TW201448322A - 電池用包裝材用聚氨酯接著劑、電池用包裝材、電池用容器及電池 - Google Patents
電池用包裝材用聚氨酯接著劑、電池用包裝材、電池用容器及電池 Download PDFInfo
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- TW201448322A TW201448322A TW103106038A TW103106038A TW201448322A TW 201448322 A TW201448322 A TW 201448322A TW 103106038 A TW103106038 A TW 103106038A TW 103106038 A TW103106038 A TW 103106038A TW 201448322 A TW201448322 A TW 201448322A
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Classifications
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
本發明提供一種在長期耐久試驗後亦可維持大的接著強度、可形成成型性優異的電池用包裝材的接著劑。本發明的電池用包裝材用聚氨酯接著劑含有主劑與硬化劑,主劑包含數量平均分子量為10,000~100,000、且羥值為1 mgKOH/g~100 mgKOH/g的丙烯酸系多元醇(A),相對於源自丙烯酸系多元醇(A)的羥基,源自硬化劑中所含的芳香族異氰酸酯(B)的異氰酸酯基的當量比[NCO]/[OH]設為10~30。
Description
本發明是有關於一種用以形成電池用容器或電池封裝(pack)的電池用包裝材用聚氨酯接著劑。並且本發明是有關於一種使用上述電池用包裝材用聚氨酯接著劑而積層的電池用包裝材。而且本發明是有關於一種將上述電池用包裝材成型而成的電池用容器、及使用上述電池用容器而成的電池。
由於行動電話、可攜型電腦等電子設備的急速成長,輕量且小型的鋰離子電池等二次電池的需求增大。作為二次電池的外包裝體,先前使用金屬製罐,但就輕量化或生產性的觀點而言,將塑膠膜或鋁箔等積層而成的包裝材正成為主流。
作為最簡易的包裝材,可列舉:如圖1所示的自外層側起依序包含外層側樹脂膜層(11)、外層側接著劑層(12)、金屬箔層(13)、內層側接著劑層(14)及含有熱密封層等的內面層(15)的積層體。作為電池用容器,例如如圖2所示,有以外層側樹脂
膜層(11)構成凸面、內面層(15)構成凹面的方式將上述包裝材成型(伸拉成型加工、突出成型加工等)者。電池可藉由在電池用容器的凹面側封入電極或電解液等進行密封而製造。
作為電池用包裝材,揭示有以下的構成:在外層側積層
耐熱性樹脂延伸膜層、在內層側積層熱塑性樹脂未延伸膜層、在該些兩膜之間積層鋁箔層的電池用容器包材中,熱塑性樹脂未延伸膜層與鋁箔層經由含有具有羧基的聚烯烴樹脂、及多官能異氰酸酯化合物而成的接著劑層而接著(專利文獻1)。
另外,揭示有電子零件盒用包材,其自外側起依序需要
耐熱性樹脂延伸膜層、鋁箔層及熱塑性樹脂未延伸膜層,在鋁箔層與熱塑性樹脂未延伸膜層之間設置丙烯酸系聚合物層而成(專利文獻2)。
另外揭示,在鋰電池用外包裝材中,作為在延伸聚醯胺
膜等基材層與鋁箔層之間所用的接著劑,在聚酯多元醇或丙烯酸系多元醇等主劑中,使用異氰酸酯化合物作為硬化劑,NCO/OH較佳為1~10,更佳為2~5(專利文獻3)。此外,在專利文獻4~專利文獻6中揭示電池用外包裝材。
[現有技術文獻]
[專利文獻]
[專利文獻1]日本專利特開2010-92703號公報
[專利文獻2]日本專利特開2002-187233號公報
[專利文獻3]日本專利特開2012-124067號公報第25段
[專利文獻4]日本專利特開2002-002511號公報
[專利文獻5]國際公開第2008/093778號
[專利文獻6]國際公開第2009/041077號
近年來,隨著在車載或家庭蓄電等的用途擴大,而對二次電池要求大容量化,並對電池用包裝材要求良好的成型性。
另外,車載或家庭蓄電用途的二次電池設置於室外,而進一步要求長期的耐用年數,因此要求在長期耐久試驗後亦可維持包裝材的各塑膠膜或金屬箔等層間的接著強度,而且外觀無異常。
本發明是鑒於上述背景而成者,課題是提供一種具有優異的成型性、在長期耐久性試驗後層間的接著強度亦高、且外觀性優異的電池、電池用容器、電池用包裝材及電池用包裝材用聚氨酯接著劑。
本發明是鑒於上述課題而成者,是有關於一種電池用包裝材用聚氨酯接著劑,其含有主劑與硬化劑,且上述主劑包含數量平均分子量為10,000~100,000、且羥值為1mgKOH/g~100mgKOH/g的丙烯酸系多元醇(A),相對於源自丙烯酸系多元醇(A)的羥基,源自上述硬化劑中所含的芳香族聚異氰酸酯(B)的異氰酸酯基的當量比[NCO]/[OH]為10~30。
本發明的電池用包裝材用聚氨酯接著劑較佳為丙烯酸系多元醇(A)的玻璃轉移溫度(Tg)為-20℃~30℃。
