CN1688428A - 含有纤维增强的热塑性聚合物组合物的制品 - Google Patents

含有纤维增强的热塑性聚合物组合物的制品 Download PDF

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Publication number
CN1688428A
CN1688428A CNA038243113A CN03824311A CN1688428A CN 1688428 A CN1688428 A CN 1688428A CN A038243113 A CNA038243113 A CN A038243113A CN 03824311 A CN03824311 A CN 03824311A CN 1688428 A CN1688428 A CN 1688428A
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Prior art keywords
thermoplastic polymer
polymer composition
fiber
fibre
extruder
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CNA038243113A
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English (en)
Inventor
T·R·萨顿
J·G·查理森
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Dow Global Technologies LLC
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Dow Global Technologies LLC
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Publication of CN1688428A publication Critical patent/CN1688428A/zh
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Abstract

本发明涉及一种制造纤维增强的热塑性聚合物组合物并由其形成加工制品的方法。将热塑性聚合物、含有弹性体的母炼胶和增强纤维制品进行化合，压出并立即成型为加工制品。通过压模、真空成型、热成型、注射成型、吹塑、型材挤塑或其混合制成加工制品。

Description

含有纤维增强的热塑性聚合物组合物的制品
本发明涉及一种制造含有弹性体的纤维增强热塑性聚合物组合物和由其制成加工制品的方法。
含有热塑性聚合物，特别是丙稀聚合物的模制品在如下多种应用领域内具有广泛的用途，例如在汽车、家用器具、电子外壳、家具、地板覆盖物和墙面覆盖物中的加工制品。
对这些制品物理性质的要求不等而且取决于其用途。本领域公知的是，热塑性聚合物可以含有如填料的非聚合材料来改变其某些性质。因此，可以使用各种矿物或无机填料来改变热塑性聚合物的一种或多种机械性能，例如线性热膨胀系数；模量；冲击强度，尤其是低温冲击强度；抗张强度；弯曲强度和回弹力。
形成增强热塑性材料(例如玻璃纤维增强的聚丙稀)片材的方法是公知的。例如，美国专利No.4,439,387揭示了一种通过将流体热塑性树脂从伸长模头中压出的同时向该模头中加入大量连续纤维增强束来制造复合增强结构的方法。然而，制成的复合材料显示出各向异性的机械性能。通过加入无规定向纤维和/或补充填料可得到改进的性能。
通常，制造由增强热塑性材料制成的加工制品的铸工从制造商处购买材料，所购买材料是如片材或垫块的所需预成型坯。可以由玻璃纤维制成所述垫块并且将其层压在如聚丙烯的热塑性树脂中。铸工再次加热所述预成型坯，然后将其插入铸模机中以压模所需零件。但是，这种方法具有许多缺点，包括不能在需要时快速改变材料组成和预成型坯的形状。
