CN116635230A - 涂布剂、层叠体、包装材料 - Google Patents
涂布剂、层叠体、包装材料 Download PDFInfo
- Publication number
- CN116635230A CN116635230A CN202180077177.XA CN202180077177A CN116635230A CN 116635230 A CN116635230 A CN 116635230A CN 202180077177 A CN202180077177 A CN 202180077177A CN 116635230 A CN116635230 A CN 116635230A
- Authority
- CN
- China
- Prior art keywords
- gas barrier
- coating
- coating agent
- laminate
- polyalkyleneimine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 150000001336 alkenes Chemical class 0.000 abstract description 14
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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
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Abstract
本发明提供对包括烯烃系基材的各种基材的密合性优异、用于赋予阻气性的涂布剂、使用该涂布剂而得到的阻气性优异的层叠体、包装材料。一种包含树脂(A)和水性溶剂(B)、且上述树脂(A)包含乙烯醇系聚合物(A1)和聚亚烷基亚胺(A2)的涂布剂、具有由该涂布剂形成的阻气涂层的层叠体、由该层叠体形成的包装材料。
Description
技术领域
本发明涉及涂布剂、使用该涂布剂而得到的层叠体、包装材料。
背景技术
出于防止来自外部空气的水分、氧等气体的侵入的目的,阻气性材料在各个方面中使用。例如关于食品、饮料等的包装中使用的包装材料,以保护内容物免受各种流通、冷藏等保存、加热杀菌等处理等的影响、食品长期保存为目的,要求为了抑制氧化而防止来自外部的氧的侵入的阻氧性、二氧化碳阻隔性、对各种香气成分等的阻隔性功能。另外,太阳能电池、液晶、有机或无机电致发光(以下称为“EL”)等各种显示器、以及电子纸等电子器件通常使用玻璃基板作为用于保护其内部结构、阻断来自外部的氧、水蒸气的密封材料,但出于提供薄型化、轻量化、或柔性的制品的目的,正在逐步地研究以塑料膜为基材的透明阻气性膜的使用。(例如,参照专利文献1、2)。
作为赋予塑料膜阻气性的手段,已知有涂布使用涂布剂的方法,该涂布剂使用了聚乙烯醇、乙烯乙烯醇等(专利文献3)。
现有技术文献
专利文献
专利文献1:日本特开2005-077553号公报
专利文献2:日本特开2010-253861号公报
专利文献3:日本特开2017-115076号公报
发明内容
发明要解决的课题
然而,聚乙烯醇、乙烯乙烯醇虽然阻气性优异,但对聚乙烯、聚丙烯之类的烯烃系基材的密合性极低。
用于解决课题的手段
