TWI683873B - 接著劑、使用其之層合體、電池外裝材、電池盒及其製造方法 - Google Patents
接著劑、使用其之層合體、電池外裝材、電池盒及其製造方法 Download PDFInfo
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- TWI683873B TWI683873B TW106133096A TW106133096A TWI683873B TW I683873 B TWI683873 B TW I683873B TW 106133096 A TW106133096 A TW 106133096A TW 106133096 A TW106133096 A TW 106133096A TW I683873 B TWI683873 B TW I683873B
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- TW
- Taiwan
- Prior art keywords
- polyisocyanate
- adhesive
- polymer
- polyolefin resin
- resin film
- Prior art date
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- 239000000853 adhesive Substances 0.000 title claims abstract description 85
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 80
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- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000005056 polyisocyanate Substances 0.000 claims abstract description 86
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 86
- 229910052751 metal Inorganic materials 0.000 claims abstract description 73
- 239000002184 metal Substances 0.000 claims abstract description 73
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- 229920000642 polymer Polymers 0.000 claims abstract description 63
- 239000011347 resin Substances 0.000 claims abstract description 63
- 229920005672 polyolefin resin Polymers 0.000 claims abstract description 62
- 239000011888 foil Substances 0.000 claims abstract description 48
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 36
- 150000001875 compounds Chemical class 0.000 claims abstract description 34
- 125000002723 alicyclic group Chemical group 0.000 claims abstract description 19
- 125000003118 aryl group Chemical group 0.000 claims abstract description 19
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 18
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- -1 polymethylene Polymers 0.000 claims description 31
- 150000007942 carboxylates Chemical class 0.000 claims description 21
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 13
- 229910052782 aluminium Inorganic materials 0.000 claims description 12
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- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 claims description 12
- 239000000178 monomer Substances 0.000 claims description 12
