TWI813648B - 聚烯烴系黏接劑組成物 - Google Patents
聚烯烴系黏接劑組成物 Download PDFInfo
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- TWI813648B TWI813648B TW108109484A TW108109484A TWI813648B TW I813648 B TWI813648 B TW I813648B TW 108109484 A TW108109484 A TW 108109484A TW 108109484 A TW108109484 A TW 108109484A TW I813648 B TWI813648 B TW I813648B
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- adhesive composition
- modified polyolefin
- modified
- propylene
- item
- Prior art date
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Abstract
本發明之課題係提供可於低溫進行貼合及熟化,且黏接性、耐電解液性、耐熱性、耐久性、成形性優異的黏接劑組成物。一種黏接劑組成物,含有改性聚烯烴(A1)、熔點比起改性聚烯烴(A1)更高的改性聚烯烴(A2)、及熱塑性樹脂(B)。
Description
本發明關於黏接劑組成物、疊層體、及鋰離子電池用包裝材料。
近年,作為使用於個人電腦、行動電話等行動終端裝置、視訊攝影機、衛星等的電池,正積極開發可超薄型化、小型化的鋰離子電池(LiB)。該LiB之包裝材料與以往使用的金屬製罐不同,由於係輕量且可自由地選擇電池之形狀的優點,已開始使用如基材層/阻隔層/密封劑層之構成的疊層體。
LiB含有正極材及負極材,同時還含有將鋰鹽溶解於碳酸伸丙酯、碳酸伸乙酯、碳酸二甲酯、碳酸二乙酯、碳酸乙基甲酯等非質子性溶劑而得的電解液或由含浸有該電解液之聚合物凝膠構成的電解質層作為電池內容物。如此之強滲透性溶劑若通過密封劑層的話,會使阻隔層與密封劑層間的層合強度降低並發生分層(delamination),最終會產生諸如電解液漏出的問題。又,就電池之電解質即鋰鹽而言,係使用LiPF6、LiBF4等物質,但該等鹽會因與水分之水解反應而產生氫氟酸,氫氟酸會腐蝕阻隔層,從而使得層合強度降低。如此般,電池用包裝材料需具有對於電解質之耐受性。
又,設想LiB會使用在各種環境下,需具備更加嚴苛的耐受性。例如使用於行動設備(mobile equipment)時,要求諸如車內等在60~70℃之高溫環境下的耐漏液性。又,使用於行動電話時,設想不小心掉入水中的情形,亦需水分不會滲入的耐水性。
基於如此之狀況,有人提出了各種改善耐電解液性的鋰離子電池用包裝材料(例如,參照專利文獻1~2)。
[先前技術文獻]
[專利文獻]
[專利文獻1]國際公開2014/123183號小冊
[專利文獻2]國際公開2017/187904號小冊
[發明所欲解決之課題]
但是,前述提出之黏接劑組成物,在成形性方面尚未令人滿意。具體而言,將包裝材料加工成囊袋狀時,有時會有黏接層無法追隨基材間之延伸而發生剝離的情況。又,於高溫環境下硬化後的黏接劑之黏接性會變差,或因拉伸力而發生斷裂,在耐熱性及耐久性方面亦尚未令人滿意。
本發明提供一種黏接劑組成物,展現出和聚烯烴樹脂基材及金屬基材之良好黏接性以及耐電解液性,對於基材具有顯著的追隨性,且可於低溫進行貼合。而且,硬化後滿足展現優異耐熱性及耐久性所需的儲存彈性模量及斷裂伸度。進一步,本發明提供包含由該黏接劑組成物構成之黏接劑層的電池用包裝材料及使用了前述包裝材料的電池。
[解決課題之手段]
為了達成上述課題,本案發明人等進行努力研究,發現摻合熔點不同的2種改性聚烯烴、及熱塑性樹脂係有效,並提出了以下之發明。
一種黏接劑組成物,包含改性聚烯烴(A1)、含有30莫耳%以上之丙烯且熔點比起改性聚烯烴(A1)更高的改性聚烯烴(A2)、及熱塑性樹脂(B)。
前述改性聚烯烴(A1)之丙烯與1-丁烯的莫耳比宜為丙烯/1-丁烯=98~40/2~60,前述改性聚烯烴(A2)之丙烯與1-丁烯的莫耳比宜為丙烯/1-丁烯=99~55/1~45。
又,前述改性聚烯烴(A1)與前述改性聚烯烴(A2)之熔點的差宜為3~55℃,熔點為50~160℃較佳,前述改性聚烯烴(A1)及前述改性聚烯烴(A2)之酸價宜分別為2~50mgKOH/g。
前述熱塑性樹脂(B)可為酸改性熱塑性樹脂,宜具有2~50mgKOH/g之酸價。又,前述熱塑性樹脂(B)宜為苯乙烯系熱塑性樹脂,前述熱塑性樹脂(B)之質量比,相對於前述改性聚烯烴(A1)及前述改性聚烯烴(A2)之合計量100質量份宜為5~30質量份。
宜更包含硬化劑(C),前述硬化劑(C)為環氧硬化劑或異氰酸酯硬化劑較佳。
前述任一項記載之黏接劑組成物可使用於聚烯烴樹脂基材與金屬基材之黏接。
一種聚烯烴樹脂基材與金屬基材之疊層體,係利用前述任一項記載之黏接劑組成物黏接而成;以及一種鋰離子電池用包裝材料,係以前述疊層體作為構成構件。
