CN115594876B - 一种高阻隔吸塑包装片材及其制备方法 - Google Patents
一种高阻隔吸塑包装片材及其制备方法 Download PDFInfo
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- CN115594876B CN115594876B CN202211316118.6A CN202211316118A CN115594876B CN 115594876 B CN115594876 B CN 115594876B CN 202211316118 A CN202211316118 A CN 202211316118A CN 115594876 B CN115594876 B CN 115594876B
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- barrier
- packaging sheet
- mica
- barrier layer
- modified resin
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- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 3
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Abstract
本申请涉及包装材料技术领域,具体公开了一种高阻隔吸塑包装片材及其制备方法。一种高阻隔吸塑包装片材,包括依次相连的聚氯乙烯基材层与阻隔层,阻隔层由包含以下重量份的原料组成:改性树脂55‑70份;片层状填料2‑7份;交联剂5‑8份,改性树脂由二异氰酸酯、多元醇和双端羟基聚硅氧烷反应制得。本申请的一种高阻隔吸塑包装片材具有良好的气体阻隔性能。
Description
技术领域
本申请涉及包装材料技术领域,更具体地说,它涉及一种高阻隔吸塑包装片材及其制备方法。
背景技术
吸塑成型作为塑料成型的主要方式之一,由于其具有成型材料重量轻、密封性好、可包装各种异型材料的性能,被广泛用于工业生产及日常生活中的各类产品的包装。如奶制品、食品、化妆品、药类(医药、农药类)等包装。由于吸塑成型可通过不同模具形状设计来实现风格各异,样式丰富的包装,在追求物质及文化多样性的今天,具有独特的吸引力和巨大的销售市场。
为了避免包装的内容物变质,保持其功能和性能,要求用于食品、药品及电子物品的包装材料具有防止由气体(如氧气、水蒸气等)通过包装材料而引起包装内容物变质的性能。然而使用传统的吸塑材料对液体或膏体物料进行包装时,为了使得产品使用过程包装外壳方便撕开使用,通常采用单一易撕型包装片材,虽可以达到方便撕开的目的,但很难获得良好的气体阻隔性能,因此,亟需开发一种高阻隔吸塑包装片材。
发明内容
为了解决吸塑包装片材的气体阻隔性能不佳的问题,本申请提供一种高阻隔吸塑包装片材及其制备方法。
第一方面,本申请提供一种高阻隔吸塑包装片材,采用如下的技术方案:
一种高阻隔吸塑包装片材,包括依次相连的聚氯乙烯基材层与阻隔层,所述阻隔层由包含以下重量份的原料制成:改性树脂55-70份、片层状填料2-7份、交联剂5-8份;
所述改性树脂的制备方法,包括如下步骤:
S1,将二异氰酸酯与多元醇按照质量比为1:(0.6-0.8)反应,得到聚氨酯预聚体;
S2,将聚氨酯预聚体与双端羟基聚硅氧烷按照质量比为1:(0.6-0.8)混合反应,得到改性树脂。
