TW201842050A - 樹脂組成物、成形體、積層體、被覆材料及接著劑 - Google Patents
樹脂組成物、成形體、積層體、被覆材料及接著劑 Download PDFInfo
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- TW201842050A TW201842050A TW107108568A TW107108568A TW201842050A TW 201842050 A TW201842050 A TW 201842050A TW 107108568 A TW107108568 A TW 107108568A TW 107108568 A TW107108568 A TW 107108568A TW 201842050 A TW201842050 A TW 201842050A
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- resin composition
- mass
- epoxy compound
- bentonite
- lithium
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Abstract
一種樹脂組成物,其含有環氧化合物及鋰部分固定型膨潤石。
Description
本發明係關於樹脂組成物、成形體、積層體、被覆材料及接著劑。
在食品等之包裝用的包裝材料上,要求具有內容物之保護、耐殺菌性、耐熱性、透明性、加工性的功能。為了保持內容物之品質,氣體阻隔性變得特別重要。最近不僅包裝材料,太陽電池、半導體等電子材料所用的材料亦被要求高氣體阻隔性。
在專利文獻1中,記載藉由將具有羥基之樹脂及異氰酸酯化合物、與黏土礦物等板狀無機化合物及光遮斷劑組合,以提高氣體阻隔性等特性。
又,在專利文獻2中記載以改質黏土作為主要構成成分之材料,藉由使用改質黏土,且視需要使用添加劑,使改質黏土結晶配向,緻密地積層,而得到能利用作為自立膜且具備機械強度、氣體阻隔性、耐水性、熱安定性及柔軟性之膜材料。
專利文獻1 國際公開第2013/027609號
專利文獻2 日本特開2007-277078號公報
如專利文獻1所記載之板狀無機化合物體積大,又難以得到與樹脂之良好親和性。因此,添加量及分散性有限度。所以,藉由使添加量增加以得到更高氣體阻隔性有困難,即使假設可增加填充劑之添加量,仍無法得到充分的分散性,而無法得到充分的氣體阻隔性。
又,在專利文獻2中所記載之黏土膜,由於成膜後藉由加熱來形成自立膜,所以對於黏度膜將成膜於上的基材(例如樹脂基材),要求非常高之耐熱性。因此,在專利文獻2中記載之黏度膜,只能使用耐熱性非常高之基材(例如樹脂基材),有使用用途受限的問題。再者,在專利文獻2中記載之自立膜,為了發揮高氣體阻隔性,摻入許多填充劑。然而,若填充劑量過多,由於損及組成物之柔軟性,在使用於例如軟包裝用之薄膜用途等的情況,有薄膜之柔軟性不足的問題。因此,仍然尋求不管填充劑為高充填之情況、或為低充填之情況,均能發揮高氣體阻隔性的樹脂組成物。
於是,本發明之目的為提供與先前之樹脂組成物相較,氣體阻隔性,尤其水蒸氣阻隔性及氧阻隔性更優良的樹脂組成物。
本發明之一面向,為提供含有環氧化合物及鋰部分固定型膨潤石之樹脂組成物。該樹脂組成物由 於係將環氧化合物與鋰部分固定型膨潤石組合,水蒸氣阻隔性、氧阻隔性(例如高濕度下之氧阻隔性)等氣體阻隔性優良。亦即,若藉由該樹脂組成物,可得到具有優良氣體阻隔性之樹脂膜。
環氧化合物之環氧當量以50~3000g/eq為較佳。藉此,水蒸氣阻隔性及氧阻隔性成為更優良者。
環氧化合物以含芳香環結構及脂環結構中之至少一種結構為較佳。藉此,水蒸氣阻隔性及氧阻隔性成為更優良者。
鋰部分固定型膨潤石,以陽離子交換容量係1~70meq/100g為較佳。藉此,水蒸氣阻隔性及氧阻隔性成為更優良者。
樹脂組成物可進一步含有硬化劑。在樹脂組成物含有硬化劑之情況,藉由熱可使環氧基開環聚合而硬化,而可得到具有更優良阻隔性之樹脂膜。
硬化劑以選自包含酸酐系硬化劑、酚系硬化劑及醯胺系硬化劑之群組中的至少一種硬化劑為較佳。亦即,樹脂組成物以含有此等硬化劑中之至少一種為較佳。藉此,水蒸氣阻隔性及氧阻隔性成為更優良者。
鋰部分固定型膨潤石之含量,較佳為相對於樹脂組成物之不揮發成分總量而言為3~70質量%。藉由此種含量,成為水蒸氣阻隔性及氧阻隔性優良,同時成形性亦更為優良者。
本發明在一面向中,提供上述樹脂組成物之成形體、及於基材上具備該成形體之積層體(具備基材,及設置於該基材上之成形體的積層體)。
本發明之一面向之樹脂組成物,由於水蒸氣阻隔性及氧阻隔性優良,所以適合用於氣體阻隔材料、被覆材料、接著劑等用途。
若依照本發明,可提供氣體阻隔性、尤其水蒸氣阻隔性及氧阻隔性更優良之樹脂組成物。
以下,對於本發明之適當實施態樣詳細地說明。但是,本發明不受以下之實施態樣限定。
本實施態樣之樹脂組成物含有環氧化合物及鋰部分固定型膨潤石。
膨潤石意指具有層結構之層狀矽酸鹽礦物(層狀黏土礦物)的一種。就膨潤石之具體結構而言,已知有蒙脫石、貝得石(beidellite)、皂石、水輝石(hectorite)、矽鎂石、鋅皂石(sauconite)等之結構。此等中,就黏土材料之結構而言,以選自包含蒙脫石及矽鎂石之群組中的至少一種結構為較佳。此等結構在八面體片(octahedral sheet)之金屬元素的一部分,具有與低原子價金屬元素之同型置換、缺陷等。因此,八面體片帶負電。其結果,此等結構在八面體片具有空位點,具有此等結構之膨潤石,如後述方式,鋰離子移動後可安定存在。
將保有之陽離子為鋰離子的膨潤石稱為鋰型膨潤石(但是,在本說明書中,排除後述之鋰部分固定型膨潤石)。就使膨潤石所具有之陽離子交換成鋰離子的方法而言,可列舉例如在天然之鈉型膨潤石之分散液(分散漿液)中,添加氫氧化鋰、氯化鋰等鋰鹽,以進行陽離子交換的方法。藉由調節分散液中所添加的鋰之量,可適宜調節鋰離子在所得到之鋰型膨潤石之浸出陽離子量中所佔的量。又,鋰型膨潤石亦可使用陽離子交換樹脂進行離子交換成鋰離子的管柱法、或批次法而得到。
在實施態樣中,鋰部分固定型膨潤石,意指鋰型膨潤石中鋰離子之一部分被固定化於八面體片之空位點而成的膨潤石。鋰部分固定型膨潤石可藉由例如鋰型膨潤石之加熱處理,將層間之鋰離子固定化於八面體片之空位點而得到。藉由將鋰離子固定化,可使膨潤石耐水化。
