CN116157475A - 氟聚合物组合物 - Google Patents
氟聚合物组合物 Download PDFInfo
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- CN116157475A CN116157475A CN202180052582.6A CN202180052582A CN116157475A CN 116157475 A CN116157475 A CN 116157475A CN 202180052582 A CN202180052582 A CN 202180052582A CN 116157475 A CN116157475 A CN 116157475A
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- UUAGAQFQZIEFAH-UHFFFAOYSA-N chlorotrifluoroethylene Chemical group FC(F)=C(F)Cl UUAGAQFQZIEFAH-UHFFFAOYSA-N 0.000 claims abstract description 35
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Abstract
本发明涉及一种热塑性氟聚合物组合物,其包含一种或多种聚合物A以及一种或多种聚合物B,该聚合物A包含衍生自乙烯的重复单元和衍生自选自氯三氟乙烯(CTFE)和四氟乙烯(TFE)的卤化单体的重复单元,该聚合物B包含衍生自乙烯的重复单元、衍生自选自CTFE和TFE的卤化单体的重复单元、以及衍生自六氟异丁烯(HFIB)和/或全氟丙基乙烯基醚(PPVE)的重复单元。所得组合物允许制造具有优异透明性和良好机械特性的膜,该膜可用作例如建筑膜。
Description
技术领域
本申请要求于2020年9月1日提交的欧洲专利申请号20193970.9的优先权,出于所有目的将该申请的全部内容通过援引并入本申请。
本发明涉及一种氟聚合物组合物,其包含一种或多种半结晶聚合物A和一种或多种氟化聚合物B,该半结晶聚合物A包含乙烯重复单元(E)和选自氯三氟乙烯(CTFE)、四氟乙烯(TFE)或其混合物的卤化重复单元;该氟化聚合物B包含乙烯重复单元(E),选自氯三氟乙烯(CTFE)、四氟乙烯(TFE)或其混合物的卤化重复单元以及衍生自六氟异丁烯(HFIB)和/或全氟丙基乙烯基醚(PPVE)的另外的重复单元。如果与现有技术的解决方案相比,本发明的组合物允许生产具有改善的机械特性和透明性平衡的膜。
背景技术
乙烯与氯三氟乙烯(ECTFE)、四氟乙烯(ETFE)或其混合物的共聚物在本领域是众所周知的,特别是用于制造膜和保护层。
这些材料提供了具有优异的耐气候性、耐污性和相对好的透明性水平的膜,这些特性通常被认为是保护膜的有价值的特性;当这些保护膜旨在用作建筑膜、农用膜、用于光伏电池的保护片、包装材料等时,尤其如此。
为了改善这些材料的光学特性,已经发现半结晶ECTFE提供了具有优异透明性的膜,然而发现如果与广泛用于建筑覆盖物工业的ETFE膜相比,由这些材料制成的膜具有稍微降低的机械阻力,但是另一方面,在透明性方面提供了相对差的性能。来自索尔维特种聚合物意大利公司(Solvay Specialty Polymers Italy)的WO 2012049242 A1描述了包含半结晶ECTFE或ETFE聚合物和分散的UV阻断剂化合物颗粒的组合物,由这些组合物可以获得透明膜。
因此,需要提供热塑性氟聚合物组合物,如果与现有技术的解决方案相比,这些组合物可以形成具有优异透明性并且同时具有优异机械特性的膜。
发明内容
本发明涉及一种热塑性氟聚合物组合物,其包含:
-基于该组合物的总重量按重量计51%-99%的一种或多种聚合物A,该聚合物A包含衍生自乙烯的重复单元和衍生自选自氯三氟乙烯(CTFE)和四氟乙烯(TFE)的卤化单体的重复单元,其中该乙烯重复单元与该卤化重复单元之间的摩尔比是从40:60至49:51,以及
-基于该组合物的总重量按重量计1%-49%的一种或多种聚合物B,该聚合物B包含衍生自乙烯的重复单元、衍生自选自氯三氟乙烯(CTFE)和四氟乙烯(TFE)的卤化单体的重复单元、以及基于该聚合物中重复单元的总摩尔按摩尔计1%-20%的衍生自六氟异丁烯(HFIB)和/或全氟丙基乙烯基醚(PPVE)的重复单元,并且其中所述乙烯重复单元与所述卤化重复单元之间的摩尔比是从40:60至60:40。
本发明还涉及:一种用于制造上述组合物的方法;该组合物用于制造膜的用途;由该组合物获得的膜;包含该膜的多层结构;以及这些膜或多层结构作为建筑膜,立面,用于光伏组件的保护膜,用于运输、工业和食品包装、或药物储存和包装的膜的用途。
具体实施方式
本发明涉及一种热塑性氟聚合物组合物,其将优异的透明性与良好的机械特性结合。本发明的组合物特别应用于制造可用于建筑的膜,例如用于屋顶或立面的透明覆盖物。本发明的组合物还可以成功地用于目前使用基于ETFE或ECTFE聚合物的组合物的任何应用中,例如用于光伏组件(作为保护膜),用于运输的膜,食品、农业和药品包装,家具、吊舱(pod)、玩具的设计和构造,以及通常用于需要具有高透明性和良好机械阻力结合耐候性和耐污性的热塑性材料的任何应用。
本领域内众所周知的是,50/50mol/mol ECTFE或ETFE共聚物显示出最大结晶度,即最大熔点和熔解热。
如引言中所提及,具有过量卤化重复单元的ETFE和ECTFE聚合物(典型地具有从40:60至49:51的乙烯重复单元与卤化重复单元之间的摩尔比)具有较低的结晶度,并且已知提供了具有优异透明性的膜。同时,这些材料具有稍微降低的机械阻力,这使得它们与50/50mol/mol ECTFE或ETFE共聚物相比,不太适合于那些其中机械阻力是非常重要的应用,例如像用于建筑覆盖物的膜。
然而,对于相同的应用,特别是在建筑、以及食品包装和其他方面,透明性是非常希望的益处,因此,持续需要提供来自ECTFE/ETFE聚合物的膜,这些膜在维持50/50mol/molECTFE或ETFE共聚物的机械阻力的同时,还具有改善的透明性。
本发明的组合物通过将较大量的一种或多种高度透明聚合物与较少量的第二增强聚合物结合来解决该技术问题,该高度透明聚合物是具有过量卤化单体的半结晶ECTFE或ETFE聚合物,该第二增强聚合物包含衍生自乙烯的重复单元、一种或多种来自氯三氟乙烯和四氟乙烯的重复单元以及一种或多种来自六氟异丁烯(HFIB)和/或全氟丙基乙烯基醚(PPVE)的重复单元。
已经发现,包含属于这两类的聚合物的组合物所提供的膜基本上与高度透明聚合物一样透明,但是具有大大改善的机械阻力。这种效果是出乎意料的,因为一般来说,不同聚合物的混合物,基本上是当考虑几乎完全透明和无雾度的材料时,由于组分的不完全混合,产生了雾度的增加和可见光透射率的降低。
更具体地,本发明涉及热塑性氟聚合物组合物,其包含按重量计51%-99%、优选51%-90%、更优选51%-80%、甚至更优选55%-70%(基于组合物的总重量)的一种或多种聚合物A和按重量计1%-49%、优选10%-49%、更优选20%-49%、最优选30%-45%(基于组合物的总重量)的一种或多种聚合物B。
聚合物A被定义为包含衍生自乙烯的重复单元和衍生自选自氯三氟乙烯(CTFE)和四氟乙烯(TFE)的卤化单体的重复单元的聚合物,其中乙烯重复单元与卤化重复单元之间的摩尔比是从40:60至49:51、优选从42:58至46:54。换句话说,其中卤化重复单元是以如上述比率范围所定义的摩尔过量存在。