[發明之效果]
本發明之黏接劑組成物含有熔點不同的2種改性聚烯烴及熱塑性樹脂,且具有與基材之顯著追隨性,故成形性(深抽拉性)等加工特性優異。又,即使於如聚烯烴基材之熱收縮影響小之80℃以下之低溫進行貼合,並於如40℃以下之低溫進行熟化,仍可展現出和聚烯烴樹脂基材及金屬基材之良好黏接性以及耐電解液性,且硬化後可展現優異的耐熱性、及耐久性。
以下,針對本發明之實施形態進行詳細地說明。
>改性聚烯烴(A1)及(A2)>
本發明中使用之改性聚烯烴(A1)及(A2)並無限定,宜為對聚乙烯、聚丙烯及丙烯-α-烯烴共聚物中之至少1種施以改性而得者。又,改性聚烯烴(A1)及(A2)為對聚丙烯或丙烯-α-烯烴共聚物施以改性而得者更佳。
丙烯-α-烯烴共聚物係以丙烯作為主體且與α-烯烴共聚而得者。就α-烯烴而言,例如可使用乙烯、丙烯、1-丁烯、1-庚烯、1-辛烯、4-甲基-1-戊烯、乙酸乙烯酯等中之1種或多種。丙烯-α-烯烴共聚物中之丙烯成分與α-烯烴成分的莫耳比宜為99~40/1~60,為98~45/2~55更佳,為94~60/6~40尤佳。又,丙烯-α-烯烴共聚物中之丙烯成分與1-丁烯成分之合計量宜為72莫耳%以上,更佳為80莫耳%以上,尤佳為90莫耳%以上,最佳為100莫耳%。又,丙烯-α-烯烴共聚物之乙烯含量宜為少量。
改性聚烯烴(A1)中之丙烯含量宜為28莫耳%以上,為40莫耳%以上更佳,為50莫耳%以上尤佳,為65莫耳%以上特佳。又,宜為100莫耳%以下,為98莫耳%以下更佳,為90莫耳%以下特佳。藉由含有30莫耳%以上之丙烯,有助於與丙烯基材之密接性變得良好。又,在丙烯以外亦可含有α-烯烴成分。
改性聚烯烴(A1)之丙烯與1-丁烯的莫耳比宜為丙烯/1-丁烯=98~40/2~60。丙烯的莫耳比為50%以上更佳,尤佳為60%以上,又更佳為70%以上。藉由丙烯的莫耳比為40%以上,可展現出與聚烯烴基材,特別是與聚丙烯基材之優異密接性。又,丙烯的莫耳比為95%以下更佳。尤佳為93%以下,最佳為90%以下。進一步,1-丁烯的莫耳比為2%以上的話,改性聚烯烴變柔軟,與基材之追隨性等加工特性得到改善。1-丁烯的莫耳比為5%以上更佳,尤佳為7%以上,最佳為10%以上。1-丁烯的莫耳比為50%以下更佳。尤佳為40%以下,最佳為30%以下。
改性聚烯烴(A2)中之丙烯含量宜為30莫耳%以上,為40莫耳%以上更佳,為45莫耳%以上尤佳,為60莫耳%以上特佳,為70莫耳%以上最佳。又,宜為100莫耳%以下,為99莫耳%以下更佳,為97莫耳%以下特佳。藉由含有30莫耳%以上之丙烯,會有展現出與丙烯基材之良好密接性的傾向。又,在丙烯以外亦可含有α-烯烴成分。
改性聚烯烴(A2)之丙烯與1-丁烯的莫耳比宜為丙烯/1-丁烯=99~45/1~55。丙烯的莫耳比為55%以上更佳,尤佳為65%以上,更佳為76%以上。藉由丙烯的莫耳比為45%以上,可展現出與聚烯烴基材,特別是與聚丙烯基材之優異密接性。又,丙烯的莫耳比為97%以下更佳。尤佳為94%以下,最佳為92%以下。進一步,1-丁烯的莫耳比為1%以上的話,改性聚烯烴變柔軟,與基材之追隨性等加工特性得到改善。1-丁烯的莫耳比為3%以上更佳,尤佳為6%以上,最佳為8%以上。1-丁烯的莫耳比為45%以下更佳。尤佳為35%以下,最佳為24%以下。
本發明中使用之改性聚烯烴(A1)及(A2)的改性,具體而言可列舉酸改性、氯改性、丙烯酸改性、羥基改性等。(A1)及(A2)之兩者需分別施以改性。又,改性聚烯烴(A1)及(A2)為經酸改性特佳。
就改性聚烯烴(A1)、(A2)而言,宜利用α,β-不飽和羧酸及其酸酐對聚烯烴進行酸改性。α,β-不飽和羧酸及其酸酐,例如可列舉馬來酸、伊康酸、檸康酸及它們的酸酐。該等中,宜為酸酐,為馬來酸酐更佳。該等α,β-不飽和羧酸及其酸酐可使用1種或將2種以上組合使用。
改性聚烯烴(A1)及(A2)之酸價,考量和聚烯烴樹脂基材及金屬基材之黏接性以及耐電解液性的觀點,宜分別為2~50mgKOH/g之範圍。更佳為3~45mgKOH/g,尤佳為5~40mgKOH/g,特佳為7~35mgKOH/g之範圍。未達2mgKOH/g的話,有時會欠缺與硬化劑之相容性。因此,有時會有交聯密度低,黏接強度、耐藥品性(耐電解液性)降低的情況。超過前述值的話,分子量低,凝聚力會變弱,因而有時會有黏接強度、耐藥品性(耐電解液性)降低的情況。進一步,製造效率亦會降低故不佳。又,改性聚烯烴(A1)與(A2)之酸價可相同也可不同,但宜相同。
可藉由α,β-不飽和羧酸、α,β-不飽和羧酸之酸酐及自由基產生劑的使用量調整改性聚烯烴(A1)及(A2)之酸價。
改性聚烯烴(A1)及(A2)需彼此熔點不同。藉由倂用高熔點之改性聚烯烴與低熔點之改性聚烯烴,即使於如聚烯烴基材之熱收縮影響小之80℃以下之低溫進行貼合,並於如40℃以下之低溫進行熟化,仍可展現出和聚烯烴樹脂基材及金屬基材之良好黏接性以及耐藥品性,且硬化後具有優異的耐熱性。
改性聚烯烴(A1)與(A2)之熔點不同,且相較於(A1),(A2)之熔點更高。(A1)與(A2)之熔點的差宜為3~55℃,更佳為4~45℃,尤佳為5~30℃。落在前述範圍外時,會有無法兼顧低溫加工性、耐電解液性、及於高溫條件之耐久性之虞。