將鋰部分固定之加熱處理的溫度條件,只要能將鋰離子固定化即可,無特別限制。如後述,在陽離子交換容量(CEC:Cation Exchange Capacity)小之情況,摻入鋰部分固定型膨潤石之樹脂組成物的水蒸氣阻隔性及氧阻隔性更為提高。再者,從將鋰離子有效率地固定化,使陽離子交換容量大幅降低之觀點而言,以加熱至150℃以上為較佳。上述加熱處理之溫度,更佳為150~600℃,進一步更佳為180~600℃,特佳為200~500℃,最佳為250~500℃。藉由以上述溫度加熱,可使陽離子交換容量更有效率地降低,同時可抑制膨潤 石中之羥基的脫水反應等。上述加熱處理以用開放系電氣爐實施為較佳。在此情況,加熱時之相對濕度為5%以下,壓力為常壓。上述加熱處理之時間,只要能將鋰部分地固定即可,無特別限制,然而從生產效率性之觀點,以0.5~48小時為較佳,以1~24小時為更佳。
是否為鋰部分固定型膨潤石,可藉由X射線光電子分光(XPS:X-ray Photoelectron Spectroscopy)分析而判斷。具體而言,在藉由XPS分析所測得之XPS光譜中,確認來自Li離子之結合能的峰位置。例如,在膨潤石為蒙脫石之情況,將鋰型膨潤石藉由加熱處理等,形成鋰部分固定型膨潤石,XPS光譜中來自Li離子之結合能的峰位置為57.0ev至55.4ev位移。因此,在膨潤石為蒙脫石之情況,藉由是否具有55.4ev之結合能峰,可判斷是否為部分固定型。
鋰部分固定型膨潤石之陽離子交換容量,從水蒸氣阻隔性及氧阻隔性(例如高濕度下之氧阻隔性)更為優良的觀點而言,較佳為70meq/100g以下,更佳為60meq/100g以下。鋰部分固定型膨潤石之陽離子交換容量,從水蒸氣阻隔性及氧阻隔性(例如高濕度下之氧阻隔性)更為優良之觀點而言,為1meq/100g以上,更佳為5meq/100g以上,進一步更佳為10meq/100g以上。從此等觀點而言,鋰部分固定型膨潤石之陽離子交換容量為1~70meq/100g,更佳為5~70meq/100g,進一步更佳為10~60meq/100g。例如,在膨潤石為蒙脫石之情況,通常離子交換容量為約80~150meq/100g,然而藉由進行部分 固定化處理,可成為5~70meq/100g。鋰部分固定型膨潤石之陽離子交換容量可為小於60meq/100g,亦可為50meq/100g以下。例如,鋰部分固定型膨潤石之陽離子交換容量可為1meq/100g以上且小於60meq/100g,亦可為5meq/100g以上且小於60meq/100g,亦可為10meq/100g以上且小於60meq/100g。
膨潤石之陽離子交換容量,可依照以Schollenberger法(黏土手冊第三版,日本黏土學會編,2009年5月,p.453-454)為基準之方法測定。更具體而言,可依照日本皂土(bentonite)工業會標準試驗方法JBAS-106-77記載之方法測定。
膨潤石之浸出陽離子量,可藉由對於0.5g之膨潤石,使用100mL之1M乙酸銨水溶液以4小時以上浸出膨潤石之層間陽離子,將所得到之溶液中各種陽離子的濃度,藉由ICP發光分析、原子吸光分析等測定及算出。
相對於樹脂組成物中之不揮發成分總量,鋰部分固定型膨潤石之含量較佳為3質量%以上。在鋰部分固定型膨潤石之含量相對於不揮發成分總量而言為3質量%以上的情況,水蒸氣阻隔性及氧阻隔性(例如高濕度下之氧阻隔性)更為優良。從同樣之觀點,相對於樹脂組成物中之不揮發成分總量,鋰部分固定型膨潤石之含量可為5質量%以上、7質量%以上、9質量%以上、10質量%以上、15質量%以上、18質量%以上、20質量%以上、25質量%以上或30質量%以上。鋰部分固定型 膨潤石之含量較佳為相對於樹脂組成物中之不揮發成分總量而言為70質量%以下。在鋰部分固定型膨潤石之含量為70質量%以下的情況,樹脂組成物之成形性變得更優良,且對基材之密接性提高。又,在高濕度下,可得到更高氧阻隔性。從同樣之觀點,相對於樹脂組成物中之不揮發成分總量,鋰部分固定型膨潤石之含量可為50質量%以下、45質量%以下、40質量%以下、35質量%以下、30質量%以下。上述之上限值及下限值可任意地組合。亦即,鋰部分固定型膨潤石之含量,例如,可為相對於樹脂組成物中之不揮發成分總量而言為3~70質量%、3~50質量%、3~35質量%、5~35質量%、5~30質量%、7~30質量%、9~30質量%、10~30質量%等。在本說明書中同樣之記載中,個別地記載之上限值及下限值亦可任意地組合。再者,不揮發成分,意指從樹脂組成物總質量,除去稀釋溶劑質量、以及環氧樹脂、硬化劑、修飾劑及各種添加劑所含之揮發成分質量所得到的質量。
實施態樣之樹脂組成物含有環氧化合物。環氧化合物意指含有環氧基之化合物。就環氧化合物而言,可列舉例如活性氫化合物(較佳為具有2個以上活性氫之化合物)與環氧氯丙烷之縮合物、烯烴之氧化物、(甲基)丙烯酸縮水甘油酯等具有縮水甘油基之烯性不飽和化合物的聚合物等。就上述縮合物而言,以縮水甘油基醚型之環氧化合物、縮水甘油基胺型之環氧化合物、縮水甘油基酯型之環氧化合物為代表。此等之中,較佳為 雙酚A、雙酚F、酚醛清漆樹脂等具有2個以上羥基之化合物與環氧氯丙烷之縮合物,即縮水甘油基醚型環氧化合物。環氧化合物可為固狀,亦可為液狀。在環氧化合物為固狀之情況,可溶解於溶媒中而使用。
環氧化合物之環氧當量較佳為50g/eq以上,更佳為100g/eq以上。在環氧當量為50g/eq以上之情況,將樹脂膜硬化所得到的成形體(硬化膜)之柔軟性優良。環氧化合物之環氧當量,只要為5000g/eq以下即可,較佳為3000g/eq以下,更佳為2500g/eq以下,進一步更佳為2200g/eq以下。在環氧當量為3000g/eq以下之情況,水蒸氣阻隔性及氧阻隔性(例如高濕度下之氧阻隔性)更優良。從此等觀點,環氧化合物之環氧當量,例如,可為50~5000g/eq、50~3000g/eq、50~2500g/eq、50~2200g/eq、100~3000g/eq、100~2500g/eq或100~2200g/eq。環氧當量可為150g/eq以上或180g/eq以上,可為2000g/eq以下,1500g/eq以下,1100g/eq以下,700g/eq以下或500g/eq。再者,環氧當量可依照JIS K7236:2001測定。