在美国专利No.5,401,154中说明了一种在连续加工中化合增强热塑性材料(但仅限于压模制品)的方法。然而，该方法缺乏成本效率，因为其以低生产率运行并且需要可互换螺杆构造以便对不同的材料性质进行选择性控制。
已知的是，为了克服不足的冲击强度，已经将如乙烯-丙稀共聚型橡胶、乙烯-丙稀-二烯共聚型橡胶或乙烯-丁烯共聚型橡胶的橡胶态弹性材料与丙稀聚合物混合。例如，参看美国专利No.5,391,618，其公开了含乙烯α-烯烃共聚物的低结晶聚丙烯聚合物组合物；美国专利No.5,576,374，其公开了含基本线型乙烯聚合物的聚丙烯聚合物组合物；美国专利No.5,639,829，其公开了含乙烯和1-丁烯无规共聚物的丙稀聚合物组合物。然而，在冲击性能提高的同时，由这些丙稀聚合物组合物制成的加工制品没有表现出良好的刚度与韧性平衡。
此外，对于特定的用途，例如紫外线稳定性、热稳定性、颜色、热塑性聚合物和纤维的相容性、可燃性和热膨胀系数的其它热塑性聚合物性能可能不足。可能需要一种或多种额外添加剂，而导致需要额外且昂贵制造工艺使用设备的复杂且昂贵的储存和处理操作。
考虑到传统热塑性聚合物组合物以及由其模制加工制品方法的缺陷，极其需要提供一种热塑性聚合物组合物和一种节省成本的由其模制加工制品的方法，所述制品具有良好的刚度与韧性平衡。
本发明就是这样所需的热塑性聚合物组合物及方法。本发明提供一种节省成本的制造纤维增强热塑性聚合物组合物和由其制成的加工制品的方法，该制品具有良好的刚度与韧性平衡。
在一个具体实施方式中，本发明涉及制造纤维增强热塑性聚合物组合物的方法，包括下列步骤：在压出机中加入热塑性聚合物和含弹性体的母炼胶，在压出机中塑炼热塑性聚合物和母炼胶以形成熔融的热塑性聚合物组合物，在熔融的热塑性聚合物组合物中加入连续的增强纤维材料，将熔融的纤维增强热塑性聚合物组合物压出并形成包含纤维增强热塑性聚合物组合物的加工制品。
在优选实施方式中，本发明是如上所述制造纤维增强热塑性聚合物组合物和由其制成的加工制品的方法，进一步包括下列步骤：将熔融的纤维增强热塑性聚合物组合物从一个模头中压出以形成具有所需横截面形状的加热纤维增强热塑性聚合物组合物的连续挤压件，将该加热纤维增强热塑性聚合物组合物的连续挤压件输送到切断机上，将连续挤压件切成多个预成型坯，并将这些预成型坯运离所述切断机并输送到真空成型塑模或热成型塑模，优选压塑模中。
本发明的另一个优选实施方式是如上所述制造纤维增强热塑性聚合物组合物和加工制品的方法，进一步包括下列步骤：将熔融纤维增强热塑性聚合物组合物输送到聚积器中，聚积所需量的加热纤维增强热塑性聚合物组合物以形成颗粒(shot)并将该颗粒注入注模中。
本发明的另一个优选实施方式是如上所述制造纤维增强热塑性聚合物组合物和加工制品的方法，进一步包括下列步骤：将熔融的纤维增强热塑性聚合物从一个模头中压出以形成型坯，将所述型坯置于吹塑模中，封闭所述塑模并将气体注入所述塑模中。
本发明的另一个优选实施方式是如上所述制造纤维增强热塑性聚合物组合物和由其制成的加工制品的方法，进一步包括下列步骤：将熔融的纤维增强热塑性聚合物组合物从一个具有所需形状的型材挤塑模头中压出。
在本发明的又一个具体实施方式中，优选的增强纤维是大量的连续玻璃纤维，优选的弹性体是含乙烯和1-辛烯的基本线型的乙烯聚合物。
本发明的纤维增强热塑性聚合物组合物在制备具有大表面积的加工制品中尤为有用，该大表面积需要在刚度与冲击强度性能、延性、抗张强度、表面美观性和耐气候性之间具有良好平衡。这些性能对用于车辆应用领域的加工制品而言是特别理想的。车辆包括，但不限于，机动车(轿车和卡车)、公共汽车、火车、地铁列车、摩托雪橇、私人船只、所有的地面运动车辆、草坪和园艺拖拉机、农场设备、飞机、船和高尔夫球车。车辆应用包括，但不限于，仪表盘、门板、前端托架、车身底板、车身底板保护、台阶垫(step pad)、后挡板、整流罩、挡泥板、面板、车体外壳和底座衬垫(bed liners)。其它应用包括电气或电子设备器件外壳和外罩；以及其它家庭和个人用品，例如机箱；草坪和庭园用具；建筑物地板和墙面覆盖物。此外，本发明的方法通过减少加入压出机中的原材料进料数量、消除额外的进料器、降低添加组分时的计量误差、在压力下具有挠曲性以使冲击性能适应特定的应用需要、降低库存空间、消除在形成加工制品之前额外的重新加热增强热塑性预成型坯的步骤、或综合上述因素，来提高成本竞争力。
