TW201639900A - 共聚碳酸酯及包含彼之組成物 - Google Patents
共聚碳酸酯及包含彼之組成物 Download PDFInfo
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- TW201639900A TW201639900A TW104140531A TW104140531A TW201639900A TW 201639900 A TW201639900 A TW 201639900A TW 104140531 A TW104140531 A TW 104140531A TW 104140531 A TW104140531 A TW 104140531A TW 201639900 A TW201639900 A TW 201639900A
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- copolycarbonate
- chemical formula
- bis
- repeating unit
- hydroxyphenyl
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Abstract
本發明關於共聚碳酸酯和包含彼之模塑物件。根據本發明之共聚碳酸酯具有特定矽氧烷化合物被引入聚碳酸酯的主鏈中之結構,且因此具有提供極佳蓄熱穩定性的特性。
Description
本申請案主張向韓國智慧財產局(Korean Intellectual Property Office)申請於2014年12月4日之韓國專利申請案第10-2014-0173005號和申請於2015年12月1日申請之韓國專利案第10-2015-0169804號的權益,該等申請案之揭示以其全文引用方式併入本文中。
本發明關於一種共聚碳酸酯及含彼之組成物,且更具體而言關於一種經濟地製造且具有極佳蓄熱穩定性之共聚碳酸酯,及關於一種含彼之組成物。
聚碳酸酯樹脂係藉由芳族二醇諸如雙酚A與碳酸酯前驅物諸如光氣之縮合聚合製備並具有極佳衝擊強度、尺寸穩定性、耐熱性和透明性。因此,聚碳酸酯樹脂具有在廣泛用途的應用,諸如電氣和電子產品、汽車零件、建築材
料、光學元件的外部材料。
最近,為了將這些聚碳酸酯樹脂應用至更多不同的領域,已經進行了許多研究,以藉由共聚合二或多種彼此具有不同結構的芳族二醇化合物並將具有不同結構的單元引入聚碳酸酯的主鏈中來獲得所要的物理性質。
尤其,已進行對於聚碳酸酯的主鏈中引入聚矽氧烷結構的研究,但大多數這些技術有高生產成本,及熱穩定性低的缺點。
鑑於上述情況,本發明人已進行了深入的研究,以克服上述先前技術中所遇到的缺點,並開發具有改良熱穩定性之共聚碳酸酯。結果,本發明人已發現一種其中如下所述的特定矽氧烷化合物被引入聚碳酸酯的主鏈中之共聚碳酸酯滿足上述性質,從而完成本發明。
本發明之一目的為提供一種具有極佳蓄熱穩定性之共聚碳酸酯。
本發明之另一目的為提供一種括含上述共聚碳酸酯之組成物。
為了達成上述目的,本發明提供一種共聚碳酸酯,其
包含:以芳族聚碳酸酯為基礎之第一重複單元;及一或多種具有矽氧烷鍵且具有如根據下列方程式1測得之0.5至5的△YI之以芳族聚碳酸酯為基礎之第二重複單元,[方程式1]△YI=YI(320℃,15分鐘)-YI(320℃,0分鐘)
在方程式1中,YI(320℃,0分鐘)為試樣(寬度/長度/厚度=60mm/40mm/3mm)根據ASTM D1925測得之YI(黃色指數),該試樣係藉由將該共聚碳酸酯在320℃下射出模塑而獲得,及YI(320℃,15分鐘)為試樣(寬度/長度/厚度=60mm/40mm/3mm)根據ASTM D1925測得之YI(黃色指數),該試樣係藉由將該共聚碳酸酯在320℃下滯留15分鐘,然後進行射出模塑而獲得。
當使用共聚碳酸酯製備產物時,該產物通常是藉由射出模塑方法形成。在射出模塑期間,高溫係施加至共聚碳酸酯經某段時間,且因此在此過程中可產生變形諸如熱分解。因此,為了增加共聚碳酸酯的適用性,在射出過程中所造成的變形應最小化,及為了評估此變形,在本發明中評估'蓄熱穩定性'。