通过采用上述技术方案,将过量的二异氰酸酯与多元醇反应得到聚氨酯预聚体,聚氨酯预聚体的两端均为NCO基团,聚氨酯预聚体两端的NCO基团与双端羟基聚硅氧烷反应,得到改性树脂,疏水的聚硅氧烷被接入到改性树脂中,改性树脂与交联剂交联,形成致密的网络结构,具有良好的疏水性能;
改性树脂中的氨基甲酸酯基与聚氯乙烯分子之间通过氢键相互作用,赋予阻隔层与聚氯乙烯基材层之间良好的相容性;改性树脂中的聚氨酯分子链段赋予阻隔层良好的韧性,将阻隔层涂覆到聚氯乙烯基材层上,提升了聚氯乙烯基材层的力学性能。
片层状填料在阻隔层中,具有以下作用:第一,气体在扩散进入阻隔层的过程中,遇到片层状填料绕道而行,气体路径发生曲折,以至于气体穿过阻隔层的路径增加,气体分子的扩散速率降低,提升了阻隔层的气体阻隔性能;第二,片层状填料填充在三维网络结构中,减小了阻隔层内部的空间间隙,提高了阻隔层结构的致密度。将阻隔层与聚氯乙烯基材层结合,得到的高阻隔吸塑包装片材,具有良好的气体阻隔性能和力学性能,从而解决了吸塑包装材料气体阻隔性能不佳的问题。
优选的,所述片层状填料为蒙脱土、云母、滑石、蛭石中的一种或多种。
通过采用上述技术方案,上述片层状填料上含亲水基团,与改性树脂通过氢键结合,与改性树脂的界面结合性能较好,片层状填料在阻隔层中的分散性能较好,气体穿过阻隔层时与片层状填料碰撞的概率较高,吸塑包装片材的气体阻隔性能与力学性能较好。
优选的,所述S2步骤中,聚氨酯预聚体与双端羟基聚硅氧烷混合反应后,再与氨基酸反应,得到改性树脂;其中,聚氨酯预聚体与氨基酸的质量比为1:(0.2-0.3)。
通过采用上述技术方案,步骤S2中,将聚氨酯预聚体与双端羟基聚硅氧烷混合反应后,得到硅烷改性聚氨酯,硅烷改性聚氨酯再经过氨基酸改性。硅烷改性聚氨酯中含有NCO基团和羟基等基团,上述基团与氨基酸通过氢键作用交联,提高了阻隔层结构的致密程度,进一步提高吸塑包装片材的气体阻隔性能和力学性能。
优选的,所述聚氨酯预聚体与双端羟基聚硅氧烷的质量比为1:(0.65-0.7)。
通过采用上述技术方案,当所述聚氨酯预聚体与双端羟基聚硅氧烷的质量比为1:(0.65-0.7)时,聚氨酯预聚体与双端羟基聚硅氧烷的比例适中,制得的阻隔层既具有良好的疏水性能,又与聚氯乙烯基材层具有良好的相容性。
优选的,所述片层状填料的重量份为3-5份。
通过采用上述技术方案,当片层状填料的重量份为3-5份时,在阻隔层中分散得较为均匀,气体穿过阻隔层时与片层状填料碰撞的概率较高,吸塑包装片材的气体阻隔性能与力学性能较好。
优选的,所述多元醇为聚酯多元醇。
通过采用上述技术方案,聚酯多元醇中的酯基与聚氯乙烯基材层的亲和性能较好,制得的阻隔层与聚氯乙烯基材层的相容性较好,吸塑包装片材的力学性能较好。
优选的,所述交联剂为FEVE型氟树脂。
通过采用上述技术方案,FEVE型氟树脂含有羟基,一方面能够与改性树脂进行氢键交联,提高阻隔层的致密性,另一方面引入电负性较大的氟元素,含氟结构提升了阻隔层良好的疏水性能,提高吸塑包装片材的气体阻隔性能。
优选的,所述片层状填料为云母,云母经过改性处理,改性处理的方法,包括如下步骤:
将云母升温活化,得到热活化云母;
将热活化云母酸化,得到酸化云母;
将酸化云母与钠盐混合,得到钠化云母;
将钠化云母与改性剂按照质量比为1:(0.08-0.12)混合,得到改性云母,改性剂为十四烷基三甲基溴化铵、十二烷基三甲基溴化铵、十八烷基三乙基溴化铵中的一种或多种。
通过采用上述技术方案,对云母进行插层改性处理,具有以下作用,第一,改性前的云母层间结合紧密,自然状态下有聚集倾向,插层改性后的云母层间距得到一定程度的扩张,聚集倾向减小,有效阻隔面积较大,可以起到较好的气体阻隔作用;第二,插层处理使得片层结构变得疏松,以较小的片状结构在阻隔层中分散得更加均匀。