图1是图解本发明方法步骤的流程图。
图2是图解提供压模成型、热成型或真空成型加工制品的本发明方法步骤的流程图。
图3是图解提供注射成型加工制品的本发明方法步骤的流程图。
图4是图解提供吹塑加工制品的本发明方法步骤的流程图。
图5是图解提供挤塑型材加工制品的本发明方法步骤的流程图。
图6是按照本发明制造和形成的纤维增强热塑性聚合物组合物加工制品所用装置的侧视示意图；和
图7是图6中沿线段A---A截取并包括额外纤维源的模头和罩壳的截面示意图。
图1表示本发明方法的步骤。本发明是形成含纤维增强热塑性聚合物组合物的加工制品的方法。该方法包括压模、热成型或真空成型步骤(图2)、注射成型步骤(图3)、吹塑步骤(图4)、型材挤塑步骤(图5)中的至少一种或其结合。当使用玻璃作纤维增强材料时，该方法有时指长玻璃纤维(LGF)直接法，例如LGF直接压模法或LGF直接注射成型法。
适合实施本发明方法的装置是本领域已知的。例如，参看USP5,401,154；5,798,128；6,444,153和6,238,733。
例如，图6中显示了装置7，其用于连续化合纤维增强热塑性聚合物组合物、将该材料从具有特定形状(典型但不一定是矩形)的模头中压出、形成具有特定形状的连续压出物。例如，如果该模头制成矩形压出物，那么连续压出物可以是带状的。从该带状物上切割预成型坯并立即由仍然热的预成型坯制成加工制品。压出物的形状、宽度和厚度不限，但其是通过包括压出机类型、尺寸、容量、压出机模头形状在内的几个因素来进行测定的。根据由其形成的制品，将从连续压出物上切下的预成型坯切成任何所需的长度，切得的预成型坯有多种名称，通常被称作片材、原材(logs)或装料(charges)来命名某些预成型坯。典型地，压出物和/或由其切割成的预成型坯可以是6英寸(15.24厘米)至60英寸(152.40厘米)宽，优选12英寸(30.48厘米)至48英寸(121.92厘米)宽，更优选12英寸(30.48厘米)至36英寸(91.44厘米)宽。典型地，压出物和/或由其切割成的预成型坯是0.125英寸(0.32厘米)至12英寸(30.48厘米)厚、优选0.125英寸(0.32厘米)至8英寸(20.32厘米)厚，更优选0.5英寸(1.27厘米)至6英寸(1 5.24厘米)厚，更优选1英寸(2.54厘米)至6英寸(15.24厘米)厚，最优选2英寸(5.08厘米)至5英寸(12.70厘米)厚。
装置7包括一个多段机筒，一个复合压出机8(包括一个单螺杆，优选一个双螺杆)，其机筒区段一9位于带有一个原材料入口10的该压出机入口端。热塑性聚合物源11向入口10供应热塑性聚合物12，例如聚丙烯。母炼胶源13向入口10供应含弹性体(例如基本线型的乙烯聚合物)和其它添加剂(例如色料、稳定剂和/或偶联剂)的母炼胶14。如果有任何原材料是吸湿的，可能需要一个干燥器以便在这些材料进入入口10之前去除湿气。压出机8包括数个可以封闭也可以在顶部或侧面含有进料口的中间区段。例如，机筒区段六17有一个与纤维源19邻接的第一顶部入口18，以便将许多第一增强纤维20(例如连续玻璃纤维)加入到机筒中的熔融热塑性聚合物组合物中。压出机8还可以任选地包括一个或多个额外的中间入口区段，例如含有一个第二顶部入口22的机筒区段八21，该入口与纤维源23邻接以便将许多第二增强纤维24加入到熔融热塑性聚合物组合物中。当需要使用具有不同特性(例如材料、直径或长度)的纤维时，可能需要第二纤维源。如下所释，纤维20和24优选以具有任何所需长度的无规定向增强纤维的形式与熔融的热塑性聚合物组合物混合。机筒区段九25位于压出机8的出口端以便排放出添加有增强纤维的熔融热塑性聚合物组合物。由此，可以选择构成压出机8的区段的数量和类型以使其适合正处理的热塑性材料和纤维。此外，压出机的出料端可以包括一个材料聚积器。例如，如果压出机螺杆没有延伸到机筒区段九25，该区段的内部空腔S提供了一个用来聚积一定量熔融纤维增强热塑性聚合物组合物的空间。可以在区段21和25之间插入追加的机筒区段以增加聚积器空腔S的容量。
