CN1312207C - 吸氧树脂组合物和层压体 - Google Patents
吸氧树脂组合物和层压体 Download PDFInfo
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- CN1312207C CN1312207C CNB038226316A CN03822631A CN1312207C CN 1312207 C CN1312207 C CN 1312207C CN B038226316 A CNB038226316 A CN B038226316A CN 03822631 A CN03822631 A CN 03822631A CN 1312207 C CN1312207 C CN 1312207C
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- resin
- oxygen
- oxygen uptake
- resin combination
- copolymer
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Abstract
本发明的目的是提供一种吸氧树脂组合物,它具有高的吸氧性和能长时间段地吸收氧气。本发明提供一种吸氧树脂组合物,它包括通过聚合具有2-8个碳原子的烯烃而获得的聚烯烃树脂(A),树脂(B)和过渡金属催化剂(C),其中所述树脂(B)是除了树脂(A)以外的树脂,且起到树脂(A)氧化的引发物的作用,其中树脂(B)分散在树脂(A)的基体内,以便当吸氧树脂组合物与氧气接触时,引起基体树脂(A)的氧化反应并进而吸收氧气。该吸氧树脂组合物具有高的吸氧性且由于氧气被吸附在树脂(A)内,因此在成本上具有优势。
Description
(发明背景)
本发明涉及吸氧树脂组合物及其层压体。
最近,各种塑料容器由于它的诸如轻质、透明和容易模塑之类的优点,已被用于包装。
由于塑料容器的氧气阻挡性能低于金属容器和玻璃容器,因此塑料容器的问题在于,容器的内容物变性及其风味下降。
为了防止这些问题,塑料容器壁具有多层结构,其中至少一层由氧气阻挡性能优良的树脂如乙烯/乙烯醇共聚物制造。存在其它种类的容器,其具有吸氧层用以吸收残留在容器内的氧气以及从外部渗透到容器内的氧气。形成吸氧层所使用的氧气吸收剂(脱氧剂(disoxidant))包括,例如主要含还原物质如铁粉的那些(参见例如,日本专利公报Kokoku No.Sho 62-1824)和含氧气清除剂的那些,所述氧气清除剂由烯键式不饱和烃和过渡金属催化剂组成(日本专利公报KokaiNos.2001-39475和Hei5-115776以及日本专利Kohyo No.Hei8-502306)。
然而,尽管其中吸氧剂如铁粉被掺入到形成容器壁用包装材料所使用的树脂内的方法,在吸氧能力方面是满意的,但该包装材料的使用局限于其中不要求透明度高的包装领域,这是因为树脂被着成特殊的色泽所致。在其中使用由烯键式不饱和烃和过渡金属催化剂组成的氧气清除剂的方法中,必须使用相对大量的烯键式不饱和烃,这是因为烯键式不饱和烃本身吸收氧气,显示出氧气阻挡性能所致。然而,当增加烯键式不饱和烃的相对含量时,出现其中树脂组合物的模塑性和透明度劣化的问题。在这些条件下有效地吸收氧气的时间段有限。因此,该方法不可能满足长时间段地储存的要求。另外,因吸收氧气引起着色和气味。
(发明公开)
在以上所述的情况下,本发明的目的是提供一种吸氧树脂组合物,它具有高的吸氧性,能长时间地吸收氧气,且没有因吸收氧气而引起着色或气味。
为了解决这一问题,本发明者研究之后,发现通过形成含特定量的树脂(A)、树脂(B)和过渡金属催化剂(C)的树脂组合物,可显著改进树脂组合物的氧气吸收性,其中所述树脂(A)通过聚合具有2-8个碳原子的烯烃而获得,所述树脂(B)是除了树脂(A)以外的树脂,且起到树脂(A)氧化的引发物的作用,由于树脂(B)起到聚烯烃树脂(A)氧化的引发物作用,结果聚烯烃树脂(A)吸收氧气。基于这一发现,从而完成本发明。
于是,本发明提供一种吸氧树脂组合物,它包括通过聚合具有2-8个碳原子的烯烃而获得的聚烯烃树脂(A),树脂(B)和过渡金属催化剂(C),其中所述树脂(B)是除了树脂(A)以外的树脂,且起到树脂(A)氧化的引发物的作用,其中树脂(B)分散在树脂(A)的基体内,以便当吸氧树脂组合物与氧气接触时,引起基体树脂(A)的氧化反应并进而吸收氧气。
本发明还提供一种层压体,它具有含以上所述的吸氧树脂组合物的至少一层。
具体地说,本发明公开了以下内容:
