CN114340889A - 多层结构体、其制备方法及包装容器 - Google Patents
多层结构体、其制备方法及包装容器 Download PDFInfo
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- CN114340889A CN114340889A CN202080064032.1A CN202080064032A CN114340889A CN 114340889 A CN114340889 A CN 114340889A CN 202080064032 A CN202080064032 A CN 202080064032A CN 114340889 A CN114340889 A CN 114340889A
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Abstract
本发明涉及多层结构体,其依次含有淀粉层(A)、粘接层(B)和基材层(C),其中,构成淀粉层(A)的材料含有淀粉和水,构成粘接层(B)的材料含有密度为0.920g/cm3以下的热塑性树脂,构成所述粘接层(B)的材料的酸值为0.3mgKOH/g以上,基材层(C)是拉伸弹性模量为100MPa以上的层。
Description
技术领域
本发明涉及多层结构体、其制备方法及含有该多层结构体而成的包装容器。
背景技术
以淀粉为主要成分的树脂层具有生物降解性,并且阻气性优异,因此被广泛用在包装食品的容器中。
以淀粉为主要成分的树脂层的亲水性高,容易因湿度的影响而显著损害阻隔性,因此在特别要求阻隔性的情况下,需要用具有耐水性的材料形成多层(专利文献1和2)。作为用于形成多层的方法,从生产率的观点出发,经常使用采用外层材料的挤出涂布法。作为外层材料,使用PET、PE、PP、尼龙、聚氯乙烯、聚偏氯乙烯等。
现有技术文献
专利文献
专利文献1:日本特表2015-508341号公报,
专利文献2:日本特表2015-533733号公报。
发明内容
发明所要解决的课题
关于含有淀粉树脂层的多层结构体的制备,在以往的技术中有可在挤出涂布法中使用淀粉树脂和粘接性树脂的记载。但是,淀粉树脂层受外部温度和湿度的影响,会通过吸放水分而伸缩数%以上。因此,特别是在低湿下保管的情况下,由于与粘接性树脂层的伸缩率不同,具有发生剥离强度的显著降低的问题。
因此,本发明的目的在于提供:即使在低湿下保管的情况下也可维持剥离强度的具有淀粉树脂层的多层结构体、其制备方法及含有该多层结构体而成的包装容器。
解决课题的手段
本发明人进行了深入研究,结果发现可解决上述课题,从而完成了本发明。即,本发明包含以下适宜的方式。
[1] 多层结构体,其依次含有淀粉层(A)、粘接层(B)和基材层(C),其中,
构成淀粉层(A)的材料含有淀粉和水,
构成粘接层(B)的材料含有密度为0.920g/cm3以下的热塑性树脂,
基材层(C)是拉伸弹性模量为100MPa以上的层。
[2] 根据[1]所述的多层结构体,其中,构成所述淀粉层(A)的材料中,淀粉的含量为20质量%以上,并且该淀粉中的直链淀粉含量为50质量%以上。
[3] 根据[1]或[2]所述的多层结构体,其中,构成所述淀粉层(A)的材料含有至少一种水溶性聚合物。
[4] 根据[1]~[3]中任一项所述的多层结构体,其中,构成所述淀粉层(A)的材料含有至少一种粘土。
[5] 根据[1]~[4]中任一项所述的多层结构体,其中,构成所述粘接层(B)的材料的酸值为0.3mgKOH/g以上。
[6] 根据[1]~[5]中任一项所述的多层结构体,其中,构成所述粘接层(B)的材料含有聚烯烃系聚合物。
[7] 根据[1]~[6]中任一项所述的多层结构体,其中,构成所述基材层(C)的材料含有选自聚对苯二甲酸乙二醇酯、聚乳酸、聚乙烯、聚丙烯、赛璐玢、芳族聚酯和聚琥珀酸丁二醇酯的至少1种。
[8] 方法,其是根据[1]~[7]中任一项所述的多层结构体的制备方法,包括:
将粘接层(B)和基材层(C)共挤出的工序,和
接着将粘接层(B)侧涂布在淀粉层(A)上的工序。
[9] 方法,其是根据[1]~[7]中任一项所述的多层结构体的制备方法,包括:
将粘接层(B)挤出的工序,和
接着将粘接层(B)涂布在淀粉层(A)与基材层(C)之间的工序。
[10] 包装容器,其含有根据[1]~[7]中任一项所述的多层结构体而成。
发明的效果
本发明的多层结构体可提供:即使在低湿下保管的情况下也可维持剥离强度的具有淀粉树脂层的多层结构体。
附图说明
[图1] 表示实施例中淀粉层(A)的制作所使用的双轴挤出机的概略图。
具体实施方式
本发明的多层结构体依次含有淀粉层(A)、粘接层(B)和基材层(C)。构成淀粉层(A)的材料含有淀粉和水,构成粘接层(B)的材料含有密度为0.920g/cm3以下的热塑性树脂,构成上述粘接层(B)的材料的酸值为0.3mgKOH/g以上,基材层(C)是拉伸弹性模量为100MPa以上的层。
<淀粉层(A)>
构成淀粉层(A)的材料含有淀粉(A1)和水。淀粉层(A)中,优选淀粉(A1)的含量为20质量%以上,并且该淀粉(A1)中的直链淀粉的含量为50质量%以上。此外,构成淀粉层(A)的材料中的淀粉(A1)的含量优选为50~98质量%,更优选为70~98质量%。若淀粉(A1)的含量为上述范围,则有容易得到良好的阻气性的倾向。
[淀粉(A1)]
作为淀粉(A1),例如可列举出来源于木薯(cassava)、玉米、马铃薯、甘薯、西米、木薯粉(tapioca)、高粱、大豆、蕨菜、藕莲、菱角、小麦、大米、燕麦、葛根、豌豆等的淀粉。
淀粉(A1)可以是经改性的改性淀粉。从直链淀粉含量的观点出发,成为改性淀粉的原料的淀粉优选为来源于玉米(玉蜀黍)或木薯的淀粉,更优选为来源于玉米的淀粉。作为改性淀粉,例如可列举出醚化淀粉、酯化淀粉、阳离子化淀粉和交联淀粉。构成淀粉层(A)的材料可含有1种或2种以上的这些改性淀粉。