本发明是为了解决这样的课题的至少一部分而完成的,其目的在于提供对烯烃系基材的密合性优异的阻气性涂布剂、使用该涂布剂而得到的层叠体、包装材料。
发明效果
根据本发明,能够提供对包括烯烃系基材的各种基材的密合性优异的阻气涂布剂。
具体实施方式
<涂布剂>
本发明的涂布剂包含树脂(A)和水性溶剂(B),树脂包含乙烯醇系聚合物(A1)和聚亚烷基亚胺(A2)作为必需成分。以下,对本发明的涂布剂进行详述。
(乙烯醇系聚合物(A1))
作为乙烯醇系聚合物(A1),为乙烯基酯(a1)的均聚物或共聚物的水解物(A1-1),并可以使用通过公知惯用的方法而得到的物质。或者,作为乙烯醇系聚合物(A1),为乙烯基酯(a1)的均聚物或共聚物的水解物与醛的反应产物(A1-2),并可以使用通过公知惯用的方法而得到的物质。
作为乙烯基酯(a1),可举出甲酸乙烯酯、乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、异丁酸乙烯酯、特戊酸乙烯酯、叔碳酸乙烯酯、己酸乙烯酯、辛酸乙烯酯、月桂酸乙烯酯、棕榈酸乙烯酯、硬脂酸乙烯酯、油酸乙烯酯、苯甲酸乙烯酯等,可以使用1种或组合使用2种以上。优选使用乙酸乙烯酯。
作为能够与乙烯基酯(a1)共聚的聚合性化合物(a2),可举出乙烯、丙烯、1-丁烯、异丁烯、1,3-丁二烯、乙酸异丙烯酯、乙酸2-丙烯酯、苯乙烯、α-甲基苯乙烯、氯乙烯、丙烯腈、马来酸酐、丙烯酸甲酯、甲基丙烯酸甲酯、N-乙烯基-N-甲基甲酰胺、乙烯基乙酰胺、N-乙烯基甲酰胺、N-(羟基甲基)-N-乙烯基甲酰胺丙烯酸羟基乙酯、甲基乙烯基酮和二丙酮丙烯酰胺等,可以使用1种或组合使用2种以上。其中,优选使用乙烯、乙酸异丙烯酯、乙酸2-丙烯酯。
在并用乙烯基酯(a1)和聚合性化合物(a2)的情况下,它们的使用量可适当调整,从阻气性的观点出发,优选将聚合性化合物(a2)的配合量限于乙烯基酯(a1)与聚合性化合物(a2)的总量的60摩尔%以下,更优选限于25摩尔%以下。
作为乙烯醇系聚合物(A1-1)或(A-2)的前体的乙烯基酯聚合物的聚合度没有特别限定,作为一例,为500~10000,更优选为800~6000,更优选为1000~3000。由此,能够制成阻气性与涂敷适应性的平衡优异的涂布剂。
作为缩醛化中使用的醛,可以举出甲醛、乙醛、丙醛、丁醛、辛醛、十二烷基醛等脂肪族醛;环己烷甲醛等脂环族醛;苯甲醛、萘甲醛、蒽甲醛、苯乙醛、甲苯甲醛、二甲基苯甲醛、枯茗醛、苄基醛等芳香族醛;环己烯醛、二甲基环己烯醛、丙烯醛等不饱和醛;糠醛、5-甲基糠醛等具有杂环的醛;葡萄糖、葡糖胺等半缩醛;4-氨基丁醛等具有氨基的醛等,另外,可以使用1种或组合使用2种以上的2-丙酮、甲乙酮、3-戊酮、2-己酮等脂肪族酮;环戊酮、环己酮等脂肪脂环式酮、苯乙酮、二苯甲酮等芳香族酮等。
作为缩醛化时使用的酸催化剂,可以使用乙酸、对甲苯磺酸、硝酸、硫酸、盐酸等以往公知的有机酸、无机酸。
作为乙烯醇系聚合物(A1)的适宜的具体例,可举出聚乙烯醇、乙烯乙烯醇、聚乙烯醇缩丁醛等。可以单独使用1种,也可以并用2种以上。从阻气性与密合性的平衡的观点出发,更优选使用聚乙烯醇、乙烯乙烯醇中的任一者或并用两者。
关于乙烯醇聚合物(A1-1),从阻气性优异的方面出发,皂化度优选为90%以上,优选为95%以上。也可以为100%。皂化度例如可以使用由OMNIC软件控制的Nicolet5700FTIR光谱仪并通过FTIR进行测定。
