TW202225221A - 液晶裝置用膜、液晶裝置、及調光裝置 - Google Patents
液晶裝置用膜、液晶裝置、及調光裝置 Download PDFInfo
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- TW202225221A TW202225221A TW110141655A TW110141655A TW202225221A TW 202225221 A TW202225221 A TW 202225221A TW 110141655 A TW110141655 A TW 110141655A TW 110141655 A TW110141655 A TW 110141655A TW 202225221 A TW202225221 A TW 202225221A
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- liquid crystal
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- plasticizer
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Abstract
本發明係一種液晶裝置用膜,其係用於液晶裝置之膜,含有熱塑性樹脂,與液晶接觸時之NI點變化為-2℃~+2℃。
Description
本發明係關於一種液晶裝置用膜、及具有液晶裝置用膜之液晶裝置及調光裝置。
於窗玻璃、特別是汽車用窗玻璃中,廣泛使用2片玻璃板經由中間膜接著而成之層合玻璃。層合玻璃用中間膜為了確保耐貫通性、與玻璃之接著性、衝擊吸收性,一般使用摻合有塑化劑之聚乙烯縮醛樹脂等熱塑性樹脂。
另一方面,已研究於窗玻璃等透明構件導入具備液晶層之調光膜以便可調整透光性等,對於層合玻璃,亦已研究於中間膜中組入調光膜。
例如,於專利文獻1中揭示有一種設置有層壓於第1及第2玻璃層間之中間層構造之層壓窗板,其中,液晶膜內置於中間層構造之內部。中間層構造具備配置於液晶膜外周側之邊框狀之第1中間層、及以將液晶膜配置於其間之方式積層之第2及第3中間層。又,於專利文獻2示出:於2片玻璃板之間配置由液晶膜等所構成之2個調光單元,並且於各玻璃板與調光單元之間或調光單元彼此之間配置中間膜,玻璃板與調光單元或調光單元彼此經由中間膜接合。
組入有調光膜之中間膜構造有時存在低分子成分溶出至液晶,而產生液晶污染之情況。若低分子成分溶出至液晶,則液晶之相轉移被阻礙,成為顯示不均等之原因。因此,於專利文獻1中示出:中間層材料之成分不含塑化劑,或者以不於液晶膜內移動之方式含有塑化劑。又,專利文獻2亦使用中間膜不含塑化劑者。
先前技術文獻
專利文獻
專利文獻1:日本特表2009-534557號公報
專利文獻2:日本特開2020-030355號公報
[發明所欲解決之課題]
然而,於專利文獻1、2中並未示出中間層或中間膜之詳細組成,於專利文獻1、2之揭示內容中,不明確是否可適當地防止液晶污染,需進一步改善。
因此,本發明之課題在於提供一種可防止液晶裝置中之液晶污染,抑制顯示不均等缺陷之液晶裝置用膜。
[解決課題之技術手段]
本發明人等經深入研究,結果發現藉由將液晶裝置用膜與液晶接觸時之NI點變化抑制於一定範圍內,可解決上述課題,從而完成以下之本發明。即,本發明之主旨如以下之[1]至[30]。
[1]一種液晶裝置用膜,其係用於液晶裝置者,含有熱塑性樹脂,且
液晶裝置用膜與液晶接觸時之NI點變化為-2℃~+2℃。
[2]如上述[1]中所記載之液晶裝置用膜,其不含塑化劑,或者含有具有羥基之塑化劑及不具有羥基之塑化劑之至少任一者,
上述具有羥基之塑化劑之含量相對於上述熱塑性樹脂100質量份為70質量份以下,且
上述不具有羥基之塑化劑之含量相對於上述熱塑性樹脂100質量份為25質量份以下。
[3]如上述[2]中所記載之液晶裝置用膜,其不含塑化劑,或者含有相對於熱塑性樹脂100質量份為70質量份以下之含有羥基之塑化劑。
[4]如上述[1]至[3]中任一項所記載之液晶裝置用膜,其中,上述熱塑性樹脂為選自由聚乙烯縮醛系樹脂、離子聚合物樹脂、聚胺酯樹脂、聚烯烴樹脂及乙烯-乙酸乙烯酯共聚樹脂所組成之群中之至少1種。
[5]如上述[4]中所記載之液晶裝置用膜,其中,上述熱塑性樹脂為聚乙烯縮醛系樹脂。
[6]如上述[4]或[5]中所記載之液晶裝置用膜,其中,上述聚乙烯縮醛系樹脂包含具有縮醛基、乙醯基及羥基以外之單元之改質聚乙烯縮醛樹脂。
[7]如上述[4]至[6]中任一項所記載之液晶裝置用膜,其中,上述聚乙烯縮醛系樹脂具有聚氧伸烷基。
[8]如上述[4]至[7]中任一項所記載之液晶裝置用膜,其中,上述聚乙烯縮醛系樹脂於側鏈具有構成縮醛基及乙醯基之烴基以外之烴基或聚氧伸烷基之至少任一者。
[9]如上述[8]中所記載之液晶裝置用膜,其中,上述烴基或聚氧伸烷基之至少任一者藉由酯鍵、醚鍵、-CH
2O-、-CH
2CH
2O-、-CONH-及胺酯鍵之任一連結基與主鏈連結。
[10]如上述[8]或[9]中所記載之液晶裝置用膜,其中,上述烴基之碳數為2~30。
[11]如上述[7]至[10]中任一項所記載之液晶裝置用膜,其中,上述聚氧伸烷基經由醚鍵及-CH
2O-之任一者連結於主鏈。
[12]如上述[7]至[11]中任一項所記載之液晶裝置用膜,其中,利用上述選自由烴基及聚氧伸烷基所組成之群中之官能基所得之改質量例如為0.2莫耳%以上25莫耳%以下。
[13]如上述[7]至[12]中任一項所記載之液晶裝置用膜,其中,利用上述聚氧伸烷基所得之改質量為0.2莫耳%以上12莫耳%以下。
[14]如上述[7]至[13]中任一項所記載之液晶裝置用膜,其中,上述聚氧伸烷基之平均重複數為4~120。
[15]如上述[4]至[14]中任一項所記載之液晶裝置用膜,其中,上述聚乙烯縮醛系樹脂之縮醛化度為40莫耳%以上90莫耳%以下。
[16]如上述[4]至[15]中任一項所記載之液晶裝置用膜,其中,上述聚乙烯縮醛系樹脂之羥基量為0莫耳%以上35莫耳%以下。
[17]如上述[1]至[16]中任一項所記載之液晶裝置用膜,其玻璃轉移溫度為55℃以下。
[18]如上述[1]至[17]中任一項所記載之液晶裝置用膜,其中,上述NI點變化為-1℃~+1℃。
[19]如上述[1]至[18]中任一項所記載之液晶裝置用膜,其中,測定上述NI點變化時所使用之液晶為Chisso公司製造之「JC-5001LA」。
[20]如上述[1]至[19]中任一項所記載之液晶裝置用膜,其玻璃轉移溫度為5℃以上。
[21]如上述[1]至[20]中任一項所記載之液晶裝置用膜,其含有具有羥基之塑化劑,且具有羥基之塑化劑之含量相對於熱塑性樹脂100質量份為5質量份以上。
[22]如上述[1]至[21]中任一項所記載之液晶裝置用膜,其含有具有羥基之塑化劑,且上述具有羥基之塑化劑為選自由(聚)醚多元醇、聚酯多元醇及(聚)醚多元醇之醚化合物所組成之群中之至少1種。
[23]如上述[1]至[22]中任一項所記載之液晶裝置用膜,其含有不具有羥基之塑化劑,且上述不具有羥基之塑化劑為有機酯塑化劑。
[24]如上述[1]至[23]中任一項所記載之液晶裝置用膜,其具有100 μm以上2000 μm以下之厚度。
[25]如上述[1]至[24]中任一項所記載之液晶裝置用膜,其係液晶調光單元用。
[26]一種液晶裝置,其設置有上述[1]至[25]中任一項所記載之液晶裝置用膜。
[27]一種調光裝置,其具備上述[25]中所記載之液晶裝置用膜及液晶調光單元。
[28]如上述[27]中所記載之調光裝置,其進而具備2片透明板及中間膜,上述液晶調光單元配置於2片透明板之間,上述中間膜配置於上述透明板之至少一者與液晶調光單元之間而將該等接合,且
上述中間膜包含上述液晶裝置用膜。
[29]如上述[27]或[28]中所記載之調光裝置,其進而具備2片透明板及中間膜,於上述2片透明板之間設置2個以上之上述液晶調光單元,上述中間膜配置於液晶調光單元彼此之間而將該等接合,且
上述中間膜包含上述液晶裝置用膜。
[30]一種電子裝置用膜,其係用於電子裝置者,
含有熱塑性樹脂,且
不含塑化劑,或者含有具有羥基之塑化劑及不具有羥基之塑化劑之至少任一者,
上述具有羥基之塑化劑之含量相對於上述熱塑性樹脂100質量份為70質量份以下,
上述不具有羥基之塑化劑之含量相對於上述熱塑性樹脂100質量份為25質量份以下。
[發明之效果]
於本發明中,提供一種可防止液晶裝置中之液晶污染,且抑制顯示不均等缺陷之液晶裝置用膜。
<液晶裝置用膜>
本發明之液晶裝置用膜含有熱塑性樹脂,使液晶裝置用膜與液晶接觸時之NI點變化為-2℃~+2℃。
此處,所謂NI點係液晶自向列相相轉移至各向同性相(isotropic phase)時之溫度,可使用示差熱分析裝置(DSC)並根據吸熱峰頂來測定。液晶之NI點由液晶之各成分之混合組成決定,基於各組成而成為固有之值。另一方面,若塑化劑等物質混合於液晶中而污染液晶,則NI點大幅度變化。因此,藉由觀察NI點變化,可評價對液晶之污染程度。並且,於本發明中,若使液晶裝置用膜與液晶接觸時之NI點變化為-2℃~+2℃,則即便在與液晶裝置接觸或接近之環境下使用液晶裝置用膜,亦可不污染液晶而防止顯示不均等缺陷。