如本文所用,術語'蓄熱穩定性'意指該共聚碳酸酯在某高溫下滯留某段時間,及接著射出以製備試樣,及測定試樣的YI(黃色指數),接著與沒有滯留之試樣的YI(黃色指數)比較。特別地,在本發明中,施加如方程式
1中所示之試樣於320℃滯留15分鐘的條件。
當蓄熱穩定性極佳時,即使在高溫下滯留某段時間時,幾乎不產生變形諸如熱分解,因此如與沒有滯留之試樣的YI(黃色指數)比較,沒有大的差異。
特別地,根據本發明之共聚碳酸酯具有如根據方程式1測得之0.5至5的△YI。較佳地,根據方程式1測得之△YI為不大於4.5,不大於4.0,不大於3.5,不大於3.0,不大於2.5,不大於2.0,不大於1.9,不大於1.8,不大於1.7,不大於1.6,或不大於1.5。
此外,較小量的△YI意指極佳蓄熱穩定性,且其不限於任何下限值。然而,作為一實例,較佳的是不小於0.5,不小於0.6,不小於0.7,不小於0.8,不小於0.9,或不小於1.0。
另外,較佳地,根據本發明之共聚碳酸酯具有大於0,不大於9,不大於8,不大於7,不大於6,或不大於5的YI(320℃,15分鐘)。另外,較佳地,根據本發明之共聚碳酸酯具有大於0,不大於5,或不大於4的YI(320℃,0分鐘)。
另外,較佳地,根據本發明之共聚碳酸酯具有根據ASTM D256(1/8吋,缺口衝擊(Notched Izod))在-30℃下測得之600至1000J/m的低溫衝擊強度。
另外,較佳地,根據本發明之共聚碳酸酯具有1,000至100,000g/mol之重量平均分子量且較佳為15,000至35,000g/mol。在此重量平均分子量的範圍內,該共聚碳
酸酯具有提供極佳滯留熱穩定性的效果。
更佳地,上述重量平均分子量為不小於20,000g/mol,不小於21,000g/mol,不小於22,000g/mol,不小於23,000g/mol,不小於24,000g/mol,不小於25,000g/mol,不小於26,000g/mol,不小於27,000g/mol,或不小於28,000g/mol。且,上述重量平均分子量為不大於34,000g/mol,不大於33,000g/mol,或不大於32,000g/mol。
另外,較佳地,根據本發明之共聚碳酸酯具有如根據ASTM D1238(300℃,1.2kg之條件)測得之3至20g/10min的融熔指數。
更佳地,融熔指數為不小於5g/10min,不小於6g/10min,不小於7g/10min,或不小於8g/10min;且不大於15g/10min,不大於14g/min,不大於13g/min,或不大於12g/10min。
另外,較佳地,根據本發明之共聚碳酸酯包含二種具有矽氧烷鍵的以芳族聚碳酸酯為基礎之第二重複單元。
另外,較佳地,在根據本發明之共聚碳酸酯中,以芳族聚碳酸酯為基礎之第一重複單元的含量相對於該以芳族聚碳酸酯為基礎之第一重複單元和一或多種具有矽氧烷鍵的以芳族聚碳酸酯為基礎之第二重複單元的總重量為90至99%。在此含量之範圍內,該共聚碳酸酯具有提供極佳滯留熱穩定性的效果。
更佳地,以芳族聚碳酸酯為基礎之第一重複單元的含
量相對於該以芳族聚碳酸酯為基礎之第一重複單元和一或多種具有矽氧烷鍵的以芳族聚碳酸酯為基礎之第二重複單元的總重量為不小於91%,不小於92%,不小於93%,或不小於94%;且不大於98%,不大於97%,或不大於96%。另外,上述含量可根據稍後描述之芳族二醇化合物和矽氧烷化合物的重量比決定。
另外,在根據本發明之共聚碳酸酯中,以芳族聚碳酸酯為基礎之第一重複單元較佳係藉由使芳族二醇化合物和碳酸酯前驅物反應而形成,且其更佳以下列化學式1表示:
在化學式1中,R1、R2、R3和R4各自獨立地為氫、C1-10烷基、C1-10烷氧基、或鹵素,Z為未經取代或經苯基取代之C1-10伸烷基、未經取代或經C1-10烷基取代之C3-15伸環烷基、O、S、SO、SO2、或CO。
較佳地,在化學式1中,R1、R2、R3和R4各自獨立地為氫、甲基、氯基、或溴基。