另外,本發明的電池用包裝材用聚氨酯接著劑較佳為進一步
含有:選自由矽烷偶合劑(C)、及磷酸或磷酸系化合物(D)所組成的組群的至少一種添加劑。
另外,本發明是有關於一種電池用包裝材,其自外層起
依序需要外層側樹脂膜層、外層側接著劑層、金屬箔層、內層側接著劑層、內面層,其特徵在於:上述外層側接著劑層藉由上述本發明的電池用包裝材用聚氨酯接著劑而形成。
本申請案發明的電池用包裝材較佳為上述外層側樹脂膜層為聚醯胺膜或/及聚酯膜,上述內面層為聚烯烴系膜。
而且,本發明是有關於一種電池用容器,其由上述電池
用包裝材成型而成,且外層側樹脂膜層構成凸面,內面層構成凹面。
而且,本發明是有關於一種電池,其使用上述電池用容
器而成。
根據本發明,會發揮出如下的優異效果:可提供具有優異的成型性、在長期耐久性試驗後層間的接著強度亦高、且外觀性優異的電池、電池用容器、電池用包裝材及電池用包裝材用聚氨酯接著劑。
(11)‧‧‧外層側樹脂膜層
(12)‧‧‧外層側接著劑層
(13)‧‧‧金屬箔層
(14)‧‧‧內層側接著劑層
(15)‧‧‧內面層
圖1是表示本發明的電池用包裝材的一個形態的示意性剖面圖。
圖2是本發明的電池用容器的一個形態(托盤狀)的示意性立體圖。
以下,對本發明的實施形態進行詳細地說明。另外,在本說明書中,「任意的數A~任意的數B」的記載是指數A及大於數A的範圍、且數B及小於數B的範圍。
本發明的聚氨酯接著劑用於形成用以獲得電池用容器的電池用包裝材。電池用容器的形狀並無特別限定,除了如圖2所示的托盤狀者外,可例示:筒狀(圓筒、四角筒、橢圓筒等)者。該些電池用容器可將平的狀態的電池用包裝材進行成型加工而得。電池用容器的內側、即與電解液接觸的面為內面層(15)。作為內面層(15)的較佳的例子,可列舉熱密封層。藉由使用熱密封層,而使凸緣部的內面層(15)、與構成另外電池用包裝材的內面層(15)或另外電池用容器的凸緣部的內面層(15)對向、接觸,並加熱,藉此可使內面層(15)彼此融接,並封入電解液。內面層在不脫離本發明的主旨的範圍內並無限定,可例示聚烯烴系膜作為較佳的例子。
電池用容器具備金屬箔(13)。在電池用容器中,通常以金屬箔(13)為界將靠近電解液之側稱為「內側」,將內側的層稱為「內層」,將遠側稱為「外側」,將外側的層稱為「外層」。因此,在形成電池用容器的預定的電池用包裝材中,亦以金屬箔(13)為界將位置靠近電解液的預定之側稱為「內側」,將內側的層稱為
「內層」,將位置遠離的預定之側稱為「外側」,將外側的層稱為「外層」。
本發明的聚氨酯系接著劑適合於用以將外層側樹脂膜層(11)與金屬箔層(13)積層(貼合)的用途。
本發明的聚氨酯系接著劑是使用主劑與硬化劑者。可為在使用時將主劑與硬化劑混合的所謂的二液混合型接著劑,亦可為預先混合主劑與硬化劑的一液型接著劑。而且,還可為在使用時將多種主劑及/或多種硬化劑混合的類型。
本發明的聚氨酯系接著劑是主劑具有羥基的多元醇成分,並含有丙烯酸系多元醇(A)。多元醇成分在滿足本發明的目的、效果的範圍內可進一步包含丙烯酸系多元醇(A)以外的多元醇。
丙烯酸系多元醇(A)較佳為使用:含有羥基的單(甲基)丙烯酸酯單體、與不含有羥基的單(甲基)丙烯酸酯單體的共聚物。含有羥基的單(甲基)丙烯酸酯單體是在1分子中含有1個(甲基)丙烯醯基與1個以上羥基的單體,且除了一元醇外,還包括二元醇的單(甲基)丙烯酸酯單體等。
具有1個羥基的單(甲基)丙烯酸酯單體例如可藉由使二元醇與(甲基)丙烯酸反應而得。作為具體例,可列舉:(甲基)丙烯酸2-羥基乙酯、(甲基)丙烯酸2-羥基丙酯、(甲基)丙烯酸3-羥基丙酯、(甲基)丙烯酸2-羥基丁酯、丙烯酸4-羥基丁酯(商品名4HBA、三菱化學公司製造)、甲基丙烯酸4-羥基丁酯、丙烯酸α-羥基甲基
乙酯、丙烯酸α-羥基甲酯、己內酯改質羥基(甲基)丙烯酸酯(商品名PLACCEL F系列、大賽璐化學工業(Daicel Chemical industries)公司製造)、(聚)乙二醇單(甲基)丙烯酸酯。
而且,亦可利用如(甲基)丙烯酸2,3-二羥基丙酯等般的
具有2個羥基的單(甲基)丙烯酸酯單體。例如可使三元醇與(甲基)丙烯酸反應而得。
作為單(甲基)丙烯酸酯單體,可列舉:(甲基)丙烯酸環
己酯、(甲基)丙烯酸甲基環己酯、(甲基)丙烯酸第三丁基環己酯、(甲基)丙烯酸環十二烷基酯等含有環烷基的單體,丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丁酯、丙烯酸異丁酯、丙烯酸第三丁酯、丙烯酸第二丁酯、丙烯酸正丙酯、丙烯酸異丙酯、丙烯酸異戊酯、丙烯酸2-乙基己酯、丙烯酸異癸酯、丙烯酸十三烷基酯、丙烯酸正辛酯、丙烯酸異辛酯、丙烯酸正月桂酯、丙烯酸苄酯、丙烯酸二環戊酯、丙烯酸正硬脂酯、丙烯酸異硬脂酯、丙烯酸異冰片酯、丙烯酸2-(乙醯乙醯氧基)乙酯、丙烯酸苯氧基乙酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸正丁酯、甲基丙烯酸異丁酯、甲基丙烯酸第三丁酯、甲基丙烯酸第二丁酯、甲基丙烯酸正丙酯、甲基丙烯酸異丙酯、甲基丙烯酸異戊酯、甲基丙烯酸2-乙基己酯、甲基丙烯酸異癸酯、甲基丙烯酸十三烷基酯、甲基丙烯酸正辛酯、甲基丙烯酸異辛酯、甲基丙烯酸正月桂酯、甲基丙烯酸苄酯、甲基丙烯酸二環戊酯、甲基丙烯酸正硬脂酯、甲基丙烯酸異硬脂酯、甲基丙烯酸異冰片酯、甲基丙烯酸2-乙醯乙醯氧基乙酯(商品名