1.一种吸氧树脂组合物,它包括通过聚合具有2-8个碳原子的烯烃而获得的聚烯烃树脂(A),树脂(B)和过渡金属催化剂(C),其中所述树脂(B)是除了树脂(A)以外的树脂,且起到树脂(A)氧化的引发物的作用,其中树脂(A)是一种具有乙烯结构的树脂,其侧链中具有苯环的树脂(B)是聚苯乙烯或至少含10重量%苯乙烯部分的苯乙烯共聚物,树脂(B)分散在树脂(A)的基体内,以便当吸氧树脂组合物与氧气接触时,引起基体树脂(A)的氧化反应并进而吸收氧气。
2.上款1的吸氧树脂组合物,其中过渡金属催化剂(C)包含在至少树脂(A)内。
3.上款1或2的吸氧树脂组合物,其中具有乙烯结构的树脂是低密度聚乙烯或线性低密度聚乙烯。
4.上款1或2的吸氧树脂组合物,其中所述组合物中树脂(A)的含量为90-99wt%。
5.上款1或2的吸氧树脂组合物,其中所述组合物中树脂(B)的含量为1.0-10wt%。
6.上款1或2的吸氧树脂组合物,其中苯乙烯共聚物是嵌段共聚物。
7.上款1或2的吸氧树脂组合物,其中苯乙烯共聚物是在分子端部分具有聚苯乙烯嵌段的嵌段共聚物。
8.上款1或2的吸氧树脂组合物,其中苯乙烯共聚物是具有异戊二烯单元的嵌段共聚物。
9.上款8的吸氧树脂组合物,其中具有异戊二烯单元的嵌段共聚物是苯乙烯/异戊二烯/苯乙烯三嵌段共聚物。
10.上款1或2的吸氧树脂组合物,其中所述组合物含有0.001eq/g或更低的除了苯环中的那些以外的碳碳双键。
11.上款1或2的吸氧树脂组合物,其中基于金属的重量,所述组合物含有10-3000ppm的过渡金属催化剂。
12.一种吸氧片材,它含有上款1-11中任何一项的吸氧树脂组合物。
13.一种层压体,它具有含上款1-11中任何一项的吸氧树脂组合物的至少一层。
14.上款13的层压体,它进一步具有至少一层氧气阻挡层。
(附图简述)
图1是在其中间层含有本发明的吸氧树脂组合物的瓶体壁的截面的扫描电子显微照片。
(实施本发明的最佳方式)
[吸氧树脂组合物]
本发明的吸氧树脂组合物包括通过聚合具有2-8个碳原子的烯烃而获得的聚烯烃树脂(A),树脂(B)和过渡金属催化剂(C),其中所述树脂(B)是除了树脂(A)以外的树脂,且起到引起树脂(A)氧化的引发物的作用。
通过聚合具有2-8个碳原子的烯烃而获得的聚烯烃树脂(A)包括例如低密度聚乙烯、中密度聚乙烯、高密度聚乙烯、线性低密度聚乙烯、线性甚低密度聚乙烯、等规或间规聚丙烯、乙烯/丙烯共聚物、聚丁烯-1、乙烯/丁烷-1-共聚物、丙烯/丁烷-1-共聚物、乙烯/丙烯/丁烷-1-共聚物、乙烯/乙酸乙烯酯共聚物、离子交联的烯烃共聚物及其共混物。通过接枝改性以上所述的树脂获得的酸改性的烯烃树脂作为具有不饱和羧酸或其衍生物的基础聚合物也是可用的。优选的聚烯烃树脂是在它们的分子结构内具有乙烯结构的乙烯共聚物,如低密度聚乙烯、中密度聚乙烯、高密度聚乙烯、线性低密度聚乙烯、线性甚低密度聚乙烯、乙烯/丙烯共聚物和乙烯/丁烷-1-共聚物。特别优选低密度聚乙烯或线性低密度聚乙烯。可使用这些树脂之一或它们中的两种或多种的结合。
在普通的吸氧剂,如日本专利Kokai No.Hei5-115776中所公开的含烯键式不饱和烃和过渡金属催化剂的氧气清除剂中,氧气的吸收随着烯键式不饱和烃中不饱和键的数量而变化。氧气清除剂通常被掺入到另一热塑性树脂内,这取决于其应用。当氧气清除剂的相对量增加时,树脂组合物的耐久性和模塑性下降和其透明度降低。因此,氧气清除剂的用量有限和树脂组合物的吸氧性也受到限制。
在本发明的吸氧树脂组合物中,树脂(B)优选处于分散在树脂(A)基体内的状态下。树脂(B)以平均粒径优选10微米或更低,更优选5微米或更低的微粒形式被分散。通过均匀分散在树脂(A)基体内的树脂(B)的引发功能,树脂(A)本身起到吸氧剂的作用。亦即,由于基体树脂本身吸收氧气,因此本发明的吸氧树脂组合物能吸收的氧气量远大于普通氧气清除剂所吸收的氧气量。因此,本发明的树脂组合物能比普通氧气清除剂更长时间段地有效吸收氧气。在没有妨碍引发功能且没有损害基体树脂(A)的可模塑性的情况下,树脂(B)的用量尽可能小。本发明的树脂组合物的另一优点是,由于可在商业树脂内吸收氧气因此成本下降。
优选以相对大的用量包含树脂(A),以便使得可能形成基体和通过氧化吸收大量的氧气。树脂(A)的含量优选在90-99wt%范围内,更优选92.5-97.5wt%。优选地,树脂(B)的含量相对低,以便树脂(B)可保持分散在树脂(A)基体内和以便它可充分地显示出它作为树脂(A)氧化的引发物的功能。从膜、片材、杯子、托盘、瓶子或管道的生产中组合物的可模塑性的角度考虑,树脂(B)的含量优选在1.0-10.0wt%范围内,更优选2.5-7.5wt%。可用电子显微镜容易地观察树脂(B)在树脂(A)基体内的分散状态。例如,图1示出了中间层包括下述的树脂组合物的瓶体的截面的扫描电子显微照片(JSM-6300F;JEOL),所述树脂组合物包括100重量份低密度聚乙烯、5重量份苯乙烯/异戊二烯/苯乙烯三嵌段共聚物树脂和过渡金属催化剂。根据图1可了解到,平均粒径为约1微米的树脂(B)颗粒均匀地分散在树脂(A)基体内。