机筒区段九25具有一个与模头26的入口相连的出口(未标示)，用以将含增强纤维的熔融热塑性聚合物组合物加入模头以挤压成所需形状。从模头26的出口挤出纤维增强热塑性聚合物组合物的具有预定截面形状的连续挤压件，例如带状物27。如图6所示，带状物27通常具有预定厚度和宽度的矩形截面，不过根据用途，带状物27的截面可以具有不同厚度和/或宽度。将该带状物27支托在以预定速度运行的带式运输机28上。该运输机28将带状物27输送到切刀设备29处，该设备以运行方向的横向横切该带状物以形成热塑性增强聚合物组合物的单个预成型坯，例如片材30。将片材30支托在第一片材运输机31上，该运输机的传动速度与带式运输机28相同。第一片材运输机31将从带状物27上切下的片材(例如在先的片材32)输送到第二片材运输机33上，其以较快的传动速度分离片材30和32。任何其它将片材从切刀处输送到塑模中的方法(例如手动或通过机器人技术或类似方法或包括使用运输机和/或手动和/或机器人技术在内的任何组合方式)都在本发明的范围内。
任选地，模头26、运输机28和31、一部分切刀29和至少部分至全部的运输机33都包在使这些片材保持在模制温度的温度控制罩壳34中。在运输机33上，片材32之前的片材35如图所示进入塑模36中。该塑模36是一个支承在底座38之上的且由压机37驱动的压塑型塑模。或者，塑模36是真空成型塑模或热成型塑模，其中压机37和底座38发挥其所需功能以使加工制品真空成型或热成型。根据成型制品，对每个模制周期将一个或多个预成型坯放在该模塑中。例如，成型的制品可能需要在每个模制周期的塑模中放入一至六个预成型坯，优选一至四个预成型坯，或更优选一至三个预成型坯。如果使用多个预成型坯，其都可以具有相同尺寸和形状，都具有不同尺寸或形状或综合这两种情况。
任选地，将由带式运输机28支托的带状物27输送到切刀设备29处。当运输机上达到预定量的带状物后，将压出机关闭，运输机停止并将带状物切成片材30，重新启动压出机和运输机，并将片材30输送到塑模中并重复该过程。
典型地，由许多可以聚成线的单丝纤维和许多可以聚成束的这些线形成纤维束以便运送给买家。由于单丝纤维和纤维线可以互相之间缠绕、扭曲并盘绕，所以必须通过任何合适的方式将纤维束展开以使纤维遍布于熔融热塑性聚合物组合物中。或者，纤维源19可以供应短切纤维，将其以与热塑性聚合物12类似的方式加入到入口18中。纤维源23和任何向压出机8中进料的追加纤维源可以具有类似的构造。
图7表示图6所示的模头26和罩壳34的截面图。模头26使熔融热塑性聚合物组合物成型为具有预定厚度和预定宽度的带状物27。如果需要在熔融的热塑性聚合物组合物中加入单向增强纤维，由于单向纤维是连续的而且是在带状物27的纵轴方向上延伸的，所以纤维源优选位于压出机8的下游。如图7所示，纤维源59位于模头26上方。许多单丝增强纤维60从纤维源59进入模头26顶部的入口61。纤维源59可以是任何适合于加入许多越过带状物27的宽度展开的单丝纤维的设备，例如横转向带状物27运行路径的纤维源19。
优选地，模头26是相对较长的低压模头，其将树脂吸到离开压出机的熔融材料的表面。该富含树脂的表面产生A等网纹表面。如上所述，模头制成具有任何所需截面形状的连续挤压件。