AAEM、伊士曼(Eastman))、甲基丙烯酸苯氧基乙酯等。而且可使用:(甲基)丙烯酸、順丁烯二酸、順丁烯二酸酐等含有羧基的單體、或其酐,或苯乙烯等乙烯系單體。
作為丙烯酸系多元醇(A)的分子量,數量平均分子量
較佳為10,000~100,000,更佳為20,000~70,000。
在工業上生產電池用包裝材時,將長條狀態者捲取成卷狀。並且,為了使捲取成卷狀的積層體中的接著劑層充分地硬化,而在維持為高溫的倉庫中進行數天老化。
藉由將丙烯酸系多元醇(A)的數量平均分子量設為10,000以上,而可提高老化前或硬化中途所存在的接著劑層的凝聚力,並可抑制、防止外觀不良等加工異常(捲取狀態下產生偏移或***)的產生。而且藉由將丙烯酸系多元醇(A)的數量平均分子量設為10,000以上,而可抑制、防止硬化塗膜的脆化,並可確保基材與接著劑間的剝離應力緩和,還可抑制、防止因積層強度的降低或接著力不足引起的***的產生。
另一方面,藉由將丙烯酸系多元醇(A)的數量平均分子量設為100,000以下,而可確保在稀釋溶劑中的溶解性,並可使接著劑塗敷時的黏度為適度的範圍,而確保塗敷性。另外認為,塗敷接著劑的硬化初始階段的乾燥塗膜藉由丙烯酸系分子鏈的相互纏繞,而結構黏性變高,在側鏈所具有的羥基的自由度降低,而阻礙丙烯酸系多元醇(A)中的羥基與後述的硬化劑中的異氰酸酯基的反應。藉由將丙烯酸系多元醇(A)的數量平均分子量設為
100,000以下,而抑制硬化初始階段的丙烯酸系分子鏈的相互纏繞,並抑制羥基與異氰酸酯基的反應阻礙,藉此可確保充分的氨酯交聯度,並獲得成型性優異的包裝材。
丙烯酸系多元醇(A)的數量平均分子量是藉由凝膠滲
透層析法(Gel Permeation Chromatography,GPC)而得的聚苯乙烯換算的值。例如,將管柱(昭和電工公司製造的KF-805L、KF-803L、及KF-802)的溫度設為40℃,使用四氫呋喃(tetrahydrofuran,THF)作為溶離液,將流速設為0.2mL/min,將檢測設為折射率(Refractive Index,RI),將試樣濃度設為0.02%,並使用聚苯乙烯作為標準試樣而進行測定。本發明的數量平均分子量記載藉由上述方法而測定的值。
丙烯酸系多元醇(A)的羥值為1mgKOH/g~100
mgKOH/g,較佳為1mgKOH/g~50mgKOH/g,更佳為1mgKOH/g~15mgKOH/g。若羥值超過100mgKOH/g,則丙烯酸系多元醇(A)與作為硬化劑而含有的芳香族異氰酸酯(B)的交聯密度變得過高,而與外層側樹脂膜層的接著力降低,並且成型性亦降低。
藉由丙烯酸系多元醇(A)的羥值為上述範圍,而外層側樹脂膜層及金屬箔層的接著強度變得良好,而且丙烯酸系多元醇(A)與硬化劑中所含的芳香族異氰酸酯(B)形成恰當的交聯密度,藉此獲得良好的成型性。
另外,丙烯酸系多元醇(A)的玻璃轉移溫度較佳為-20℃
~30℃的範圍,更佳為0℃~15℃的範圍。
藉由丙烯酸系多元醇(A)的玻璃轉移溫度為上述範圍,而充分具有保持剛積層後的接著強度的初始黏性,並獲得成型性或成型物的耐濕熱性優異的成型物。
丙烯酸系多元醇(A)的玻璃轉移溫度藉由示差掃描熱量儀(Differential Scanning Calorimeter,DSC)測定而求出。具體而言,將約10mg的試樣冷卻至-100℃後,以10℃/min升溫而獲得DSC圖表,並根據該DSC圖表求出玻璃轉移溫度。在丙烯酸系多元醇(A)溶解於有機溶劑時,進行乾燥後以相同的方式求出玻璃轉移溫度。
作為主劑所含的多元醇成分,亦可併用丙烯酸系多元醇
(A)以外的多元醇。例如可例示:乙二醇、三羥甲基丙烷等低分子多元醇,及聚醚多元醇,聚碳酸酯多元醇,聚烯烴多元醇,聚酯多元醇。另外可列舉:使該些單獨或併用2種以上與有機異氰酸酯反應而得的聚氨酯多元醇等。丙烯酸系多元醇(A)以外的多元醇可在不對接著強度或成型性造成不良影響的程度下使用。
本發明的聚氨酯接著劑包含芳香族聚異氰酸酯(B)作
為硬化劑。芳香族聚異氰酸酯(B)可為藉由有機溶劑稀釋聚異氰酸酯而成的狀態者,亦可為未稀釋的狀態者。
作為芳香族聚異氰酸酯(B),可列舉:間苯二異氰酸酯、對苯二異氰酸酯、4,4'-二苯基二異氰酸酯、1,5-萘二異氰酸酯、4,4'-二苯基甲烷二異氰酸酯、2,4-甲苯二異氰酸酯或2,6-甲苯二異氰酸酯或其混合物、4,4'-甲苯胺二異氰酸酯、聯茴香胺二異氰酸酯、
