TW202300619A - 熱熔黏接劑組成物及疊層體 - Google Patents
熱熔黏接劑組成物及疊層體 Download PDFInfo
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- TW202300619A TW202300619A TW111110455A TW111110455A TW202300619A TW 202300619 A TW202300619 A TW 202300619A TW 111110455 A TW111110455 A TW 111110455A TW 111110455 A TW111110455 A TW 111110455A TW 202300619 A TW202300619 A TW 202300619A
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- acid
- modified polyolefin
- copolyester
- adhesive composition
- mass
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229920001634 Copolyester Polymers 0.000 claims description 70
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Classifications
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/304—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
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Abstract
本發明之課題係提供作業性、生產性經改良,對於聚丙烯等烯烴基材具有良好的黏接性,且對於PVC、PET等高極性基材亦具有良好的黏接性,更具有優異機械特性的熱熔黏接劑組成物。一種熱熔黏接劑組成物,含有酸改性聚烯烴與共聚聚酯,並滿足下列(1)~(5)。
(1)共聚聚酯係由二羧酸成分與二醇成分構成,利用差示掃描型熱量計(DSC)獲得之熔點(T1)為80~150℃之範圍。
(2)酸改性聚烯烴之利用差示掃描型熱量計(DSC)獲得之熔點(T2)為60~150℃之範圍。
(3)|T1-T2|≦40℃。
(4)令酸改性聚烯烴之酸價為AV(eq/ton)、共聚聚酯之羥值為OHV(eq/ton)時,0.5≦AV/OHV≦4.5。
(5)令酸改性聚烯烴與共聚聚酯之合計為100質量%時,含有5~40質量%之酸改性聚烯烴,並含有60~95質量%之共聚聚酯,且令熱熔黏接劑組成物全體之合計為100質量%時,酸改性聚烯烴與共聚聚酯之合計量為70質量%以上。
Description
本發明關於熱熔黏接劑組成物及利用該熱熔黏接劑組成物進行黏接而得之疊層體。
聚丙烯(PP)、丙烯-α-烯烴共聚物等烯烴樹脂,因價格低廉、質量輕、強度、耐藥品性、耐水解性優異,而廣泛使用於以汽車、家電製品為首的各種領域。尤其近年為了提高汽車的燃油效率而強烈要求輕量化,作為金屬的替代物被廣泛研究。但是,如此的烯烴樹脂由於不具極性,對於該等成形品、薄膜難以獲得良好的黏接性。為了改善該缺點,已有人嘗試諸如利用藥劑所為之化學處理、電暈放電處理、電漿處理、火焰處理等手法對烯烴樹脂表面進行氧化處理的各種手法。但是,該等方法中,不僅需要特殊的裝置,而且黏接性、塗裝性的改良效果難謂充分。
為了以較簡便的方法賦予烯烴樹脂良好的塗裝性、黏接性,已有人開發了氯化聚烯烴、酸改性聚烯烴。通常聚烯烴不溶於溶劑,因此設計出藉由氯化、或與α-烯烴的共聚合,而使結晶性降低,並提高溶解性。又,藉由實施酸改性,結晶性亦降低,因此利用酸改性,也可獲得溶解性較良好的樹脂。但是,該等樹脂與極性樹脂的相容性低,存在難以獲得與聚氯乙烯(PVC)、聚對苯二甲酸乙二醇酯(PET)這類高極性樹脂等的良好黏接性的問題。
因此,烯烴樹脂與酯樹脂之黏接係使用環氧系黏接劑、胺甲酸酯系黏接劑。該等因藉由樹脂與硬化劑的反應形成三維交聯,而展現出優異的機械特性(例如,專利文獻1)。又,揭示有由聚酯與改性聚烯烴構成的樹脂組成物(例如,專利文獻2)。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本特開平4-323292號公報
[專利文獻2]日本特開平5-86239號公報
[發明所欲解決之課題]