改性聚烯烴(A1)之熔點(Tm)宜為50℃~155℃之範圍,更佳為55℃~120℃之範圍。尤佳為60℃~100℃之範圍,最佳為70℃~90℃之範圍。未達前述值的話,有時會有源自結晶之凝聚力變弱,黏接性、耐藥品性差的情況。另一方面,超過前述值的話,有時會有溶液穩定性、流動性低,黏接時操作性產生問題的情況。
改性聚烯烴(A2)之熔點(Tm)宜為55℃~160℃之範圍,更佳為60℃~125℃之範圍。尤佳為65℃~105℃之範圍,最佳為75℃~95℃之範圍。未達前述值的話,有時會有源自結晶之凝聚力變弱,黏接性、耐藥品性差的情況。另一方面,超過前述值的話,有時會有溶液穩定性、流動性低,黏接時操作性產生問題的情況。
改性聚烯烴(A1)及(A2)之質量比為(A1)/(A2)=99~21/1~79,宜為75~25/25~75之範圍。更佳為60~40/40~60之範圍。在前述範圍內的話,可兼顧低溫加工性、耐電解液性、及於高溫條件之耐久性。
改性聚烯烴(A1)及(A2)之熔解熱(ΔH)宜為1J/g~60J/g之範圍。更佳為3J/g~50J/g之範圍,最佳為5J/g~40J/g之範圍。未達前述值的話,有時會有源自結晶之凝聚力變弱,黏接性、耐藥品性差的情況。另一方面,超過前述值的話,有時會有溶液穩定性、流動性低,黏接時操作性產生問題的情況。
改性聚烯烴(A1)及(A2)之製造方法並無特別限定,例如可列舉自由基接枝反應(亦即,對於成為主鏈之聚合物生成自由基物種,以該自由基物種作為聚合起始點而使不飽和羧酸及酸酐進行接枝聚合反應)等。
自由基產生劑並無特別限定,例如可列舉有機過氧化物、偶氮腈類等,宜使用有機過氧化物。有機過氧化物並無特別限定,可列舉過氧化苯二甲酸二-第三丁酯、第三丁基過氧化氫、過氧化二異丙苯、過氧化苯甲醯、過氧化苯甲酸第三丁酯、過氧化-2-乙基己酸第三丁酯、過氧化新戊酸第三丁酯、過氧化甲乙酮、二-第三丁基過氧化物、過氧化月桂醯等,偶氮腈類可列舉偶氮雙異丁腈、偶氮雙異丙腈等。
改性聚烯烴(A1)及(A2)之重量平均分子量(Mw)宜為10,000~200,000之範圍。更佳為20,000~180,000之範圍,尤佳為30,000~160,000之範圍,特佳為40,000~140,000之範圍,最佳為50,000~110,000之範圍。未達前述值的話,有時會有凝聚力變弱,黏接性差的情況。另一方面,超過前述值的話,有時會有流動性低,黏接時操作性產生問題的情況。在前述範圍內的話,與硬化劑之硬化反應得以發揮,故較佳。
>熱塑性樹脂(B)>
本發明中使用之熱塑性樹脂(B)並無特別限定,可使用具有苯乙烯骨架之熱塑性樹脂。作為苯乙烯系熱塑性樹脂,具體而言可列舉:苯乙烯-乙烯-丁烯-苯乙烯共聚樹脂、苯乙烯-乙烯-丙烯-苯乙烯共聚樹脂、苯乙烯-丁二烯共聚樹脂、苯乙烯-乙烯共聚樹脂、苯乙烯-丁烯共聚樹脂、苯乙烯-乙烯-苯乙烯共聚樹脂、苯乙烯-丁烯-苯乙烯共聚樹脂等苯乙烯系彈性體等。又,作為不具有苯乙烯骨架之熱塑性樹脂,可列舉乙烯-丙烯共聚樹脂、乙烯-丁烯共聚樹脂、乙烯-乙酸乙烯酯共聚樹脂、乙烯-丙烯酸乙酯共聚樹脂等烯烴系彈性體等。其中,苯乙烯-乙烯-丁烯-苯乙烯共聚樹脂、苯乙烯-乙烯-丙烯-苯乙烯等苯乙烯系彈性體,就與改性聚烯烴(A1)及(A2)之相容性、耐熱性的觀點為較佳。
熱塑性樹脂(B)也可具有酸價。宜以2~50mgKOH/g之範圍,更佳為3~45mgKOH/g之範圍,尤佳為5~40mgKOH/g之範圍,特佳為7~35mgKOH/g之範圍具有酸價。又,熱塑性樹脂(B)為經酸改性時,宜為經馬來酸酐改性。藉由具有前述範圍之酸價,和改性聚烯烴(A1)及(A2)、以及硬化劑(C)之相容性變得良好,且藉由與硬化劑(C)之交聯使得凝聚力、黏接力及耐熱性得到改善。
熱塑性樹脂(B)的摻合量,相對於改性聚烯烴(A1)及(A2)之合計量100質量份宜為3~60質量份。更佳為5~40質量份之範圍,為8~30質量份之範圍尤佳,為10~20質量份之範圍特佳。藉由為前述範圍內,作為黏接劑組成物具有適度的柔軟性,且可兼具深抽拉性等加工特性及與聚烯烴基材之黏接性。
>黏接劑組成物>
本發明之黏接劑組成物係含有改性聚烯烴(A1)及(A2)、以及熱塑性樹脂(B)的組成物。本發明之黏接劑組成物可更含有硬化劑(C)。
黏接劑組成物之非揮發性成分中之(A1)、(A2)及(B)之合計量宜為60質量%以上,為70質量%以上更佳,最佳為80質量%以上。
>硬化劑(C)>
本發明中使用之硬化劑(C)並無特別限定,例如可列舉環氧硬化劑、異氰酸酯硬化劑、碳二亞胺系硬化劑、㗁唑啉系硬化劑等,宜為環氧硬化劑或異氰酸酯硬化劑。
本發明中使用之環氧硬化劑並無特別限定,可理想地使用環氧樹脂及由環氧樹脂衍生而來的化合物。就具體例而言,可列舉:環氧丙胺型環氧樹脂、環氧丙醚型環氧樹脂、六氫苯二甲酸環氧丙酯、二聚酸環氧丙酯等環氧丙酯類型、或3’,4’-環氧環己基甲基-3,4-環氧環己烷羧酸酯、環氧化聚丁二烯、環氧化大豆油等脂環族或脂肪族環氧化物等,可單獨使用1種或倂用2種以上。