另外,Z較佳為未經取代或經苯基取代之直鏈或支鏈C1-10伸烷基,且更佳為亞甲基、乙烷-1,1-二基、
丙烷-2,2-二基、丁烷-2,2-二基、1-苯基乙烷-1,1-二基或二苯基亞甲基。另外,較佳地,Z為環己烷-1,1-二基、O、S、SO、SO2、或CO。
較佳地,該以化學式1表示之重複單元可衍生自一或多種選自由下列所組成群組的芳族二醇化合物:雙(4-羥基苯基)甲烷、雙(4-羥基苯基)醚、雙(4-羥基苯基)碸、雙(4-羥基苯基)亞碸、雙(4-羥基苯基)硫醚、雙(4-羥基苯基)酮、1,1-雙(4-羥基苯基)乙烷、雙酚A、2,2-雙(4-羥基苯基)丁烷、1,1-雙(4-羥基苯基)環己烷、2,2-雙(4-羥基-3,5-二溴苯基)丙烷、2,2-雙(4-羥基-3,5-二氯苯基)丙烷、2,2-雙(4-羥基-3-溴苯基)丙烷、2,2-雙(4-羥基-3-氯苯基)丙烷、2,2-雙(4-羥基-3-甲基苯基)丙烷、2,2-雙(4-羥基-3,5-二甲基苯基)丙烷、1,1-雙(4-羥基苯基)-1-苯基乙烷、雙(4-羥基苯基)二苯基甲烷、及α,ω-雙[3-(鄰-羥基苯基)丙基]聚二甲基矽氧烷。
如本文所用,'衍生自芳族二醇化合物'意指芳族二醇化合物之羥基和碳酸酯前驅物反應而形成以化學式1表示之重複單元。
例如,當雙酚A(其為芳族二醇化合物)和三光氣(其為碳酸酯前驅物)聚合時,以化學式1表示之重複單元係以下列化學式1-1表示:式1-1:
本文所用之碳酸酯前驅物可包括一或多種選自由下列所組成之群組:碳酸二甲酯、碳酸二乙酯、碳酸二丁酯、碳酸二己酯、碳酸二苯酯、碳酸二甲苯酯、雙(氯苯基)碳酸酯、碳酸二間-甲苯酚基酯、碳酸二萘酯、雙(二苯基)碳酸酯、光氣、三光氣、雙光氣、溴光氣和雙鹵甲酸酯。較佳地,可使用三光氣或光氣。
另外,較佳地,在根據本發明之共聚碳酸酯中,一或多種具有矽氧烷鍵的以芳族聚碳酸酯為基礎之第二重複單元係藉由使一或多種矽氧烷化合物和碳酸酯前驅物反應而形成,且更佳地其包含以下列化學式2表示之重複單元和以下列化學式3表示之重複單元:
在化學式2中,X1分別獨立地為C1-10伸烷基,R5分別獨立地為氫;未經取代或經環氧乙烷基、經環氧乙烷基取代之C1-10烷氧基、或C6-20芳基取代之
C1-15烷基;鹵素;C1-10烷氧基;烯丙基;C1-10鹵烷基;或C6-20芳基,及n為10至200的整數,
在化學式3中,X2分別獨立地為C1-10伸烷基,Y1分別獨立地為氫、C1-6烷基、鹵素、羥基、C1-6烷氧基、或C6-20芳基,R6分別獨立地為氫;或未經取代或經環氧乙烷基、經環氧乙烷基取代之C1-10烷氧基、或C6-20芳基取代之C1-15烷基;鹵素;C1-10烷氧基;烯丙基;C1-10鹵烷基;或C6-20芳基,及m為10至200的整數。
在化學式2中,X1較佳分別獨立地為C2-10伸烷基,更佳為C2-4伸烷基且最佳為丙烷-1,3-二基。
且,較佳地,R5較佳分別獨立地為氫、甲基、乙基、丙基、3-苯基丙基、2-苯基丙基、3-(環氧乙烷基甲氧基)丙基、氟基、氯基、溴基、碘基、甲氧基、乙氧基、丙氧基、烯丙基、2,2,2-三氟乙基、3,3,3-三氟丙基、苯基、或萘基。此外,R5較佳分別獨立地為C1-10烷基,更佳為C1-6烷基,更佳為C1-3烷基及最佳為甲基。
另外,較佳地,n為不小於10,不小於15,不小於20,不小於25,不小於30,不小於31,或不小於32;且不大於50,不大於45,不大於40,不大於39,不大於38,或不大於37的整數。
在化學式3中,X2較佳分別獨立地為C2-10伸烷基,更佳為C2-6伸烷基且最佳為伸異丁基。
另外,較佳地,Y1為氫。
另外,較佳地,R6分別獨立地為氫、甲基、乙基、丙基、3-苯基丙基、2-苯基丙基、3-(環氧乙烷基甲氧基)丙基、氟基、氯基、溴基、碘基、甲氧基、乙氧基、丙氧基、烯丙基、2,2,2-三氟乙基、3,3,3-三氟丙基、苯基、或萘基。另外,較佳地,R6分別獨立地為C1-10烷基,更佳為C1-6烷基,更佳為C1-3烷基,且最佳為甲基。