環氧化合物較佳為包含芳香環結構及脂環結構之中的至少一種結構。在此情況,水蒸氣阻隔性及氧阻隔性(例如高濕度下之氧阻隔性)更優良。得到此種效果之理由雖不明確,然而藉由包含上述結構,所得到之樹脂膜中水蒸氣的溶解性降低,研判為理由之一。環氧化合物可只包含芳香環結構及脂環結構之一種結構,亦可包含兩者之結構。從容易得到上述效果之觀點而 言,以使用包含芳香環結構之環氧化合物為更佳。以下,將包含芳香環結構之環氧化合物稱為「芳香族環氧化合物」,將包含脂環結構之環氧化合物稱為「脂環式環氧化合物」。
芳香族環氧化合物所含之芳香環結構,可為單環,亦可為稠合環。芳香環結構以具有碳數6~18之芳香環的結構(二價之芳香環基)為較佳。就此種芳香環結構而言,可列舉苯環結構(伸苯基)、萘環結構(伸萘基)、菲環結構(伸菲基)、蒽環結構(伸蒽基)等。更佳為苯環結構或萘結構,進一步更佳為苯環結構。芳香族環氧化合物所含的芳香環結構之數目,可為一個,亦可為複數個。
就芳香族環氧化合物而言,可列舉如:雙酚A型環氧化合物、雙酚F型環氧化合物、雙酚S型環氧化合物、雙酚AD型環氧化合物、間苯二酚型環氧化合物、二羥基萘型環氧化合物、聯苯型環氧化合物、四甲基聯苯型環氧化合物、具有蒽、聯苯、雙酚A、雙酚F、雙酚S的結構之3官能以上的環氧化合物、苯酚酚醛清漆型環氧化合物、甲酚酚醛清漆型環氧化合物、三苯基甲烷型環氧化合物、四苯基乙烷型環氧化合物、二環戊二烯-酚加成反應型環氧化合物、苯酚芳烷基型環氧化合物、萘酚酚醛清漆型環氧化合物、萘酚芳烷基型環氧化合物、萘酚-酚共縮酚醛清漆型環氧化合物、萘酚-甲酚共縮酚醛清漆型環氧化合物、經芳香族烴甲醛化合物改質之苯酚化合物型環氧化合物、經聯苯改質之酚醛清漆 型環氧化合物等。此等之中,從水蒸氣阻隔性及氧阻隔性(例如高濕度下之氧阻隔性)更優良的觀點而言,以使用雙酚A型環氧化合物及雙酚F型環氧化合物為較佳。雙酚A型環氧化合物可為液狀,亦可為固狀。
就芳香族環氧化合物而言,亦可使用市售之芳香族環氧化合物。就市售之芳香族環氧化合物而言,可列舉例如苯基二縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-141」)(Denacol為註冊商標;以下相同)、對-三級丁基苯基縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-146」)、間苯二酚二縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-201」)、雙酚A二縮水甘油基醚(DIC股份有限公司製「EPICLON850、850-S、860、1050、2050,3050、4050、7050、HM-091」)(EPICLON為註冊商標;以下相同)、雙酚F二縮水甘油基醚(DIC股份有限公司製「EPICLON830」)、苯酚酚醛清漆型聚縮水甘油基醚(DIC股份有限公司製「EPICLON N-740、770」)、甲酚酚醛清漆型聚縮水甘油基醚(DIC股份有限公司製「EPICLON N-660」)、二環戊二烯-苯酚加成反應型聚縮水甘油基醚(DIC股份有限公司製「EPICLON HP-7200」)、2-苯基苯酚縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-142」)、1,6-萘二縮水甘油基醚(DIC股份有限公司製「EPICLON HP-4032」、1-氯-2,3-環氧丙烷‧2,7-萘二醇‧甲醛聚縮合物(DIC股份有限公司製「EPICLON EXA-4700」)、鄰苯二甲酸二縮 水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-721」)、對苯二甲酸二縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-711」)、1,6-己二醇二縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-212」)、N,N,N’,N’-四縮水甘油基間二甲苯二胺(三菱氣體化學股份有限公司製「TETRAD-X」)、三菱化學股份有限公司製之「jER806」、「jER4004P」、「jER YX4000」、ADEKA股份有限公司製之「Adeka Resin EP-4100」、「Adeka Resin EP-4901」等。
脂環式環氧化合物中所含之脂環結構,可為單環,亦可為稠合環。脂環結構較佳為環烷結構。環烷結構之碳數可為4以上、10以下。例如,環烷結構可為環戊烷結構、環己烷結構、環庚烷結構、環辛烷結構、環壬烷結構、環癸烷結構等。脂環式環氧化合物中所含之脂環結構之數,可為一,亦可為複數。
就脂環式環氧化合物而言,可列舉環烯氧化物化合物、脂環族多元醇聚縮水甘油基醚化合物等。就脂環式環氧化合物而言,亦可使用市售之脂環式環氧化合物。就市售之脂環式環氧化合物而言,可列舉例如3,4-環氧環己基甲基-3’,4’-環氧環己烷甲酸酯(Daicel股份有限公司製「Celloxide 2021P」)(Celloxide為註冊商標;以下相同)、1,2:8,9二環氧檸檬烯(Daicel股份有限公司製「Celloxide 3000」)、二環戊二烯型環氧樹脂(DIC股份有限公司製「EPICLON HP-7200」)、氫化雙酚A二縮水甘油基醚(Nagase ChemteX股份有限公司製 「Denacol EX-252」)、六氫酞酸二縮水甘油基醚(阪本藥品工業股份有限公司製「SR-HHPA」)、1,4-環己烷二甲醇二縮水甘油基醚(新日本理化股份有限公司製「Rikaresin DME-100」)、1,3-雙胺基甲基環己烷(三菱氣體化學股份有限公司製)、1,3-雙(N,N-二縮水甘油基胺基甲基)環己烷(三菱氣體化學股份有限公司製「TETRAD-C」)、2,2-雙(羥基甲基)-1-丁醇之1,2-環氧-4-(2-環氧乙烷基)環己烷加成物(Daicel股份有限公司製「EHPE3150」)、SYNASIA公司製之「Syna-Epoxy 21」、「Syna-Epoxy 28」等。
