CN115667417B - 阻气性涂料组合物和阻气性层叠体 - Google Patents
阻气性涂料组合物和阻气性层叠体 Download PDFInfo
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- CN115667417B CN115667417B CN202180036873.6A CN202180036873A CN115667417B CN 115667417 B CN115667417 B CN 115667417B CN 202180036873 A CN202180036873 A CN 202180036873A CN 115667417 B CN115667417 B CN 115667417B
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Abstract
本发明涉及阻气性涂料组合物,其包含金属氧化物、磷酸化合物和胺化合物,并且提供不仅具有优异的氧气阻隔性和水分阻隔性而且具有优异的透明性的阻气性涂膜,以及包括该涂膜的阻气性层叠体。
Description
技术领域
本发明涉及阻气性涂料组合物,其包含金属氧化物、磷酸化合物和胺化合物作为构成成分。更具体地,本发明涉及不仅具有优异氧气阻隔性和水分阻隔性还具有优异的透明性且能够形成涂膜的涂料组合物,以及包括该涂膜的阻气性层叠体。
背景技术
以往已知通过在塑料基材上形成包含金属原子和磷原子作为构成成分的膜而获得的阻气性层叠体。
例如,下述专利文献1中提出了实质上连续且实质上非结晶性的防透气膜,其中金属与磷的原子比为约2.3~0.5,金属原子中的50%~100%为铝,金属原子中的0~50%选自锡、钛和锆,和金属原子中的0~约20%为选自锌、铬和镁的金属正磷酸盐。
然而,所述防透气膜在氧气阻隔性和水蒸气阻隔性的方面仍不令人满意。尽管专利文献1公开了添加树脂来尝试改善涂层对基质的附着力,但其并没有教导通过添加树脂来改善涂膜的氧气阻隔性和水蒸气阻隔性的效果。为了解决这些问题,下述专利文献2记载了一种复合结构体,其具有基材(X)和层叠于所述基材(X)的层(Y),层(Y)包含由至少金属氧化物(A)与磷化合物(B)反应而形成的反应产物(S),层(Y)具有在800~1400cm-1的范围内的红外线吸收光谱,其中红外线吸收成为最大的波数(n1)在1080~1130cm-1的范围内,构成金属氧化物(A)的金属原子(M)为铝。
现有技术文献:
专利文献:
专利文献1:JP-B-57-42032
专利文献2:日本专利No.4961054
发明内容
发明要解决的问题
上述专利文献2所公开的复合结构体满足氧气阻隔性和水蒸气阻隔性二者。然而,该复合结构体主要由铝构成,其在对由内容物所具有的酸和碱的安全性方面仍不令人满意。
为了解决这些问题,本发明人提出了一种使用特定的锆化合物的阻气性膜(日本专利申请No.2019-152688)。另外,本发明人已发现如下事实:使用特定的添加剂时,可以获得能够形成表现出更优异的氧气阻隔性和水蒸气阻隔性的涂膜的金属氧化物和磷酸化合物的阻气性涂料组合物。
因此,本发明的目的是提供一种包含金属氧化物和磷酸化合物的阻气性涂料组合物,其能够形成表现出更优异的氧气阻隔性、水蒸气阻隔性和透明性的阻气性膜,以及提供一种设置有该阻气性涂膜(阻气层)的阻气性层叠体。
用于解决问题的方案
根据本发明,提供一种阻气性涂料组合物,其特征在于,其包含金属氧化物、磷酸化合物和胺化合物。
在本发明的阻气性涂料组合物中,期望:
1.胺化合物为多胺化合物(polyamine compound)、氨基糖化合物和氨基酸化合物中的至少一种;
2.胺化合物为聚烯丙基胺、聚乙烯亚胺、壳聚糖、甘氨酸和精氨酸中的至少一种;
3.金属氧化物为锆氧化物(zirconium oxide);和
4.磷酸化合物为正磷酸、偏磷酸、多磷酸和环状多磷酸中的至少一种。
此外,根据本发明,提供一种阻气性层叠体,其特征在于,在基材上具有上述阻气性涂料组合物的涂膜。
在本发明的阻气性层叠体中,期望:
1.涂膜具有使得在其红外线吸收光谱中在1000~1050cm-1的范围内红外线吸收成为最大的吸收峰。
2.涂膜具有使得通过XPS测量的N的结合能量在400~405eV的范围内成为最大的峰。
3.锚固层设置在基材和涂膜之间。
4.当基材为12μm厚的双轴拉伸聚酯、涂膜以1.0g/m2的涂布量形成在基材上、和在涂膜上配置50μm厚的未拉伸聚丙烯膜时,透氧量为25cc/m2·天·atm(40℃90%RH)以下,水蒸气透过量为5.5g/m2·天(40℃90%RH)以下。
发明的效果