較佳地,m為不小於40,不小於45,不小於50,不小於55,不小於56,不小於57,或不小於58;且不大於80,不大於75,不大於70,不大於65,不大於64,不大於63,或不大於62的整數。
以化學式2表示之重複單元和以化學式3表示之重複單元係分別衍生自下列以化學式2-1表示之矽氧烷化合物和以下列化學式3-1表示之矽氧烷化合物:
在化學式2-1中,X1、R5和n係與如前述所定義者相同,
在化學式3-1中,X2、Y1、R6和m係與如前述所定義者相同。
如本文所用,'衍生自矽氧烷化合物'意指各個矽氧烷化合物之羥基和碳酸酯前驅物反應以形成以化學式2表示之重複單元和以化學式3表示之重複單元。另外,可用於形成以化學式2和3表示之重複單元的碳酸酯前驅物係與針對可用於形成上述以化學式1表示之重複單元的碳酸酯前驅物所述者相同。
製備以化學式2-1表示之矽氧烷化合物和以化學式3-1表示之矽氧烷化合物的方法分別係以下列反應流程1和2表示:
在反應流程1中,X1'為C2-10烯基,及X1、R5和n係與如前述所定義者相同,
在反應流程2中,X2'為C2-10烯基,及X2、Y1、R6和m係與如前述所定義者相同。
在反應流程1和反應流程2中,反應較佳係在金屬觸
媒存在下進行。作為金屬觸媒,較佳使用Pt觸媒。本文所用之Pt觸媒可包括一或多種選自由下列所組成之群組:Ashby觸媒、Karstedt觸媒、Lamoreaux觸媒、Speier觸媒、PtCl2(COD)、PtCl2(苯甲腈)2和H2PtBr6。金屬觸媒之使用量以100重量份的以化學式7或9表示之化合物為基準計可為不小於0.001重量份、不小於0.005重量份、或不小於0.01重量份;且不大於1重量份、不大於0.1重量份、或不大於0.05重量份。
另外,上述反應溫度較佳為80至100℃。另外,上述反應時間較佳為1至5小時。
此外,以化學式7或9表示之化合物可藉由使有機二矽氧烷和有機環矽氧烷在酸觸媒存在下反應而製備,及n和m可藉由調整所用反應物的量來調整。反應溫度較佳為50至70℃。且,反應時間較佳為1至6小時。
上述有機二矽氧烷可包括一或多種選自由下列所組成之群組:四甲基二矽氧烷、四苯基二矽氧烷、六甲基二矽氧烷和六苯基二矽氧烷。此外,上述有機環矽氧烷可包括(例如)有機環四矽氧烷。作為其一實例,可包括八甲基環四矽氧烷和八苯基環四矽氧烷或類似者。
上述有機二矽氧烷之使用量,以100重量份的有機環矽氧烷為基準計,可為不小於0.1重量份,或不小於2重量份;且不大於10重量份或不大於8重量份。
上述可使用於本文中之酸觸媒包括一或多種選自由下列所組成之群組:H2SO4、HClO4、AlCl3、SbCl5、SnCl4
和酸性白土(漂白土)。另外,酸觸媒之使用量以100重量份的有機環矽氧烷為基準計可為不小於0.1重量份、不小於0.5重量份或不小於1重量份;且不大於10重量份、不大於5重量份或不大於3重量份。
特別地,藉由調整以化學式2表示之重複單元和以化學式3表示之重複單元的含量,可同時改良共聚碳酸酯的低溫衝擊強度和YI(黃色指數)。較佳地,上述重複單元之間的重量比可從1:99至99:1。較佳地,重量比係從3:97至97:3、從5:95至95:5、從10:90至90:10、或從15:85至85:15,及更佳為從20:80至80:20。上述重複單元之重量比對應於矽氧烷化合物(例如以化學式2-1表示之矽氧烷化合物和以化學式3-1表示之矽氧烷化合物)的重量比。
較佳地,以化學式2表示之重複單元係以下列化學式2-2表示:
在化學式2-2中,R5和n係與如前述所定義者相同。較佳地,R5為甲基。
且,較佳地,以化學式3表示之重複單元係以下列化學式3-2表示:
在化學式3-2中,R6和m係與如前述所定義者相同。較佳地,R6為甲基。
另外,根據本發明之共聚碳酸酯包含以化學式1-1表示之重複單元、以化學式2-2表示之重複單元、和以化學式3-2表示之重複單元全部。
另外,本發明提供一種製備共聚碳酸酯之方法,其包含聚合芳族二醇化合物、碳酸酯前驅物和一或多種矽氧烷化合物之步驟。