但是,專利文獻1的黏接劑通常為由樹脂與硬化劑構成的二液型者,其問題可列舉使用前需進行正確的稱量、混合,作業性差。另外,混合後為了於短時間進行凝膠化,可使用時間為約數十分鐘~數小時之短,不適合使用點膠機等的自動塗布,存在需丟棄剩餘分的問題。另外,硬化需要數十分鐘~數小時的時間,故生產性低也成為問題。又,專利文獻2的樹脂組成物,由於使用具有醯胺鍵的聚酯,存在因聚酯之醯胺鍵彼此的氫鍵、醯胺鍵與改性聚烯烴的氫鍵,而導致熔融黏度顯著增加,黏接性也降低的問題。
本發明之課題係提供前述作業性、生產性經改良,對於聚丙烯等烯烴基材具有良好的黏接性,且對於PVC、PET等高極性基材也具有良好的黏接性,更具有優異機械特性的熱熔黏接劑組成物。
[解決課題之手段]
為了達成上述目的,本案發明人等進行努力研究,提出了下列發明。亦即,本發明係關於以下所示之熱熔黏接劑組成物、及使用了該熱熔黏接劑組成物的疊層體。
一種熱熔黏接劑組成物,含有酸改性聚烯烴與共聚聚酯,並滿足下列(1)~(5)。
(1)共聚聚酯係由二羧酸成分與二醇成分構成,利用差示掃描型熱量計(DSC)獲得之熔點(T1)為80~150℃之範圍。
(2)酸改性聚烯烴之利用差示掃描型熱量計(DSC)獲得之熔點(T2)為60~150℃之範圍。
(3)|T1-T2|≦40℃。
(4)令酸改性聚烯烴之酸價為AV(eq/ton)、共聚聚酯之羥值為OHV(eq/ton)時,0.5≦AV/OHV≦4.5。
(5)令酸改性聚烯烴與共聚聚酯之合計為100質量%時,含有5~40質量%之酸改性聚烯烴,並含有60~95質量%之共聚聚酯,且令熱熔黏接劑組成物全體之合計為100質量%時,酸改性聚烯烴與共聚聚酯之合計量為70質量%以上。
前述酸改性聚烯烴樹脂宜為馬來酸酐改性聚烯烴。
又,共聚聚酯之多元羧酸成分宜包含芳香族二羧酸及脂肪族二羧酸之兩者,伸烷二醇成分為飽和脂肪族二醇較佳。
一種疊層體,係利用上述記載之熱熔黏接劑組成物進行黏接而成的聚氯乙烯基材與聚烯烴基材之疊層體。
[發明之效果]
本發明之熱熔黏接劑組成物,藉由以特定量使用特定的共聚聚酯及酸改性聚烯烴,兼具非極性成分及極性成分之兩者,因此在聚丙烯等烯烴基材與PVC、PET等極性基材之異種基材間具有良好的黏接性。
以下詳述本發明。本發明之熱熔黏接劑組成物含有酸改性聚烯烴與共聚聚酯,並需滿足下列(1)~(5)。
<滿足(1)之熱熔黏接劑組成物>
針對(1)進行說明。本發明之熱熔黏接劑組成物中使用之共聚聚酯,係由二羧酸成分與二醇成分構成,且利用差示掃描型熱量計(DSC)獲得之熔點(T1)為80~150℃之範圍。宜為90~120℃,更佳為95~115℃。T1為80℃以上的情況下,會有熱熔黏接劑組成物之耐熱性變得良好的傾向。T1超過150℃的情況下,使熱熔黏接劑組成物熔融時,需施加更多的熱量,故會對經濟性及環境造成不良影響。
<滿足(2)之熱熔黏接劑組成物>
針對(2)進行說明。本發明中使用之酸改性聚烯烴之利用差示掃描型熱量計(DSC)獲得之熔點(T2)為60~150℃之範圍。宜為65~125℃,更佳為70~110℃。T2為60℃以下的情況下,熱熔黏接劑組成物之耐熱性降低。T2為150℃以上的情況下,使熱熔黏接劑組成物熔融時,需施加更多的熱量,故會對經濟性及環境造成不良影響。
<滿足(3)之熱熔黏接劑組成物>
針對(3)進行說明。本發明中使用之熱熔黏接劑組成物係|T1-T2|≦40(℃)。宜為|T1-T2|≦30(℃),更佳為|T1-T2|≦20(℃)。|T1-T2|超過40℃的情況下,利用加熱進行黏接時,僅低熔點成分會先融化,從而會有與極性基材之黏接強度降低的情況。
<滿足(4)之熱熔黏接劑組成物>
針對(4)進行說明。令構成本發明之熱熔黏接劑組成物的酸改性聚烯烴之酸價為AV(eq/ton)、共聚聚酯之羥值為OHV(eq/ton)時,為0.5≦AV/OHV≦4.5。宜為0.8≦AV/OHV≦3.5,更佳為1.0≦AV/OHV≦3.0。0.5>AV/OHV時,聚酯中之羥基相對於酸改性聚烯烴中之酸的比率變小,導致氫鍵變弱,熔融黏度變低。熔融黏度變低的話,利用熔融混練製作熱熔黏接劑組成物時,不會施加剪切力,酸改性聚烯烴與聚酯不會成為良好的分散狀態,與基材之黏接力降低。藉由為AV/OHV≦4.5,熱熔黏接劑組成物之熔融黏度不會變得過高,對於基材之潤濕性良好,尤其與聚氯乙烯(PVC)之黏接力變得良好。
<滿足(5)之熱熔黏接劑組成物>