4,4'-二苯醚二異氰酸酯等芳香族二異氰酸酯;三苯基甲烷-4,4',4"-三異氰酸酯、1,3,5-三異氰酸酯苯、2,4,6-三異氰酸酯甲苯等有機三異氰酸酯,4,4'-二苯基二甲基甲烷-2,2'-5,5'-四異氰酸酯等有機四異氰酸酯等聚異氰酸酯單體;由上述聚異氰酸酯單體衍生的二聚物、三聚物、縮二脲、脲基甲酸酯,由二氧化碳與上述聚異氰酸酯單體而得的具有2,4,6-噁二嗪三酮環的聚異氰酸酯;或乙二醇、丙二醇、丁二醇、己二醇、新戊二醇、1,6-己二醇、3-甲基-1,5-戊二醇、3,3'-二羥甲基丙烷、環己烷二甲醇、二乙二醇、三乙二醇、二丙二醇、甘油、三羥甲基丙烷、季戊四醇、山梨糖醇等分子量小於200的低分子多元醇與上述聚異氰酸酯單體加成而得的加成物;或分子量為200~20,000的聚酯多元醇、聚醚酯多元醇、聚酯醯胺多元醇、聚己內酯多元醇、聚戊內酯多元醇、丙烯酸系多元醇、聚碳酸酯多元醇、聚羥基烷烴、蓖麻油、聚氨酯多元醇等與上述聚異氰酸酯單體加成而得的加成物等。
其中,就包裝材的生產性及成型性的觀點而言,更佳為由4,4'-二苯基甲烷二異氰酸酯、及2,4-甲苯二異氰酸酯或2,6-甲苯二異氰酸酯衍生的有機聚異氰酸酯。
本發明的聚氨酯接著劑相對於主劑中所含的丙烯酸系
多元醇(A)所具有的羥基,源自硬化劑中所含的芳香族異氰酸酯(B)的異氰酸酯基的當量比[NCO]/[OH]為10~30,較佳為15~
25。藉由相對於羥基1莫耳,而將芳香族異氰酸酯基設為10莫耳以上,而可形成充分的交聯密度的接著劑層,並可獲得成型性優異的包裝體。另一方面,藉由相對於羥基1莫耳,而將芳香族異氰酸酯基設為30莫耳以下,而直至硬化結束為止不需要長時間,並可獲得積層強度優異的包裝體。而且就衛生性、經濟性的方面而言,亦較佳為將芳香族異氰酸酯基設為30莫耳以下。
一般認為,藉由當量比為上述的範圍內,藉由芳香族異氰酸酯基彼此利用脲鍵的自交聯、及利用一部分芳香族異氰酸酯與水分的反應的末端胺化,而可形成不但具有對金屬箔層的牢固的接著性而且一併具有需要高的楊氏模數(Young Modulus)的成型性的塗膜。
就提高對於金屬箔等金屬系原材料的接著強度的觀點而言,本發明的聚氨酯接著劑較佳為包含矽烷偶合劑(C)。
作為矽烷偶合劑(C),例如可列舉:乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷等具有乙烯基的三烷氧基矽烷;3-胺基丙基三乙氧基矽烷、N-(2-胺基乙基)3-胺基丙基三甲氧基矽烷等具有胺基的三烷氧基矽烷;3-縮水甘油氧基丙基三甲氧基矽烷、2-(3,4-環氧環己基)乙基三甲氧基矽烷、3-縮水甘油氧基丙基三乙氧基矽烷等具有縮水甘油基的三烷氧基矽烷。該些分別可單獨使用,或者可任意地組合2種以上而使用。
相對於多元醇成分的固體成分100質量份,矽烷偶合劑(C)的添加量較佳為0.1質量份~5質量份,更佳為0.5質量份~3質
量份。藉由添加上述範圍的矽烷偶合劑(C),而可提高對於金屬箔的接著強度。另外,矽烷偶合劑(C)較佳為與丙烯酸系多元醇(A)一起包含在主劑中。
就提高對於金屬箔等金屬系原材料的接著強度的觀點
而言,本發明所使用的聚氨酯接著劑較佳為包含磷酸或磷酸系化合物(D)。另外,磷酸或磷酸系化合物(D)較佳為與丙烯酸系多元醇(A)一起包含在主劑中。
在磷酸或磷酸系化合物(D)中,作為磷酸,只要為具
有至少1個游離的氧酸者即可,例如可列舉:次磷酸(hypophosphorous acid)、亞磷酸、正磷酸、低磷酸(hypophosphoric acid)等磷酸類,偏磷酸、焦磷酸、三聚磷酸、聚磷酸、超磷酸等縮合磷酸類。另外,作為磷酸的衍生物的磷酸系化合物可列舉:使上述磷酸在殘留至少1個游離的氧酸的狀態下與醇類部分地酯化者等。作為該些醇,可列舉:甲醇、乙醇、乙二醇、甘油等脂肪族醇,苯酚、二甲苯酚、對苯二酚、鄰苯二酚、間苯三酚等芳香族醇等。磷酸或磷酸系化合物(D)能以1種使用,亦能以任意的組合而組合2種以上來使用。磷酸或磷酸系化合物(D)的添加量以接著劑的固體成分為基準較佳為0.01質量%~10質量%,更佳為0.05質量%~5質量%,特佳為0.05質量%~1質量%。
此外,作為接著劑用途,可在主劑、或硬化劑中調配公
知的添加劑。例如可使用反應促進劑。例如可列舉:二乙酸二丁基錫、二月桂酸二丁基錫、二月桂酸二辛基錫、二順丁烯二酸二
丁基錫等金屬系觸媒;1,8-二氮雜雙環(5,4,0)十一碳烯-7、1,5-二氮雜雙環(4,3,0)壬烯-5、6-二丁基胺基-1,8-二氮雜雙環(5,4,0)十一碳烯-7等三級胺;如三乙醇胺般的反應性三級胺等,可使用選自該些的組群的1種或2種以上反應促進劑。
為了提高積層外觀,亦可在主劑中調配公知的勻平劑或消泡劑。作為勻平劑,例如可列舉:聚醚改質聚二甲基矽氧烷、聚酯改質聚二甲基矽氧烷、芳烷基改質聚甲基烷基矽氧烷、聚酯改質含有羥基的聚二甲基矽氧烷、聚醚酯改質含有羥基的聚二甲基矽氧烷、丙烯酸系共聚物、甲基丙烯酸系共聚物、聚醚改質聚甲基烷基矽氧烷、丙烯酸烷基酯共聚物、甲基丙烯酸烷基酯共聚物、卵磷脂等。
作為消泡劑,可列舉:矽酮樹脂、矽酮溶液、烷基乙烯醚與丙烯酸烷基酯及甲基丙烯酸烷基酯的共聚物等公知者。
本發明的電池用包裝材例如可藉由通常所用的方法而製造。