芳族二醇化合物、碳酸酯前驅物和一或多種矽氧烷化合物係與如前所述者相同。
在聚合期間,一或多種矽氧烷化合物之使用量以芳族二醇化合物、碳酸酯前驅物和一或多種矽氧烷化合物之總共100重量%為基準計可為不小於0.1重量%、不小於0.5重量%、不小於1重量%或不小於1.5重量%;且不大於20重量%、不大於10重量%、不大於7重量%、不大於5重量%、不大於4重量%、不大於3重量%或不大於2重量%。且,上述芳族二醇化合物之使用量以芳族二醇化合物、碳酸酯前驅物和一或多種矽氧烷化合物之總共100重量%為基準計可為不小於40重量%、不小於50重量%、或不小於55重量%;且不大於80重量%、不大於70重量
%、或不大於65重量%。上述碳酸酯前驅物之使用量以芳族二醇化合物、碳酸酯前驅物和一或多種矽氧烷化合物之總共100重量%為基準計可為不小於10重量%、不小於20重量%、或不小於30重量%;且不大於60重量%、不大於50重量%、或不大於40重量%。
另外,關於聚合方法,可使用界面聚合法作為一個實例。在此情況下,有聚合反應可在低溫和大氣壓下進行,及分子量控制容易的效果。上述界面聚合較佳在酸黏合劑和有機溶劑存在下進行。再者,上述界面聚合可包含(例如)進行預聚合,然後添加偶聯劑和再次進行聚合之步驟。在此情況下,可獲得具有高分子量的共聚碳酸酯。
不特別限制界面聚合中所使用的材料,只要彼等可使用於聚碳酸酯的聚合中即可。可根據需要控制其使用量。
酸黏合劑可包括(例如)鹼金屬氫氧化物諸如氫氧化鈉或氫氧化鉀、或胺化合物諸如吡啶。
不特別限制該有機溶劑,只要其為通常可使用於聚碳酸酯的聚合之溶劑即可。作為一個實例,可使用鹵化烴諸如二氯甲烷或氯苯。
另外,在界面聚合期間,反應加速劑(例如)三級胺化合物諸如三乙胺、溴化四正丁銨和溴化四正丁鏻、或四級銨化合物或四級鏻化合物可進一步用於加速反應。
在界面聚合中,反應溫度較佳為從0至40℃和反應時間較佳為從10分鐘至5小時。另外,在界面聚合反應期間,pH較佳保持在9或更高、或11或更高。
此外,界面聚合可藉由另外包括分子量改質劑來進行。分子量改質劑可在聚合引發之前、聚合引發期間、或聚合引發之後添加。
作為上述分子量改質劑,可使用單烷基酚。作為一個實例,單烷基酚為一或多種選自由下列所組成之群組:對三級丁基酚、對-異丙苯基酚、癸基酚、十二基酚、十四基酚、十六基酚、十八基酚、二十基酚、二十二基酚和三十基酚,且較佳為對三級丁基酚。在此情況下,調節分子量的效果很大。
上述分子量改質劑之含量以100重量份的芳族二醇化合物為基準計(例如)為不小於0.01重量份、不小於0.1重量份或不小於1重量份;且含量不大於10重量份、不大於6重量份、或不大於5重量份。在此範圍內,可獲得所要分子量。
此外,本發明提供一種包含上述共聚碳酸酯和聚碳酸酯之聚碳酸酯組成物。共聚碳酸酯可單獨使用,但如需要控制共聚碳酸酯的物理性質時,其可與聚碳酸酯一起使用。
上述聚碳酸酯與根據本發明之共聚碳酸酯的區別在於聚矽氧烷結構不被引入聚碳酸酯的主鏈中。
較佳地,上述聚碳酸酯包含以下列化學式4表示之重複單元:
在化學式4中,R'1、R'2、R'3和R'4各自獨立地為氫、C1-10烷基,C1-10烷氧基、或鹵素,Z'為未經取代或經苯基取代之C1-10伸烷基或未經取代或經C1-10烷基取代之C3-15伸環烷基或O或S或SO或SO2或CO。
另外,較佳地,上述聚碳酸酯具有15,000至35,000g/mol之重量平均分子量。更佳地,上述重量平均分子量(g/mol)為不小於20,000,不小於21,000,不小於22,000,不小於23,000,不小於24,000,不小於25,000,不小於26,000,不小於27,000,或不小於28,000。另外,上述重量平均分子量(g/mol)為不大於34,000,不大於33,000,或不大於32,000。
以化學式4表示之重複單元係藉由反應芳族二醇化合物和碳酸酯前驅物而形成。可使用於本文中之芳族二醇化合物和碳酸酯前驅物與前文中針對以化學式1表示之重複單元所述者相同。
