CN108883567B - 生产填充膜带的方法 - Google Patents
生产填充膜带的方法 Download PDFInfo
- Publication number
- CN108883567B CN108883567B CN201780019253.5A CN201780019253A CN108883567B CN 108883567 B CN108883567 B CN 108883567B CN 201780019253 A CN201780019253 A CN 201780019253A CN 108883567 B CN108883567 B CN 108883567B
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- film
- polymer component
- melting polymer
- tape
- microporous
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Abstract
本发明涉及一种用于由包含热塑性聚合物材料的微孔初始膜带生产填充膜带的方法,所述填充膜带包含至少一种低熔点聚合物组分,高熔点聚合物组分和填料,其中该方法包括:将所述微孔初始膜带加热到部分熔融状态,在该状态中至少一种低熔点聚合物组分处于熔流状态并且至少一种高熔点聚合物组分不处于熔流状态,和通过引导所述部分熔融的膜带穿过冷却的辊隙进行冷却。本发明还涉及利用所述方法生产的膜带及其用途。
Description
技术领域
本发明涉及一种用于生产填充膜带的方法,一种由此生产的膜带以及其用途,例如用于卫生行业。
背景技术
在关于资源保护和可持续性的环境讨论过程中,为了节省原材料,在薄膜领域,首先是用于卫生行业的一次性产品的薄膜,生产比过去更薄的薄膜,变得越来越重要。另一方面,对填充和透气薄膜的兴趣正在增加,因为它们允许进一步节省塑料。
EP-A-0 768 168和EP-A-1 716 830公开了用于生产能够在卫生领域使用的未填充薄膜的方法。由于它们的应用领域,这种卫生薄膜受到多种要求的限制。它们应该是液密的并且具有特定的触觉特性,例如柔软性,柔韧性,低噪音性和织物感。卫生领域的薄膜应具有柔软的类似材料的手感。特别是,当其用于失禁产品时,噪音应尽可能低,就是说,薄膜应该是低噪音的。与低光泽度相结合,这导致非常有织物感的薄膜,这在卫生领域是理想的。此外,近年来,包含在尿布和失禁产品中的吸收体已经变得越来越薄,这特别是通过使用超吸收聚合物实现的。这些超吸收聚合物以粗粒粉末的形式使用,并且卫生薄膜必须具有这样的强度,使得以高安全性避免由单个颗粒,例如在负重时由于穿戴者坐下或者其它运动而穿透薄膜。必须避免由于超吸收性聚合物形成孔洞(“针孔”)和包装单元中成品薄膜产品的破裂。卫生薄膜的另一个要求在于在例如尿布和卫生巾制造商的高速运转机器(转炉)上加工膜带所需的最小抗拉强度。该最小抗拉强度通常针对纵向(MD)或横向(CD)上5%,10%或25%的拉伸而给定。目前,纵向上5%的拉伸(5%模量)下的抗拉强度应至少为2.5牛/英寸。此外,用于卫生应用的薄膜应该具有一定的强度,例如,单层后片具有至少10牛/英寸的纵向撕裂强度和至少5牛/英寸的横向撕裂强度。如果该后片与绒毛物层压时,纵向撕裂强度应至少为5牛/英寸,并且横向撕裂强度至少为2牛/英寸。
生产透气薄膜的方法例如由EP 0 921 943 B1,EP 1 226 013 B1,EP 1 711 330B1和GB 2 364 512 B已知。透气薄膜必须满足上述针对机械特性的要求,例如未填充的薄膜,并且此外必须是液密性的。即使使用它们,也寻求小的厚度。由此可能会导致多种问题。
为了生产透气的薄膜,薄膜被填充有大约60%的惰性材料并且在挤出后经受拉伸过程(多数情况下是纵向上的拉伸),从而使薄膜透气。使用的填料通常是白垩(CaCO3),粒径为0.8至2μm。在拉伸过程中,薄膜的弹性聚合物部分被拉伸,并且在白垩颗粒的边缘处朝向聚合物基质形成孔。由于扩大白垩粒径(至12μm或更大),总是形成可能导致密封性问题的孔径。如果在拉伸时为了生产尽可能薄的透气薄膜需要相对高的拉伸率,例如2:1至3:1,则该问题会恶化。在纵向上拉伸的薄膜也部分地显示了不密封(即所谓泄漏)的低安全性。还存在一种危险,即在薄膜的一些位置处所形成的孔会过大(>1μm)并且由此形成浸透的问题(就是说,流体抗穿透值(液体冲击值)大于3g/m2)。理想的是流体抗穿透值小于2g/m2或甚至小于1.5g/m2。
众所周知,薄膜具有所谓的追溯效应。这意味着例如已经在80℃下被拉伸并且在100℃下随后经受退火的薄膜在再次达到这些温度时,例如在转炉中非常热的热熔胶(约160℃)时,试图收缩。恰好在填充白垩的薄膜中由于其具有良好的导热性以及特别是在很薄的薄膜中会出现这种问题。在温度负荷太高或薄膜厚度太小时,则会很快形成不期望的孔洞(即所谓的烧穿效应)。
通常现今的透气薄膜在拉伸过程后临时存储几天并且在进行进一步处理,例如印花之前等待后结晶,因为薄膜可能后收缩。因此,如果要印花薄膜,则在拉伸过程之后和印刷之前必须等待约1至3天的结晶时间。该过程导致非常高的成本并妨碍薄膜的联线印刷。
填充和拉伸的薄膜倾向于在成品卷上形成阻塞。阻塞意味着薄膜层通过后收缩而这样彼此粘附,使得在展开时出现困难,例如,该薄膜显示出所谓的螺旋裂缝。在螺旋裂缝中,薄膜部分地粘附在下面的薄膜层上。这导致在展开过程中薄膜撕裂,其中切割镜附近的区域受到特别的影响。阻塞首先在展开薄膜时是一个问题。
在纵向(MD)上拉伸的薄膜对锋利边缘的超吸收颗粒具有低抗穿透性,所述锋利边缘的超吸收颗粒经常在卫生产品中用于流体吸入。因为这些颗粒通常与薄膜直接接触,所以可能导致成品中的针孔和不密封(泄漏)。另外,填充和MD拉伸的薄膜表现出低MD再撕裂强度和低MD撕裂强度。滚卷正面上的最轻微损伤或滚卷上的薄膜轻微堵塞可能导致撕裂和再撕裂,由此形成螺旋裂缝。