本發明中使用之環氧丙胺型環氧樹脂之具體例並無特別限定,可列舉四環氧丙基二胺基二苯基甲烷、三環氧丙基對胺苯酚、四環氧丙基雙胺基甲基環己酮、N,N,N’,N’-四環氧丙基-間二甲苯二胺等環氧丙胺系等。其中,宜為N,N,N’,N’-四環氧丙基-間二甲苯二胺。該等環氧丙胺型環氧樹脂可單獨使用或倂用2種以上。
環氧丙醚型環氧樹脂之具體例並無特別限定,可列舉苯酚酚醛清漆型環氧樹脂、甲酚酚醛清漆型環氧樹脂,該等就與金屬基材之黏接性及耐藥品性之觀點係較佳。該等環氧丙醚型環氧樹脂可單獨使用或倂用2種以上。
本發明中使用之環氧硬化劑,考量與金屬基材之黏接性及耐藥品性的觀點,宜倂用環氧丙胺型環氧樹脂與環氧丙醚型環氧樹脂。較佳質量比為環氧丙胺型環氧樹脂/環氧丙醚型環氧樹脂=1~30/99~70,更佳為5~20/95~80,尤佳為8~15/92~85。
本發明中使用之異氰酸酯硬化劑並無特別限定,可理想地使用二異氰酸酯、三異氰酸酯及由該等衍生而來的化合物。
例如可列舉:2,4-二異氰酸甲苯酯、2,6-二異氰酸甲苯酯、二異氰酸二甲苯酯、二苯基甲烷二異氰酸酯、異佛酮二異氰酸酯、1,5-二異氰酸萘酯、二異氰酸六亞甲酯、雙(4-異氰酸酯環己基)甲烷、或氫化二苯基甲烷二異氰酸酯等二異氰酸酯。進一步,可列舉由前述二異氰酸酯衍生而來的化合物,亦即,前述二異氰酸酯之異氰尿酸酯體、加成物、雙脲型、脲二酮體、脲基甲酸酯(allophanate)體、具有異氰酸酯殘基之預聚物(由二異氰酸酯與多元醇獲得之低聚物)、異氰尿酸三環氧丙酯、或它們的複合體等。該等可單獨使用,亦可將2種以上任意組合使用。
本發明中使用之異氰酸酯硬化劑,其中,考量耐電解液性優異的理由,宜具有前述二異氰酸酯化合物之異氰尿酸酯體。
本發明中使用之硬化劑(C),除可列舉環氧硬化劑、異氰酸酯硬化劑外,亦可列舉碳二亞胺化合物、㗁唑啉化合物、偶聯劑類等。作為碳二亞胺化合物,可列舉:二甲基碳二亞胺、二異丙基碳二亞胺、二環己基碳二亞胺、第三丁基異丙基碳二亞胺、二苯基碳二亞胺、二-β-萘基碳二亞胺等單碳二亞胺化合物類;或可藉由使脂肪族二異氰酸酯、芳香族二異氰酸酯、或脂環族二異氰酸酯等有機二異氰酸酯,在縮合觸媒的存在下、無溶劑或鈍性溶劑中進行脫碳酸縮合反應而製造的聚碳二亞胺化合物類等。又,作為㗁唑啉化合物,可列舉:2-㗁唑啉、2-甲基-2-㗁唑啉、2-苯基-2-㗁唑啉、2,5-二甲基-2-㗁唑啉、或2,4-二苯基-2-㗁唑啉等單㗁唑啉化合物;2,2’-(1,3-伸苯基)-雙(2-㗁唑啉)、2,2’-(1,2-伸乙基)-雙(2-㗁唑啉)、2,2’-(1,4-伸丁基)-雙(2-㗁唑啉)、或2,2’-(1,4-伸苯基)-雙(2-㗁唑啉)等二㗁唑啉化合物等。又,作為偶聯劑,可列舉矽烷偶聯劑、鈦酸酯偶聯劑等。
本發明之黏接劑組成物含有硬化劑(C)時,硬化劑(C)的摻合量相對於改性聚烯烴(A1)及(A2)之合計量(A1)+(A2)100質量份,宜為0.5~40質量份之範圍,更佳為1~35質量份,尤佳為2~30質量份,特佳為3~25質量份之範圍。未達前述值的話,有時會有無法獲得充分的硬化效果,黏接性及耐藥品性低的情況。超過前述範圍的話,有時會有適用期(pot life)性能、黏接性降低的情況,又,有時會因追隨性降低而導致成形時產生針孔。進一步,就成本面的觀點為不佳。
本發明之黏接劑組成物,在不損及本發明之性能的範圍內,除摻合前述改性聚烯烴(A1)及(A2)、熱塑性樹脂(B)以及硬化劑(C)以外,可摻合並使用各種黏著賦予劑、塑化劑、硬化促進劑、阻燃劑、顏料、抗黏連劑等添加劑。
本發明之黏接劑組成物,在不損及本發明之性能的範圍內,可更含有有機溶劑。就有機溶劑而言,只要是會使改性聚烯烴(A1)及(A2)、熱塑性樹脂(B)及硬化劑(C)溶解或分散者,則並無特別限定,可例示脂肪族烴及脂環族烴等低極性溶劑、醇系溶劑、醚系溶劑、酮系溶劑、酯系溶劑等高極性溶劑等。考量保存穩定性、適用期的觀點,宜倂用低極性溶劑與高極性溶劑。高極性溶劑與低極性溶劑之含量比宜為50~3/50~97(質量比),為45~5/55~95更佳,為40~10/60~90尤佳。
脂肪族烴可列舉己烷、庚烷、辛烷、癸烷等。脂環族烴可列舉環己烷、環己烯、甲基環己烷、乙基環己烷等。醇系溶劑可列舉甲醇、乙醇、異丙醇、丁醇、戊醇、己醇、丙烷二醇等。醚系溶劑可列舉乙二醇單-正丁醚、乙二醇單-異丁醚、乙二醇單-第三丁醚、二乙二醇單-正丁醚、二乙二醇單-異丁醚、三乙二醇單-正丁醚、四乙二醇單-正丁醚等。酮系溶劑可列舉丙酮、甲基異丁基酮、甲乙酮、戊酮、己酮、環己酮、異佛酮、苯乙酮等。酯系溶劑可列舉乙酸甲酯、乙酸乙酯、乙酸丁酯、丙酸甲酯、甲酸丁酯等。
前述有機溶劑中,就低極性溶劑而言,宜為係脂環族烴之環己烷等,就高極性溶劑而言,宜為係酮系溶劑之甲乙酮等,其中,為環己烷與甲乙酮之混合溶劑更佳。該等有機溶劑之含量,相對於(A1)、(A2)、及(B)之合計量100質量份宜為80~2000質量份。更佳為90~1600質量份,尤佳為100~1200質量份,特佳為110~800質量份之範圍。在前述範圍內時,溶液狀態及適用期性能容易變得良好。
>疊層體>
本發明之疊層體係將聚烯烴樹脂基材與金屬基材利用本發明之黏接劑組成物進行疊層而成者。