乙烯醇聚合物(A1-2)优选为将皂化度为95%以上的前体进行缩醛化而得的物质。
(聚亚烷基亚胺(A2))
聚亚烷基亚胺(A2)是具有聚亚烷基亚胺骨架的树脂,其是通过常规方法将亚烷基亚胺(例如亚乙基亚胺、亚丙基亚胺)中的1种或2种以上进行聚合而得到的。通过并用乙烯醇系聚合物(A1)和聚亚烷基亚胺(A2),能够维持涂布剂的阻气性并且提高对烯烃系基材的密合性。
聚亚烷基亚胺(A2)可以是由直链状聚亚烷基亚胺链形成的直链聚亚烷基亚胺,也可以是具有支链状聚亚烷基亚胺链的支链聚亚烷基亚胺。作为聚亚烷基亚胺(A2),例如可举出聚亚乙基亚胺、聚亚丙基亚胺。聚亚烷基亚胺(A2)可以是在聚亚烷基亚胺链的至少一部分氮原子上导入取代基(例如羟丙基、羟乙基)而成的物质。可以使用用钛酸四异丙酯、钛酸四正丁酯、钛酸丁酯二聚物、钛酸四(2-乙基己基)酯、钛酸四甲酯、多羟基硬脂酸钛、双乙酰丙酮钛、四乙酰丙酮钛、聚乙酰丙酮钛、辛二醇酸钛、乙酰乙酸乙酯合钛、乳酸钛、三乙醇胺合钛、硬脂酸钛等有机金属化合物改性而成的物质,也可以并用2种以上的聚亚烷基亚胺。
认为聚亚烷基亚胺(A2)通过氨基(NHR基、NH2基)和亚乙基而有助于提高乙烯醇系聚合物(A1)与烯烃膜的密合性,从对密合性的提高为有效的方面出发,聚亚烷基亚胺(A2)优选包含支链状聚亚烷基亚胺。聚亚烷基亚胺(A2)的支化的程度可以用聚亚烷基亚胺(A2)所具有的伯氨基、仲氨基、叔氨基的比例来表示。可根据所使用的乙烯醇系聚合物(A1)、其配合量来适当调整,作为一例,优选使用伯氨基的比例为20~40%、仲氨基的比例为30~60%、叔氨基的比例为20~35%的聚亚烷基亚胺(A2)。聚亚烷基亚胺(A2)中所含的伯胺基、仲胺基、叔胺基的比例可以利用13C-NMR光谱法进行测定。支链聚亚烷基亚胺优选为支链聚亚乙基亚胺。
从密合性优异的方面出发,聚亚烷基亚胺(A2)的数均分子量优选为5,000以上,更优选为9,000以上,进一步优选为50,000以上。对于上限没有特别限定,作为一例,为100,000以下。聚亚烷基亚胺(A2)的数均分子量是以普鲁兰多糖为标准物质并通过GPC(凝胶渗透色谱)法进行测定而得的数均分子量。
在本发明的涂布剂中,聚烷基亚胺(A2)的配合量优选为乙烯醇系聚合物(A1)与聚烷基亚胺(A2)的总量的1质量%以上且90质量%以下。由此,能够维持本发明的涂布剂的阻气性、并且更可靠地提高对烯烃系基材的密合性。更优选为10质量%以上且50质量%以下。在本发明的涂布剂不含聚亚烷基亚胺(A2)的情况下,对烯烃系基材的密合性不充分。在不含乙烯醇系聚合物(A1)的情况(树脂(A)仅由聚亚烷基亚胺(A2)形成的情况)下,涂膜具有粘合性,不适于后加工。
本发明的涂布剂可以包含除了乙烯醇系聚合物(A1)、聚烷基亚胺(A2)以外的树脂(A3)。作为这样的树脂(A3),例如可举出纤维素树脂、聚酯、聚氨酯、烯烃、苯乙烯的均聚物或共聚物等乙烯基树脂、丙烯酸类树脂、环氧树脂、酰胺树脂、天然橡胶、它们的复合体(例如核-壳型树脂)等,可以使用一种或组合使用2种以上。如果树脂(A3)的配合量过多,则有时阻气性降低,因此树脂(A3)的配合量优选限于树脂(A)(乙烯醇系聚合物(A1)、聚烷基亚胺(A2)、树脂(A3)的总量)的10质量%以下。更优选为5质量%以下,更优选为1质量%以下。也可以为0质量%。
本发明的涂布剂中的树脂(A)的配合量可根据涂敷适应性等而适当调整。
(水性溶剂(B))
