TW202309215A - 黏接劑組成物及黏接劑組成物之製造方法 - Google Patents
黏接劑組成物及黏接劑組成物之製造方法 Download PDFInfo
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- TW202309215A TW202309215A TW111128855A TW111128855A TW202309215A TW 202309215 A TW202309215 A TW 202309215A TW 111128855 A TW111128855 A TW 111128855A TW 111128855 A TW111128855 A TW 111128855A TW 202309215 A TW202309215 A TW 202309215A
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Abstract
本發明的課題在於提供一種與基材的拉伸剪切特性、硬化性、耐熱性等特性優異的環氧系黏接劑。
本發明的解決手段為一種黏接劑組成物,含有:環氧樹脂組成物(A)、硬化觸媒(B)及觸變減黏劑(C),前述環氧樹脂組成物(A)係包含環氧樹脂(a)與具有酚性羥基之化合物(b)的反應產物(c)者,凝膠滲透層析術測定之面積比中,設前述環氧樹脂(a)、前述具有酚性羥基之化合物(b)及前述反應產物(c)的合計為100%時,前述反應產物(c)的面積比超過2.0%且為10%以下。
Description
本發明係關於黏接性、硬化性及耐熱性優異的黏接劑組成物。更詳細而言,係關於用於黏接汽車等車輛等結構物之結構用黏接劑組成物。
以往,環氧系黏接劑係機械特性、耐水性、耐化學性、耐熱性等特性優異,使用於塗料、成型材料、散熱材料、黏接劑等廣泛的領域,成為產業界不可或缺的素材。環氧系黏接劑通常為包含環氧樹脂、硬化劑及觸媒之熱固性樹脂,環氧乙烷環藉由加熱與硬化劑反應、複加成以形成硬化體。已知這樣的熱固性樹脂與各種素材相比,機械特性、耐蝕性、黏接性等較優異。藉由此等特徵,環氧系黏接劑廣泛使用於接合汽車、列車等車輛、飛機等結構體。這樣的黏接劑被稱為結構用黏接劑。
另一方面,由於環氧系黏接劑脆,正在廣泛探討改質劑的添加、硬化體的交聯密度控制等。例如,如專利文獻1,藉由摻合含有羧基的丁二烯-丙烯腈液狀橡膠以於所得之硬化體導入柔軟鏈,使韌性提升。
又,若依照非專利文獻1,有提案適當選擇環氧種類、硬化劑,進一步使交聯密度降低,藉此能夠使環氧樹脂強韌化。
〔先前技術文獻〕
〔專利文獻〕
[專利文獻1]日本特開平5-148337
〔非專利文獻〕
[非專利文獻1] L. D. Bravence et al : 34th International SAMPE Symposium (19)
〔發明所欲解決之問題〕
專利文獻1的方法中藉由柔軟鏈的導入來改善韌性,但有耐熱性差的問題。又,非專利文獻1中,確認存在下列課題:使低官能性的成分比率變多之環氧樹脂組成物係硬化性降低,即使在規定的溫度條件處理,硬化也不會充分地進行,黏接性變低。本發明係以該先前技術的問題為背景所完成者。即,本發明的目的在於提供與基材的黏接性、硬化性及耐熱性優異的環氧系黏接劑。
〔解決問題之方式〕
本發明係以該先前技術的課題為背景所完成者。本案發明人們仔細探討的結果,發現藉由以下所示之手段,能夠解決上述課題,而達成本發明。即,本發明係由以下構成所構成。
[1]一種黏接劑組成物,含有:環氧樹脂組成物(A)、硬化觸媒(B)及觸變減黏劑(C),
前述環氧樹脂組成物(A)係包含環氧樹脂(a)與具有酚性羥基之化合物(b)的反應產物(c)者,
凝膠滲透層析術測定之面積比中,設前述環氧樹脂(a)、前述具有酚性羥基之化合物(b)及前述反應產物(c)的各面積比的合計為100%時,前述反應產物(c)的面積比超過2.0%且為10%以下。
[2]一種黏接劑組成物,含有:環氧樹脂組成物(A)、硬化觸媒(B)及觸變減黏劑(C),
前述環氧樹脂組成物(A)係包含環氧樹脂(a)與具有酚性羥基之化合物(b)的反應產物(c)者,
以170℃30分鐘硬化、在25℃浸漬於四氫呋喃1小時後的凝膠分率為90質量%以上。
[3]如前述[1]或[2]中記載之黏接劑組成物,其中,
前述反應產物(c)的數量平均分子量為前述環氧樹脂(a)的數量平均分子量的1.5倍以上5.0倍以下。
[4]如前述[1]至[3]中任一項記載之黏接劑組成物,其中,
前述反應產物(c)的數量平均分子量為550以上3000以下。
[5]如前述[1]至[4]中任一項記載之黏接劑組成物,其中,
前述環氧樹脂(a)及前述具有酚性羥基之化合物(b)的數量平均分子量皆為1000以下。
[6]如前述[1]至[5]中任一項記載之黏接劑組成物,其中,
前述具有酚性羥基之化合物(b)所具有之酚性羥基的數目為每1分子2個。