拉伸过程通常放大薄膜中厚位置和薄位置之间的差异,并且还可能导致边缘增厚,也称为“颈缩”。这两种效应都会在成品滚卷上产生所谓的活塞环。这意味着,在这些滚卷展开时会在薄膜中形成长边或松弛,这又可能导致转换过程中的很大困难(例如,薄膜的CD偏移)。高拉伸度放大薄膜的边缘增厚(颈缩)、拉伸过程后薄膜的后收缩和纵向上薄膜的非常低的再撕裂强度。通常,滚卷也被临时存储在所谓的母滚卷中并且只在完成后收缩(结晶)之后供应给切割重卷机,在该切割重卷机中然后将所述滚卷切割成所需的客户宽度。透气薄膜的后收缩会在成品滚卷上触发相当大的层压力,这又会在薄膜层之间触发阻塞,并在薄膜展开时导致螺旋裂缝。
特别是在后片(即尿布和卫生产品的衬垫层)的情况下,边缘增厚效应,例如松弛和长薄膜边缘,在进入转炉时会引起很大问题,因为一方面,纵向上的拉伸过程剧烈放大了厚位置和薄位置,另一方面,薄膜的偏移可能在横向(CD)上发生,这可能最终导致转炉的停顿。因此,转炉中计划安排的后片进入非常重要。
发明内容
为了解决这些问题中的一个或多个,本发明建议将填充的微孔初始膜带加热到部分熔流状态并且随后在冷却的辊隙中快速冷却。填充的微孔初始膜带具有微孔。如果在孔之间存在连接,则薄膜是透气的。令人惊讶地发现,当薄膜被加热到部分熔流状态时,填充的透气薄膜和填充的不透气薄膜情况下的孔不会闭合,而是仍然存在。通过部分熔流状态和随后的薄膜冷却,薄膜的性能得到显著改善并且上述问题由此得到解决。
因此,本发明涉及一种用于由包含热塑性聚合物材料的微孔初始膜带生产填充膜带的方法,所述填充膜带包含至少一种低熔点聚合物组分,高熔点聚合物组分和填料,其中该方法包括以下步骤:将所述微孔初始膜带加热到部分熔融状态,在该状态中至少一种低熔点聚合物组分处于熔流状态并且至少一种高熔点聚合物组分不处于熔流状态,和通过引导所述部分熔融的膜带穿过冷却的辊隙进行冷却。
填充的微孔初始膜带可能是透气的或不透气的。在这种情况下,概念“微孔”是指存在基本上大小为0.1至5μm的孔。基本上就是说至少90%的孔,优选95%,更优选99%的孔,或甚至99.9%的孔具有0.1至5μm的大小并且剩余的孔稍大,一般可达15μm。
微孔初始膜带可以是多层的或多个分层的。在优选实施方式中,微孔初始膜带是共挤出的膜带。在其它实施方式中,微孔初始膜带不共挤出。在另一些实施方式中,微孔初始膜带是多层或多个分层的非共挤出的膜带。
在其它实施方式中,微孔初始膜带是单层的。
在本发明的一种优选实施方式中,该初始膜带在纵向(MD)或横向(CD)上,或在纵向和横向上拉伸。在另一优选实施方式中,该初始膜带在生产时,例如在其挤出之后,以1.2:1至4:1,特别是1.3:1至3.5:1或1.5:1至3:1的拉伸比被拉伸。
优选地,微孔初始膜带,基于100重量%的初始膜带,包含10至90重量%的填料,特别是20至80重量%的填料,优选30至75重量%的填料,更优选50至60重量%的填料。在一种优选实施方式中,初始膜带是透气的。在另一优选实施方式中,微孔初始膜带不透气。在另一优选实施方式中,在根据ASTM E398在37.8℃和90%相对湿度下测量时,膜带具有在24小时内500至5000g/m2的水蒸气渗透率。这里给出的水蒸气渗透率的值或值范围涉及这个测量方法。例如,可以用测量设备Lyssy测量。
在进一步优选实施方式中,基于100重量%的低熔点和高熔点聚合物组分,使用具有15至85重量%的低熔点聚合物组分和85至15重量%的高熔点聚合物组分的初始膜带。优选地,使用具有至少一种聚乙烯作为低熔点聚合物组分和至少一种聚丙烯作为高熔点聚合物组分的初始膜带。
特别地,加热初始膜带到低于至少一种高熔点聚合物组分的结晶熔点的5至20℃。优选地,通过加热筒加热初始膜带,其中这样选择加热筒的温度,使得在加热筒的缠绕段上进行加热。
在优选实施方式中,微孔初始膜带的加热通过加热筒进行,其中在加热筒和膜带之间不存在绒毛物(Vlies)。在这些实施方式中,膜带与加热筒直接接触。也可能是这样的实施方式,其中在加热筒和膜带之间不存在绒毛物,并且绒毛物带搁置在膜带上或在所述膜带上方被引导。在其它优选实施方式中,微孔初始膜带的加热在没有绒毛物的情况下通过加热筒实施。这意味着,在加热筒和膜带之间没有绒毛物,并且在膜带上没有绒毛物。在其它具有绒毛物的实施方式中,绒毛物存在于加热筒与膜带之间。
在进一步优选的实施方式中,将冷却的辊隙中的膜带冷却到至少一种低熔点聚合物组分的结晶熔点以下至少10至30℃。优选地,冷却的辊隙由压花辊和橡胶辊构成。冷却后可以印刷膜带。
另外,本发明还涉及一种利用前述方法生产的膜带,例如具有1至30g/m2,特别是5至25g/m2,优选为7至20g/m2,更优选为10至20g/m2的单位面积重量,以及其用途,特别是在卫生或医疗领域,例如用于尿布中的后片,用于床垫或卫生巾。此外,本发明还涉及所生产的膜带在建筑领域中的用途,例如用作盖膜,或用作汽车保护膜。
附图说明
本发明的优选实施方式在以下描写、附图、示例和从属权利要求中得到描述。
在附图中:
图1示出了用于实施根据本发明的方法的一种优选实施方式。
图2示出了薄膜的根据其加热筒温度的收缩率和单位面积重量。
图3示出了薄膜和对比薄膜根据水浴温度的收缩率。
具体实施方式
在本发明中,给出的熔点,熔化范围和结晶熔点涉及根据DSC(差示扫描量热法)测定。