优选地,聚合物A是半结晶聚合物。出于本发明的目的,半结晶聚合物被定义为具有相对低熔解热的聚合物。优选地聚合物A具有至多35J/g、优选至多30J/g、更优选至多25J/g的熔解热。
在熔解热的下限不是关键性的情况下,然而,应理解的是,聚合物A将通常具有至少1J/g、优选至少2J/g、更优选至少5J/g的熔解热。
根据ASTM D 3418,通过差示扫描热量法(DSC)以10℃/min的加热速率确定聚合物A的熔解热。
如以上所提及,50/50mol/mol ECTFE或ETFE共聚物示出最大的结晶度,因此,相对于该50/50摩尔比,对于至多35J/g的熔解热的要求可以通过增加或减小乙烯的量来实现。
然而,应理解的是,出于本发明的目的,聚合物A实际上是包含过量的如以上所提及的卤化重复单元的那些。
优选地,对于聚合物A,衍生自乙烯的重复单元和衍生自选自CTFE和TFE的卤化单体的重复单元的总和占构成聚合物A的重复单元总量的按摩尔计大于90%、优选大于95%、更优选大于97.5%、甚至更优选大于99%、并且最优选100%。
在非优选的实施例中,当聚合物A中存在除乙烯、CTFE和TFE之外的另外的共聚单体时,优选地这种另外的共聚单体是选自(甲基)丙烯酸单体的组的氢化的共聚单体。更优选地,该氢化的共聚单体选自丙烯酸羟烷基酯共聚单体(如丙烯酸羟乙基酯、丙烯酸羟丙基酯和丙烯酸(羟基)乙基己基酯)以及丙烯酸烷基酯共聚单体(如丙烯酸正丁基酯)的组。
在聚合物A之中,优选ECTFE共聚物,即乙烯和CTFE以及任选地如上详述的另外的共聚单体的共聚物。
适合在本发明组合物中作为聚合物A的ECTFE聚合物典型地具有不超过225℃、优选不超过215℃、更优选不超过210℃、甚至更优选不超过207℃的熔融温度。同时,适合在本发明组合物中作为聚合物A的ECTFE聚合物典型地具有至少160℃、优选至少180℃、更优选至少190℃、甚至更优选至少200℃的熔融温度。
根据ASTM D 3418,通过差示扫描量热法(DSC)以10℃/min的加热速率确定熔融温度。
已经发现作为聚合物A给出特别良好结果的聚合物是基本上由衍生自以下的重复单元组成的那些:
(a)按摩尔计从40%至49%、优选从42%至46%的乙烯(E);
(b)按摩尔计从51%至60%、优选从54%至58%的氯三氟乙烯(CTFE)。
导致重复单元不同于上文提及的那些的端链、缺陷或少量单体杂质仍可以包含在聚合物A中,而不影响该材料的特性。
按照ASTM 3275-81程序在275℃和2.16Kg下测量的聚合物A的熔体流动速率通常在从0.01至75g/10min、优选从0.1至50g/10min、更优选从0.5至30g/10min的范围内。
聚合物B被定义为包含衍生自乙烯的重复单元,衍生自选自氯三氟乙烯(CTFE)和四氟乙烯(TFE)的卤化单体的重复单元,以及按摩尔计1%-20%、优选2%-15%、更优选2%-10%、甚至更优选3%-7%(基于聚合物中重复单元的总摩尔)的衍生自六氟异丁烯(HFIB)和/或全氟丙基乙烯基醚(PPVE)的另外的重复单元的聚合物。在最优选的实施例中,所述另外的重复单元全部衍生自HFIB。所述乙烯重复单元与所述卤化重复单元之间的摩尔比是从40:60至60:40、优选从45:55至55:45、最优选从49:51至51:49。
优选地,对于聚合物B,衍生自乙烯、CTFE、TFE、HFIB和PPVE的重复单元的总和占构成聚合物B的重复单元总量的按摩尔计大于90%、优选大于95%、更优选大于97.5%、甚至更优选大于99%、并且最优选100%。