就環氧化合物而言,可使用不含芳香環結構及脂環結構之環氧化合物(亦稱為「脂肪族環氧」)。就脂肪族環氧化合物而言,可使用市售之脂肪族環氧化合物。就市售之脂肪族環氧化合物而言,可列舉例如新戊二醇二縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-211」)、1,6-己二醇二縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-212P」)、乙二醇二縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-810」)、聚乙二醇二縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-861」)、丙二醇二縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-911」)、聚丙二醇二縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-941、EX-920、EX-931」)、甘油聚縮水甘油基醚(阪本藥品工業股份有限公司製「SR-GLG」)、二甘油聚縮水甘油基醚(阪本藥 品工業股份有限公司製「SR-DGE」)、三羥甲基丙烷聚縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-321」)、新戊四醇聚縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-411」)、己二酸二縮水甘油基醚(Nagase ChemteX股份有限公司製「Denacol EX-701」)、聚甘油聚縮水甘油基醚(阪本藥品工業股份有限公司製「SR-4GL」)、山梨醇系聚縮水甘油基醚(阪本藥品工業股份有限公司製「SR-SEP」)、聚丁二烯型環氧樹脂(Daicel股份有限公司製「Epolead PB3600」、Nagase ChemteX股份有限公司製「Denacol R-15EPT」、「FCA-061L]、「FCA-061M」)等。
樹脂組成物,就環氧化合物而言,亦可包含含有環氧基之矽烷偶合劑。就含有環氧基之矽烷偶合劑而言,可列舉如3-縮水甘油氧基丙基三甲氧基矽烷(3-glycidoxypropyltrimethoxysilane)、3-縮水甘油氧基丙基三乙氧基矽烷、3-縮水甘油氧基丙基甲基二乙氧基矽烷、2-(3,4環氧環己基)乙基三甲氧基矽烷等。
就環氧化合物而言,可將1種環氧化合物單獨使用,亦可將複數種環氧化合物組合使用。
樹脂組成物可依據用途,使環氧基開環聚合而硬化。就使其聚合之能量而言,無特別限定,可列舉熱及光。亦即,樹脂組成物可為熱硬化性,亦可為光硬化性。在使樹脂組成物藉由熱而硬化之情況,樹脂組成物可含有硬化劑。在將樹脂組成物藉由光硬化之情況,樹脂組成物可含有光聚合起始劑。
就硬化劑而言,可列舉例如胺系硬化劑、醯胺系硬化劑、酸酐系硬化劑、酚系硬化劑、活性酯系硬化劑、含有羧基之硬化劑、硫醇系硬化劑等。樹脂組成物,從水蒸氣阻隔性及氧阻隔性(例如高濕度下之氧阻隔性)更優良之觀點而言,以含有選自包含酸酐系硬化劑、酚系硬化劑及醯胺系硬化劑之群組中的至少一種硬化劑為較佳,以含有酸酐系硬化劑及酚系硬化劑中之至少一種為更佳。此等硬化劑可單獨使用1種,亦可將2種以上組合使用。
就胺系硬化劑而言,可列舉例如二胺基二苯基甲烷、二胺基二苯基乙烷、二胺基二苯基醚、二胺基二苯基碸、鄰苯二胺、間苯二胺、對苯二胺、間二甲苯二胺、對二甲苯二胺、二乙基甲苯二胺、二伸乙基三胺、三伸乙基四胺、異佛爾酮二胺、咪唑、BF3-胺錯合物、胍衍生物及胍胺衍生物。
就醯胺系硬化劑而言,可列舉二氰二胺(dicyanodiamide)、聚醯胺樹脂等。聚醯胺樹脂可藉由次亞麻油酸(linolenic acid)之二聚體及伸乙基二胺合成。就醯胺系硬化劑而言,從水蒸氣阻隔性及氧阻隔性(例如高濕度下之氧阻隔性)更優良之觀點而言,以使用二氰二胺為較佳。
就酸酐系硬化劑而言,可列舉琥珀酸酐、酞酸酐、偏苯三酸酐、苯均四酸酐(pyromellitic anhydride)、馬來酸酐、四氫酞酸酐、甲基四氫酞酸酐、甲基納迪克酸酐、六氫酞酸酐、甲基六氫酞酸酐、烯基 琥珀酸酐等。就酸酐系硬化劑而言,從水蒸氣阻隔性及氧阻隔性(例如高濕度下之氧阻隔性)更優良之觀點而言,以使用甲基四氫酞酸酐為較佳。
就酚系硬化劑而言,可例示由多元羥基化合物與甲醛所合成者。就多元羥基化合物而言,可列舉雙酚A、雙酚F、雙酚S、間苯二酚、氫醌、茀雙酚、4,4’-聯苯酚、4,4’,4”-三羥基三苯基甲烷、1,1,2,2-肆(4-羥基苯基)乙烷、杯芳烴(calixarene)等。就酚系硬化劑而言,具體言之,可列舉苯酚酚醛清漆樹脂、甲酚酚醛清漆樹脂、芳香族烴甲醛樹脂、改質酚樹脂、二環戊二烯酚加成型樹脂、苯酚芳烷基樹脂(Xylok樹脂)、間苯二酚酚醛清漆樹脂等。就酚系硬化劑而言,從水蒸氣阻隔性及氧阻隔性(例如高濕度下之氧阻隔性)更優良之觀點而言,以使用苯酚酚醛清漆樹脂為較佳。
從以上所述,樹脂組成物以含有選自包含酸酐系硬化劑、苯酚酚醛清漆樹脂及二氰二胺之群組的至少一種硬化劑為較佳,以含有選自包含甲基四氫酞酸酐、苯酚酚醛清漆樹脂及二氰二胺之群組的至少一種硬化劑為更佳。
在將樹脂組成物藉由熱使其硬化之情況,該樹脂組成物可進一步含有硬化促進劑(硬化觸媒)。硬化促進劑可單獨使用,亦可與上述硬化劑併用。就硬化促進劑而言,可使用促進環氧化合物之硬化反應的各種化合物。就硬化促進劑而言,可列舉例如磷系化合物、3級胺化合物、咪唑化合物、有機酸金屬鹽、路易士酸、 胺錯鹽等。就磷系化合物而言,可列舉如三苯基膦、三對甲苯基膦、及二苯基環己基膦。就3級胺化合物而言,可列舉如N,N-二甲基苄基胺、1,8-二吖雙環(5,4,0)十一烯-7、1,5-二吖雙環(4,3,0)壬烯-5、及參(二甲基胺基甲基)苯酚。就咪唑化合物而言,可列舉例如1-氰基乙基-2-乙基-4-甲基咪唑、及2-乙基-4-甲基咪唑。
就光聚合起始劑而言,只要用於藉由光照射使環氧基進行開環聚合之起始劑即可,無特別限定,例如可為光陽離子聚合起始劑。光聚合起始劑可為離子性光酸產生型,亦可為非離子性光酸產生型。
就離子性光酸產生型之光陽離子聚合起始劑而言,無特別限制,可列舉芳香族重氮鹽、芳香族鹵素鎓鹽、芳香族鋶鹽等鎓鹽類;鐵-芳烴錯合物、二茂鈦錯合物、芳基矽烷醇-鋁錯合物等有機金屬錯合物類。此等離子性光酸產生型之光陽離子聚合起始劑,可單獨使用,亦可將2種以上併用。
就非離子性光酸產生型之光陽離子聚合起始劑而言,無特別限定,可列舉例如硝基苄基酯、磺酸衍生物、磷酸酯、酚磺酸酯、偶氮萘醌、N-羥基亞胺膦酸等。此等非離子性光酸產生型之光陽離子聚合起始劑,可單獨使用,亦可將2種以上併用。
樹脂組成物中光聚合起始劑之摻配量,無特別限定,相對於100質量份之樹脂組成物總量,通常為0.1~10質量份。亦即,樹脂組成物中之光聚合起始劑的摻配量,相對於100質量份之樹脂組成物總量,可為0.1質量份以上,亦可為10質量份以下。