針對(5)進行說明。本發明之熱熔黏接劑組成物,令酸改性聚烯烴與共聚聚酯之合計為100質量%時,含有5~40質量%之酸改性聚烯烴,並含有60~95質量%之共聚聚酯。宜含有20~40質量%之酸改性聚烯烴,並含有60~80質量%之共聚聚酯。更佳為含有25~35質量%之酸改性聚烯烴,並含有65~75質量%之共聚聚酯。上述之範圍以外之組成的話,在對於異種基材之黏接中,會失去極性的平衡,故無法獲得對於兩基材的良好黏接力。又,酸改性聚烯烴與共聚聚酯之組成滿足上述範圍且令熱熔黏接劑組成物全體之合計為100質量%時,酸改性聚烯烴與共聚聚酯之合計量需為70質量%以上。宜為80質量%以上,更佳為90質量%以上。
<酸改性聚烯烴>
作為本發明中使用之酸改性聚烯烴之原料的被酸改性聚烯烴,可列舉:聚乙烯、聚丙烯、乙烯-丙烯共聚物、丙烯-丁烯共聚物、乙烯-丙烯-丁烯共聚物等。其中,為選自由聚丙烯、乙烯-丙烯共聚物、及乙烯-丙烯-丁烯共聚物構成之群組中之1種以上(以下,亦稱為丙烯系聚合物。)時,就耐熱性、與共聚聚酯之相容性的觀點係較理想。丙烯系聚合物中之丙烯成分宜為50莫耳%以上,為70莫耳%以上更佳。又,被酸改性聚烯烴可使用(甲基)丙烯酸酯、(甲基)丙烯酸等不飽和酸及不飽和酸之烷基酯、乙酸乙烯酯、乙烯、丙烯及α-烯烴共聚合而成者。
本發明中使用之酸改性聚烯烴,宜為將選自由碳數3~10之不飽和羧酸、其酸酐及其酯構成之群組中之至少1種進行接枝聚合(以下,亦稱為酸改性。)而得者。接枝鏈相對於酸改性聚烯烴全體的重量(以下,亦稱為酸改性量。)宜為0.5~10質量%。更佳為0.7~3質量%。接枝鏈的重量分率落在上述範圍外的話,會有與聚烯烴基材之黏接性降低的情況。
作為碳數3~10之不飽和羧酸、其酸酐及其酯,例如可列舉:丙烯酸、甲基丙烯酸、馬來酸、富馬酸、伊康酸、檸康酸等不飽和羧酸;馬來酸酐、伊康酸酐、檸康酸酐等不飽和羧酸的酸酐;丙烯酸甲酯、甲基丙烯酸甲酯、馬來酸二甲酯等不飽和羧酸之烷基酯。該等之中,宜為馬來酸、伊康酸及它們的酸酐。
製造本發明中之酸改性聚烯烴時之接枝聚合可利用習知的方法實施,其方法並無特別限定。例如,可於前述聚烯烴與前述不飽和羧酸成分的熔融混合物中,添加有機過氧化物而進行。或可於將前述聚烯烴與前述不飽和羧酸成分溶解於甲苯、二甲苯等溶劑而得的混合物溶液中,添加有機過氧化物而進行。進行接枝聚合時,宜避免空氣及氧的混入,在氮氣等鈍性氣體環境下進行較佳。作為前述有機過氧化物之示例,可列舉:過氧化乙醯基環己基磺醯、過氧化苯甲醯、過氧化二氯苯甲醯、過氧化二異丙苯、二第三丁基過氧化物、過氧化月桂醯等,該等可使用1種或倂用2種以上。
酸改性聚烯烴於190℃之熔融黏度宜為1,000~20,000mPa・s,更佳為2,000~15,000mPa・s,尤佳為3,000~13,000mPa・s。熔融黏度為1,000mPa・s以下的話,由於凝聚力變低,對於基材之黏接強度降低,為20,000mPa・s以上的話,基材之密接性降低。另外,共聚聚酯於190℃之熔融黏度宜為220,000mPa・s以下,為200,000mPa・s以下更佳。為220,000mPa・s以上的話,對於基材之密接性降低。
酸改性聚烯烴之熔點T1宜為60℃以上,更佳為65℃以上,尤佳為70℃以上。又,宜為150℃以下,更佳為140℃以下,尤佳為130℃以下。酸改性聚烯烴之熔點未達60℃的情況下,會有因使用環境之溫度上升而導致黏接性顯著降低之虞,超過150℃的情況下,黏接時會有烯烴基材融化之虞。另外,令共聚聚酯之熔點為T2時,宜為|T1-T2|≦40(℃)。|T1-T2|超過40℃的情況下,利用加熱進行黏接時,僅低熔點成分會先融化,從而會有與極性基材之黏接強度降低的情況。
酸改性聚烯烴之重量平均分子量(Mw)宜為30,000~120,000,更佳為40,000~110,000,尤佳為50,000~100,000。又,數量平均分子量(Mn)宜為10,000~70,000,更佳為15,000~60,000,尤佳為20,000~55,000。另外,分子量分布(Mw/Mn)宜為3以下,更佳為2.8以下。藉由使用上述範圍的酸改性聚烯烴,與共聚聚酯之相容性得到改善,熱熔黏接劑組成物之黏接性會變良好。
酸改性聚烯烴之AV宜為50~500,更佳為100~400,尤佳為150~300。50>AV的話,由於酸改性聚烯烴對於聚烯烴基材之密接力低,黏接力降低。500<AV的話,酸改性聚烯烴之凝聚力變小,黏接力降低。
<共聚聚酯>
本發明中使用之共聚聚酯,例如可藉由將二羧酸或其酐、烷基酯等二羧酸成分與二醇成分進行脫水縮合或脫醇縮合而獲得。
作為形成前述二羧酸成分的化合物,可列舉:對苯二甲酸、間苯二甲酸、鄰苯二甲酸、1,2-萘二甲酸、1,6-萘二甲酸等芳香族二元酸、或琥珀酸、己二酸、壬二酸、癸二酸、十二烷酸、二聚酸、氫化二聚酸、十二烯基琥珀酸酐、富馬酸、十二烷二酸、1,2-環己烷二甲酸、1,4-環己烷二甲酸、4-甲基-1,2-環己烷二甲酸、六氫鄰苯二甲酸酐、四氫鄰苯二甲酸酐等、馬來酸、馬來酸酐、伊康酸、檸康酸等脂肪族二羧酸、脂環族二羧酸。