作为醚化淀粉,可列举出例如甲基醚化淀粉等烷基醚化淀粉,例如羧甲基醚化淀粉等羧烷基醚化淀粉,例如具有碳原子数为2~6个的羟烷基的醚化淀粉等羟烷基醚化淀粉。另外,也可使用烯丙基醚化淀粉等。
作为酯化淀粉,可列举出:例如具有来源于乙酸的结构单元的酯化淀粉等具有来源于羧酸的结构单元的酯化淀粉,例如具有来源于马来酸酐的结构单元的酯化淀粉、具有来源于邻苯二甲酸酐的结构单元的酯化淀粉、具有来源于辛烯基琥珀酸酐的结构单元的酯化淀粉等具有来源于二羧酸酐的结构单元的酯化淀粉,例如硝酸酯化淀粉、磷酸酯化淀粉、尿素磷酸酯化淀粉等具有来源于含氧酸的结构单元的酯化淀粉。作为其它实例,可列举出黄原酸酯化淀粉、乙酰乙酸酯化淀粉等。
作为阳离子化淀粉,可列举出淀粉与2-二乙氨基氯乙烷的反应物、淀粉与2,3-环氧丙基三甲基氯化铵的反应物等。
作为交联淀粉,可列举出甲醛交联淀粉、表氯醇交联淀粉、磷酸交联淀粉、丙烯醛交联淀粉等。
在这些改性淀粉中,从容易抑制低湿度下的剥离强度降低的观点出发,优选具有碳原子数为2~6个的羟烷基的醚化淀粉、具有来源于二羧酸酐的结构单元的酯化淀粉或它们的组合,更优选羟乙基醚化淀粉、羟丙基醚化淀粉、羟基丁基醚化淀粉、具有来源于马来酸酐的结构单元的酯化淀粉、具有来源于邻苯二甲酸酐的结构单元的酯化淀粉、具有来源于辛烯基琥珀酸酐的结构单元的酯化淀粉或它们的组合。
具有碳原子数为2~6个的羟烷基的醚化淀粉可通过环氧烷烃与淀粉的反应得到。作为环氧烷烃,例如可列举出环氧乙烷、环氧丙烷、环氧丁烷等。改性所使用的羟基的平均数优选相对于淀粉中的1个葡萄糖单元为0.05~2个。
改性淀粉可通过利用本技术领域已知的方法将具有规定的直链淀粉含量的淀粉改性来制备,也可使用市售的改性淀粉。作为改性淀粉的代表性市售品的实例,例如可列举出从Ingredion公司可获得的作为羟丙基醚化淀粉的ECOFILM (注册商标)或National 7(注册商标)。
对于淀粉层(A)中含有的淀粉(A1),淀粉(A1)中的直链淀粉的含量优选为50质量%以上,更优选为55质量%以上,进一步优选为60质量%以上。在淀粉(A1)中的直链淀粉的含量为50质量%以上的情况下,抑制粘度的上升,容易得到片材成型性。另外,对于淀粉(A1),通常淀粉(A1)中的直链淀粉的含量为90质量%以下。淀粉(A1)中的直链淀粉的含量例如可通过“Starch 50 No.4 158-163(1998)”中记载的碘显色法测定。在淀粉层(A)中含有2种以上的淀粉(A1)的情况下,淀粉(A1)的直链淀粉含量是指考虑了2种以上的淀粉的构成比例的加权平均值、即平均直链淀粉含量。
淀粉(A1)中的含水量优选为2~15质量%。该含水量例如可通过卤素水分仪求得。
[水]
构成淀粉层(A)的材料含有水。淀粉层(A)中的水的含量优选为5~25质量%,更优选为10~15质量%。若水的含量在上述范围内,则有热成型性优异的倾向。
[水溶性聚合物]
构成淀粉层(A)的材料可含有至少一种水溶性聚合物。构成淀粉层(A)的材料中的上述水溶性聚合物的含量优选为2~50质量%,更优选为2~35质量%。若水溶性聚合物的含量为上述范围,则有容易得到低温下的强度的倾向。作为水溶性聚合物,可列举出聚乙烯醇(A2)、聚环氧乙烷、聚丙烯酰胺等,其中,从机械物性的观点出发,优选聚乙烯醇(A2)。聚乙烯醇(A2)的皂化度优选为80~99.8摩尔%。在聚乙烯醇(A2)的皂化度在上述范围内的情况下,容易得到充分的强度和阻氧性。皂化度更优选为85摩尔%以上,进一步优选为88摩尔%以上。需说明的是,在本说明书中,皂化度是指聚乙烯醇(A2)中的羟基相对于羟基与酯基之和的摩尔分数。上述皂化度例如可通过用氢氧化钠对试样中的残留乙酸基进行定量而求得。
上述聚乙烯醇(A2)还可含有除乙烯醇单元以外的其它单体单元。作为其它单体单元,可列举出来源于烯属不饱和单体的单体单元等。作为烯属不饱和单体,可示例出:乙烯、丙烯、正丁烯、异丁烯、1-己烯等α-烯烃类,丙烯酸及其盐,具有丙烯酸酯基的不饱和单体,甲基丙烯酸及其盐,具有甲基丙烯酸酯基的不饱和单体,丙烯酰胺、N-甲基丙烯酰胺、N-乙基丙烯酰胺、N,N-二甲基丙烯酰胺、双丙酮丙烯酰胺、丙烯酰胺丙磺酸及其盐、丙烯酰胺丙基二甲基胺及其盐(例如季铵盐),甲基丙烯酰胺、N-甲基甲基丙烯酰胺、N-乙基甲基丙烯酰胺、甲基丙烯酰胺丙磺酸及其盐、甲基丙烯酰胺丙基二甲基胺及其盐(例如季铵盐),甲基乙烯基醚、乙基乙烯基醚、正丙基乙烯基醚、异丙基乙烯基醚、正丁基乙烯基醚、异丁基乙烯基醚、叔丁基乙烯基醚、十二烷基乙烯基醚、硬脂基乙烯基醚、2,3-二乙酰氧基-1-乙烯基氧基丙烷等乙烯基醚类,丙烯腈、甲基丙烯腈等乙烯基氰类,氯乙烯、氟乙烯等卤代乙烯类,偏氯乙烯、偏氟乙烯等卤代亚乙烯基(vinylidene halide)类,乙酸烯丙酯、2,3-二乙酰氧基-1-烯丙氧基丙烷、烯丙基氯等烯丙基化合物,马来酸、衣康酸、富马酸等不饱和二羧酸及其盐或酯,乙烯基三甲氧基硅烷等乙烯基甲硅烷基化合物、乙酸异丙烯酯,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、苯甲酸乙烯酯等乙烯酯单体。其它单体单元的含量优选为10摩尔%以下,更优选为5摩尔%以下。聚乙烯醇中的单体单元例如可使用13C-NMR或IR法等测定。
上述聚乙烯醇(A2)的制备方法无特殊限定。例如可列举出将乙烯醇单体与其它单体共聚,将得到的共聚物皂化而转化为乙烯醇单元的方法。作为共聚时的聚合方式,可列举出间歇聚合、半间歇聚合、连续聚合、半连续聚合等。作为聚合方法,可列举出本体聚合法、溶液聚合法、悬浮聚合法、乳液聚合法等公知的方法。共聚物的皂化可应用公知的方法。例如可在该共聚物溶解在醇或含水醇中的状态下进行。此时可使用的醇例如优选为甲醇、乙醇等低级醇。