在使樹脂組成物藉由光而硬化之情況,為使光之感度提高,及為使光源之光的波長保持感度,可適宜地添加增感劑。此等增感劑為了調整硬化性,可與上述光聚合起始劑(例如光陽離子聚合起始劑)併用。就增感劑而言,可列舉蒽系化合物、噻噸酮(thioxanthone)系化合物等。
就用於使樹脂組成物進行光硬化之光源而言,只要使用在光聚合起始劑及增感劑之吸收波長發光的光源即可,可使用通常包含200~450nm範圍之波長的光源。具體而言,例如,可使用高壓水銀燈、超高壓水銀燈、金屬鹵化物燈、高功率金屬鹵化物燈、氙燈、碳弧燈、發光二極管等。
樹脂組成物可進一步含有修飾劑。就修飾劑而言,可列舉偶合劑、矽烷化合物等。此等修飾劑,可單獨使用1種,亦可將複數種組合使用。在樹脂組成物含有此等修飾劑之情況,鋰部分固定型膨潤石之濡濕性提高,在樹脂組成物中之分散性提高。再者,上述之酸酐可含於樹脂組成物中,作為修飾劑。
就偶合劑而言,可列舉如矽烷偶合劑、鈦偶合劑、鋯偶合劑、鋁偶合劑等。
就矽烷偶合劑而言,可列舉如含有胺基之矽烷偶合劑、含有(甲基)丙烯醯基之矽烷偶合劑、含有異氰酸基之矽烷偶合劑等。就含有胺基之矽烷偶合劑而言,可列舉如3-胺基丙基三甲氧基矽烷、N-2-(胺基乙基)-3-胺基丙基甲基二甲氧基矽烷、3-三乙氧基矽烷基 -N-(1,3-二甲基亞丁基)丙基胺、N-苯基-γ-胺基丙基三甲氧基矽烷等。就含有(甲基)丙烯醯基之矽烷偶合劑而言,可列舉例如3-丙烯醯氧基丙基三甲氧基矽烷、3-甲基丙烯醯氧基丙基三甲氧基矽烷、3-甲基丙烯醯氧基丙基三乙氧基矽烷等。就含有異氰酸基之矽烷偶合劑而言,可列舉例如3-異氰酸基丙基三乙氧基矽烷等。
就鈦偶合劑而言,可列舉例如異丙基三異硬脂醯基鈦酸酯、異丙基三辛醯基鈦酸酯、異丙基二甲基丙烯醯基異硬脂醯基鈦酸酯、異丙基異硬脂醯基二丙烯醯基鈦酸酯、異丙基參(二辛基焦磷酸酯)鈦酸酯、四辛基雙(二-十三基磷酸酯)鈦酸酯、四(2,2-二烯丙氧基甲基-1-丁基)雙(二-十三基)磷酸酯鈦酸酯、雙(二辛基焦磷酸酯)氧乙酸酯鈦酸酯、雙(二辛基焦磷酸酯)伸乙基鈦酸酯等。
就鋯偶合劑而言,可列舉例如乙酸鋯、碳酸鋯銨、氟化鋯等。
就鋁偶合劑而言,可列舉二異丙醇乙醯烷氧基鋁(acetoalkoxyaluminum diisopropylate)、二異丙氧基單乙基乙醯乙酸鋁(aluminum diisopropoxy monoethyl acetoacetate)、參(乙基乙醯乙酸)鋁(aluminum tris ethylacetoacetate)、參(乙醯基丙酮)鋁(aluminum tris acetylacetonate)等。
就矽烷化合物而言,可列舉烷氧基矽烷、矽氮烷、矽氧烷等。就烷氧基矽烷而言,可列舉甲基三甲氧基矽烷、二甲基二甲氧基矽烷、苯基三甲氧基矽烷、 甲基三乙氧基矽烷、二甲基二乙氧基矽烷、苯基三乙氧基矽烷、正丙基三甲氧基矽烷、正丙基三乙氧基矽烷、己基三甲氧基矽烷、己基三乙氧基矽烷、辛基三乙氧基矽烷、癸基三甲氧基矽烷、1,6-雙(三甲氧基矽烷基)己烷、三氟丙基三甲氧基矽烷等。就矽氮烷而言,可列舉六甲基二矽氮烷等。就矽氧烷而言,可列舉含有水解性基之矽氧烷等。
就修飾劑之摻配量而言,較佳為相對於鋰部分固定型膨潤石總量而言為0.1~50質量%。修飾劑之摻配量若為0.1質量%以上,鋰部分固定型膨潤石對樹脂組成物之分散性變得更為良好。又,若修飾劑之摻配量為50質量%以下,更能抑制修飾劑對樹脂組成物之機械物性的影響。修飾劑之摻配量,較佳為0.3~30質量%,更佳為0.5~15質量%。
樹脂組成物可依據使用用途而含有溶劑。就溶劑而言,可列舉有機溶劑,例如甲基乙基酮、丙酮、乙酸乙酯、乙酸丁酯、甲苯、二甲基甲醯胺、乙腈、甲基異丁基酮、甲醇、乙醇、丙醇、甲氧基丙醇、環己酮、甲基溶纖劑、乙基二乙二醇乙酸酯、丙二醇單甲基醚乙酸酯等。溶劑之種類及使用量可依據使用用途而適宜選擇。
樹脂組成物可在無損於本發明之效果的範圍,含有各種添加劑(除了相當於環氧化合物、鋰部分固定型膨潤石及修飾劑之化合物以外)。就添加劑而言,可例示例如有機填充劑、無機填充劑、安定劑(抗氧化劑、 熱安定劑、紫外線吸收劑等)、可塑劑、抗靜電劑、潤滑劑、抗結塊劑、著色劑、結晶成核劑、氧捕捉劑(具有氧捕捉功能之化合物)、賦黏劑等。此等各種添加劑可單獨使用或將二種以上組合使用。
添加劑之中,就無機填充劑而言,可列舉金屬、金屬氧化物、樹脂、礦物等無機物及此等之複合物。就無機填充劑之具體例而言,可列舉矽石、礬土、鈦、氧化鋯、銅、鐵、銀、雲母、滑石、鋁鱗片、玻璃鱗片、黏土礦物等。此等中,在使氣體阻隔性提高為目的時,較佳為使用黏土礦物,黏土礦物之中,更佳為使用膨潤性無機層狀化合物。
就膨潤性無機層狀化合物而言,可列舉例如含水矽酸鹽(層狀矽酸鹽(phyllosilicate)礦物等)、高嶺石族黏土礦物(禾樂石(halloysite)等)、膨潤石族黏土礦物(蒙脫石、貝得石、綠脫石、皂石、水輝石、鋅皂石、矽鎂石等)、蛭石族黏土礦物(蛭石等)等。此等礦物可為天然黏土礦物,亦可為合成黏土礦物。
就具有氧捕捉功能之化合物而言,可列舉例如受阻酚系化合物、維生素C、維生素E、有機磷化合物、沒食子酸、五倍子酚(pyrogallol)等與氧反應之低分子有機化合物,或鈷、錳、鎳、鐵、銅等過渡金屬化合物等。
就賦黏劑而言,可列舉二甲苯樹脂、萜樹脂、酚樹脂(酚系硬化劑除外)、松香樹脂等。藉由添加賦黏劑可使剛塗布後對各種薄膜材料之黏著性提高。相 對於100質量份之樹脂組成物總量,賦黏劑之添加量較佳為0.01~5質量份。
實施態樣之成形體,可將上述樹脂組成物成形而得到。成形方法為任意,可隨用途而適時選擇。成形體可由樹脂組成物構成,亦可由樹脂組成物之硬化物構成。成形體之形狀無限制,可為板狀、片狀、或薄膜狀,亦可具有立體形狀,可為塗布於基材者,亦可為存在於基材與基材之間之形式而成形者。
在製造板狀、片狀之成形體的情況,可列舉例如採用押出成形法、平面壓製、異形押出成形法、吹製成形法、壓縮成形法、真空成形法、射出成形法等之將樹脂組成物成形的方法。又,在製造薄膜狀之成形體的情況,可列舉如熔融押出法、溶液鑄造法、吹脹薄膜成形、製造成形、押出積層成形、壓延成形、片成形、纖維成形、吹製成形、射出成形、旋轉成形、被覆成形。在為使用熱或活性能量射線硬化之樹脂組成物的情況,可採取使用熱或活性能量射線的各種硬化方法將樹脂組成物成形。