优选的,所述改性剂为十八烷基三乙基溴化铵。
通过采用上述技术方案,选择十八烷基三乙基溴化铵作为改性剂,一方面,十八烷基三乙基溴化铵具有较长的分子链,可以使改性后的云母层间距较大程度地扩张,很好地减弱了层间结合力,并获得较高的插层率;另一方面,十八烷基三乙基溴化铵上的长链可以与改性树脂物理缠结,显著提高了改性树脂与云母的界面结合性能,进而提升了高阻隔吸塑包装片材的力学性能。
第二方面,本申请提供一种高阻隔吸塑包装片材的制备方法,采用如下的技术方案:
一种高阻隔吸塑包装片材的制备方法,包括如下步骤:
将阻隔层的原料与聚氯乙烯基材层的原料分别投入至挤出机中熔融加工,将阻隔层的原料熔体与聚氯乙烯基材层的原料熔体送入流延机或吹塑机中共挤成膜、冷却,形成依次相连的聚氯乙烯基材层与阻隔层,得到高阻隔吸塑包装片材。
综上所述,本申请具有以下有益效果:
1、由于本申请将聚硅氧烷作为疏水链段引入聚氨酯分子链中,得到改性树脂,改性树脂中的氨基甲酸酯与聚氯乙烯基材层通过氢键结合,使得改性树脂与聚氯乙烯基材层的相容性较好;从而制得疏水性能较好,对水蒸气的阻隔性能较佳的高阻隔吸塑包装片材。
2、本申请中优选含有亲水基团的片层状填料,亲水基团与改性树脂通过氢键结合,与改性树脂的界面结合性能较好,均匀地填充在改性树脂中,提高阻隔层的致密性;气体在扩散进入阻隔层的过程中,遇到片层状填料绕道而行,气体路径发生曲折,以至于气体穿过阻隔层的路径增加,气体分子的扩散速率降低,提升了阻隔层的气体阻隔性能。
3、本申请优选经过改性处理的云母作为片层状填料,改性处理时将酸化云母与钠盐混合,得到钠化云母,再用改性剂对钠化云母进行改性处理,将层间不易置换的钾离子置换为容易置换的钠离子,以此获得了更加优异的插层改性效果,改性处理后的云母层间距变大,有效阻隔面积变大。
具体实施方式
以下结合实施例对本申请做进一步详细说明。
若无特殊说明,以下实施例以及对比例中所用的原料规格详见表1。
表1.原料规格信息
改性云母的制备例
制备例A
改性云母,按照如下步骤制得:
取300g云母,阶段性升温,200℃以下时,升温速率为5℃/min,接下来以10℃/min的速率升温至800℃,得到热活化云母,将热活化云母降温至25℃;
取200g降温后的热活化云母,加入200g的0.1mol/L的盐酸中,在80℃下搅拌反应6h,抽滤、洗涤,得到酸化云母;
取150g酸化云母,加入200g的饱和氯化钠溶液中,在80℃下搅拌反应3h,抽滤、洗涤,
得到钠化云母;
取100g钠化云母、8g改性剂十二烷基三甲基溴化铵和200g水混合,调节pH值为5,在75℃下搅拌,反应20h,得到改性云母。
制备例B
改性云母,与制备例A的区别点在于:改性剂十四烷基三甲基溴化铵的质量不同,本制备例十二烷基三甲基溴化铵的质量为12g。
制备例C
改性云母,与制备例B的区别点在于:改性剂的选择不同,本制备例选择十八烷基三乙基溴化铵。
改性树脂的制备例
制备例1
改性树脂,按照如下步骤制得:
将聚醚多元醇、羟基硅油在110℃真空干燥3h除去水分,降温至25℃,再取1200g除去水分的聚醚多元醇、2000g异佛尔酮二异氰酸酯、5000g丙酮和0.5g二月桂酸二丁基锡混合搅拌,升温至60℃,保温反应2h,减压蒸除丙酮,得到聚氨酯预聚体;将5000g丙酮、1000g聚氨酯预聚体、600g羟基硅油和100g二羟甲基丙酸混合搅拌,升温至80℃,反应3h后降温至30℃,加入100g三乙胺混合反应,减压蒸除丙酮,得到改性树脂。
制备例2
改性树脂,与制备例3的区别点在于:二异氰酸酯与多元醇的质量比不同,本制备例二异氰酸酯与多元醇的质量比为1:0.8。