就更有效地防止液晶污染之觀點而言,NI點變化較佳為-1.5℃~+1.5℃,更佳為-1℃~+1℃,進而較佳為-0.5℃~+0.5℃,特佳為-0.3℃~+0.3℃。
於本發明中,上述NI點變化可藉由適宜地調整熱塑性樹脂之構成、塑化劑之有無及塑化劑之種類與量而調整至上述範圍內。
再者,NI點變化可藉由如下方式求出:將添加有液晶裝置用膜及液晶(Chisso公司製造之「JC-5001LA」)之樣品瓶於100℃放置1小時,其後,恢復至室溫(25℃)後取出液晶部分,製成評價用液晶樣品,測定空白液晶及評價用液晶樣品之NI點,算出其差。測定條件之詳細情況如實施例所記載。再者,液晶亦可使用4-氰基-4'-戊基聯苯(5CB)代替上述「JC-5001LA」。
[玻璃轉移溫度]
本發明之液晶裝置用膜之玻璃轉移溫度(Tg)例如為75℃以下,較佳為55℃以下。液晶裝置用膜藉由使玻璃轉移溫度(Tg)為55℃以下,柔軟性提高,且可改善衝擊吸收性或用於中間膜時之耐貫通性。進而,即便於80℃左右之相對低溫進行熱壓接合,亦可以較高之接著力接著於玻璃板或構成液晶裝置之基材(基材膜或塑膠基板等)等。再者,一般而言,液晶裝置若加熱至高溫則有時會損傷,但若如上所述藉由低溫之熱壓接合進行接著,則可不損傷而藉由液晶裝置用膜使液晶裝置接合於玻璃板等其他構件。
就接著性、耐貫通性、衝擊吸收性等觀點而言,上述玻璃轉移溫度(Tg)更佳為50℃以下,進而較佳為45℃以下。
液晶裝置用膜之玻璃轉移溫度(Tg)之下限值並無特別限定,就不表現出黏著性等而改善使用性之觀點及容易將NI點變化調整至上述範圍內之觀點而言,例如為5℃以上,較佳為10℃以上,更佳為15℃以上。
再者,液晶裝置用膜之玻璃轉移溫度可藉由如下方式檢測出:使用動態黏彈性測定裝置進行黏彈性測定,讀取由黏彈性測定之結果所獲得之損耗正切tanδ之峰值溫度。測定條件之詳細情況如實施例所記載。
[熱塑性樹脂]
液晶裝置用膜中所含有之熱塑性樹脂較佳為自聚乙烯縮醛系樹脂、離子聚合物樹脂、聚胺酯樹脂、聚烯烴樹脂、及乙烯-乙酸乙烯酯共聚樹脂中選擇。藉由使用該等樹脂,改善對玻璃板或構成液晶裝置之基材等之接著性,並且容易將NI點變化調整至特定範圍內。該等熱塑性樹脂可單獨使用1種,亦可併用2種以上。該等中,較佳為聚乙烯縮醛系樹脂。藉由使用聚乙烯縮醛系樹脂,可對玻璃板或構成液晶裝置之基材等發揮優異之接著性。
(聚乙烯縮醛系樹脂)
液晶裝置用膜所使用之聚乙烯縮醛系樹脂可為改質聚乙烯縮醛樹脂,亦可為未改質聚乙烯縮醛樹脂。
聚乙烯縮醛系樹脂典型地於側鏈具有縮醛基、羥基及乙醯基,改質聚乙烯縮醛樹脂具有該等以外之單元,典型地於側鏈具有該等以外之單元。改質聚乙烯縮醛樹脂較佳為典型地於側鏈具有烴基或聚氧伸烷基作為上述以外之單元。再者,此處所謂之烴基為除構成縮醛基及乙醯基之烴基以外之烴基,於以下之聚乙烯縮醛樹脂之說明中,在敍述為「烴基」之情形時,除說明縮醛基及乙醯基之烴基之情形以外,亦為相同之意義。
藉由使聚乙烯縮醛系樹脂具有烴基或聚氧伸烷基,即便液晶裝置用膜不含塑化劑,或者含有少量塑化劑,亦可降低玻璃轉移溫度(Tg),確保一定之柔軟性,並且改善與構成液晶裝置之基材或玻璃板等之接著性。
又,聚乙烯縮醛系樹脂較佳為上述中於側鏈具有聚氧伸烷基之改質聚乙烯縮醛樹脂。
未改質聚乙烯縮醛樹脂係利用醛使聚乙烯醇縮醛化而獲得者。改質聚乙烯縮醛樹脂例如係利用醛使聚乙烯醇縮醛化,進而使其與改質劑反應而獲得者。又,改質聚乙烯縮醛樹脂可為使用改質聚乙烯醇作為成為原料之聚乙烯醇,利用醛使該改質聚乙烯醇縮醛化而獲得者。
縮醛基、羥基及乙醯基以外之單元較佳為藉由酯鍵、醚鍵、-CH
2O-、-CH
2CH
2O-、-CONH-及胺酯鍵之任一連結基與主鏈連結。更具體而言,較佳為烴基及聚氧伸烷基之任一者經由上述連結基與主鏈連結。再者,-CH
2O-為碳原子連結於主鏈即可。同樣地,-CH
2CH
2O-及-CONH-亦為碳原子連結於主鏈即可。又,烴基例如碳數為2~30。藉由使液晶裝置用膜中所包含之聚乙烯縮醛系樹脂具有以上之結構,可降低玻璃轉移溫度(Tg),提高柔軟性,並且改善與構成液晶裝置之基材或玻璃板等之接著性。
關於聚乙烯縮醛系樹脂中之縮醛基、羥基及乙醯基以外之單元,於包含烴基之情形時,較佳為具有該烴基經由酯鍵及胺酯鍵之任一者連結於主鏈之結構。又,於包含聚氧伸烷基之情形時,較佳為具有聚氧伸烷基經由醚鍵及-CH
2O-之任一者連結於主鏈之結構。
更具體而言,聚乙烯縮醛系樹脂較佳為具有選自以下之式(1-1)~式(1-3)所表示之官能基中之至少1個。藉由使聚乙烯縮醛系樹脂至少具有式(1-1)~(1-3)所表示之官能基,即便不含大量塑化劑,亦可降低液晶裝置用膜之玻璃轉移溫度(Tg),確保一定之柔軟性,且改善與玻璃板或構成液晶裝置之基材等之接著性。又,就接著性等觀點而言,更佳為具有式(1-3)所示之官能基。
(於式(1-1)、(1-2)中,R
1、R
2分別獨立地為碳數為2~30之烴基。於式(1-3)中,Y為氧原子、-CH
2O-、-CH
2CH
2O-或-CONH-之任一者,A
1O為碳數2~4之氧伸烷基,m為平均重複數,為4~120。R
3獨立地為碳數為1~4之烷基或氫原子。再者,氧伸烷基可為單獨1種,亦可混合存在有2種以上,例如氧伸乙基與氧伸丙基等)
R
1、R
2中之烴基可具有芳香環,亦可不具有,較佳為不具有芳香環之脂肪族烴基。藉由使其為脂肪族烴基,容易提昇對聚碳酸酯板等有機玻璃或構成液晶裝置之基材等之接著性。又,脂肪族烴基可為直鏈狀,亦可具有支鏈,還可具有環結構。例如,若脂肪族烴基具有支鏈,則容易降低玻璃轉移溫度(Tg)。
進而,脂肪族烴基可具有不飽和鍵,亦可不具有不飽和鍵。脂肪族烴基較佳為烯基、烷基、炔基,更佳為烷基。
R
1、R
2各者之碳數較佳為3以上,更佳為5以上,進而較佳為7以上,進而更佳為11以上。藉由增大R
1、R
2各者之碳數,液晶裝置用膜之玻璃轉移溫度(Tg)亦容易降低,且容易提昇對有機玻璃等之接著性。
就防止結晶化等而容易提昇透過率之觀點而言,R
1、R
2各者之碳數較佳為24以下,更佳為20以下,進而較佳為18以下。
因此,R
1、R
2分別較佳為碳數3~24之烷基,更佳為碳數5~20之烷基,進而較佳為碳數7~18之烷基,進而更佳為碳數11~18之烷基。
作為R
1、R
2之具體例,可例舉:正丙基、異丙基、正丁基、第二丁基、第三丁基等支鏈丁基、正戊基、支鏈戊基、正己基、支鏈己基、正庚基、異庚基、3-庚基等支鏈庚基、正辛基、異辛基、2-乙基己基等支鏈辛基、正壬基、異壬基等支鏈壬基、正癸基、支鏈癸基、正十一烷基、支鏈十一烷基、正十二烷基、支鏈十二烷基、正十三烷基、支鏈十三烷基、正十四烷基、支鏈十四烷基、正十五烷基、支鏈十五烷基、正十六烷基、支鏈十六烷基、正十七烷基、支鏈十七烷基、正十八烷基、支鏈十八烷基、正十九烷基、支鏈十九烷基、正二十烷基、支鏈二十烷基、正二十一烷基、支鏈二十一烷基、正二十二烷基、支鏈二十二烷基、正二十三烷基、支鏈二十二烷基、正二十四烷基、支鏈二十四烷基、油基(oleyl group)等。
於式(1-3)中,A
1O為碳數2~4之氧伸烷基。碳數2~4之氧伸烷基為氧伸乙基、氧伸丙基或氧伸丁基,較佳為氧伸乙基、氧伸丙基,更佳為氧伸乙基。再者,氧伸烷基可單獨使用1種,亦可併用2種以上,於該情形時,各氧伸烷基可無規地加成,亦可以嵌段加成。
m表示氧伸烷基之平均重複數,為4~120,較佳為8~110,更佳為12~100。
又,關於R
3中之烷基,可例舉:甲基、乙基、正丙基、異丙基、正丁基、第二丁基、第三丁基等。又,R
3為碳數1~4之烷基或氫原子,較佳為碳數1~2之烷基或氫原子,更佳為甲基或氫原子,進而較佳為氫原子。
於式(1-3)中,Y為氧原子(醚鍵)、-CH
2O-、-CH
2CH
2O-或-CONH-之任一者,較佳為氧原子或-CH
2O-之任一者。因此,較佳為以下之式(1-4)、(1-5)所示之官能基。再者,於-CH
2O-及-CH
2CH
2O中,氧原子鍵結於A
1O之碳原子(A
1)即可,於-CONH-中,氮原子鍵結於A
1O之碳原子(A
1)即可。
(於式(1-4)、(1-5)中,A
1O、m及R
3分別與上述相同)
因此,式(1-3)所表示之官能基特佳為-O-(CH
2CH
2O)
m-H所表示之官能基或-CH
2O-(CH
2CH
2O)
m-H所表示之官能基。再者,於該等情形時,m之較佳之範圍亦如上所述。
如上所述,聚乙烯縮醛系樹脂典型地具有縮醛基、羥基及乙醯基。但是,聚乙烯縮醛系樹脂亦可藉由被官能基改質等而不含羥基。
又,聚乙烯縮醛系樹脂藉由進行改質,如上所述,較佳為於側鏈具有烴基或聚氧伸烷基,具體而言,較佳為具有選自上述式(1-1)~式(1-3)所表示之官能基中之至少1種官能基。
再者,關於於側鏈具有烴基或聚氧伸烷基之聚乙烯縮醛系樹脂、典型地具有上述式(1-1)~式(1-3)所表示之官能基之任一者之聚乙烯縮醛系樹脂,為了區別於其他聚乙烯縮醛系樹脂而進行說明,有時會以聚乙烯縮醛系樹脂(A)之形式進行說明。
聚乙烯縮醛系樹脂(A)之利用選自烴基及聚氧伸烷基中之官能基所得之改質量例如為0.2莫耳%以上25莫耳%以下。再者,該改質量典型地為利用上述式(1-1)~式(1-3)所表示之官能基所得之改質量。
藉由將改質量設為上述範圍內,容易降低玻璃轉移溫度(Tg),提昇膜之柔軟性,且亦容易提昇對玻璃板或構成液晶裝置之基材等之接著性。