在非优选的情况中,其中聚合物B中存在除乙烯、CTFE、TFE、HFIB和PPVE之外的另外的共聚单体,优选地这种另外的共聚单体是选自(甲基)丙烯酸单体的组的氢化的共聚单体。更优选地,该氢化的共聚单体选自丙烯酸羟烷基酯共聚单体(如丙烯酸羟乙基酯、丙烯酸羟丙基酯和丙烯酸(羟基)乙基己基酯)以及丙烯酸烷基酯共聚单体(如丙烯酸正丁基酯)的组。
导致重复单元不同于上文提及的那些的端链、缺陷或少量单体杂质仍可以包含在聚合物B中,而不影响该材料的特性。
虽然本发明的组合物优选地基本上仅由聚合物A和聚合物B组成,但是它们还可以含有另外的常规成分和添加剂,如颜料、染料、UV过滤剂、稳定剂、增塑剂、防腐剂、抗氧化剂等。通常,优选的是基于组合物的总重量,所有这些不同于聚合物A或B的另外的成分的组合不超过按重量计20%、优选10%、更优选5%、甚至更优选1%。
根据本发明的组合物特别适合于制造建筑膜,但还可以用于ECTFE和ETFE膜(如保护膜,其包括用于保护光伏组件的膜(特别是用于PV电池的前板或背板)、农用膜、包装膜等)的所有应用中。
本发明的另一方面涉及一种用于制造如上所述的热塑性氟聚合物组合物的方法,所述方法包括将如上详述的聚合物A和B混合。这种混合可以用本领域已知的用于共混热塑性聚合物用于干共混和/或熔融配混的任何技术来获得。例如,可以将聚合物A和B的粉末或粒料预混合,并且然后熔融配混到挤出机中,将该挤出机在比最高熔点组分的熔融温度高约30℃的温度下加热。可替代地,可以将聚合物单独熔融,并且然后在混合器或挤出机中熔融配混。最后,一旦以熔融状态形成组合物,可以将组合物挤出并造粒用于进一步加工。
以连续方式熔融配混本发明的热塑性氟聚合物组合物的合适装置的实例是螺杆挤出机。在这种情况下,可以将聚合物A和B以及任选地其他成分进料到挤出机中,并且挤出本发明的热塑性氟聚合物组合物。
此操作方法可以应用于为了制造最终产物(例如像膜、空心体、管、层压件、压延制品),或者为了具有可获得的颗粒,这些颗粒以合适的比例以粒料的形式含有所希望的组合物,这促进随后转化成成品。从后者的目的考虑,可以将本发明的热塑性氟聚合物组合物有利地挤出成条并且可以将这些条被切碎成粒料。
优选地,将本发明的组合物在单螺杆或双螺杆挤出机中熔融配混。很好地适应本发明方法的适合的挤出机的实例是从莱斯特瑞兹公司(Leistritz)、马里斯美国公司(Maris America Corp.)、维尔纳和弗莱德尔公司(Werner and Pfleiderer)以及从法雷尔公司(Farrel)可获得的那些。
本发明的还另一个目的是本发明的热塑性氟聚合物组合物用于制造膜的用途。
用于制造膜的技术是本领域众所周知的。本发明的组合物可以优选地通过流延挤出或热吹塑挤出技术,任选地使用单-或双-轴取向,以膜的形式进行加工。
特别适合制造本发明的组合物的膜的技术涉及将熔融组合物通过具有细长形状的模具挤出以获得挤出条带并且将所述挤出条带流延/压延以获得膜。
条带可以通过穿过适当的辊压延成膜,这些辊可以维持在适当的温度下,并且其速度可以调节以实现所要求的厚度。
从本发明的组合物获得的膜优选地是透明膜,即,当根据ASTM E1003使用ByKHaze Guard plus设备在水中测量时,在具有约250μm厚度的膜上确定时,膜具有大于80%、优选大于90%、甚至更优选大于95%的总透射率。
从本发明的组合物获得的膜优选地为使得限制穿过它们的光的透射、散射(负责所观察的图像的对比的减小)。换句话说,当根据ASTM E1003使用ByK Haze Guard plus设备在水中测量时,在具有约250μm厚度的膜上确定时,由本发明的组合物获得的膜具有小于10、优选小于5%、甚至更优选小于3%的雾度值。
如此获得的膜是本发明的另一个目的。
本发明的膜可以有利地以多层结构组装。包含本发明的膜的多层结构仍然是本发明的目的。