[7]如前述[1]至[6]中任一項記載之黏接劑組成物,更含有氧化鈣(D)。
[8]一種積層體,具有將如前述[1]至[7]中任一項記載之黏接劑組成物硬化而成之黏接劑層。
[9]一種黏接劑組成物之製造方法,具有下列步驟:
至少混合環氧樹脂(a)及具有酚性羥基之化合物(b),使其反應而得到環氧樹脂組成物(A);
接著至少混合環氧樹脂組成物(A)、硬化觸媒(B)及觸變減黏劑(C)。
〔發明之效果〕
依據本發明,能夠提供黏接性、硬化性及耐熱性優異的黏接劑組成物。因此,本發明的黏接劑組成物能夠作為結構用黏接劑合適地使用。
以下,詳述本發明實施的一形態。但是,本發明未限定於此,能夠在已述之範圍內以加入各種變形之態樣實施。本發明的黏接劑組成物含有環氧樹脂組成物(A)、硬化觸媒(B)、及觸變減黏劑(C),前述環氧樹脂組成物(A)係包含環氧樹脂(a)與具有酚性羥基之化合物(b)的反應產物(c)者。
<環氧樹脂(a)>
本發明所使用之環氧樹脂(a),只要為具有2官能以上的環氧乙烷環之化合物則未特別限定,具體而言,能夠列舉:將雙酚A、雙酚F、雙酚AP、雙酚AF、雙酚B、雙酚BP、雙酚C、雙酚E、雙酚M、雙酚S、雙酚P、雙酚PH、雙酚Z等予以環氧丙基醚化而得之雙酚型環氧樹脂、及此等部分地縮合之混合物;兒茶酚、間苯二酚、對苯二酚、鄰苯二甲酸等之二環氧丙基醚化物;將萘、聯苯、四甲基聯苯、雙酚茀、雙甲酚茀、四酚乙烷等在結構中具有2個酚性羥基之化合物予以環氧丙基醚化而得之環氧丙基醚化合物、及此等部分地縮合之混合物;將酚酚醛清漆、甲酚酚醛清漆、雙酚A酚醛清漆等予以環氧丙基醚化而得之酚醛清漆型環氧樹脂;將苯胺、鄰甲基苯胺、對胺基酚、間伸苯基二胺等予以環氧丙基醚化之環氧丙基胺型環氧樹脂;三聚異氰酸三環氧丙酯、三苯基環氧丙基醚甲烷型環氧樹脂、伸茬基型環氧樹脂、肆酚乙烷型環氧樹脂、萘型環氧樹脂等多官能環氧樹脂;將雙酚A的環氧乙烷加成物、雙酚A的環氧丙烷加成物等予以環氧丙基醚化而得之二環氧丙基化合物;將1,4-丁二醇、1,6-己二醇、1,12-十二烷二醇、環己烷二甲醇、2,2-二甲基丙二醇、三羥甲基丙烷、二環戊二烯二甲醇、氫化雙酚A、二聚物酸、六氫鄰苯二甲酸、六氫對苯二甲酸、聚丁二烯、聚異戊二烯、聚丁二烯二醇、山梨醇、新戊四醇、聚甘油等予以環氧丙基化而得之環氧丙基化合物等。
此等之中,環氧樹脂(a)較佳為2官能的環氧樹脂,考量黏接性及耐熱性等機械特性的觀點,尤其是雙酚型環氧樹脂為較佳,特佳為雙酚A型環氧樹脂、雙酚F型環氧樹脂。可單獨使用1種此等環氧樹脂(a),亦可併用2種以上。
本發明所使用之環氧樹脂(a)較佳為在室溫下為液狀。較佳為在室溫下具有50000mPa.s以下的黏度,進一步較佳為30000mPa.s以下,更佳為20000mPa.s以下。又,環氧樹脂(a)的數量平均分子量較佳為1,000以下。若數量平均分子量超過1000則有在室溫固體化的情況、黏度變高而處理性顯著變差的情況。
<具有酚性羥基之化合物(b)>
本發明所使用之具有酚性羥基之化合物(b),能夠列舉例如:雙酚A、雙酚F、雙酚E等雙酚類化合物;兒茶酚、間苯二酚、甲基兒茶酚等兒茶酚類化合物;聯苯酚、四甲基聯苯酚等聯苯酚類化合物;雙甲酚茀等雙甲酚類化合物;對苯二酚等對苯二酚類化合物;酚酚醛清漆、甲酚酚醛清漆、雙酚A酚醛清漆、伸茬基酚醛清漆、三苯基甲烷酚醛清漆、聯苯酚醛清漆、二環戊二烯酚酚醛清漆、萜烯酚酚醛清漆等酚醛清漆類化合物等。此等之中,考量對環氧樹脂(a)的溶解性的觀點、及為了具有良好的剝離強度,尤其是雙酚類化合物、兒茶酚類化合物為較佳,更佳為雙酚類化合物,特佳為雙酚A、雙酚F。可單獨使用1種此等具有酚性羥基之化合物(b),亦可併用2種以上。
具有酚性羥基之化合物(b)的分子量較佳為1,000以下。若分子量超過1000則有在室溫固體化的情況、黏度變高而處理性顯著變差的情況。又,考量硬化後的韌性的觀點,具有酚性羥基之化合物(b)所具有之酚性羥基的數目較佳為2以上,又,較佳為4以下,更佳為3以下,最佳為2。
<反應產物(c)>
本發明所使用之環氧樹脂組成物(A)係包含環氧樹脂(a)與具有酚性羥基之化合物(b)的反應產物(c)者。反應產物(c)的數量平均分子量較佳為環氧樹脂(a)的數量平均分子量的1.5倍以上,進一步較佳為1.6倍以上。若為前述值以上,則產生適度的分支,因而硬化性變得良好。又,較佳為5.0倍以下,更佳為4.0倍以下,進一步較佳為3.5倍以下。若為前述值以下,則黏度的上升變得適度,作業性佳。又,反應產物(c)的數量平均分子量較佳為550以上,更佳為600以上,進一步較佳為800以上。又,數量平均分子量較佳為3,000以下,更佳為2,000以下,又更佳為1,500以下。藉由數量平均分子量為前述範圍內,硬化性、黏接性及耐熱性變得良好而較佳。