上述改質量之較佳值根據官能基之種類而有所不同。例如,就上述提昇接著性之觀點等而言,於側鏈具有烴基之聚乙烯縮醛系樹脂(以下,為了方便,有時稱為「聚乙烯縮醛系樹脂(A-1)」)之利用烴基(典型地為式(1-1)及式(1-2)所表示之官能基)所得之改質量較佳為5莫耳%以上25莫耳%以下。又,該改質量更佳為6莫耳%以上,進而較佳為8莫耳%以上,進而更佳為10莫耳%以上,又,較佳為25莫耳%以下,更佳為22莫耳%以下。
又,就上述提昇接著性之觀點而言,於側鏈具有聚氧伸烷基之聚乙烯縮醛系樹脂(以下,為了方便,有時稱為「聚乙烯縮醛系樹脂(A-2)」)之利用聚氧伸烷基(典型地為式(1-3)所表示之官能基)所得之改質量較佳為0.2莫耳%以上12莫耳%以下。又,該改質量更佳為0.5莫耳%以上,進而較佳為0.6莫耳%以上,進而更佳為0.8莫耳%以上,又,更佳為10莫耳%以下,進而較佳為8莫耳%以下,進而更佳為6莫耳%以下。
再者,利用各官能基所得之改質量表示各官能基相對於構成聚乙烯縮醛系樹脂之總乙烯基單體單位之比率,例如,利用式(1-1)及式(1-2)所表示之官能基所得之改質量表示該等官能基之比率之合計量。再者,改質量可對聚乙烯縮醛系樹脂進行質子NMR測定,根據所獲得之光譜而算出。下述縮醛化度、羥基量及乙醯化度亦同樣地,可進行質子NMR測定,根據所獲得之光譜而算出。
聚乙烯縮醛系樹脂可不於側鏈具有聚氧伸烷基、烴基。該種聚乙烯縮醛系樹脂可為具有除聚氧伸烷基、烴基以外之官能基(典型地為除式(1-1)~(1-3)所表示之官能基以外之官能基)之改質聚乙烯縮醛樹脂,亦可為未改質聚乙烯縮醛樹脂。即便為未改質聚乙烯縮醛樹脂,亦如下所述藉由摻合塑化劑,容易降低玻璃轉移溫度(Tg)。
聚乙烯縮醛系樹脂係具有源自乙烯基之構成單位作為主鏈者,式(1-1)~(1-3)所表示之官能基鍵結於構成主鏈之源自乙烯基之構成單位即可。因此,聚乙烯縮醛系樹脂較佳為具有以下之式(2-1)~式(2-3)所表示之構成單位之任一者,更佳為具有式(2-3)所表示之構成單位之任一者。
(於式(2-1)、(2-2)中,R
1、R
2分別與上述相同。於式(2-3)中,Y、A
1O、m及R
3分別與上述相同)
聚乙烯縮醛系樹脂典型地具有縮醛基、羥基及乙醯基,即,聚乙烯縮醛系樹脂典型地具有以下之式(3-1)、式(3-2)及式(3-3)所表示之構成單位。因此,改質聚乙烯縮醛樹脂較佳為具有以下之式(3-1)、式(3-2)及式(3-3)所表示之構成單位及選自上述式(2-1)~式(2-3)中之至少1種構成單位。
其中,如上所述,聚乙烯縮醛系樹脂可不具有羥基,亦可不具有式(3-2)所表示之構成單位。即,聚乙烯縮醛系樹脂具有以下之式(3-1)及式(3-3)所表示之構成單位,較佳為進而具有以下之式(3-2)所表示之構成單位。
如上所述,聚乙烯縮醛系樹脂係利用醛使聚乙烯醇或將聚乙烯醇改質而成之改質聚乙烯醇縮醛化,其後,視需要進行改質而獲得者,聚乙烯醇一般使用皂化度為80~99.8莫耳%之聚乙烯醇。又,為了將聚乙烯縮醛系樹脂之平均聚合度調整至所需範圍內,聚乙烯醇之平均聚合度較佳為300以上5000以下。聚乙烯醇之平均聚合度藉由依據JIS K6726「聚乙烯醇試驗方法」之方法來求出。
聚乙烯縮醛系樹脂中所包含之縮醛基之碳數並無特別限定,如上述式(3-1)所示,例如為1~20,較佳為2~10,更佳為2~6,進而較佳為2、3或4。因此,上述式(3-1)所示之R
5之碳數較佳為1~9,更佳為1~5,進而較佳為1~3。
作為縮醛基,具體而言,特佳為丁醛基,因此,作為聚乙烯縮醛系樹脂,較佳為聚乙烯縮丁醛系樹脂。聚乙烯縮醛系樹脂之縮醛化度(即縮醛基量)較佳為40莫耳%以上90莫耳%以下。又,縮醛化度更佳為55莫耳%以上,進而較佳為60莫耳%以上,又,更佳為85莫耳%以下,進而較佳為83莫耳%以下。藉由將縮醛化度設為該等範圍內,容易將羥基之量設為適度之量,並且含有一定量之式(1-1)~式(1-3)所表示之官能基。
再者,關於縮醛化度,於聚乙烯縮醛系樹脂之縮醛基為乙醯縮醛基之情形時,意指乙醯縮醛化度,於縮醛基為丁醛基之情形時,意指丁醛化度。
又,縮醛化度表示經縮醛化之乙烯醇單位相對於構成聚乙烯縮醛系樹脂之總乙烯基單體單位之比率。
聚乙烯縮醛系樹脂之羥基量較佳為35莫耳%以下。若將羥基量設為35莫耳%以下,則容易降低玻璃轉移溫度(Tg),且提高對聚碳酸酯板等有機玻璃之接著性。就該種觀點而言,於為聚乙烯縮醛系樹脂(A)之情形時,羥基量更佳為30莫耳%以下,進而較佳為25莫耳%以下。
聚乙烯縮醛系樹脂之羥基量為0莫耳%以上即可,於為聚乙烯縮醛系樹脂(A)之情形時,就防止膜變得過於柔軟之觀點而言,含有一定量以上之羥基即可,例如5莫耳%以上,較佳為9莫耳%以上,更佳為11莫耳%以上。
另一方面,如上所述,未改質聚乙烯縮醛樹脂之羥基量較佳為35莫耳%以下,20莫耳%以上亦較佳,更佳為25莫耳%以上。
再者,羥基量表示羥基相對於構成聚乙烯縮醛系樹脂之總乙烯基單體單位之比率。
上述聚乙烯縮醛系樹脂之乙醯化度(乙醯基量)例如為40莫耳%以下,較佳為20莫耳%以下,更佳為10莫耳%以下。藉由將乙醯化度設為上述上限值以下,例如,於為聚乙烯縮醛系樹脂(A)之情形時,可使利用烴基或聚氧伸烷基等官能基所得之改質量為一定值以上。又,聚乙烯縮醛系樹脂之乙醯化度例如為0.01莫耳%以上,較佳為0.1莫耳%以上,更佳為0.5莫耳%以上。
再者,乙醯化度表示乙醯基相對於構成聚乙烯縮醛系樹脂之總乙烯基單體單位之比率。
聚乙烯縮醛系樹脂之平均聚合度較佳為300以上5000以下。藉由將平均聚合度調整至上述範圍內,容易良好地維持機械強度、柔軟性等,並且提昇接著性。聚乙烯縮醛系樹脂之平均聚合度更佳為500以上,進而較佳為700以上。又,藉由降低平均聚合度,可降低玻璃轉移溫度,從而成膜時之加工性等提昇。就此種觀點而言,平均聚合度更佳為4500以下,進而更佳為3500以下。
再者,聚乙烯縮醛系樹脂之平均聚合度與作為原料之聚乙烯醇之平均聚合度相同,可藉由聚乙烯醇之平均聚合度來求出。
製造聚乙烯縮醛系樹脂時所使用之醛並無特別限定,例如為碳數1~20之醛,適宜使用碳數為2~10之醛。上述碳數為2~10之醛並無特別限定,例如可例舉:乙醛、丙醛、正丁醛、異丁醛、正戊醛、2-乙基丁醛、正己醛、正辛醛、正壬醛、正癸醛、苯甲醛等。其中,較佳為乙醛、正丁醛、正己醛、正戊醛等碳數2~6之醛,更佳為碳數2、3、4之醛,進而較佳為正丁醛。該等醛可單獨使用,亦可併用2種以上。
本發明所使用之聚乙烯縮醛系樹脂可單獨使用1種,亦可併用2種以上。
於使用聚乙烯縮醛系樹脂作為熱塑性樹脂之情形時,本發明之液晶裝置用膜可單獨使用聚乙烯縮醛系樹脂,亦可與除聚乙烯縮醛系樹脂以外之熱塑性樹脂併用。除聚乙烯縮醛系樹脂以外之熱塑性樹脂可自上述熱塑性樹脂中適宜地選擇。其中,較佳為聚乙烯縮醛系樹脂為主成分。具體而言,聚乙烯縮醛系樹脂之合計量以液晶裝置用膜中所含有之樹脂總量為基準,例如為50質量%以上,較佳為70質量%以上,更佳為90質量%以上,最佳為100質量%。
《聚乙烯縮醛系樹脂之製造方法》
於本發明中,用於液晶裝置用膜之聚乙烯縮醛系樹脂係利用醛使聚乙烯醇(亦稱為「原料聚乙烯醇」)縮醛化,其後,視需要使其與改質劑反應而成者。原料聚乙烯醇可為未改質聚乙烯醇,於獲得改質聚乙烯縮醛樹脂之情形時,亦可使用改質聚乙烯醇作為原料聚乙烯醇。
具體而言,例如,製造具有選自上述式(1-1)及式(1-2)所表示之官能基中之至少1種之聚乙烯縮醛系樹脂(改質聚乙烯縮醛樹脂(A-1))時,較佳為藉由以下之製造方法(1)來製造。
(製造方法(1))
於本製造方法(1)中,利用醛使原料聚乙烯醇縮醛化,而獲得聚乙烯縮醛系樹脂(以下,亦稱為原料聚乙烯縮醛系樹脂)。此處所使用之原料聚乙烯醇係使聚乙烯酯皂化而獲得者,較佳為未改質聚乙烯醇。
其次,使具有R
1或R
2之改質劑與上述原料聚乙烯縮醛系樹脂進行反應,而將式(1-1)及式(1-2)所表示之官能基之至少任一者導入至原料聚乙烯縮醛系樹脂中。此處,作為改質劑,為與原料聚乙烯縮醛系樹脂所具有之羥基進行反應,而形成式(1-1)所示之胺酯鍵或者形成式(1-2)所示之酯鍵的具有反應性基之化合物即可。
具體而言,作為與羥基進行反應而形成胺酯鍵之具有反應性基之化合物,可例舉R
1-NCO(其中,R
1與上述相同)所表示之異氰酸酯化合物。異氰酸酯化合物與原料聚乙烯縮醛系樹脂所具有之羥基之反應性較高,可容易地導入式(1-1)所表示之官能基。
又,作為與羥基進行反應而形成酯鍵之具有反應性基之化合物,可例舉R
2-COOH(其中,R
2與上述相同)所表示之羧酸或羧酸酐、羧酸酯、羧酸鹵化物等羧酸衍生物。該等中,較佳為R
2-COX(其中,R
2與上述相同,X為鹵素原子)所表示之羧酸鹵化物,更佳為X為氯原子之羧酸氯化物。羧酸氯化物等羧酸鹵化物與原料聚乙烯縮醛系樹脂所具有之羥基之反應性較高,可容易地導入式(1-2)所表示之官能基。
作為較佳之異氰酸酯化合物之具體例,可例舉異氰酸己酯、異氰酸2-乙基己酯、異氰酸正辛酯、異氰酸正壬酯、異氰酸正癸酯、異氰酸正十一烷基酯、異氰酸正十二烷基酯、異氰酸正十四烷基酯、異氰酸正十六烷基酯、異氰酸正十八烷基酯、異氰酸正二十烷基酯等異氰酸烷基酯,較佳為異氰酸正十八烷基酯。
又,作為較佳之羧酸氯化物,可例舉:2-乙基己醯氯、正辛醯氯、正壬醯氯、正癸醯氯、正十一碳醯氯、月桂醯氯、肉豆蔻醯氯、棕櫚醯氯、異棕櫚醯氯、硬脂醯氯、異硬脂醯氯、油醯氯、二十二醯氯等。該等中,較佳為2-乙基己醯氯、月桂醯氯、肉豆蔻醯氯、棕櫚醯氯、硬脂醯氯之任一者,更佳為月桂醯氯、肉豆蔻醯氯、棕櫚醯氯。