例如,使用本發明的聚氨酯接著劑將外層側樹脂膜層(11)與金屬箔層(13)積層,而獲得中間積層體。繼而,可使用內層側接著劑在中間積層體的金屬箔層(13)面積層內面層(15)。
或者,使用內層側接著劑將金屬箔層(13)與內面層(15)積層,而獲得中間積層體。繼而,可使用本發明的聚氨酯接著劑,將中間積層體的金屬箔層(13)與外層側樹脂膜層(11)積層。
為前者時,本發明的聚氨酯接著劑只要塗佈在外層側樹脂膜
層(11)或金屬箔層(13)的任一層的基材的單面,使溶劑揮發後,在加熱加壓下在接著劑層上重疊另一基材,繼而在常溫或加溫下老化,使接著劑層硬化即可。接著劑層量較佳為1g/m2~15g/m2左右。
後者的情形亦相同,本發明的聚氨酯接著劑只要塗佈於外層側樹脂膜層(11)或中間積層體的金屬箔層(13)面的任一層面上即可。
在將聚氨酯系接著劑塗敷於基材上時,為了將塗液調整
為適度的黏度,而可在乾燥步驟中在對基材無影響的範圍內包含溶劑。
作為溶劑,可列舉:丙酮、甲基乙基酮、甲基異丁基酮、環己酮等酮系化合物,乙酸甲酯、乙酸乙酯、乙酸丁酯、乳酸乙酯、乙酸甲氧基乙酯等酯系化合物,二***、乙二醇二甲醚等醚系化合物,甲苯、二甲苯等芳香族化合物,戊烷、己烷等脂肪族化合物,二氯甲烷、氯苯、氯仿等鹵化烴化合物,乙醇、異丙醇、正丁醇等醇類,水等。該些溶劑可單獨使用,亦可併用2種以上。
作為本發明中塗敷聚氨酯系接著劑的裝置,可列舉:缺
角輪塗佈機(comma coater)、乾式貼合機、輥刀片塗佈機、模塗機、輥塗機、棒塗機、凹版輥塗佈機、逆輥塗佈機、刮刀塗佈機(blade coater)、凹版塗佈機、微凹版塗佈機等。
構成本發明的電池用外包裝材的外層側樹脂膜層(11)並無特別限定,較佳為使用包含聚醯胺或聚酯的延伸膜。另外,
可藉由碳黑或氧化鈦等顏料進行著色。另外,亦可塗佈用以賦予滑性或防止受傷或對於氫氟酸的防止腐蝕的塗佈劑、或旨在創意設計性的油墨等。另外,亦可預先積層2層以上的膜。膜層的厚度並無特別限定,較佳為12μm~100μm。
構成本發明的電池用外包裝材的金屬箔層(13)的厚度
並無特別限定,較佳為20μm~80μm。另外,較佳為在金屬箔層表面進行藉由磷酸鹽、鉻酸鹽、氟化物、三嗪硫醇化合物、異氰酸酯化合物等的化成處理。藉由實施化成處理,而可抑制因電池的電解液引起的金屬箔層表面的腐蝕劣化。而且較佳為在化成處理表面上在200℃左右的高溫下將醯胺樹脂、丙烯酸系樹脂、偶合劑等公知的金屬處理劑燒附於金屬,進行有機處理。藉由實施有機處理,而使金屬箔層與接著劑更牢固地接著,而可進一步抑制金屬箔層與接著劑間的***。
構成本發明的電池用外包裝材的內面層(15)並無特別
限定,較佳為熱密封層,較佳為包含選自由聚乙烯、聚丙烯、烯烴系共聚物、該些的酸變成物及離子聚合物所組成的組群的至少1種熱塑性樹脂的未延伸膜。膜的厚度並無特別限定,較佳為20μm~150μm。
形成構成本發明的電池用外包裝材的內層側接著劑層(14)的接著劑並無特別限定,較佳為金屬箔層(13)與內面層(15)的接著強度不會因電池的電解液而降低者,可使用公知的接著劑。
例如,可藉由凹版塗佈機等將組合了聚烯烴樹脂與多官能異氰酸酯的接著劑或組合了多元醇與多官能異氰酸酯的接著劑塗佈於金屬箔層上,使溶劑乾燥,在加熱加壓下在接著劑層上重疊內面層(15),繼而在常溫或加溫下老化並使金屬箔層(13)與內面層(15)貼合。
或者,可藉由T模擠出機將酸改質聚丙烯等接著劑熔融擠出至金屬箔層(13)上而形成接著劑層,在上述接著劑層上重疊內面層(15),並使金屬箔層(13)與內面層(15)貼合。
在外層側接著劑層(12)及內層側接著劑層(14)這兩者需要老化時,可一併老化。另外,老化溫度設為室溫~90℃,藉此在2天~2週(week)內完成硬化,而表現出成型性。
本發明的電池用容器可使用上述電池用外包裝材,以外
層側樹脂膜層(11)構成凸面、內面層(15)構成凹面的方式進行成型而得。
另外,本發明中所謂的「凹面」,是指在將平的狀態的電池用包裝材進行成型加工而形成如圖2所示的托盤狀時,具有內部可收納電解液的凹陷的面,本發明中所謂的「凸面」,是指具有上述凹陷的面的自身背面。
根據本發明的電池用包裝材,為了形成外層側接著劑
層,而使用本發明的聚氨酯接著劑,因此層間的接著強度優異,成型時可有效地防止膜的斷裂,而有效地防止成型部的***的產生。另外,可提供在耐久性試驗後,亦可維持上述性能的電池用
包裝材。藉由使用上述電池用包裝材而成的電池用容器,而可提供可靠性優異的電池。
[實施例]
繼而,列舉實施例及比較例對本發明進行更具體地說明。實施例及比較例中的%全部是指質量%。
(丙烯酸系多元醇合成例)
在具備冷凝器、氮氣導入管、滴液漏斗、及溫度計的四口燒瓶中,投入乙酸乙酯100質量份,並升溫至80℃。繼而,自滴液漏斗歷時2小時在四口燒瓶中滴加:預先混合丙烯酸正丁酯41.5質量份、甲基丙烯酸乙酯56.5質量份、丙烯酸1.0質量份、丙烯酸2-羥基乙酯1.0質量份、及偶氮雙異丁腈0.4質量份而成的單體液。然後,反應1小時並添加偶氮雙異丁腈0.04質量份,繼而反應1小時後,進行冷卻,添加乙酸乙酯而獲得固體成分為50%的丙烯酸系多元醇溶液(A-1)。