树脂(B)是不同于树脂(A)的树脂,且起到树脂(A)氧化的引发物的作用。树脂(B)包括例如在其主链或侧链内具有脂族碳碳双键的树脂,在其主链内具有叔碳原子的树脂,和在主链内具有活性亚甲基的树脂。
树脂(B)之一或它们的两种或多种的结合可包含在树脂(A)内。
在其主链或侧链内具有脂族碳碳双键的树脂(B)包括含有衍生于直链或环状、共轭或非共轭多烯烃的单元的树脂。
这些单体包括例如共轭二烯烃,如丁二烯和异戊二烯;非共轭线性二烯烃如1,4-己二烯、3-甲基-1,4-己二烯、4-甲基-1,4-己二烯、5-甲基-1,4-己二烯、4,5-二甲基-1,4-己二烯和7-甲基-1,6-辛二烯;非共轭环状二烯烃如甲基四氢茚、5-亚乙基-2-降冰片烯、5-亚甲基-2-降冰片烯、5-亚异丙基-2-降冰片烯、5-亚乙烯基-2-降冰片烯、6-氯甲基-5-异丙烯基-2-降冰片烯和二环戊二烯;和三烯烃如2,3-二亚异丙基-5-降冰片烯、2-亚乙基-3-亚异丙基-5-降冰片烯和2-丙烯基-2,2-降冰片二烯。
聚合物的具体实例包括聚-1,2-丁二烯、聚-1,4-丁二烯、聚-1,2-异戊二烯、聚-1,4-异戊二烯、苯乙烯/丁二烯共聚物、苯乙烯/异戊二烯共聚物和乙烯/丙烯/二烯烃共聚物。
作为在主链上具有叔碳原子的树脂(B),优选使用含有衍生于具有3-20个碳原子的α-烯烃的单元的聚合物或共聚物,或者在其侧链上具有苯环的聚合物或共聚物。α-烯烃的具体实例包括丙烯、1-丁烯、4-甲基-1-戊烯、1-己烯、1-庚烯、1-辛烯、1-壬烯、1-癸烯、1-十一碳烯、1-十二碳烯、1-十三碳烯、1-十四碳烯、1-十五碳烯、1-十六碳烯、1-十七碳烯、1-十九碳烯、1-二十碳烯、9-甲基-1-癸烯、11-甲基-1-十二碳烯和12-乙基-1-十四碳烯。特别地,聚合物的具体实例包括聚丙烯、聚-1-丁烯、聚-1-己烯、聚-1-辛烯、乙烯/丙烯共聚物、乙烯/丁烷-1-共聚物和乙烯/丙烯/1-丁烷共聚物。在其侧链上具有苯环的单体包括链烯基苯如苯乙烯、3-苯基丙烯和2-苯基-2-丁烯。聚合物的具体实例包括聚苯乙烯和苯乙烯共聚物。
在主链上具有活性亚甲基的树脂(B)是在其主链上具有吸电子基团,尤其是羰基,和相邻的亚甲基的树脂。具体地,树脂(B)包括一氧化碳和烯烃的共聚物,尤其是一氧化碳/乙烯共聚物。
作为树脂(B),从其作为在树脂(A)的氧化中的引发物的功能的角度考虑,特别优选在侧链上具有苯环的聚苯乙烯或苯乙烯共聚物。
在苯乙烯共聚物中,鉴于自由基的形成效率,苯乙烯部分的含量优选为苯乙烯共聚物的10wt%或更多,和更优选为苯乙烯共聚物的15-50wt%。
当苯乙烯共聚物是嵌段共聚物时,它们具有的优点是与树脂(A)的相容度高且分散度高。
从树脂组合物的机械性能的角度考虑,苯乙烯共聚物优选是在分子的末端部分具有聚苯乙烯嵌段的嵌段共聚物。从对树脂(A)的引发效果角度考虑,苯乙烯共聚物优选是具有异戊二烯单元的嵌段共聚物。
亦即,树脂(B)优选是苯乙烯共聚物如苯乙烯/异戊二烯共聚物。它们特别优选是属于苯乙烯/异戊二烯共聚物的苯乙烯/异戊二烯/苯乙烯三嵌段共聚物。
鉴于在形成树脂组合物过程中的热稳定性和在树脂(A)的氧化上引发物的影响,在树脂(B)内包括的在其主链或侧链上具有碳碳双键的树脂、在其主链内具有叔碳原子的树脂,和在其主链内具有活性亚甲基的树脂,优选除了苯环以外的碳碳双键为0.018eq/g或更低,更优选在0.0001-0.015eq/g范围内的那些。
在本发明的吸氧树脂组合物中,除了苯环那些双键以外的碳碳双键的含量优选为0.001eq/g或更低,更优选在0.00001-0.0007eq/g范围内。但当除了苯环那些双键以外的碳碳双键的含量过量时,树脂(A)的氧化倾向于受到抑制。
尽管没有特别限制树脂(B)的分子链,但鉴于树脂(B)在树脂(A)内的分散度,其数均分子量优选在1000-500000范围内,更优选10000-250000。
在本发明中使用的过渡金属催化剂(C)中的金属包括周期表的第VIII族金属如铁、钴和镍,周期表的第I族金属如铜和银,周期表的第IV族金属如锡、钛和锆,周期表的第V族金属如钒,周期表的第VI族金属如铬,和周期表的第VII族金属如锰。在过渡金属催化剂(C)中的优选金属是周期表的第VIII族金属如铁、钴和镍,特别优选钴,这是因为树脂组合物的吸氧速度高。
以以上所述的具有低价键的过渡金属的无机酸盐、有机酸盐或络合物盐的形式使用过渡金属催化剂(C)。