制备例3
改性树脂,与制备例4的区别点在于:聚氨酯预聚体与羟基硅油的质量比不同,本制备例聚氨酯预聚体与羟基硅油的质量比为1:0.8。
制备例4
改性树脂,按照如下步骤制得:
将聚醚多元醇、羟基硅油在110℃真空干燥3h除去水分,降温至25℃,再取1600g除去水分的聚醚多元醇、2000g异佛尔酮二异氰酸酯、5000g丙酮和0.5g二月桂酸二丁基锡混合搅拌,升温至60℃,保温反应2h,减压蒸除丙酮、得到聚氨酯预聚体;将5000g丙酮、1000g聚氨酯预聚体、800g羟基硅油和100g二羟甲基丙酸混合搅拌,升温至80℃,反应3h后降温至30℃,加入200g的谷氨酸和100g三乙胺,混合反应,减压蒸除丙酮,得到改性树脂。
制备例5
改性树脂,与制备例4的区别点在于:谷氨酸的质量不同,本制备例中谷氨酸的质量为300g。
制备例6
改性树脂,与制备例5的区别点在于:聚氨酯预聚体与双端羟基聚硅氧烷的质量比不同,本制备例聚氨酯预聚体与双端羟基聚硅氧烷的质量比为1:0.65。
制备例7
改性树脂,与制备例6的区别点在于:聚氨酯预聚体与双端羟基聚硅氧烷的质量比不同,本制备例聚氨酯预聚体与双端羟基聚硅氧烷的质量比为1:0.7。
制备例8
改性树脂,与制备例7的区别点在于:多元醇的选择不同,本制备例将聚醚多元醇等质量更换为聚酯多元醇。
改性树脂的制备对比例
制备对比例1
改性树脂,按照如下步骤制得:
将聚醚多元醇在110℃真空干燥3h除去水分,再取1200g除去水分的聚醚多元醇、2000g异佛尔酮二异氰酸酯、5000g丙酮和0.5g二月桂酸二丁基锡混合搅拌,升温至60℃,保温反应2h,减压蒸除丙酮,得到聚氨酯预聚体;将5000g丙酮、1000g聚氨酯预聚体和100g二羟甲基丙酸混合搅拌,升温至80℃,反应3h后降温至30℃,加入100g三乙胺混合反应,减压蒸除丙酮,得到改性树脂。
实施例
实施例1
一种高阻隔吸塑包装片材,按照如下步骤制得:
向550g由制备例1制得的改性树脂中加入50g交联剂丙烯酸羟乙酯、5000g丙酮,反应30min后,加入20g片层状填料石墨烯和分散剂十二烷基三甲基溴化铵,片层状填料石墨烯与分散剂十二烷基三甲基溴化铵的质量比为1:0.08,混合均匀,减压蒸除丙酮,得到阻隔层原料;
将阻隔层原料进行干燥;
取100g干燥后的阻隔层原料和300g聚氯乙烯树脂分别投入至双螺杆挤出机中熔融加工,然后将上述挤出的阻隔层原料熔体和聚氯乙烯树脂熔体送入流延机中共挤成膜,冷却,形成依次相连的聚氯乙烯基材层与阻隔层,得到高阻隔吸塑包装片材。
实施例2-3
一种高阻隔吸塑包装片材,与实施例1的区别点在于:
阻隔层原料的组成不同,具体组成如下表2所示:
表2.阻隔层原料的组成
项目 | 改性树脂 | 片层状填料 | 交联剂 |
实施例1 | 550 | 20 | 50 |
实施例2 | 700 | 70 | 80 |
实施例3 | 600 | 50 | 60 |
实施例4
一种高阻隔吸塑包装片材,与实施例3的区别点在于,改性树脂的选择不同,本实施例选择制备例2制得的改性树脂。
实施例5
一种高阻隔吸塑包装片材,与实施例4的区别点在于,改性树脂的选择不同,本实施例选择制备例3制得的改性树脂。
实施例6
一种高阻隔吸塑包装片材,与实施例5的区别点在于:片层状填料的选择不同,将石墨烯等质量更换为蒙脱土。
实施例7
一种高阻隔吸塑包装片材,与实施例5的区别点在于:片层状填料的选择不同,将石墨烯等质量更换为云母。
实施例8
一种高阻隔吸塑包装片材,与实施例5的区别点在于:片层状填料的选择不同,将石墨烯等质量更换为制备例A制得的改性云母。