根据本发明,初始膜带包含或包括至少一种低熔点聚合物组分和至少一种高熔点聚合物组分。换言之,初始膜带包含一种或多种低熔点聚合物组分和一种或多种高熔点聚合物组分。本发明中此外还使用的概念“低熔点聚合物组分”和“高熔点聚合物组分”也是同样的含义,就是说,它们还包括一种或多种低熔点或高熔点聚合物组分。初始膜带优选包括一种,优选两种低熔点聚合物组分。它优选包含一种,特别是两种高熔点聚合物组分。在本发明的其它实施方式中,它优选包含三种低熔点聚合物组分和/或三种高熔点聚合物组分。根据本发明,初始膜带的聚合物材料属于低熔点聚合物组分还是属于高熔点聚合物组分,取决于聚合物材料相对于加热温度的相应结晶熔点,熔点或熔化范围。在给定的加热温度下,将熔流的聚合物材料归为低熔点聚合物组分,将非熔流聚合物材料归为高熔点聚合物组分。
众所周知,聚合物不具有明确限定的熔点,而是具有熔化范围,然而其中可以使结晶熔点对应聚合物的结晶区域。这个结晶熔点总是高于非结晶构成部分的熔点或熔化范围。通过剪切模量接近零来描述熔流状态。在具有结晶区域的聚合物的情况下,后者不再可检测到。剪切模量可以例如根据ISO6721-1和2确定。在本发明中,将初始膜带加热到低熔点聚合物组分的剪切模数为零,且高熔点聚合物组分的剪切模数不为零的温度。然后对于低熔点聚合物组分,不再能检测到结晶区域,并且低熔点聚合物组分处于熔流状态。相反,对于高熔点聚合物组分,仍然可以检测到结晶区域,并且这些高熔点聚合物组分处于熔流状态以下。总之,初始膜带的整个聚合物材料的剪切模数因此不为零,并且仍然可以检测到高熔点聚合物组分的结晶区域。因此存在一个部分融化的膜带。
原则上,作为用于初始膜带的两种聚合物组分的材料考虑使用具有相应熔点的所有热塑性聚合物。为此,大量商业产品可以在市场上获得。优选地,使用不同的聚烯烃,特别是聚乙烯,聚丙烯,乙烯和丙烯的共聚物,乙烯和丙烯和其它共聚单体的共聚物,或它们的混合物。此外,乙烯醋酸乙烯酯(EVA),乙烯丙烯酸酯(EA),乙烯丙烯酸乙酯(EEA),乙烯丙烯酸(EAA),乙烯丙烯酸甲酯(EMA),乙烯丙烯酸丁酯(EBA),聚酯(PET),聚酰胺(PA),例如,尼龙,乙烯乙烯醇(EVOH),聚苯乙烯(PS),聚氨酯(PU),热塑性烯烃弹性体或热塑性醚酯嵌段弹性体(TPE-E)是合适的。
低熔点聚合物组分的总量优选为90至10重量%,特别是90至20重量%,优选80至30重量%,更优选为80至40重量%,最优选70至50重量%。各自基于100重量%的低熔点和高熔点聚合物组分,高熔点聚合物组分的总量优选为10至90重量%,特别是10至80重量%,优选20至70重量%,更优选为20至60重量%,最优选30至50重量%。可替代地,再次基于100重量%的低熔点组分和高熔点组分,优选低熔点聚合物组分的总量为85至15重量%,特别是75至25重量%,且高熔点聚合物组分的总量为15至85重量%,特别是25至75重量%。例如,这些量在低熔点聚合物组分中可以涉及一种或多种聚乙烯,在高熔点聚合物组分中可以涉及一种或多种聚丙烯。
在一种特别优选实施方式中,初始膜带包含至少一种聚乙烯作为低熔点聚合物组分和至少一种聚丙烯作为高熔点聚合物组分。
优选地,低熔点聚合物组分包含乙烯聚合物或由其构成,其中乙烯均聚物和具有乙烯的乙烯共聚物两者作为主要单体,以及乙烯均聚物和乙烯共聚物的混合物(共混物)是合适的。合适的乙烯均聚物是LDPE(低密度聚乙烯),LLDPE(线性低密度聚乙烯),MDPE(中密度聚乙烯),和HDPE(高密度聚乙烯)。用于乙烯共聚物的优选共聚单体是乙烯以外的其它烯烃,除了丙烯,例如丁烯,己烯或辛烯。在乙烯共聚物的情况下,共聚单体含量优选低于20重量%,特别是低于15重量%。在一种优选实施方式中,低熔点聚合物组分仅由乙烯均聚物或乙烯均聚物(例如LDPE和LLDPE)的混合物构成,它们各自的含量可为10至90重量%,以及0至50重量%的MDPE。特定的实例是60重量%的LDPE和40重量%的LLDPE构成的聚乙烯或80重量%的LDPE和20重量%的LLDPE构成的聚乙烯。
除乙烯均聚物和/或乙烯共聚物外,低熔点聚合物组分还可包含其它热塑性聚合物。这些热塑性聚合物不受限制,只要全部低熔点聚合物组分处于熔流状态的温度不接近高熔点聚合物组分处于熔融状态的温度即可。也可能的是,低熔点聚合物组分包含聚丙烯,其熔点或熔化范围不高于乙烯均聚物或乙烯共聚物的熔点或熔化范围,或高于此值,但仍低于所用的加热温度。众所周知,存在高度结晶的全同立构,较少结晶的间同立构和非晶无规立构聚丙烯,它们具有不同的熔点,熔化范围或结晶熔点。当使用非晶无规立构聚丙烯,其熔点或熔化范围比全同立构和需要时的间同立构聚丙烯低得多时,这可取决于加热温度,在需要时将其归于低熔点聚合物组分。
优选地,高熔点聚合物组分包含至少一种聚丙烯,其熔点,熔化范围或结晶熔点显著高于低熔点聚合物组分的熔点,熔化范围或结晶熔点。合适的聚丙烯特别是全同立构聚丙烯。还可以使用间同立构聚丙烯,条件是其熔点,熔化范围或结晶熔点显著高于低熔点聚合物组分的熔点,熔化范围或结晶熔点。合适的聚丙烯是可商购的,例如用于生产吹塑薄膜和/或流延薄膜(浇铸薄膜)。
高熔点聚合物组分可包括丙烯均聚物和以丙烯作为主要单体的丙烯共聚物。在丙烯共聚物中,共聚单体的比例,即非丙烯的比例,在这种情况下,取决于其它组分和低或高熔点聚合物组分的加热温度。适用于丙烯共聚物的共聚单体是丙烯以外的其它烯烃,优选乙烯。在丙烯-乙烯共聚物中,乙烯含量优选为2至30重量%,特别优选2至20重量%,并且特别是2至15重量%,其中实际上在乙烯含量为3至20重量%时获得了非常好的结果。这些数值也适用于其它烯烃。
下面给出若干聚乙烯和聚丙烯的熔化范围:
LDPE:110-114℃;
LLDPE:115-130℃;
HDPE:125-135℃;
丙烯均聚物:150-165℃;
丙烯-乙烯共聚物:120-162℃,乙烯含量很少时,温度也会更高;
双模态丙烯-乙烯(均聚)共聚物:110-165℃。