无机酸盐包括氯化物、硫氧酸盐如硫酸盐、氮氧酸盐如硝酸盐、磷氧酸盐如磷酸盐和硅酸盐。
有机酸盐例如是羧酸盐、磺酸盐和膦酸盐。在这些盐当中优选羧酸盐。过渡金属的有机酸盐的实例包括乙酸、丙酸、异丙酸、丁酸、异丁酸、戊酸、异戊酸、己酸、庚酸、异庚酸、辛酸、2-乙基己酸、壬酸、3,5,5-三甲基己酸、癸酸、新癸酸、十一烷酸、月桂酸、肉豆蔻酸、棕榈酸、十七烷酸、硬脂酸、花生酸、十二烯酸、粗租酸、岩芹酸、油酸、亚油酸、亚麻酸、花生四烯酸、甲酸、草酸、氨基磺酸和环烷酸的过渡金属盐。
此处所使用的过渡金属络合物是具有β-二酮或β-酮酸酯的络合物。此处可用的β-二酮和β-酮酸酯例如是,乙酰丙酮、乙基乙酰丙酮、1,3-环己二酮、亚甲基-1,3-环己二酮、2-苄基-1,3-环己二酮、乙酰基四氢萘酮、棕榈酰基四氢萘酮、硬脂酰基四氢萘酮、苯甲酰基四氢萘酮、2-乙酰基环己酮、2-苯甲酰基环己酮、2-乙酰基-1,3-环己二酮、苯甲酰基对氯苯甲酰基甲烷、双(4-甲基苯甲酰基)甲烷、双(2-羟基苯甲酰基)甲烷、苯甲酰基丙酮、三苯甲酰基甲烷、二乙酰基苯甲酰基甲烷、硬脂酰基苯甲酰基甲烷、棕榈酰基苯甲酰基甲烷、月桂酰基苯甲酰基甲烷、二苯甲酰基甲烷、双(4-氯苯甲酰基)甲烷、双(亚甲基-3,4-二氧基苯甲酰基)甲烷、苯甲酰基乙酰基苯基甲烷、硬脂酰基(4-甲氧基苯甲酰基)甲烷、丁酰基丙酮、二硬脂酰基甲烷、乙酰基丙酮、硬脂酰基丙酮、双(环己酰基)甲烷和二新戊酰基甲烷。在本发明中,可使用过渡金属催化剂(C)之一或它们的两种或多种的结合。
过渡金属催化剂(C)优选至少存在于树脂(A)内。该催化剂可促进树脂(A)的氧化反应的进程,以便有效地吸收氧气。更优选,过渡金属催化剂(C)可存在于树脂(A)和树脂(B)这二者内,以促进树脂(B)的引发功能。根据所使用的过渡金属催化剂的特性特征,过渡金属催化剂(C)的用量使得它可促进树脂(A)的氧化反应。为了有效地促进树脂(A)的氧化反应和为了防止因流动特征劣化导致的树脂组合物模塑性的下降,过渡金属催化剂(C)的用量通常优选在10-3000ppm范围内,更优选在50-1000ppm范围内。
尽管在本发明的吸氧树脂组合物内产生树脂(B)的引发作用的效果的机理尚未得到充分地阐述,本发明的发明者估计机理如下所述,但这决不限制产生引发作用的机理。
据认为,在本发明的吸氧树脂组合物内,由过渡金属催化剂(C)从树脂(B)中引出氢,在树脂(B)内形成自由基。然后,通过该自由基和过渡金属催化剂(C)的进攻,从树脂(A)中引出氢,也在树脂(A)内形成自由基。假设当在如此形成的自由基存在下,氧气与树脂(A)接触时,发生树脂(A)的主要氧化。之后,通过过渡金属催化剂的作用,树脂(A)的链氧化反应根据自氧化理论进行。于是,树脂(A)本身起到吸氧剂的作用。
如上所述,在产生该功能的估计机理中,重要的是首先在过渡金属催化剂(C)存在下形成树脂(B)的自由基。因此,树脂(B)优选具有与亚甲基链相比,氢更容易从中引出的碳碳双键。当使用这种树脂(B)时,可有效地供应自由基和可显示出优良的引发功能。作为引出氢的容易程度的指数,例如可提及C-H键裂解能。这一键裂解能是裂解分子(自由基)内的特定C-H键所要求的能量。用R-H表示分子(自由基),C-H键的键裂解能表示为在下述反应内的焓变,和可例如通过分子轨道的计算来测定其数值。表1示出了如此测定的典型数值(KagakuBinran Kiso Hen,第二版,Nihon Kagakukai Corporation,由MaruzenCo.,Ltd.出版)。
R-H(g)→R(g)+H(g)
表1
化学键(R-H) | 键裂解能(kJ.mol-1) |
CH3CH2-H | 410 |
H(CH3)2C-H | 395 |
(CH3)3C-H | 381 |
C6H5CH2-H | 356 |
CH2=CHCH2-H | 366 |
在生产本发明的吸氧树脂组合物的方法中,以上所述的3种组分,即(A)-(C),可单独混合,或者事先一起混合这三种组分中的两种和将所得混合物与其余组分混合。例如,树脂(A)事先与树脂(B)混合,和所得混合物进一步与过渡金属催化剂(C)混合;或者树脂(A)事先与过渡金属催化剂(C)混合,和所得混合物进一步与树脂(A)混合。
树脂(A)和/或树脂(B)可通过各种方法与过渡金属催化剂(C)混合。例如,过渡金属催化剂(C)与树脂干混;或者过渡金属催化剂(C)溶解在有机溶剂内,然后所得分散液体与粉状或粒状树脂混合,和视需要,在惰性氛围内干燥所得混合物。由于与树脂的用量相比,过渡金属催化剂(C)的用量较小,因此优选其中包括下述步骤的方法:将过渡金属催化剂(C)溶解在有机溶剂内,和将所得分散液体与粉状或粒状树脂混合,获得均匀共混物。