上述聚乙烯醇(A2)依据JIS Z 8803测定的4%水溶液的20℃下的粘度优选为1mPa·s以上,更优选为2mPa·s以上,进一步优选为3mPa·s以上,优选为45mPa·s以下,更优选为35mPa·s以下。在聚乙烯醇(A2)的上述粘度为上述下限值以上和上述上限值以下的情况下,容易得到充分的强度和阻氧性。
[粘土]
构成淀粉层(A)的材料可含有至少一种粘土。作为粘土,可列举出合成或天然层状硅酸盐粘土,例如可列举出蒙脱石、膨润土、贝得石、云母(mica)、锂蒙脱石、皂石、绿脱石(nontronite)、锌蒙脱石、蛭石、伊利石(ledikite)、麦羟硅钠石(magadiite)、斜水硅钠石(kenyaite)、硅镁石(stevensite)、铬岭石(volkonskoite)和它们的混合物。
在一些实施方式中,上述粘土可被改性成疏水性或亲水性。
在一些实施方式中,层状硅酸盐粘土可被改性成疏水性或亲水性。
“疏水性粘土”或“被改性成疏水性的层状硅酸盐粘土”优选为通过与含有长链烷基的表面活性剂的交换而被改性的粘土。长链烷基中每条链可含有超过4个、超过5个或超过6个的碳原子。优选的表面活性剂含有长链烷基铵离子、例如单-或二-C12-C22烷基铵离子。优选上述长链烷基不含极性取代基,例如不含羟基和羧基。优选的被改性成疏水性的粘土的实例为来自Nanocor, Inc公司的NANOMER I.40P或来自Southern Clay Products,Inc公司的CLOISITE (注册商标) 20A或CLOISITE (注册商标) 25A。
构成淀粉层(A)的材料中的粘土的含量优选为0.1~5质量%,更优选为0.1~3质量%,进一步优选为0.5~2质量%。在以上述范围的量含有粘土的情况下,有透明性、柔软性、拉伸强度、耐冲击性和/或拉伸特性容易提高的倾向。
[其它添加剂]
构成淀粉层(A)的材料可含有增塑剂、保湿剂、润滑剂、其它添加剂。
作为增塑剂,例如可列举出多元醇、聚乙二醇、环氧化亚麻籽油、环氧化大豆油、柠檬酸三丁酯、二异丁酸2,2,4-三甲基-1,3-戊二醇酯和柠檬酸乙酰基三乙酯。在构成淀粉层(A)的材料中,增塑剂的含量优选为20质量%以下。
作为保湿剂,例如可列举出角叉菜胶、黄原胶、***胶、瓜尔胶、明胶、三乙酸甘油酯。保湿剂有时也会作为水结合材料或胶凝剂发挥功能。在构成淀粉层(A)的材料中,保湿剂的含量优选为20质量%以下。
作为润滑剂,例如可列举出脂肪酸、脂肪酸盐。特别优选来源于C12~22脂肪酸的润滑剂。具体而言,例如可列举出硬脂酸、硬脂酸的钠盐、硬脂酸的钾盐。在构成淀粉层(A)的材料中,润滑剂的含量优选为1.5质量%以下。
<粘接层(B)>
构成粘接层(B)的材料含有密度为0.920g/cm3以下的热塑性树脂。可含有1种或2种以上的热塑性树脂。在构成粘接层(B)的材料不含密度为0.920g/cm3以下的热塑性树脂的情况下,难以抑制低湿度下的剥离强度的降低。该密度优选为0.9182g/cm3以下,更优选为0.9100g/cm3以下,进一步优选为0.9000g/cm3以下,更进一步优选为0.8900g/cm3以下。另外,该密度优选为0.5g/cm3以上,更优选为0.85g/cm3以上。若构成粘接层(B)的材料含有密度为0.920g/cm3以下的热塑性树脂,则可缓和在低湿保管时因淀粉层脱水收缩而产生的应力,因此倾向于在低湿度下可抑制剥离强度的降低。在这里,在构成粘接层(B)的材料含有2种以上的热塑性树脂的情况下,只要至少1种热塑性树脂的密度为0.920g/cm3以下即可,在这种情况下优选考虑了2种以上的热塑性树脂的构成比例的加权平均值为0.920g/cm3以下。上述密度例如可通过后述实施例中记载的方法测定。
构成粘接层(B)的材料的酸值为0.3mgKOH/g以上。若上述酸值低于0.3mgKOH/g,则有可能无法充分得到淀粉层(A)与粘接层(B)的粘接强度,低湿度下的剥离强度也降低。构成粘接层(B)的材料的酸值优选为0.4mgKOH/g以上,更优选为0.5mgKOH/以上,进一步优选为0.6mgKOH/g以上,更进一步优选为1.5mgKOH/g以上。另外,该酸值优选为5mgKOH/g以下,更优选为3mgKOH/g以下。若构成粘接层(B)的材料的酸值为上述下限值以上,则淀粉层(A)与粘接层(B)的粘接强度变得充分,若为上述上限值以下,则热成型时的反应适度地进行,因此难以引起成型不良。上述酸值例如可通过后述实施例中记载的方法测定。在构成粘接层(B)的材料含有2种以上的热塑性树脂的情况下,该材料的酸值如后述实施例所记载,是指测定为混合物形式的材料而得到的酸值。
需说明的是,酸值与粘接层(B)中的酸的量相关。认为粘接层(B)中的酸通过与淀粉层(A)表面的羟基反应而得到粘接性,特别是有助于初期粘接强度和低湿度下的剥离强度。认为初期粘接力和低湿度下的剥离强度与上述粘接层(B)中的酸与淀粉层(A)中的羟基的反应所伴随的效果和淀粉层(A)与粘接层(B)的相容性所带来的效果两者有关。因此,为了实现良好的粘接性,作为构成本发明的多层结构体的粘接层(B)的材料,认为需要0.3mgKOH/g以上的酸值,更优选为0.4mgKOH/g以上。构成粘接层(B)的材料的酸值例如可通过适当调节构成后述热塑性树脂的结构单元的种类和构成比例等,来调整为上述下限值以上。
[热塑性树脂]