也可以使用所谓的双模态聚丙烯。这些是两种不同的聚丙烯,每种聚丙烯具有不同的共聚物含量,它们在一种原料中混合。这种双模态聚丙烯具有两个结晶熔点,其中两种聚丙烯的大概比例通常也可以通过DSC分析来确定。作为一个例子,可提及双模态聚丙烯,其结晶熔点为125℃和143℃,两种不同的聚丙烯的比例为25/75。根据本发明,在130℃的加热温度下,25%的聚丙烯会分配具有低熔点聚合物组分的结晶熔点125℃并且75%的聚丙烯会分配具有高熔点聚合物组分的结晶熔点143℃。
在一种特别的实施方式中,使用具有以下聚合物构成部分的初始膜带:25至80重量%,特别是25至60重量%的LLDPE,例如具有5至15重量%辛烯部分的乙烯-辛烯共聚物;20至30重量%的丙烯-乙烯共聚物,具有3至12重量%的乙烯;和其余LDPE;各自基于100重量%的低熔点和高熔点聚合物组分。
正如在低熔点聚合物组分中可存在特定熔融聚丙烯一样,在高熔点聚合物组分中也可存在特定未熔融聚乙烯,其然后被算作高熔点聚合物组分。以下示例说明了这一点。一种适合用于微孔初始膜带的配方作为聚合物构成部分包括:30重量%的LDPE(熔点112℃),30重量%的LLDPE(熔点124℃),20重量%的HDPE(熔点130℃)和20重量%的聚丙烯(熔点160℃)。如果将膜带加热到126℃的温度,则LDPE和LLDPE根据本发明处于熔流状态,但不仅聚丙烯而且HDPE也不处于熔流状态。
用于实施本发明方法的微孔初始膜带可通过本领域已知的任何方法生产。例如,可以生产初始膜带,其方法在于将聚合物构成部分和填料在挤出机,例如复合挤出机中加热至明显高于聚合物构成部分的熔体流动温度的温度(例如,高于200℃)并熔融。接下来是铸造过程(铸造方法),例如通过狭缝喷嘴,或吹塑方法。这些方法在本领域中是已知的。在狭缝喷嘴方法中,薄膜通过宽狭缝喷嘴挤出。优选吹塑方法,其中构成吹塑软管。所构成的软管薄膜可以折叠成扁平并在端部处切开以形成两个膜带,每个膜带都可以用作初始膜带。
为了产生初始膜带的微孔性,可以对挤出薄膜实施拉伸过程。可以在纵向(MD),横向(CD)或纵向和横向方向上进行拉伸。另外,可以进行环轧。
初始膜带可以拉伸。拉伸,延伸或扩展薄膜意味着薄膜在给定方向上膨胀,导致薄膜厚度减小。薄膜可以在机器或纵向方向(MD)上拉伸,例如通过包括两个或更多辊的拉伸单元,例如以不同速度驱动的三个辊。例如,薄膜可以以1:1.5的拉伸比拉伸,这意味着薄膜厚度由例如15μm减少到10μm。还可以使膜带进行横向扩展(CD)。这种双轴扩展可以通过例如市场上可获得的拉伸机,例如布鲁克纳(Brückner)公司获得的拉伸机来实现。所使用的拉伸比取决于薄膜配方和所选择的方法参数,并且可以是至少1:1.2,优选至少1:1.5,特别是至少1:2,更优选至少1:2.5,再优选至少1:3或者至少1:4。
根据本发明使用的初始膜带包含填料。合适的填料不受任何限制,并且是本领域技术人员已知的。所有可以研磨成一定尺寸但在挤出机中不熔化且不能拉伸的物质都是合适的。特别合适的是无机填料,例如白垩(碳酸钙),粘土,高岭土,硫酸钙(石膏)或氧化镁。此外,合成填料,例如碳纤维,纤维素衍生物,研磨塑料或弹性体也是合适的。最优选的是碳酸钙或白垩,因为其价格低廉,但从可持续性的角度来看也是如此。填料的粒度可以是例如0.8至2μm。如果需要具有比白垩更均匀的粒度的填料,也可以使用具有均匀粒度或粒度分布的合成填料。该薄膜可包含少量填料,例如5至45重量%或10至50重量%,从而尽管在拉伸过程中形成孔,但这些孔是隔离存在的并且薄膜不透气。为了实现该薄膜的透气性,有利地是基于100%重量的包括填料的初始膜带的总配方,使用至少35重量%的填料,特别是至少45重量%的填料,优选至少55重量%的填料,更优选至少65重量%的填料。填料的上限由此确定,即不再更多产生孔,而是形成孔洞或薄膜破裂。具有填料的合适的薄膜配方可以由本领域技术人员常规确定。特别合适的是具有35至75重量%,特别是45至75重量%,优选55至70重量%的填料的配方,基于100重量%的初始膜带。非透气性薄膜的示例性的配方包括5至50重量%,特别是10至40重量%的填料,基于100重量%的初始膜带。基于100重量%的初始膜带,透气薄膜的示例性配方包括35重量%至80重量%,特别是45重量%至75重量%的填料。应注意不要将低熔点组分的比例选择为高到达到透气性的程度,由于孔再次闭合,透气性会再次丢失。
如果微孔初始膜带是多层且不透气的,则填料可以在初始幅的一个或多个薄膜层中。如果微孔初始膜带是多层和透气的,则所述填料可位于的初始幅的一个或多个薄膜层中,其中每个薄膜层中的填料的量被选择为使得该薄膜层是透气的。
微孔初始膜带优选具有0.1至5μm,特别是0.1至3μm,或0.2至1μm的微孔。此外,可能存在若干较大的孔。
初始膜带可以是单层或多层的,即单一挤出或共挤出。使用的层数或分层数没有限制。可能有一个或多个层或分层,例如一层,两层,三层或四层。也可能是5,7或9层。所述层或分层可具有相同或不同的配方,其中分配给所述低或高熔点聚合物组分各自通过结晶熔点得到测定。这些层或分层可以通过吹塑挤出或流延挤出(Castextrusion)制成。在多层初始膜带的情况下,至少一层可通过吹塑挤出生产,并且至少另一层可通过流延挤出生产。吹塑挤出和/或流延挤出的薄膜,薄膜层或薄膜分层的组合没有限制。共挤出层或分层的数量没有限制。
在其它实施方式中,初始膜带不共挤出。
初始膜带也可以在示例性实施方式中如下所述制造:
-吹塑挤出,切割,在两个单独的带或单独的滚卷上;
-吹塑挤出,切割,同时成两个或更多单独的带;
-吹塑挤出,切割,平放为非分离软管;
-吹塑挤出,切割成来自不同挤出机的两个或更多单独的带;或
-同时流延挤出成两个或更多单独的带。
也可以联线生产薄膜。在这种情况下,存在用于挤出和拉伸(MDO,双轴或环轧制)过程以及进一步处理(例如压花和印刷)的生产步骤。