疊層的方法可利用以往公知的層合製造技術。例如可於金屬基材之表面利用輥塗機、塗布棒等適當的塗布工具塗布黏接劑組成物並使其乾燥。乾燥後,在形成於金屬基材表面的黏接劑組成物之層(黏接劑層)處於熔融狀態的期間,於其塗布面疊層黏接(層合黏接)聚烯烴樹脂基材而獲得疊層體,並無特別限定。
利用前述黏接劑組成物形成之黏接劑層的厚度並無特別限定,宜為0.5~10μm,為0.8~9.5μm更佳,為1~9μm尤佳。
>聚烯烴樹脂基材>
就聚烯烴樹脂基材而言,從以往公知的聚烯烴樹脂中適當選擇即可。例如可使用聚乙烯、聚丙烯、乙烯-丙烯共聚物等,並無特別限定。其中,宜使用聚丙烯之無延伸薄膜(以下,亦稱為CPP。)。其厚度並無特別限定,宜為20~100μm,為25~95μm更佳,為30~90μm尤佳。此外,亦可視需要在聚烯烴樹脂基材中摻合顏料、各種添加物,也可施以表面處理。
>金屬基材>
金屬基材並無特別限定,例如可使用鋁、銅、鋼鐵、鉻、鋅、硬鋁(duralumin)、壓鑄件(die cast)等各種金屬及其合金。又,其形狀可採金屬箔、壓延鋼板、平板、管、罐、蓋等任意形狀。一般而言,考量加工性等的觀點,宜為鋁箔。又,取決於使用目的而有所不同,但一般係以0.01~10mm,較佳為0.02~5mm之厚度的片材形式使用。
又,該等金屬基材的表面可預先施以表面處理,也可為未處理。無論何種情形均可發揮同等的效果。
[實施例]
以下,舉實施例對本發明進行更加詳細地說明。惟,本發明並不限定於實施例。
>改性聚烯烴(A)之製造例>
製造例1
於1L高壓釜中加入丙烯-1-丁烯共聚物(Tm:80℃、丙烯/1-丁烯=80/20莫耳比)100質量份、甲苯233質量份及馬來酸酐20質量份、二-第三丁基過氧化物5質量份,升溫至140℃後,進一步攪拌1小時(此處,稱為「反應」1小時)。之後,將獲得之反應液冷卻至100℃後,邊攪拌邊注入到裝有預先加溫至40℃的甲苯717質量份與甲乙酮950質量份的容器中,冷卻至40℃,更攪拌30分鐘,進一步冷卻至25℃,藉此使樹脂析出(此處,藉由將反應液邊攪拌邊注入到甲乙酮等溶劑中,並進行冷卻以使樹脂析出的操作稱為「再沉澱」)。之後,藉由將含有該樹脂之漿液進行離心分離,而將接枝聚合有馬來酸酐之酸改性丙烯-1-丁烯共聚物與(聚)馬來酸酐及低分子量物予以分離。
進一步,將已離心分離並取出的酸改性丙烯-1-丁烯共聚物邊攪拌邊投入到另外裝有預先保溫於25℃的2000質量份之甲乙酮的容器中,繼續攪拌1小時。之後,藉由將漿液進行離心分離,進一步將酸改性丙烯-1-丁烯共聚物與(聚)馬來酸酐及低分子量物予以分離。重複該操作2次,藉此進行精製(此處,將已離心分離並取出的酸改性丙烯-1-丁烯共聚物邊攪拌邊投入到甲乙酮中,並再次離心分離,藉此以強化精製的操作稱為「再漿洗(reslurry)」)。
精製後,藉由於減壓下、70℃使其乾燥5小時,得到係改性聚烯烴的馬來酸酐改性丙烯-1-丁烯共聚物(PO-1、酸價25mgKOH/g、重量平均分子量60,000、Tm80℃)。
製造例2
將製造例1中使用之丙烯-1-丁烯共聚物(Tm:80℃)變更為丙烯-1-丁烯共聚物(Tm:90℃、丙烯/1-丁烯=85/15莫耳比),再漿洗次數變更為1次,再漿洗時投入之甲乙酮的量變更為1000質量份,除此以外,與製造例1同樣進行,藉此獲得係改性聚烯烴的馬來酸酐改性丙烯-1-丁烯共聚物(PO-2、酸價25mgKOH/g、重量平均分子量60,000、Tm90℃)。
製造例3
將馬來酸酐的加入量變更為3質量份,二-第三丁基過氧化物的加入量變更為1質量份,再漿洗次數變更為1次,再漿洗時投入之甲乙酮的量變更為1000質量份,除此以外,與製造例1同樣進行,藉此獲得係改性聚烯烴的馬來酸酐改性丙烯-1-丁烯共聚物(PO-3、酸價5mgKOH/g、重量平均分子量90,000、Tm80℃)。
製造例4
將製造例1中使用之丙烯-1-丁烯共聚物變更為乙烯-丙烯共聚物(Tm:100℃、乙烯/丙烯=75/25莫耳比),除此以外,與製造例1同樣進行,藉此獲得係改性聚烯烴的馬來酸酐改性乙烯-丙烯共聚物(PO-4、酸價25mgKOH/g、重量平均分子量60,000、Tm100℃)。
[表1]
表1中使用之熱塑性樹脂(B)如下。
B-1:Kraton公司製Kraton(註冊商標)FG1924(馬來酸酐改性苯乙烯-乙烯-丁烯-苯乙烯樹脂、酸價11mgKOH/g)
B-2:旭化成公司製Tuftec(註冊商標)M1911(馬來酸酐改性苯乙烯-乙烯-丁烯-苯乙烯樹脂、酸價2mgKOH/g)
B-3:Kraton公司製Kraton(註冊商標)FG1901(馬來酸酐改性苯乙烯-乙烯-丁烯-苯乙烯樹脂、酸價19mgKOH/g)
B-4:Tafmer(註冊商標)MH7020(馬來酸酐改性乙烯‐1-丁烯共聚物、酸價11mgKOH/g)
B-5:旭化成公司製Tuftec(註冊商標)H1517(苯乙烯-乙烯-丁烯-苯乙烯樹脂、酸價0mgKOH/g)
B-6:Kraton公司製Kraton(註冊商標)G1730(苯乙烯-乙烯-丙烯-苯乙烯樹脂、酸價0mgKOH/g)
