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CN102947391A - 膜或板 - Google Patents

膜或板 Download PDF

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CN102947391A
CN102947391A CN2011800313373A CN201180031337A CN102947391A CN 102947391 A CN102947391 A CN 102947391A CN 2011800313373 A CN2011800313373 A CN 2011800313373A CN 201180031337 A CN201180031337 A CN 201180031337A CN 102947391 A CN102947391 A CN 102947391A
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film
plate
polymeric amide
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亚历山大·安东尼厄斯·马莉亚·斯特雷克斯
凯塔琳娜·托米奇
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Abstract

本发明涉及包含具有1，4-丁二胺单体单元和癸二酸单体单元的聚酰胺(PA410)的膜或板。在一个优选的实施方式中，所述膜或板包含PA410以及至少一种另一聚合物。

Description

膜或板
本发明涉及包含聚酰胺的膜或板。
聚酰胺的膜和板已广泛使用。所述膜和板具有优异的性能，如例如良好的机械性能和良好的光学性能，这使膜或板非常适合于生产所有种类产品(特别是食品)的包装。虽然尼龙膜和板具有良好的阻隔性能，但仍需要改进这些性能。这将可以例如使膜和板更薄。
因此，本发明的目标是提供包含聚酰胺的膜或板，其中膜或板表现出改善的阻隔性能。
令人惊奇的是，如果膜或板包含具有1，4-丁二胺单体单元和癸二酸单体单元的聚酰胺，则可实现该目标。具有1，4-丁二胺单体单元和癸二酸单体单元的聚酰胺以下也称为PA410。
包含PA410的膜和板表现出改善的阻隔性能来保护食物。膜和板对含羟基的有机化合物(例如醇，如乙醇)表现出特别好的阻隔性能。这使膜或板也非常地适合于燃料(特别是生物燃料)的包装体的生产。也可用于铰长时间储存例如食物，而不失去味道或风味。
另一个优点是，得到当增加湿度时表现出稳定的氧渗透性的膜和板。这允许灵活设计。另外一个优点是，膜和板展现出高的耐穿刺性。当膜和板用于为了避免对内容物(例如食物或燃料)的损伤的包装时，该性能特别重要。
膜和板为宽和长比其厚度大好几倍的实体。尽管膜和板之间的差异是任意的，但经常假定膜具有相对低的厚度，因而膜非常柔软，使得其可被卷起。板具有较大的厚度，从而不能将其卷起或只能以大的半径(例如至少300mm的半径)卷起，因为否则的话，板将发生永久变形或会断裂。在本发明申请中，假设膜厚度至多为2mm而板厚度在2mm以上到例如20mm。膜可以是例如单层膜或多层膜。当膜为多层膜时，多层膜优选地包含聚烯烃层、连接层和至少一层含PA410的聚合物组合物。聚烯烃为例如聚乙烯或聚丙烯。膜或板可以由包含PA410作为聚合物组合物中的唯一热塑性聚合物的聚合物组合物组成。优选地，膜或板包含至少一种另一聚合物。在一个实施方式中，膜或板由含PA410和至少一种另一聚合物的聚合物组合物组成。在另一个实施方式中，膜或板包含至少一层含PA410的聚合物组合物和至少一层包含所述另一聚合物的聚合物组合物。
作为另一聚合物，聚合物组合物适宜地包含其他脂族聚酰胺(例如PA6、PA66)、(半)芳族聚酰胺(例如诸如PAI-6T、MXD6)、聚酯(例如诸如聚对苯二甲酸乙二醇酯(PET)和聚萘二甲酸乙二醇酯(PEN))、乙烯-乙烯醇共聚物(EVOH)和聚烯烃(例如PE和PP)。可存在连接层，用来在含PA410层和其他层之间获得足够的粘附力。
优选地，膜或板包含至少一层含PA410和另一聚酰胺的聚合物组合物。
一个优点是，较之已知的聚酰胺组合物的膜和板，所得的膜和板具有改善的阻隔性能，但仍可经济地生产。另一个重要的改进是，根据本发明的膜和板不再完全基于化石碳，因为PA410可至少部分基于可再生资源。这是特别有利的，即使膜或板的聚合物组合物只包含一小部分PA410以及还有另一聚酰胺。由膜生产的包装通常只用于作为一次性包装的包装。因此，这些产品对温室气体产生有大的贡献。用至少部分基于源自天然资源的单体的PA410替代所述另一聚酰胺，已经提供了对于温室气体产生的重大减少。