在樹脂組成物為液狀之情況,可藉由塗敷成形。就塗敷方法而言,可列舉噴霧法、旋塗法、浸漬法、輥塗法、刀片塗布法、刮刀輥法、刮刀片法、淋幕塗布法、狹縫塗布法、網版印刷法、噴墨法、滴塗(dispensing)法等。
實施態樣之積層體為於基材上備有上述成形體者。積層體可為2層結構,亦可為3層結構以上。
基材之材質無特別限定,可依據用途而適宜選擇,可列舉如木材、金屬、塑膠、紙、矽或改質矽等,亦可為將不同原材料接合所得到的基材。基材之形狀無特別限制,可為平板、片狀、或三維形狀整面或一部分具有曲率者等視需要的任何形狀。又,基材之硬度、厚度等亦無限制。
積層體可藉由將上述成形體積層在基材上而得到。在基材上積層之成形體,可藉由對基材直接塗敷或直接成形而形成,亦可將樹脂組成物之成形體積層。在直接塗敷之情況,就塗敷方法而言,無特別限定,可列舉噴霧法、旋塗法、浸漬法、輥塗法、刀片塗布法、刮刀輥法、刮刀片法、淋幕塗布法、狹縫塗布法、網版印刷法、噴墨法等。在直接成形之情況,可列舉模內成形、插入成形、真空成形、押出積層成形、壓製成形等。在將樹脂組成物之成形體積層的情況,可將未硬化或半硬化之樹脂組成物層積層於基材上後使其硬化,亦可將樹脂組成物完全硬化的硬化物層積層於基材上。
又,積層體,可藉由對樹脂組成物之硬化物塗敷基材之前驅體並使其硬化而得到,亦可於基材之前驅體或樹脂組成物未硬化或半硬化之狀態,使其接著後硬化而得到。就基材之前驅體而言,無特別限定,可列舉各種硬化性樹脂組成物等。又,亦可藉由使用實施態樣之樹脂組成物作為接著劑,製成積層體。
上述之樹脂組成物由於水蒸氣阻隔性及氧阻隔性優良,適合使用作為氣體阻隔材料。氣體阻隔材料只要包含上述之樹脂組成物即可。
又,上述之樹脂組成物適合使用作為被覆材料。被覆材料只要包含上述之樹脂組成物即可。只要滿足作為阻隔被覆材料之各種特性,被覆材料之形式無限定。例如,若為熱硬化型之被覆材料,可為預先使環氧化合物與硬化劑混合後,再摻配鋰部分固定型膨潤石的1液型之被覆材料,亦可為將環氧化合物與硬化劑分開的2液混合型之被覆材料。在2液混合型之情況,可將鋰部分固定型膨潤石混合在環氧化合物及硬化劑之任一者或兩者中。
就被覆材料之被覆方法而言,無特別限制。就具體之方法而言,可例示輥塗、凹輪塗布等各種被覆方法。又,關於被覆裝置亦無特別限定。上述之樹脂組成物由於具有高氣體阻隔性,可適合利用作為氣體阻隔用被覆材料。
又,上述之樹脂組成物由於接著性優良,適合使用作為接著劑。接著劑只要包含上述樹脂組成物即可。接著劑之態樣無特別限定,可為液狀或糊狀之接著劑,亦可為固體狀之接著劑。樹脂組成物由於具有高氣體阻隔性,其接著劑適合利用作為氣體阻隔用接著劑。
在液狀或糊狀之接著劑的情況,可成為1液型之接著劑,亦可成為將硬化劑分開的2液型之接著劑。在液狀或糊狀之接著劑的情況,就使用方法而言,無特別限定,可塗布在一方之接著面後,貼合另一方之接著面並使其接著,亦可於注入接著面之界面後,使其接著。
在固體狀之接著劑的情況,可將成形為粉末狀、顆粒狀、或片狀之接著劑設置於接著面之界面,藉由熱熔解使其接著,並硬化。
以下,藉由實施例,進一步具體地說明本發明,然而本發明不受其限定。
就樹脂組成物所含有之填充劑而言,使用鋰部分固定型膨潤石或非鋰部分固定之膨潤石。鋰部分固定型膨潤石係使用Kunimine工業股份有限公司製之蒙脫石漿液(商品名:RCEC-W,陽離子交換容量:39.0meq/100g)。該分散漿液中之鋰部分固定型膨潤石的含量(w/w%)為20w/w%。又,非鋰部分固定之膨潤石係使用天然蒙脫石(商品名:Kunipia F,陽離子交換容量:108meq/100g,Kunimine工業股份有限公司製)(Kunipia為註冊商標)。
就修飾劑而言,使用為矽烷偶合劑之KBM-503(3-甲基丙烯醯氧基丙基三甲氧基矽烷,商品名,信越化學工業股份有限公司製)或為矽烷化合物之KBM-3033(正丙基三甲氧基矽烷,商品名,信越化學工業股份有限公司製)。
(實施例1)
相對於100質量份之雙酚A型液狀環氧化合物(商品名:EPICLON 850-S,DIC股份有限公司製),加入210質量份之上述鋰部分固定型膨潤石漿液,作為溶媒之384 質量份之乙腈、43質量份之水及93質量份之2-丙醇,與59.5質量份之修飾劑溶液,並保持攪拌8小時。然後,添加90質量份之甲基四氫酞酸酐(商品名:EPICLON B-570H,DIC股份有限公司製)、及1質量份之N,N-二甲基苄基胺(和光純藥工業股份有限公司製)。藉此,得到實施例1之樹脂組成物。將其設為塗敷液1。再者,修飾劑溶液係藉由將包含2.8質量份之KBM-503、0.6質量份之水、56.0質量份之2-丙醇、及0.1質量份之鹽酸(濃度:0.1mol/l)的溶液攪拌2小時而調製。
使用棒塗布器,將所得到之塗敷液1以乾燥後塗敷厚度成為2μm之方式塗敷於25μm之聚醯亞胺薄膜(東麗‧杜邦股份有限公司製Kapton薄膜)(Kapton為註冊商標;以下相同)上。將塗敷後之聚醯亞胺薄膜,於塗敷後立即於120℃之乾燥機中加熱1分鐘中。然後,於120℃之乾燥機中加熱處理3小時,進一步於175℃之乾燥機中加熱處理5小時。藉此,在聚醯亞胺薄膜上形成實施例1之樹脂組成物的成形體,而得到實施例1之積層薄膜。
在上述實施例1之樹脂組成物及成形體中,鋰部分固定型膨潤石之含量(填充劑量)係相對於不揮發成分總量而言為18質量%。
(實施例2~10)
除了使用表1所示之環氧化合物代替EPICLON 850-S、視情況使用甲基乙基酮(MEK)代替所用的乙腈及 水(參照實施例5及實施例6)作為溶媒、將各成分之摻配量變更為表1所示之值、以及使用以表1所示之摻配量調製的修飾劑溶液作為修飾劑溶液以外,係以與實施例1同樣之方法,得到實施例2~10之樹脂組成物。將此等分別設為塗敷液2~10。再者,修飾劑溶液係使用表1所示之調製溶液所用之各成分之摻配量的合計量。又,實施例2~6及實施例10中,將環氧化合物預先溶解於少量之MEK再使用。此時,實施例2~4及10中,使100質量份之環氧化合物溶解於42.9質量份之MEK。實施例5中,使100質量份之環氧化合物溶解於78.6質量份之MEK。實施例6中,使100質量份之環氧化合物溶解於150質量份之MEK。
繼而,除分別使用塗敷液2~10代替塗敷液1以外,係以與實施例1同樣方法,在25μm之聚醯亞胺薄膜(東麗‧杜邦股份有限公司製Kapton薄膜)上形成實施例2~10之樹脂組成物的成形體,得到實施例2~10之積層薄膜。