除了根據聚合起始劑偶氮雙異丁腈的添加量調節分子量、或更換單體組成以外,以相同的方式,藉由表1所示的單體組成獲得固體成分為50%的丙烯酸系多元醇溶液(A-2)~丙烯酸系多元醇溶液(A-12)。
另外,數量平均分子量、玻璃轉移溫度如上所述,藉由GPC及DSC而求出。
具體而言,數量平均分子量是將管柱(昭和電工公司製造的KF-805L、KF-803L、及KF-802)的溫度設為40℃,使用THF作
為溶離液,並將流速設為0.2mL/min,將檢測設為RI,將試樣濃度設為0.02%,使用聚苯乙烯作為標準試樣而求出。
另外,玻璃轉移溫度是使用精工電子(Seiko Instruments)公司製造的DSC「RDC220」,在鋁盤中秤取約10mg的試樣,並設置於DSC裝置中藉由液氮冷卻至-100℃後,以10℃/min升溫而獲得DSC圖表,並根據該DSC圖表求出。
另外,酸值、羥值藉由以下方式而求出。
<酸值(Acid Value,AV)的測定>在共塞錐形瓶中精密地秤取試樣(聚酯多元醇溶液)約1g,添加甲苯/乙醇(容量比:甲苯/乙醇=2/1)混合液100mL而溶解。於其中添加酚酞試劑作為指示劑,並保持30秒鐘。然後,藉由0.1N醇性氫氧化鉀溶液進行滴定直至溶液呈現淡紅色為止。酸值藉由下式而求出(單位:mgKOH/g)。
酸值(mgKOH/g)=(5.611×p×F)/S
其中,S:試樣的採集量(g)
p:0.1N醇性氫氧化鉀溶液的消耗量(mL)
F:0.1N醇性氫氧化鉀溶液的力價
<羥值(Hydroxyl Value,OHV)的測定>在共塞錐形瓶中精密地秤取試樣(多元醇溶液)約1g,添加甲苯/乙醇(容量比:甲苯/乙醇=2/1)混合液100mL而溶解。繼而準確地添加5mL
的乙醯化劑(在吡啶中溶解乙酸酐25g,製成體積為100mL的溶液),並攪拌約1小時。於其中添加酚酞試劑作為指示劑,並持續30秒鐘。然後,藉由0.1N醇性氫氧化鉀溶液進行滴定直至溶液呈現淡紅色為止。
羥值藉由下式而求出(單位:mgKOH/g)。
羥值(mgKOH/g)=[{(q-p)×F×28.05}/S]+D
其中,S:試樣的採集量(g)
p:0.1N醇性氫氧化鉀溶液的消耗量(mL)
q:空實驗的0.1N醇性氫氧化鉀溶液的消耗量(mL)
F:0.1N醇性氫氧化鉀溶液的力價
D:酸值(mgKOH/g)
[主劑的製造]實施例1~實施例7、實施例9、實施例12、實施例13與比較例1~比較例5中,僅使用丙烯酸系多元醇溶液(A-1)~丙烯酸系多元醇溶液(A-7)、丙烯酸系多元醇溶液(A-10)~丙烯酸系多元醇溶液(A-12),實施例8中添加矽烷偶合劑(KBM-403)與磷酸,實施例10與實施例11中,添加矽烷偶合劑獲得主劑。
(硬化劑(B)的製造)
硬化劑B1:將藉由乙酸乙酯稀釋4,4'-二苯基甲烷二異氰酸酯的三羥甲基丙烷改質體(三羥甲基丙烷(Trimethylolpropane,TMP)
加合物改質體)而製成固體成分為70%的樹脂溶液者設為硬化劑B1。硬化劑B1的NCO%為10.0%。
硬化劑B2:將藉由乙酸乙酯稀釋甲苯二異氰酸酯的三羥甲基丙烷改質體(TMP加合物改質體)而製成固體成分為52.5%的樹脂溶液者設為硬化劑B2。硬化劑B2的NCO%為9.0%。
硬化劑B3:將藉由乙酸乙酯稀釋六亞甲基二異氰酸酯的三羥甲基丙烷改質體(TMP加合物改質體)而製成固體成分為75%的樹脂溶液者設為硬化劑B3。硬化劑B3的NCO%為12.5%。
(實施例1~實施例13、比較例1~比較例5)以表2所示的比例(g)調配主劑與硬化劑後,以非揮發成分為30%的方式添加乙酸乙酯,而獲得聚氨酯接著劑。
相對於主劑中所含的羥值與酸值的合計的硬化劑中的異氰酸酯基的當量[NCO]/[OH]藉由以下方式而求出。
[NCO]/[OH]=[561×(硬化劑的NCO%)×(相對於主劑100g的硬化劑調配量(g))]/[(主劑的羥值的合計(mgKOH/g))×42×100]
(比較例6)主劑使用AD-502(東洋摩頓(Toyo-Morton)公司製造的聚酯多元醇),硬化劑使用CAT-10(東洋摩頓公司製造的異氰酸酯硬化劑),以表2所示的比例(g)調配主劑與硬化劑後,以非揮發成分為30%的方式添加乙酸乙酯,
而獲得聚氨酯接著劑。
(比較例7)投入間苯二甲酸83.2g、對苯二甲酸83.2
g、乙二醇142.6g,在200℃~220℃下進行8小時酯化反應,將特定量的水餾出後,添加壬二酸188g,繼而進行4小時酯化反應。
將特定量的水餾出後,添加鈦酸四異丁酯0.13g,並緩慢地減壓,在1.3hPa~2.7hPa、230℃~250℃下進行3小時酯交換反應,而獲得數量平均分子量為22,000、Tg-5℃的聚酯多元醇。
藉由乙酸乙酯將該聚酯多元醇調整成非揮發成分為50%,而獲得羥值為2.45mgKOH/g、酸值為0.1mgKOH/g的聚酯多元醇溶液(X)。
以表2所示的比例(g)調配該聚酯多元醇溶液(X)與硬化劑(B)後,以非揮發成分為30%的方式,添加乙酸乙酯而獲得聚氨酯接著劑。