优选地，聚合物组合物包含PA6和/或PA66作为另一聚酰胺。
另一个令人惊奇的优点是，膜和板具有有利的光学性能。膜具有高透明度和低雾度。这是非常令人惊奇的，因为含两种或更多种不同聚合物的聚合物组合物的膜和板通常表现出低水平的光学性能。然而，本发明的膜和板的透明度甚至可比包含PA6或PA66作为唯一聚合物的膜或板的透明度更高。
由二胺和二酸制成的聚酰胺通常表示为AABB树脂，参见例如NylonPlastics Handbook，Edited by Melvin I.Kohan，Hanser Publishers，1995，第5页。命名法遵守如在Nylon Plastics Handbook中所使用的；例如，PA410表示以1，4-丁二胺和癸二酸为构筑基元的聚酰胺。
优选地，至少一层含PA410和所述另一聚酰胺的聚合物组合物包含1-50重量份数(pbw)的PA410和99-50pbw的所述另一聚酰胺，PA410和所述另一聚酰胺总计为100份。更优选地，聚合物组合物包含10-40份的PA410和90-60份的所述另一聚酰胺。
优选地，聚合物组合物包含PA410和所述另一聚酰胺作为全部聚合物。
除PA410外，根据本发明的膜和板的组合物还可包含其他添加剂，例如稳定剂、加工添加剂、成核添加剂。优选地，组合物包含每100pbw的PA410和另一聚酰胺，至多20pbw、更优选至多10pbw、甚至更优选至多5pbw、最优选至多2pbw的其他添加剂。
根据本发明的膜的聚合物组合物可通过以下制成：第一步制备组分PA410(如果合适的话，还有所述另一聚酰胺、其他添加剂)的粉末或颗粒的干混物，其他添加剂以母料提供。此后，组合物颗粒可通过使用熔融混合的装置(例如双螺杆挤出机)来生产。组合物颗粒可被供料至挤出机，来生产膜或板。也可作为干混物将多种组分单独地供料至挤出机。
根据本发明的膜可通过使用用于生产膜的已知工艺(例如吹塑膜工艺和流延膜工艺)来生产。板可通过使用用于生产板的已知工艺来生产，例如通过将熔体挤出通过狭缝模，并最终在两个冷却辊之间成型以及冷却熔体。
根据本发明的膜可以经过面内拉伸。拉伸可以以双轴平面方式进行，无论是以依次方式还是以同步方式。令人惊奇的是，已经发现，能够容易地拉伸根据本发明的膜，这允许快速的加工速度。此外，膜可以经受热定形步骤。
在生产多层膜或板时，使用用于该目的的挤出机。
如果通过吹塑膜工艺生产膜，则得到的管状膜可被进一步加工成袋，优选地用作食品包装的用途。通过流延膜工艺得到的膜可在第一步中焊接成管并随后被加工成袋。
膜还可有利地用作柔性电路板(FCB)的基板材料，因为其表现出改善的尺寸稳定性，或用作太阳能电池的覆盖膜。
可通过深拉工艺(deep drawing processes)由板生产包装。例如可生产盒子、瓶子和盖子，如可用作食品包装的。也可以生产焊接在一起的容器的两部分，例如生产燃料容器。
实施例
除另有说明外，量以相对于组合物中聚酰胺总量的wt％表示。
粘度数(VN)
根据2007版ISO 307，通过以0.005g/ml的浓度溶解PA410样品于甲酸(90wt.％)中，并用Ubelohde粘度计在25℃下测量溶剂(t0)和溶液(t1)的流动时间并通过式VN＝[(t1/t0)-1]×200ml/克计算粘度数，来确定粘度数。
所用化合物
1，10-癸二酸，由中国Dong Fang提供。
1，4-丁二胺，由荷兰DSM提供。
PA410的生产
将350克1，10-癸二酸、157克1，4-丁二胺和420克水在高压釜中90℃下搅拌30分钟，以得到在水中浓度为55wt.％的所述二胺和所述酸的盐溶液。然后通过如下来除水：先在10分钟内升高温度至150℃，在蒸馏下除去约一半量的水，再升高温度至150℃并通过蒸馏进一步除水，以得到含6wt.％水的浓缩溶液。然后，封闭高压釜，升高高压釜中温度至200℃。在该温度下进行30分钟预聚合，随后在氮气气氛下闪蒸高压釜中的内容物，预聚物被造粒并冷却。
将预聚物的颗粒置于滚筒中，在220℃温度下在氮气/水蒸汽气氛(75/25wt.％)中干燥并后缩合48小时。得到的PA410的VN为179ml/g。并且，还得到VN为150ml/g的PA410。除另有说明外，所有含PA410的膜均由VN为150ml/g的PA410制备。
光学透明度；透射率以及雾度的测量；实施例1至14以及对比例A- D