又,凝膠滲透層析術測定之面積比中,設環氧樹脂(a)、具有酚性羥基之化合物(b)及反應產物(c)的合計為100%時,反應產物(c)的面積比超過2.0%且為10%以下。較佳為3.0%以上,進一步較佳為4.0%以上。又,較佳為9.0%以下,進一步較佳為8.0%以下。藉由反應產物(c)的面積比為前述範圍內,成為硬化性、黏接性及耐熱性優異的黏接劑組成物。又,黏度不會變得過高,考量作業性的觀點亦為較佳。其理由並未明確,但推測:相對於在硬化觸媒存在下之硬化反應中酚性羥基與環氧樹脂的反應會優先進行,在環氧樹脂組成物(A)中,首先環氧樹脂(a)與具有酚性羥基之化合物(b)反應而生成之二級羥基進一步與另一環氧樹脂(a)進行反應者係優先進行,因而生成具有分支結構之化合物,因此成為硬化性、黏接性及耐熱性優異的黏接劑組成物。又,反應產物(c)的分子量峰較佳為比源自環氧樹脂(a)及具有酚性羥基之化合物(b)的最大分子量峰高300以上。凝膠滲透層析術的測定能夠以實施例中記載的條件實施。
<硬化觸媒(B)>
本發明所使用之硬化觸媒,只要為能夠促進環氧樹脂(a)與具有酚性羥基之化合物(b)的反應者則未特別限定,具體而言,能夠列舉以下的化合物。能夠列舉:3-(4-氯苯基)-1,1-二甲基脲、3-(3,4-二氯苯基)-1,1-二甲基脲、N,N’-(4-甲基-1,3-伸苯基)雙[N’,N’-二甲基脲]、N’-[3-[[[(二甲基胺基)羰基]胺基]甲基]-3,5,5-三甲基環己基]-N,N-二甲基脲等脲類;DBU(1,8-二氮雜雙環[5.4.0]十一碳-7-烯)、DBU-酚鹽、DBU-辛酸鹽、DBU-甲酸鹽、DBU-對甲苯磺酸鹽等DBU型胺類;DBN(1,5-二氮雜雙環[4.3.0]壬- 5-烯);三乙胺、N,N,N’,N’-四甲基乙二胺、四甲基胍、三乙二胺等三級胺系;二甲基胺基甲醇、二甲基胺基乙醇等醇胺類;雙(2-二甲基胺基乙基)醚等醚胺類;2,4,6-參(二甲基胺基甲基)酚(DMP-30)等具有酚基之三級胺類;胺加成物類;1,2-二甲基咪唑、2-乙基-4-甲基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑、N-苄基-2-甲基咪唑、N-苄基-2-苯基咪唑、2,4-二甲基咪唑、咪唑、1-甲基咪唑、2-甲基咪唑、2,4-二胺基-6-[2’-甲基咪唑基-(1’)]-乙基-s-三𠯤異三聚氰酸加成物、2-苯基-4,5-二羥甲基咪唑、2,4-二胺基-6-[2’-甲基咪唑基-(1’)]-乙基-s-三𠯤、1-氰乙基-2-苯基偏苯三酸咪唑鎓等咪唑類;AMICURE PN-23、PN-23J、PN-H、PN-31、PN-31J、PN-40、PN-40J、PN-50(皆為味之素精密技術製)、NOVACURE HX-3722、HX-3742、HX-3792(皆為旭化成製)等咪唑加成物類;三苯基膦、三鄰甲苯基膦、三間甲苯基膦、三對甲苯基膦、三-2,4-茬基膦、三-2,5-茬基膦、三-3,5-茬基膦、參(對甲氧基苯基)膦、參(鄰甲氧基苯基)膦、三苯基膦-三苯基硼烷錯合物、四苯基硼酸四苯基鏻、四對甲苯基硼酸四苯基鏻、參(2,6-二甲氧基苯基)膦等磷類等。此等之中,考量硬化性、黏接性及耐熱性與潛在性的觀點,較佳為咪唑加成物類、或者磷類的觸媒。
就本發明的黏接劑組成物中之較佳的硬化觸媒(B)的含量而言,考量硬化之活性與穩定性的觀點,相對於100質量份的環氧樹脂組成物(A)為0.5~20質量份,更佳為0.5~10質量份,進一步較佳為0.5~8質量份。若含量為前述下限值以上,則硬化性會提升。又,若使用量為前述上限值以下,則保持觸媒效果的潛在性,且良好地保持黏接劑組成物的穩定性,因而較佳。
<觸變減黏劑(C)>
本發明所使用之觸變減黏劑(C),只要為環氧系黏接劑中有賦予觸變減黏性之效果的周知者則未特別限定,具體而言,能夠列舉:親水性氣相二氧化矽、疏水性氣相二氧化矽等氣相二氧化矽類;碳黑、各金屬粉等微細粒子類;砂灰石、雲母、滑石、高嶺土、硫酸鋇、碳酸鈣、氫氧化鎂、黏土等長寬比高的無機填料類等。此等之中,考量可得到適度的觸變減黏性、且疏水性高的點,較佳為經疏水性的官能基修飾之表面處理氣相二氧化矽。
就本發明的黏接劑組成物中之較佳的觸變減黏劑(C)的含量而言,相對於100質量份的環氧樹脂組成物(A)為0.5~20質量份,更佳為1~15質量份,進一步較佳為1~10質量份。若含量為前述範圍內,則適當地保持黏接劑塗布時、硬化時的黏度範圍,且作業性變得良好,而為較佳。
<氧化鈣(D)>
本發明的黏接劑組成物含有氧化鈣(D)亦為較佳。藉由含有氧化鈣(D),黏接性及耐熱性會提升。本發明所使用之氧化鈣,只要為以氧化鈣為主要成分者即可,不因有無表面處理、粒徑等而特別限定。
就本發明的黏接劑組成物中之較佳的氧化鈣(D)的含量而言,相對於100質量份的環氧樹脂組成物(A)為0.5~10質量份,更佳為1~10質量份,進一步較佳為1.5~10質量份。若使用量為前述範圍內,則黏接性及耐熱性等機械特性變得良好,而為較佳。
<其他成分>
本發明的黏接劑組成物包含環氧樹脂組成物(A)、硬化觸媒(B)及觸變減黏劑(C)。除了此等之外,亦可進一步含有硬化劑、彈性體、核殼橡膠、偶合劑、無機填料、間隔物、各種添加劑等。