此处可用于过渡金属催化剂(C)的溶剂包括醇溶剂如甲醇、乙醇和丁醇、醚溶剂如二甲醚、二***、甲***、四氢呋喃和二烷、酮溶剂如甲乙酮和环己酮,和烃溶剂如正己烷和环己烷。过渡金属催化剂(C)的浓度优选5-90wt%。
优选一起混合树脂(A)、树脂(B)和过渡金属催化剂(C)和在非氧化氛围下储存所得组合物,以便该组合物在使用之前未被氧化。亦即,优选在减压下或在氮气流中进行混合和储存。
优选使用排气式挤塑机或注塑机或带干燥器的这种机器,这是因为可在模塑步骤之前进行混合和干燥,和还因为不需要特别考虑关于含过渡金属催化剂的树脂的储存。
还可以制备含相对高浓度的过渡金属催化剂的树脂的母炼胶,然后干混所得母炼胶和另一树脂。
可将各种添加剂如自由基引发剂和光敏剂掺入到本发明的吸氧树脂组合物中。
此处可用的自由基引发剂和光敏剂是通常被称为光引发剂的那些,例如苯偶姻及其烷基醚类如苯偶姻、苯偶姻甲醚、苯偶姻***和苯偶姻异丙醚;乙酰苯类化合物如乙酰苯、2,2-二甲氧基-2-苯基乙酰苯、2,2-二乙氧基-2-苯基乙酰苯、1,1-二氯乙酰苯、1-羟基环己基苯基酮、2-羟基环己基苯基酮和2-甲基-1-[4-(甲硫基)苯基]-2-吗啉代-丙烷-1-酮;蒽醌类如2-甲基蒽醌和2-戊基蒽醌;噻吨酮类如2,4-二甲基噻吨酮、2,4-二乙基噻吨酮、2-氯噻吨酮和2,4-二异丙基噻吨酮;缩酮类如乙酰苯二甲基缩酮和苄基二甲基缩酮;二苯酮类化合物如二苯酮;和呫吨酮。可结合一种或多种已知、常见的光聚合促进剂如苯甲酸类化合物和叔胺类使用光自由基引发剂。
其它添加剂包括填料、着色剂、热稳定剂、气候稳定剂、抗氧剂、抗老化剂、光稳定剂、紫外线吸收剂、抗静电剂、润滑剂如金属皂和石蜡、改性树脂和橡胶。可通过本身已知的方法将这些添加剂掺入到树脂组合物内。例如通过以这一方式使用润滑剂,可改进在螺杆内树脂的粘着。瓶体润滑剂包括金属皂如硬脂酸镁和硬脂酸钙;烃润滑剂如液体、天然或合成烷属烃、微晶蜡(microwax)、聚乙烯蜡和聚氯乙烯蜡;脂肪酸如硬脂酸和月桂酸;脂族酸单酰胺或双酰胺如硬脂酰胺、棕榈酰胺、油酸酰胺、亚甲基双硬脂酰胺和亚乙基双硬脂酰胺;酯如硬脂酸丁酯、固化的蓖麻油和乙二醇单硬脂酸酯;和它们的混合物。润滑剂的合适用量范围为以聚酰胺的用量计为50-1000ppm。
本发明的吸氧组合物可以以粉末、颗粒或片材的形式用于密封包装内的氧气吸收。也可将该吸氧组合物掺入到树脂或橡胶内用于形成衬里、垫圈或涂层以吸收残留在包装内的氧气。该吸氧组合物也可进一步用于制造包装如以膜或片材形式的包装材料或容器如杯子、托盘、瓶子、管状容器形式的包装容器或类似物。
优选以层压体形式使用本发明的吸氧树脂组合物,所述层压体包括含组合物的至少一层和其它树脂层。
[层压体]
本发明的层压体含有含以上所述的吸氧树脂组合物的至少一层(下文称为吸氧层)。“含吸氧树脂组合物的层”包括含有仅仅以上所述的吸氧树脂组合物的层以及含吸氧树脂组合物和另一树脂作为基础的层。
构成层压体的除了吸氧层以外的树脂层,可合适地选自热塑性树脂和热固性树脂的层,这取决于使用方式和层压体所要求的功能。构成层压体的树脂例如是烯烃树脂、热塑性聚酯和氧气阻挡树脂。
烯烃树脂包括例如,低密度聚乙烯(LDPE)、中密度聚乙烯(MDPE)、高密度聚乙烯(HDPE)、线性低密度聚乙烯(LLDPE)、线性甚低密度聚乙烯(LVLDPE)、聚丙烯(PP)、乙烯/丙烯共聚物、聚丁烯-1、乙烯/丁烷-1共聚物、丙烯/丁烷-1共聚物、乙烯/丙烯/丁烷-1共聚物、乙烯/乙酸乙烯酯共聚物和离子交联的烯烃共聚物(离聚物)以及它们的共混物。
热塑性聚酯树脂包括例如聚对苯二甲酸乙二酯(PET)、聚对苯二甲酸丁二酯(PBT)和聚萘二甲酸乙二酯(PEN)以及共聚物聚酯和它们的共混物。
氧气阻挡树脂包括乙烯/乙烯醇共聚物(EVOH)。例如,可使用通过皂化乙烯/乙酸乙烯酯共聚物获得的皂化共聚物,其中所述乙烯/乙酸乙烯酯共聚物的乙烯含量为20-60mol%,优选25-50mol%,以达到至少96mol%的皂化度优选至少99mol皂化度。
皂化的乙烯乙烯醇共聚物具有使得形成膜的分子量。该共聚物的粘度为至少0.01dl/g,优选至少0.05dl/g,这通过在重量比为85∶15的苯酚和水的混合溶剂中在30℃下测定。
氧气阻挡树脂的其它实例是聚酰胺树脂如聚己二酰间苯二甲胺(MXD6)和聚酯树脂如聚乙醇酸。
取决于使用方式和所要求的功能,可合适地选择本发明的层压体的结构。例如,层压体具有下述结构,其中OAR表示吸氧层:
两层结构:PET/OAR、PE/OAR、OPP/OAR,
三层结构:PE/OAR/PET、PET/OAR/PET、PE/OAR/OPP、EVOH/OAR/PET、PE/OAR/COC,