作为水性溶剂(B),可以使用水、溶解于水的水溶性有机溶剂等。作为水,可以使用离子交换水、超滤水、反渗透水、蒸馏水等纯水、或超纯水。为了能够防止霉菌或细菌的产生,从长期保存的观点出发,优选使用通过紫外线照射或过氧化氢添加等进行了灭菌的水。
作为水溶性有机溶剂,例如可举出乙二醇、二乙二醇、三乙二醇、四乙二醇、丙二醇、聚乙二醇、聚丙二醇等二醇类;丁二醇、戊二醇、己二醇等二醇类;月桂酸丙二醇酯等二醇酯;二乙二醇单乙醚、二乙二醇单丁醚、二乙二醇单己醚、卡必醇等二乙二醇醚类;包含丙二醇醚、二丙二醇醚和三乙二醇醚的溶纤剂等二醇醚类;甲醇、乙醇、异丙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、丁醇、戊醇等醇类;环丁砜、酯、酮、γ-丁内酯等内酯类、N-(2-羟基乙基)吡咯烷酮等内酰胺类、甘油及其聚环氧烷加成物等作为水性有机溶剂而已知的其他各种溶剂等。这些水性有机溶剂可以单独使用或组合使用2种以上。
(添加剂(C))
本发明的涂布剂除了树脂(A)、水性溶剂(B)以外还可以进一步包含添加剂(C)。作为添加剂(C),可例示层状无机化合物、能够与乙烯醇系聚合物(A1)、聚烷基亚胺(A2)所具有的官能团反应的交联剂、无机填充剂、消泡剂、稳定剂(抗氧化剂、热稳定剂、紫外线吸收剂等)、增塑剂、抗静电剂、润滑剂、防粘连剂、着色剂、流平剂等。
作为层状无机化合物,可举出以蒙脱石等为代表的天然蒙脱土、合成蒙脱土、天然云母、合成云母、水滑石和滑石、以及对它们进行有机处理而得的亲油性处理蒙脱土和亲油性合成云母等。通过使用层状无机化合物,从而涂布剂的阻气性提高,但存在对烯烃系基材的密合性降低的倾向。层状无机化合物的配合量相对于树脂(A)100质量份为10质量份以上且100质量份以下时,阻气性与密合性的平衡优异,是优选的。
作为交联剂,可举出福尔马林、戊二醛等醛类;戊二醛的二缩醛化物等缩醛类;以六亚甲基二异氰酸酯或其衍生物(加合物、脲酸酯体、缩二脲体等)为代表的脂肪族多异氰酸酯、以苯二亚甲基二异氰酸酯或其衍生物为代表的芳香脂肪族多异氰酸酯、以甲苯二异氰酸酯或其衍生物为代表的芳香族多异氰酸酯、作为这些异氰酸酯与多元醇的反应产物的氨基甲酸酯预聚物等异氰酸酯类;环氧类;钛、硅、铝、锆、硼等与醇盐等的有机金属化合物;羟甲基脲、羟甲基三聚氰胺等羟甲基脲类;聚丙烯酸系聚合物、马来酸酐系聚合物等含羧基的聚合物类;对亚苯基-双(2,6-二甲苯基碳二亚胺)、四亚甲基-双(叔丁基碳二亚胺)、环己烷-1,4-双(亚甲基-叔丁基碳二亚胺)等碳二亚胺类;硼酸;乳酸钛等。异氰酸酯类可以使用利用了公知的封端剂而得的封端异氰酸酯,也可以使用乳液型异氰酸酯。
通过使用交联剂,从而对烯烃系基材的密合性提高,但存在阻气性降低的倾向。交联剂的配合量相对于树脂(A)100质量份为5质量份以上且50质量份以下时,阻气性与密合性的平衡优异,是优选的。
<层叠体>
本发明的层叠体是在基材上涂布本发明的涂布剂并使其干燥而得到的。需要说明的是,以下也将本发明的涂布剂的干燥涂膜简称为阻气涂层。作为能够应用本发明的涂布剂的基材,没有特别限定,可举出聚对苯二甲酸乙二醇酯(PET)膜、聚苯乙烯膜、聚酰胺膜、聚丙烯腈膜、聚乙烯膜(OPE:双轴拉伸聚乙烯膜、LLDPE:低密度聚乙烯膜、HDPE:高密度聚乙烯膜)、聚丙烯膜(CPP:未拉伸聚丙烯膜、OPP:双轴拉伸聚丙烯膜)等聚烯烃膜、聚乙烯醇膜、乙烯-乙烯醇共聚物膜等。