- 239000012948 isocyanate Substances 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
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- 150000008064 anhydrides Chemical class 0.000 claims description 4
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- 239000000155 melt Substances 0.000 claims description 3
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- 239000012790 adhesive layer Substances 0.000 description 23
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 11
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 6
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- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
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- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 3
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- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 3
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- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 3
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- 239000005058 Isophorone diisocyanate Substances 0.000 description 2
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- B32B2457/10—Batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
本發明提供可作為金屬箔與樹脂薄膜之層合用接著劑,可安定地展現良好接著性,而且可獲得耐電解液及耐熱性更優異之層合體之接著劑。 該接著劑含有具有羧基的聚烯烴樹脂(A)、及聚異氰酸酯化合物(B),前述聚異氰酸酯化合物(B)包含飽和脂肪族聚異氰酸酯的多聚物(B1)、飽和脂環式聚異氰酸酯的多聚物(B2)、及芳香族聚異氰酸酯的多聚物(B3)。
Description
[0001] 本發明係有關可較好地使用於鋰離子電池等之二次電池的外裝材之金屬箔與樹脂薄膜之層合用接著劑、使用該接著劑之層合體、電池外裝材、以及電池盒及其製造方法。
[0002] 鋰離子電池為高能量密度、小型且輕量之二次電池,故已廣泛使用於筆記型電腦或智慧型手機、面板終端等之移動電子機器、電動車等之電源等。 鋰離子電池為了防止電解洩漏或水分朝電子內部之侵入,而於其電池盒使用對於電池材料之電解質或隔離件等之密封性高的外裝材。 [0003] 作為上述外裝材,一般係使用依序層合由耐熱性樹脂薄膜所成之外層、鋁箔等之具有水蒸氣障壁性之中間層、及具有耐電解液性之聚烯烴樹脂薄膜等所成之內層之層合體。此等層合體中,由於係設為密封性高的外裝材,故要求使用具有高接著強度之接著劑,使各層接著並一體化。 [0004] 關於上述此等接著劑,於專利文獻1及2中,記載有經由接著劑層接著之電池盒用包材,該接著劑含有以不飽和羧酸或其酸酐使聚丙烯等接枝改質之具有羧基之聚烯烴樹脂與異氰酸酯化合物而成。 [先前技術文獻] [專利文獻] [0005] [專利文獻1] 日本特開2010-92703號公報 [專利文獻2] 國際公開第2013/114934號
[發明欲解決之課題] [0006] 然而,上述專利文獻1及2中記載之接著劑層所用之改質聚烯烴樹脂,於接著劑之塗佈或養生之際,易受到起因於濕度或層合體各層之厚度等所致之接著劑含水量變動之影響。且,上述專利文獻1及2中記載之接著劑中,作為異氰酸酯化合物,具體而言,僅揭示使用六亞甲基二異氰酸酯或其聚合物之僅一種。該等接著劑難以獲得安定之接著性,層合體之耐電解液性及耐熱性無法說是必定充分。 [0007] 因此,對於電池外裝材所用之接著劑要求為可展現良好接著性,且可獲得耐電解液及耐熱性更優異之層合體者。 [0008] 本發明係為解決上述課題而完成者,目的在於提供可作為金屬箔與樹脂薄膜之層合用接著劑,可安定地展現良好接著性,而且可獲得耐電解液及耐熱性更優異之層合體之接著劑。 又,本發明之目的亦在於提供耐電解液及耐熱性更優異之層合體、電池外裝材及電池盒及其製造方法。 [用以解決課題之手段] [0009] 本發明係於藉由於含有聚烯烴樹脂及異氰酸酯之接著劑中,發現著眼於異氰酸酯化合物之種類,藉由使用特定複數種異氰酸酯化合物,於金屬箔與樹脂薄膜之層合時,可獲得良好接著性,可提高層合體之耐電解液性及耐熱性,因而完成者。 [0010] 亦即,本發明係提供以下之[1]~[16]者。 [1] 一種金屬箔與樹脂薄膜之層合用接著劑,其特徵係含有具有羧基的聚烯烴樹脂(A)、及聚異氰酸酯化合物(B),前述聚異氰酸酯化合物(B)包含飽和脂肪族聚異氰酸酯的多聚物(B1)、飽和脂環式聚異氰酸酯的多聚物(B2)、及芳香族聚異氰酸酯的多聚物(B3)。 [2] 如上述[1]記載之接著劑,其中,前述飽和脂肪族聚異氰酸酯的多聚物(B1)包含選自飽和脂肪族聚異氰酸酯的脲甲酸酯化多聚物、及飽和脂肪族聚異氰酸酯的異氰脲酸酯體中的1種以上。 [3] 如上述[1]或[2]記載之接著劑,其中,前述飽和脂環式聚異氰酸酯的多聚物(B2)包含選自飽和脂環式聚異氰酸酯的脲甲酸酯化多聚物、及飽和脂環式聚異氰酸酯的異氰脲酸酯體中的1種以上。 [4] 如上述[1]~[3]中任1項記載之接著劑,其中,前述芳香族聚異氰酸酯的多聚物(B3)包含選自芳香族聚異氰酸酯的脲甲酸酯化多聚物、芳香族聚異氰酸酯的異氰脲酸酯體、及聚亞甲基聚苯基聚異氰酸酯中的1種以上。 [5] 如上述[1]~[4]中任1項記載之接著劑,其中,前述飽和脂肪族聚異氰酸酯的多聚物(B1)、前述飽和脂環式聚異氰酸酯的多聚物(B2)、及前述芳香族聚異氰酸酯的多聚物(B3)的各異氰酸基的莫耳比為3~20:1~6:1。 [6] 如上述[1]~[5]中任1項記載之接著劑,其中,前述聚烯烴樹脂(A)包含選自丙烯、乙烯及丁烯中的1種以上之單體單位。 [7] 如上述[1]~[6]中任1項記載之接著劑,其中,前述聚烯烴樹脂(A)包含被選自乙烯性不飽和羧酸或其酸酐中的1種以上改性的聚烯烴樹脂。 [8] 如上述[1]~[7]中任1項記載之接著劑,其中,前述聚烯烴樹脂(A)依據JIS K 7210-1:2014,在溫度130℃、以荷重2.16kg測定的熔體流動速率為2~50g/10分鐘。 [9] 如上述[1]~[8]中任1項記載之接著劑,其中,相對於前述聚烯烴樹脂(A)的羧基1莫耳之前述聚異氰酸酯化合物(B)的異氰酸基的莫耳比率為0.3~30。 [10] 如上述[1]~[9]中任1項記載之接著劑,其中,再含有金屬羧酸鹽(C)。 [0011] [11] 一種層合體,其特徵係金屬箔與樹脂薄膜使用上述[1]~[10]中任1項記載之接著劑層合而成。 [12] 如上述[11]記載之層合體,其中,前述金屬箔為鋁箔且前述樹脂薄膜為熱融著性樹脂薄膜。 [13] 如上述[11]或[12]記載之層合體,其中,前述金屬箔的厚度為10~100μm,且前述樹脂薄膜的厚度為9~100μm。 [0012] [14] 一種電池外裝材,其特徵係使用上述[11]~[13]中任1項記載之層合體。 [15] 一種電池盒,其特徵係使用上述[14]記載之電池外裝材。 [16] 一種電池盒之製造方法,其特徵係具有將上述[14]記載之電池外裝材進行深拉伸加工或撐壓加工而成形之步驟。 [發明效果] [0013] 依據本發明之接著劑,於金屬箔與樹脂薄膜之層合中,可安定地展現良好接著性,而且可獲得耐電解液及耐熱性更優異之層合體。因此,使用該接著劑形成之層合體係各層之接著性良好,且耐電解液及耐熱性優異,而較好地適於電池外裝材。 因此,使用此等電池外裝材之電池盒亦有助於製造壽命長且安全之二次電池。
[0014] 以下針對本發明詳細說明。 又,本說明書中之「x~y」之數值範圍意指「x以上y以下」。又,所謂「(甲基)丙烯酸酯」意指丙烯酸酯及甲基丙基酸酯中之任一種以上。且,所謂「單體單位」意指藉由聚合獲得樹脂時之原料單體。 [0015] [接著劑] 本發明之接著劑係金屬箔與樹脂薄膜之層合用接著劑。而且特徵係含有具有羧基的聚烯烴樹脂(A)及聚異氰酸酯化合物(B),聚異氰酸酯化合物(B)包含飽和脂肪族聚異氰酸酯的多聚物(B1)、飽和脂環式聚異氰酸酯的多聚物(B2)、及芳香族聚異氰酸酯的多聚物(B3)。 藉由對於接著劑之主劑的具有羧基的聚烯烴樹脂,併用如上述之特定複數種作為硬化劑的聚異氰酸酯化合物,於金屬箔與樹脂薄膜之層合中,可提高接著性,且可獲得耐電解液及耐熱性優異之層合體。 [0016] (聚烯烴樹脂(A)) 本發明之接著劑的構成成分之聚烯烴樹脂(A)若為具有羧基之聚烯烴樹脂,則未特別限定。 [0017] 聚烯烴樹脂(A)中之聚烯烴骨架之單體單位舉例為乙烯、丙烯、丁烯、戊烯、己烯、庚烯、辛烯、4-甲基-1-戊烯等之單烯烴;環戊烯、環己烯等之脂環族烯烴;1,4-己二烯、1,5-己二烯、二乙烯基苯、1,3-環戊二烯、1,3-環己二烯、5-乙烯基-2-降冰片烯等之鏈狀或環狀聚烯等。該等可單獨使用1種亦可併用2種以上。該等中,基於對於被接著物的樹脂薄膜,尤其是聚烯烴樹脂薄膜之接著性之觀點,較好為乙烯、丙烯及丁烯。 [0018] 聚烯烴樹脂(A)所具有之羧基亦即鍵結於聚烯烴之取代基的羧基係源自羧酸者,亦可為源自羧酸酐者。 作為具有羧基之聚烯烴樹脂(A)舉例為改質之聚烯烴樹脂。作為此等改質聚烯烴樹脂舉例為例如使具有羧基之單體接枝聚合於聚烯烴之接枝聚合物、具有羧基之單體與烯烴之共聚物,又,舉例為具有前述接枝聚合物之部位與前述共聚物之部位者等。 [0019] 作為如上述之改質聚烯烴樹脂所用之具有羧基之單體舉例為例如(甲基)丙烯酸等之乙烯性不飽和羧酸;馬來酸酐、檸康酸酐、依康酸酐等之乙烯性不飽和羧酸酐;(甲基)丙烯酸β-羧基乙酯等之含羧基之乙烯性不飽和羧酸酯等。該等可單獨使用1種,亦可併用2種以上。該等中,較好為乙烯性不飽和羧酸或其酸酐,其中,更好為乙烯性不飽和羧酸酐,再更好為馬來酸酐。 [0020] 聚烯烴樹脂(A)係具有羧基之聚烯烴樹脂,作為構成其之單體單位,可包含不具有羧基之乙烯性不飽和羧酸酯。作為不具有羧基之乙烯性不飽和羧酸酯舉例為例如(甲基)丙烯酸與碳數1~20之不具有羧基之醇之酯化物,舉例為(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸己酯、(甲基)丙烯酸辛酯、(甲基)丙烯酸癸酯、(甲基)丙烯酸十二烷酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸硬脂酯等。該等可單獨使用1種,亦可併用2種以上。 [0021] 聚烯烴樹脂(A)依據JIS K 7210-1:2014,在溫度130℃、以荷重2.16kg測定的熔體流動速率(MFR:melt mass-flow rate)為2~50g/10分鐘。MFR更好為3~45g/10分鐘,又更好為8~40g/10分鐘。 MFR若為2g/10分鐘以上,則由該接著劑形成之接著劑層之接著性即使於與電解液接觸之情況亦難以降低故而較佳。且,MFR若為50g/10分鐘以下,則該接著劑之塗佈性良好。 [0022] 聚烯烴樹脂(A)之酸價係成為羧基含量之指標者,基於接著劑之接著性之觀點,較好為3~60mgKOH/g,更好為4~30mgKOH/g,又更好為5~15mgKOH/g。 酸價若為3mgKOH/g以上,則由該接著劑形成之接著劑層之接著性即使於與電解液接觸之情況亦難以降低故而較佳。且,若為60mgKOH/g以下,則該接著劑之塗佈性良好。 又,本說明書中之「酸價」意指依據JIS K 0070:1992測定之值。 [0023] (聚異氰酸酯化合物(B)) 本發明之接著劑之構成成分的聚異氰酸酯化合物(B)係作為對於聚烯烴樹脂(A)之硬化劑發揮作用者,且包含飽和脂肪族聚異氰酸酯的多聚物(B1)、飽和脂環式聚異氰酸酯的多聚物(B2)、及芳香族聚異氰酸酯的多聚物(B3)之3種類。 作為聚異氰酸酯化合物,藉由使用此等3種多聚物,於金屬箔與樹脂薄膜之層合時,可獲得耐電解液性及耐熱性優異之層合體。 [0024] 聚異氰酸酯化合物(B)除(B1)~(B3)以外,亦可含有例如(B1)~(B3)之多聚物之構成單位的單體等之其他異氰酸酯化合物。該情況下,聚異氰酸酯化合物(B)中之(B1)~(B3)之多聚物之合計含量,基於藉由該等多聚物而於金屬箔與樹脂薄膜之層合時可獲得耐電解液性優異之層合體之觀點,較好為80質量%以上,更好為90質量%以上,又更好為95質量%以上,再更好為98質量%以上。 [0025] 作為飽和脂肪族聚異氰酸酯的多聚物(B1),舉例為例如六亞甲基二異氰酸酯、2,4,4-三甲基六亞甲基二異氰酸酯、2,2,4-三甲基六亞甲基二異氰酸酯等之脂肪族二異氰酸酯之多聚物。該等可單獨使用1種,亦可併用2種以上。 作為多聚物之形態,舉例為例如脲甲酸酯化多聚物、異氰脲酸酯體、縮二脲改質物等。該等中,較好為脲甲酸酯化多聚物及異氰脲酸酯體,更好使用異氰脲酸酯體。 [0026] 作為飽和脂環式聚異氰酸酯的多聚物(B2),舉例為例如1,4-環己烷二異氰酸酯、異佛酮二異氰酸酯、亞甲基雙(4-環己基異氰酸酯)、1,3-雙(異氰酸酯基甲基)環己烷、1,4-雙(異氰酸酯基甲基)環己烷、降冰片烷二異氰酸酯等之飽和脂環式聚異氰酸酯之多聚物。該等可單獨使用1種,亦可併用2種以上。 作為多聚物之形態,舉例為例如脲甲酸酯化多聚物、異氰脲酸酯體、縮二脲改質物等。該等中,較好為脲甲酸酯化多聚物及異氰脲酸酯體,更好使用異氰脲酸酯體。 [0027] 作為芳香族聚異氰酸酯的多聚物(B3),舉例為例如2,4-甲苯二異氰酸酯、2,6-甲苯二異氰酸酯、二苯基甲烷-4,4’-二異氰酸酯(單聚MDI)、1,3-二甲苯二異氰酸酯、1,4-二甲苯二異氰酸酯等之芳香族之二異氰酸酯的多聚物或聚亞甲基聚苯基聚異氰酸酯(聚合MDI)。該等可單獨使用1種,亦可併用2種以上。又,本發明中,所謂「芳香族聚異氰酸酯」意指構造式中之任一者中具有芳香環之聚異氰酸酯。 作為多聚物之形態,舉例為例如脲甲酸酯化多聚物、異氰脲酸酯體、縮二脲改質物、聚合MDI等。該等中,較好為脲甲酸酯化多聚物、異氰脲酸酯體及聚合MDI,更好為聚合MDI。又,聚合MDI亦可較好地作為包含單聚MDI之聚合MDI混合物而使用。 [0028] 聚異氰酸酯化合物(B)中之飽和脂肪族聚異氰酸酯之多聚物(B1)、飽和脂環式聚異氰酸酯的多聚物(B2)及芳香族聚異氰酸酯的多聚物(B3)之摻合比,較好各多聚物之異氰酸酯基之莫耳比為3~20:1~6:1,更好為5~20:1.5~6:1,又更好為8~12:2~4:1。 藉由使(B1)~(B3)之各多聚物成為此摻合比,於由該接著劑形成之接著劑層中,可保持飽和脂肪族聚異氰酸酯之多聚物(B1)之優異接著性,同時藉由飽和脂環式聚異氰酸酯的多聚物(B2)及芳香族聚異氰酸酯的多聚物(B3),可均衡良好地提高耐電解液性及耐熱性。 [0029] 聚異氰酸酯化合物(B)之異氰酸酯基,相對於聚烯烴樹脂(A)之羧基1莫耳,莫耳比率(以下記載為「NCO/COOH比」)較好為0.3~30,更好為5~25,又更好為10~20。 