B-7:三井化學公司製Tafmer(註冊商標)DF640(乙烯-丁二烯樹脂、酸價0mgKOH/g)
實施例1
於配備有水冷回流冷凝器與攪拌機的500ml四口燒瓶中,加入製造例1獲得之馬來酸酐改性丙烯-1-丁烯共聚物(PO-1)90質量份、馬來酸酐改性丙烯-1-丁烯共聚物(PO-2)10質量份、熱塑性樹脂Kraton FG1924(B-1)15質量份、環己烷424質量份及甲乙酮228質量份,邊攪拌邊升溫至80℃,繼續攪拌1小時後,摻合硬化劑(C-1)3.8質量份、(C-2)0.5質量份,得到黏接劑組成物。使用該黏接劑組成物,依下列方法製作疊層體。評價結果示於表1。
實施例2~15、比較例1~6
如表1及表2所示般變更酸改性丙烯-1-丁烯共聚物或酸改性乙烯-丙烯共聚物、熱塑性樹脂,並利用與實施例1同樣的方法製作實施例2~15、比較例1~6。摻合量及評價結果示於表1及表2。
[表2]
金屬基材與聚烯烴樹脂基材之疊層體的製作
金屬基材使用鋁箔(住輕鋁箔公司製,8079-0,厚度40μm),聚烯烴樹脂基材使用無延伸聚丙烯薄膜(東洋紡公司製Pylen(註冊商標)薄膜CT,厚度40μm)(以下,亦稱為CPP。)。
利用塗布棒將獲得之黏接劑組成物塗布於金屬基材,進行調整使乾燥後之黏接劑層之膜厚成為3μm。使用溫風乾燥機於100℃環境將塗布面乾燥1分鐘,獲得疊層有膜厚3μm之黏接劑層的金屬基材。在前述黏接劑層表面重疊聚烯烴樹脂基材,使用TESTER SANGYO公司製之小型桌上測試層合機(Test Laminator,SA-1010-S),於層合溫度80℃,以0.3MPa、1m/分鐘的條件貼合,在40℃、50%RH熟化5天以獲得疊層體。
針對獲得之疊層體,進行黏接性、耐電解液性、成形性、斷裂伸度及儲存彈性模量的評價。結果示於表1及表2。
表1及表2中使用之硬化劑如下。
(C-1)環氧丙醚型環氧樹脂:jER(註冊商標)152(三菱化學公司製)
(C-2)環氧丙胺型環氧樹脂:TETRAD(註冊商標)-X(三菱瓦斯化學公司製)
(C-3)多官能多異氰酸酯:SUMIDUR(註冊商標)N3300(Covestro公司製)
針對以上述方式獲得之各改性聚烯烴及黏接劑組成物,依下列方法進行分析測定及評價。
酸價的測定
本發明中之酸價(mgKOH/g),係指中和1g的試樣所需之KOH量,依據JIS K0070(1992)之試驗方法測定。具體而言,將改性聚烯烴或熱塑性樹脂1g溶解於溫度調整成100℃之二甲苯100g,然後,於同溫度以酚酞作為指示劑,利用0.1mol/L氫氧化鉀乙醇溶液[商品名「0.1mol/L乙醇性氫氧化鉀溶液」,和光純藥(股)製]進行滴定。此時,將滴定所需之氫氧化鉀量換算成mg而算出酸價(mgKOH/g)。
重量平均分子量(Mw)的測定
本發明中之重量平均分子量,係利用日本Waters公司製凝膠滲透層析儀Alliance e2695(以下稱為GPC,標準物質:聚苯乙烯樹脂,移動相:四氫呋喃,管柱:Shodex KF-806+KF-803,管柱溫度:40℃,流速:1.0ml/分鐘,檢測器:光二極體陣列檢測器(波長254nm=紫外線))測得的値。
熔點的測定
本發明中之熔點係由使用差示掃描熱量計(以下稱為DSC,TA Instrument Japan製,Q-2000),以10℃/分鐘之速度升溫至200℃後,以相同速度冷卻至-50℃,再次以相同速度升溫時之熔解峰部之頂部溫度測得的値。
適用期性能的評價
適用期性能係指在改性聚烯烴中摻合硬化劑,於剛摻合時或摻合後經一定時間後之該溶液的穩定性。適用期性能良好時,係指溶液之黏度上升少,可長期間保存;適用期性能不良時,係指溶液之黏度上升(增黏),嚴重時會發生凝膠化現象,難以塗布於基材,無法長期間保存。
黏接劑組成物之適用期性能,係藉由在25℃環境保存24小時後,使用B型黏度計於25℃測定溶液黏度以進行評價。
評價結果示於表1及表2。
>評價基準>
☆(實用上極為優異):未達300mPa・s
◎(實用上特別優異):300mPa・s以上且未達500mPa・s
○(實用上優異):500mPa・s以上且未達800mPa・s
△(可實用):800mPa・s以上且未達1000mPa・s
×(不可實用):1000mPa・s以上或因凝膠化而無法測定黏度
>初始黏接性的評價>
將疊層體裁切成100mm×15mm大小,利用T型剝離試驗依以下之基準評價黏接性。
T型剝離試驗係依據ASTM-D1876-61之試驗法,使用Oritentic Coporation製的TENSILON RTM-100,於25℃環境下測定於拉伸速度50mm/分鐘之剝離強度。金屬基材/聚烯烴樹脂基材間的剝離強度(N/cm)係取5次試驗值之平均值。
評價基準如下。
☆(實用上極為優異):8.0N/cm以上
◎(實用上特別優異):7.5N/cm以上且未達8.0N/cm
○(實用上優異):7.0N/cm以上且未達7.5N/cm
△(可實用):6.5N/cm以上且未達7.0N/cm
×(不可實用):未達6.5N/cm
>85℃耐電解液性的評價>