於上述製造方法(1)中,原料聚乙烯縮醛系樹脂與異氰酸酯化合物或羧酸鹵化物等改質劑之反應並無特別限定,例如,將原料聚乙烯縮醛系樹脂及改質劑於溶劑下例如加熱至30℃以上150℃以下、較佳為加熱至50℃以上140℃以下左右而進行即可。反應可於鹼或酸存在下等進行,鹼例如使用吡啶等。
其中,製造改質聚乙烯縮醛樹脂(A-1)之方法並不限定於上述,亦可如以下之製造方法(2)所示般獲得改質聚乙烯醇,使該改質聚乙烯醇縮醛化而製造。
(製造方法2)
於本製造方法(2)中,首先,製造改質聚乙烯醇作為原料聚乙烯醇。具體而言,使改質劑與使聚乙烯酯皂化而獲得之未改質聚乙烯醇進行反應,向聚乙烯醇之側鏈之一部分導入式(1-1)或式(1-2)之官能基。再者,改質劑之具體例如上述製造方法(1)所示。然後,利用醛使所獲得之改質聚乙烯醇縮醛化,而獲得聚乙烯縮醛系樹脂(A)。
又,例如,製造具有上述式(1-3)所表示之官能基之至少任一者之聚乙烯縮醛系樹脂(改質聚乙烯縮醛樹脂(A-2))時,較佳為藉由以下之製造方法(3)來製造。
(製造方法(3))
於本製造方法(3)中,首先,製造聚氧伸烷基改質聚乙烯醇作為原料聚乙烯醇。具體而言,可藉由如下方式獲得:使乙烯酯與具有聚氧伸烷基且具有雙鍵之單體聚合而獲得聚合物後,對聚合物進行皂化。皂化一般使用鹼或酸,較佳為使用鹼。PVA系聚合物可僅使用1種,亦可併用2種以上。
繼而,利用醛對上述所獲得之聚氧伸烷基改質聚乙烯醇進行縮醛化,而獲得改質聚乙烯縮醛樹脂(A-2)即可。關於縮醛化之方法,以公知之方法進行即可。
製造方法(3)所使用之乙烯酯可使用乙酸乙烯酯、甲酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、異丁酸乙烯酯、三甲基乙酸乙烯酯、叔羧酸(versatic acid)乙烯酯、己酸乙烯酯、辛酸乙烯酯、月桂酸乙烯酯、棕櫚酸乙烯酯、硬脂酸乙烯酯、油酸乙烯酯、苯甲酸乙烯酯等。該等中,較佳為乙酸乙烯酯。
又,作為製造方法(3)所使用之具有聚氧伸烷基且具有雙鍵之單體,可例舉具有乙烯基之乙烯基單體等,具體而言,可例舉以下之式(4)所示之單體。
上述具有聚氧伸烷基且具有雙鍵之單體較佳為如上所述Y為氧原子之乙烯醚、Y為-CH
2O-之烯丙醚。作為較佳之具體例,可例舉聚氧乙烯單乙烯醚、聚氧乙烯聚氧丙烯單乙烯醚、聚氧丙烯單乙烯醚、聚氧乙烯單烯丙醚、聚氧乙烯聚氧丙烯單烯丙醚、聚氧丙烯單烯丙醚,該等中,更佳為聚氧乙烯單乙烯醚、聚氧乙烯單烯丙醚、聚氧丙烯單乙烯醚、聚氧丙烯單烯丙醚、聚氧乙烯聚氧丙烯單烯丙醚。
(乙烯-乙酸乙烯酯共聚物樹脂)
乙烯-乙酸乙烯酯共聚物樹脂可為非交聯型之乙烯-乙酸乙烯酯共聚物樹脂,又,亦可為高溫交聯型之乙烯-乙酸乙烯酯共聚物樹脂。乙烯-乙酸乙烯酯共聚物樹脂亦可使用如乙烯-乙酸乙烯酯共聚物皂化物、乙烯-乙酸乙烯酯之水解物等之乙烯-乙酸乙烯酯改質體樹脂。
乙烯-乙酸乙烯酯共聚物樹脂之依據JIS K 6730「乙烯-乙酸乙烯酯樹脂試驗方法」或JIS K 6924-2:1997所測得之乙酸乙烯酯含量較佳為10質量%以上50質量%以下,更佳為25質量%以上45質量%以下。藉由將乙酸乙烯酯含量設為該等下限值以上,對玻璃之接著性提高,又,用於層合玻璃時,容易改善層合玻璃之耐貫通性。又,藉由將乙酸乙烯酯含量設為該等上限值以下,樹脂層之斷裂強度提高,改善層合玻璃之耐衝擊性。
(離子聚合物樹脂)
離子聚合物樹脂並無特別限定,可使用各種離子聚合物樹脂。具體而言,可例舉:乙烯系離子聚合物、苯乙烯系離子聚合物、全氟碳系離子聚合物、遙爪離子聚合物、聚胺酯離子聚合物等。該等中,就改善下述層合玻璃之機械強度、耐久性、透明性等之方面、對玻璃之接著性優異之方面而言,較佳為乙烯系離子聚合物。
關於乙烯系離子聚合物,乙烯-不飽和羧酸共聚物之離子聚合物由於透明性及強韌性優異而適宜使用。乙烯-不飽和羧酸共聚物為至少具有源自乙烯之構成單位及源自不飽和羧酸之構成單位之共聚物,亦可具有源自其他單體之構成單位。
作為不飽和羧酸,可例舉丙烯酸、甲基丙烯酸、馬來酸等,較佳為丙烯酸、甲基丙烯酸,特佳為甲基丙烯酸。又,作為其他單體,可例舉丙烯酸酯、甲基丙烯酸酯、1-丁烯等。
關於乙烯-不飽和羧酸共聚物,若將該共聚物所具有之總構成單位設為100莫耳%,則較佳為具有75~99莫耳%之源自乙烯之構成單位,且較佳為具有1~25莫耳%之源自不飽和羧酸之構成單位。
乙烯-不飽和羧酸共聚物之離子聚合物係利用金屬離子對乙烯-不飽和羧酸共聚物所具有之羧基之至少一部分進行中和或交聯而獲得之離子聚合物樹脂,該羧基之中和度通常為1~90%,較佳為5~85%。
作為離子聚合物樹脂中之離子源,可例舉鋰、鈉、鉀、銣、銫等鹼金屬、鎂、鈣、鋅等多價金屬,較佳為鈉、鋅。
離子聚合物樹脂之製造方法並無特別限定,可藉由習知公知之製造方法來製造。例如,於使用乙烯-不飽和羧酸共聚物之離子聚合物作為離子聚合物樹脂之情形時,例如,使乙烯及不飽和羧酸於高溫、高壓下進行自由基共聚,製造乙烯-不飽和羧酸共聚物。繼而,使該乙烯-不飽和羧酸共聚物與包含上述離子源之金屬化合物進行反應,藉此可製造乙烯-不飽和羧酸共聚物之離子聚合物。
(聚胺酯樹脂)
作為聚胺酯樹脂,可例舉:使異氰酸酯化合物與二醇化合物進行反應而獲得之聚胺酯;使異氰酸酯化合物、二醇化合物、進而多胺等擴鏈劑進行反應而獲得之聚胺酯等。又,聚胺酯樹脂可含有硫原子。於該情形時,使上述二醇之一部分或全部為選自聚硫醇及含硫多元醇中者即可。聚胺酯樹脂可改善與有機玻璃之接著性。因此,適宜用於接著於有機玻璃之用途。
(聚烯烴系樹脂)
聚烯烴系樹脂可為聚乙烯系樹脂、聚丙烯系樹脂、聚丁烯系樹脂、聚(4-甲基戊烯-1)系樹脂等,亦可為環狀烯烴系共聚物等。
[塑化劑]
本發明之液晶裝置用膜可含有塑化劑,亦可不含塑化劑。若液晶裝置用膜含有塑化劑,則可降低玻璃轉移溫度,柔軟性可提高。因此,容易改善接著性、耐貫通性、衝擊吸收性等。於使用塑化劑之情形時,較佳為與聚乙烯縮醛系樹脂併用。藉由將塑化劑與聚乙烯縮醛系樹脂併用,容易更進一步提昇接著性。
另一方面,藉由使液晶裝置用膜不含塑化劑,可防止因塑化劑所導致之液晶污染,減小上述NI點變化。又,若液晶裝置用膜含有塑化劑,則有時會浸蝕有機玻璃或構成液晶裝置之基材(基材膜或塑膠基板等),但藉由不含塑化劑,亦可防止浸蝕有機玻璃或基材。
塑化劑可為具有羥基之塑化劑、不具有羥基之塑化劑之任一者,較佳為具有羥基之塑化劑。具有羥基之塑化劑可提高液晶裝置用膜之柔軟性,可抑制溶出至液晶而抑制NI點變化。又,亦可抑制對有機玻璃或構成液晶裝置之基材之浸蝕。進而,對玻璃之接著性等亦容易改善。
另一方面,不具有羥基之塑化劑容易溶出至液晶,成為使液晶之NI點改變之主要原因,若為相對少量,則NI點變化亦較小而可使用。又,不具有羥基之塑化劑若為相對少量,則亦可抑制對有機玻璃或構成液晶裝置之基材之浸蝕。
就以上之觀點而言,本發明之液晶裝置用膜較佳為不含塑化劑之形態或僅含少量塑化劑之形態。
又,於液晶裝置用膜含有塑化劑之情形時,較佳為使用含有羥基之塑化劑之形態,於該情形時,液晶裝置用膜亦可相對大量地含有具有羥基之塑化劑。具體而言,於使用具有羥基之塑化劑之情形時,液晶裝置用膜中之具有羥基之塑化劑之含量較佳為相對於熱塑性樹脂100質量份為70質量份以下。藉由將其設為70質量份以下,可降低玻璃轉移溫度,並且抑制塑化劑溶出至液晶,亦可將NI點變化抑制為較小。進而,亦可抑制對有機玻璃或構成液晶裝置之基材等之浸蝕。就以上之觀點而言,含有羥基之塑化劑之含量相對於熱塑性樹脂100質量份,更佳為60質量份以下,進而較佳為50質量份以下。
又,於液晶裝置用膜含有具有羥基之塑化劑之情形時,其含量相對於熱塑性樹脂100質量份,較佳為5質量份以上,更佳為10質量份以上,進而較佳為15質量份以上。藉由將具有羥基之塑化劑之含量設為該等下限值以上,可充分降低玻璃轉移溫度,改善柔軟性、接著性等。
另一方面,於使用不具有羥基之塑化劑之情形時,不含羥基之塑化劑之使用量為少量即可。具體而言,於液晶裝置用膜中,不含羥基之塑化劑之含量相對於熱塑性樹脂100質量份為25質量份以下即可。若為25質量份以下,則即便為不具有羥基之塑化劑,亦可相對抑制NI點變化,使NI點變化處於上述範圍內。又,亦可抑制對有機玻璃或構成液晶裝置之基材等之浸蝕。
就該等觀點而言,不含羥基之塑化劑之含量相對於熱塑性樹脂100質量份,較佳為20質量份以下,更佳為10質量份以下,進而較佳為5質量份以下,進而更佳為3質量份以下,最佳為0質量份。即,液晶裝置用膜最佳為不含不具有羥基之塑化劑。
電子裝置用膜可僅含有具有羥基之塑化劑及不具有羥基之塑化劑之任一者,亦可併用該等。於併用之情形時,各塑化劑(具有羥基之塑化劑及不具有羥基之塑化劑)之含量如上所述即可。其中,就降低玻璃轉移溫度並提昇柔軟性、接著性,並且抑制NI點變化,進而抑制對有機玻璃或基材之浸蝕之觀點而言,併用時之塑化劑之含量合計相對於熱塑性樹脂100質量份,較佳為70質量份以下,更佳為60質量份以下,進而較佳為50質量份以下,又,較佳為10質量份以上,更佳為20質量份以上,進而較佳為30質量份以上。
《含有羥基之塑化劑》
作為具有羥基之塑化劑,可例舉:(聚)醚多元醇、聚酯多元醇等多元醇或(聚)醚多元醇之醚化合物等。(聚)醚多元醇為具有1個或2個以上之醚基之多元醇,可例舉(聚)伸烷基二醇等。作為(聚)醚多元醇之醚化合物,可例舉聚氧伸烷基醚等。