本发明的阻气性涂料组合物使用金属氧化物、磷酸化合物和胺化合物。这里,假设金属氧化物颗粒尺寸较小,则金属氧化物颗粒更容易分散,因此,通过金属氧化物和磷酸化合物产生更均匀且致密的交联结构,使得可以形成能够表现出优异的氧气阻隔性和水蒸气阻隔性的涂膜。此外,胺化合物也被吸收到交联结构中,因此在金属氧化物颗粒中起粘结剂的作用。由此形成具有较少缺陷的涂膜,其表现出通过形成上述均匀且致密的交联结构而复合的更优异的氧气阻隔性和水蒸气阻隔性。因此,本发明的阻气性涂料组合物能够提供可应用于非蒸煮用途和蒸煮灭菌两者的阻气性层叠体。
此外,在使用锆氧化物作为金属化合物时,可以形成即使对内容物中的酸和碱也保持稳定的涂膜,因此,可以表现出更优异的氧气阻隔性和水蒸气阻隔性。
附图说明
[图1]其为以截面示出本发明的阻气性层叠体的结构的图。
[图2]其为以截面示出本发明的阻气性层叠体的另一结构的图。
具体实施方式
(阻气性涂料组合物)
本发明的阻气性涂料组合物的重要特征在于,其包含金属氧化物、磷酸化合物和胺化合物。
如上所述,根据本发明,发现在包含金属氧化物、磷酸化合物以及胺化合物时,涂膜表现出比由包含金属氧化物和磷酸化合物的涂料组合物形成的涂膜更优异的氧气阻隔性和水蒸气阻隔性。
[金属氧化物]
作为用于本发明的阻气性涂料组合物的金属氧化物,期望使用化合价为2以上的金属原子的氧化物。尽管不仅限于此,但可以使用镁、钙、铁、锌、铝、硅、钛和锆的氧化物。其中,可以优选使用锆氧化物。
锆氧化物包含Zr和O作为组成元素。这里,非晶质锆氧化物包含氢氧化锆(Zr(OH)4)和/或氢氧化氧锆(zirconyl hydroxide)(ZrO(OH)2)作为主要组分,而晶质锆氧化物包含水合氧化锆(ZrO2·xH2O)和/或氧化锆(ZrO2)作为主要组分。这里,主要组分是指以50%以上的比例包含的组分。关于锆氧化物和进行了阻气膜化的锆氧化物的结晶性,可以通过借助使用以往公知的X射线结构衍射装置来鉴别结晶性锆所特有的X射线峰来进行评价。
本发明中,锆氧化物可以为晶质或非晶质的锆氧化物(氧化锆(zirconia))。
根据本发明人先前提交的上述日本专利申请No.2019-152688,优选使用用于磷酸化反应的包含多个羟基的非晶质锆氧化物作为锆氧化物。然而,由于发现即使当使用晶质锆氧化物时,也可以通过添加胺化合物形成更均匀、致密的无缺陷涂膜,现在使得可以同时实现等同于使用非晶质锆时得到的氧气阻隔性和水分阻隔性。
此外,锆氧化物的一次平均粒径(D50)应当为100nm以下,优选50nm以下,更优选30nm以下。这使得可以形成透明性优异的均匀涂膜。这里,平均粒径(D50)是通过激光衍射·光散射法测量的体积平均粒径,并且D50是基于体积的粒度分布的50%处的值。通过使用细颗粒类型的锆氧化物作为原料,可以实现优异的透明性。
[磷酸化合物]
作为用于本发明的磷酸化合物,可以示例正磷酸、偏磷酸、多磷酸、亚磷酸、膦酸以及它们的衍生物。多磷酸的具体实例包括焦磷酸、三磷酸、和其中四个以上的磷酸缩合而成的多磷酸等。作为它们的衍生物,可以示例正磷酸、偏磷酸、多磷酸、亚磷酸、和膦酸的盐、(部分)酯化合物、卤化物(氯化物等)、和脱水物(五氧化二磷等)等。此外,作为膦酸的衍生物,可以示例与膦酸(H-P(=O)(OH)2)中的磷原子直接键合的氢原子被可以具有各种官能团的烷基取代的化合物(例如,次氨基三(亚甲基膦酸)、N,N,N’,N’-乙二胺四(亚甲基膦酸)等)、它们的盐、(部分)酯化合物、卤化物以及脱水物。此外,可以使用如磷酸化淀粉等具有磷原子的有机高分子。这些磷酸化合物可以单独使用或以两种以上的组合使用。
本发明中,特别期望使用正磷酸、偏磷酸、多磷酸和环状多磷酸中的至少一种。
[胺化合物]
作为胺化合物,本发明使用以往公知的胺化合物如单胺、多胺、多胺化合物、氨基糖化合物或氨基酸化合物。
作为单胺,尽管不限于此,但可以示例伯胺,例如甲胺、乙胺、正丙胺、异丙胺、正丁胺、异丁胺、仲丁胺、叔丁胺、戊胺、异戊胺、环己胺、苄胺和烯丙胺;仲胺,如二甲胺、甲基乙胺、二乙胺、甲基丙胺、甲基异丙胺、乙基丙胺、甲基丁胺、乙基丁胺、二正丙胺和二烯丙胺;和叔胺,如三甲胺、三乙胺、二甲基乙胺、二乙基甲胺和二异丙基乙胺。
作为多胺,尽管不限于此,但可以示例二胺,例如乙二胺、1,2-丙二胺、三亚甲基二胺、四亚甲基二胺、五亚甲基二胺、六亚甲基二胺、双(二甲基氨基)甲烷、N,N-二甲基乙二胺、N,N’-二甲基乙二胺、N-乙基乙二胺、N-甲基-1,3-丙二胺、1,3-二氨基戊烷、N-异丙基乙二胺、N-异丙基-1,3-丙二胺、N,N,N’,N’-四甲基乙二胺、N,N,N’,N’-四甲基三亚甲基二胺、N,N,N’,N’-四甲基-1,2-丙二胺、N,N,2,2-四甲基-1,3-丙二胺、N,N,N’,N’-四甲基四亚甲基二胺、N,N-二甲基-1,6-二氨基己烷、N,N,N’,N’-四甲基-2,2-二甲基-1,3-丙二胺、和N,N,N’,N’-四甲基六亚甲基二胺;和在分子中具有三个以上的氨基的多胺,例如二乙烯三胺、双(3-氨基丙基)胺、N-(3-氨基丙基)-1,3-丙二胺、3,3’-二氨基-N-甲基二丙胺、亚精胺、N,N,N’,N’,N”-五甲基二乙烯三胺、3,3’-亚氨基双(N,N-二甲基丙胺)、双(六亚甲基)三胺、三乙烯三胺、N,N’-双(3-氨基丙基)乙二胺和四乙烯五胺。
