平而言能夠轉動約+/-45。;■滾輪輸送機;■厚度測量;■保護膜之雙向塗敷設備;■取出(take-off)設備;■捲繞機。
使粒狀材料從乾燥機離開輸送入擠壓機的進料漏斗。在由擠壓機圓柱/螺桿構成的塑化系統中,進行材料熔融及輸送。從平板鑄模,熔體抵達軋光機。在軋光機上(由三個輥組成),進行膜的測定性塑型及冷卻。針對紋理化膜表面之目的,關於此點利用兩個拋光的鉻滾輪(光澤/光澤表面用)。隨後透過取出(take-off)運輸膜,塗敷保護膜於兩側,然後舉行膜的捲繞。
用上述膜擠壓線,以主要擠壓機溫度240℃至260℃,製造由共聚酯I組成具有厚度760μm之單層膜。
用如實施例1相同的膜擠壓線,以主要擠壓機溫度220℃至240℃,製造由ISOPLAST 2530組成具有厚度750μm之單層膜。
使用之膜擠壓線由下列組成:■擠壓機,具有螺桿105mm直徑(D)及具有長度41xD;螺桿展現除氣區域;■塗敷頂層之共擠壓機,具有螺桿長度25D及具有直徑35mm;■十字頭;■特殊共擠壓膜鑄模,具有寬度1500mm;■三輥軋光機,具有水平滾輪排列,第三個滾輪就水平而言能夠轉動約+/-45。;■滾輪輸送機;■在兩者表面上塗敷保護膜之設備; ■取出(take-off)設備;■捲繞機。
將基礎材料之粒狀材料供應給主要擠壓機的進料漏斗。在由圓柱/螺桿構成的分別塑化系統中,進行分別材料熔融及輸送。將兩者材料熔體一起帶至共擠壓噴嘴中。從噴嘴,熔體抵達軋光機。在輥軋光機上,舉行材料的測定性塑型及冷卻。針對結構化膜表面之目的,關於此點利用兩個拋光的鉻滾輪(光澤/光澤表面用)。隨後透過取出(take-off)運輸膜,塗敷保護膜於兩側,然後舉行膜的捲繞。
用此膜擠壓線,以主要擠壓機溫度220℃至240℃及以共擠壓機溫度228℃至260℃,擠壓出根據本發明具有兩個光滑光澤側且具有層厚800μm之三層膜,共聚酯核心層為650μm厚,各側上熱塑性聚胺基甲酸酯層於各情況中為75μm厚。
在如實施例3之膜擠壓線中,為製造三層膜之目的,利用更迅速流動的共聚酯II而取代共聚酯I。
從此,以主要擠壓機溫度220℃至235℃及以共擠壓機溫度227℃至260℃,擠壓出根據本發明具有兩個光滑閃耀側且具有層厚800μm之三層膜,共聚酯核心層為650μm厚,各側上熱塑性聚胺基甲酸酯層於各情況中為75μm厚。
在與實施例3相同之膜擠壓線中,擠壓出根據本發明具有一個光澤表面及一個無光澤表面之膜。
關於此點,針對結構化膜表面之目的,利用一個拋光的鉻滾輪及一個結構化的聚矽氧橡膠滾輪。用於結構化膜 表面之橡膠滾輪係敘述於Nauta Roll Corporation持有之DE 32 28 002(或於相等案US 4,368,240)。
以主要擠壓機溫度220℃至235℃及以共擠壓機溫度227℃至260℃,擠壓出根據本發明具有光滑光澤側及具有無光澤側且具有層厚800μm之三層膜,共聚酯核心層為650μm厚,各側上熱塑性聚胺基甲酸酯層於各情況中為75μm厚。
在如實施例3之膜擠壓線中,為製造三層膜之目的,對主要擠壓機利用60重量%MAKROLON 3108及40重量%POCAN B 1600之摻混物而取代共聚酯I且對共擠壓機利用TEXIN 970U。TEXIN 970U形成外層,MAKROLON/POCAN摻混物形成核心層。
從此,以主要擠壓機溫度260℃至270℃及以共擠壓機溫度210℃至230℃,擠壓出根據本發明具有兩個光滑閃耀側且具有層厚750μm之三層膜,共聚酯核心層為550μm厚,各側上熱塑性聚胺基甲酸酯層於各情況中為100μm厚。
在如實施例3之膜擠壓線中,為製造三層膜之目的,對主要擠壓機利用60重量%MAKROLON 3108及40重量%POCAN B 1600之摻混物而取代共聚酯I且對共擠壓機利用HYTREL 7246。HYTREL 7246形成外層,MAKROLON/POCAN摻混物形成核心層。
從此,以主要擠壓機溫度260℃至270℃及以共擠壓機溫度227℃至245℃,擠壓出根據本發明具有兩個光滑閃耀側且具有層厚750μm之三層膜,共聚酯核心層為550μm厚,各側上熱塑性聚胺基甲酸酯層於各情況中為 100μm厚。