作為(聚)伸烷基二醇,具體而言可例舉選自乙二醇、1,2-丙二醇、1,3-丙二醇、丁二醇等中之1種以上之單獨之化合物或其聚合物,具體的是聚乙二醇、聚丙二醇、聚(環氧乙烷/環氧丙烷)嵌段或無規共聚物等,進而亦可為聚四亞甲基醚二醇等。
聚氧伸烷基醚為一元或多元醇與聚氧伸烷基之醚化合物。例如可例舉:聚氧乙烯己醚、聚氧乙烯庚醚、聚氧乙烯辛醚、聚氧乙烯-2-乙基己醚、聚氧乙烯壬醚、聚氧乙烯癸醚、聚氧乙烯烯丙醚、聚氧丙烯烯丙醚、聚氧乙烯甘油醚、聚氧丙烯甘油醚、聚氧乙烯雙甘油醚、聚氧丙烯雙甘油醚、聚氧伸烷基新戊四醇醚等。作為聚氧伸烷基醚,較佳為多元醇與聚氧伸烷基之醚化合物,更佳為甘油或雙甘油與聚氧伸烷基之醚化合物,進而較佳為甘油或雙甘油與聚氧丙烯之醚化合物。
聚酯多元醇有多元羧酸與多元醇之縮合系、利用ε-己內酯之聚合所得之內酯系等。於縮合系中,多元羧酸較佳為二羧酸。作為多元羧酸之例子,可例舉:對苯二甲酸、間苯二甲酸、己二酸、1,2,4-苯三甲酸、檸檬酸等。作為多元醇,可例舉:乙二醇、二乙二醇、丙二醇、丁二醇、新戊二醇、1,6-己二醇、辛二醇、甘油、新戊四醇等。
又,作為內酯系,可例舉:聚丙內酯二醇、聚丁內酯二醇、聚己內酯二醇(polyhexanolactone diol)、聚己內酯二醇(polycaprolactone diol)等。又,作為聚酯多元醇,亦可例舉:聚乳酸交酯(polylactide)、聚乙交酯(polyglycolide)、聚二氧雜環己酮、聚(乳酸交酯-共聚-乙交酯)(poly(lactide-co-glycolide))等。
作為含有羥基之塑化劑,此外亦可例舉:辛醇、癸醇、月桂醇、肉豆蔻醇、鯨蠟醇、鯨蠟硬脂醇、硬脂醇、二十二醇、2-己基-1-癸醇、2-辛基十二烷醇、鄰苯二甲酸羥基乙酯2-乙基己酯等。
含有羥基之塑化劑可單獨使用1種,亦可併用2種以上。
具有羥基之塑化劑於分子中具有至少1個羥基即可,羥基之數量所表示之平均官能基數較佳為具有2個以上,更佳為2~4。
含有羥基之塑化劑並無特別限定,分子量較佳為150~10000,更佳為200~5000。若分子量為該等下限值以上,則與液晶之相溶性降低,可防止因塑化劑所導致之液晶污染,抑制產生NI點變化。又,藉由使分子量為10000以下,改善與聚乙烯縮醛系樹脂等熱塑性樹脂之相溶性,可確保液晶裝置用膜之透明性。
再者,關於上述分子量,於為單體且可特定出式量之情形時,為以式量求出之分子量,於為混合物之情形時,為數量平均分子量即可。又,關於多元醇,測定羥值(mgKOH/g)並藉由下式求出即可。
數量平均分子量=羥值×N×1,000/56.11
N:多元醇之平均官能基數
再者,羥值藉由JIS K 1557-1測定即可。
《不具有羥基之塑化劑》
作為不具有羥基之塑化劑,例如可例舉有機酯塑化劑、以及有機磷酸塑化劑及有機亞磷酸塑化劑等磷系塑化劑等。塑化劑可單獨使用1種,亦可併用2種以上。其中,較佳為有機酯塑化劑。作為有機酯塑化劑,可例舉一元有機酸酯及多元有機酸酯等。
作為一元有機酸酯,可例舉二醇與一元有機酸之酯。作為二醇,可例舉:各伸烷基單位之碳數為2~4、較佳為碳數為2或3,且伸烷基單位之重複數為2~10、較佳為2~4之聚伸烷基二醇。又,二醇亦可為碳數2~4、較佳為碳數2或3之單伸烷基二醇(即,重複單位為1)。
作為二醇,具體而言可例舉:乙二醇、二乙二醇、三乙二醇、四乙二醇、丙二醇、二丙二醇、三丙二醇、四丙二醇、丁二醇等。
作為一元有機酸,可例舉碳數3~10之有機酸,具體而言,可例舉丁酸、異丁酸、己酸、2-乙基丁酸、庚酸、正辛酸、2-乙基己酸、正壬酸及癸酸等。
作為具體之一元有機酸,可例舉:三乙二醇二-2-乙基丁酸酯、三乙二醇二-2-乙基己酸酯、三乙二醇二辛酸酯、三乙二醇二正辛酸酯、三乙二醇二正庚酸酯、四乙二醇二正庚酸酯、四乙二醇二-2-乙基己酸酯、二乙二醇二-2-乙基丁酸酯、二乙二醇二-2-乙基己酸酯、二丙二醇二-2-乙基丁酸酯、三乙二醇二-2-乙基戊酸酯、四乙二醇二-2-乙基丁酸酯、二乙二醇二辛酸酯、三乙二醇二正庚酸酯、四乙二醇二正庚酸酯、三乙二醇二-2-乙基丁酸酯、乙二醇二-2-乙基丁酸酯、1,2-丙二醇二-2-乙基丁酸酯、1,3-丙二醇二-2-乙基丁酸酯、1,4-丁二醇二-2-乙基丁酸酯、1,2-丁二醇二-2-乙基丁酸酯等。
又,作為多元有機酸酯,例如可例舉:己二酸、癸二酸、壬二酸等碳數4~12之二元有機酸與碳數4~10之醇之酯化合物。碳數4~10之醇可為直鏈,亦可具有支鏈結構,還可具有環狀結構。
具體而言,可例舉:癸二酸二丁酯、壬二酸二辛酯、己二酸二己酯、己二酸二辛酯、己二酸己基環己酯、己二酸二異壬酯、己二酸庚基壬酯、二丁基卡必醇己二酸酯、混合型己二酸酯等。又,可為油改質癸二酸醇酸等。作為混合型己二酸酯,可例舉:由選自碳數4~9之烷基醇及碳數4~9之環狀醇中之2種以上之醇所製作之己二酸酯。
作為上述有機磷酸塑化劑,可例舉磷酸三丁氧基乙酯、磷酸異癸基苯酯及磷酸三異丙酯等磷酸酯等。
塑化劑特別適宜使用上述中之三乙二醇-二-2-乙基己酸酯(3GO)。
不含羥基之塑化劑可單獨使用1種,亦可併用2種以上。
(其他添加劑)
液晶裝置用膜除塑化劑以外,亦可適宜地含有與聚乙烯縮醛系樹脂等熱塑性樹脂併用之公知之添加劑。關於除塑化劑以外之添加劑,具體而言可例舉:紫外線吸收劑、紅外線吸收劑、抗氧化劑、光穩定劑、接著力調整劑、顏料、染料、螢光增白劑、結晶成核劑等。
(液晶裝置用膜之厚度)
本發明之液晶裝置用膜之厚度例如為100 μm以上2000 μm以下,較佳為200 μm以上1500 μm以下,進而較佳為250 μm以上900 μm以下。藉由使液晶裝置用膜之厚度處於此種範圍內,可改善對液晶裝置或玻璃板等之接著性而不會過厚。
[多層膜]
又,本發明之液晶裝置用膜可用於具備複數個樹脂層之多層膜。於用於多層膜之情形時,將複數個樹脂層中之至少1個作為本發明之液晶裝置用膜即可。
於該情形時,液晶裝置用膜可構成複數個樹脂層中之任一樹脂層,較佳為構成最外層。藉由使本發明之液晶裝置用膜構成最外層,多層膜例如亦存在使本發明之液晶裝置用膜與液晶裝置接觸,進而使液晶裝置用膜接著於液晶裝置而使用之情況,於該種情形時,可有效抑制液晶污染。又,亦可藉由降低液晶裝置用膜之玻璃轉移溫度,而以較高之接著力接著於液晶裝置。
如上所述,多層膜中之複數個樹脂層中之1個以上可不為本發明之液晶裝置用膜,於該情形時,樹脂層亦較佳為熱塑性樹脂層。構成熱塑性樹脂層之熱塑性樹脂為上述各種熱塑性樹脂即可,又,亦可視需要向熱塑性樹脂層中摻合塑化劑或其他添加劑。
<液晶裝置用膜之製造方法>
於液晶裝置用膜之製造中,首先,製備用於獲得液晶裝置用膜之膜用原料。關於膜用原料,可直接使用如上所述製造之聚乙烯縮醛系樹脂或其他熱塑性樹脂作為膜用原料。又,膜用原料亦可視需要向如上所述製造之聚乙烯縮醛系樹脂或其他熱塑性樹脂中添加塑化劑、其他添加劑等而製備。又,膜用原料可適宜地稀釋於溶劑中。
上述膜用原料以公知之方法成形為膜狀而製成液晶裝置用膜即可。具體而言,可將膜用原料塗佈於離型片等支持體,或者流入至模框,視需要適宜地進行加熱、乾燥,而成形為片狀,亦可藉由擠壓成形、加壓成形等進行成形。
又,如上所述,於使原料聚乙烯縮醛系樹脂與改質劑進行反應,而獲得聚乙烯縮醛系樹脂之情形時,可以如下方式成形。即,將包含原料聚乙烯縮醛系樹脂、改質劑及其他視需要摻合之塑化劑等添加劑之膜用原料塗佈於剝離片等支持體上,或者流入至模框,其後,進行加熱,藉此可使改質劑與原料聚乙烯縮醛系樹脂進行反應,且成形為膜狀,而獲得液晶裝置用膜。
進而,關於液晶裝置用膜,於用於多層膜之情形時,與用於獲得除液晶裝置用膜以外之樹脂層(其他樹脂層)之膜用原料一併準備,由該膜用原料獲得其他樹脂層即可。於多層膜之情形時,液晶裝置用膜與其他樹脂層適宜地重疊而成形即可,例如可藉由共擠壓等進行成形。
<液晶裝置>
本發明之液晶裝置用膜用於液晶裝置。液晶裝置用膜只要用於液晶裝置就並無特別限定,例如,可積層於液晶裝置而使用,亦可配置於液晶裝置之周圍而使用。在配置於周圍之情形時,液晶裝置用膜可以包圍液晶裝置之方式成形為框狀。又,液晶裝置用膜較佳為配置於與液晶裝置接觸之位置。進而,液晶裝置用膜亦較佳為積層於液晶裝置,而用於使液晶裝置接合於其他構件。
又,於將具有液晶裝置用膜之多層膜用於液晶裝置之情形時,多層膜亦可與上述液晶裝置用膜相同地配置,由液晶裝置用膜所構成之多層膜之最外層較佳為配置於與液晶裝置接觸之位置。
液晶裝置為具有液晶層之裝置即可,可例舉液晶調光單元、液晶顯示器等,該等中,較佳為液晶調光單元。液晶調光單元之構造相對簡單,故而液晶裝置用膜若被用於液晶調光單元,則膜成分容易自液晶調光單元之端面滲入而與液晶調光單元之液晶接觸,但本發明之液晶裝置用膜可減小NI點變化,故而可防止膜成分溶出至液晶,抑制液晶污染。
液晶調光單元一般具有液晶層。液晶層並無特別限定,可使用扭轉向列型、超扭轉向列型、相轉移型、主客型、鐵電液晶等,亦可使用高分子分散型之液晶,例如PDLC(聚合物分散型液晶)等。作為聚合物分散型液晶,可例舉藉由聚合物於液晶層中形成網狀結構而成之被稱為網絡液晶者。又,可為對液晶進行微膠囊化而使其分散於黏合劑樹脂中而成之微膠囊型液晶(PDMLC)。又,關於液晶層,例如可例舉藉由間隔物等形成用於將液晶填充於內部之空間,向該空間內填充液晶並進行密封而成者,亦可沒有間隔物。