硬化劑係用以改善黏接劑組成物的諸物性。能夠列舉例如:二氰二胺;己二酸二醯肼、間苯二甲酸二醯肼、二元酸二醯肼等醯肼類;二伸乙三胺、三伸乙四胺、四伸乙五胺、三甲基六亞甲基二胺、2-甲基五亞甲基二胺、二乙基胺基丙胺等脂肪族胺類;異佛酮二胺、1,3-雙胺基甲基環己烷、雙(4-胺基環己基)甲烷、降莰烯二胺、1,2-二胺基環己烷、Laromin C-260等脂環式多胺類;聚氧丙烯二胺、聚氧丙烯三胺等聚醚型多胺類;聚環己基多胺混合物;哌𠯤、N-胺基乙基哌𠯤等哌𠯤類;半卡肼、氰基乙醯胺等多胺基醯胺類;將二聚物酸、脂肪酸與多胺縮合而成之聚醯胺胺類;使環氧樹脂與胺反應而成之胺-環氧加成物類;使胺與丙烯酸化合物反應而成之麥可加成多胺類;曼尼希反應產物;酮亞胺類;三聚氰胺類、乙胍𠯤、苯胍𠯤等胍胺(guanamine)類、胍類、間二甲苯二胺、4,4’-二胺基二苯基甲烷、4,4’-二胺基二苯基碸、間苯二胺等芳香族胺類;四氫鄰苯二甲酸酐、六氫鄰苯二甲酸酐、甲基四氫鄰苯二甲酸酐、甲基六氫鄰苯二甲酸、二苯基酮四甲酸酐、均苯四酸酐、偏苯三酸酐、甲基納迪克酸、氫化甲基納迪克酸酐、十二烯基琥珀酸酐、琥珀酸酐、鄰苯二甲酸酐、脂肪族二元酸多酐、乙二醇雙氫化偏苯三酸酐等酸酐類;三氟化硼錯合物、三氯化硼錯合物、鋶鹽、鎓鹽、多羧酸的活性酯類等。此等之中,考量潛在性的點,較佳為二氰二胺。
硬化劑的使用量,相對於環氧基,較佳為設活性氫基的比例為0.9~1.1的範圍。若為上述範圍內,則環氧基與活性氫基的反應平衡良好,能夠發揮充分的硬化性。
彈性體用於黏接劑組成物的改質。例如:NBR、SBR、聚丁二烯、末端羧酸改性丙烯腈-丁二烯等橡膠改性環氧樹脂類;例如:ADEKA RESIN EPR系列(ADEKA製)、Hypox RA840、RA1340等Hypox系列(CVC製)等;分子中具有胺甲酸乙酯鍵且具有2個以上環氧乙烷環之胺甲酸乙酯改性環氧樹脂類;只要具有上述組成則未特別限定,能夠列舉例如:ADEKA RESIN EPR1630等ADEKA RESIN EPR系列、Hypox UA10等Hypox系列(CVC製)等;NBR、SBR、聚丁二烯等液狀橡膠;矽氧樹脂;交聯NBR、交聯BR等交聯橡膠微粒子;胺甲酸乙酯橡膠;末端羧酸、末端胺基型丙烯腈-丁二烯橡膠(CTBN、ATBN);主鏈具有羧酸之NBR橡膠;末端羧酸型聚丁二烯;液狀多硫化物;各種胺甲酸乙酯預聚合物;聚醚碸、聚醯胺、聚醚醯亞胺、丙烯酸樹脂、聚酯、聚碳酸酯等工程塑膠樹脂微粒子等。此等可單獨使用,亦可併用2種以上。
核殼橡膠係至少具有由橡膠成分構成之核層、與堅硬的殼層之2層結構的粒子。藉由含有核殼橡膠,能夠期待剝離強度等韌性的提升。又,核殼橡膠用於利用黏接劑的改質、物理交聯之零件的暫時固定。就核殼橡膠而言,能夠列舉例如:Kane Ace MX153、MX154、MX-257、MX-960、MX-136、MX-217(皆為卡內卡製)、GANZPEARL(愛克工業製)等。
就核層而言,使用橡膠狀物質,例如:由聚丁二烯等共軛二烯、及/或丙烯酸低級烷酯聚合而成之聚合物、與能夠與此等共聚合之單體共聚合成之聚合物、聚矽氧烷等構成。考量低溫下的耐衝擊性的改善、剝離強度的提升的觀點,核層較佳為玻璃轉移溫度為-20度以下的物質。
就殼層而言,較佳為與環氧樹脂的親和性高,且不顯示橡膠彈性的成分。若為這樣的成分則未特別限定,考量接枝聚合性和與環氧樹脂的親和性的觀點,較佳為由甲基丙烯酸甲酯、及/或苯乙烯的單體聚合而成之聚合物、或與可與此等共聚合的單體共聚合成之聚合物構成。此外,考量黏接性的觀點,殼層較佳為玻璃轉移點為50℃以上的物質。
偶合劑用於對基材、填料、樹脂等的密合性改良。可列舉例如:乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、2-(3,4-乙氧基環己基)乙基三甲氧基矽烷、3-環氧丙氧基丙基甲基二甲氧基矽烷、3-環氧丙氧基丙基三甲氧基矽烷、3-環氧丙氧基丙基甲基二乙氧基矽烷、3-環氧丙氧基丙基三乙氧基矽烷、對苯乙烯基三甲氧基矽烷、3-甲基丙烯醯氧基丙基甲基二甲氧基矽烷、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甲基二乙氧基矽烷、3-甲基丙烯醯氧基丙基三乙氧基矽烷、3-丙烯醯氧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、N-2-(胺基乙基)-3-胺基丙基三甲氧基矽烷、3-胺基丙基三甲氧基矽烷、3-胺基丙基三乙氧基矽烷、3-乙氧基矽基-N-(1,3-二甲基-亞丁基)丙胺、N-苯基-3-胺基丙基三甲氧基矽烷、三聚異氰酸參-(三甲氧基矽基丙基)酯、3-巰基丙基甲基二甲氧基矽烷、3-巰基丙基三甲氧基矽烷、3-異氰酸酯丙基三乙氧基矽烷、3-三甲氧基矽基丙基琥珀酸酐等矽烷偶合劑類。