令全部二羧酸成分為100莫耳%時,宜含有40莫耳%以上之芳香族二羧酸,為45莫耳%以上更佳,為50莫耳%以上尤佳。上限並無特別限定,為100莫耳%亦無妨,但宜為95莫耳%以下,為90莫耳%以下更佳。脂肪族二羧酸及脂環族二羧酸之含量宜為60莫耳%以下,為55莫耳%以下更佳,為50莫耳%以下尤佳。芳香族二羧酸過少,或脂肪族二羧酸及脂環族二羧酸過多的話,會有熱熔黏接劑組成物之黏接性及耐熱性降低的情況。
共聚聚酯之OHV宜為20~200。更佳為30~170,尤佳為50~150。30>OHV的話,與酸改性聚烯烴之交互作用變小,進行熔融混練時會分散不良。150<OHV的話,貼合黏接劑層時與聚烯烴基材之密接性降低。
作為其他二醇成分,可列舉:乙二醇、二乙二醇、三乙二醇、1,2-丙二醇、1,3-丙二醇、1,2-丁二醇、1,3-丁二醇、2,3-丁二醇、1,4-丁二醇、2-甲基-1,3-丙二醇、新戊二醇、1,6-六亞甲基二醇、3-甲基-1,5-戊二醇、2,2,4-三甲基-1,3-戊二醇、2,4-二乙基-1,5-戊二醇、2-乙基-1,3-己二醇、2,2-二甲基-3-羥基丙基-2’,2’-二甲基-3’-羥基丙酸酯、2-(正丁基)-2-乙基-1,3-丙二醇、3-乙基-1,5-戊二醇、3-丙基-1,5-戊二醇、2,2-二乙基-1,3-丙二醇、3-辛基-1,5-戊二醇等脂肪族二醇類;1,3-雙(羥基甲基)環己烷、1,4-雙(羥基甲基)環己烷、1,4-雙(羥基乙基)環己烷、1,4-雙(羥基丙基)環己烷、1,4-雙(羥基甲氧基)環己烷、1,4-雙(羥基乙氧基)環己烷、2,2-雙(4-羥基甲氧基環己基)丙烷、2,2-雙(4-羥基乙氧基環己基)丙烷、雙(4-羥基環己基)甲烷、2,2-雙(4-羥基環己基)丙烷、3(4),8(9)-三環[5.2.1.02,6]癸烷二甲醇等脂環族二醇類;或雙酚A之環氧乙烷加成物、環氧丙烷加成物等芳香族系二醇類;或聚乙二醇、聚丙二醇、聚三亞甲基二醇等。該等可使用1種或倂用2種以上。
另外,本發明中使用之共聚聚酯中,也可將前述二羧酸成分之一部分置換為3官能以上之羧酸,或將前述二醇成分之一部分置換為3官能以上之多元醇並進行共聚合。作為該等3官能以上之化合物,可列舉:偏苯三甲酸、均苯四甲酸、二苯甲酮四甲酸、聯苯四甲酸、乙二醇雙(脫水偏苯三甲酸酯)、甘油參(脫水偏苯三甲酸酯)等多元羧酸等或它們的酸酐;三羥甲基丙烷、新戊四醇、甘油、聚甘油等多官能二醇。
另外,本發明中使用之共聚聚酯中,也可進行乙醇酸、內酯類、乳酸交酯類、(聚)碳酸酯類的共聚合、後加成、或酸酐的後加成、乙醇酸的共聚合。
本發明中使用之共聚聚酯,宜為主鏈中不含醯胺鍵者。共聚聚酯之主鏈中之醯胺鍵量,宜為共聚聚酯每100g中未達5×10
-4莫耳較理想。更佳為1×10
-4莫耳以下,尤佳為1×10
-5莫耳以下。含有5×10
-4莫耳以上之醯胺鍵時,會有因共聚聚酯中之醯胺鍵彼此的氫鍵、醯胺鍵與酸改性聚烯烴之酸改性部的氫鍵,而導致熔融黏度顯著增加,黏接性降低之虞。
共聚聚酯於190℃之熔融黏度宜為220,000mPa・s以下,為200,000mPa・s以下更佳。為220,000mPa・s以下的話,對於基材之密接性良好。
共聚聚酯之熔點T2宜為80℃以上,更佳為85℃以上,尤佳為90℃以上。又,宜為150℃以下,更佳為130℃以下,尤佳為120℃以下。T2未達80℃的情況下,會有因使用環境之溫度上升而導致黏接性顯著降低之虞,超過150℃的情況下,黏接時會有烯烴基材融化之虞。
共聚聚酯可為結晶性共聚聚酯,也可為非晶性共聚聚酯,宜為結晶性共聚聚酯。為結晶性共聚聚酯的話,可期待因結晶化所致之樹脂強度改善導致黏接強度得到改善。
又,本發明之熱熔黏接劑組成物中,宜加入抗氧化劑。理想的抗氧化劑可列舉:受阻酚系抗氧化劑、磷系抗氧化劑、硫系抗氧化劑、胺系抗氧化劑等,該等可使用1種或倂用2種以上。尤其倂用受阻酚系抗氧化劑與其他抗氧化劑係有效。又,添加抗熱老化劑、銅害防止劑、抗靜電劑、耐光穩定劑、紫外線吸收劑等穩定劑較理想。尤其使用分子內含有磷原子的苯酚系抗氧化劑的話,就可有效地捕捉自由基的觀點係較理想。另外,亦可添加結晶成核劑、阻燃劑等。