实施例9
一种高阻隔吸塑包装片材,与实施例5的区别点在于:片层状填料的选择不同,将石墨烯等质量更换为制备例B制得的改性云母。
实施例10
一种高阻隔吸塑包装片材,与实施例5的区别点在于:片层状填料的选择不同,将石墨烯等质量更换为制备例C制得的改性云母。
实施例11
一种高阻隔吸塑包装片材,与实施例10的区别点在于:改性树脂的选择不同,本实施例选择制备例4制得的改性树脂。
实施例12
一种高阻隔吸塑包装片材,与实施例11的区别点在于:改性树脂的选择不同,本实施例选择制备例5制得的改性树脂。
实施例13
一种高阻隔吸塑包装片材,与实施例12的区别点在于:改性树脂的选择不同,本实施例选择制备例6制得的改性树脂。
实施例14
一种高阻隔吸塑包装片材,与实施例13的区别点在于:改性树脂的选择不同,本实施例选择制备例7制得的改性树脂。
实施例15
一种高阻隔吸塑包装片材,与实施例14的区别点在于:改性树脂的选择不同,本实施例选择制备例8制得的改性树脂。
实施例16
一种高阻隔吸塑包装片材,与实施例15的区别点在于:片层状填料的质量不同,本实施例片层状填料的质量为30g。
实施例17
一种高阻隔吸塑包装片材,与实施例16的区别点在于:交联剂的选择不同,本实施例将丙烯酸羟乙酯等质量更换为FEVE型氟树脂。
实施例18
一种高阻隔吸塑包装片材,按照如下步骤制得:
向550g由制备例1制得的改性树脂中加入50g交联剂丙烯酸羟乙酯、5000g丙酮,反应30min后,加入20g片层状填料石墨烯和分散剂十二烷基三甲基溴化铵,片层状填料石墨烯与分散剂十二烷基三甲基溴化铵的质量比为1:0.08,混合均匀,减压蒸除丙酮,得到阻隔层原料;
取100g阻隔层原料、300g水和200g丙酮混合,25℃下剪切乳化,减压蒸除丙酮,得到涂料;
取300g聚氯乙烯树脂投入至双螺杆挤出机中熔融加工,然后将上述挤出的聚氯乙烯树脂熔体送入流延机中挤出成膜,冷却,得到聚氯乙烯基材层;
将涂料涂覆于聚氯乙烯基材层上,在80℃下固化30min,形成依次相连的聚氯乙烯基材层与阻隔层,得到高阻隔吸塑包装片材。
对比例
对比例1
一种高阻隔吸塑包装片材,与实施例1的区别点在于,改性树脂的选择不同,本对比例选择制备对比例1制得的改性树脂。
对比例2
一种高阻隔吸塑包装片材,与实施例1的区别点在于,本对比例将改性树脂等质量更换为羟基硅油。
对比例3
一种高阻隔吸塑包装片材,与实施例1的区别点在于,阻隔层原料的组成不同,具体组成如下表3所示:
表3.阻隔层原料的组成
项目 | 改性树脂 | 片层状填料 | 交联剂 |
实施例1 | 550 | 20 | 50 |
对比例3 | 560 | 0 | 60 |
检测方法
按照GB/T 1038-2000测试实施例1-18和对比例1-3制得的高阻隔吸塑包装片材的氧气透过量,以此表征高阻隔吸塑包装片材的氧气阻隔性能;
按照GB/T 1037-88测试实施例1-18和对比例1-3制得的高阻隔吸塑包装片材的水蒸气透过量,以此表征高阻隔吸塑包装片材的水蒸气阻隔性能;
按照按GB/T 1040.1-2006测试实施例1-18和对比例1-3制得的高阻隔吸塑包装片材的拉伸强度,具体检测结果如下表4所示:
检测结果
表4.高阻隔吸塑包装片材的性能测试
由表6可知,本申请实施例制得的高阻隔吸塑包装片材的拉伸强度≧21.6MPa、氧气透过量≦0.58(cm3/m2·24h·bar)、水蒸气透过量≦0.645(g/m2·24h),可见本申请一种高阻隔吸塑包装片材气体阻隔性能较好,力学性能较佳。