该装置可以包括一个或多个压出机，参看USP 6,238,733。例如，当使用两个压出机时，第一压出机将热塑性聚合物组分和含弹性体的母炼胶塑炼制成熔融的热塑性聚合物组合物。将该熔融的热塑性聚合物组合物加入到第二压出机中，在其中加入纤维增强材料，优选连续纤维材料并使其包覆上熔融的热塑性聚合物组合物。在第二压出机中，当使用连续纤维材料时，包覆后的连续增强纤维仍然保持连续，或优选地，将其切成所需范围的长度。通过第二压出机将熔融的纤维增强热塑性聚合物组合物通过模头压出，形成具有所需形状(例如带状)的压出物。将该带状物输送到切刀处，切成具有所需尺寸的预成型坯(例如片材)。通过传送装置将片材输送到压塑模、真空成型塑模或热成型塑模中。将该材料压模、真空成型或热成型为加工制品，冷却并脱模。或者，可以使用第三压出机。将第二热塑性聚合材料(例如，与加入第一压出机中的第一热塑性聚合物相同或不同的再循环热塑性聚合物)加入到第三压出机中并在此塑炼，以形成第二熔融热塑性聚合物组合物，将其与来自第一压出机的第一熔融热塑性聚合物组合物和连续纤维增强材料一起加入第二压出机中。随后如上所述进行所述过程。
当使用一个以上压出机时，其中一个压出机可以是注模机。在LGF直接注射成型法中，注模机可以含有一个或多个聚积器。例如，在半连续法中，压出机可以将压出物输送到聚积器中，当聚积器充满时，通过切断装置暂时停止压出，并且通常通过柱塞将聚积的压出物(有时称作注射料)注射到注模的模腔中。或者，在连续法中，注模机可以含有两个或多个聚积器，其中将每个聚积器交替填满并注入注模的模腔中，优选地，在将第二聚积器内的注射料注入注模模腔的同时填充第一聚积器，然后在填充第二聚积器的同时将刚刚填入第一聚积器的注射料注入注模的模腔中，并重复这一过程。每个聚积器的塑模可以相同或不同。可以使用多个注模，例如，当使用两个聚积器时，每个聚积器可以有自己的注模，形成相同或不同的加工制品。
或者，可以使用本发明的方法形成吹塑加工制品。将熔融的纤维增强热塑性聚合物组合物通过模头压出，形成任何所需形状和大小的管状型坯，典型地，模头形成椭圆形或圆形型坯。接下来，将型坯置于开口成形的吹塑模中，将该塑模封闭，并将一种气体，优选空气、氮气或二氧化碳吹入该塑模以按照该塑模的轮廓塑造型坯，产生中空的模制加工制品。
此外，本发明的方法可用于形成连续型材挤出件。将熔融的纤维增强热塑性聚合物组合物从具有所需形状的型材挤塑模头中挤出以形成挤塑型材。
本发明的方法可用于处理新料或用于处理含再循环热塑性聚合物的混合物、再循环纤维增强热塑性聚合物组合物、或其混合物。在EP1008434中公开了具有将再循环材料加入纤维增强热塑性聚合物组合物中能力的两个压出机装置的例子。
本发明的纤维增强热塑性聚合物组合物所含的纤维包括0至100％的无规纤维和100至0％的单向纤维，或者50至100％的无规纤维和0至50％的单向纤维。按照本发明，化合热塑性聚合物组合物的方法对于无规纤维和单向纤维是相同的。如上所述，差异在于是在下游设备中将单向纤维与已加入压出机的无规纤维混合。
本发明的方法将增强纤维、热塑性聚合物和含弹性体的母炼胶以某种方式结合，使得制成的加工成品表现出良好的表面光洁度和良好的强度、刚度、韧性、延性和冲击强度性能的平衡。
本发明的优选实施方式采用同步旋转双螺杆压出机，优选通风的双螺杆压出机。双螺杆压出机用来将长丝增强纤维加入到热塑性树脂中。根据螺杆设计，可以使用长度从1/32英寸(0.08厘米)至连续的无规纤维。在热塑性聚合物和母炼胶的进料口下游的某个位置将增强纤维加入双螺杆压出机中，这样在与增强纤维接触之前将热塑性聚合物和母炼胶化合，换言之，进行机械加工、掺合和加热。优选地，出自双螺杆压出机的压出物含有热塑性聚合物组合物的均质熔融体，纤维在其中无规分散。然后将熔融的纤维增强热塑性聚合物组合物加入如模头的二级设备中以测定制成压出物和/或预成型坯的大小、重量和形状。可以在模头中加入单向增强纤维。
当然，纤维增强材料的物理性质还取决于所选的热塑性聚合物和弹性体以及纤维含量。通常，增强纤维的用量大于或等于纤维增强热塑性聚合物组合物重量的5重量份，优选大于或等于10重量份，更优选大于或等于15重量份，甚至更优选大于或等于20重量份，最优选大于或等于25重量份。典型地，增强纤维的用量小于或等于纤维增强热塑性聚合物组合物80重量份，优选小于或等于60重量份，更优选小于或等于45重量份，最优选小于或等于35重量份。使用本发明的方法，可以即时改变增强纤维的百分比以获得所制成型加工制品所需的物理性质。