在23℃、50％湿度下对50微米的流延膜进行透射实验。在无样品时，进行空白测试，且每个波长下透射到检测器的光被设为100％。放置样品并重复测量。在每个波长下记录的光透射相对于空白测试标准化，并因此得到以％计的透射率值。基于聚酰胺的总量，测量100wt％PA410的膜(实施例1)，以及PA6分别与1wt％、5wt％、10wt％、25wt％和50wt％的PA410的共混物(分别为实施例2至6)。还测量了PA66与PA410的共混物(实施例7)。作为对比，测量了PA6分别与1wt％和10wt％PA610的两个共混物(对比例A和B)。
并且，根据ASTM标准D 1003-00，程序B在50微米膜上进行雾度测量。在780nm和380nm之间的光谱范围内，得到样品的四个透射光谱。如表1中所描述，四次测量的每一个都需要不同的积分球设置。
表1：确定雾度的测量的概述
测量 放置样品 放置反射率标准 代表量
T1 否 是 入射光
T2 是 是 由样品透射的全部光
T3 否 否 由仪器散射的光
T4 是 否 由仪器和样品散射的光
然后按如下计算百分比雾度：
雾度＝[(T4/T2)-(T3/T1)]×100％
基于流延成50微米的膜的聚酰胺的总量，测量100wt％PA410的膜(实施例8)以及PA6分别与1wt％、5wt％、10wt％、25wt％和50wt％的PA410的共混物(实施例9至13)的雾度。还测量了PA66与PA410的共混物(实施例14)。作为对比，测量了PA6分别与1和10wt％PA610的两个共混物(对比例C和D)。
结果：
实施例1示出了至少91％的透射率。相对于纯PA6膜以及100wt％PA410(实施例1)，实施例2至5示出小于0.2％的透射率差异。共混物的可见光波长的透射率也为至少91％。对包含聚酰胺6，6和聚酰胺4，10的共混物的膜(即实施例7)，观察到类似的效果。相对于纯PA6膜，对100wt％PA410膜(实施例8)以及PA6和PA410的共混物(实施例9至13)，观察到小于0.6％的雾度差异。此外，对于350和1150nm之间的波长，观察到所有实施例的雾度少于1％，这表明非常高的光透射率。对实施例14，即包含PA6，6和PA410的共混物，也观察到类似结果。这些结果清楚地表明根据本发明的膜可得到良好的光学透明度，且在共混物中PA410的量增加时，光学透明度依然良好。
PA610和PA6的共混物的对比测量表明在共混物中PA6，10的量增加后，透射率明显降低(对比例A和B)，以及雾度升高(对比例C和D)。这表明，含聚酰胺6，10的共混物的膜不如根据本发明的膜。
氧透过率，实施例15至22；对比例F
在50微米膜上，对包含聚酰胺6分别与1wt％、5wt％、10wt％的PA410的共混物进行氧透过率测量(实施例15至17)。令人惊奇的是，在干燥条件下，相对于100wt％PA6膜的氧透过率，这些共混物充分保持氧透过率。在潮湿条件(85％相对湿度)下，对于包含聚酰胺6分别与1wt％、5wt％、10wt％的PA410的共混物(实施例18至20)，氧透过率甚至降低。在干燥条件下100wt％PA410膜(实施例21)的氧透过率为4.1ccmm/m2天，这表明较之100wt％PA610膜(对比例E)的氧透过率(表明为6.8ccmm/m2天)更低。在85％的相对湿度下，100％PA410膜的氧透过率为3.67ccmm/m2天(实施例22)，这与100％PA6膜(其为3.24ccmm/m2天，对比例F)是相当的。令人惊奇的是，当作为相对湿度的函数外推氧透过率时，可以看出，当相对湿度为100％时，100％PA410膜展现出比100％PA6膜更低的氧透过率。这对于其中存在湿气的膜应用是有利的。
耐穿刺性；实施例23；对比例G
对根据本发明的膜测量耐穿刺性。从所提供的膜刺冲制出直径70mm的圆形样品。这些圆形样品夹持在内径20mm的铺展工具(span tool)上。将直径为6mm且顶部半径7mm的圆柱状压头以50mm/min的恒速推动穿过样品，直至破裂。在配备了用于负载测量的200N负载传感器的标准拉伸测试机(Zwick Z1474)上进行测试。通过横向位移来确定压头位移。在23℃和50％相对湿度下进行测量，并平行进行6次。通过在负载-位移曲线下的面积除以膜厚度来确定标准化的破裂能(N mm/μm)。结果表示于表2中。
表2耐穿刺性
Figure BDA00002642393800071
Fmax/厚度-标准化的力
W-破裂能
令人惊奇的是，100％PA-410膜的耐穿刺性与100％PA-6膜相当。与其他良好机械性能一起，高的耐穿刺性对膜和板的食品应用是有利的。