作為受阻酚系抗氧化劑、穩定劑,可列舉:1,3,5-參(3,5-二第三丁基-4-羥基苄基)異氰尿酸酯、1,1,3-三(4-羥基-2-甲基-5-第三丁基苯基)丁烷、1,1-雙(3-第三丁基-6-甲基-4-羥基苯基)丁烷、3,5-雙(1,1-二甲基乙基)-4-羥基-苯丙酸、新戊四醇肆[3-(3,5-二第三丁基-4-羥基苯基)丙酸酯]、3-(1,1-二甲基乙基)-4-羥基-5-甲基-苯丙酸、3,9-雙[1,1-二甲基-2-[(3-第三丁基-4-羥基-5-甲基苯基)丙醯氧基]乙基]-2,4,8,10-四氧雜螺[5.5]十一烷、1,3,5-三甲基-2,4,6-參(3’,5’-二第三丁基-4’-羥基苄基)苯、硫代二伸乙基雙[3-(3,5-二第三丁基-4-羥基苯基)丙酸酯]、十八烷基-3-(3,5-二第三丁基-4-羥基苯基)丙酸酯、N,N’-己烷-1,6二基雙[3-(3,5-二第三丁基-4-羥基苯基丙醯胺)、3,3’,3”,5,5’,5”-六第三丁基-a,a’,a”-(均三甲苯-2,4,6-三基)三-對甲酚、二乙基[[3,5-雙[1,1-二甲基乙基]-4-羥基苯基]甲基]磷酸酯、4,4’-亞丁基雙(3-甲基-6-第三丁基苯酚)、2’,3-雙[[3-[3,5-二第三丁基-4-羥基苯基]丙醯基]]丙醯肼、3,9-雙{2-[3-(3-第三丁基-4-羥基-5-甲基苯基)丙醯氧基]-1,1-二甲基乙基}-2,4-8,10-四氧雜螺[5・5]十一烷等。
作為磷系抗氧化劑、穩定劑,可列舉:3,9-雙(對壬基苯氧基)-2,4,8,10-四氧雜-3,9-二磷雜螺[5.5]十一烷、3,9-雙(十八烷氧基)-2,4,8,10-四氧雜-3,9-二磷雜螺[5.5]十一烷、亞磷酸三(單壬基苯基)酯、三苯氧基膦、亞磷酸異癸酯、亞磷酸異癸基苯基酯、亞磷酸二苯基2-乙基己基酯、亞磷酸二壬基苯基雙(壬基苯基)酯、1,1,3-參(2-甲基-4-二(十三烷基)亞磷酸酯-5-第三丁基苯基)丁烷、亞磷酸參(2,4-二第三丁基苯基)酯、新戊四醇雙(2,4-二第三丁基苯基亞磷酸酯)、2,2’-亞甲基雙(4,6-二第三丁基苯基)2-乙基己基亞磷酸酯、雙(2,6-二第三丁基-4-甲基苯基)新戊四醇二亞磷酸酯、亞磷酸雙[2,4-雙[1,1-二甲基乙基]-6-甲基苯基]乙基酯、6-[3-(3-第三丁基-4-羥基-5-甲基)丙氧基]-2,4,8,10-四第三丁基二苯并[d,f][1,3,2]-二噁磷環庚烷、肆(2,4-二第三丁基苯基)[1,1-聯苯]-4,4’-二基雙亞膦酸酯、雙(2,4-二第三丁基苯基)新戊四醇二亞磷酸酯等。
作為硫系抗氧化劑、穩定劑,可列舉:4,4’-硫代雙[2-第三丁基-5-甲基苯酚]雙[3-(十二烷基硫基)丙酸酯]、硫代雙[2-(1,1-二甲基乙基)-5-甲基-4,1-伸苯基]雙[3-(十四烷基硫基)-丙酸酯]、新戊四醇肆(3-正十二烷基硫基丙酸酯)、硫代二丙酸雙(十三烷基)酯、3,3’-硫代二丙酸二(十二烷基)酯、3,3’-硫代二丙酸二(十八烷基)酯、4,6-雙(辛基硫甲基)-鄰甲酚、4,4-硫代雙(3-甲基-6-第三丁基苯酚)等。
作為胺系抗氧化劑、穩定劑,可列舉:4,4’-雙(α,α-二甲基苄基)二苯胺、2’,3-雙[[3-[3,5-二第三丁基-4-羥基苯基]丙醯基]]丙醯肼、N,N’-二-2萘基-對苯二胺、N-苯基-N’-4,4’-硫代雙(2-第三丁基-5-甲基苯酚)、2,2-雙[3-(十二烷基硫基)丙醯氧基甲基]-1,3-丙二醇雙[3-(十二烷基硫基)丙酸酯]等。
抗氧化劑的添加量,相對於熱熔黏接劑組成物全體宜為0.1質量%以上且5質量%以下。未達0.1質量%的話,會有防止熱劣化的效果變差的情況。超過5質量%的話,會有對黏接性等造成不良影響的情況。
本發明之熱熔黏接劑組成物中,在不損及本發明之性能的範圍內,也可摻合環氧樹脂、聚醯胺樹脂、聚烯烴樹脂、聚碳酸酯樹脂、丙烯酸樹脂、乙烯乙酸乙烯酯樹脂、酚醛樹脂等其他樹脂,會有黏接性、柔軟性、耐久性等得到改良的情況。其他樹脂的摻合量亦未達熱熔黏接劑組成物全體的5質量%較理想。又,亦可摻合異氰酸酯化合物、三聚氰胺等硬化劑、滑石、雲母等填充材、碳黑、氧化鈦等顏料、三氧化銻、溴化聚苯乙烯等阻燃劑。
本發明之熱熔黏接劑組成物中,可摻合松香、萜烯等增黏劑,會有黏接性得到改善的情況。摻合量宜未達熱熔黏接劑組成物全體的5質量%較理想。
就製作本發明之熱熔黏接劑組成物的方法而言,並無特別限定,例如可列舉:利用單軸擠壓機、雙軸擠壓機等擠壓機進行熔融混練的方法、進行丸粒摻配並利用成形機等進行熔融混練而直接獲得成形品的方法、或在共聚聚酯之聚合時投入酸改性聚烯烴並進行混合的方法、在溶液中將兩者予以摻配的方法等,為使用了可施加高剪切應力的雙軸擠壓機的方法特佳。使用雙軸擠壓機時,宜於比所使用之酸改性聚烯烴、共聚聚酯之熔點更高的溫度進行熔融混練,具體而言,於150~300℃進行熔融混練較佳。
<基材>
就本發明中使用之極性基材而言,可使用聚對苯二甲酸乙二醇酯(PET)、聚氯乙烯(PVC)等基材。又,聚烯烴基材並無特別限定,可使用聚乙烯(PE)、聚丙烯(PP)等基材。其中,宜為PVC與PP的組合。
<疊層體>