四层结构:PE/PET/OAR/PET、PE/OAR/EVOH/PET、PET/OAR/EVOH/PET、PE/OAR/EVOH/COC、PE/OAR/EVOH/PE,
五层结构:PET/OAR/PET/OAR/PET、PE/PET/OAR/EVOH/PET、PET/OAR/EVOH/COC/PET、PET/OAR/PET/COC/PET、PE/OAR/EVOH/COC/PET、PE/EVOH/OAR/EVOH/PE、PP/EVOH/OAR/EVOH/PP,
六层结构:PET/OAR/PET/OAR/EVOH/PET、PE/PET/OAR/COC/EVOH/PET、PET/OAR/EVOH/PET/COC/PET、PE/EVOH/OAR/PE/EVOH/PE、PP/EVOH/OAR/PP/EVOH/PP,和
七层结构:PET/OAR/COC/PET/EVOH/OAR/PET。
PE表示低密度聚乙烯(LDPE)、中密度聚乙烯(MDPE)、高密度聚乙烯(HDPE)、线性低密度聚乙烯(LLDPE)、或线性甚低密度聚乙烯(LVLDPE)、
在这些结构中,优选具有至少一层氧气阻挡层的结构,这是因为可延长在该结构内的吸氧层的寿命。
视需要,可在该层压体的树脂层之间放置粘合层。粘合剂树脂包括羧酸、羧酸酐和在主链或侧链内含有1-70Omeq羧酸/10Og树脂,优选10-500meq/100g树脂的聚合物。
粘合剂树脂包括,例如乙烯/丙烯酸共聚物、离子交联的烯烃共聚物、马来酸酐接枝聚乙烯、马来酸酐接枝聚丙烯、丙烯酸接枝聚烯烃、乙烯/乙酸乙烯酯共聚物、聚酯共聚物和聚酰胺共聚物。也可使用它们的两种或多种的结合。
这些粘合剂树脂藉助共挤塑、夹芯层压或类似方法可用于层压。热固性粘合剂树脂如异氰酸酯或环氧树脂也可用于在先模塑的气体阻挡树脂膜和防潮树脂膜的粘合层压。
本身已知的共挤塑方法可用于生产层压体。可通过例如采用多层多模头和数量可变的挤塑机(这取决于树脂的种类)的挤出模塑,来生产层压体。
因此,层压体可被模塑成膜、片材、瓶子、杯子、盖子、形成管道的型坯或管道和形成瓶子或管道的料坯。
可以以各种形状的包装袋,如具有3或4个密封侧的普通袋子,具有撑板的袋子,自立式袋子和波浪形包装袋的形式使用包装材料如膜。
通过用一对分瓣模具截坯型坯、管道或料坯,并在其内吹塑液体,从而可容易地生产瓶子。通过冷却管道或料坯,加热它到拉伸温度,和沿轴向拉伸它,并同时在垂直方向上吹塑拉伸它,可获得吹塑瓶子和类似物。
此外,可通过真空成型、空气压力成型、膜泡成型、模塞助压成型或类似方法,由膜或片材获得包装容器如杯子和托盘。
可通过使用注塑机,通过共注塑方法或分步注塑方法,生产多层注塑件,其中注塑机的使用数量随树脂种类而变化。
可通过挤出贴面方法或者夹芯层压方法生产多层膜和多层片材。也可通过干燥层压在先形成的膜,生产多层膜和多层片材。
本发明的层压体优选可用于生产包装材料或包装容器,这是因为它们可有效地截断氧气。该层压体可用于生产能防止其内容物的风味和味道劣化并长时间地延长内容物的储存期限的包装,这是因为它们能长时间地吸收氧气。
本发明的层压体尤其用作饮料如啤酒、果汁和软碳酸饮料、食品如水果、坚果、植物、动物产品、婴儿食品、咖啡、果酱、蛋黄酱、番茄酱、烹饪用油、调味品、酱油、在豆酱内蒸煮的食品和奶制品以及药品、化妆品和汽油的包装材料。
下述实施例将进一步阐述本发明,这些实施例决不限制本发明。
[实施例]
[苯乙烯/二烯烃共聚物的碳碳双键含量的测定]
在氘代氯仿内溶解树脂,获得浓度为10-15wt%的溶液,然后通过13C-NMR测定(JNM-EX270,JEOL的产品),光谱鉴定树脂的结构。通过计算包含在1g树脂内的双键的摩尔数(eq/g)来测定碳碳双键的含量。
[观察在吸氧树脂组合物内树脂(B)的分散状态的方法]
将吸氧树脂组合物包埋在用于电子显微的环氧/胺包埋树脂内,然后固化该包埋树脂。用切片机研磨并刮削包埋树脂,获得吸氧树脂组合物样品的截面。通过用超微切片机磨蚀抛光包埋树脂样品的截面。用扫描电子显微镜(JSM-6300F,JEOL的产品)拍摄抛光磨蚀截面的SEM照片,观察在吸氧树脂组合物内树脂(B)的分散状态。
1.吸氧树脂组合物
[实施例1]
将100重量份低密度聚乙烯树脂[JB221R;一种Japan PolyolefinCo.,Ltd.的产品]与5重量份苯乙烯树脂[HRM 24N;一种Toyo StyreneCo.,Ltd.的产品]和350ppm(以钴为单位计)作为过渡金属催化剂的新癸酸钴[DICNATE 5000;一种Dainippon Ink and Chemicals,Inc.的产品]混合。事先用搅拌干燥器[一种DALTON公司的产品]捏合所得混合物,然后经具有定量喂料器的料斗,供料到双螺杆挤出机(TEM 37,一种Toshiba Machine Co,Ltd.的产品)内。在100RPM的旋转速度下,在210℃下以线材形式挤出该混合物,然后造粒。