构成粘接层(B)的材料含有热塑性树脂。作为热塑性树脂,例如可列举出聚烯烃系聚合物、聚酯系聚合物、聚酰胺系聚合物等,优选含有聚烯烃系聚合物,其中优选含有改性聚烯烃系聚合物。作为改性聚烯烃系聚合物,可列举出将乙烯、丙烯、1-丁烯、3-甲基-1-丁烯、1-戊烯,4-甲基-1-戊烯、1-己烯、1-辛烯、1-癸烯等碳原子数为2~20左右的聚烯烃改性而得到的树脂,乙酸乙烯酯、氯乙烯、丙烯酸、甲基丙烯酸、丙烯酸酯、甲基丙烯酸酯、聚苯乙烯等乙烯基化合物与烯烃的共聚物,将乙烯-丙烯共聚物、乙烯-丙烯-二烯共聚物、乙烯-1-丁烯共聚物、丙烯-1-丁烯共聚物等聚烯烃系共聚物改性而得到的树脂作为代表性的物质。作为改性的方法,可列举出基于接枝反应条件下的改性。作为接枝反应所使用的物质,可列举出丙烯酸、甲基丙烯酸、巴豆酸、异巴豆酸、马来酸、富马酸、衣康酸、柠康酸、四氢邻苯二甲酸等不饱和羧酸,另外,可列举出其酰卤、酰胺、酰亚胺、酐、酯等衍生物。具体而言,可列举出马来酰氯、马来酰亚胺、马来酸酐、柠康酸酐、马来酸单甲酯、马来酸二甲酯、马来酸缩水甘油酯等。若使用这些改性聚烯烃系聚合物,则容易抑制多层结构体在使用时的黄变。
另一方面,从抑制多层结构体在使用时的黄变的观点出发,构成粘接层(B)的材料中的氨基甲酸酯系树脂的含量优选为50质量%以下,优选为10质量%以下,最优选为0质量%。
作为改性聚烯烃系聚合物,其中,从反应性和作为食品包装材料的卫生性的观点出发,优选用不饱和二羧酸或其酐、特别是马来酸或其酐改性的树脂。作为改性的树脂,优选乙烯系树脂、丙烯系树脂、乙烯-丙烯共聚物或乙烯-1-丁烯共聚物。因此,在本发明的优选的一个方式中,优选使用用马来酸酐改性的聚烯烃系聚合物、即具有来源于马来酸酐的结构单元的聚烯烃系聚合物。
<基材层(C)>
基材层(C)是拉伸弹性模量为100MPa以上的层。上述拉伸弹性模量为100MPa以上,优选为200MPa以上,更优选为300MPa以上,进一步优选为500MPa以上,更进一步优选为1000MPa以上、特别优选为2000MPa以上,进一步特别优选为3000MPa以上。上述弹性模量例如可用后述实施例中记载的方法测定。通常,上述弹性模量为8000MPa以下。为了使基材层(C)的拉伸弹性模量为上述下限值以上,可通过调整构成基材层(C)的材料的种类和构成比例等,来调整为上述下限值以上。若上述弹性模量低于100MPa,则基材层强度不足,容易产生基材断裂。构成基材层(C)的材料优选含有选自聚对苯二甲酸乙二醇酯(PET)、聚乳酸(PLA)、聚乙烯、聚丙烯、赛璐玢(cellophanes)、芳族聚酯和聚琥珀酸丁二醇酯(PBS)的至少1种。基材层(C)中的上述材料的含量优选为10~100质量%,更优选为20~90质量%。构成基材层(C)的材料还可含有聚烯烃、尼龙、聚氯乙烯、聚偏二氯乙烯等其它材料。在基材层(C)含有其它材料的情况下,基材层(C)中的其它材料的含量可优选为5~50质量% (基材层(C)中的全部材料之和为100质量%)。
基材层(C)含有的树脂材料可以是生物降解性树脂。作为生物降解性树脂,可列举出聚己二酸丁二醇酯-对苯二甲酸丁二醇酯共聚物(PBAT)、聚羟基丁酸酯、聚己内酯、聚羟基链烷酸酯、聚乙醇酸、改性聚乙烯醇、淀粉、纤维素等。构成基材层(C)的材料可含有1种生物降解性树脂,也可含有2种以上的生物降解性树脂,含有2种以上时的掺混比率无特殊限定。
<多层结构体>
本发明的多层结构体的厚度优选为30~1000μm。淀粉层(A)的厚度优选为20~500μm,基材层(C)的厚度优选为10~500μm。若淀粉层(A)的厚度在上述范围内,则倾向于具有良好的阻气性。另外,若基材层(C)的厚度在上述范围内,则难以引起基材断裂。
粘接层(B)的厚度优选为5~50μm,更优选为10~30μm。若为5μm以上,则容易得到充分的层间粘接强度,另外,若为50μm以下,则在热成型之后实施的容器的冲压加工时难以产生被称为须状毛刺(whisker burr)的外观不良,因而优选。
多层结构体层的层结构只要是依次含有淀粉层(A)、粘接层(B)和基材层(C)这3层的结构,则无特殊限定。在将淀粉层(A)记作A、将粘接层(B)记作B、将基材层(C)记作C的情况下,例如可列举出A/B/C的3层结构,A/B/C/B/A、A/B/A/B/C、C/B/A/B/C的5层结构等。此外,还可含有除淀粉层(A)、粘接层(B)、基材层(C)以外的层(D)。在将层(D)记作D的情况下,可列举出D/A/B/C、D/B/A/B/C、A/D/B/C、A/B/D/B/C、A/B/D/C、A/B/D/B/C、A/B/C/D、A/B/C/B/D、D/A/B/C/D、D/B/A/B/C/B/D等结构。其中优选A与B邻接、B与C邻接的D/A/B/C、A/B/C/D、D/A/B/C/D的结构。作为层(D),无特殊限制,例如可列举出纸。对纸无特殊限制,例如可列举出玻璃纸、牛皮纸、优质纸、中质纸、压花纸、涂布纸、无碳纸、纸板等。
将本发明的多层结构体在温度为23℃、湿度为50%RH下放置1周后的淀粉层(A)与粘接层(B)之间的剥离强度(P1)优选为1.0kgf/15mm以上。另外,将本发明的多层结构体在温度为40℃、湿度为15%RH下放置48小时后的淀粉层(A)与粘接层(B)之间的剥离强度(P2)优选为0.5kgf/15mm以上。另外,用下式表示的剥离强度的降低率通常低于60%,优选低于50%,更优选低于30%。上述剥离强度例如可通过后述实施例中记载的方法测定。
剥离强度的降低率
=100×[剥离强度(P1)-剥离强度(P2)]/剥离强度(P1)。
<多层结构体的制备方法>
本发明的多层结构体的制备方法无特殊限制。例如可列举出包括以下工序的方法:将粘接层(B)和基材层(C)共挤出的工序,和接着将粘接层(B)侧涂布在淀粉层(A)上的工序。此外,例如还可列举出包括以下工序的方法:将粘接层(B)挤出的工序,和接着将粘接层(B)涂布在淀粉层(A)与基材层(C)之间的工序。