無機填料用於填充、機械物性的提升等目的。可列舉例如:砂灰石、雲母、滑石、高嶺土、硫酸鋇、碳酸鈣、氫氧化鎂、黏土、矽酸鈣、矽酸鋁、氫氧化鈣、氫氧化鎂、氫氧化鋁、碳酸鎂、碳酸鋇、正長岩、綠泥石、膨土、蒙脫石、重晶石、白雲石、石英、玻璃、長石、矽藻土、雲母、高嶺土、氧化鋁、石墨、碳纖維、玻璃纖維等纖維、結晶二氧化矽、非晶二氧化矽、熔融二氧化矽、氣相二氧化矽、鍛燒二氧化矽、沉降二氧化矽、粉碎(微粉末)二氧化矽等二氧化矽、氧化鐵、氧化鋅、氧化鈦、氧化鋇、二氧化鈦、中空玻璃珠、聚合物中空珠等。此等可單獨使用,亦可併用2種以上。
間隔物用以調整黏接體的厚度。可列舉例如:玻璃珠、纖維、樹脂珠、具有一定以上的硬度與粒徑之無機填料等。此等可單獨使用,亦可併用2種以上。
考量控制黏接體的厚度、黏接體的應力的觀點,間隔物的粒子徑較佳為1~200μm,更佳為10~150μm。
間隔物的形狀,可列舉例如:球狀粒子、纖維狀粒子等。此等之中,考量容易控制粒子徑,較佳為球狀粒子。
使用間隔物時的使用量,較佳為每100質量份的環氧樹脂組成物(A)為0.2~1.5質量份,更佳為0.5~1質量份。
就各種添加劑而言,能夠摻合例如:塑化劑、反應性稀釋劑、保存穩定性化劑、抗老化劑、抗氧化劑、顏料、染料、著色劑、偶合劑、調平劑、黏接賦予劑、阻燃劑、抗靜電劑、導電性賦予劑、潤滑劑、滑動性賦予劑、紫外線吸收劑、界面活性劑、分散劑、分散穩定劑、消泡劑、脫水劑、交聯劑、防鏽劑、溶劑等。
<黏接劑組成物>
本發明的黏接劑組成物,含有環氧樹脂組成物(A)、硬化觸媒(B)、及觸變減黏劑(C),前述環氧樹脂組成物(A)係包含環氧樹脂(a)與具有酚性羥基之化合物(b)的反應產物(c)者。亦可包含前述之其他成分。
本發明的黏接劑組成物,較佳為以170℃30分鐘硬化、浸漬於四氫呋喃1小時後的凝膠分率為90質量%以上。更佳為95質量%以上,進一步較佳為97質量%以上。本發明的黏接劑組成物若凝膠分率的值為前述值以上,則硬化性優異,成為黏接性、耐熱性優異的黏接劑組成物。為了提升凝膠分率,能夠藉由前述反應產物(c)的數量平均分子量、環氧樹脂組成物(A)中的面積比、硬化觸媒的選定來調整。
<黏接劑組成物之製造方法>
本發明的黏接劑組成物,能夠混合上述之各成分來製造。就混合方法而言,可列舉:分散機、雙行星混合機、自轉公轉混合機、均質機、三輥、混練機、捏合機等。
<黏接劑組成物之塗布方法>
就本發明的黏接劑組成物之塗布方法而言,可列舉:利用分配器塗布填充於注射器等之黏接劑組成物之方法,噴霧、槍、刷毛塗布等方法。本步驟中,黏接劑組成物的塗布溫度較佳為30~60℃。又,黏接劑組成物的硬化溫度較佳為120~220℃,更佳為140~200℃。硬化時間較佳為20~120分鐘,更佳為30~90分鐘,進一步較佳為30~60分鐘。
<積層體之製造方法>
本發明的積層體係將前述黏接劑組成物配置於基材1與基材2之間並使其硬化而得之黏接劑層構成者。基材1與基材2各自可列舉:鐵、鋁、鋼等金屬類;CFRP、GFRP等纖維強化塑膠;聚對苯二甲酸乙二酯(PET)、聚對苯二甲酸丁二酯(PBT)、聚碳酸酯(PC)、聚醯亞胺(PI)、聚醯胺(PA)等工程塑膠樹脂類;玻璃等。
[實施例]
以下顯示實施例具體地說明本發明,但本發明未限定於實施例。又,各測定項目係依照以下方法。
<拉伸剪切強度>
使用以丙酮將下述基材脫脂者作為被黏材,依據JIS K6850:1999進行試驗片的製備與測定。設拉伸速度為10mm/min。以黏接劑層的厚度成為0.1mm的方式塗布黏接劑組成物,將以170℃30分鐘硬化所製備之試驗片的拉伸剪切強度為20MPa以上的水準評為○,將未達20MPa的水準評為×。
基材:SPCC-SD(冷間壓延鋼板)(1.6mm×25mm×100mm,工程測試服務公司製)
<T-Peel(T型剝離強度)>
使用以丙酮將下述基材脫脂者作為被黏材,依據JIS K6854-3:1999進行試驗片的製備與測定。設拉伸速度為10mm/min。以黏接劑層的厚度成為0.1mm的方式塗布黏接劑組成物,將以170℃30分鐘硬化所製備之試驗片的T-Peel為75N/25mm以上的水準評為○,將未達75N/25mm的水準評為×。
基材:SPCC-SD(冷間壓延鋼板)(0.5mm×25mm×200mm,工程測試服務公司製)
<凝膠分率>
將以170℃30分鐘硬化之黏接劑組成物切下縱2.5cm橫5cm厚度0.1mm的長條狀以測定重量(將此重量作為A),在25℃浸漬於100mL的四氫呋喃1小時。取出長條狀之硬化之黏接劑組成物以熱風乾燥機在100℃乾燥1小時,測定重量(將此重量作為B)。將利用以下的式子算出之數值作為凝膠分率(%)。將凝膠分率為90%以上的水準評為○,將未達90%的水準評為×。
凝膠分率(%)=B/A×100
<耐熱性>