NCO/COOH比若為0.3以上,由該接著劑形成之接著劑層之接著性尤其是對於樹脂薄膜之接著性成為良好,再者,若為10以上,則成為前述接著劑層之耐熱性亦更優異者。且,NCO/COOH比若為30以下,則該接著劑形成之接著劑層之接著性即使於與電解液接觸時亦難以降低故而較佳。 [0030] 又,聚烯烴樹脂(A)之羧基莫耳數可自上述酸價求出,又,聚異氰酸酯化合物(B)之異氰酸酯基莫耳數可依據JIS K 6806:2003之方法求得。 又,自聚烯烴樹脂(A)之構成單體算出NCO/COOH比時,於聚烯烴樹脂(A)具有源自羧酸酐之羧基時,該羧酸酐1莫耳視為相當於羧基2莫耳加以計算。 [0031] (金屬羧酸鹽(C)) 本發明之接著劑除了聚烯烴樹脂(A)及聚異氰酸酯化合物(B)以外,亦可含有金屬羧酸鹽(C)。 金屬羧酸鹽(C)係發揮促進聚烯烴樹脂(A)及聚異氰酸酯化合物(B)之反應的作用者,基於促進由該接著劑形成之接著劑層之接著性展現之觀點,更好於接著劑中摻合。 [0032] 作為金屬羧酸鹽(C)舉例為例如金屬乙酸鹽、金屬己酸鹽、金屬2-乙基己酸鹽等之金屬辛酸鹽、金屬新癸酸鹽、金屬月桂酸鹽、金屬硬脂酸鹽、金屬油酸鹽等之金屬羧酸鹽;金屬乙醯丙酮酸鹽等。作為金屬羧酸鹽(C)之金屬,較好為選自週期表第7族、第12族及第14族中之1種以上之金屬。該等可單獨使用1種,亦可併用2種以上。該等中,基於由該接著劑形成之接著劑層接觸於電解液時之接著性之觀點,更好為錫、鋅及錳中之任一者之羧酸鹽以及乙醯基丙酮酸鹽。 具體而言,舉例為新癸酸鋅、二月桂酸二丁基錫、二月桂酸二辛基錫、二乙酸二辛基錫、雙(新癸酸)鋅、雙(2-乙基己酸)鋅、二硬脂酸鋅、乙醯丙酮酸鋅(II)、雙(2-乙基己酸)錳等。該等中,基於由該接著劑形成之接著劑層之接著性、耐電解液性及耐熱性之均衡之觀點,更好為二月桂酸二丁基錫、二月桂酸二辛基錫。 [0033] 接著劑中之金屬羧酸鹽(C)之摻合量並未特別限定,但相對於聚烯烴樹脂(A)100質量份,以金屬成分換算較好為0.0001~5質量份,更好為0.0005~3質量份,又更好為0.001~1質量份。 若為0.0001質量份以上,則由該接著劑形成之接著劑層接觸於電解液時,亦可獲得優異接著性。且若為5質量份以下,則可獲得由該接著劑形成之接著劑層於常態下之優異接著性。 又,金屬羧酸鹽(C)可於聚烯烴樹脂(A)之添加,可於其製造時添加,或亦可於接著劑之調製時添加。 [0034] <溶劑(D)> 本發明之接著劑,基於黏性之調整及處理性等之觀點,亦可根據需要含有溶劑(D)。溶劑(D)若為可溶解或分散聚烯烴樹脂(A)、聚異氰酸酯化合物(B)及金屬羧酸鹽(C)者,則未特別限定。舉例為例如甲苯、二甲苯等之芳香族系有機溶劑;環己烷、甲基環己烷、乙基環己烷等之脂環式系有機溶劑;正己烷、正庚烷等之脂肪族系有機溶劑;乙酸乙酯、乙酸丙酯、乙酸丁酯等之酯系有機溶劑;丙酮、甲基乙基酮、甲基丁基酮等之酮系有機溶劑、其他礦油精等。該等可單獨使用1種,亦可併用2種以上。該等中,基於聚烯烴樹脂(A)之溶解性之觀點,較好為甲苯、乙酸乙酯、乙酸丙酯、乙酸丁酯、甲基環己烷及甲基乙基酮,更好為甲苯、乙酸乙酯及乙酸丁酯。又,礦油精有時含於金屬羧酸鹽(C)之市售品中。 [0035] 接著劑中之溶劑(D)之含量,於聚烯烴樹脂(A)、聚異氰酸酯化合物(B)、金屬羧酸鹽(C)及溶劑(D)之合計100質量%中,較好為30~95質量%,更好為40~90質量%,又更好為50~90質量%。 含量若為30質量%以上,則該接著劑之塗佈性變良好。又,若為95質量%以上,則使用該接著劑而層合之層合體之厚度控制性良好。 [0036] (添加劑) 本發明之接著劑除了聚烯烴樹脂(A)、聚異氰酸酯化合物(B)、金屬羧酸鹽(C)及溶劑(D)以外,根據需要,於不損及本發明效果之範圍內,可含有任意添加劑。作為添加劑舉例為例如反應促進劑、黏著賦予劑、可塑劑等。該等中,可單獨使用1種,亦可併用2種以上。 接著劑含添加劑時,聚烯烴樹脂(A)、聚異氰酸酯化合物(B)、金屬羧酸鹽(C)及溶劑(D)之合計含量,基於充分發揮接著劑中之該等(A)~(D)之各成分之作用之觀點,較好為80質量%以上,更好為90質量%以上,又更好為95質量%以上,再更好為98質量%以上。 [0037] 作為反應促進劑,作為與金屬羧酸鹽(C)具有同樣功能之化合物,舉例為例如2,4,6-三(二甲胺基甲基)苯酚、N,N-二甲基苯胺、N,N-二甲基-對-甲苯胺、對-甲苯二乙醇胺等之三級胺。該等可單獨使用1種,亦可併用2種以上。該反應促進劑亦可代替金屬羧酸鹽(C)使用,或亦可與金屬羧酸鹽(C)併用。 [0038] 黏著賦予劑並未特別限制。舉例為例如聚萜烯系樹脂、松脂系樹脂等之天然者;因石油腦熱分解所副生之餾分的脂肪族(C5)系樹脂、芳香族(C9)系樹脂、C5與C9之共聚合系樹脂、脂環族系樹脂等之石油系者等。又,亦舉例該等樹脂之雙鍵部分經氫化之氫化樹脂。該等可單獨使用1種,亦可併用2種以上。 [0039] 可塑劑亦未特別限定,可單獨使用該等中之1種,亦可併用2種以上。舉例為例如聚異戊二烯、聚丁烯等之液狀橡膠;加工油等,以及聚烯烴樹脂(A)以外之聚烯烴樹脂、其他熱塑性樹脂或熱塑性彈性體等。作為熱塑性樹脂及熱塑性彈性體,舉例為例如乙烯-乙酸乙醯酯共聚合樹脂、乙烯-丙烯酸乙酯共聚合樹脂、苯乙烯-乙烯-丁烯-苯乙烯(SEBS)共聚合樹脂、苯乙烯-乙烯-丙烯-苯乙烯(SEPS)共聚合樹脂等。 [0040] [層合體] 本發明之層合體係使用前述接著劑將金屬箔及樹脂薄膜層合而成者。亦即,以前述接著劑將金屬箔及樹脂薄膜接著,於前述金屬箔及前述樹脂薄膜之兩者之接著面上,接觸由前述接著劑形成之接著劑層。 又,金屬箔彼此或樹脂薄膜彼此等之接著,亦即金屬箔與樹脂薄膜之間以外之接著亦可使用前述接著劑以外之其他接著劑,但前述接著劑於該等之間之接著中亦可展現良好接著性。 [0041] 作為層合之方法可使用熱層合方式或乾層合方式等之習知方法。 所謂熱層合方式係使不含溶劑(D)之接著劑於被接著物之接著面上加熱熔融或與被接著物一起加熱擠出之方式,藉此,介隔於金屬箔及樹脂薄膜之間形成接著劑層者。 另一方面,所謂乾層合方式係將含溶劑(D)之接著劑塗佈於被接著物之接著面並乾燥後,與另一被接著物之接著面重疊並壓著之方式,藉此,介隔於金屬箔及樹脂薄膜之間形成接著劑層者。 [0042] 金屬箔一般係使用純鋁系或鋁-鐵系合金之O材(軟質材)等之鋁箔,可較好地使用此等鋁箔。 金屬箔之厚度,基於加工性及防止層合體中之氧及水分之透過之障壁性之觀點,較好為10~100μm,更好為30~50μm,更好為35~50μm,又更好為40~50μm。 厚度若為10μm以上,則可充分抑制成形時金屬箔之破裂或因針孔發生所致之氧及水分透過該層合體。又,若為100μm以下,則容易進行層合體之總厚或質量等之適度調整。 又,為了提高與樹脂薄膜之接著性或提高耐腐蝕性,較好對金屬箔施以矽烷偶合劑或鈦偶合劑等之底塗處理;鉻酸鹽處理等之化學處理。 [0043] 樹脂薄膜基於具有熱密封性、獲得優異耐電解液性之觀點,作為其材質較好為熱熔黏性樹脂,舉例為例如聚丙烯、聚乙烯、馬來酸改質聚丙烯、乙烯-丙烯酸酯共聚物、離子聚合物樹脂等。樹脂薄膜可為單層,且亦可藉由共擠出等以複數層構成。複數層時,各層材質可相同,亦可每各層不同。 樹脂薄膜厚度較好為9~100μm,更好為20~90μm,又更好為40~ 80μm。 厚度若為9μm以上,則藉由層合可獲得與金屬箔之充分接著性,薄膜本身之強度亦充分,可獲得優異之耐電解液性。且若為100μm以下,則可獲得良好成形性。 [0044] 層合體之用途並未特別限定,例如可較好地使用作為包裝材。作為被包裝物舉例為例如含有酸、鹼、有機溶劑等之液狀物。具體而言,舉例為附厚油灰、附薄油灰等之油灰;油性塗料等之塗料;透明清漆等之清漆;溶劑系之汽車用混合物;鋰離子電池等之二次電池之電解液等。 [0045] [電池外裝材] 前述層合體可較好地使用於電池外裝體。如上述,前述層合體由於對於鋰離子電池等之二次電池之電解液之耐電解液性優異,故電池外裝材為前述層合體之較佳用途。 電池外裝材較好為具有於金屬箔之外側面設有樹脂薄膜之構成的層合體。電池外裝材,基於更提高機械強度或耐電解液性等之觀點,除前述層合體之層構成以外,亦可根據需要,為具有中間樹脂層或外層進而具有塗佈層等之構成。舉例為例如下述(1)~(4)所示之層構成。又,下述例示中,所謂接著劑層係指由本發明之接著劑形成之層。 (1)外層/金屬箔/接著劑層/樹脂薄膜 (2)外層/中間樹脂層/金屬箔/接著劑層/樹脂薄膜 (3)塗佈層/外層/金屬箔/接著劑層/樹脂薄膜 (4)塗佈層/外層/中間樹脂層/金屬箔/接著劑層/樹脂薄膜 [0046] 外層通常由樹脂薄膜形成,基於耐熱性、成形性及絕緣性等之觀點,較好使用例如聚醯胺(尼龍)樹脂、聚酯樹脂等之延伸薄膜等。 外層厚度較好為9~50μm,更好為10~40μm,又更好為20~30μm。 厚度若為9μm以上,可充分確保電池外裝材之成形時之樹脂薄膜伸展性,抑制金屬箔之窄縮、成形性良好。又,若考慮成本,藉由50μm以下之厚度可獲得充分之耐熱性及絕緣性。 [0047] 外層中使用之樹脂薄膜為延伸薄膜時,基於獲得更良好成形性之觀點,較好對於延伸方向為0°、45°、90°之各3方向之任一方向,拉伸強度均為150N/mm2
以上,更好為200N/mm2
以上,又更好為250N/mm2
以上。且,直至斷裂之伸長率較好為80%以上,更好為100%以上,又更好為120%以上。 又,本說明書中所謂「拉伸強度」及「直至斷裂之伸長率」係將前述3方向之延伸方向作為長度方向,切出長150mm×寬15mm×厚9~50μm之試料薄膜,以拉伸速度100mm/分鐘進行拉伸試驗,於試料薄膜斷裂時之強度及伸長之值。 [0048] 作為上述層構成(2)及(4)中之中間樹脂層之材質,基於提高電池外裝材之機械強度之觀點,舉例為例如聚醯胺樹脂、聚酯樹脂、聚乙烯樹脂等。中間樹脂層可為單層樹脂薄膜,或亦可為複數層之共擠出樹脂薄膜等。中間樹脂層厚度並未特別限定,通常為0.1~30μm左右。 [0049] 作為上述層構成(3)及(4)中之塗佈層,通常係基於賦予對水蒸氣及其他氣體之氣體障壁性之觀點所設置者,可以習知材質形成。例如可塗佈具有氣體障壁性之聚合物,藉由蒸鍍或塗佈鋁等之金屬、或氧化矽、氧化鋁等之無機氧化物而形成。 [0050] [電池盒] 前述電池外裝材,由於耐電解液性或耐熱性、氣體障壁性等優異,故可尤其較好地使用作為鋰離子電池之電池盒。 又,前述電池外裝材由於成形性優異,故可藉由習知方法成形,簡便地製造電池盒。成形方法並未特別限定,但基於對應於複雜形狀或高的尺寸精度之觀點,較好藉由深拉伸加工或撐壓加工而成形。 [實施例] [0051] 以下,藉由實施例詳細說明本發明,但本發明不由該等所限定。 [0052] [聚烯烴樹脂(A)之合成] 分別由下述合成例1~8製造下述表1所示之聚烯烴樹脂(A1)~(A8)。 (合成例1) 將使用茂金屬觸媒作為聚合觸媒所製造之丙烯-乙烯無規共聚物(丙烯-乙烯莫耳比97:3,MFR10g/10分鐘) 100質量份、馬來酸酐0.5質量份、甲基丙烯酸月桂酯1質量份及第三丁基過氧化物1.5質量份,使用螺桿部之最高溫設定為170℃之雙軸擠出機進行混練並反應。隨後,使擠出機內減壓脫氣,去除未反應殘留物,獲得具有羧基之聚烯烴樹脂(A1)。 [0053] (合成例2~5) 於合成例1中,除了使用如下述表1所示之MFR值不同之丙烯-乙烯無規共聚物以外,與合成例1同樣,獲得聚烯烴樹脂(A2)~(A5)。 [0054] (合成例6~8) 於合成例1中,除了代替丙烯-乙烯無歸共聚物,而使用如下述表1所示之丙烯-丁烯無規共聚物(A6)、丙烯聚合物(A7)或丙烯-乙烯-丁烯無規共聚物(A8)以外,與合成例1同樣,獲得聚烯烴樹脂(A6)~(A8)。 [0055] 針對上述合成之各聚烯烴樹脂(A),如下述般,測定酸價及MFR。該等測定結果彙總示於表1。 <酸價> 依據JIS K 0070:1992,以氫氧化鉀乙醇溶液中和滴定求出酸價。 <MFR測定> 依據JIS K 7210-1:2014,在溫度130℃、以荷重2.16kg之條件測定。 [0056][0057] [接著劑之調製] 如以下般調製金屬箔與樹脂薄膜之層合用接著劑。各接著劑中摻合之化合物示於以下。 <聚烯烴樹脂(A)> 上述合成例1~8製造之聚烯烴樹脂(A1)~(A8)。 <聚異氰酸酯化合物(B)> (B1)六亞甲基二異氰酸酯之異氰脲酸體:「DURANATE(註冊商標) TKA-100」,旭化成股份有限公司製;異氰酸酯基含量21.7質量% (B2)異佛酮二異氰酸酯之異氰脲酸體:「DESMODUR (註冊商標)Z 4470 BA」,COVESTRO公司製;乙酸丁酯溶液(濃度70質量%);異氰酸酯基含量8.3質量% (B3)聚合MDI:「SUMIMODUR(註冊商標)44V40」,COVESTRO公司製;與單聚MDI之混合物(單聚MDI含量32.0質量%);異氰酸酯基含量30.0質量% [0058] <金屬羧酸鹽(C)> (C1)新癸酸鋅:「BiCAT(註冊商標) Z(M)」,SHEPHERD CHEMICAL公司製,金屬(鋅)含量19質量% (C2)二月桂酸二丁基錫:「KS-1260」,堺化學工業股份有限公司製 (C3)雙(2-乙基己酸)鋅;「己酸鋅15%」,東榮化工股份有限公司製;礦油精溶液(濃度65質量%);金屬(鋅含量15質量%) (C4)二硬脂酸鋅:「EFCO-CHEM ZNS-P」,ADEKA股份有限公司製 (C5)乙醯丙酮酸鋅(II):試藥,東京化成工業股份有限公司製 (C6)雙(2-乙基己酸)錳:「己酸錳6%」,東榮化工股份有限公司製,礦油精溶液(濃度42質量%);金屬(錳含量6質量%) <溶劑(D)> 甲苯-乙酸乙酯混合溶劑(混合質量比9:1) [0059] (實施例1) 將聚烯烴樹脂(A1)15.00g溶解於溶劑(D)85.0g中。其次,添加作為聚異氰酸酯化合物(B)之(B1)2.96g、(B2)2.29g及(B3)0.21g並攪拌混合,調製金屬箔與樹脂薄膜之層合用接著劑。 [0060] (實施例2~8) 實施例1中,除了代替聚烯烴樹脂(A1),分別使用(A2)~(A8)以外,與實施例1同樣,調製各接著劑。 [0061] (實施例9~13) 實施例6中,除了作為原料進而分別添加0.02質量份之金屬羧酸鹽(C1)~(C5)以外,與實施例6同樣,調製各接著劑。 [0062] (比較例1~6) 實施例6中,除了聚異氰酸酯化合物(B)之摻合組成分別變更為下述表3所示以外,與實施例6同樣,調製各接著劑。 [0063] 針對上述實施例及比較例調製之接著劑,如下述般,求出NCO/COOH比。 又,上述實施例及比較例中,以使NCO/COOH比均成為14.0之方式,調整聚烯烴樹脂(A)及聚異氰酸酯化合物(B)之摻合組成。 <NCO/COOH比> 藉由依據JIS K 6806:2003之方法,求出聚異氰酸酯化合物(B)中之NCO量,算出異氰酸酯基之莫耳數。 又,自上述求出之聚烯烴樹脂(A)之酸價,算出聚烯烴樹脂(A)中之羧基莫耳數。 接著將異氰酸酯基之莫耳數除以羧基莫耳數,求出NCO/COOH比。 [0064] [電池外裝材之製造] 使用上述實施例及比較例之接著劑,以乾層合方式,製造具有外層/中間樹脂層/鋁箔/接著劑層/樹脂薄膜之層構成之電池外裝材。又,層合後之養生及乾燥條件設為溫度40℃、濕度5%RH、5天。 電池外裝材之各層材料如以下。 <外層> 聚對苯二甲酸乙二酯/延伸聚醯胺層合薄膜;厚27μm;對於延伸方向0°、45°、90°之各3方向任一方向拉伸強度均為270N/mm2
,直至斷裂之伸長度為150%。 <中間樹脂層> 胺基甲酸酯系乾層合用接著劑:「AD-502 /CAT10L」,東洋MORTON股份有限公司製;塗佈量3g/m2