本發明之疊層體,係利用熱熔黏接劑組成物將極性基材與聚烯烴基材予以疊層而成的3層疊層體(極性基材/熱熔黏接劑組成物層/聚烯烴基材)。疊層體例如可藉由於聚酯基材(或聚烯烴基材)疊層或塗布熱熔黏接劑組成物,進一步以聚烯烴基材(或聚酯基材)夾持,並進行熱壓接而製作。疊層體中之熱熔黏接劑組成物層的厚度宜為5~200μm,更佳為10~100μm,尤佳為15~50μm。厚度過薄的話,會有無法充分獲得黏接性能的情況,過厚的話,會有生產性降低的情況。
[實施例]
以下,舉實施例針對本發明進行更詳細地說明。惟,本發明不限定於實施例。此外,實施例及比較例中的簡稱份表示質量份,%表示質量%。
<<樹脂及熱熔黏接劑組成物的評價方法>>
<組成比>
將樣品(共聚聚酯或酸改性聚烯烴)溶解於氘代氯仿中,使用Varian公司製核磁共振分析計(NMR)Gemini-200進行1H-NMR分析來決定。
<酸改性聚烯烴之酸價(AV)>
本發明中之酸改性聚烯烴之酸價(eq/ton),係使用FT-IR(島津製作所公司製、FT-IR8200PC),並利用馬來酸酐之羰基(C=O)鍵之伸縮峰部(1780cm
-1)的吸光度(I)、同排聚合物所特有之峰部(840cm
-1)的吸光度(II)、及由馬來酸酐(東京化成製)之氯仿溶液所製作之檢量線獲得的係數(f)根據下式算出,該算出的值以樹脂1ton中之當量(eq/ton)表示。
酸價=[吸光度(I)/吸光度(II)×(f)/馬來酸酐之分子量×2×10
4]
馬來酸酐之分子量:98.06
<共聚聚酯之羥值(OHV)>
本發明中之共聚聚酯之羥值係如下述般求出。將共聚聚酯:50g溶解於熱氯仿:120g中,加入4,4’-二苯基甲烷二異氰酸酯:70g,於70℃反應2小時。然後,利用滴定對反應液中之殘存異氰酸酯基濃度進行定量,求出羥值(eq/ton)。
<熔融黏度>
利用島津製作所製流動性測定儀(flow tester)(CFT-500C型),將已乾燥至水分率0.1%以下之樹脂試樣(共聚聚酯或酸改性聚烯烴)填充到設定為190℃之加熱體中央之缸體中。填充經過3分鐘後,藉由柱塞對試樣施加壓力(4.9MPa),從缸體底部之模具(孔徑:0.5mm、厚度:20mm)將已熔融的試樣擠壓出,記錄柱塞的下降距離與下降時間,算出熔融黏度(mPa・s)。
<重量平均分子量(Mw)、數量平均分子量(Mn)>
本發明中之Mw及Mn,係利用日本Waters公司製凝膠滲透層析儀Alliance e2695(以下,亦稱為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))測得之值。
<熔點>
利用精工電子工業(股)公司製的差示掃描熱量分析計「DSC220型」,將測定試樣(共聚聚酯或酸改性聚烯烴)5mg放入鋁盤,加蓋並予以密封,先在250℃保持5分鐘,使試樣完全熔融後,利用液態氮快速冷卻,之後以20℃/min之升溫速度從-150℃到250℃進行測定。由獲得之熱譜曲線(thermogram curve)求出熔解熱的最大吸熱峰部作為熔點。
<熱熔黏接劑組成物之片狀樣品的製作>
使用Tester Sangyo(股)公司製桌上型測試加壓機(Tabletop Test Press)SA-302,以160℃、保持壓力20MPa、保持壓力時間10秒之條件,成形厚度20μm之熱熔黏接劑組成物之片狀樣品。
<黏接強度評價>
以C.I. TAKIRON(股)公司製PVC薄膜(BONLEX BE、50μm厚)與Nippon Testpanel(股)公司製聚丙烯板(2.5mm厚)夾持片狀樣品,並使用井元製作所(股)公司熱封試驗機IMC-0800,以140℃、保持壓力0.1MPa之條件進行120秒壓力保持,藉此成形黏接強度測定用樣品。將前述黏接強度測定用樣品裁切成10mm寬,於島津製作所(股)公司製拉伸試驗機之上部夾頭夾持黏接強度測定用樣品的PVC薄膜,並於下部夾頭夾持聚丙烯板,在23℃、60%Rh之環境下使用Autograph AGX-V以拉伸速度50mm/分鐘進行上下拉伸,藉此測定180°剝離黏接強度。評價係由測定值與綜合評價進行。
(綜合評價)
○:熱熔黏接劑組成物凝聚破壞,且剝離強度為15N/10mm以上。
△:(1)熱熔黏接劑組成物在聚丙烯板或PVC薄膜界面剝離,且剝離強度為10N/10mm以上;或(2)熱熔黏接劑組成物凝聚破壞,且剝離強度為10N/10mm以上且未達15N/10mm之範圍。
×:剝離強度未達10N/10mm。
<<製造例及實施例>>
酸改性聚烯烴(a)之製造例