在實施例2~10之樹脂組成物及成形體中,鋰部分固定型膨潤石之含量(填充劑量)皆相對於不揮發成分總量而言為18質量%。
(實施例11~13)
除了使用表2所示之硬化劑代替B-570H、不使用N,N-二甲基苄基胺作為觸媒(硬化促進劑)、視情況不使用水作為溶媒(參照實施例12)、將各成分之摻配量變更 為表2所示之值、及使用以表2所示之摻配量調製的修飾劑溶液作為修飾劑溶液以外,係以與實施例1同樣之方法,得到實施例11~13之樹脂組成物。將此等分別設為塗敷液11~13。再者,修飾劑溶液係使用表2所示之調製溶液所用之各成分之摻配量的合計量。
繼而,除了分別使用塗敷液11~13代替塗敷液1以外,係以與實施例1同樣之方法,在25μm之聚醯亞胺薄膜(東麗‧杜邦股份有限公司製Kapton薄膜)上形成實施例11~13之樹脂組成物的成形體,得到實施例11~13之積層薄膜。
在實施例11~13之樹脂組成物及成形體中,鋰部分固定型膨潤石之含量(填充劑量)皆相對於不揮發成分總量而言為18質量%。
(實施例14)
除使用KBM3033代替KBM-503作為修飾劑、將各成分之摻配量變更為表2所示之值、及使用以表2所示之摻配量調製的修飾劑溶液作為修飾劑溶液以外,係以與實施例1同樣之方法,得到實施例14之樹脂組成物。將其設為塗敷液14。再者,修飾劑溶液係使用表2所示之調製溶液所用的各成分之摻配量的合計量。
繼而,除了使用塗敷液14代替塗敷液1以外,係以與實施例1同樣之方法,在25μm之聚醯亞胺薄膜(東麗‧杜邦股份有限公司製Kapton薄膜)上形成實施例14之樹脂組成物的成形體,得到實施例14之積層薄膜。
在實施例14之樹脂組成物及成形體中,鋰部分固定型膨潤石之含量(填充劑量)係相對於不揮發成分總量而言為18質量%。
(實施例15~18)
除了將各成分之摻配量變更為表2所示之值、及使用以表2所示之摻配量調製的修飾劑溶液作為修飾劑溶液以外,係以與實施例1同樣之方法,得到實施例15~18之樹脂組成物。將此等分別設為塗敷液15~18。再者,修飾劑溶液係使用表2所示之調製溶液所用之各成分之摻配量的合計量。
繼而,除了分別使用塗敷液15~18代替塗敷液1以外,係以與實施例1同樣之方法,在25μm之聚醯亞胺薄膜(東麗‧杜邦股份有限公司製Kapton薄膜)上形成實施例15~18之樹脂組成物的成形體,得到實施例15~18之積層薄膜。
在實施例15~18之樹脂組成物及成形體中,鋰部分固定型膨潤石之含量(填充劑量)分別相對於不揮發成分總量而言為5質量%、10質量%、30質量%、70質量%。
(比較例1)
相對於100質量份之雙酚A型液狀環氧化合物(商品名:EPICLON 850-S,DIC股份有限公司製),添加446質量份之上述天然蒙脫石(Kunipia F)、作為溶媒之3841 質量份之乙腈、427質量份之水及64質量份之2-丙醇,與126.5份之修飾劑溶液,保持攪拌8小時。然後,加入90質量份之甲基四氫酞酸酐(商品名:EPICLON B-570H,DIC股份有限公司製)、及1質量份之N,N-二甲基苄基胺(和光純藥工業股份有限公司製)。由此,得到比較例1之樹脂組成物。將其設為塗敷液19。再者,修飾劑溶液係藉由將包含24.2質量份之KBM503、5.3質量份之水、97.0質量份之2-丙醇、及0.1質量份之鹽酸(濃度:0.1mol/l)的溶液攪拌2小時而調製。
繼而,除了使用塗敷液19代替塗敷液1以外,係以與實施例1同樣之方法,形成比較例1之樹脂組成物的成形體,得到比較例1之積層薄膜。
在上述比較例1之樹脂組成物及成形體中,天然蒙脫石之含量(填充劑量)係相對於不揮發成分總量而言為70質量%,修飾劑之摻配量(修飾劑量)係相對於天然蒙脫石(填充劑)總量而言為5質量%。
(比較例2)
相對於100質量份之雙酚A型液狀環氧化合物(商品名:EPICLON 850-S、DIC股份有限公司製),添加500質量份之乙腈,保持攪拌8小時。然後,加入90質量份之甲基四氫酞酸酐(商品名:EPICLON B-570H,DIC股份有限公司製)、及1質量份之N,N-二甲基苄基胺(和光純藥工業股份有限公司製)。藉此,得到比較例2之樹脂組成物。將其設為塗敷液20。
繼而,除了使用塗敷液20代替塗敷液1以外,係以與實施例1同樣之方法,形成比較例2之樹脂組成物的成形體,得到比較例2之積層薄膜。
<評價>
關於實施例1~18及比較例1~2之積層薄膜,評價成膜性、氧透過性及水蒸氣透過性。評價結果如表1及表2所示。再者,成膜性、氧透過性及水蒸氣透過性之評價係藉由以下之方法實施。
(成膜性)
成膜性,以積層薄膜之塗敷面為平滑的情況評價為「A」,塗敷面不平滑之情況評價為「B」。
(氧透過率)
氧透過率之測定係以JIS-K7126(等壓法)為基準,使用MOCON公司製氧透過率測定裝置OX-TRAN1/50,於溫度23℃、濕度0%RH之氣體環境下以及溫度23℃、濕度90%RH之氣體環境下實施。再者,RH表示相對濕度。
(水蒸氣透過率)
水蒸氣透過率之測定係以JIS-K7129為基準,使用Illinois公司製水蒸氣透過率測定裝置7001,於溫度40℃、濕度90%RH之氣體環境下測定。
表1及表2所示之各環氧化合物及硬化劑之詳細如以下所示。
‧EP850S:雙酚A型液狀環氧化合物,商品名:EPICLON 850-S,DIC股份有限公司製,環氧當量:185g/eq
‧EP1050:雙酚A型固體環氧化合物,商品名:EPICLON 1050,DIC股份有限公司製,環氧當量:500g/eq
‧EP2050:雙酚A型固體環氧化合物,商品名:EPICLON 2050,DIC股份有限公司製,環氧當量:650g/eq
‧EP4050:雙酚A型固體環氧化合物,商品名:EPICLON 4050,DIC股份有限公司製,環氧當量:1000g/eq
‧EO7050:雙酚A型固體環氧化合物,商品名:EPICLON 7050,DIC股份有限公司製,環氧當量:2100g/eq
‧HM-091:雙酚A型固體環氧化合物,商品名:EPICLON HM-091,DIC股份有限公司製,環氧當量:2310g/eq
‧EP830:雙酚F型環氧化合物,商品名:EPICLON 830,DIC股份有限公司製,環氧當量:170g/eq
‧2021P:3,4-環氧環己基甲基-3’,4’-環氧環己烷甲酸酯,商品名:Celloxide 2021P,Daicel股份有限公司,環氧當量:130g/eq
‧EX-212:1,6己烷二醇二縮水甘油基醚,商品名:Denacol EX-212,Nagase ChemteX股份有限公司,環氧當量:116g/eq