作为多胺化合物,可以示例聚亚烷基亚胺、聚二烯丙基胺、聚烯丙基胺、聚乙烯胺和聚乙烯亚胺。期望多胺化合物的重均分子量在1,600~25,000的范围内。
作为氨基糖化合物,可以示例单糖类,如葡糖胺、半乳糖胺和甘露糖胺;和多糖类,如几丁质和壳聚糖。
作为氨基酸化合物,可以示例α-氨基酸,如甘氨酸、丙氨酸、丝氨酸、色氨酸、谷氨酰胺和精氨酸;β-氨基酸,如β-丙氨酸等;γ-氨基酸,如γ-氨基丁酸等;和氨基酸的聚合物等。
本发明中,特别期望使用聚烯丙基胺、聚乙烯亚胺、壳聚糖、甘氨酸和精氨酸中的至少一种。
[组合物的制备]
本发明的阻气性涂料组合物为水系或溶剂系的组合物,只要其包含上述金属氧化物、磷酸化合物和胺化合物即可,但优选为水性组合物。
为了制备阻气性涂料组合物,期望金属氧化物以其中金属氧化物细颗粒作为分散相存在的溶胶的形式使用。
此外,尽管对于使用胺化合物的本发明不是必须的,但是金属氧化物也可以以分散液的形式使用,该分散液通过在胶溶剂的存在下使其中金属氧化物细颗粒作为分散相存在的溶胶分散而具有优异的透明性和粘度稳定性。作为胶溶剂,可以示例硝酸、盐酸、高氯酸、甲酸、乙酸、柠檬酸、苹果酸和乳酸。其中,期望使用分散液形式的乙酸、盐酸、硝酸或柠檬酸。通过使用分散液,金属氧化物可以容易且均匀地分散在阻气性涂料组合物中或通过使用阻气性涂料组合物形成的阻气性涂膜中。
当硝酸(浓度=1mol/L)用作胶溶剂(浓度=1mol/L)时,期望硝酸的添加量为相对于21.9g其中锆氧化物作为分散相存在的溶胶为0.01~30g、特别是2.68~5.36g。
接下来,将磷酸化合物、胺化合物和锆氧化物在能够溶解磷酸化合物和胺化合物的溶剂中混合在一起。
作为水性介质,可以使用任何已知的水性介质,例如蒸馏水、离子交换水或纯水。与已知的水性组合物一样,水性介质可以包含有机溶剂,例如醇、多元醇、或它们的衍生物。这种共溶剂的用量可以为相对于水性组合物中树脂组分为1~90重量%。在包含上述范围内的量的溶剂时,成膜性改善。有机溶剂应当优选是两性的。其实例包括甲醇、乙醇、异丙醇、正丁醇、甲基乙基酮、丁基溶纤剂、丙二醇单丙基醚、乙二醇单丁基醚、丙二醇单甲基醚、丙二醇单丁基醚、二丙二醇单甲基醚、二丙二醇单丁基醚、三丙二醇单甲基醚和3-甲基3-甲氧基丁醇。
在制备本发明的阻气性涂料组合物时,磷酸化合物和胺化合物可以以它们不损害氧气阻隔性和水蒸气阻隔性的范围内的量添加。磷酸化合物期望以如下的量添加:金属氧化物和磷酸化合物在荧光X-射线测量中的净强度比P(P–kα)/M(M–kα)落在0.5~10的范围内。当锆氧化物用作金属氧化物时,磷酸化合物期望以如下的量使用:锆氧化物和磷酸化合物在荧光X-射线测量中的净强度比P(P–kα)/Zr(Zr–kα)落在2.8~8.0的范围内、特别是2.8~7.1的范围内。
此外,在制备阻气性涂料组合物时,胺化合物的添加量尽管依赖于所使用的胺化合物的种类,但期望相对于100质量份金属氧化物为0.1~100质量份、特别是1.0~40质量份。当其添加量小于上述范围时,与当添加量在上述范围内时获得的作用和效果相比,由添加胺化合物产生的作用和效果是不充分的。另一方面,即使当其添加量大于上述范围时,也没有获得改善的效果,此外,与当其添加量在上述范围内时获得的涂膜的阻隔结构相比,涂膜的阻隔结构会变得有缺陷。
除了上述组分之外,阻气性涂料组合物还可以包含交联剂、金属配合物、高分子化合物、填料、增塑剂、抗氧化剂、紫外线吸收剂、阻燃剂、着色剂等。
(阻气性涂膜)
由本发明的阻气性涂料组合物形成的阻气性涂膜包含上述金属氧化物、磷酸化合物和胺化合物。具体来说,阻气性涂膜形成其中形成磷酸酯键,金属氧化物和磷酸化合物交联,并且胺化合物在与金属离子和磷酸反应时形成铵盐化合物的复合结构。
因此,由本发明的阻气性涂料组合物形成的涂膜的特征在于,在涂膜的FT-IR测量中,在800~1400cm-1范围内的红外线吸收光谱中,其具有在1000~1050cm-1范围内红外线吸收成为最大的吸收峰,并且进一步地,其另一特征在于,在阻气性涂膜的X射线光电子能谱(XPS)中的氮(N)的结合能量(400~405eV)的范围内具有最大峰。