用于本发明方法的初始膜带可以用二氧化钛着色,例如白色。此外,初始膜带可包含常规添加剂和加工助剂。特别地,在这种情况下,除了上述填料还涉及颜料或其它着色剂,防粘连剂,润滑剂,加工助剂,抗静电剂,杀菌剂(杀生物剂),抗氧化剂,热稳定剂,抗紫外光的稳定剂或其它用于属性改进的添加剂。通常,这种材料以及填料在根据本发明的初始膜带加热之前加入,例如当初始膜带在聚合物熔体中生产时或在挤出成薄膜之前。
该初始膜带优选具有的单位面积重量在小于50g/m2的范围内,特别是小于40g/m2,优选小于30g/m2,更优选小于20g/m2。单位面积重量在10g/m2以下或5g/m2以下也是可能的。优选单位面积重量在1至30g/m2,1至25g/m2或1至20g/m2,特别是从1至15g/m2,更优选2至10g/m2或7至20g/m2范围内。单位面积重量也可以是1至10g/m2,5至10g/m2或5至15g/m2。初始膜带的厚度可以为2至30μm,特别是2至15μm,5至20μm或5至10μm。
在本发明的方法中,执行初始膜带的加热直到或高于低熔点聚合物组分的熔流状态并低于高熔点聚合物组分的熔流状态。在这种情况下,直到熔流状态意味着低熔点聚合物组分处于熔流状态。然而,其仅被加热到高熔点聚合物组分不处于熔流状态。
为了能够在更长的时间段内实现稳定的过程引导,低熔点和高熔点聚合物组分的(结晶)熔点应该有利地彼此不太接近。优选地,低熔点聚合物组分的结晶熔点,或者在存在多种低熔点聚合物组分的情况下,多种低熔点聚合物组分中具有最高的结晶熔点的低熔点聚合物组分的结晶熔点为低于上述结晶熔点或高熔点聚合物组分的熔流状态至少约5℃,优选至少约10℃,特别是至少约20℃,或在存在多种高熔点聚合物组分的情况下,比具有最低的结晶熔点的高熔点聚合物组分低至少约5℃,优选至少约10℃,特别是至少约20℃。
为了实现低熔点聚合物组分的熔流状态,但不是高熔点聚合物组分的熔流状态,特定选择的温度差没有特别的限制,只要上述条件得到满足。通过关于方法实施的安全性的实际考虑或通过经济方面的考虑方便地确定所选择的温度差。例如,如果在某一温度下低熔点聚合物组分已熔化,则进一步升温将不会产生更好的结果。另外,热消耗增加,并且需要时,太接近高熔点聚合物组分的熔化范围,从而该方法更难以进行。因此,优选地,本发明的方法这样实施,使得初始膜带被加热至低于高熔点聚合物组分的结晶熔点5至20℃,优选5至15℃或10至20℃,特别是10至15℃或15至20℃。可替代地,加热至高于低熔点聚合物组分的结晶熔点或熔流状态尤其为1至20℃,优选2至10℃的温度下进行,。必须确保达到低熔点聚合物组分的结晶熔点。
根据本发明,初始膜带的加热可以借助至少一个加热辊进行。优选地,借助作为接触辊的一个或多个加热辊进行加热,所述加热辊借助热载体(例如蒸汽,水,油)加热到预定温度。在一种优选实施方式中,使用单个加热辊或接触辊。然而,也可以使用两个或更多个加热辊,其中必须确保在冷却的辊隙之前达到低熔点聚合物组分的熔流状态。为了确保初始膜带实际上达到加热辊的温度或者在高生产速度下(其中加热筒的表面温度高于薄膜的表面温度)可靠地实现低熔点聚合物组分的熔流状态,必须确保初始膜带在加热辊表面上的足够停留时间。这可以通过根据薄膜厚度的加热筒的相应的环形段,加热辊直径和/或膜带速度达到。有利的是,可以使用具有不粘涂层表面的加热辊,以使膜带更容易从加热辊上脱离并且由此防止膜带撕裂。由此避免了脱离点在加热辊的旋转方向上偏移,并且不需要或仅需要小的提前量。例如,PTFE(聚四氟乙烯)涂覆的加热辊用于此目的。
膜带的加热也可以用其它加热方法进行,例如辐射热,例如用红外加热或辐射。除了一个或多个加热辊之外,还可以设置另外的加热,例如红外加热。
在一种优选实施方式中,在没有绒毛物带的情况下,将填充的拉伸膜带加热至部分熔流状态。与EP 1784 306 A1不同,在本发明的情况下,可以在没有绒毛物带的情况下在加热筒和膜带之间加热至部分熔流状态。在优选实施方式中,微孔初始膜带的加热通过加热筒进行,其中在加热筒和膜带之间不存在绒毛物。在这些实施方式中,膜带与加热筒直接接触。也有可能在加热筒和膜带之间不存在绒毛物,并且绒毛物带放置在膜带上或在膜带上方引导。在其它优选实施方式中,微孔初始膜带的加热在没有绒毛物的情况下通过加热筒进行。这意味着在加热筒和膜带之间没有绒毛物,并且膜带上没有绒毛物。在可选的实施方式中,在加热筒和膜带之间存在绒毛物。
根据本发明,在加热之后引导膜带穿过冷却的辊隙。构成冷却的辊隙的辊子这样被冷却,从而实现快速和迅速的冷却。冷却至低于低熔点聚合物组分的结晶熔点的温度,优选冷却到低于低熔点聚合物组分的结晶熔点的温度至少5℃,特别是冷却到低于低熔点聚合物组分的结晶熔点的温度至少10℃,是有利的。优选的冷却范围是低于低熔点聚合物组分的结晶熔点的5至10℃,更优选10至30℃。例如,用水在5至20℃的温度范围内,例如用约为10℃的水冷却辊。加热辊或者(当使用多个加热辊时)最后一个加热辊和/或其它加热源和冷却的辊隙之间的距离由于可能的热损耗而选择得不太大。
冷却的辊隙在最简单的情况下例如可以是具有两个平滑辊子的平滑辊隙。然而,在卫生薄膜的情况下,辊隙优选由具有图案辊和平滑辊(例如橡胶辊)的一对辊构成,由此膜带获得结构化的表面。卫生领域中的优选结构是微结构,例如截头金字塔。优选地,冷却的辊隙由钢辊和反压工作橡胶辊构成,其中钢辊配备有结构化的表面。钢辊可以配设有织物状雕刻,其增强了膜表面的织物外观。钢辊的压花结构进一步降低了薄膜的光泽度。
构成冷却的辊隙的辊的速度可以这样选择,使得该速度等于加热辊的速度,或者在使用多个加热辊的情况下,等于最后加热辊的速度,从而薄膜在其间不被拉伸。构成冷却的辊隙的辊的速度也可以这样选择,使得该速度大于或小于加热辊的速度,或者在使用多个加热辊,大于或小于最后加热辊的速度,从而薄膜在其间被拉伸或收缩。由于热量损耗,加热辊和冷却的辊隙之间的距离应保持尽可能低。