較佳地,化學式4中之R'1、R'2、R'3、R'4和Z'分別與前文中針對化學式1中之R1、R2、R3、R4所述者相同。
另外,較佳地,以化學式4表示之重複單元為以下列化學式4-1表示之重複單元:
在聚碳酸酯組成物中,共聚碳酸酯和聚碳酸酯之重量比較佳為從99:1至1:99,更佳為從90:10至50:50,及最佳為從80:20至60:40。
此外,本發明提供一種包含上述共聚碳酸酯或聚碳酸酯組成物之物件。
較佳地,上述物件為射出模塑物件。此外,該物件可進一步包含(例如)一或多種選自由下列所組成之群組:抗氧化劑、熱穩定劑、光穩定劑、塑化劑、抗靜電劑、成核劑、阻燃劑、潤滑劑、衝擊增強劑、螢光增白劑、紫外線吸收劑、顏料和染料。
如上所述,根據本發明之共聚碳酸酯具有極佳滯留熱穩定性,且因此即使在射出模塑所施用之高溫下幾乎不產生變形諸如熱分解。因此,在射出模塑物件之製造過程中可保持共聚碳酸酯的原來特性,且幾乎不產生變化諸如顏色變化。
用於製備物件之方法可包含下列之步驟:使用混合器混合根據本發明之共聚碳酸酯和添加劑諸如抗氧化劑,用擠壓機將混合物擠壓模塑以製造粒料,乾燥該粒料及然後
用射出模塑機射出乾燥的粒料。
如上所述,根據本發明,其中特定矽氧烷化合物被引入聚碳酸酯的主鏈中之共聚碳酸酯具有提供極佳蓄熱穩定性之效果。
以下,將提供較佳實施態樣以幫助本揭示的理解。然而,提供這些實施例僅用於舉例說明本發明,且不應被解釋為將本發明限制於這些實施例。
混合47.60g(160mmol)的八甲基環四矽氧烷和2.40g(17.8mmol)的四甲基二矽氧烷。接著將混合物與相對於100重量份的八甲基環四矽氧烷之1重量份的酸性白土(DC-A3)一起放入3L燒瓶中,並在60℃下反應4小時。反應完成後,將反應產物用乙酸乙酯稀釋並使用矽藻土迅速過濾。當經由1H NMR確認時,由此製備之末端未改質的聚有機矽氧烷之重複單元(n)為34。
將4.81g(35.9mmol)的2-烯丙基酚和0.01g(50ppm)的Karstedt氏鉑觸媒加至所得末端未改質的聚有機矽氧烷,並在90℃下反應3小時。反應完成後,藉由在120℃和1托的條件下進行蒸發移除未反應的矽氧烷。由此製備之末端改質的聚有機矽氧烷命名為AP-PDMS(n=34)。AP-PDMS為淡黃色油且當經由使用Varian500 MHz的1H NMR確認時,重複單元(n)為34,且不需要進一步純化。
混合47.60g(160mmol)的八甲基環四矽氧烷和1.5g(11mmol)的四甲基二矽氧烷。接著將混合物與相對於100重量份的八甲基環四矽氧烷之1重量份的酸性白土(DC-A3)一起引入3L燒瓶中,並在60℃下反應4小時。反應完成後,將反應產物用乙酸乙酯稀釋並使用矽藻土迅速過濾。當經由1H NMR確認時,由此製備之未改質的聚有機矽氧烷之重複單元(m)為58。
將6.13g(29.7mmol)的4-羥基苯甲酸3-甲基丁-3-烯基酯和0.01g(50ppm)的Karstedt氏鉑觸媒加至所得末端未改質的聚有機矽氧烷,並在90℃下反應3小時。反應完成後,藉由在120℃和1托的條件下進行蒸發移除未反應的矽氧烷。由此製備之末端改質的聚有機矽氧烷命
名為MBHB-PDMS(m=58)。MBHB-PDMS為淡黃色油且當經由使用Varian500 MHz的1H NMR確認時,重複單元(m)為58,且不需要進一步純化。
混合47.60g(160mmol)的八甲基環四矽氧烷和1.7g(13mmol)的四甲基二矽氧烷。接著將混合物與相對於100重量份的八甲基環四矽氧烷之1重量份的酸性白土(DC-A3)一起引入3L燒瓶中,並在60℃下反應4小時。反應完成後,將反應產物用乙酸乙酯稀釋並使用矽藻土迅速過濾。當經由1H NMR確認時,由此製備之未改質的聚有機矽氧烷之重複單元(n)為50。
將6.13g(29.7mmol)的丁香酚和0.01g(50ppm)的Karstedt氏鉑觸媒加至所得末端未改質的聚有機矽氧烷,並在90℃下反應3小時。反應完成後,藉由在120℃和1托的條件下進行蒸發移除未反應的矽氧烷。由此製備之末端改質的聚有機矽氧烷命名為丁香酚-PDMS。丁香酚-PDMS為淡黃色油且當經由使用Varian500 MHz的1H NMR確認時,重複單元(n)為50,且不需要進一步純化。