在将粘接层(B)和基材层(C)共挤出的工序中,例如可使用双组分双层共挤出流延制膜设备(Research Laboratory of Plastics Technology Co., Ltd.制挤出机) (挤出机(1)基材层(C)用:单轴、螺杆直径40mm、L/D=32,挤出机(2)粘接层(B)用:单轴、螺杆直径32mm、L/D=26)。挤出机的温度条件只要根据所使用的热塑性树脂适当设定即可,例如在用挤出机(1)基材层(C)用挤出PET (聚对苯二甲酸乙二醇酯)的情况下,可将料筒温度设为250~270℃,将转接器温度设为270℃,将模头温度设为275℃。
另外,例如在用挤出机(2)粘接层(B)用挤出聚烯烃的情况下,可将料筒温度设为175~270℃,将转接器温度设为270℃,将模头温度设为275℃。另外,挤出机(1)的模头温度与挤出机(2)的模头温度之差的绝对值优选为10℃以内,更优选为0℃。例如,在挤出机(1)所使用的树脂和挤出机(2)所使用的树脂的最适宜模头温度不同的情况下,优选采用最适宜模头温度高的一方来调整模头温度。
然后,在将粘接层(B)侧涂布在淀粉层(A)上的工序中,例如可采用将共挤出的层叠体的粘接层(B)侧边拉取边涂布在淀粉层(A)上,并用夹辊贴合的方法。拉取速度优选为1~10m/分钟。
<包装容器>
本发明的包装容器含有本发明的多层结构体而成。包装容器可只由本发明的多层结构体构成,也可复合有其它材料。例如可将本发明的多层结构体热成型以制成包装容器。作为热成型方法,无特殊限定,可列举出一般的真空成型、加压成型,或作为它们的应用,可列举出使柱塞与多层结构体的单面接触来进行成型的柱塞辅助法、或使成对的阳模阴模与多层结构体的两面接触来进行成型的被称为所谓的多模具成型的方法等。另外,作为在成型前将多层结构体加热软化的方法,可列举出非接触加热或直接加热,作为非接触加热,可列举出利用红外线加热器等的辐射加热。另外,作为直接加热,可应用与热板直接接触的热板加热等公知的加热方法。
由本发明的多层结构体构成的包装容器即使在低湿下保管的情况下也可维持剥离强度,因此作为包装容器是优异的。此外,在优选的方式中,由于阻氧性、生物降解性优异,所以可特别优选用作食品用的包装容器。
实施例
通过以下实施例等,对本发明进行更具体的说明,但本发明不因这些实施例等而受到任何限定。
<基材层(C)的拉伸弹性模量>
将用作基材层(C)的树脂材料在下述表1中记载的条件下用单轴挤出机(ResearchLaboratory of Plastics Technology Co., Ltd.制挤出机,直径40mm、L/D=25)挤出。
[表1]
PHA:3-羟基丁酸酯-3-羟基己酸酯共聚物
将上述挤出的树脂排出到流延辊上,制作厚度为30μm的基材层(C)的单层膜。另外,作为赛璐玢,使用市售品Nature Flex NK19 (厚度为20μm)的膜。
将得到的膜在23℃、50%RH的调节室中保管一周进行调湿后,切断成宽15mm、长150mm而制成试验片。用拉伸试验机(Instron Corporation制,INSTRON 3367),在速度为20mm/分钟、卡盘间距离为50mm的条件下实施试验片的拉伸弹性模量测定。进行共5次相同的试验,将平均值作为拉伸弹性模量的值。
<多层结构体的剥离强度(常湿)>
将实施例和比较例中制作的多层结构体在23℃、50%RH的调节室中保管一周进行调湿,切成15mm×150mm而制成试验片。
对于多层结构体的淀粉层(A)与粘接层(B)的层间,用拉伸试验机(InstronCorporation制,INSTRON 3367),在速度为50mm/分钟、卡盘间距离为50mm、剥离角度为180°的条件下进行层间剥离,从而实施剥离强度测定。进行共5次相同的试验,将平均值作为剥离强度的值。
<多层结构体的剥离强度(低湿)>
将实施例和比较例中制作的多层结构体在23℃、50%RH的调节室中保管一周进行调湿,进而在40℃、15%RH的调节室中保管48小时进行调湿,切成15mm×150mm,从而制成试验片。
除了改变所使用的试验片以外,用与上述<多层结构体的剥离强度(常湿)>相同的方法求得剥离强度的值。
需说明的是,包装材料的低湿下和常湿下的剥离强度的要求值根据制品形状而不同。例如,在由本发明的多层结构体通过热成型等得到的托盘状包装材料中优选为1.5kgf/15mm以上,在由本发明的多层结构体构成的软包装材料中0.5kgf/15mm以上成为优选的目标。虽然该基准值根据用途而增减,但低于0.4kgf/15mm的剥离强度无法满足大多数的制品形状、用途的要求性能。
<构成粘接层(B)的热塑性树脂的密度>
使用岛津制作所制AccuPyc II1340,在装置温度为25℃(±1℃)的条件下,通过使用气体(氦气)的干式测定法对热塑性树脂的粒料进行测定。进行共3次相同的试验,将平均值作为密度的值。
<构成粘接层(B)的材料的酸值>
在三角烧瓶中称取400mg的构成粘接层(B)的热塑性树脂,并投入80ml的二甲苯。搅拌升温至130℃,使热塑性树脂溶解。在溶解液中添加微量的酚酞,用0.05mol/L氢氧化钾-乙醇溶液进行滴定,从而求得酸值。
<多层结构体的紫外线褪色计试验(黄变)>
将实施例和比较例中制作的多层结构体在23℃、50%RH的调节室中保管一周进行调湿,切成50mm×100mm而制成试验片。
用紫外线褪色计(Suga Test Instruments Co., Ltd.制,U48H),在照射强度为0.70W/m2、黑色面板温度为63±3℃、照射时间为100小时的条件下对各试验片的淀粉层(A)侧照射紫外线以实施测定,目视评价黄变。
<淀粉层(A)的制作>