液晶調光單元具備2片基材膜及配置於2片基材膜之間之液晶層即可。作為基材膜,可例舉使用聚對苯二甲酸乙二酯、聚萘二甲酸乙二酯等聚酯樹脂、丙烯酸系樹脂、三乙醯基纖維素(TAC)等纖維素衍生物、聚醚碸(PES)樹脂、聚醯亞胺樹脂等作為樹脂成分之樹脂膜。該等中,就使用性等觀點而言,較佳為聚酯樹脂膜,其中,更佳為聚對苯二甲酸乙二酯膜。
又,2片基材膜各自於液晶層側之面設置電極層即可。電極層可使用習知公知之具有透明性之電極材料,並無特別限定,例如可例舉:銦錫氧化物(ITO)導電膜、氧化錫導電膜、氧化鋅導電膜、高分子導電膜等。於電極層連接引出電極,經由引出電極於電極層間施加電壓即可。
液晶調光單元藉由於電極層間施加電壓,而改變液晶層之配向狀態,改變光線透過率。更具體而言,例如根據是否施加電壓,切換光透過模式與光散射,於光散射模式下使光散射而使光線透過率降低,另一方面,於光透過模式下透過光線而使光線透過率提高即可。
液晶調光單元之厚度並無特別限定,例如為0.05 mm以上2 mm以下,較佳為0.1 mm以上1 mm以下,更佳為0.2 mm以上0.8 mm以下。
[調光裝置]
如上所述,本發明之液晶裝置用膜例如較佳為用於積層於液晶裝置而接著於液晶裝置,使液晶裝置接合於其他構件之用途。
液晶裝置用膜特佳為用於具有液晶調光單元之調光裝置。具體而言,液晶裝置用膜較佳為用於具備2片透明板及配置於2片透明板之間之至少1個液晶調光單元之調光裝置。液晶裝置用膜可用作配置於透明板與液晶調光單元之間,將該等接合之中間膜。又,於在2片透明板之間設置2個以上之液晶調光單元之情形時,液晶裝置用膜可用作配置於液晶調光單元彼此之間,將該等接合之中間膜。作為透明板,如下所述,可例舉無機玻璃、有機玻璃等玻璃板。又,亦可使用上述多層膜作為中間膜。
其次,參照圖1、2進一步對調光裝置之具體例進行詳細說明。圖1所示之調光裝置10具備第1及第2透明板11、12、配置於該等之間之液晶調光單元13、配置於第1透明板11與液晶調光單元13之間之第1中間膜15及配置於第2透明板12與液晶調光單元13之間之第2中間膜16。
於調光裝置10中,第1中間膜15接合第1透明板11與液晶調光單元13,第2中間膜16接合第2透明板11與液晶調光單元13,藉此調光裝置10成為經一體化之積層體。再者,如上所述,液晶調光單元13例如於2片基材膜之間配置液晶層而構成,兩外表面由基材膜所構成即可。因此,第1及第2中間膜15、16分別接著於液晶調光單元13之基材膜即可。
第1及第2中間膜15、16之至少任一者由上述本發明之液晶裝置用膜所構成,較佳為兩者均由本發明之液晶裝置用膜所構成。
圖2所示之調光裝置20為具備2個液晶調光單元23、24之調光裝置。
具體而言,調光裝置20具備第1及第2透明板21、22及配置於該等之間之第1及第2液晶調光單元23、24。第1及第2液晶調光單元23、24排列於調光裝置20之厚度方向。藉由於調光裝置20中設置2個液晶調光單元23、24,例如,於光透過模式下可確保較高之光透過率,另一方面,於光散射模式下可確保較高之遮光性。又,藉由適當地切換2個液晶調光單元23、24之開-關,可精密地調整光之透過率或遮光性等。
調光裝置20於第1透明板21與第1液晶調光單元23之間、第1及第2液晶調光單元23、24之間及第2液晶調光單元24與第2透明板22之間各具備第1、第2及第3中間膜25、26、27。並且,第1中間膜25接合第1透明板21與第1液晶調光單元23,第2中間膜26將第1及第2液晶調光單元23、24彼此接合,且第3中間膜27接合第2液晶調光單元24與第2透明板22,藉此,調光裝置20成為經一體化之積層體。再者,如上所述,各液晶調光單元23、24例如於2片基材膜之間配置液晶層而構成,兩外表面由基材膜所構成即可,因此,各中間膜25、26、27分別接著於液晶調光單元23、24之基材膜即可。
第1~第3中間膜25、26、27之至少任一者由上述本發明之液晶裝置用膜所構成,較佳為全部由本發明之液晶裝置用膜所構成。
又,於各調光裝置10、20中,液晶調光單元之周端面視需要可藉由邊緣密封材料(未圖示)被密封。
於各調光裝置10、20中,液晶裝置用膜如圖1、2所示,例如與液晶調光單元接觸而使用,可減小NI點變化,故而可防止液晶污染。因此,於液晶調光單元中,可抑制顯示不均等缺陷。又,本發明之液晶裝置用膜藉由降低玻璃轉移溫度,亦可改善對液晶調光單元之基材膜或透明板之接著性,例如,即便於低溫下進行熱壓接合,亦可以較高之接著力接著於液晶調光單元或透明板。
又,於上述圖1、2所示之調光裝置中,中間膜示出單層構造之中間膜之形態,但中間膜亦可具有多層構造。於該情形時,中間膜較佳為上述多層膜,其中,較佳為接著於液晶調光單元之位置所配置之樹脂層由液晶裝置用膜所構成。
藉由使接著於液晶調光單元之位置所配置之樹脂層為本發明之液晶裝置用膜,於多層結構之情形時,亦可有效防止液晶污染。又,本發明之液晶裝置用膜藉由降低玻璃轉移溫度,亦可改善對液晶調光單元之基材膜之接著性。因此,於使用多層膜之情形時,亦可以較高之接著力接著於液晶調光單元等。
(透明板)
用於本發明之調光裝置之透明板(例如,上述第1及第2透明板21、22)可使用玻璃板。玻璃板可為無機玻璃及有機玻璃之任一者。調光裝置中之第1及第2透明板可一者為有機玻璃,另一者為無機玻璃,亦可兩者均為有機玻璃,還可兩者均為無機玻璃。
無機玻璃並無特別限定,例如可例舉:浮法板玻璃、強化玻璃、著色玻璃、研磨板玻璃、壓花玻璃、嵌網板玻璃、嵌線板玻璃、紫外線吸收板玻璃、紅外線反射板玻璃、紅外線吸收板玻璃、綠色玻璃等各種玻璃板。無機玻璃可進行表面處理等。
無機玻璃之厚度並無特別限定,較佳為0.1 mm以上,進而較佳為1.0 mm以上,又,較佳為5.0 mm以下,進而較佳為3.2 mm以下。
有機玻璃並無特別限定,可例舉:聚碳酸酯板、聚甲基丙烯酸甲酯板等甲基丙烯酸酯板、丙烯腈-苯乙烯共聚物板、丙烯腈-丁二烯-苯乙烯共聚物板、聚酯板、氟系樹脂板、聚氯乙烯板、氯化聚氯乙烯板、聚丙烯板、聚苯乙烯板、聚碸板、環氧樹脂板、酚樹脂板、不飽和聚酯樹脂板、聚醯亞胺樹脂板等各種有機玻璃板。有機玻璃可適宜地進行表面處理等。
上述中,就透明性、耐衝擊性、耐燃燒性優異之方面而言,較佳為聚碳酸酯板,就透明性較高,耐候性、機械強度優異之方面而言,較佳為聚甲基丙烯酸甲酯板等甲基丙烯酸酯板,該等中,較佳為聚碳酸酯板。於本發明中,即便使用聚碳酸酯板或甲基丙烯酸酯板等疏水性較高之有機玻璃作為透明板,亦可將液晶裝置用膜以較高之接著性接著於透明板。又,亦可藉由液晶裝置用膜防止有機玻璃被浸蝕。
有機玻璃之厚度並無特別限定,較佳為0.1 mm以上,進而較佳為0.3 mm以上,又,較佳為5.0 mm以下,進而較佳為3.0 mm以下。
本發明之調光裝置可藉由如下方式製造:經由中間膜並藉由熱壓接合等將透明板與液晶調光單元、或液晶調光單元彼此接合。例如,圖1所示之調光裝置藉由如下方式製造即可:將第1透明板11、第1中間膜15、液晶調光單元13、第2中間膜16及第2透明板12以該順序重疊並對該等進行熱壓接合。
又,圖2所示之調光裝置20藉由如下方式製造即可:將第1透明板21、第1中間膜25、第1液晶調光單元23、第2中間膜26、第2液晶調光單元24、第3中間膜27及第2透明板22以該順序重疊並對該等進行熱壓接合。
調光裝置製造中之熱壓接合時之溫度並無特別限定,例如為40℃以上120℃以下,較佳為50℃以上100℃以下。藉由將熱壓接合時之溫度設為上述上限以下,可不使液晶調光單元損傷或劣化等而經由中間膜將液晶調光單元與透明板、或液晶調光單元彼此接合。又,於本發明中,藉由如上所述地降低電子裝置用膜之玻璃轉移溫度,即便於低溫度下進行熱壓接合,亦可以較高之接著強度進行接著。
本發明之調光裝置可用於各種領域。具體而言,用於汽車、電車等車輛、船舶、飛機等各種交通工具、或者大廈、公寓、獨棟住宅、會館、體育館等各種建築物、或者切削、研磨等工具機、挖土機或起重機等建設機械等之窗玻璃等。又,亦可用於建築物內部之隔間等。
<電子裝置用膜>
本發明於另一態樣中亦提供一種用於電子裝置之電子裝置用膜。本發明之電子裝置用膜含有熱塑性樹脂。又,本發明之電子裝置用膜不含塑化劑,或者含有具有羥基之塑化劑及不具有羥基之塑化劑之至少任一者。並且,具有羥基之塑化劑之含量相對於熱塑性樹脂100質量份為70質量份以下,不具有羥基之塑化劑之含量相對於熱塑性樹脂100質量份為25質量份以下。
具有以上之構成之電子裝置用膜可防止塑化劑溶出至電子裝置,或因塑化劑浸蝕電子裝置之基材。
作為電子裝置,除上述液晶裝置以外,亦可例舉有機EL裝置、電漿顯示裝置等。上述電子裝置大多具有塑膠基板或膜基材,本發明之電子裝置用膜如上所述,可藉由調整塑化劑之種類及量,而防止電子裝置之基材(例如,塑膠基板或膜基材)之浸蝕。又,亦可有效防止液晶層等除基材以外之電子裝置之各種構件之污染。
於本發明中,電子裝置用膜之構成為與上述本發明之液晶裝置用膜相同之構成,熱塑性樹脂、塑化劑及其他添加劑之構成、玻璃轉移溫度、厚度等之詳細情況如上述液晶裝置用膜中所說明,故而省略其說明。又,電子裝置用膜如上所述,電子裝置用膜與液晶接觸時之NI點變化較佳為-2℃~+2℃,更佳為-1.5℃~+1.5℃,進而較佳為-1℃~+1℃,進而更佳為-0.5℃~+0.5℃,特佳為-0.3℃~+0.3℃。