因此,由如上详述的本发明的组合物获得的膜和/或如上所指定的包括该膜的多层组件作为建筑膜(包括立面、吊舱、气球覆盖物等),用于光伏组件的保护膜,用于运输、工业和食品包装、药物储存和包装的膜的用途仍在本发明的框架内,并且通常在使用基于ETFE或ECTFE的膜并且其中需要高透明性的任何情况下。
如果通过援引方式并入本申请的任何专利、专利申请以及公开物的披露内容与本申请的描述相冲突到了可能导致术语不清楚的程度,则本说明应该优先。
现在将参考以下实例更详细地说明本发明,这些实例的目的仅仅是说明性的。
原料
聚合物
ECTFE-B:是来自索尔维公司(Solvay)的47/47/6摩尔%的E/CTFE/HFIB三元共聚物,具有224℃的熔点,和11g/10min(275℃/2.16kg)的MFI。
ETFE是ETFE聚合物(来自3M公司(3MTM),以DyneonTM氟塑料ET 6235Z销售),其是典型的用于建筑覆盖物的ETFE等级。
本发明的组合物的通用制造程序
聚合物以粉末的形式提供。在根据本发明的组合物的情况下,将组分聚合物ECTFE-A和ECTFE-B预混合。在比最高熔点组分的熔点高30℃的温度下将粉末(在样品由多于一种组分形成的情况下为共混粉末)熔融,并在单螺杆挤出机中挤出,从而获得相同组成的粒料。
为了制造薄膜,在配备有常规成膜头的挤出机中加工粒料以便获得约250μm的膜厚度。
膜表征
将如上详述获得的250μm厚的膜进行光学测试。
根据ASTM E1003使用ByK Haze Guard plus设备在水中测量总透射率(TT)和雾度。
黄色指数(YI)是根据ASTM E313使用ByK彩色视图色度计(使用D65日光光源和在10°处的观察者)测量。
机械特性
根据ASTM D3307,在25℃、46℃和57℃下,在5个膜样品的纵向(MD)和横向(TD)上对250μm厚的膜进行屈服应力测量。为了测量,已使用了具有1kN电池和平夹具的Instron5965仪器。牵引速度是50mm/min。夹持距离是22mm。
表1-机械和光学特性
表中呈现的数据示出,用本发明的组合物制成的膜相对于ECTFE-A具有改善的机械特性,并且具有与ETFE膜可比的机械特性,ETFE膜是建筑膜中良好机械特性的工业标准。此外,与ETFE膜相比,根据本发明的膜具有改善的总透射率和降低的雾度,并且具有与仅由ECTFE-A制成的膜(其是高透射率膜的工业标准)基本上相同的总透射率和雾度。由ECTFE B制成的膜不仅具有非常好的机械特性,而且具有差的透明性和雾度。总的来说,相对于已知材料,根据本发明的组合物提供了在机械特性与光学特性(透射率和雾度)之间具有改善的平衡的膜。
Claims (15)
1.一种热塑性氟聚合物组合物,其包含:
-基于该组合物的总重量按重量计51%-99%的一种或多种聚合物A,所述聚合物A包含衍生自乙烯的重复单元和衍生自选自氯三氟乙烯(CTFE)和四氟乙烯(TFE)的卤化单体的重复单元,其中所述乙烯重复单元与所述卤化重复单元之间的摩尔比是从40:60至49:51,
以及
-基于该组合物的总重量按重量计1%-49%的一种或多种聚合物B,所述聚合物B包含衍生自乙烯的重复单元、衍生自选自氯三氟乙烯(CTFE)和四氟乙烯(TFE)的卤化单体的重复单元、以及基于该聚合物中重复单元的总摩尔按摩尔计1%-20%的衍生自六氟异丁烯(HFIB)和/或全氟丙基乙烯基醚(PPVE)的重复单元,并且其中所述乙烯重复单元与所述卤化重复单元之间的摩尔比是从40:60至60:40。
2.根据权利要求1所述的热塑性氟聚合物组合物,其中,所述聚合物A具有至多35J/g、优选至多30J/g、更优选至多25J/g的熔解热。
3.根据任一前述权利要求所述的热塑性氟聚合物组合物,其中,在所述聚合物A中,该乙烯重复单元与卤化重复单元之间的摩尔比是从42:58至46:54。