將結晶性聚丙烯(聚烯烴樹脂1)100質量份、馬來酸酐8質量份、過氧化二異丙苯2質量份及甲苯150質量份,投入安裝有攪拌機之高壓釜中,密閉後進行5分鐘氮氣置換。之後,邊加熱攪拌邊於140℃反應5小時。反應結束後,將反應液投入至大量的甲乙酮中,使樹脂析出。將析出的樹脂取出,進一步以甲乙酮清洗數次後乾燥,得到酸改性聚烯烴(a)。組成及特性示於表1。
酸改性聚烯烴(b)~(e)之製造例
與上述酸改性聚烯烴(a)同樣進行,變更被改性聚烯烴樹脂的種類,藉此得到酸改性聚烯烴(b)~(e)。各酸改性聚烯烴之組成及特性示於表1。
[表1]
聚烯烴樹脂1:丙烯-丁烯(=70/30(莫耳比))共聚物(重量平均分子量230,000)
聚烯烴樹脂2:丙烯-丁烯(=90/10(莫耳比))共聚物(重量平均分子量180,000)
聚烯烴樹脂3:丙烯-乙烯-丁烯(=70/10/20(莫耳比))共聚物(重量平均分子量170,000)
酸改性聚烯烴 | a | b | c | d | e | |
樹脂製造時之進料組成(質量份) | 聚烯烴樹脂1 | 100 | 100 | |||
聚烯烴樹脂2 | 100 | |||||
聚烯烴樹脂3 | 100 | 100 | ||||
馬來酸酐 | 8 | 6 | 8 | 15 | 20 | |
過氧化二異丙苯 | 2 | 2 | 2 | 2 | 2 | |
樹脂特性 | 酸加成量(eq/ton) | 200 | 160 | 220 | 300 | 400 |
熔融黏度(mPa・s@190℃) | 6000 | 10000 | 6000 | 5000 | 4000 | |
熔點(℃) | 70 | 70 | 90 | 125 | 125 |
共聚聚酯(A)之製造例
在裝設有攪拌機、溫度計、餾出用冷卻器之反應槽內,加入對苯二甲酸30質量份、間苯二甲酸20質量份、己二酸50質量份、1,4-丁二醇100質量份、鈦酸四丁酯0.25質量份,於170~220℃進行2小時酯化反應。酯化反應結束後,投入受阻酚系抗氧化劑「IRGANOX(註冊商標)1330」(BASF Japan(股)公司製)0.5質量份,升溫至255℃,另一方面,將系內緩慢減壓,歷時60分鐘成為255℃且665Pa。進一步,於133Pa以下進行30分鐘縮聚反應,得到聚酯樹脂(A)。該聚酯樹脂(A)之熔點為110℃,於190℃之熔融黏度為180,000mPa・s。
共聚聚酯(B)~(D)之製造例
與共聚聚酯(A)同樣進行,變更二羧酸成分、二醇成分,藉此得到共聚聚酯樹脂(B)~(D)。各樹脂之特性示於表2。
[表2]
TPA:對苯二甲酸
IPA:間苯二甲酸
AA:己二酸
EG:乙二醇
BD:1,4-丁二醇
PTMG1000:聚四亞甲基二醇(數量平均分子量1000)
共聚聚酯 | A | B | C | D | ||
組成莫耳% | 二羧酸成分 | TPA | 30 | 60 | 65 | 50 |
IPA | 20 | 35 | 40 | |||
AA | 50 | 40 | 10 | |||
二醇成分 | EG | 40 | ||||
BD | 100 | 59 | 80 | 100 | ||
PTMG1000 | 1 | 20 | ||||
樹脂特性 | OHV(eq/ton) | 70 | 80 | 100 | 100 | |
熔融黏度(mPa・s@190℃) | 180000 | 160000 | 200000 | 210000 | ||
熔點(℃) | 110 | 90 | 125 | 130 |
實施例1
熱熔黏接劑組成物(1)
加入作為酸改性聚烯烴之上述酸改性聚烯烴(a)30質量份、作為共聚聚酯之上述共聚聚酯(A)70質量份,使用雙軸擠壓機於190℃進行熔融混練,藉此得到熱熔黏接劑組成物(1)。利用前述方法測定黏接強度,結果為20N/cm。組成及特性示於表3。
實施例2~9、比較例1~8
熱熔黏接劑組成物之製造例2~17
依表3、4之組合,與製造例1同樣進行,得到熱熔黏接劑組成物2~17。利用前述方法測定黏接強度。組成及特性示於表3、4。
[表3]
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 | 實施例8 | 實施例9 | ||
熱熔黏接劑組成物 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | |
組成物摻合(質量份) | 共聚聚酯(A) | 70 | 90 | 60 | 70 | 70 | 70 | |||
共聚聚酯(B) | 70 | |||||||||
共聚聚酯(C) | 70 | |||||||||
共聚聚酯(D) | 70 | |||||||||
酸改性聚烯烴(a) | 30 | 10 | 40 | 30 | ||||||
酸改性聚烯烴(b) | 30 | |||||||||