藉由動態黏彈性測定裝置(DVA-220,艾蒂測量控制公司製)來測定。將以170℃30分鐘硬化之黏接劑組成物切下長條狀,以頻率10Hz、升溫速度4℃/min測定,測定黏接劑組成物的動態黏彈性。將由測定所得之在250℃保持塗膜之水準評為○,將在250℃塗膜拉伸而無法測定之水準評為×。
<數量平均分子量(Mn)>
將試料(環氧樹脂組成物(A))以試料濃度成為0.5質量%左右的方式溶解或稀釋於四氫呋喃,將以孔徑0.5μm的聚四氟乙烯製膜過濾器過濾者作為測定用試料。利用將四氫呋喃作為移動相並將微差折射器作為檢測器之凝膠滲透層析術測定數量平均分子量。設流速為1mL/分鐘,設管柱溫度為30℃。管柱係使用昭和電工製KF-802、804L、806L。分子量標準係使用單分散聚苯乙烯。但是,試料不溶解於四氫呋喃時,使用N,N-二甲基甲醯胺代替四氫呋喃。
<環氧樹脂組成物(A1)的製備>
於裝備有攪拌機、溫度計、冷卻管之反應罐內,進料50質量份的jER807、53質量份的jER828、64質量份的雙酚A,慢慢地加熱至150℃以進行反應。利用GPC產生數量平均分子量為600以上的波峰,確認反應產物(c1)生成。在反應產物(c1)的波峰的面積比成為2.0%之階段結束反應,得到環氧樹脂組成物(A1)。所得之環氧樹脂組成物(A1)所含之反應產物(c1)的數量平均分子量為960,反應產物(c1)/環氧樹脂(a)的分子量比為1.8,GPC的面積比為4.8%。
<環氧樹脂組成物(A2)的製備>
於裝備有攪拌機、溫度計、冷卻管之反應罐內,進料105質量份的jER828、62質量份的雙酚A,慢慢地加熱至150℃以進行反應。利用GPC產生數量平均分子量為600以上的波峰,確認反應產物(c2)生成。在反應產物(c2)的波峰的面積比成為2.0%之階段結束反應,得到環氧樹脂組成物(A2)。所得之環氧樹脂組成物(A2)所含之反應產物(c2)的數量平均分子量為940,反應產物(c2)/環氧樹脂(a)的分子量比為1.7,GPC的面積比為4.9%。
<環氧樹脂組成物(A3)的製備>
於裝備有攪拌機、溫度計、冷卻管之反應罐內,進料105質量份的jER828、62質量份的雙酚A,慢慢地加熱至140℃以進行反應。利用GPC產生數量平均分子量為600以上的波峰,確認反應產物(c3)生成。在反應產物(c3)的波峰的面積比成為2.0%之階段結束反應,得到環氧樹脂組成物(A3)。所得之環氧樹脂組成物(A3)所含之反應產物(c3)的數量平均分子量為1000,反應產物(c3)/環氧樹脂(a)的分子量比為1.9,GPC的面積比為2.3%。
<環氧樹脂組成物(A4)的製備>
於裝備有攪拌機、溫度計、冷卻管之反應罐內,進料90質量份的YDF8170C、62質量份的雙酚A,慢慢地加熱至150℃以進行反應。利用GPC產生數量平均分子量為600以上的波峰,確認反應產物(c4)生成。在反應產物(c4)的波峰的面積比成為2.0%之階段結束反應,得到環氧樹脂組成物(A4)。所得之環氧樹脂組成物(A4)所含之反應產物(c4)的數量平均分子量為600,反應產物(c4)/環氧樹脂(a)的分子量比為2.2,GPC的面積比為5.4%。
<環氧樹脂組成物(A5)的製備>
於裝備有攪拌機、溫度計、冷卻管之反應罐內,進料77質量份的YDF8170C、62質量份的雙酚A,慢慢地加熱至150℃以進行反應。利用GPC產生數量平均分子量為600以上的波峰,確認反應產物(c5)生成。在反應產物(c5)的波峰的面積比成為2.0%之階段結束反應,得到環氧樹脂組成物(A5)。所得之環氧樹脂組成物(A5)所含之反應產物(c5)的數量平均分子量為600,反應產物(c5)/環氧樹脂(a)的分子量比為2.2,GPC的面積比為4.9%。
<環氧樹脂組成物(A6)的製備>
於裝備有攪拌機、溫度計、冷卻管之反應罐內,進料50質量份的jER807、53質量份的jER828、64質量份的雙酚A,慢慢地加熱至130℃以進行反應。利用GPC產生數量平均分子量為600以上的波峰,確認反應產物(c6)生成。在反應產物(c6)的波峰的面積比成為2.0%之前結束反應,得到環氧樹脂組成物(A6)。所得之環氧樹脂組成物(A6)所含之反應產物(c6)的數量平均分子量為830,反應產物(c6)/環氧樹脂(a)的分子量比為1.5,GPC的面積比為0.5%。
<環氧樹脂組成物(A7)的製備>
於裝備有攪拌機、溫度計、冷卻管之反應罐內,進料50質量份的jER807、53質量份的jER828、64質量份的雙酚A,慢慢地加熱至150℃以進行反應。利用GPC產生數量平均分子量為600以上的波峰,確認反應產物(c7)生成。在反應產物(c7)的波峰的面積比成為2.0%之前結束反應,得到環氧樹脂組成物(A7)。所得之環氧樹脂組成物(A7)所含之反應產物(c7)的數量平均分子量為830,反應產物(c7)/環氧樹脂(a)的分子量比為1.5,GPC的面積比為2.0%。
<環氧樹脂組成物(A8)的製備>