Claims (11)

1.膜或板，其包含具有1，4-丁二胺单体单元和癸二酸单体单元的聚酰胺(PA410)。
2.如权利要求1所述的膜或板，其特征在于所述膜或板包含PA410以及至少一种另一聚合物。
3.如权利要求2所述的膜或板，其特征在于所述膜或板由包含PA410和所述另一聚合物的聚合物组合物组成。
4.如权利要求2所述的膜或板，其特征在于所述膜或板包含至少一层含PA410的聚合物组合物和至少一层含所述另一聚合物的聚合物组合物。
5.如权利要求2和4中任意一项所述的膜或板，其特征在于所述膜或板包含至少一层含PA410和另一聚酰胺的聚合物组合物。
6.如权利要求5所述的膜或板，其特征在于所述另一聚酰胺为PA6或PA66。
7.如权利要求5或6所述的膜或板，其特征在于所述至少一层的所述聚合物组合物包含1-50pbw(重量份数)的PA410和99-50pbw的所述另外一聚酰胺，PA410和所述另一聚酰胺总计为100pbw。
8.由如权利要求1-7中任意一项所述的膜或板制成的包装。
9.如权利要求1-7中任意一项所述的膜作为太阳能电池覆盖膜的用途。
10.如权利要求1-7中任意一项所述的膜作为柔性电路板的基板材料的用途。
11.如权利要求1-7中任意一项所述的膜作为用于食物或燃料的包装的用途。
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