另外,也可以使用在这些膜上层叠铝等金属、二氧化硅、氧化铝等金属氧化物等无机蒸镀层而成的膜。作为具体的膜,可举出具有铝蒸镀层的OPP膜、PET膜、LLDPE膜、CPP膜、具有二氧化硅蒸镀层的OPP膜、PET膜、尼龙膜、具有氧化铝蒸镀层的OPP膜、PET膜、尼龙膜等。本发明的涂布剂对包括聚烯烃膜的这些基材的密合性优异,能够提高基材的阻气性、各种香味成分的保香性。
作为本发明的涂布剂的涂布方法,没有特别限定,可以使用喷涂法、旋涂法、浸渍法、辊涂法、刮涂法、刮刀辊法、刮刀法、帘式涂布法、狭缝涂布法、丝网印刷法、喷墨法、分配法、模涂(模涂布)法、直接凹版法、反向凹版法、柔版法、刮刀式涂布法、点涂法等。
阻气涂层的膜厚可根据基材的种类、目标阻气性的程度而适当调整,作为一例,为0.2μm以上且2.0μm以下。如果膜厚过薄,则不能那么期待阻气性的提高,如果过厚,则密合性有可能会降低。
也可以使用粘接剂将具有阻气涂层的层叠体进一步与其他基材贴合。或者,也可以通过挤出法在具有阻气涂层的层叠体上层叠其他基材。作为其他基材,可以使用与上述相同的基材。作为粘接剂,例如可以使用通常用于膜的粘接的双组份固化型氨基甲酸酯系的溶剂型或无溶剂型粘接剂。粘接剂优选使用固化涂膜的芳香环浓度成为0.5mmоl/g以上且7.0mmоl/g以下的粘接剂,从成为阻气性优异的层叠体的方面出发,更优选使用成为3.5mmоl/g以上且7.0mmоl/g以下的粘接剂。
粘接剂的芳香环浓度是将具有芳香环的单体在粘接剂中配合的多元醇组合物、多异氰酸酯组合物的合成中使用的单体的总当量(X)中所占的总当量(Y)除以粘接剂的固体成分总质量(Z)而得的值。在使用一分子中具有x个芳香环的单体(y)来制备多元醇组合物或多异氰酸酯组合物的情况下,在计算单体的总当量(Y)时,使单体(y)的当量为x倍。例如,后述的实施例中使用的粘接剂1以固体成分质量比成为1:1的方式配合有多元醇组合物1和多异氰酸酯组合物1。因此,其芳香环浓度根据下述式为2.2mmоl/g。
[数学式1]
本发明的层叠体可以进一步具有印刷层。利用凹版油墨、柔版油墨、胶版油墨、孔版油墨、喷墨油墨等各种印刷油墨,并通过以往对聚合物膜的印刷中所用的通常的印刷方法,印刷层形成于层叠体的任意位置。这些油墨可以为单组份型,也可以为与异氰酸酯等固化剂组合使用的双组份型。
作为本发明的层叠体的具体方式的一例,可举出:
(1)基材/阻气涂层/印刷层/粘接层/密封层
(2)基材/印刷层/阻气涂层/密封层
(3)基材/阻气涂层/印刷层/阻气涂层/密封层
(4)基材/阻气涂层/印刷层/粘接层/无机蒸镀层/密封层
(5)基材/无机蒸镀层/阻气涂层/印刷层/粘接层/密封层
(6)基材/印刷层/粘接层/基材/无机蒸镀层/阻气涂层/粘接层/密封层等,但不限于此。
由于阻气涂层对烯烃基材的密合性优异,所以作为构成例(1)-(4)的基材,可以使用OPP膜、OPE膜,也可以使用PET膜、尼龙等聚酰胺膜。作为密封层,可以使用LLDPE膜、CPP膜,作为具有无机蒸镀层的密封层,可以使用铝蒸镀LLDPE膜、铝蒸镀CPP膜。
由于阻气涂层对无机蒸镀层的密合性也优异,所以也优选(5)、(6)这样的构成。作为构成(5)中的具有无机蒸镀层的基材,可举出具有氧化铝蒸镀层的OPP膜。作为构成(6)中的具有无机蒸镀层的基材,可举出铝蒸镀OPP膜。在任一构成例中,如果使用OPP膜或OPE膜(或对它们实施了无机蒸镀的膜)作为基材,则成为再利用性优异的层叠体,因此优选。