淀粉层(A)的材料用以下方法进行调制。以使构成淀粉层(A)的材料中的改性淀粉(i) [ECOFILM (注册商标),Ingredion制,用丙基氧化物(环氧丙烷)改性的玉米淀粉,直链淀粉含量为70质量%]的含量为40质量%~70质量%、具有水溶性的树脂(ii) [聚乙烯醇 溶液粘度为30mPa·s,皂化度为99%]的含量为5质量%~35质量%的方式进行掺混,在转鼓混合机内混合2小时。将通过混合得到的粉末以3.5kg/小时的速度经由重量送料器供给到挤出机的加料斗中。以使得水的量相对于粉末与水的合计质量为25质量%的方式使水通过液体输送泵,喷射到挤出机的机筒(barrel)内,并在机筒中调制淀粉层(A)的材料。
从挤出机的模头挤出,冷却,且设定拉取速度以使得干燥后的厚度为150μm,从而得到淀粉层(A)。制备淀粉层(A)时的料筒温度设定为如下述表2中记载的温度分布。C5~C9为蒸煮(cooking)处理区域。
[表2]
温度分布(℃)
<实施例1>
使用PET (聚对苯二甲酸乙二醇酯) (M&G CHEMICALS SA制Traytuf 7300)作为基材层(C)的材料。使用聚烯烃(三井化学公司制Admer SE800)作为粘接层(B)的材料。
通过将基材层(C)的材料在料筒温度为250℃~270℃、转接器温度为270℃、模头温度为275℃下挤出,将粘接层(B)的材料在料筒温度为175℃~270℃、转接器温度为270℃、模头温度为275℃下挤出,来进行共挤出,得到由粘接层(B)和基材层(C)构成的层叠膜[粘接层(B)厚度20μm/基材层(C)厚度150μm]。
将层叠膜的粘接层(B)侧涂布在上述<淀粉层(A)的制作>中得到的150μm的淀粉层(A)膜上,用夹辊使其贴合,以3m/分钟的拉取速度制作多层结构体[淀粉层(A)厚度150μm/粘接层(B)厚度20μm/基材层(C)厚度150μm]。
<实施例2>
除了将粘接层(B)的材料变为聚烯烃(三井化学公司制Admer SE810)以外,与实施例1相同地制作多层结构体。
<实施例3>
除了将粘接层(B)的材料变为聚烯烃(三井化学公司制Admer SF741)以外,与实施例1相同地制作多层结构体。
<实施例4>
除了将粘接层(B)的材料变为聚烯烃(三井化学公司制Admer SF725)以外,与实施例1相同地制作多层结构体。
<实施例5>
除了将基材层(C)的材料变为PBS (聚琥珀酸丁二醇酯) (三菱化学公司制PBSFZ91),并在料筒温度为180℃~200℃、转接器温度为200℃、模头温度为200℃下进行挤出以外,与实施例4相同地制作多层结构体。
<实施例6>
将基材层(C)的材料变为PLA (聚乳酸) (三菱化学公司制ECOLOJU SA104),且变更挤出条件(挤出机料筒温度为180℃~200℃,转接器温度为200℃,模头温度为200℃)。
另外,变更粘接层(B)的材料即聚烯烃(三井化学公司制Admer SF725)的挤出条件(挤出机料筒温度为175~200℃,转接器温度为200℃,模头温度为200℃)。除此之外,与实施例4相同地制作多层结构体。
<实施例7>
作为粘接层(B)的材料,对聚烯烃(三井化学公司制Admer SF725)进行单层挤出(挤出机料筒温度为160℃~200℃,转接器温度为200℃,模头温度为200℃),将粘接层(B)涂布在淀粉层(A)上。接着,作为基材层(C),将厚度为20μm的赛璐玢(Futamura ChemicalCo., Ltd.制Nature Flex NK19)在粘接层(B)面上进行沙粒层压(sand-laminate),从而制作多层结构体。
<实施例8>
将基材层(C)的材料变为PHA (3-羟基丁酸酯-3-羟基己酸酯共聚物) (KanekaCorporation制PHBH 151N),且变更挤出条件(挤出机料筒温度为130℃~160℃,转接器温度为160℃,模头温度为160℃)。变更粘接层(B)的材料即聚烯烃(三井化学公司制AdmerSF725)的挤出条件(挤出机料筒温度为150~160℃,转接器温度为160℃,模头温度为160℃)。除此之外,与实施例4相同地制作多层结构体。
<实施例9>
将基材层(C)的材料变为PBAT (聚己二酸丁二醇酯-对苯二甲酸丁二醇酯共聚物)(BASF公司制Ecovio FT2341),且变更挤出条件(挤出机料筒温度为160℃~200℃,转接器温度为200℃,模头温度为200℃)。变更粘接层(B)的材料即聚烯烃(三井化学公司制AdmerSF725)的挤出条件(挤出机料筒温度为160~200℃,转接器温度为200℃,模头温度为200℃)。除此之外,与实施例4相同地制作多层结构体。
<实施例10>
将基材层(C)的材料变为LDPE (聚烯烃) (Japan Polyethylene Corporation制NOVATEC LD LJ400),且变更挤出条件(挤出机料筒温度为160℃~200℃,转接器温度为200℃,模头温度为220℃)。变更粘接层(B)的材料即聚烯烃(三井化学公司制Admer SF725)的挤出条件(挤出机料筒温度为160~220℃,转接器温度为220℃,模头温度为220℃)。在这里,关于模头温度,与所要求的温度高的材料一方(在这里为粘接层(B))相应地进行设定。除此之外,与实施例4相同地制作多层结构体。
<实施例11>
作为粘接层(B)的材料,将聚烯烃(三井化学公司制Admer SF725)与另一聚烯烃(三井化学公司制Admer NF567)以75:25的质量比干混并使用,除此之外,与实施例4相同地制作多层结构体。
<实施例12>
作为粘接层(B)的材料,将聚烯烃(三井化学公司制Admer SE800)与LDPE (聚烯烃) (Japan Polyethylene Corporation制NOVATEC LD LC600A)以75:25的质量比干混并使用,除此之外,与实施例4相同地制作多层结构体。
<比较例1>
除了将粘接层(B)的材料变为聚烯烃(Arkema K.K.制Lotader 4503)以外,与实施例1相同地制作多层结构体。