又,電子裝置用膜只要用於電子裝置就並無特別限定,例如,可積層於電子裝置而使用,亦可配置於電子裝置之周圍而使用。又,電子裝置用膜較佳為配置於與電子裝置接觸之位置。又,電子裝置用膜亦較佳為積層於電子裝置,而用於使電子裝置與其他構件接合。
又,電子裝置用膜與液晶裝置用膜相同地,可以單層使用,亦可製成多層結構而使用。於多層結構之情形時,以電子裝置用膜構成複數個樹脂層中之至少1層即可,較佳為藉由電子裝置用膜構成最外層。於多層膜之情形時,亦與上述電子裝置用膜相同地使用即可,較佳為由電子裝置用膜所構成之多層膜之最外層配置於與電子裝置接觸之位置。
電子裝置較佳為液晶裝置。因此,電子裝置用膜較佳為用於液晶裝置,於該情形時,液晶裝置或具備液晶裝置(液晶調光單元)之調光裝置之構成如上述所說明。
實施例
藉由實施例,進一步對本發明進行詳細說明,但本發明不受該等例任何限定。
再者,本發明中之各物性值之測定方法及評價方法如下。
<NI點變化>
將液晶裝置用膜切割為10 mm×5 mm,裝入至樣品瓶(No.2,容量為6 ml)中,進而添加0.5 g之液晶(Chisso公司製造之「JC-5001LA」或4-氰基-4'-戊基聯苯(5CB))。將該瓶投入至100℃之烘箱中,並於100℃之環境下放置1小時,其後,於室溫靜置,恢復至室溫(25℃)後,取出液晶部分,製成評價用液晶樣品。
測定係使用示差掃描型熱量計(DSC,日立高新技術公司製造,「DSC7000X」),將5 mg之評價用液晶樣品封入至鋁樣品盤,於升溫速度10℃/分鐘之條件下進行,求出測定用液晶樣品之NI點(轉移溫度)。
又,將裝入至樣品瓶前之5 mg之單獨之液晶封入至鋁樣品盤,於相同條件下測定NI點,將其結果作為空白樣品。空白樣品之NI點為76.8℃。將單獨之液晶(空白樣品)與評價用液晶樣品之轉移溫度差作為NI點變化。
將變化溫度為-1~+1℃者設為「A」,將變化溫度不為-1~+1℃但為-2~+2℃者設為「B」,將更高之變化溫度設為「C」,而進行評價。
<接著性>
準備製成縱15 mm及橫15 mm之尺寸之液晶裝置用膜,進而,準備2片依據JIS K6735之厚度2 mm、縱25 mm及橫100 mm之玻璃板。介隔液晶裝置用膜,將2片玻璃板以彼此之長邊方向垂直之方式配置而重疊為十字狀。
其後,以液晶裝置用膜之厚度成為一定之方式,使用與液晶裝置用膜相同厚度之間隔物,於真空貼合機中,將介隔液晶裝置用膜重疊之2片玻璃板於100℃、0.1 MPa之條件下暫時壓接3分鐘。其後,將經暫時壓接之2片聚碳酸酯板玻璃於100℃、0.5 MPa之條件下進而正式壓接1小時,獲得層合玻璃樣品。
對所獲得之層合玻璃樣品進行十字剝離試驗。具體而言,測定於溫度23℃之環境下,將層合玻璃樣品以速度10 mm/分鐘沿與接著面垂直之方向剝離時之最大負載(N)。將其最大負載(N)作為接著力,基於下述基準進行評價。
(評價基準)
A:最大負載為150 N以上。
B:最大負載為80 N以上且未達150 N。
C:最大負載未達80 N。
<玻璃轉移溫度(Tg)>
以長度10 mm、寬度5 mm切割實施例、比較例所獲得之液晶裝置用膜,使用動態黏彈性測定裝置(日本IT計測控制股份有限公司製造,商品名為「DVA-200」),於以下之測定條件下測定黏彈性。讀取由黏彈性測定之結果所獲得之損耗正切tanδ之峰值溫度。於-50~150℃之溫度範圍內自低溫側開始數將第1個峰值溫度作為玻璃轉移溫度(Tg)。
(測定條件)
變化樣式:剪切模式;測定溫度:-50℃~200℃;升溫速度:5℃/分鐘;測定頻率:1 Hz;應變:1%
<改質量、縮醛化度、乙醯化度及羥基量>
將聚乙烯縮醛系樹脂溶解於DMSO-d6或氯仿-d中,使用1H-NMR(核磁共振譜)進行測定,對各單元之莫耳比進行分析,藉此求出。將結果記載於表1。
(實施例1)
[環氧乙烷改質聚乙烯醇之合成]向附有攪拌機、溫度計、滴液漏斗及回流冷凝器之燒瓶中添加1000質量份之乙酸乙烯酯、320質量份之平均重複單位m=10之聚氧乙烯單乙烯醚及300質量份之甲醇,進行系統內之氮氣置換後,將溫度提昇至60℃。向該系統內添加1.1質量份之2,2-偶氮二異丁腈,開始聚合。自開始聚合起5小時停止聚合。聚合停止時之系統內之固形物成分濃度為53質量%,相對於總單體之聚合產率為65質量%。於減壓下去除未反應之單體後,獲得共聚物之30質量%甲醇溶液。由未反應之單體之定量確認:所獲得之共聚物含有95.0莫耳%之乙酸乙烯酯單位、5.0莫耳%之含有環氧乙烷之烷基乙烯基醚單位。
於40℃一面攪拌100質量份之所獲得之共聚物之甲醇溶液,一面添加6.0質量份之3質量%之NaOH甲醇溶液,充分混合後進行放置。2小時後,利用粉碎機粉碎固化之聚合物,利用甲醇洗淨後,進行乾燥而獲得聚合物粉末(環氧乙烷改質聚乙烯醇)。環氧乙烷改質聚乙烯醇具有1莫耳%之乙醯基、5莫耳%之環氧乙烷單位量,聚合度為700。
[聚乙烯縮丁醛(PVB1)之製備]
將100質量份之所獲得之聚合物粉末添加至753質量份之純水中,於90℃之溫度約攪拌2小時而使其溶解。將該溶液冷卻至40℃,添加56質量份之濃度35質量%之鹽酸及54質量份之正丁醛,將液溫降低至20℃,保持溫度進行縮醛化反應,使反應產物析出。其後,將液溫設為40℃保持3小時後結束反應,藉由常規方法進行中和、水洗及乾燥,獲得聚乙烯縮醛系樹脂(PVB1)之白色粉末。
[液晶裝置用膜之製作]
將所獲得之聚乙烯縮醛系樹脂於溫度160℃、壓力20 MPa下加壓成形,而獲得厚度800 μm之樹脂膜(液晶裝置用膜)。
(實施例2)
獲得除將320質量份之平均重複單位m=10之聚氧乙烯單乙烯醚變更為180質量份之重複單位m=30之聚氧乙烯單乙烯醚以外,以與實施例1相同之方法製備之PVB2。環氧乙烷改質聚乙烯醇之聚合度為860。使用PVB2並以與實施例1相同之方法獲得厚度800 μm之樹脂膜(液晶裝置用膜)。
(實施例3)
獲得除將6.0質量份之3質量%之NaOH甲醇溶液變更為2.7質量份以外,以與實施例2相同之方法製備之PVB2-2。使用PVB2並以與實施例1相同之方法獲得厚度800 μm之樹脂膜(液晶裝置用膜)。
(實施例4)
獲得除將320質量份之平均重複單位m=10之聚氧乙烯單乙烯醚變更為180質量份之重複單位m=30之聚氧丙烯單烯丙醚以外,以與實施例1相同之方法製備之PVB3。環氧乙烷改質聚乙烯醇之聚合度為1100。使用PVB3並以與實施例1相同之方法獲得厚度800 μm之樹脂膜(液晶裝置用膜)。
(實施例5)
獲得除將320質量份之平均重複單位m=10之聚氧乙烯單乙烯醚變更為520質量份之重複單位m=50之聚氧乙烯聚氧丙烯單烯丙醚以外,以與實施例1相同之方法製備之PVB3-2。環氧乙烷及環氧丙烷改質聚乙烯醇之聚合度為1500。使用PVB2並以與實施例1相同之方法獲得厚度800 μm之樹脂膜(液晶裝置用膜)。
(實施例6)
向於氮氣氣流下經乾燥之500 mL可分離式燒瓶中加入300 g之THF及30 g之聚乙烯縮丁醛(聚合度為1700,積水化學公司製造,PVB4),於65℃利用攪拌葉進行攪拌,而使聚乙烯縮丁醛溶解。
向該溶液中添加30 g之作為改質劑之異氰酸正十八烷基酯並攪拌10分鐘。自可分離式燒瓶中取出溶液,流入至以剝離處理面成為上表面之方式鋪有PET離型膜(商品名為「PET50D1-C」,Nippa公司製造)之鋁墊後,利用烘箱於130℃加熱2小時進行反應,獲得由具有式(1-1)之官能基之聚乙烯縮醛系樹脂(PVB6)所構成之膜。將所獲得之聚乙烯縮醛系樹脂於溫度160℃、壓力20 MPa下加壓成形而獲得厚度800 μm之樹脂膜(液晶裝置用膜)。利用紅外分光光度計(IR)對所獲得之樹脂膜進行測定,結果,根據異氰酸酯基(波數為2260 cm
-1)之波峰消失,可確認反應之進行。
(實施例7)
使用實施例4所使用之PVB4(聚合度為1700,積水化學公司製造)代替PVB1,以與實施例1相同之方法製作樹脂膜(液晶裝置用膜)。
(實施例8)
將PVB4及作為塑化劑之聚酯多元醇(DIC公司製造之「OD-X-2586」,羥基為3個,分子量為850)以表1之比率充分混練,獲得膜用組成物。將所獲得之膜用組成物於溫度160℃、壓力20 MPa下加壓成形而獲得厚度800 μm之樹脂膜(液晶裝置用膜)。
(實施例9~11、比較例1~2)
將PVB1、PVB4及PVB5與作為塑化劑之三乙二醇二-2-乙基己酸酯(3GO)(羥基為0個)以表1之比率充分混練,獲得膜用組成物。將所獲得之膜用組成物於溫度160℃、壓力20 MPa下加壓成形而獲得厚度800 μm之樹脂膜(液晶裝置用膜)。
再者,PVB5為平均聚合度830之聚乙烯縮丁醛樹脂。
(實施例12)
獲得除將320質量份之平均重複單位m=10之聚氧乙烯單乙烯醚變更為110質量份之重複單位m=30之聚氧丙烯單烯丙醚以外,以與實施例1相同之方法製備之PVB7。環氧乙烷改質聚乙烯醇之聚合度為1100。使用PVB7,將三乙二醇二-2-乙基己酸酯(3GO)(羥基為0個)變更為數量平均分子量為1000之聚丙二醇(富士膠片和光純藥公司製造,PPG1000,羥基為2個),除此以外,以與實施例9~11相同之方法獲得厚度800 μm之樹脂膜(液晶裝置用膜)。
(實施例13)
將聚丙二醇變更為數量平均分子量為700之聚氧丙烯雙甘油醚(日油股份有限公司製造,商品名為「Unilub DGP-700」,羥基為4個),除此以外,以與實施例12相同之方法獲得厚度800 μm之樹脂膜(液晶裝置用膜)。