<包装材料>
本发明的包装材料是使用本发明的层叠体、使层叠体的密封膜的面相对地重叠后、将其周边端部热封而得到的。作为制袋方法,可举出如下方法:将本发明的层叠体弯折或重叠而使其内层的面(密封膜的面)相对,将其周边端部根据例如侧面密封型、两侧密封型、三侧密封型、四侧密封型、信封贴合密封型、合掌贴合密封型、带褶密封型、平底密封型、方底密封型、角撑型、其它热封型等形态进行热封。本发明的包装材料可根据内容物、使用环境、使用形态而采取各种形态。也可以是自立性包装材料(自立袋)等。作为热封的方法,可以通过棒密封、旋转辊密封、带密封、脉冲密封、高频密封、超声波密封等公知的方法进行。
在本发明的包装材料中,从其开口部填充内容物后,将开口部热封,制造使用了本发明的包装材料的制品。作为所填充的内容物,可举出米制点心、豆制点心、坚果类、饼干/曲奇、薄饼点心、果汁软糖、馅饼、半熟蛋糕、糖果、零食点心等点心类、面包、干脆面、方便面、干面、意大利面、无菌包装米饭、菜粥、粥、包装年糕、谷类食品等食料品类、咸菜、煮豆、纳豆、味噌、冻豆腐、豆腐、滑菇、魔芋、野菜加工品、果酱类、花生酱、色拉类、冷冻蔬菜、马铃薯加工品等农产加工品、火腿类、培根、香肠类、鸡肉加工品、牛肉罐头类等畜产加工品、鱼肉火腿/香肠、水产炼制品、鱼糕、海苔、咸烹海味、干制鲣鱼、咸鱼肉、烟熏鲑鱼、芥末明太子等水产加工品、桃子、橘子、菠萝、苹果、洋梨、樱桃等果肉类、玉米、芦笋、蘑菇、洋葱、红萝卜、白萝卜、土豆等蔬菜类、以汉堡排、肉丸、水产炸物、饺子、可乐饼等为代表的冷冻副食、冷藏副食等预制食品、黄油、人造奶油、奶酪、奶油、速溶奶精、育儿用配方奶粉等乳制品、液体调味料、蒸煮咖哩、宠物食品等食品类。另外,本发明的包装材料也可用作香烟、一次性怀炉、输液袋等医药品、化妆品、真空绝热材料等的包装材料。
实施例
以下,列举具体的合成例、实施例更详细地说明本发明,但本发明并不限定于这些实施例。需要说明的是,在以下的例子中,只要没有特别说明,则“份”和“%”分别表示“质量份”和“质量%。
<涂布剂的制备>
(实施例1-20)
在设置有搅拌机、氮气导入管、回流冷凝管的反应容器中投入乙烯醇系聚合物(A1)、离子交换水,缓慢加热至90℃并搅拌4小时,使乙烯醇系聚合物(A)溶解后,冷却至室温,得到乙烯醇系聚合物(A1)的水溶液。向其中添加聚亚烷基亚胺(A2)的水溶液、水、异丙醇,使得树脂(A)的固体成分成为5质量%、水/IPA成为7/3,得到实施例1-14的涂布剂。需要说明的是,实施例1-20中的乙烯醇系聚合物(A1)、聚亚烷基亚胺(A2)的配合比(固体成分)如表1-4所示。
(比较例1-3)
不使用聚亚烷基亚胺(A2),除此以外,与实施例同样地操作,得到比较例1、2的涂布剂。不使用乙烯醇系聚合物(A1),除此以外,与实施例同样地操作,得到比较例3的涂布剂。
实施例、比较例中使用的乙烯醇系聚合物(A1)、聚亚烷基亚胺(A2)如下所述。
(乙烯醇系聚合物(A1-1))
聚乙烯醇,聚合度:2400,皂化度:98%以上
(乙烯醇系聚合物(A1-2))
聚乙烯醇,聚合度:1700,皂化度:98%以上
(乙烯醇系聚合物(A1-3))
聚乙烯醇缩丁醛,聚合度:600,缩醛化度:10%
(乙烯醇系聚合物(A1-4))
使用Exceval AQ-4104(Kuraray株式会社制)。
(聚亚烷基亚胺(A2-1)