為了探討作為鋰離子電池之包裝材的利用性,實施耐電解液性的評價。將疊層體裁切成100mm×15mm大小,於電解液[在碳酸伸乙酯/碳酸二乙酯/碳酸二甲酯=1/1/1(容積比)100g中添加有六氟化磷酸鋰13g而得者]中在85℃浸漬1天。之後,取出疊層體並以離子交換水洗滌,用擦拭紙(paper wiper)擦掉水,使水分充分乾燥,利用T型剝離試驗依下列基準進行耐電解液性評價。
☆(實用上極為優異):8.0N/cm以上
◎(實用上特別優異):7.5N/cm以上且未達8.0N/cm
○(實用上優異):7.0N/cm以上且未達7.5N/cm
△(可實用):6.5N/cm以上且未達7.0N/cm
×(不可實用):未達6.5N/cm
>成形性的評價>
成形性係利用所製作之疊層體的極限成形深度(深抽拉性)進行評價。極限成形深度依以下之方法實施。
將疊層體裁切成80×120mm大小,並進行冷成形。具體而言,使用AMADA(股)公司製的拉伸成形機(品號:TP-25C-X2)、具有55mm×35mm之口徑的形成模具(母模)及與之對應的成形模具(公模),以推壓壓力0.4MPa從0.5mm之成形深度以0.5mm單位改變成形深度,針對10個樣品(疊層體)分別進行冷成形。針對冷成形後之樣品,將10個樣品中均未產生皺紋、鋁箔均未產生針孔、裂紋的最深的成形深度作為該樣品的極限成形深度。由該極限成形深度依下列基準進行電池用包裝材料之成形性評價。評價結果示於表1及表2。
>評價基準>
☆(實用上極為優異):極限成形深度6.0mm以上
◎(實用上特別優異):極限成形深度4.0mm以上且未達6.0mm
○(實用上優異):極限成形深度3.0mm以上且未達4.0mm
△(可實用):極限成形深度2.0mm以上且未達3.0mm
×(不可實用):極限成形深度未達2.0mm
耐熱性及耐久性係利用拉伸斷裂伸度與儲存彈性模量進行評價。
斷裂伸度的測定
本發明中之25℃之拉伸斷裂伸度(Eb)係依據JIS K7161(2014)之試驗法測定。具體而言,係使用Oritentic Coporation製的TENSILON RTM-100,於25℃環境下以速度50mm/分鐘進行拉伸,並測定斷裂時的伸度(%)而得的值。
又,85℃之斷裂伸度係在85℃環境下以同樣方式測得的值。將獲得之黏接劑組成物利用500μm塗抹機塗布於Teflon(註冊商標)片,進行調整使乾燥後之黏接劑層之膜厚成為50μm。使用溫風乾燥機於100℃環境將塗布面乾燥1分鐘。從Teflon片剝離黏接劑層,得到膜厚50μm之試驗片。將試驗片裁切成50mm×15mm,以與前述T型剝離試驗同樣之方法實施,利用試驗片斷裂時之伸長率進行評價。
☆(實用上極為優異):300%以上
◎(實用上特別優異):250%以上且未達300%
○(實用上優異):220%以上且未達250%
△(可實用):200%以上且未達220%
×(不可實用):未達200%
儲存彈性模量的測定
本發明中之儲存彈性模量(E’)係依據JIS K7244-4(1999)之試驗法測定。具體而言,使用IT Keisoku Seigyo公司製動態黏彈性測定裝置DVA-200,於頻率10Hz從-50℃以5℃/分鐘之速度升溫並進行測定而得的值。儲存彈性模量係於80℃環境下、及110℃環境下分別測定。試驗片以與前述斷裂伸度的測定中使用之試驗片同樣的方式製作。
☆(實用上極為優異):1.0×106
Pa以上
◎(實用上特別優異):1.0×105
Pa以上且未達1.0×106
Pa
○(實用上優異):5.0×104
Pa以上且未達1.0×105
Pa
△(可實用):1.0×104
Pa以上且未達5.0×104
Pa
×(不可實用):未達1.0×104
Pa
[產業上利用性]
本發明之黏接劑組成物含有熔點彼此不同的改性聚烯烴、熱塑性樹脂及硬化劑,且展現與基材之顯著追隨性,故深抽拉性等加工特性優異。又,即使於低溫之貼合條件下,仍可展現出和聚烯烴樹脂基材及金屬基材之良好黏接性以及耐藥品性,且硬化後具有優異的耐熱性及耐久性。因此,由本發明之黏接劑組成物形成的聚烯烴樹脂基材與金屬基材之疊層體,不僅可用在家電外板、家具用素材、建築內裝用構件等領域,亦可廣泛用作使用於個人電腦、行動電話、視訊攝影機等的鋰離子電池之包裝材(囊袋形態)。
Claims (13)
- 一種黏接劑組成物,包含改性聚烯烴(A1)、含有30莫耳%以上之丙烯且熔點比起改性聚烯烴(A1)更高的改性聚烯烴(A2)、及熱塑性樹脂(B),該改性聚烯烴(A1)及該改性聚烯烴(A2)為利用α,β-不飽和羧酸及其酸酐中之至少1種進行酸改性而成之酸改性聚烯烴,該改性聚烯烴(A1)之熔點為60~90℃,該熱塑性樹脂(B)為酸改性苯乙烯系熱塑性樹脂或酸改性烯烴系彈性體。
- 如申請專利範圍第1項之黏接劑組成物,其中,該改性聚烯烴(A1)之丙烯與1-丁烯的莫耳比為丙烯/1-丁烯=98~40/2~60,該改性聚烯烴(A2)之丙烯與1-丁烯的莫耳比為丙烯/1-丁烯=99~55/1~45。
- 如申請專利範圍第1或2項之黏接劑組成物,其中,該改性聚烯烴(A1)與該改性聚烯烴(A2)之熔點的差為3~55℃。
- 如申請專利範圍第1或2項之黏接劑組成物,其中,該改性聚烯烴(A1)及該改性聚烯烴(A2)之酸價分別為2~50mgKOH/g。