‧EX-861:聚乙二醇二縮水甘油基醯,商品名:Denacol EX-861,Nagase ChemteX股份有限公司,環氧當量:550g/eq
‧B-570H:甲基四氫酞酸酐,商品名:EPICLON B-570H,DIC股份有限公司製
‧DICY7:二氰二胺,商品名,三菱化學股份有限公司製
‧TD-2090:苯酚酚醛清漆樹脂,商品名PHENOLITE TD-2090,DIC股份有限公司製
‧IPD:異佛爾酮二胺,商品名:Vestamin IPD,EVONIK公司製
本發明之樹脂組成物由於氣體阻隔性,尤其水蒸氣阻隔性及氧阻隔性優良,可適合使用於包裝材料,以及電子材料、建築材料等各種領域中。
Claims (12)
- 一種樹脂組成物,其含有環氧化合物及鋰部分固定型膨潤石。
- 如請求項1之樹脂組成物,其中前述環氧化合物之環氧當量為50~3000g/eq。
- 如請求項1或2之樹脂組成物,其中前述環氧化合物包含芳香環結構及脂環結構之中的至少一種結構。
- 如請求項1至3中任一項之樹脂組成物,其中前述鋰部分固定型膨潤石之陽離子交換容量為1~70meq/100g。
- 如請求項1至4中任一項之樹脂組成物,其進一步含有硬化劑。
- 如請求項5之樹脂組成物,其中前述硬化劑為選自包含酸酐系硬化劑、酚系硬化劑及醯胺系硬化劑之群組中的至少一種硬化劑。
- 如請求項1至6中任一項之樹脂組成物,其中相對於前述樹脂組成物之不揮發成分總量,前述鋰部分固定型膨潤石之含量為3~70質量%。
- 一種成形體,其為如請求項1至7中任一項之樹脂組成物的成形體。
- 一種積層體,其具備基材、及設置在該基材上的如請求項8之成形體。
- 一種氣體阻隔材料,其包含如請求項1至7中任一項之樹脂組成物。
- 一種被覆材料,其包含如請求項1至7中任一項之樹脂組成物。
- 一種接著劑,其包含如請求項1至7中任一項之樹脂組成物。
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CN (1) | CN110291151B (zh) |
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JP6901086B2 (ja) * | 2017-07-26 | 2021-07-14 | Dic株式会社 | 樹脂組成物、成形体、積層体、ガスバリア材、コーティング材及び接着剤 |
JP2019026813A (ja) * | 2017-08-03 | 2019-02-21 | Dic株式会社 | 樹脂組成物、成形体、積層体、ガスバリア材、コーティング材及び接着剤 |
JP6960629B2 (ja) * | 2017-08-22 | 2021-11-05 | Dic株式会社 | 樹脂組成物、成形体、積層体、ガスバリア材、コーティング材、接着剤及び積層体の製造方法 |
JP2020055936A (ja) * | 2018-10-01 | 2020-04-09 | Dic株式会社 | 封止剤および電子材料 |
CN110423586A (zh) * | 2019-08-15 | 2019-11-08 | 苏粤娟 | 一种用于食品包装的防水防霉粘合剂及其制备方法 |
US20220289901A1 (en) * | 2019-09-24 | 2022-09-15 | National University Corporation Yokohama National University | Epoxy resin, epoxy resin cured product, and epoxy resin composition |
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TW523532B (en) * | 2001-08-09 | 2003-03-11 | Ind Tech Res Inst | Epoxy/clay nanocomposite for copper clad laminate applications |
JP5099412B2 (ja) * | 2006-03-11 | 2012-12-19 | 独立行政法人産業技術総合研究所 | 変性粘土を用いた膜 |
JP4930917B2 (ja) * | 2006-08-28 | 2012-05-16 | 株式会社巴川製紙所 | 粘土薄膜フィルム、その製造方法および粘土薄膜積層体 |
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JP5212965B2 (ja) * | 2007-03-30 | 2013-06-19 | クニミネ工業株式会社 | 合成粘土材料及び粘土フィルム |
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JP5648814B2 (ja) * | 2010-06-03 | 2015-01-07 | 独立行政法人産業技術総合研究所 | 水蒸気バリア性フィルム及びその製造方法 |
JP2012121777A (ja) * | 2010-12-09 | 2012-06-28 | National Institute Of Advanced Industrial Science & Technology | もみ殻灰を用いた合成粘土及び粘土膜の製造方法 |
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- 2018-03-13 JP JP2019506050A patent/JP7072806B2/ja active Active
- 2018-03-13 CN CN201880011307.8A patent/CN110291151B/zh active Active
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US20200002465A1 (en) | 2020-01-02 |
WO2018168862A1 (ja) | 2018-09-20 |
JPWO2018168862A1 (ja) | 2020-01-23 |
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