此外,期望本发明的阻气性涂料组合物的涂膜的金属氧化物和磷酸化合物在荧光X-射线测量中的净强度比P(P–kα)/M(M–kα)为0.5~10,当金属氧化物为锆氧化物时,在2.8~8.0的范围内、特别是在2.8~7.1的范围内。当净强度比P(P–kα)/M(M–kα)落在上述范围内时,磷酸化合物充分且有效地与涂膜中的金属氧化物的羟基反应,使得涂膜能够变得均匀且致密,因而使得涂膜表现出优异的氧气阻隔性和水蒸气阻隔性。即,当在荧光X-射线测量中的净强度比小于上述范围且磷酸化合物的量不充分时,金属颗粒不能彼此结合至充分的程度,金属颗粒表面上的羟基的量增加,由此氧气阻隔性和水蒸气阻隔性会降低。另一方面,当在荧光X-射线测量中的净强度比大于上述范围时,磷酸化合物过量,源自磷酸的羟基的量增加,在此情况下,氧气阻隔性和水蒸气阻隔性也会降低。
(阻气性层叠体)
本发明的阻气性层叠体为在基材的至少一个表面上具有由上述阻气性涂膜形成的阻气层的层叠体。优选地,如图1所示,阻气性层叠体具有经由稍后将描述的锚固层2形成在基材1上的阻气层3。锚固层2为优异地密合至塑料基材1的涂膜。在涂膜上形成阻气层的情况下,大幅改善阻气层和塑料基材之间的层间密合性。因此,即使当层叠体进行蒸煮灭菌时,也有效地防止阻气层从基材剥离。
此外,在如图2所示的本发明的阻气性层叠体中,如未拉伸聚丙烯树脂膜等热塑性树脂的耐湿性树脂层4可以优选形成在阻气层3上。
在本发明的阻气性层叠体中,阻气层本身具有充分程度的阻气性,具体地,氧气阻隔性和水蒸气阻隔性。当阻气性层叠体包括12μm厚的双轴拉伸聚酯的基材膜、通过以1.0g/m2的量涂布而在其上形成的阻气性涂膜、以及厚度为50μm的未拉伸聚丙烯膜时,表现出优异的氧气阻隔性和耐蒸煮性,其中透氧量(根据JIS K-7126)为25cc/m2·天·atm(40℃90%RH)以下,水蒸气透过量为5.5g/m2·天(40℃90%RH)以下。
此外,由此构成的阻气性层叠体表现出其中全光线透过量为85%以上、雾度为30%以下的优异的透明性。
[基材]
作为阻气性层叠体的基材,可以使用如热塑性树脂或热固性树脂等树脂或者如纸或无纺布等纤维的任何已知的基材。优选地,可使用通过如挤出成形、注塑成形、吹塑成形、拉伸吹塑成形或压力成形等手段由可热成形的热塑性树脂制得的膜或片材。或者可以使用瓶状、杯状、盘状、罐状等的任何包装材料。
作为构成基材的热塑性树脂,可以示例烯烃系共聚物,如低密度、中密度或高密度聚乙烯、线性低密度聚乙烯、聚丙烯、乙烯-丙烯共聚物、乙烯-丁烯共聚物、离聚物、乙烯-乙酸乙烯酯共聚物和乙烯乙烯醇共聚物;聚酯,如聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、聚对苯二甲酸乙二醇酯/间苯二甲酸乙二醇酯和聚萘二甲酸乙二醇酯;聚酰胺,如尼龙6、尼龙6,6、尼龙6,10和己二酰间苯二甲胺;苯乙烯系共聚物,如聚苯乙烯、苯乙烯-丁二烯嵌段共聚物、苯乙烯-丙烯腈共聚物和苯乙烯-丁二烯-丙烯腈共聚物(ABS);氯乙烯系共聚物,如聚氯乙烯和氯乙烯-乙酸乙烯酯共聚物;丙烯酸系共聚物,如聚甲基丙烯酸甲酯和甲基丙烯酸甲酯·丙烯酸乙酯共聚物;和聚碳酸酯。
本发明特别优选使用聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯或聚丙烯的片材。
这些热塑性树脂可以单独使用或作为其两种以上的共混物使用。或者可以使不同的树脂以层叠体的形式存在。塑料基材可以呈现单层构造,或者可以是通过例如同时熔融挤出或通过任何其它层叠获得的两层以上的层叠体。
可熔融成形的热塑性树脂可以根据需要以相对于100质量份树脂在0.001份~5.0份的范围内的总量共混有一种或两种以上的添加剂,例如颜料、抗氧化剂、抗静电剂、紫外线吸收剂和润滑剂。
此外,为了增强容器,热塑性树脂可以以相对于100质量份热塑性树脂为2~150质量份的总量进一步共混有一种或两种以上的纤维增强材料,如玻璃纤维、芳香族聚酰胺纤维、碳纤维、纸浆或棉花·棉绒(cotton·linter);粉末状增强材料,如炭黑或白碳;和片状增强材料,如玻璃片或铝片。此外,为了增加量,根据本身已知的配方,热塑性树脂可以以相对于100质量份热塑性树脂为5~100质量份的总量共混有一种或两种以上的重质或软质碳酸钙、云母、滑石、高岭土、石膏、粘土、硫酸钡、氧化铝粉末、二氧化硅粉末和碳酸镁。
此外,为了改善阻气性,热塑性树脂可以没有任何问题地根据本身已知的配方以相对于100质量份热塑性树脂为5~100质量份的总量共混有鳞片状无机细粉末如水溶胀性云母或粘土。
类似地,为了改善阻气性,可通过物理或化学气相沉积法在塑料基材上设置硅氧化物或铝氧化物的无机物系的薄层。
基材可以为例如最终膜、片或容器等成形品,或者待成形为容器的、其上预先形成有膜的预成形体。预成形体的实例包括待进行双轴拉伸吹塑成形的有底或无底筒状型坯,待成形为塑料罐的管,待进行真空成形、气压成形或模塞助压成形的片材,热封盖和用于制袋的膜。
[锚固层]
作为根据需要成形在基材的表面上的锚固层,可以使用已经用于阻气性层叠体、以往公知的、包含多元醇和异氰酸酯化合物的聚氨酯系树脂的锚固层。然而,优选使用本发明人已经提出的、包含聚氨酯系树脂和硅烷偶联剂的锚固层。