在厚度為40μm的鋁箔的一個面上,以塗佈量為5g/m2
的量藉由乾式貼合機,塗佈上述聚氨酯接著劑作為外層用接著劑,使溶劑揮發後,積層厚度為30μm的延伸聚醯胺膜。
繼而,在所得的積層膜的鋁箔的另一個面上,以塗佈量為5g/m2的量藉由乾式貼合機塗佈下述內層用接著劑,使溶劑揮發後,積層厚度為30μm的未延伸聚丙烯膜,然後,在60℃下進行7天的硬化(老化),使外層用接著劑及內層用接著劑硬化而獲得電池用包裝材。
(內層用接著劑)
在容器中加入:順丁烯二酸改質聚丙烯(在丙烯與乙烯的共聚物中接枝聚合順丁烯二酸酐而成的改質聚丙烯樹脂、熔解溫度:67℃、酸值:13mgKOH/g):60質量份、作為黏著賦予劑的完全氫化C9樹脂(軟化點:140℃、無酸值):40質量份,藉由甲苯/甲基乙基酮=8/2的混合溶劑進行稀釋,並在50℃下加熱攪拌3小時而獲得主劑,將上述主劑與藉由甲苯稀釋六亞甲基二異氰酸酯的三聚物製成固體成分為50%溶液而得的硬化劑,以質量比計為主劑/硬化劑=100/10進行調配,以非揮發成分為30%的方式,添加甲苯而製成內層用接著劑。
根據下述評價法,對以上述方式而得的電池用包裝材進
行性能評價。
<耐濕熱性試驗前、後的積層強度>將電池用包裝材切割成200mm×15mm的大小,在溫度為20℃、相對濕度為65%的環境下,使用拉伸試驗機以負荷速度為300mm/分鐘進行T型剝離試驗。以各5個試驗片的平均值表示延伸聚醯胺膜與鋁箔間的剝離強度(N/15mm寬度)(耐濕熱性試驗前的積層強度)。
另外,將電池用包裝材放入85℃、85%RH環境的恆溫恆濕槽中,靜置168小時後,將電池用包裝材自恆溫恆濕槽取出,以與試驗前相同的方式,測定積層強度(耐濕熱性試驗後的積層強度)。根據各剝離強度的平均值,進行以下4階段的評價。
aa:6N/15mm以上(實用上優異)
a:4N/15mm以上、小於6N/15mm(實用區域)
b:2N/15mm以上、小於4N/15mm(實用下限)
c:小於2N/15mm
將以上結果一併表示於表3。
<成型性評價法>將電池用包裝材切割成80mm×80mm的大小,並作為空白樣品(被成型材、原材料)。對上述空白樣品,以延伸聚醯胺膜成為外側的方式,藉由無成型高度限制的直模具進行突出而進行1階段成型,並根據鋁箔未產生斷裂、且各層間未產生***的最大的成型高度評價成型性。
另外,所使用的模具的打孔機形狀是一條邊為30mm的正方形、圓角R 2mm、打孔機肩R 1mm。所使用的模具的模具孔形狀是一片為34mm的正方形、模具孔圓角R 2mm、模具孔肩R:1mm,打孔機與模具孔的間隙(clearance)是單側為0.3mm。由於上述間隙而產生與成型高度對應的傾斜。根據成型的高度,進行以下的4階段的評價。
aa:6mm以上(實用上優異)
a:4mm以上、小於6mm(實用區域)
b:2mm以上、小於4mm(實用下限)
c:小於2mm
將以上的結果表示於表3。
<成型物的耐濕熱性>將電池用包裝材切割成60mm×60mm的大小,並作為空白樣品(被成型材、原材料)。對上述空白樣品,以延伸聚醯胺膜成為外側的方式,藉由無成型高度
限制的直模具以成型高度為3mm進行突出而進行1階段成型。將所得的30mm方形托盤放入至85℃、85%RH環境下的恆溫恆濕槽中,並靜置168小時。自恆溫恆濕槽取出上述托盤,確認凸緣部與側壁部的邊界部附近的外觀,並評價是否在延伸聚醯胺膜與鋁箔之間產生***。
另外,所使用的模具的打孔機形狀是一條邊為30mm的正方形、圓角R 2mm、打孔機肩R 1mm、模具肩R:1mm。
a:無***
c:產生***
將以上的結果一併表示於表3。
根據表3的結果可知,藉由使用包含數量平均分子量為
10,000~100,000、且羥值為1mgKOH/g~100mgKOH/g的丙烯酸系多元醇(A),且在相對於源自丙烯酸系多元醇(A)的羥基、源自硬化劑中所含的芳香族聚異氰酸酯(B)的異氰酸酯基的當量比[NCO]/[OH]為10~30的範圍內調配而成的電池用包裝材用聚氨酯接著劑,而可提供耐濕熱性試驗前、後的積層強度、成型性優異,在長期耐久性試驗中層間的接著強度亦高,且外觀性優異
的電池用包裝材。另外亦可知,可由使用電池用包裝材用聚氨酯接著劑的電池用包裝材形成耐濕熱性優異的成型物。
比較例1中,在耐濕熱性試驗前的積層強度的方面,並
不遜於實施例,但由於硬化劑的聚異氰酸酯為脂肪族聚異氰酸酯,因此雖然耐濕熱試驗後的積層強度為實用水準內,但有降低的傾向,並且成型性與成型物的耐濕熱性差。
比較例2中,相對於源自主劑中的多元醇(A)的羥基,芳香族聚異氰酸酯硬化劑中所含的異氰酸酯基的當量比過小,因此雖然耐濕熱試驗後的積層強度為實用水準內,但有降低的傾向,並且成型性與成型物的耐濕熱性差。
另外,比較例3中,由於丙烯酸系多元醇的數量平均分子量過小,因此耐濕熱試驗前後的積層強度差。比較例4中,由於丙烯酸系多元醇的數量平均分子量過大,因此源自主劑的羥基與源自硬化劑的異氰酸酯基的反應受到阻礙,雖然成型性為實用水準內,但有降低的傾向,並且成型物的耐濕熱性差。