结合实施例1和对比例1并结合表6可以看出,实施例1的水蒸气透过量远小于对比例1,这可能是因为:制备对比例1制得的改性树脂没有经过羟基硅油改性,改性树脂的疏水性能较差,导致对比例1的水蒸气阻隔性能较差。
结合实施例1和对比例2并结合表6可以看出,实施例1的拉伸强度远大于对比例2,而氧气透过量和水蒸气透过量远小于对比例2,这可能是因为:对比例2用羟基硅油替代改性树脂,羟基硅油中没有氨基甲酸酯基,无法与聚氯乙烯基材层通过氢键相互作用,导致对比例2中阻隔层与聚氯乙烯基材层的相容性不佳,制得的高阻隔吸塑包装片材的力学性能和气体阻隔性能均不佳。
结合实施例1和对比例3并结合表6可以看出,实施例1的拉伸强度远大于对比例3,而氧气透过量和水蒸气透过量远小于对比例3,这可能是因为:实施例1中加入了片层状填料,片层状填料具有以下作用:第一,气体在扩散进入阻隔层的过程中,遇到片层状填料绕道而行,气体路径发生曲折,以至于气体穿过阻隔层的路径增加,气体分子的扩散速率降低,提升了阻隔层的气体阻隔性能;第二,片层状填料填充在三维网络结构中,减小了阻隔层内部的空间间隙,提高了阻隔层结构的致密度。将阻隔层与聚氯乙烯基材层结合,得到的高阻隔吸塑包装片材,具有良好的气体阻隔性能和力学性能。
本具体实施例仅仅是对本申请的解释,其并不是对本申请的限制,本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改,但只要在本申请的权利要求范围内都受到专利法的保护。
Claims (5)
1.一种高阻隔吸塑包装片材,其特征在于:包括依次相连的聚氯乙烯基材层与阻隔层,所述阻隔层由包含以下重量份的原料制成:改性树脂55-70份、片层状填料2-7份、交联剂5-8份;
所述改性树脂的制备方法,包括如下步骤:
S1,将二异氰酸酯与多元醇按照质量比为1:(0.6-0.8)反应,得到聚氨酯预聚体;
S2,将聚氨酯预聚体与双端羟基聚硅氧烷按照质量比为1:(0.6-0.8)混合反应,得到改性树脂;
所述S2步骤中,聚氨酯预聚体与双端羟基聚硅氧烷混合反应后,再与氨基酸反应,得到改性树脂;其中,聚氨酯预聚体与氨基酸的质量比为1:(0.2-0.3);
所述片层状填料为云母,所述云母经过改性处理,所述改性处理的方法如下:
将云母升温活化,得到热活化云母;
将热活化云母酸化,得到酸化云母;
将酸化云母与钠盐混合,得到钠化云母;
将钠化云母与改性剂按照质量比为1:(0.08-0.12)混合,得到改性云母;
所述改性剂为十八烷基三乙基溴化铵;
所述交联剂为FEVE型氟树脂;
一种高阻隔吸塑包装片材的制备方法,包括如下步骤:将阻隔层的原料与聚氯乙烯基材层的原料分别投入至挤出机中熔融加工,将阻隔层的原料熔体与聚氯乙烯基材层的原料熔体送入流延机或吹塑机中共挤成膜、冷却,形成依次相连的聚氯乙烯基材层与阻隔层,得到高阻隔吸塑包装片材。
2.根据权利要求1所述的一种高阻隔吸塑包装片材,其特征在于:所述聚氨酯预聚体与双端羟基聚硅氧烷的质量比为1:(0.65-0.7)。
3.根据权利要求1所述的一种高阻隔吸塑包装片材,其特征在于:所述片层状填料的重量份为3-5份。
4.根据权利要求1所述的一种高阻隔吸塑包装片材,其特征在于:所述多元醇为聚酯多元醇。
5.权利要求1-4任一所述的一种高阻隔吸塑包装片材的制备方法,其特征在于,包括如下步骤:
将阻隔层的原料与聚氯乙烯基材层的原料分别投入至挤出机中熔融加工,将阻隔层的原料熔体与聚氯乙烯基材层的原料熔体送入流延机或吹塑机中共挤成膜、冷却,形成依次相连的聚氯乙烯基材层与阻隔层,得到高阻隔吸塑包装片材。
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