在如實施例3之膜擠壓線中,為製造三層膜之目的,對主要擠壓機利用60重量%MAKROLON 3108及40重量%POCAN B 1600之摻混物而取代共聚酯I且對共擠壓機利用ISOPLAST 2530。ISOPLAST 2530形成外層,MAKROLON/POCAN摻混物形成核心層。
從此,以主要擠壓機溫度260℃至270℃及以共擠壓機溫度210℃至240℃,擠壓出根據本發明具有兩個光滑閃耀側且具有層厚750μm之三層膜,共聚酯核心層為550μm厚,各側上熱塑性聚胺基甲酸酯層於各情況中為100μm厚。
測定在實施例3至5共聚酯層上熱塑性聚胺基甲酸酯(TPU)層之剝離強度的方法
1.模切樣本成4吋長x0.76吋寬(10mm L x 19.3mm W):鑄模尺寸可隨可得性而改變(W:0.75~1吋,L:最小4吋)。
2.標記欲試驗的TPU層之側。翻轉樣品至另一側。從樣本一個邊緣之7mm處用尖銳切割器刮出一條線。
3.沿著切割線溫和彎曲樣本,同時令試驗的TPU完整無缺。
4.藉由拉扯小的切割部分,從切割線溫和開始剝離TPU層。
5.繼續剝離直到剝離TPU層長度為13mm。確保TPU層均勻剝離穿過全部樣本寬度。
6.切割樣本另一端以使總黏著區域長度為62mm。
遵循ASTM D 903 98模型進行測定剝離強度。將根據實施例6方法製備之樣本貯存於50%相對溼度及23℃且隨後在此等條件下試驗。分離速率總計為305mm/min。從校正曲線評估介於5mm至25mm之平均值。
在樣本三個不同位置已進行測定。以下顯示計算的平均結果。
對底層測量每單位寬度之平均負載,實施例3為0.76N/mm,實施例4為0.79N/mm,實施例5為0.97N/mm。對頂層測量每單位寬度之平均負載,實施例3為1.13N/mm,實施例4為0.60N/mm,實施例5為1.10N/mm。結果顯示根據本發明膜展現介於共聚酯核心層與TPU外層間之優異黏著性。
針對根據實施例6至8的三層膜,介於外層與核心層之剝離強度如此高以致於未損害外層下不可能分離,以致此等根據本發明膜展現介於核心層與外層間之優異黏著性。
遵循ASTM D 638模型進行測量張力強度。在ZwickZ020/148385類型之張力試驗機上進行張力試驗。使用類型4之張力試驗樣本。針對評估之目的,採用5次測量之平均值。將樣本於50%相對溼度及23℃貯存>48小時且隨後在此等條件下試驗。試驗速率總計為12.7mm/min,在測定楊氏模數(彈性模數)期間,1mm/min。
在樣本三個不同位置已進行測定。下表顯示計算的平 均結果。
結果:
結果顯示根據本發明膜展現優異張力強度及傑出張力模數。
根據修飾ASTM D790測定應力鬆弛:
-樣品尺寸:51mm(長)x21.5mm(寬)x~0.8mm(厚)
-在測量應力鬆弛前於定義溫度(25℃或50℃)水浸泡樣品
-以5%應變於三點彎曲
-撐體跨距:16mm
結果:
關於此點,最初負載數值表示時間於貯存前(亦即時間t=0)之測量數值,剩餘負載數值表示時間於24h貯存後之測量數值。
結果顯示在兩種貯存溫度,根據本發明三層膜於24h貯存後較實施例2的TPU單層膜展現更高剩餘負載。特別針對實施例3及7,雖然在兩種貯存溫度,根據本發明三層膜於時間貯存前皆展現清楚更低的最初負載,但更驚人地於貯存24h後仍能夠運用的力僅下降相當較輕程度。
僅有由根據本發明三層膜組成之樣品在潮濕環境中貯存期間展現小的張力模數減少。此外,根據本發明膜顯露介於核心層與外層間之傑出黏著性。
雖然本發明已詳細敘述於前面以為闡明目的,但欲了解如此細節僅為彼目的,且除了申請專利範圍可限制者外,熟習技藝者在未背離發明精髓及範疇下可做成變化。
Claims (18)
- 一種三層塑膠膜,特徵在於- 其具有核心層A,其含有具有玻璃轉移溫度Tg為80℃至200℃之至少一種聚碳酸酯或共聚碳酸酯及/或聚酯或共聚酯,- 此核心層係座落介於兩個外層B間,其含有展現硬度為45蕭耳D至85蕭耳D之至少一種熱塑性聚胺基甲酸酯及/或聚酯或共聚酯- 其中該三層塑膠膜具有總厚度為300μm至2000μm。
- 根據申請專利範圍第1項之三層塑膠膜,特徵在於其具有核心層A,該核心層A含有具有固有黏度為0.50dL/g至1.20dL/g及玻璃轉移溫度Tg為80℃至200℃之至少一種聚酯或共聚酯。