<比较例2>
除了将粘接层(B)的材料变为聚烯烃(The Dow Chemical Company制AmplifyTY4351)以外,与实施例1相同地制作多层结构体。
<比较例3>
除了将粘接层(B)的材料变为聚烯烃(DuPont de Nemours, Inc.制Bynel21E830)以外,与实施例1相同地制作多层结构体。
<比较例4>
使用聚对苯二甲酸乙二醇酯(M&G CHEMICALS SA制Traytuf 7300)作为基材层(C)的材料。使用聚氨酯系粘接剂(Rohm and Haas公司制MOR Free PU粘接剂)作为粘接层(B)的材料。
将基材层(C)的材料在料筒温度为250℃~270℃、转接器温度为270℃、模头温度为275℃下挤出,制作厚度为150μm的片材。用干式层压的方法将粘接层(B)的材料以15μm的厚度涂布在基材层(C)上。用夹辊将由粘接层(B)和基材层(C)构成的层叠膜的粘接层(B)侧贴合在上述<淀粉层(A)的制作>中得到的厚度为150μm的淀粉层(A)膜上,制作多层结构体(淀粉层(A)厚度150μm/粘接层(B)厚度15μm/基材层(C)厚度150μm)。
<比较例5>
作为粘接层(B)的材料,将聚烯烃(三井化学公司制Admer SE800)和LDPE (聚烯烃) (Japan Polyethylene Corporation制NOVATEC LD LC600A)以50:50的质量比干混并使用,除此之外,与实施例4相同地制作多层结构体。
对于实施例1~12、比较例1~5中制作的多层结构体,进行各种评价。将结果示出于表3中。需说明的是,在粘接层(B)含有2种热塑性树脂的情况下,其密度表示考虑了热塑性树脂的构成比例的加权平均值。
[表3]
如表3所示,将多层结构体在40℃、15%RH的恒温室中静置48小时,结果可确认,在如实施例1~12这样的构成粘接层(B)的材料含有0.920g/cm3以下的热塑性树脂、且材料的酸值为0.3mgKOH/g以上的情况下,剥离强度的降低率低,即使在低湿下保管的情况下也可维持剥离强度。另外,不产生黄变,具有良好的外观。
Claims (9)
1.多层结构体,其依次含有淀粉层(A)、粘接层(B)和基材层(C),其中,
构成淀粉层(A)的材料含有淀粉和水,
构成粘接层(B)的材料含有密度为0.920g/cm3以下的热塑性树脂,构成所述粘接层(B)的材料的酸值为0.3mgKOH/g以上,
基材层(C)是拉伸弹性模量为100MPa以上的层。
2.根据权利要求1所述的多层结构体,其中,构成所述淀粉层(A)的材料中,淀粉的含量为20质量%以上,并且该淀粉中的直链淀粉含量为50质量%以上。
3.根据权利要求1或2所述的多层结构体,其中,构成所述淀粉层(A)的材料含有至少一种水溶性聚合物。
4.根据权利要求1~3中任一项所述的多层结构体,其中,构成所述淀粉层(A)的材料含有至少一种粘土。
5.根据权利要求1~4中任一项所述的多层结构体,其中,构成所述粘接层(B)的材料含有聚烯烃系聚合物。
6.根据权利要求1~5中任一项所述的多层结构体,其中,构成所述基材层(C)的材料含有选自聚对苯二甲酸乙二醇酯、聚乳酸、聚乙烯、聚丙烯、赛璐玢、芳族聚酯和聚琥珀酸丁二醇酯的至少1种。
7.多层结构体的制备方法,其是根据权利要求1~6中任一项所述的多层结构体的制备方法,所述方法包括:
将粘接层(B)和基材层(C)共挤出的工序,和
接着将粘接层(B)侧涂布在淀粉层(A)上的工序。
8.多层结构体的制备方法,其是根据权利要求1~6中任一项所述的多层结构体的制备方法,所述方法包括:
将粘接层(B)挤出的工序,和
接着将粘接层(B)涂布在淀粉层(A)与基材层(C)之间的工序。
9.包装容器,其含有根据权利要求1~6中任一项所述的多层结构体而成。
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WO (1) | WO2021048795A1 (zh) |
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GB1115464A (en) * | 1964-06-29 | 1968-05-29 | Staley Mfg Co A E | Multiply film |
JPH0994905A (ja) * | 1995-09-28 | 1997-04-08 | Dainippon Printing Co Ltd | 積層体とこれを用いた蓋材 |
JP2004017991A (ja) * | 2002-06-13 | 2004-01-22 | Dainippon Printing Co Ltd | レトルト処理用紙容器およびそれを使用したレトルト処理包装体 |
US20070292665A1 (en) * | 2004-09-30 | 2007-12-20 | Nippon Paper Industries, Co., Ltd. | Laminated Sheet |
US20140349047A1 (en) * | 2011-12-22 | 2014-11-27 | Plantic Technologies Limited | Multilayer Films |
WO2015042641A1 (en) * | 2013-09-25 | 2015-04-02 | Douglas Michael Trenchard | An agricultural plastic mulch film and a composite thereof |
US20150210461A1 (en) * | 2012-09-21 | 2015-07-30 | Plantic Technologies Ltd | Food Package |