將1784g的水、385g的NaOH和232g的BPA(雙酚A)加至聚合反應器中,並在N2氛圍下混合。將4.3g的PTBP(對-三級丁基酚)和5.91g的製備例1中所製備之AP-PDMS(n=34)和0.66g的製備例2中所製備之MBHB-PDMS(m=58)的混合溶液溶解在MC(二氯甲烷)中且然後加入其中。之後,將128g的TPG(三光氣)溶解在MC中且將溶解之TPG溶液加至其中並反應1小時,同時將TPG溶液之pH保持於11或更高。10分鐘之後,對其添加46g的TEA(三乙胺)以進行偶合反應。1小時又20分鐘的總反應時間之後,將pH降低至4以移除TEA,及接著藉由用蒸餾水洗滌三次將所製造之聚合物的pH調整至6至7之中性pH。將由此獲得之聚合物再沉澱於甲醇和己烷的混合溶液中,及然後在120℃下乾燥以產生最終共聚碳酸酯。
將1784g的水、385g的NaOH和232g的BPA(雙酚A)加至聚合反應器中,並在N2氛圍下混合。將4.3g的PTBP(對-三級丁基酚)和6.57g的AP-PDMS(n=34)溶解在MC(二氯甲烷)中且然後加入其中。之後,將128g的TPG(三光氣)溶解在MC中且將溶解之TPG溶液加至其中並反應1小時,同時將TPG溶液之pH
保持於11或更高。10分鐘之後,對其添加46g的TEA(三乙胺)以進行偶合反應。1小時又20分鐘的總反應時間之後,將pH降低至4以移除TEA,及用蒸餾水洗滌三次將所製造之聚合物的pH調整至6至7之中性pH。將由此得到的聚合物再沉澱於甲醇和己烷的混合溶液中,及然後在120℃下乾燥以產生最終共聚碳酸酯。
以與比較例1中相同之方法製備共聚碳酸酯,不同的是使用製備例3中所製備之Eu-PDMS(n=50)代替製備例1中所製備之AP-PDMS(n=34)。
以與比較例1中相同之方法製備共聚碳酸酯,不同的是不使用製備例1中所製備之AP-PDMS(n=34)。
混合80重量份的實施例1中所製備之共聚碳酸酯與20重量份的比較例3中所製備之聚碳酸酯以製備聚碳酸酯組成物。
以與比較例1中相同之方法製備共聚碳酸酯,不同的是使用6.24g的製備例1中所製備之AP-PDMS(n=34)
和0.33g的製備例2中所製備之MBHB-PDMS(m=58)。
使用具有Agilent 1200系列之PC標準以GPC測量實施例和比較例中所製備之共聚碳酸酯和聚碳酸酯組成物的重量平均分子量。且,根據ASTM D1238(300℃,1.2kg之條件)測量融熔指數(MI)。
此外,相對於1重量份的實施例和比較例中所製備之各個共聚碳酸酯和聚碳酸酯組成物,對其添加0.050重量份的參(2,4-二-三級丁基苯基)亞磷酸酯、0.010重量份的十八基-3-(3,5-二-三級丁基-4-羥基苯基)丙酸酯,及0.030重量份的四硬脂酸季戊四醇酯,並使用具備排氣孔之Φ30mm雙螺桿擠壓機將所得混合物造粒,及使用N-20C射出模塑機(JSW,Co.,Ltd.製造)在300℃的機筒溫度和80℃的模具溫度射出模塑以製備所要試樣。用此試樣,根據ASTM D256(1/8吋,缺口衝擊)在-30℃下測量低溫衝擊強度。
測定蓄熱穩定性如下。
使用具備排氣孔之Φ30mm雙螺桿擠壓機將實施例和比較例中所製備之共聚碳酸酯和聚碳酸酯組成物造粒,及使用射出模塑機N-20C(JSW,Ltd.製造)而無滯留時間在320℃的機筒溫度和90℃的模具溫度射出模塑以製備所要試樣(寬度/長度/厚度=60mm/40mm/3mm)。使用
Color-Eye 7000A(X-Rite Ltd.製造)根據ASTM D1925測量YI(320℃,0分鐘)。
另外,重複上述程序,但將共聚碳酸酯和聚碳酸酯組成物裝進圓筒並使滯留在其中15分鐘。然後,藉由射出模塑製備試樣(寬度/長度/厚度=60mm/40mm/3mm)。使用Color-Eye 7000A(X-Rite Ltd.製造)根據ASTM D1925測量YI(320℃,15分鐘)。