用冷冻粉碎器粉碎如此获得的粒料,然后测量适量的粒料。将如此获得的粉末与1.0ml蒸馏水一起放置在85ml氧气不可渗透的容器[hi-Retoflex:Toyo Seikan Kaisha,Ltd.的HR 78-84聚丙烯/钢片/聚丙烯层压的杯状容器]内。用由聚丙烯(里层)/铝片/聚酯(外层)组成的盖材料热密封该容器,然后在50℃下储存。在一定的时间间隔处,用气相色谱[GC-8A,一种Shimadzu公司的产品]测定容器内的氧气浓度,以计算氧气的吸收(cc/g)。表2示出了结果。观察每一粒料的截面,和发现苯乙烯树脂均匀地分散在低密度聚乙烯树脂基体内。
[实施例2]
以与实施例1相同的方式制备粒料,所不同的是用苯乙烯含量为15wt%的苯乙烯/异戊二烯/苯乙烯三嵌段共聚物树脂[SIS 5200;碳碳双键含量为0.014eq/g的JSR Co.,Ltd.的产品]替代苯乙烯,然后以与实施例1相同的方式测定容器内的氧气浓度和计算氧气的吸收(cc/g)。表2示出了结果。以与实施例1相同的方式观察每一粒料的截面,和发现苯乙烯/异戊二烯/苯乙烯三嵌段共聚物树脂均匀地分散在低密度聚乙烯树脂基体内。
[实施例3]
以与实施例2相同的方式制备粒料,所不同的是用线性低密度聚乙烯树脂[ULTZEX 2020SB;Mitsui Sumitomo Polyolefin Co.,Ltd.]替代低密度聚乙烯。然后以与实施例2相同的方式测定容器内的氧气浓度和计算氧气的吸收(cc/g)。表2示出了结果。以与实施例1相同的方式观察每一粒料的截面,和发现苯乙烯/异戊二烯/苯乙烯三嵌段共聚物树脂均匀地分散在线性低密度聚乙烯树脂基体内。
[实施例4]
以与实施例2相同的方式制备粒料,所不同的是用高密度聚乙烯树脂[KZ145N;一种日本Polyolefin Co.,Ltd.的产品]替代低密度聚乙烯。然后以与实施例2相同的方式测定容器内的氧气浓度和计算氧气的吸收(cc/g)。表2示出了结果。以与实施例1相同的方式观察每一粒料的截面,和发现苯乙烯/异戊二烯/苯乙烯三嵌段共聚物树脂均匀地分散在高密度聚乙烯树脂基体内。
[对比例1]
以与实施例1相同的方式制备粒料,所不同的是不使用苯乙烯树脂[HRM24N;一种Toyo Styrene Co.,Ltd.的产品]。以与实施例1相同的方式测定容器内的氧气浓度和计算氧气的吸收(cc/g)。表2示出了结果。
[对比例2]
以与对比例1相同的方式制备粒料,所不同的是用线性低密度聚乙烯树脂[ULTZEX 2020SB;Mitsui Sumitomo Polyolefin Co.,Ltd.]替代低密度聚乙烯。然后以与对比例1相同的方式测定容器内的氧气浓度和计算氧气的吸收(cc/g)。表2示出了结果。
[对比例3]
以与对比例1相同的方式制备粒料,所不同的是用高密度聚乙烯树脂[KZ 145N;一种日本Polyolefin Co.,Ltd.的产品]替代低密度聚乙烯。然后以与对比例1相同的方式测定容器内的氧气浓度和计算氧气的吸收(cc/g)。表2示出了结果。
表2
氧气的吸收(cc/g) | ||||
2天之后 | 7天之后 | 14天之后 | 30天之后 | |
实施例1 | 0.0 | 0.5 | 24.1 | 60.0 |
实施例2 | 13.5 | 27.5 | 47.6 | 87.2 |
实施例3 | 11.9 | 26.6 | 47.0 | 86.8 |
实施例4 | 10.9 | 25.8 | 45.5 | 86.5 |
对比例1 | 0.0 | 0.0 | 0.0 | 11.9 |
对比例2 | 0.0 | 0.0 | 0.0 | 9.5 |
对比例3 | 0.0 | 0.0 | 0.0 | 0.0 |
2.层压体
[实施例5]
通过公知的熔体吹塑方法,生产瓶嘴直径为45mm和容量为150ml的四种6层瓶子,该瓶子由实施例2中造粒的吸氧树脂组合物、低密度聚乙烯树脂[JB221R;日本Polyolefin Co.,Ltd.的产品]、粘合剂树脂[MODIC L522;一种Mitsubishi Chemical Corporation的产品]和阻挡树脂[EVAL F101B,一种Kuraray Co.,Ltd.的产品]制成。
产品的层结构如下:
外部:聚乙烯层/粘合层/阻挡层/粘合层/吸氧层/聚乙烯层
wt%:20/2.5/5/2.5/5/65