(塗佈時) <鋁箔> 鋁-鐵系合金之鋁箔:AA規格8079-O材;厚40μm <接著劑層> 上述實施例及比較例調製之接著劑;塗佈量:乾燥後厚2μm <樹脂薄膜> 未延伸聚丙烯薄膜;厚80μm [0065] [電池外裝材之評價] 針對上述製造之各電池外裝材,以下述所示條件之T形剝離強度試驗,進行接著性、耐電解液性及耐熱性評價。該等評價結果彙總示於表2及3。 <T形剝離強度試驗> ‧測定試料:自電池外裝材切出長150mm×寬15mm之尺寸之試驗片 ‧測定裝置:精密萬能試驗機;「AUTOGRAPH AG-X」,島津製作所股份有限公司製 ‧剝離位置:測定試料之鋁箔與樹脂薄膜之間 ‧剝離速度:100mm/分鐘 (1)接著性 於溫度23℃、濕度50%RH(常態)測定,由鋁箔與樹脂薄膜之常態T形剝離強度進行評價。 (2)耐電解液性 將測定試料浸漬於電解液溶劑(碳酸伸丙酯/碳酸二乙酯混合液;混合質量比50:50),於85℃環境下放置1天後,取出,與前述(1)同樣進行測定,由鋁箔與樹脂薄膜之浸漬後T形剝離強度進行評價。 (3)耐熱性 將測定試料於85℃環境下放置3分鐘,確認測定試料表面為85℃後,與前述(1)同樣進行測定,由鋁箔與樹脂薄膜之高溫(85℃)T形剝離強度進行評價。 [0066][0067][0068] 由表2及3所示之結果之對比可知,依據作為聚異氰酸酯化合物(B)使用特定3種之接著劑(實施例1~13),T形剝離強度均充分高,獲得良好接著性,且確認獲得耐電解液性及耐熱性亦優異之層合體。 另一方面,作為聚異氰酸酯化合物(B)僅使用前述3種中之任一種或2種之接著劑(比較例1~6),常態T形剝離強度、電解液溶劑浸漬後之T形剝離強度及高溫(85℃)T形剝離強度中之任一者或所有均無法說為充分,並非上述之接著性、耐電解液性及耐熱性之所有效果均優異者。
Claims (16)
- 一種金屬箔與樹脂薄膜之層合用接著劑,其特徵係含有具有羧基的聚烯烴樹脂(A)、及聚異氰酸酯化合物(B), 前述聚異氰酸酯化合物(B)包含飽和脂肪族聚異氰酸酯的多聚物(B1)、飽和脂環式聚異氰酸酯的多聚物(B2)、及芳香族聚異氰酸酯的多聚物(B3)。
- 如請求項1記載之接著劑,其中,前述飽和脂肪族聚異氰酸酯的多聚物(B1)包含選自飽和脂肪族聚異氰酸酯的脲甲酸酯化多聚物、及飽和脂肪族聚異氰酸酯的異氰脲酸酯體中的1種以上。
- 如請求項1記載之接著劑,其中,前述飽和脂環式聚異氰酸酯的多聚物(B2)包含選自飽和脂環式聚異氰酸酯的脲甲酸酯化多聚物、及飽和脂環式聚異氰酸酯的異氰脲酸酯體中的1種以上。
- 如請求項1記載之接著劑,其中,前述芳香族聚異氰酸酯的多聚物(B3)包含選自芳香族聚異氰酸酯的脲甲酸酯化多聚物、芳香族聚異氰酸酯的異氰脲酸酯體、及聚亞甲基聚苯基聚異氰酸酯中的1種以上。
- 如請求項1~4中任1項記載之接著劑,其中,前述飽和脂肪族聚異氰酸酯的多聚物(B1)、前述飽和脂環式聚異氰酸酯的多聚物(B2)、及前述芳香族聚異氰酸酯的多聚物(B3)的各異氰酸基的莫耳比為3~20:1~6:1。
- 如請求項1記載之接著劑,其中,前述聚烯烴樹脂(A)包含選自丙烯、乙烯及丁烯中的1種以上之單體單位。
- 如請求項1或6記載之接著劑,其中,前述聚烯烴樹脂(A)包含被選自乙烯性不飽和羧酸或其酸酐中的1種以上改性的聚烯烴樹脂。
- 如請求項1或6記載之接著劑,其中,前述聚烯烴樹脂(A)依據JIS K 7210-1:2014,在溫度130℃、以荷重2.16kg測定的熔體流動速率為2~50g/10分鐘。
- 如請求項1記載之接著劑,其中,相對於前述聚烯烴樹脂(A)的羧基1莫耳之前述聚異氰酸酯化合物(B)的異氰酸基的莫耳比率為0.3~30。
- 如請求項1記載之接著劑,其中,再含有金屬羧酸鹽(C)。
- 一種層合體,其特徵係金屬箔與樹脂薄膜使用請求項1~10中任1項記載之接著劑層合而成。
- 如請求項11記載之層合體,其中,前述金屬箔為鋁箔且前述樹脂薄膜為熱融著性樹脂薄膜。
- 如請求項11或12記載之層合體,其中,前述金屬箔的厚度為10~100μm,且前述樹脂薄膜的厚度為9~100μm。
- 一種電池外裝材,其特徵係使用請求項11~13中任1項記載之層合體。
- 一種電池盒,其特徵係使用請求項14記載之電池外裝材。
- 一種電池盒之製造方法,其特徵係具有將請求項14記載之電池外裝材進行深拉伸加工或撐壓加工而成形之步驟。
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- 2017-09-19 PL PL17882564T patent/PL3561016T3/pl unknown
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JPWO2018116555A1 (ja) | 2019-10-24 |
JP6895992B2 (ja) | 2021-06-30 |
PL3561016T3 (pl) | 2021-10-25 |
US11804631B2 (en) | 2023-10-31 |
US20190326564A1 (en) | 2019-10-24 |
KR102344139B1 (ko) | 2021-12-28 |
EP3561016A1 (en) | 2019-10-30 |
TW201823408A (zh) | 2018-07-01 |
CN110072960B (zh) | 2021-06-25 |
WO2018116555A1 (ja) | 2018-06-28 |
KR20190099205A (ko) | 2019-08-26 |
EP3561016B1 (en) | 2021-03-31 |
CN110072960A (zh) | 2019-07-30 |
EP3561016A4 (en) | 2020-06-03 |
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