於裝備有攪拌機、溫度計、冷卻管之反應罐內,進料45質量份的jER807、43質量份的jER828、62質量份的雙酚A,慢慢地加熱至150℃以進行反應。利用GPC產生數量平均分子量為600以上的波峰,確認反應產物(c8)生成。在反應產物(c8)的波峰的面積比成為2.0%之前結束反應,得到環氧樹脂組成物(A8)。所得之環氧樹脂組成物(A8)所含之反應產物(c8)的數量平均分子量為830,反應產物(c8)/環氧樹脂(a)的分子量比為1.5,GPC的面積比為2.0%。
<環氧樹脂組成物(A9)的製備>
於裝備有攪拌機、溫度計、冷卻管之反應罐內,進料105質量份的jER828、62質量份的雙酚A,慢慢地加熱至150℃以進行反應。利用GPC產生數量平均分子量為600以上的波峰,確認反應產物(c9)生成。在反應產物(c9)的波峰的面積比成為2.0%之前結束反應,得到環氧樹脂組成物(A9)。所得之環氧樹脂組成物(A9)所含之反應產物(c9)的數量平均分子量為930,反應產物(c9)/環氧樹脂(a)的分子量比為1.7,GPC的面積比為0.8%。
<環氧樹脂組成物(A10)的製備>
於裝備有攪拌機、溫度計、冷卻管之反應罐內,進料90質量份的YDF8170C、55質量份的雙酚F,慢慢地加熱至130℃以進行反應。利用GPC產生數量平均分子量為550以上的波峰,確認反應產物(c10)生成。在反應產物(c10)的波峰的面積比成為2.0%之階段結束反應,得到環氧樹脂組成物(A10)。所得之環氧樹脂組成物(A10)所含之反應產物(c10)的數量平均分子量為560,反應產物(c10)/環氧樹脂(a)的分子量比為3.1,GPC的面積比為2.5%。
<實施例1>
藉由自轉公轉混合機混合100質量份的環氧樹脂組成物(A1)、作為觸媒(B)的1.8質量份的HX3742、作為觸變減黏劑(C)的1.8質量份的AEROSIL R805及1.8質量份的氧化鈣(D),得到黏接劑組成物1。實施所得之黏接劑組成物1的拉伸剪切、T-Peel、儲存彈性模數及凝膠分率的各評價。將結果顯示於表1。
<實施例2~7、比較例1~5>
作為黏接劑組成物的摻合組成,除了變更為表1所示之內容以外,以與實施例1相同的方法,製備黏接劑組成物2~12。實施所得之各黏接劑組成物的拉伸剪切、T-Peel、儲存彈性模數及凝膠分率的各評價。將結果顯示於表1。
[表1]
摻合 | 摻合量(質量份) | ||||||||||||
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 | 比較例1 | 比較例2 | 比較例3 | 比較例4 | 比較例5 | ||
黏接劑組成物 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | |
環氧樹脂組成物(A) | 環氧樹脂組成物(A1) | 100 | |||||||||||
環氧樹脂組成物(A2) | 100 | 100 | |||||||||||
環氧樹脂組成物(A3) | 100 | ||||||||||||
環氧樹脂組成物(A4) | 100 | ||||||||||||
環氧樹脂組成物(A5) | 100 | ||||||||||||
環氧樹脂組成物(A6) | 100 | ||||||||||||
環氧樹脂組成物(A7) | 100 | ||||||||||||
環氧樹脂組成物(A8) | 100 | 100 | |||||||||||
環氧樹脂組成物(A9) | 100 | ||||||||||||
環氧樹脂組成物(A10) | 100 | ||||||||||||
觸媒(B) | HX3742 | 1.8 | 1.8 | 1.8 | 2.0 | 2.2 | 2.1 | 1.8 | 1.8 | 2.0 | 2.0 | ||
TOTP | 2.4 | 2.4 | |||||||||||
觸變減黏劑(C) | AEROSIL R805 | 1.8 | 1.8 | 1.8 | 1.8 | 2.0 | 2.2 | 2.1 | 1.8 | 1.8 | 2.0 | 2.0 | 1.8 |
氧化鈣(D) | CML#35 | 1.8 | 1.8 | 1.8 | 2.0 | 2.2 | 2.1 | 1.8 | 1.8 | 2.0 | 2.0 | ||
環氧樹脂 | jER630 | 4.4 | |||||||||||
TETRAD-X | 2.9 | ||||||||||||
改質劑 | MX154 | 16.5 | |||||||||||
環氧樹脂組成物(A)的GPC測定 | 反應產物(c) | (c1) | (c2) | (c3) | (c2) | (c4) | (c5) | (c10) | (c6) | (c7) | (c8) | (c8) | (c9) |
反應產物(c)的數量平均分子量 | 960 | 940 | 1000 | 940 | 600 | 600 | 560 | 830 | 830 | 830 | 830 | 930 | |