- 根據申請專利範圍第1或2項之三層塑膠膜,特徵在於該兩個外層B含有展現硬度為45蕭耳D至85蕭耳D之至少一種熱塑性聚胺基甲酸酯。
- 根據申請專利範圍第1或2項之三層塑膠膜,特徵在於- 其具有核心層A,其含有至少一種展現來自以下殘基之共聚酯(a)二羧酸成分,包括i)70莫耳%至100莫耳%對酞酸殘基,ii)0莫耳%至30莫耳%具有高至20個碳原子之芳香族二羧酸殘基,及iii)0莫耳%至10莫耳%具有高至16個碳原子之脂族二羧酸殘基,及(b)二醇成分,包括i)5莫耳%至50莫耳%2,2,4,4-四甲基-1,3-環丁烷二醇殘基,及ii)50莫耳%至95莫耳%1,4-環己烷二甲醇殘基,其中該二羧酸成分殘基i)至iii)之莫耳%總合總計為100莫耳%,且該二醇成分殘基i)及ii)之莫耳%總合總計為100莫耳%,且其中該共聚酯之固有黏度總計為0.50dL/g至1.20dL/g且該共聚酯展現玻璃轉移溫度Tg為80℃至150℃,- 且此核心層係座落介於兩個外層B間,其含有至少一種熱塑性聚胺基甲酸酯,該熱塑性聚胺基甲酸酯展現硬度為45蕭耳D至85蕭耳D且可從以下獲得a)一或多種線型聚醚二醇,其具有平均分子量500g/mol至10,000g/mol,且各情況中平均至少1.8及至多3.0Tserevitinov活性氫原子,b)一或多種有機二異氰酸酯,c)一或多種二醇鏈伸長劑,其具有分子量60g/mol至500g/mol且具有平均1.8至3.0Tserevitinov活性氫原子,於以下存在d)視情況一或多種觸媒,添加以下e)視情況輔助物質及添加劑,其中b)中NCO基團與a)及c)中對異氰酸酯呈反應性的基團之莫耳比率總計為0.85:1至1.2:1。
- 根據申請專利範圍第1或2項之三層塑膠膜,特徵在於該熱塑性聚胺基甲酸酯展現硬度為50蕭耳D至80蕭耳D。
- 根據申請專利範圍第4項之三層塑膠膜,特徵在於用於製造該熱塑性聚胺基甲酸酯之該聚醚二醇a)係選自一或多種以1,4-丁烷二醇單元及/或1,3-丙二醇單元為主群組之聚醚二醇。
- 根據申請專利範圍第4項之三層塑膠膜,特徵在於用於製造該熱塑性聚胺基甲酸酯之該有機二異氰酸酯b)係選自一或多種含有4,4’-二苯基甲烷二異氰酸酯、異佛酮二異氰酸酯、二環己基甲烷-4,4’-二異氰酸酯或1,6-六亞甲基二異氰酸酯群組之異氰酸酯。
- 根據申請專利範圍第4項之三層塑膠膜,特徵在於用於製造該熱塑性聚胺基甲酸酯之該二醇鏈伸長劑c)係選自一或多種含有1,4-丁烷二醇、1,3-丙烷二醇、1,2-丙烷二醇、1,2-乙二醇、1,6-己烷二醇、1,4-二(β-羥乙基)氫醌或1,4-二(β-羥乙基)雙酚A群組之鏈伸長劑。
- 根據申請專利範圍第4項之三層塑膠膜,特徵在於該熱塑性聚胺基甲酸酯係於預聚物方法中製造。
- 根據申請專利範圍第4項之三層塑膠膜,特徵在於該共聚酯之二醇成分包括10莫耳%至35莫耳%2,2,4,4-四甲基-1,3-環丁烷二醇殘基與65莫耳%至90莫耳%1,4-環己烷二甲醇殘基,此等二醇成分的兩種成分之莫耳%總和總計為100莫耳%。
- 根據申請專利範圍第4項之三層塑膠膜,特徵在於來自該聚酯之二羧酸成分之殘基包含95至100莫耳%對酞酸殘基。
- 根據申請專利範圍第1或2項之三層塑膠膜,特徵在於該膜已被共擠壓。
- 根據申請專利範圍第1或2項之三層塑膠膜,特徵在於其具有總厚度為400μm至1500μm。
- 根據申請專利範圍第1或2項之三層塑膠膜,特徵在於該核心層A具有層厚250μm至1600μ.m。
- 根據申請專利範圍第1或2項之三層塑膠膜,特徵在於該外層B各具有層厚25μm至500μm。
- 根據申請專利範圍第2項之三層塑膠膜,特徵在於含在該核心層A中之該聚酯或共聚酯展現固有黏度為0.50dL/g至0.80dL/g。
- 根據申請專利範圍第1或2項之三層塑膠膜,特徵在於含在該核心層A中之該聚酯或共聚酯展現玻璃轉移溫度Tg為85℃至130℃。
- 一種三維成型物件,其係使根據申請專利範圍第1至17項中至少一項三層塑膠膜三維成形而獲得。
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