取决于膜参数和其它工艺条件,膜带速度在50至900m/min的范围内。加热辊的速度优选为50至900m/min,特别是50至800m/min,优选100至600m/min。构成冷却的辊隙的辊的速度优选为50至900m/min,特别是50至800m/min,优选100至600m/min。这样选择加热辊和冷却辊的速度,使得根据薄膜配方和所选择的工艺参数,使得它们相同或不同,从而薄膜以所需的比例拉伸或收缩(退火)。
根据本发明的方法使得可以生产具有非常低单位面积重量的薄膜,例如,2,3,4,5,6,7,8,9,10,11,12,13,14,15,16,17,18,19,20或25g/m2。相应的膜厚度在例如25,20,19,18,17,16,15,14,13,12,11,10,9,8,7,6或甚至仅5μm的范围内。优选的薄膜的厚度为2至13μm或4至25μm,或者单位面积重量为1至15g/m2或4至25g/m2或7至20g/m2。
根据本发明获得的薄膜虽然非常薄且具有微孔性,但具有优异的机械性能,此外还具有高的抗穿透强度(即对例如尿布中的超吸收颗粒的耐受性)和高的热稳定性(即对热熔粘合剂的耐受性)。
根据本发明获得的薄膜可以以已知的方式进一步加工。例如,可以由其制造单个后片或绒毛物薄膜层压板。为了生产绒毛物薄膜层压板,薄膜可以借助粘合剂优选联线地粘合绒毛物。此外,绒毛物薄膜层压板也可以通过本领域技术人员已知的热粘合来生产,其中根据本发明获得的薄膜的材料和/或绒毛物的材料逐点地借助两个加热的辊,通常是压花辊(雕刻钢辊)和作为反辊的平滑钢辊,通过高温和高压而熔化并且由此将薄膜和绒毛物连接在一起。另外,如上所述的绒毛物薄膜层压板也可以借助热层压来生产。特别是在非常薄,例如小于10g/m2,或例如4g/m2的膜的情况下,热层压是优选的。此外,绒毛物薄膜层压板也可以借助超声波层压(例如用超声赫尔曼技术)生产。所生产的绒毛物薄膜层压板可以以常规方式进一步加工,其中也可以在纵向或横向或两个方向上进行拉伸。同样,可以进一步处理单个后片。
图1示出了用于实施根据本发明的方法的优选实施方式。例如来自挤出机的填充膜A运行经过带有辊1,2和3的拉伸单元,由此该膜变成微孔的。例如,三个辊子可以100/200/200m/min或100/150/200m/min的辊速运行。通过引导辊4,5和6使微孔初始膜带B向加热辊7上运行。加热辊7例如是抗粘涂层钢辊,其借助热量供应被加热到所需的表面温度。然后,膜带在加热辊7上运行并在此根据本发明被加热到部分熔流状态下。部分熔流的膜带C从加热辊7运行到冷却的辊隙中,该冷却的辊隙由辊8和9构成。辊8优选构成为结构或压花辊,由此膜带获得压花结构或结构化的表面。辊9优选为橡胶辊。辊对8/9优选是水冷的,例如以约10℃的水冷却。这样驱动构成冷却间隙的辊8和9,使得与加热辊7的幅速相比,形成更高,更低或相等的速度。在冷却的辊隙中,膜带被迅速冷却并压花。辊对8/9之后,膜可以直接移除,或者通过也可以被冷却的导向辊10和11也可以将膜带D提供给例如具有辊子12的印刷单元,以印刷该膜带。此后可以除去膜E。
由于生产厚度极小的膜,本发明可以节省原材料,从而有助于资源保护和可持续性。因此,它为环境保护做出了贡献。这适用于卫生部门的薄膜以及其它应用,首先是在薄膜广泛用作一次性产品的构成部分的应用中。
相反,鉴于上述现有技术中的问题,根据本发明生产的薄膜提供了许多改进和优点:
-薄膜允许高温负载,例如在热熔胶中。
–薄膜几乎没有后收缩。
–由于其压花结构,薄膜还可以防止阻塞,因为该结构用作薄膜层之间的间隔物并且由此防止薄膜各层的粘附。
-由于其压花结构,薄膜一方面可以防止薄膜各层的粘附,另一方面可以增加薄膜的平整度,因为压花结构可以平衡厚位置和薄位置。由于颈缩导致的可能的边缘增厚可以通过调整压花压力来得到均衡。
–薄膜具有增加的进一步撕裂强度(因为在拉伸过程之后薄膜的“软退火”)。因为通过压花结构在z方向上具有薄膜取向,因此三维压花结构防止了薄膜的轻易撕裂。
-薄膜具有增强的抗穿透性。三维压花结构通过超吸收颗粒防止薄膜的点状撕裂,因为z方向上的薄膜取向通过压花结构而存在。
-变得太大的孔会收缩,并且因此可以降低高液体冲击值。这意味着通过根据本发明的方法可以将大于1μm的变得太大孔收缩至<1μm的尺寸。在压花单元中,通过接触压力和迅速冷却将压花结构置入薄膜中,同时孔径被冷冻并因此固定。
-因为薄膜几乎没有任何可测量到的后收缩,所以其可以在拉伸过程之后直接联线印刷,例如采用接于中间的“热压花工艺”印刷。
-薄膜在高热负荷下,例如当施加热熔粘合剂体系时具有较高的阻力或低收缩行为或较低的所谓烧穿效应,由此减少或不再发生孔的形成。
根据本发明获得的薄膜可用于许多领域。其用于卫生或医疗领域,例如作为清洗保护膜或通常作为液体不可渗透的阻挡层,特别是作为尿布,卫生巾,床垫或类似产品中的后片。此外,这些薄膜可用于其它技术领域,例如建筑领域中作为建筑薄膜,例如用于屋顶衬垫,顶楼覆盖物或墙壁覆盖物,或用作汽车领域的汽车保护薄膜。
根据本发明获得的薄膜可以以已知的方式进一步加工,例如加工为绒毛物薄膜层压板。为了生产这种层压板,其可以用粘合剂粘合,优选联线粘合。此外,绒毛物薄膜层压板也可以通过本领域技术人员已知的热粘合来生产,其中根据本发明获得的薄膜的材料和/或绒毛物的材料逐点地借助两个加热的辊,通常是压花辊(雕刻钢辊)和作为反辊的平滑钢辊,通过高温和高压而熔化并且由此将薄膜和绒毛物连接在一起。另外,绒毛物薄膜层压板也可以借助热层压,如EP 1 784 306 B1中所述来生产。特别是在非常薄,例如4g/m2的膜的情况下,热层压是优选的。可选地,绒毛物薄膜层压板也可以借助超声波层压(例如用超声赫尔曼技术)生产。所生产的绒毛物薄膜层压板可以以常规方式进一步加工。
在不限制本发明的情况下,将参考以下示例更详细地阐述本发明。
示例
这些示例说明了根据本发明的薄膜的生产,并示出了它们在热收缩时的特性。
示例1