反應產物(c)/環氧樹脂(a) 分子量比 | 1.8 | 1.7 | 1.9 | 1.7 | 2.2 | 2.2 | 3.1 | 1.5 | 1.5 | 1.5 | 1.5 | 1.7 | |
反應產物(c)的GPC面積比(%) | 4.8 | 4.9 | 2.3 | 4.9 | 5.4 | 4.9 | 2.5 | 0.5 | 2.0 | 2.0 | 2.0 | 0.8 | |
評價項目 | 拉伸剪切強度(MPa) | ○ | ○ | ○ | ○ | ○ | ○ | ○ | × | × | × | ○ | ○ |
20 | 28 | 32 | 32 | 27 | 36 | 25 | 11 | 19 | 19 | 24 | 26 | ||
T-Peel (N/mm) | ○ | ○ | ○ | ○ | ○ | ○ | ○ | × | × | × | × | ○ | |
75 | 120 | 85 | 80 | 100 | 150 | 135 | 5 | 45 | 50 | 25 | 80 | ||
耐熱性 | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ○ | × | |
凝膠分率(%) | ○ | ○ | ○ | ○ | ○ | ○ | ○ | × | × | × | × | × | |
91 | 95 | 99 | 97 | 98 | 99 | 90 | 53 | 74 | 78 | 85 | 60 |
<原料>
使用下述者作為表1中記載的原料。
jER-807:雙酚F型環氧樹脂,三菱化學製,Mn461
jER-828:雙酚A型環氧樹脂,三菱化學製,Mn550
YDF-8170C:雙酚F型環氧樹脂,日鐵化學材料製,Mn220
jER-630:3官能的環氧丙基胺型環氧樹脂,三菱化學製,分子量277
TETRAD-X:4官能的環氧丙基胺型環氧樹脂,三菱瓦斯化學製,分子量360
MX154:包含40質量份的核殼橡膠之雙酚A型環氧樹脂,卡內卡製
雙酚A:三菱化學製
雙酚F:群榮化學工業製
HX3742:咪唑加成物型觸媒,旭化成製
TOTP:三鄰甲苯基膦,東京化成製
AEROSIL R805:疏水性氣相二氧化矽,日本AEROSIL製
CML#35:氧化鈣,近江化學製
由實施例1與比較例1、2可知,藉由在環氧樹脂組成物中包含超過2.0%的反應產物(c),硬化型會改善,諸特性會提升。根據比較例3、4,僅添加3官能或4官能的環氧樹脂的情況下諸特性的改善並不充分。由實施例2~4可知,以雙酚A型環氧樹脂為基礎而變更觸媒種類的情況下,亦為藉由包含超過2.0%的化合物(c),硬化性會改善。另一方面,由比較例5可知,反應產物(c)的GPC的面積比為2.0%以下的情況耐熱性會有問題。由實施例5、6可知,藉由在雙酚F型環氧樹脂中包含超過2.0%的反應產物(c)諸特性會改善,即使包含改質劑也不會有任何問題。
[產業上利用性]
本發明所使用之環氧組成物作為黏接劑係為有用,該黏接劑能夠適合用作黏接性、硬化性、耐熱性等優異的黏接劑,尤其是作為結構用黏接劑係為有用,因此期待為產業界帶來巨大貢獻。
Claims (9)
- 一種黏接劑組成物,含有:環氧樹脂組成物(A)、硬化觸媒(B)及觸變減黏劑(C), 該環氧樹脂組成物(A)係包含環氧樹脂(a)與具有酚性羥基之化合物(b)的反應產物(c)者, 凝膠滲透層析術測定之面積比中,設該環氧樹脂(a)、該具有酚性羥基之化合物(b)及該反應產物(c)的各面積比的合計為100%時,該反應產物(c)的面積比超過2.0%且為10%以下。
- 一種黏接劑組成物,含有:環氧樹脂組成物(A)、硬化觸媒(B)及觸變減黏劑(C), 該環氧樹脂組成物(A)係包含環氧樹脂(a)與具有酚性羥基之化合物(b)的反應產物(c)者, 以170℃30分鐘硬化、在25℃浸漬於四氫呋喃1小時後的凝膠分率為90質量%以上。
- 如請求項1或2之黏接劑組成物,其中, 該反應產物(c)的數量平均分子量為該環氧樹脂(a)的數量平均分子量的1.5倍以上5.0倍以下。
- 如請求項1或2之黏接劑組成物,其中, 該反應產物(c)的數量平均分子量為550以上3000以下。
- 如請求項1或2之黏接劑組成物,其中, 該環氧樹脂(a)及該具有酚性羥基之化合物(b)的數量平均分子量皆為1000以下。
- 如請求項1或2之黏接劑組成物,其中, 該具有酚性羥基之化合物(b)所具有之酚性羥基的數目為每1分子2個。
- 如請求項1或2之黏接劑組成物,更含有氧化鈣(D)。
- 一種積層體,具有將如請求項1或2之黏接劑組成物硬化而成之黏接劑層。
- 一種黏接劑組成物之製造方法,具有下列步驟: 至少混合環氧樹脂(a)及具有酚性羥基之化合物(b),使其反應而得到環氧樹脂組成物(A); 接著至少混合環氧樹脂組成物(A)、硬化觸媒(B)及觸變減黏劑(C)。
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