另外,比較例5中,源自主劑中的多元醇(A)的羥基過多,而丙烯酸系多元醇(A)與芳香族聚異氰酸酯的交聯密度變得過高,因此導致積層強度降低。另外,雖然成型性或成型物的耐濕熱性為實用水準內,但有降低的傾向。
另外,比較例6中,由於主劑為聚酯多元醇,因此會促進藉由耐濕熱試驗的水解,而成形物的耐濕熱性差。比較例7中亦由於主劑為聚酯多元醇,根據相同的理由,成形物的耐濕熱性差,
而且成形性亦差。另外,比較例6、比較例7中,有耐濕熱試驗後的積層強度降低的傾向。
[產業上之可利用性]
本發明的聚氨酯接著劑可作為用於形成電池用容器或電池用封裝的接著劑而廣範圍地應用。特別是,本發明的聚氨酯接著劑適合作為用於形成鋰離子電池、鋰離子聚合物電池、鉛蓄電池、鹼電池、氧化銀-鋅蓄電池、金屬空氣電池、多價陽離子電池、電容器(condenser)、電容器(capacitor)等二次電池用電池用容器或電池用封裝的接著劑。本發明的聚氨酯接著劑是用於將相同或不同的原材料的被黏接體接合者,例如可較佳地用於塑膠系原材料與金屬系原材料的多層積層體的接合。當然,亦適合於塑膠系原材料彼此、金屬系原材料彼此的接合。使用本發明的接著劑而得的積層物的成型性優異,環境耐性高,在室外暴露的條件亦可抑制經時的接著強度的降低,可長期維持強的接著強度及外觀形狀。因此,亦可用作:泡殼包裝(Press Through Package,PTP)或鋼板等需要成型性的積層物、或防壁材、屋頂材、太陽電池面板材、窗材、室外地板材、照明保護材、汽車構件等建築物等室外產業用途積層物用的接著劑。
該申請案主張基於2013年2月25日提出申請的日本專利申請案特願2013-34957及2013年12月11日提出申請的日本專利申請案特願2013-255982的優先權,並將其揭示的全部內容併入本文中。
(11)‧‧‧外層側樹脂膜層
(12)‧‧‧外層側接著劑層
(13)‧‧‧金屬箔層
(14)‧‧‧內層側接著劑層
(15)‧‧‧內面層
Claims (7)
- 一種電池用包裝材用聚氨酯接著劑,其含有主劑與硬化劑,且其特徵在於:上述主劑包含數量平均分子量為10,000~100,000、且羥值為1mgKOH/g~100mgKOH/g的丙烯酸系多元醇(A),相對於源自上述丙烯酸系多元醇(A)的羥基,源自上述硬化劑中所含的芳香族聚異氰酸酯(B)的異氰酸酯基的當量比[NCO]/[OH]為10~30。
- 如申請專利範圍第1項所述之電池用包裝材用聚氨酯接著劑,其中上述丙烯酸系多元醇(A)的玻璃轉移溫度(Tg)為-20℃~30℃。
- 如申請專利範圍第1項或第2項所述之電池用包裝材用聚氨酯接著劑,其中進一步含有選自由矽烷偶合劑(C)、及磷酸或磷酸系化合物(D)所組成的組群的至少一種添加劑。
- 一種電池用包裝材,其自外層起依序需要外層側樹脂膜層、外層側接著劑層、金屬箔層、內層側接著劑層、內面層,其特徵在於:上述外層側接著劑層藉由如申請專利範圍第1項或第2項所述之電池用包裝材用聚氨酯接著劑而形成。
- 如申請專利範圍第4項所述之電池用包裝材,其中上述外層側樹脂膜層為聚醯胺膜或/及聚酯膜,上述內面層為聚烯烴系膜。
- 一種電池用容器,其由自外層起依序需要外層側樹脂膜層、外層側接著劑層、金屬箔層、內層側接著劑層、內面層的如 申請專利範圍第4項或第5項所述之電池用包裝材成型而成,且上述外層側樹脂膜層構成凸面,上述內面層構成凹面。
- 一種電池,其使用如申請專利範圍第6項所述之電池用容器而成。
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JPWO2016068201A1 (ja) * | 2014-10-31 | 2017-08-10 | 凸版印刷株式会社 | 蓄電デバイス用外装材 |
JP6491864B2 (ja) * | 2014-12-05 | 2019-03-27 | ヘンケルジャパン株式会社 | 積層シート用接着剤 |
JP2016169318A (ja) * | 2015-03-13 | 2016-09-23 | 東洋インキScホールディングス株式会社 | 積層体用接着剤組成物 |
JP6862084B2 (ja) * | 2015-10-07 | 2021-04-21 | 昭和電工パッケージング株式会社 | 包装材、ケースおよび蓄電デバイス |
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KR101615514B1 (ko) | 2016-04-26 |
CN105122495A (zh) | 2015-12-02 |
JP5578269B1 (ja) | 2014-08-27 |
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KR20150119879A (ko) | 2015-10-26 |
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