根据常规方法,通过吹塑挤出由两种不同聚丙烯化合物构成的白垩填充膜制备薄膜。两种聚丙烯化合物具有不同的熔点/熔化范围。较高熔点的聚丙烯化合物含有92.5重量%的聚丙烯(PP)和7.5重量%的乙烯共聚物。其具有约164℃的DSC熔点并且基于100重量%所使用的聚合物材料(即,无填料)以16重量%的量得到使用。低熔点聚丙烯化合物含有90.5重量%的PP和9.5重量%的乙烯共聚物。其具有约138℃的DSC熔点,并且基于100重量%的所用的聚合物材料以80重量%的量得到使用。每种化合物的白垩含量为约60%(基于100重量%的化合物)。基于100重量%所使用的聚合物材料,仍有4重量%的LDPE(DSC熔点为111℃)。
在挤出过程之后将填充的挤出薄膜供给根据图1的拉伸压花印刷机。在这种情况下,薄膜A借助回火的拉伸辊1/2/3在纵向上扩展约2:1,以产生透气性。随后,透气薄膜B加热筒通过具有不同的加热筒温度的加热筒7加热,如下表1所示。通过加热筒7加热薄膜之后,将薄膜C供给压花单元(压花辊8和橡胶辊9),同时保持这种状态,并在其中设置压花结构。压花橡胶辊高度冷却(<30℃)并且处于数吨的相互接触压力下,例如在辊的每一侧上具有4至10吨的接触压力值。薄膜D被迅速冷却并且压花单元进行压花。
表1显示了薄膜在热收缩时如何根据使用的加热筒温度表现特性。
根据ASTM D2732-96如下确定热收缩。
描述
根据ASTM D2732-96的热收缩测试确定材料取向的程度。
在这种情况下,将限定的样品(10×10cm)在80℃的水浴中加热,并在30秒后再次冷却。
给出的收缩值是样品的长度差异,以%表示。
测试设备
收缩浴,卷尺
样品制备
在样品上,借助方板记录100×100mm的正方形,
并用卷尺控制。
样品标有纵向或横向。
执行
将收缩浴调节至80℃。
将样品浸入加热的水浴中,30秒后小心取出并冷却(水槽中的水浴)。
分析
纵向和横向的收缩值:最初标记的测量长度和收缩的测量长度之间的差异对应于以%计的收缩值。
根据表1的测量结果在指示的加热筒温度下获得。指定的加热筒温度是指通过温度传感器(铂测量电阻,Pt100元件)在加热筒内进行的测量。表1中给出的收缩方向表示测量的薄膜的收缩的方向(纵向方向md或横向方向cd)。
表1
表1清楚地显示了当薄膜随着加热筒温度增加而进入部分熔流状态时后收缩如何降低。结果也在图2中以图表的形式显示。该图表取决于加热筒温度一方面显示了薄膜的单位面积重量(图中上部;虚线),并且另一方面显示了md方向(点线)和cd方向(实线)上的热收缩(在80℃的水浴中)。在没有加热筒和冷却(压花)的情况下工作时表1中给出的收缩值未在图2中示出。表1中的值清楚地显示了在不进行根据本发明的方法的情况下收缩的程度。
示例2
根据示例1中所述的方法在135℃的加热筒温度下以16g/m2的单位面积重量生产薄膜。将该薄膜与现有技术的薄膜(对比薄膜)进行比较,所述现有技术的薄膜在不同水浴温度下的热收缩方面具有22g/m2的单位面积重量,如表2所示。收缩测量与示例1类似地进行。结果如表2所示。
表2
对于md收缩方向,表2的结果也在图3中以图形方式示出。因此,图3的图表示出了根据本发明的薄膜(虚线)和比较薄膜(比较;实线)根据给出的水浴温度在md方向上的收缩。
从表2可以看出,本发明的薄膜显示出比对比产品低得多的热收缩。因此,根据本发明的薄膜在例如在储藏室或船舶中可能出现的高温下提供了很大的优点。在较大热负荷的情况下,例如当应用热熔粘合剂系统时,它将显示出更高的阻力或低收缩特性或更低的所谓的烧穿效应。
Claims (26)
1.一种用于由包含热塑性聚合物材料的微孔初始膜带生产填充膜带的方法,所述填充膜带包含至少一种低熔点聚合物组分,高熔点聚合物组分和填料,其中该方法包括以下步骤:
将所述微孔初始膜带加热到部分熔融状态,在该状态中至少一种低熔点聚合物组分处于熔流状态并且至少一种高熔点聚合物组分不处于熔流状态,和
通过引导所述部分熔融的膜带穿过冷却的辊隙进行冷却。
2.根据权利要求1所述的方法,其特征在于,所述微孔初始膜带是单层的。
3.根据权利要求1所述的方法,其特征在于,所述微孔初始膜带是多层的。
4.根据权利要求3所述的方法,其特征在于,所述微孔初始膜带是共挤出的膜带。
5.根据权利要求1至3中的一项所述的方法,其特征在于,所述微孔初始膜带已被拉伸。
6.根据权利要求5所述的方法,其特征在于,所述初始膜带在其挤出后已被以1.2:1至4:1的拉伸比拉伸。
7.根据权利要求6所述的方法,其特征在于,所述初始膜带在其挤出后已被以1.5:1至3:1的拉伸比拉伸。
8.根据权利要求1-3中的一项所述的方法,其特征在于,基于100重量%的初始膜带,所述微孔初始膜带包含10至90重量%填料。
9.根据权利要求8所述的方法,其特征在于,基于100重量%的初始膜带,所述微孔初始膜带包含20至80重量%填料。
10.根据权利要求9所述的方法,其特征在于,基于100重量%的初始膜带,所述微孔初始膜带包含30至75重量%填料。
11.根据权利要求1-3中的一项所述的方法,其特征在于,所述微孔初始膜带是透气的。
12.根据权利要求1-3中的一项所述的方法,其特征在于,在根据ASTM E398在37.8℃和90%相对湿度下测量时,所述微孔初始膜带具有在24小时内500至5000g/m2的水蒸气渗透率。
13.根据权利要求1-3中的一项所述的方法,其特征在于,所述微孔初始膜带,基于100重量%的低熔点和高熔点聚合物组分,包括15至85重量%的低熔点聚合物组分和85至15重量%的高熔点聚合物组分。
14.根据权利要求1-3中的一项所述的方法,其特征在于,使用具有至少一种聚乙烯作为低熔点聚合物组分并具有至少一种聚丙烯作为高熔点聚合物组分的初始膜带。
15.根据权利要求1-3中的一项所述的方法,其特征在于,所述微孔初始膜带的加热通过加热筒进行,其中所述加热筒和所述膜带之间没有绒毛物。