- 如申請專利範圍第1或2項之黏接劑組成物,其中,該改性聚烯烴(A2)之熔點為65~160℃。
- 如申請專利範圍第1或2項之黏接劑組成物,其中,該熱塑性樹脂(B)具有2~50mgKOH/g之酸價。
- 如申請專利範圍第1或2項之黏接劑組成物,其中,該熱塑性樹脂(B)為苯乙烯系熱塑性樹脂。
- 如申請專利範圍第1或2項之黏接劑組成物,更包含硬化劑(C)。
- 如申請專利範圍第8項之黏接劑組成物,其中,該硬化劑(C)為環氧硬化劑或異氰酸酯硬化劑。
- 如申請專利範圍第1或2項之黏接劑組成物,其中,該熱塑性樹脂(B)之質量比,相對於該改性聚烯烴(A1)及該改性聚烯烴(A2)之合計量100質量份為5~30質量份。
- 如申請專利範圍第1或2項之黏接劑組成物,係使用於聚烯烴樹脂基材與金屬基材之黏接。
- 一種包含聚烯烴樹脂基材與金屬基材之疊層體,係利用如申請專利範圍第1或2項之黏接劑組成物黏接而成。
- 一種鋰離子電池用包裝材料,係以如申請專利範圍第12項之包含聚烯烴樹脂基材與金屬基材之疊層體作為構成構件。
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KR (1) | KR102410728B1 (zh) |
CN (1) | CN111971360B (zh) |
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CN111440593B (zh) * | 2020-04-07 | 2021-01-15 | 郑州卓而泰新材料科技有限公司 | 一种锂电池铝塑膜内层胶黏剂及其制备方法 |
KR102522216B1 (ko) | 2020-09-04 | 2023-04-18 | 율촌화학 주식회사 | 프라이머층 조성물, 이를 이용한 이차전지 파우치 필름 및 그 제조 방법 |
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CN104203567B (zh) | 2012-02-01 | 2016-11-23 | 昭和电工包装株式会社 | 成型用包装材及其制造方法 |
JP2014024945A (ja) * | 2012-07-26 | 2014-02-06 | Dic Corp | インクジェット記録用水性インクセット |
EP2955212B1 (en) | 2013-02-07 | 2020-02-05 | Mitsui Chemicals, Inc. | Adhesive, layered body, cell case packaging, cell, high-alkali solution packaging and alcohol-containing solution packaging |
KR102051425B1 (ko) | 2013-04-11 | 2019-12-03 | 에스케이플래닛 주식회사 | 광고 플랫폼들의 통합 관리를 위한 장치 및 방법 |
KR20160047468A (ko) | 2014-09-17 | 2016-05-02 | 디아이씨 가부시끼가이샤 | 라미네이트용 접착제, 그것을 사용한 적층체 및 이차 전지 |
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TW201412918A (zh) * | 2012-08-28 | 2014-04-01 | Henkel Japan Ltd | 熱熔黏著劑 |
CN105980505A (zh) * | 2014-01-22 | 2016-09-28 | 株式会社钟化 | 热熔粘接剂用聚烯烃类树脂组合物、热熔粘接膜及叠层体 |
TW201807133A (zh) * | 2016-04-27 | 2018-03-01 | 迪愛生股份有限公司 | 積層用接著劑組成物、積層體、及二次電池 |
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TW201942299A (zh) | 2019-11-01 |
KR20200135862A (ko) | 2020-12-03 |
CN111971360A (zh) | 2020-11-20 |
CN111971360B (zh) | 2022-07-08 |
EP3778819A4 (en) | 2021-12-15 |
WO2019188283A1 (ja) | 2019-10-03 |
JP7420067B2 (ja) | 2024-01-23 |
EP3778819A1 (en) | 2021-02-17 |
EP3778819B1 (en) | 2024-02-21 |
JPWO2019188283A1 (ja) | 2021-04-22 |
KR102410728B1 (ko) | 2022-06-22 |
ES2974056T3 (es) | 2024-06-25 |
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