藉由從YI(320℃,15分鐘)減去YI(320℃,0分鐘所獲得之值表示為△YI。
在此情況下,YI(黃色指數)的測量條件如下。
- 測量溫度:室溫(23℃)
- 孔徑尺寸:大面積的視野
- 測量方法:在螺旋範圍(360nm至750nm)內測量透射率
上述結果係顯示於下表1中。
如上表1中所示,可確認該:與比較例比較,實施例1至3呈現顯著低的△YI,因此呈現顯著高的蓄熱穩定性。
Claims (15)
- 一種共聚碳酸酯,其包含:以芳族聚碳酸酯為基礎之第一重複單元;及一或多種具有矽氧烷鍵且具有如根據下列方程式1測得之0.5至5的△YI之以芳族聚碳酸酯為基礎之第二重複單元,[方程式1]△YI=YI(320℃,15分鐘)-YI(320℃,0分鐘)在方程式1中,YI(320℃,0分鐘)為試樣(寬度/長度/厚度=60mm/40mm/3mm)根據ASTM D1925測得之YI(黃色指數),該試樣係藉由將該共聚碳酸酯在320℃下射出模塑而獲得,及YI(320℃,15分鐘)為試樣(寬度/長度/厚度=60mm/40mm/3mm)根據ASTM D1925測得之YI(黃色指數),該試樣係藉由將該共聚碳酸酯在320℃下滯留15分鐘,然後進行射出模塑而獲得。
- 如申請專利範圍第1項之共聚碳酸酯,其中該共聚碳酸酯具有如根據ASTM D1238(300℃及1.2kg之條件)測得之3至20g/10min的融熔指數。
- 如申請專利範圍第1項之共聚碳酸酯,其中該共聚碳酸酯具有1,000至100,000g/mol之重量平均分子量。
- 如申請專利範圍第1項之共聚碳酸酯,其中該以芳族聚碳酸酯為基礎之第一重複單元的含量相對於該以芳 族聚碳酸酯為基礎之第一重複單元和一或多種具有矽氧烷鍵的以芳族聚碳酸酯為基礎之第二重複單元的總重量為90至99%。
- 如申請專利範圍第1項之共聚碳酸酯,其中該共聚碳酸酯包含二種具有矽氧烷鍵的以芳族聚碳酸酯為基礎之第二重複單元。
- 如申請專利範圍第1項之共聚碳酸酯,其中該第一重複單元係以下列化學式1表示:
- 如申請專利範圍第6項之共聚碳酸酯,其中以化學式1表示之重複單元係衍生自一或多種選自由下列所組成群組之芳族二醇化合物:雙(4-羥基苯基)甲烷、雙(4-羥基苯基)醚、雙(4-羥基苯基)碸、雙(4-羥基苯基)亞碸、雙(4-羥基苯基)硫醚、雙(4-羥基苯基)酮、1,1-雙(4-羥基苯基)乙烷、雙酚A、2,2-雙(4- 羥基苯基)丁烷、1,1-雙(4-羥基苯基)環己烷、2,2-雙(4-羥基-3,5-二溴苯基)丙烷、2,2-雙(4-羥基-3,5-二氯苯基)丙烷、2,2-雙(4-羥基-3-溴苯基)丙烷、2,2-雙(4-羥基-3-氯苯基)丙烷、2,2-雙(4-羥基-3-甲基苯基)丙烷、2,2-雙(4-羥基-3,5-二甲基苯基)丙烷、1,1-雙(4-羥基苯基)-1-苯基乙烷、雙(4-羥基苯基)二苯基甲烷、及α,ω-雙[3-(鄰-羥基苯基)丙基]聚二甲基矽氧烷。
- 如申請專利範圍第6項之共聚碳酸酯,其中該化學式1係以下列化學式1-1表示:
- 如申請專利範圍第1項之共聚碳酸酯,其中該第二重複單元包含以下列化學式2表示之重複單元和以下列化學式3表示之重複單元:
- 如申請專利範圍第9項之共聚碳酸酯,其中該以化學式2表示之重複單元和該以化學式3表示之重複單元的重量比為1:99至99:1。
- 如申請專利範圍第9項之共聚碳酸酯,其中該以化學式2表示之重複單元係以下列化學式2-2表示:
- 如申請專利範圍第9項之共聚碳酸酯,其中該以化學式3表示之重複單元係以下列化學式3-2表示:
- 一種聚碳酸酯組成物,其包含申請專利範圍第1至12項中任一項之共聚碳酸酯,及聚碳酸酯。
- 如申請專利範圍第13項之聚碳酸酯組成物,其中聚矽氧烷結構不被引入該聚碳酸酯之主鏈中。
- 如申請專利範圍第13項之聚碳酸酯組成物,其中該聚碳酸酯包含以下列化學式4表示之重複單元:
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