聚亚乙基亚胺,数均分子量:70,000,伯氨基:25%,仲氨基:50%,叔氨基:25%
(聚亚烷基亚胺(A2-2))
聚亚乙基亚胺,数均分子量:100,000,伯氨基:31%,仲氨基:41%,叔氨基:28%
<粘接剂的制备>
(粘接剂1)
(多元醇组合物1的制备)
将Coronate T-80(东曹株式会社制,由2,4-异构体80%、2,6-异构体20%构成的甲苯二异氰酸酯)25.0份、ACTCOL D-1000(三井化学公司制,平均分子量1000的2官能聚丙二醇)35.3份、ACTCOL D-400(三井化学公司制,平均分子量400的2官能聚丙二醇)36.1份的混合物加热至100℃,搅拌4小时进行反应。此时NCO含量为1.6%。停止搅拌,向其中加入乙酸乙酯42.9份,再次开始搅拌而进行溶解,将温度降低至50℃。向其中加入二乙醇胺3.6份,利用发热并升温至75℃,保持2小时。固体成分羟值为37.4(mgKOH/g),不挥发成分为70.7%。
(多异氰酸酯组合物1的制备)
将4,4’-二苯基甲烷二异氰酸酯12.3份、20.8份的ACTCOL D-1000、ACTCOL D-700(三井化学公司制,平均分子量700的2官能聚丙二醇)14.5份、乙酸乙酯22.6份的混合物加热至80℃并搅拌4小时后,加入甲苯二异氰酸酯的三羟甲基丙烷加合物22.4份。不挥发成分为70.3%,NCO%(溶液)为4.5%。
(粘接剂1的制备)
将上述中制备的多元醇组合物1和多异氰酸酯组合物1以固体成分质量比成为1:1的方式配合,用乙酸乙酯进行稀释,制备粘接剂1。粘接剂1的芳香环浓度为2.2mmоl/g。
(粘接剂2)
(多元醇组合物2的制备)
在具备搅拌机、氮气导入管、斯奈德管(日文:スナイダー管)、冷凝器的聚酯反应容器中投入乙二醇879.37份、邻苯二甲酸酐1580.52份和四异丙醇钛0.10份,以精馏管上部温度不超过100℃的方式缓慢加热,将内温保持在200℃。在酸值成为5.0mgKOH/g以下时结束酯化反应,得到设计官能团数N=2、羟值=125的聚酯多元醇。
(多异氰酸酯组合物2的制备)
将4,4-二苯基甲烷二异氰酸酯36份、2,4’-二苯基甲烷二异氰酸酯19份投入到具备搅拌机、温度计、氮气导入管的反应容器内,在氮气下进行搅拌,加热至60℃。分为数次地滴加数均分子量400的聚丙二醇(以下,简记为“PPG”。)11份、22份的数均分子量1000的PPG、11份的数均分子量2000的PPG,搅拌5~6小时,使氨基甲酸酯化反应结束。所得到的多异氰酸酯的NCO基含有率为13.5%。
(粘接剂2的制备)
将上述中制备的多元醇组合物2和多异氰酸酯组合物2以固体成分质量比成为1:1的方式配合,用乙酸乙酯进行稀释,制备粘接剂2。粘接剂2的芳香环浓度为4.5mmоl/g。
<层叠体的制造>
(实施例1-17、比较例1-3)
在OPP膜(东洋纺公司制,P2161)上涂敷实施例、比较例中制备的涂布剂,在已设置为80℃的热风干燥机中干燥1分钟,形成阻气涂层。接着,将粘接剂1或2涂敷在阻隔涂层上,利用温度已设定为50℃的干燥机使稀释溶剂挥发后,与CPP膜(东洋纺公司制,P1128)贴合。在40℃进行3天熟化,得到评价用的层叠体(构成例1:OPP膜/阻气涂层/粘接剂层/CPP膜)。