(實施例14)
將聚丙二醇變更為數量平均分子量為1000之聚氧丙烯甘油醚(日油股份有限公司製造,商品名為「Uniol TG-1000R」,羥基為2個),除此以外,以與實施例12相同之方法獲得厚度800 μm之樹脂膜(液晶裝置用膜)。
(實施例15)
將聚丙二醇變更為數量平均分子量為1600之聚氧丙烯雙甘油醚(阪本藥品工業股份有限公司,商品名為「SCP-1600」,羥基為4個),除此以外,以與實施例12相同之方法獲得厚度800 μm之樹脂膜(液晶裝置用膜)。
[表1]
PVB種類 | 改質劑 | 實施例1 | 實施例2 | 實施例3 | 實施例4 | 實施例5 | 實施例6 | 實施例7 | 實施例8 | 實施例9 | 實施例10 | 實施例11 | 實施例12 | 實施例13 | 實施例14 | 實施例15 | 比較例1 | 比較例2 | |
樹脂(質量份) | PVB1 | EO(m=10) | 100 | 100 | |||||||||||||||
PVB2 | EO(m=30) | 100 | |||||||||||||||||
PVB2-2 | EO(m=30) | 100 | |||||||||||||||||
PVB3 | PO(m=30) | 100 | |||||||||||||||||
PVB3-2 | EO/PO(m=50) | 100 | |||||||||||||||||
PVB4 | 無 | 100 | 100 | 100 | 100 | 100 | |||||||||||||
PVB5 | 無 | 100 | |||||||||||||||||
PVB6 | 異氰酸烷基酯(C18) | 100 | |||||||||||||||||
PVB7 | EO/PO(m=30) | 100 | 100 | 100 | 100 | ||||||||||||||
塑化劑(質量份) | 3GO | 羥基為0個 | 10 | 20 | 10 | 40 | 35 | ||||||||||||
OD-X-2586 | 羥基為3個 | 40 | |||||||||||||||||
PPG1000 | 羥基為2個 | 15 | |||||||||||||||||
DGP700 | 羥基為4個 | 15 | |||||||||||||||||
TG1000R | 羥基為2個 | 15 | |||||||||||||||||
SCP-1600 | 羥基為4個 | 15 | |||||||||||||||||
液晶 | 5001LA | 5001LA | 5001LA | 5001LA | 5001LA | 5001LA | 5001LA | 5001LA | 5001LA | 5001LA | 5001LA | 5CB | 5CB | 5CB | 5CB | 5001LA | 5CB | ||
PVB | 構成單位量(mol) | 丁醛 | 77 | 78 | 78 | 72 | 75 | 66 | 66 | 66 | 64 | 66 | 77 | 73 | 73 | 73 | 73 | 66 | 66 |
乙醯基 | 1 | 1 | 8 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | ||
羥基 | 17.0 | 18.8 | 11.8 | 23.4 | 21.2 | 11.9 | 33.0 | 33.0 | 35.0 | 33.0 | 17.0 | 23.5 | 23.5 | 23.5 | 23.5 | 33.0 | 33.0 | ||
改質基 | 5.0 | 2.2 | 2.2 | 3.4 | 2.8 | 21.1 | 0.0 | 0.0 | 0.0 | 0.0 | 5.0 | 2.5 | 2.5 | 2.5 | 2.5 | 0.0 | 0.0 | ||
膜 | Tg | ℃ | 43 | 43 | 38 | 37 | 36 | 43 | 70 | 26 | 46 | 46 | 28 | 29 | 32 | 30 | 34 | 25 | 25 |
NI點變化 | ℃(100℃,1 h) | -0.01 | -0.20 | -0.23 | -0.08 | -0.09 | -0.02 | -0.03 | -0.18 | -0.86 | -1.33 | -0.91 | -0.52 | -0.22 | -0.45 | -0.31 | -2.27 | -3.12 | |
判定 | A | A | A | A | A | A | A | A | A | B | A | A | A | A | A | C | C | ||
接著力 | 判定 | A | A | A | A | A | B | C | A | B | B | A | A | A | B | B | A | A |
以上各實施例之液晶裝置用膜藉由適宜地調整熱塑性樹脂之構成、塑化劑之有無及塑化劑之種類與量,而可減小與液晶接觸時之NI點變化。因此,即便用於液晶裝置,亦可抑制液晶污染,防止產生顯示不均等缺陷。
相對於此,比較例1、2之膜由於與液晶接觸時之NI點變化較大,故而若用於液晶裝置,則認為會污染液晶,產生顯示不均等缺陷。
10,20:調光裝置
11,21:第1透明板
12,22:第2透明板
13:液晶調光單元
15,25:第1中間膜
16,26:第2中間膜
23:第1液晶調光單元
24:第2液晶調光單元
27:第3中間膜
[圖1]係表示應用本發明之液晶裝置用膜之調光裝置之一實施方式的示意性剖面圖。
[圖2]係表示應用本發明之液晶裝置用膜之調光裝置之另一實施方式的示意性剖面圖。
Claims (13)
- 一種液晶裝置用膜,其係用於液晶裝置者,含有熱塑性樹脂, 使液晶裝置用膜與液晶接觸時之NI點變化為-2℃~+2℃。
- 如請求項1之液晶裝置用膜,其不含塑化劑,或者含有具有羥基之塑化劑及不具有羥基之塑化劑之至少任一者, 上述具有羥基之塑化劑之含量相對於上述熱塑性樹脂100質量份為70質量份以下,且 上述不具有羥基之塑化劑之含量相對於上述熱塑性樹脂100質量份為25質量份以下。
- 如請求項2之液晶裝置用膜,其不含塑化劑,或者含有相對於熱塑性樹脂100質量份為70質量份以下之含有羥基之塑化劑。
- 如請求項1至3中任一項之液晶裝置用膜,其中,上述熱塑性樹脂為選自由聚乙烯縮醛系樹脂、離子聚合物樹脂、聚胺酯樹脂、聚烯烴樹脂及乙烯-乙酸乙烯酯共聚樹脂所組成之群中之至少1種。
- 如請求項4之液晶裝置用膜,其中,上述熱塑性樹脂為聚乙烯縮醛系樹脂。
- 如請求項4或5之液晶裝置用膜,其中,上述聚乙烯縮醛系樹脂包含具有縮醛基、乙醯基及羥基以外之單元之改質聚乙烯縮醛樹脂。
- 如請求項4至6中任一項之液晶裝置用膜,其中,上述聚乙烯縮醛系樹脂具有聚氧伸烷基。
- 如請求項1至7中任一項之液晶裝置用膜,其玻璃轉移溫度為55℃以下。
- 如請求項1至8中任一項之液晶裝置用膜,其中,上述NI點變化為-1℃~+1℃。
- 如請求項1至9中任一項之液晶裝置用膜,其係液晶調光單元用。
- 一種液晶裝置,其設置有請求項1至10中任一項之液晶裝置用膜。
- 一種調光裝置,其具備請求項10之液晶裝置用膜及液晶調光單元。
- 一種電子裝置用膜,其係用於電子裝置者, 含有熱塑性樹脂,且 不含塑化劑,或者含有具有羥基之塑化劑及不具有羥基之塑化劑之至少任一者, 上述具有羥基之塑化劑之含量相對於上述熱塑性樹脂100質量份為70質量份以下, 上述不具有羥基之塑化劑之含量相對於上述熱塑性樹脂100質量份為25質量份以下。
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EP (1) | EP4242739A1 (zh) |
JP (1) | JPWO2022097753A1 (zh) |
KR (1) | KR20230104874A (zh) |
CN (1) | CN116529222A (zh) |
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EP3540009A1 (en) * | 2018-03-15 | 2019-09-18 | Shark Solutions ApS | Modification of virgin and/or recycled construction polymers, using poly vinyl butyral (pvb), or recycled pvb from industrial waste streams and an alloying copolymer |
JP7286928B2 (ja) | 2018-08-23 | 2023-06-06 | 大日本印刷株式会社 | 調光装置およびその製造方法 |
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US20230399475A1 (en) | 2023-12-14 |
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EP4242739A1 (en) | 2023-09-13 |
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