US20180304573A1 (en) * | 2015-10-19 | 2018-10-25 | Denka Company Limited | Laminated sheet and formed container |
CN109575367A (zh) * | 2018-12-12 | 2019-04-05 | 湖南绿燊环保科技有限公司 | 热塑性淀粉复合材料及其制备方法 |
US20190176455A1 (en) * | 2016-08-18 | 2019-06-13 | Toppan Printing Co., Ltd. | Methods for producing paper containers for liquid, and paper containers for liquid |
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2019
- 2019-09-13 JP JP2019167518A patent/JP2021041674A/ja active Pending
-
2020
- 2020-09-11 CN CN202080064032.1A patent/CN114340889A/zh active Pending
- 2020-09-11 AU AU2020344251A patent/AU2020344251A1/en active Pending
- 2020-09-11 WO PCT/IB2020/058441 patent/WO2021048795A1/ja unknown
- 2020-09-11 JP JP2021544977A patent/JPWO2021048795A1/ja active Pending
- 2020-09-11 EP EP20863709.0A patent/EP4043207A4/en active Pending
- 2020-09-11 US US17/641,990 patent/US20230241864A1/en active Pending
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1115464A (en) * | 1964-06-29 | 1968-05-29 | Staley Mfg Co A E | Multiply film |
JPH0994905A (ja) * | 1995-09-28 | 1997-04-08 | Dainippon Printing Co Ltd | 積層体とこれを用いた蓋材 |
JP2004017991A (ja) * | 2002-06-13 | 2004-01-22 | Dainippon Printing Co Ltd | レトルト処理用紙容器およびそれを使用したレトルト処理包装体 |
US20070292665A1 (en) * | 2004-09-30 | 2007-12-20 | Nippon Paper Industries, Co., Ltd. | Laminated Sheet |
US20140349047A1 (en) * | 2011-12-22 | 2014-11-27 | Plantic Technologies Limited | Multilayer Films |
US20150210461A1 (en) * | 2012-09-21 | 2015-07-30 | Plantic Technologies Ltd | Food Package |
WO2015042641A1 (en) * | 2013-09-25 | 2015-04-02 | Douglas Michael Trenchard | An agricultural plastic mulch film and a composite thereof |
US20180304573A1 (en) * | 2015-10-19 | 2018-10-25 | Denka Company Limited | Laminated sheet and formed container |
US20190176455A1 (en) * | 2016-08-18 | 2019-06-13 | Toppan Printing Co., Ltd. | Methods for producing paper containers for liquid, and paper containers for liquid |
CN109575367A (zh) * | 2018-12-12 | 2019-04-05 | 湖南绿燊环保科技有限公司 | 热塑性淀粉复合材料及其制备方法 |
Also Published As
Publication number | Publication date |
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JPWO2021048795A1 (zh) | 2021-03-18 |
US20230241864A1 (en) | 2023-08-03 |
EP4043207A4 (en) | 2023-11-01 |
JP2021041674A (ja) | 2021-03-18 |
AU2020344251A1 (en) | 2022-03-24 |
WO2021048795A1 (ja) | 2021-03-18 |
EP4043207A1 (en) | 2022-08-17 |
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