4.根据任一前述权利要求所述的热塑性氟聚合物组合物,其包含:按重量计51%-90%、优选按重量计51%-80%、更优选按重量计55%-70%的所述聚合物A和按重量计10%-49%、优选按重量计20%-49%、更优选按重量计30%-45%的所述聚合物B。
5.根据任一前述权利要求所述的热塑性氟聚合物组合物,其中,所述聚合物B包含按摩尔计2%-15%、优选按摩尔计2%-10%、更优选按摩尔计3%-7%的量的衍生自HFIB和/或PPVE的重复单元。
6.根据任一前述权利要求所述的热塑性氟聚合物组合物,其中,所述聚合物B包含按摩尔计2%-15%、优选按摩尔计2%-10%、更优选按摩尔计3%-7%的量的衍生自HFIB的重复单元。
7.根据任一前述权利要求所述的热塑性氟聚合物组合物,其中,
-在所述聚合物A中,该衍生自乙烯的重复单元和该衍生自选自CTFE和TFE的卤化单体的重复单元的总量占构成该聚合物A的重复单元总量的按摩尔计大于90%、优选按摩尔计大于95%、更优选按摩尔计大于97.5%、甚至更优选按摩尔计大于99%、并且最优选100%,并且
-在所述聚合物B中,该衍生自乙烯的重复单元、该衍生自选自CTFE和TFE的卤化单体的重复单元、以及该衍生自HFIB和/或PPVE的重复单元的总量占构成该聚合物B的重复单元总量的按摩尔计大于90%、优选按摩尔计大于95%、更优选按摩尔计大于97.5%、甚至更优选按摩尔计大于99%、并且最优选100%。
8.根据任一前述权利要求所述的热塑性氟聚合物组合物,其中,该聚合物A是ECTFE聚合物。
9.根据权利要求8所述的热塑性氟聚合物组合物,其中,聚合物A基本上由以下组成:
(a)按摩尔计从40%至49%、优选按摩尔计从42%至46%的衍生自乙烯的重复单元;
(b)按摩尔计从51%至60%、优选按摩尔计从54%至58%的衍生自氯三氟乙烯(CTFE)的重复单元。
10.根据权利要求8-9所述的热塑性氟聚合物组合物,其中,该聚合物A具有不超过225℃、优选不超过215℃、更优选不超过210℃、甚至更优选不超过207℃,并且至少160℃、优选至少180℃、更优选至少190℃、甚至更优选至少200℃的熔融温度。
11.一种用于制造根据任一前述权利要求所述的热塑性氟聚合物组合物的方法,所述方法包括:将所述聚合物A和所述聚合物B混合。
12.根据权利要求1-10所述的热塑性氟聚合物组合物用于制造膜的用途。
13.一种膜,其由根据权利要求1-10所述的热塑性氟聚合物组合物获得。
14.一种多层结构,其包含根据权利要求13所述的膜。
15.根据权利要求13所述的膜或根据权利要求14所述的多层结构作为建筑膜,立面,用于光伏组件的保护膜,用于运输、工业和食品包装、或药物储存和包装的膜的用途。
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- 2021-08-23 US US18/043,712 patent/US20230272135A1/en active Pending
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- 2021-08-23 JP JP2023513562A patent/JP2023540700A/ja active Pending
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JP2023540700A (ja) | 2023-09-26 |
US20230272135A1 (en) | 2023-08-31 |
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