<聚氨酯系树脂>
作为用于构成锚固层的聚氨酯系树脂,可以使用迄今用作锚固层的已知聚氨酯系树脂。然而,根据本发明,期望使用玻璃化转变温度(Tg)为80℃以上、特别是在80~120℃范围内的聚氨酯系树脂。当玻璃化转变温度低于上述范围时,锚固层的耐热性倾向于变得次于当玻璃化转变温度落入上述范围内时获得的耐热性,并且此外,当锚固层和阻气层之间的收缩系数由于加热而变得不同时,阻气层倾向于破裂并且阻隔性降低。
作为聚氨酯系树脂中的主要组分的多元醇组分,可以示例二醇、聚酯多元醇、聚醚多元醇、丙烯酸系多元醇及其氨基甲酸酯改性产物。然而,这里特别希望使用二醇。
聚酯多元醇的玻璃化转变温度应当优选-50℃~100℃、更优选-20℃C~80℃。此外,聚酯多元醇的数均分子量应当优选50~100,000、更优选50~80,000。
作为二醇,可以示例乙二醇、丙二醇、二甘醇、丁二醇、新戊二醇和1,6-己二醇。
作为多元羧酸,可以示例芳香族多元羧酸,如间苯二甲酸、对苯二甲酸和萘二甲酸;以及脂肪族多元羧酸,如己二酸、壬二酸、癸二酸和环己烷二羧酸。
作为聚氨酯系树脂的固化剂的异氰酸酯组分,可以使用芳香族二异氰酸酯、脂环族二异氰酸酯或脂肪族二异氰酸酯。
作为芳香族二异氰酸酯,可以示例甲苯二异氰酸酯(2,4-或2,6-甲苯二异氰酸酯或其混合物)(TDI)、苯二异氰酸酯(间-、对-苯二异氰酸酯或其混合物)、4,4’-二苯基二异氰酸酯、1,5-萘二异氰酸酯(NDI)、二苯甲烷二异氰酸酯(4,4’-、2,4’-或2,2’-二苯基甲烷二异氰酸酯或其混合物)(MDI)、4,4’-甲苯胺二异氰酸酯(TODI)和4,4’-二苯基醚二异氰酸酯。
作为芳香族-脂肪族二异氰酸酯,可以示例二甲苯二异氰酸酯(1,3-或1,4-二甲苯二异氰酸酯或其混合物)(XDI)、四甲基二甲苯二异氰酸酯(1,3-或1,4-四甲基二甲苯二异氰酸酯或其混合物)(TMXDI)和ω,ω’-二异氰酸酯-1,4-二乙基苯。
作为脂环族二异氰酸酯,可以示例1,3-环戊烯二异氰酸酯、环己烷二异氰酸酯(1,4-环己烷二异氰酸酯、1,3-环己烷二异氰酸酯)、3-异氰酸酯甲基-3,5,5-三甲基环己基异氰酸酯(异佛尔酮二异氰酸酯,IPDI)、亚甲基双(环己基异氰酸酯)(4,4’-、2,4’-或2,2’-亚甲基双(环己基异氰酸酯))(氢化MDI)、甲基环己烷二异氰酸酯(甲基-2,4-环己烷二异氰酸酯、甲基-2,6-环己烷二异氰酸酯)和双(异氰酸酯甲基)环己烷(1,3-或1,4-双(异氰酸酯甲基)环己烷或其混合物)(氢化XDI)。
作为脂肪族二异氰酸酯,可以示例三亚甲基二异氰酸酯、1,2-亚丙基二异氰酸酯、亚丁基二异氰酸酯(四亚甲基二异氰酸酯、1,2-亚丁基二异氰酸酯、2,3-亚丁基二异氰酸酯、1,3-亚丁基二异氰酸酯)、六亚甲基二异氰酸酯、五亚甲基二异氰酸酯、2,4-,4-或2,2,4-三甲基六亚甲基二异氰酸酯和2,6-二异氰酸酯甲基咖啡酸酯。
作为多异氰酸酯组分,可以使用多官能多异氰酸酯化合物,如源自上述多异氰酸酯单体、缩二脲或脲基甲酸酯的异氰脲酸酯,或通过与三官能或更高官能的多元醇化合物如三羟甲基丙烷或甘油反应获得的具有末端异氰酸酯基团的多官能多异氰酸酯化合物。
期望多异氰酸酯组分具有50℃以上的玻璃化转变温度(Tg)和400以上的数均分子量(Mn),特别是60℃以上的玻璃化转变温度(Tg)和500以上的数均分子量(Mn)。
在上述异氰酸酯组分中,本发明优选使用二甲苯二异氰酸酯。
<硅烷偶联剂>
作为用于锚固层的硅烷偶联剂,可以优选使用环氧硅烷系偶联剂。
作为环氧硅烷系偶联剂,可以使用β-(3,4-环氧环己基)乙基三甲氧基硅烷、3-环氧丙氧基丙基甲基二甲氧基硅烷、3-环氧丙氧基丙基甲基二乙氧基硅烷、3-环氧丙氧基丙基三乙氧基硅烷和3-环氧丙氧基丙基三甲氧基硅烷。
作为硅烷偶联剂,可以进一步示例可以根据需要使用的四甲氧基硅烷、四乙氧基硅烷、3-氨基丙基三甲氧基硅烷、3-氨基丙基三乙氧基硅烷和3-异氰酸酯丙基三乙氧基硅烷。
此外,从改善耐热水和密合力的角度来看,本发明中使用的硅烷偶联剂可以根据需要进行水解和缩合反应。
[锚固层形成用组合物]
根据本发明,期望锚固层形成用组合物包含上述聚氨酯系树脂和硅烷偶联剂。锚固层形成用组合物可以为水系或溶剂系,但优选为水性组合物。因此,待使用的聚氨酯系树脂应当期望为水溶性或水分散性的。
期望锚固层形成用组合物包含相对于100质量份聚氨酯系树脂(固成分)为1至60质量份的量的环氧硅烷化合物。当环氧硅烷化合物的量小于上述范围时,与环氧硅烷化合物的量在上述范围内的情况相比,在干燥期间不能获得令人满意的抗开裂性。另一方面,即使当环氧硅烷化合物的量大于上述范围时,也不能获得更高的密合性,而是通常会降低耐热水性。
水性介质可以是众所周知的水性介质,如已经用于形成阻气层形成用组合物的水性介质,并且可以包含有机溶剂,如醇、多元醇或其衍生物。