酸改性聚烯烴(c) | 30 | |||||||||
酸改性聚烯烴(d) | 30 | 30 | ||||||||
酸改性聚烯烴(e) | 30 | |||||||||
組成物物性 | AV/OHV | 2.9 | 2.9 | 2.9 | 2.3 | 3.1 | 4.3 | 2.5 | 3.0 | 4.0 |
|T1-T2| | 40 | 40 | 40 | 40 | 20 | 15 | 20 | 0 | 5 | |
黏接強度(N/10mm) | 20 | 16 | 16 | 22 | 23 | 22 | 19 | 29 | 31 | |
剝離方式 | 凝聚破壞 | 界面剝離 | 界面剝離 | 凝聚破壞 | 界面剝離 | 界面剝離 | 凝聚破壞 | 界面剝離 | 界面剝離 | |
綜合評價 | 〇 | △ | △ | 〇 | △ | △ | 〇 | △ | △ |
[表4]
未改性聚烯烴:J-700GP(Prime Polymer(股)公司製均聚聚丙烯)
比較例1 | 比較例2 | 比較例3 | 比較例4 | 比較例5 | 比較例6 | 比較例7 | 比較例8 | ||
熱熔黏接劑組成物 | 10 | 11 | 12 | 13 | 14 | 15 | 16 | 17 | |
組成物摻合(質量份) | 共聚聚酯(A) | 98 | 50 | 70 | 100 | 70 | 35 | ||
共聚聚酯(B) | |||||||||
共聚聚酯(C) | |||||||||
共聚聚酯(D) | 70 | ||||||||
酸改性聚烯烴(a) | 2 | 50 | 30 | 100 | 15 | ||||
酸改性聚烯烴(b) | |||||||||
酸改性聚烯烴(c) | |||||||||
酸改性聚烯烴(d) | |||||||||
酸改性聚烯烴(e) | 30 | ||||||||
未改性聚烯烴 | 30 | 50 | |||||||
組成物物性 | AV/OHV | 2.9 | 2.9 | 5.7 | 2 | - | - | - | 2.9 |
|T1-T2| | 40 | 40 | 15 | 60 | - | - | - | 40 | |
黏接強度(N/10mm) | 0.4 | 5.5 | 4.7 | 6.1 | 0.3 | 0.2 | 0.3 | 3.3 | |
剝離方式 | 界面剝離 | 界面剝離 | 凝聚破壞 | 界面剝離 | 界面剝離 | 界面剝離 | 界面剝離 | 凝聚破壞 | |
綜合評價 | × | × | × | × | × | × | × | × |
實施例1~9符合發明申請專利範圍,黏接強度也良好。比較例1中,含有超過95質量%之共聚聚酯,因此落在本發明之範圍外,對於PP薄膜之黏接性低。比較例2中,含有超過50質量%之酸改性聚烯烴,因此落在本發明之範圍外,對於PVC薄膜之黏接性低。比較例3中,AV/OHV為4.5以上,落在本發明之範圍外,對於PP及PVC薄膜之黏接性低。比較例4中,|T1-T2|>40,黏接層之分散不均勻,故黏接性低。比較例5中,不含酸改性聚烯烴,故對於PP之黏接性低。比較例6中,不含共聚聚酯,故對於PVC之黏接性低。比較例7中,係使用未改性的聚烯烴黏接劑替代酸改性聚烯烴,對於PP基材之黏接性低。比較例8中,令熱熔黏接劑組成物全體之合計為100質量%時,酸改性聚烯烴與共聚聚酯之合計量未達70質量%,故黏接性低。
無
Claims (4)
- 一種熱熔黏接劑組成物,含有酸改性聚烯烴與共聚聚酯,並滿足下列(1)~(5); (1)共聚聚酯係由二羧酸成分與二醇成分構成,利用差示掃描型熱量計(DSC)獲得之熔點(T1)為80~150℃之範圍; (2)酸改性聚烯烴之利用差示掃描型熱量計(DSC)獲得之熔點(T2)為60~150℃之範圍; (3)|T1-T2|≦40℃; (4)令酸改性聚烯烴之酸價為AV(eq/ton)、共聚聚酯之羥值為OHV(eq/ton)時,0.5≦AV/OHV≦4.5; (5)令酸改性聚烯烴與共聚聚酯之合計為100質量%時,含有5~40質量%之酸改性聚烯烴,且令熱熔黏接劑組成物全體之合計為100質量%時,酸改性聚烯烴與共聚聚酯之合計量為70質量%以上。
- 如請求項1之熱熔黏接劑組成物,其中,酸改性聚烯烴樹脂為馬來酸酐改性聚烯烴。
- 如請求項1或2之熱熔黏接劑組成物,其中,共聚聚酯之二羧酸成分包含芳香族二羧酸及脂肪族二羧酸之兩者,伸烷二醇成分為飽和脂肪族二醇。
- 一種疊層體,係利用如請求項1至3中任一項之熱熔黏接劑組成物進行黏接而成的聚氯乙烯基材與聚烯烴基材之疊層體。
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