16.根据权利要求1-3中的一项所述的方法,其特征在于,通过吹塑挤出、流延挤出或吹塑挤出和流延挤出以生产所述微孔初始膜带。
17.根据权利要求1-3中的一项所述的方法,其特征在于,将冷却的辊隙中的所述膜带冷却到至少一种低熔点聚合物组分的微晶熔点以下至少10℃。
18.根据权利要求17所述的方法,其特征在于,将冷却的辊隙中的所述膜带冷却到至少一种低熔点聚合物组分的微晶熔点以下10至30℃。
19.一种通过根据前述权利要求中的一项的方法获得的膜带。
20.根据权利要求19所述的膜带,其单位面积重量为1至30g/m2。
21.根据权利要求20所述的膜带,其单位面积重量为5至25g/m2。
22.根据权利要求21所述的膜带,其单位面积重量为7至20g/m2。
23.根据权利要求22所述的膜带,其单位面积重量为10至20g/m2。
24.根据权利要求19或20所述的膜带在卫生或医疗领域中的用途。
25.根据权利要求24所述的膜带在卫生或医疗领域中的用途,所述的膜带用于尿布中的后片,用于床垫或卫生巾。
26.根据权利要求19或20所述的膜带在建筑领域中的用途或用作汽车保护膜。
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PCT/EP2017/056839 WO2017162748A1 (de) | 2016-03-22 | 2017-03-22 | Verfahren zur herstellung einer gefüllten folienbahn |
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PL3560709T3 (pl) * | 2018-04-24 | 2021-02-08 | Rkw Se | Sposób wytwarzania zadrukowanych laminatów włókninowo-foliowych |
EP3647345A1 (en) | 2018-11-05 | 2020-05-06 | Windmöller & Hölscher KG | Breathable thermoplastic film with reduced shrinkage |
US11584111B2 (en) | 2018-11-05 | 2023-02-21 | Windmoeller & Hoelscher Kg | Breathable thermoplastic film with reduced shrinkage |
CN109318505B (zh) * | 2018-11-22 | 2023-06-02 | 张家港博来珂橡塑制品有限公司 | 手套的流延制膜与模压成型联动生产工艺及联动生产线 |
DE102019111445A1 (de) | 2019-05-03 | 2020-11-05 | Rkw Se | Atmungsaktive Folie |
EP4008551A1 (en) * | 2020-12-01 | 2022-06-08 | Flexopack S.A. | Thin film for waste packing cassettes |
CN114506063A (zh) * | 2022-01-26 | 2022-05-17 | 苏州金纬片板膜智能装备有限公司 | 一种回火整平装置 |
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CN108883567A (zh) | 2018-11-23 |
ES2770138T3 (es) | 2020-06-30 |
RU2018134113A3 (zh) | 2020-06-01 |
BR112018017003A2 (pt) | 2018-12-26 |
CN108778680B (zh) | 2021-07-20 |
PL3265290T3 (pl) | 2020-05-18 |
EP3265290B1 (de) | 2019-10-30 |
EP3265290A1 (de) | 2018-01-10 |
WO2017162746A1 (de) | 2017-09-28 |
RU2018134118A3 (zh) | 2020-05-29 |
BR112018067324A2 (pt) | 2019-01-22 |
ES2701915T3 (es) | 2019-02-26 |
RU2734515C2 (ru) | 2020-10-19 |
US20190076299A1 (en) | 2019-03-14 |
MX2018011499A (es) | 2019-06-17 |
EP3222406A1 (de) | 2017-09-27 |
RU2018134113A (ru) | 2020-04-22 |
CA3016126A1 (en) | 2017-09-28 |
MX2018011518A (es) | 2019-06-17 |
US20190084280A1 (en) | 2019-03-21 |
CA3016130A1 (en) | 2017-09-28 |
EP3222406B1 (de) | 2018-09-12 |
WO2017162748A1 (de) | 2017-09-28 |
PL3222406T3 (pl) | 2019-02-28 |
AR107943A1 (es) | 2018-06-28 |
RU2018134118A (ru) | 2020-04-22 |
CN108778680A (zh) | 2018-11-09 |
RU2734514C2 (ru) | 2020-10-19 |
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