除了上述组分以外,锚固层形成用组合物可以包含以往公知的固化促进催化剂、填料、软化剂、抗老化剂、稳定剂、粘合促进剂、流平剂、消泡剂、增塑剂、无机填料、粘性赋予性树脂、纤维、如颜料等着色剂和可用的时间延长剂。
(阻气性层叠体的制造方法)
在根据本发明的阻气性层叠体的制造方法中,本发明的阻气性涂料组合物可直接涂布在上述基材的至少一个表面上。然而,优选在涂布阻气性涂料组合物之前涂布上述锚固层形成用组合物。
根据组合物中聚氨酯系树脂和硅烷偶联剂的量来确定锚固层形成用组合物的涂布量,并且不能排它性地指定。然而,期望地,锚固层形成用组合物以涂膜的固成分重量计在0.05~1.00g/m2、特别是0.10~0.50g/m2的范围内的量涂布。当锚固层的涂布量小于上述范围时,与该量在上述范围内的情况相比,锚固层通常不能牢固地固定至基材。另一方面,当锚固层的涂布量大于上述范围时,其在经济上变得不利。
尽管取决于所使用的组成和涂布量,但将涂布至基材上的锚固层形成用组合物在80~140℃的温度下干燥1~60秒以从组合物中除去溶剂。因此,即使当基材由具有低熔点的塑料材料如聚丙烯制成时,也可以经济地形成锚固层。
接下来,将阻气性涂料组合物涂布至处于溶剂已从中除去之后的干燥状态的锚固层形成用组合物上。根据组合物中金属氧化物、磷酸化合物和胺化合物的量来确定阻气性涂料组合物的涂布量,并且不能排它性地指定。然而,期望地,阻气性涂料组合物以涂膜的固成分重量计为0.05~2.0g/m2、特别是0.3~1.5g/m2范围内的量涂布。当涂料组合物的涂布量小于上述范围时,不能获得充分程度的阻隔性。即使当涂料组合物的涂布量大于上述范围时,也没有获得特别的优点,而是导致经济上的缺点。
接下来,尽管取决于组合物中金属氧化物、磷酸化合物和胺化合物的组成以及组合物的涂布量,但是将阻气性涂料组合物在80℃~220℃、特别是140℃~220℃的温度下加热1秒至10分钟,从而形成阻气层。这使得可以减小由加热引起的阻气层和锚固层之间的收缩差,并因此改善阻气层的抗开裂性以及极大地改善阻气层和锚固层之间的密合性。因此,即使当层叠体经受蒸煮灭菌时,也可以防止阻气层从基材剥离。
上述锚层形成用组合物和阻气性涂料组合物可以根据常规方法涂布并干燥或热处理。
涂布方法可以为,但不仅限于,喷涂、浸渍或使用棒涂布机、辊涂机或凹版涂布机的涂布。
干燥或加热处理可以通过烘箱干燥(加热)、红外加热或高频加热来进行。
实施例
现在将参考以下实施例更详细地描述本发明;然而,本发明决不限于此。在实施例和比较例中,通过下述方法进行测量和评价。
(实施例1)
作为金属氧化物,使用锆氧化物溶胶(Zirconia Sol,ZSL-10T,非晶质锆氧化物,固成分(以ZrO2换算)=10%,由Daiichi Kigenso Kagaku Kogyo Co.制)。然后,通过使用水/甲醇溶剂,将溶胶调整为使固成分为3.3%且水/甲醇之比为65/35。进一步,以相对于21.9g的锆氧化物溶胶(固成分(以ZrO2换算)=10%)为5.36g的量添加作为胶溶剂的硝酸(浓度=1mol/L,由Wako-Junyaku Co.制),以相对于锆氧化物溶胶的固成分(以ZrO2换算)为7.5phr的量添加聚烯丙基胺(PAA-25,浓度=10%,重均分子量M.W.=25,000,由NittoboMedical Co.制)作为胺化合物,以使得磷酸的非挥发性组分相对于锆氧化物溶胶的固成分(以ZrO2换算)为136phr的量添加磷酸(浓度=85%,由Wako-Junyaku Co.制)作为磷酸化合物。搅拌它们的混合物预定的时间,从而获得阻气性涂料组合物。
(阻气性层叠体的样品的制备方法)
通过使用上述制备的阻气性涂料组合物,以下述的方式制备阻气性层叠体的样品。通过使用棒涂布机,将阻气性涂料组合物以1.0g/m2的量涂布至12μm厚的双轴拉伸聚酯膜(Lumirror P60,由Toray Film Kako Co.制)的基材,随后在220℃的温度下在箱式烘箱中加热并干燥10分钟,从而制备阻气性层叠体的样品。
(阻气性评价用层叠体的样品的制备方法)
通过以下制备阻气性评价用层叠体的样品:通过使用棒涂布机将聚氨酯系粘合剂(Takenate A-315/Takenate A-50,由Mitsui Kagaku Co.制)涂布至已涂布有阻气性涂料组合物的阻气性层叠体的表面上,随后通过使用干燥机干燥。其后,将50μm厚的未拉伸聚丙烯膜(Torayfan ZK401,由Toray Film Kako Co.制)层叠于其上,从而制备实施例1中记载的阻气性层叠体。
(实施例2)
除了作为用于阻气性涂料组合物的胺化合物,以7.5phr的量添加聚烯丙基胺(PAA-01,浓度=10%,重均分子量M.W.=1,600,由Nittobo Medical Co.制)以外,以与实施例1相同的方式制备阻气性层叠体和阻气性评价用层叠体。