为了评价多层瓶子的氧气截断性能,将1ml蒸馏水供入到实施例1中生产且对氧气不可渗透的容器内,以评价多层瓶子的氧气不可渗透性。在氮气氛围中,用与实施例1中使用的相同盖材料紧紧地热密封瓶嘴。在容器内的起始氧气浓度为0.02%或更低。在30℃和80%RH下保持容器之后,采用气相色谱[GC-8A;一种Shimadzu Corporation的产品]测定在容器内的氧气浓度。表3示出了结果。
[对比例4]
以与实施例3相同的方式,通过使用对比例1中造粒的吸氧树脂组合物、低密度聚乙烯树脂[JB221R;日本Polyolefin Co.,Ltd.的产品]、粘合剂树脂[MODIC L522;一种Mitsubishi Chemical Corporation的产品]和阻挡树脂[EVAL F101B,一种Kuraray Co.,Ltd.的产品],生产容量为150ml的四种6层瓶子。然后测定瓶子的氧气截断性能。表3示出了结果。
表3
容器内的氧气量(cc/瓶子) | ||||
14天之后 | 1月之后 | 3月之后 | 5月之后 | |
实施例5 | 0.0 | 0.0 | 0.0 | 0.07 |
对比例4 | 0.20 | 0.44 | 1.43 | 2.25 |
Claims (14)
1.一种吸氧树脂组合物,它包括通过聚合具有2-8个碳原子的烯烃而获得的聚烯烃树脂(A),树脂(B)和过渡金属催化剂(C),其中所述树脂(B)是除了树脂(A)以外的树脂,且起到树脂(A)氧化的引发物的作用,其中树脂(A)是一种具有乙烯结构的树脂,其侧链中具有苯环的树脂(B)是聚苯乙烯或至少含10重量%苯乙烯部分的苯乙烯共聚物,树脂(B)分散在树脂(A)的基体内,以便当吸氧树脂组合物与氧气接触时,引起基体树脂(A)的氧化反应并进而吸收氧气。
2.权利要求1的吸氧树脂组合物,其中过渡金属催化剂(C)包含在至少树脂(A)内。
3.权利要求1或2的吸氧树脂组合物,其中具有乙烯结构的树脂是低密度聚乙烯或线性低密度聚乙烯。
4.权利要求1或2的吸氧树脂组合物,其中所述组合物中树脂(A)的含量为90-99wt%。
5.权利要求1或2的吸氧树脂组合物,其中所述组合物中树脂(B)的含量为1.0-10wt%。
6.权利要求1或2的吸氧树脂组合物,其中苯乙烯共聚物是嵌段共聚物。
7.权利要求1或2的吸氧树脂组合物,其中苯乙烯共聚物是在分子端部分具有聚苯乙烯嵌段的嵌段共聚物。
8.权利要求1或2的吸氧树脂组合物,其中苯乙烯共聚物是具有异戊二烯单元的嵌段共聚物。
9.权利要求8的吸氧树脂组合物,其中具有异戊二烯单元的嵌段共聚物是苯乙烯/异戊二烯/苯乙烯三嵌段共聚物。
10.权利要求1或2的吸氧树脂组合物,其中所述组合物含有0.001eq/g或更低的除了苯环中的那些以外的碳碳双键。
11.权利要求1或2的吸氧树脂组合物,其中基于金属的重量,所述组合物含有10-3000ppm的过渡金属催化剂。
12.一种吸氧片材,它含有权利要求1-11中任何一项的吸氧树脂组合物。
13.一种层压体,它具有含权利要求1-11中任何一项的吸氧树脂组合物的至少一层。
14.权利要求13的层压体,它进一步具有至少一层氧气阻挡层。
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KR (1) | KR100679310B1 (zh) |
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JP2008195949A (ja) | 2008-08-28 |
ATE551393T1 (de) | 2012-04-15 |
JP5370906B2 (ja) | 2013-12-18 |
JPWO2004018556A1 (ja) | 2005-12-08 |
WO2004018556A1 (ja) | 2004-03-04 |
AU2003262283A1 (en) | 2004-03-11 |
US20050142373A1 (en) | 2005-06-30 |
JP4314637B2 (ja) | 2009-08-19 |
EP1553137B1 (en) | 2012-03-28 |
KR20050058435A (ko) | 2005-06-16 |
US8592522B2 (en) | 2013-11-26 |
AU2003262283B2 (en) | 2007-03-22 |
CN1685005A (zh) | 2005-10-19 |
EP1553137A4 (en) | 2006-04-26 |
EP1553137A1 (en) | 2005-07-13 |
KR100679310B1 (ko) | 2007-02-06 |
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