阻气涂层的膜厚如表1-4所示。粘接剂的涂布量为2.5g/m2(固体成分)。实施例8中,使用相对于乙烯醇系聚合物(A1)和聚亚烷基亚胺(A2)的固体成分100质量份配合了10质量的水分散型多异氰酸酯(旭化成公司制,Duranate WB40-100)而成的物质,形成阻气涂层。实施例12中,使用相对于乙烯醇系聚合物(A1)和聚亚烷基亚胺(A2)的固体成分100质量份配合了10质量份的填料(KUNIMINE INDUSTRIES公司制,KUNIPIA-F)而成的物质,形成阻气涂层。
(实施例18、19)
在膜厚25μm的MDOPE膜(Tokyo Ink公司制,HIBLON PE25)上涂敷以表4所示的配方所制备的涂布剂,在已设置为80℃的热风干燥机中干燥1分钟,形成阻气涂层。接着,将粘接剂1涂敷在阻隔涂层上,用温度已设定为50℃的干燥机使稀释溶剂挥发后,与膜厚60μm的LLDPE膜(Mitsui Chemicals Tocello公司制,T.U.X-HC)贴合。在40℃进行3天熟化,得到评价用的层叠体(构成例2:MDOPE膜/阻气涂层/粘接剂层/LLDPE膜)。
(实施例20)
在膜厚25μm的BOPE膜上涂敷以表4所示的配方所制备的涂布剂,在已设置为80℃的热风干燥机中干燥1分钟,形成阻气涂层。接着,将粘接剂1涂敷于阻隔涂层上,用温度已设定为50℃的干燥机使稀释溶剂挥发后,与膜厚60μm的LLDPE膜(Mitsui ChemicalsTocello公司制,T.U.X-HC)贴合。在40℃进行3天熟化,得到评价用的层叠体(构成例3:BOPE膜/阻气涂层/粘接剂层/LLDPE膜)。
(参考例)
省略阻气涂层,除此以外,与实施例、比较例同样地操作,制造层叠体(构成例4:OPP膜/粘接剂层/CPP膜)。
<评价>
(阻氧性)
将熟化结束的层叠体调整为10cm×10cm的尺寸,使用OX-TRAN2/21(MOCON公司制:透氧率测定装置),依据JIS-K7126(等压法),在23℃、0%RH的气氛下测定透氧率(单位为cc/m2·天·atm)。需要说明的是,RH表示湿度。将结果按以下的5个等级进行评价,归纳于表1-4。
5:小于5
4:5以上且小于10
3:10以上且100以下
2:100以上且小于300
1:300以上
(密合性)
在25℃的气氛下使用拉伸试验机,将剥离速度设定为300mm/分钟,利用180°的剥离方法测定层叠体的粘接强度(单位N/15mm)。按以下的4个等级进行评价,归纳于表1-4。需要说明的是,在实施例、比较例中的任一情况下,剥离均发生在阻气涂层与OPP膜的界面。
4:2.0以上
3:1.5以上且小于2.0
2:1.0以上且小于1.5
1:小于1.0[表1]
[表2]
[表3]
[表4]
[表5]
根据表1-5可知,本发明的涂布剂的阻气性与对烯烃系基材的密合性的平衡优异。另一方面,仅为乙烯醇系聚合物(A1)或聚亚烷基亚胺(A2)时,对烯烃系基材的密合性不充分。
Claims (4)
1.一种涂布剂,其包含树脂A和水性溶剂B,
所述树脂A包含乙烯醇系聚合物A1和聚亚烷基亚胺A2。
2.根据权利要求1所述的涂布剂,其中,所述聚亚烷基亚胺A2的配合量为所述乙烯醇系聚合物A1与所述聚亚烷基亚胺A2的总量的1质量%以上且90质量%以下。
3.一种层叠体,其包含基材和阻气涂层,
所述阻气涂层为权利要求1或2中任一项所述的涂布剂的干燥涂膜。
4.一种包装材料,其由权利要求3所述的层叠体形成。
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