(实施例3)
除了作为用于阻气性涂料组合物的磷酸化合物,以110phr的量添加磷酸的非挥发性组分(浓度=75%,由Wako-Junyaku Co.制)以外,以与实施例1相同的方式制备阻气性层叠体和阻气性评价用层叠体。
(实施例4)
除了作为用于阻气性涂料组合物的磷酸化合物,以120phr的量添加磷酸的非挥发性组分(浓度=75%,由Wako-Junyaku Co.制)以外,以与实施例1相同的方式制备阻气性层叠体和阻气性评价用层叠体。
(实施例5)
除了作为用于阻气性涂料组合物的磷酸化合物,以123phr的量添加磷酸的非挥发性组分(浓度=75%,由Wako-Junyaku Co.制)以外,以与实施例1相同的方式制备阻气性层叠体和阻气性评价用层叠体。
(实施例6)
除了作为用于阻气性涂料组合物的磷酸化合物,以140phr的量添加磷酸的非挥发性组分(浓度=75%,由Wako-Junyaku Co.制)以外,以与实施例1相同的方式制备阻气性层叠体和阻气性评价用层叠体。
(实施例7)
除了作为用于阻气性涂料组合物的胺化合物,以15phr的量添加10%水溶液形式的聚乙烯亚胺(重均分子量M.W.=10,000,由Wako-Junyaku Co.制)以外,以与实施例1相同的方式制备阻气性层叠体和阻气性评价用层叠体。
(实施例8)
除了作为用于阻气性涂料组合物的胺化合物,以15phr的量添加10%水溶液形式的甘氨酸(由Wako-Junyaku Co.制)以外,以与实施例1相同的方式制备阻气性层叠体和阻气性评价用层叠体。
(实施例9)
除了作为用于阻气性涂料组合物的胺化合物,以15phr的量添加10%水溶液形式的D-精氨酸(由Wako-Junyaku Co.制)以外,以与实施例1相同的方式制备阻气性层叠体和阻气性评价用层叠体。
(实施例10)
除了作为用于阻气性涂料组合物的胺化合物,以15phr的量添加10%水溶液形式的L-精氨酸(由Wako-Junyaku Co.制)以外,以与实施例1相同的方式制备阻气性层叠体和阻气性评价用层叠体。
(实施例11)
除了不向阻气性涂料组合物中添加胶溶剂以外,以与实施例1相同的方式获得阻气性层叠体和阻气性评价用层叠体。
(实施例12)
作为金属氧化物,使用锆氧化物溶胶(Zirconia Sol,ZSL-00120A,晶质锆氧化物,固成分(以ZrO2换算)=30%,由Daiichi Kigenso Kagaku Kogyo Co.制)。然后,通过使用水/甲醇溶剂,将溶胶调整为使固成分为3.0%且水/甲醇之比为65/35。进一步,以相对于锆氧化物溶胶的固成分(以ZrO2换算)为7.5phr的量添加聚烯丙基胺(PAA-25,浓度=10%,重均分子量M.W.=25,000,由Nittobo Medical Co.制)作为胺化合物,以使得磷酸的非挥发性组分相对于锆氧化物溶胶的固成分(以ZrO2换算)为58phr的量添加磷酸(浓度=85%,由Wako-Junyaku Co.制)作为磷酸化合物。搅拌它们的混合物预定的时间,从而获得阻气性涂料组合物。以与实施例1相同的方式制备阻气性层叠体和阻气性评价用层叠体。
(比较例1)
除了作为用于阻气性涂料组合物的胶溶剂,以相对于21.9g的锆氧化物溶胶(固成分(以ZrO2换算)=10%)为2.68g的量添加硝酸(浓度=1mol/L,由Wako-Junyaku Co.制),且不添加胺化合物以外,以与实施例1相同的方式制备阻气性层叠体和阻气性评价用层叠体。
(比较例2)
除了作为用于阻气性涂料组合物的磷酸化合物,以159phr的量添加磷酸的非挥发性组分(浓度=85%,由Wako-Junyaku Co.制)以外,以与比较例1相同的方式制备阻气性层叠体和阻气性评价用层叠体。
(比较例3)
除了作为用于阻气性涂料组合物的胶溶剂,以相对于21.9g的锆氧化物溶胶(固成分(以ZrO2换算)=10%)为5.36g的量添加硝酸(浓度=1mol/L,由Wako-Junyaku Co.制),不添加胺化合物,并且作为磷酸化合物,以97phr的量添加磷酸的非挥发性组分(浓度=85%,由Wako-Junyaku Co.制)以外,以与实施例12相同的方式制备阻气性层叠体和阻气性评价用层叠体。
(参考例1)
除了使用12μm厚的双轴拉伸聚酯膜(Lumirror P60,由Toray Film Kako Co.制)作为基材,而不在其上涂布阻气性涂料组合物以外,以与实施例1相同的方式制备阻气性评价用层叠体。
(评价方法)
通过下述评价方法来评价阻气性层叠体和阻气性评价用层叠体,从而获得如表1所示的评价结果。
[氧气透过度]
实施例、比较例和参考例中制备的各阻气性评价用层叠体的性质通过使用氧气透过率测量装置(OX-TRAN 2/21,由Modern Control Co.制)在温度为40℃且相对湿度为90%的条件下测量。
[水蒸气透过度]
实施例、比较例和参考例中制备的各阻气性评价用层叠体的性质通过使用水蒸气透过率测量装置(PERMATRAN-W 3/31,由Modern Control Co.制)在温度为40℃且相对湿度为90%的条件下测量。
[光学特性]
实施例、比较例和参考例中制备的各阻气性层叠体通过使用彩色计算机(SM-4,由Suga Shikenki Co.制)以测量的光线在聚酯膜基材上入射的方式测量它们的全光线透过度(TT:%)和雾度(Hz:%)。
[红外线吸收光谱]
对于实施例、和比较例中制备的各阻气性层叠体,通过使用傅里叶变换红外分光光度计(FT/IR-6600,由Nihon Bunkoh Co.制)测量涂布至聚酯基材上的阻气性涂膜的红外线吸收光谱。
<FT-IR装置的测量条件>
装置:FT/IR-6600,由JASCO制
测量条件:
[荧光X射线评价]
作为实施例和比较例中制备的阻气性层叠体所含元素的评价方法,可以通过使用市售的荧光X射线分析仪测定磷元素和锆元素。从阻气性层叠体的测量获得的元素的净强度可以被拾取用于P和Zr,并且表示为P/Zr,以计算用于评价的膜中金属元素的含量比。
<荧光X射线分析仪的测量条件>
装置:ZSX100e,由Rigaku Denki Co.制
测定条件:
测量对象 Zr-Kα射线、P-Kα射线
测量直径 10mm
测量用X射线Rh(4.0kw)50kv
72mA(2θ=0~90)
膜测量面 通过使X射线落在涂布阻挡涂层的面上来测量。
[X射线光电子分光法]
作为实施例和比较例中制备的阻气性层叠体中所含元素的化学键状态的评价方法,用X射线照射样品表面,并且测量所产生的光电子的能量,以分析构成样品的元素和电子的状态。通过使用市售的X射线光电子分光装置来分析氮元素和锆元素。分析从阻气性层叠体的测量获得的元素的结合能量,其中Zr3d5/2的峰位置为185.0,并且评价涂膜中氮元素的结合状态。用于校正峰的Zr3d5/2的数值参见文献J.Inorg.Nucl.Chem.Vol.43,No.12,pp.3329-3334,1981。
<X射线光电子分光装置的测量条件>
使用的装置:K-ALPHA,由Thermo Fisher SCIENTIFIC Co.制
测量条件:
表1示出实施例、比较例和参考例的测量结果和评价结果。
[表1中的缩写]
ZSL-10T:非晶质锆氧化物
ZSL-00120A:晶质锆氧化物
HNO3:硝酸
PAA:聚烯丙基胺
PEI:聚乙烯亚胺
Gly:甘氨酸
Arg:精氨酸
TT:全光线透过度
Hz:雾度
P/Zr:涂膜中来自磷酸化合物的磷元素(P)和金属氧化物中的锆元素(Zr)的含量比
表1中,符号“-”是指“未添加”、“未进行”、“未检出”等。
产业上的可利用性
本发明的阻气性涂料组合物使得可以形成特征在于优异的氧气阻隔性和水蒸气阻隔性的涂膜,并且可以有利地用作制造具有高阻挡性的透明包装的材料。
附图标记说明
1 基材 2 锚固层
3 阻气层(阻气性膜)
4 耐湿性树脂层
Claims (10)
1.一种阻气性涂料组合物,其包含金属氧化物、磷酸化合物和胺化合物,所述胺化合物为多胺化合物、氨基糖化合物和氨基酸化合物中的至少一种,
所述多胺化合物的重均分子量在1,600~25,000的范围内,
所述胺化合物的添加量相对于100质量份所述金属氧化物为0.1~100质量份。
2.根据权利要求1所述的阻气性涂料组合物,其中所述胺化合物为聚烯丙基胺、聚乙烯亚胺、壳聚糖、甘氨酸和精氨酸中的至少一种。
3.根据权利要求1或2所述的阻气性涂料组合物,其中所述金属氧化物为锆氧化物。
4.根据权利要求1或2所述的阻气性涂料组合物,其中所述磷酸化合物为正磷酸、偏磷酸和多磷酸中的至少一种。
5.根据权利要求4所述的阻气性涂料组合物,其中所述磷酸化合物为环状多磷酸。
6.一种阻气性层叠体,其在基材上具有根据权利要求1至5中任一项所述的阻气性涂料组合物的涂膜。
7.根据权利要求6所述的阻气性层叠体,其中所述涂膜具有使得在其红外线吸收光谱中在1000~1050cm-1的范围内红外线吸收成为最大的吸收峰。
8.根据权利要求6或7所述的阻气性层叠体,其中所述涂膜具有使得通过XPS测量的N的结合能量在400~405eV的范围内成为最大的峰。
9.根据权利要求6或7所述的阻气性层叠体,其中锚固层设置在所述基材和所述涂膜之间。
10.根据权利要求6或7所述的阻气性层叠体,其中当所述基材为12μm厚的双轴拉伸聚酯、所述涂膜以1.0g/m2的量形成在所述基材上、和在所述涂膜上配置50μm厚的未拉伸聚丙烯膜时,40°℃90%RH下的透氧量为25cc/m2·天·atm以下,40℃90%RH下的水蒸气透过量为5.5g/m2·天以下。
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