压出之前的优选玻璃纤维增强材料是以连续玻璃粗纱的形式存在的。粗纱包括许多纤维。典型粗纱约为1,000M长，以纤度单位(tex)值表示其重量。优选地，玻璃粗纱的纤度单位值大于或等于500，更优选大于或等于1,000，最优选大于或等于2,000。优选地，玻璃粗纱的纤度单位值小于或等于10,000，更优选小于或等于5,000，最优选小于或等于3,000。优选的玻璃纤维的直径大于或等于3微米，更优选大于或等于5微米，最优选大于或等于10微米。优选的玻璃纤维的直径小于或等于40微米，更优选小于或等于30微米，最优选小于或等于20微米。以本发明的方法处理后，加工制品中的玻璃纤维的长度大于或等于0.01英寸(0.03厘米)，更优选大于或等于0.1英寸(0.25厘米)，最优选大于或等于1英寸(2.54厘米)。在本发明的方法之后，加工制品中的玻璃纤维的长度小于或等于加工制品的长度，优选小于或等于10英寸(25.40厘米)，更优选小于或等于6英寸(15.24厘米)，再优选小于或等于4英寸(10.16厘米)，最优选小于或等于2英寸(5.08厘米)。
尽管已经论述了使用连续玻璃纤维和聚丙稀树脂的例子，但不连续玻璃纤维也适用于本发明。其它连续和不连续纤维，例如碳石墨纤维、聚酯纤维(例如产自DuPont的KEVLARTM聚芳酰胺纤维)、金属纤维和镀金属纤维，以及天然纤维(例如大麻纤维)都是适合的。提高纤维和热塑性聚合物之间粘合力的涂料、胶粘剂和/或偶联剂是公知的。合适的涂料、胶粘剂和/或偶联剂的用量可以是用于本发明方法中所选的热塑性聚合物和增强纤维的典型用量。
热塑性聚合物是指任何可以通过加热和冷却反复熔融和固化的纤维。本发明的纤维增强热塑性聚合物组合物中的热塑性纤维组分可以是一种均聚物或共聚物，共聚物在此是指包括一个以上单体(即两个、三个、四个或更多个单体)的聚合产物构成的聚合物。优选地，热塑性聚合物是聚烯烃(PO)，例如聚丙烯(PP)或如低密度聚乙烯(LDPE)、线型低密度聚乙烯(LLDPE)、超低密度聚乙烯(ULDPE)、极低密度聚乙烯(VLDPE)、高密度聚乙烯(HDPE)的聚乙烯(PE)；聚碳酸酯(PC)，丙稀腈和苯乙烯共聚物(SAN)；通过整体聚合法、本体聚合法或乳化法聚合的丙稀腈、丁二烯和苯乙烯三元共聚物(ABS)；聚氯乙烯(PVC)；聚苯醚(PPO)；如尼龙6和尼龙66的聚酰胺(PA)；聚苯乙烯(PS)，如通用、耐冲击、无规立构或间同立构的聚苯乙烯；聚酯，如聚对苯二甲酸乙二酯(PET)或聚对苯二甲酸丁二酯(PBT)；聚苯硫醚(PPS)及其掺合物，如PP/PE之类的热塑性聚烯烃(TPO)；PC/ABS；PPO/PS；PC/聚酯；PA/PP、PA/PPO；PA/PO；和PO/PS。
适用于本发明的聚丙烯是文献中公知的，而且可以通过已知的技术制备。一般而言，聚丙烯是全同立构形式的，尽管也可以使用其它形式(例如间同立构和/或无规立构)。优选地，本发明的聚丙烯是具有高结晶度的全同立构聚丙烯。用于本发明的聚丙烯优选是聚丙烯的均聚物或丙稀与α-烯烃，优选C2或C4至C20α-烯烃的共聚物，例如无规或嵌段共聚物。α-烯烃在本发明的聚丙烯中的含量为不超过30mol％，优选不超过20mol％，更优选不超过15mol％，甚至更优选不超过10mol％，最优选不超过5mol％。
构成丙稀和α-烯烃共聚物的C2和C4至C20α-烯烃的例子包括乙烯、1-丁烯、1-戊烯、1-己烯、1-庚烯、1-辛稀、1-癸烯、1-十二烯、1-hexadodecene、4-甲基-1-戊烯、2-甲基-1-丁烯、3-甲基-1-丁烯、3，3-二甲基-1-丁烯、二乙基-1-丁烯、三甲基-1-丁烯、3-甲基-1-戊烯、乙基-1-戊烯、丙基-1-戊烯、二甲基-1-戊烯、甲基乙基-1-戊烯、二乙基-1-己烯、三甲基-1-戊烯、3-甲基-1-己烯、二甲基-1-己烯、3，5，5-三甲基-1-己烯、甲基乙基-1-庚烯、三甲基-1-庚烯、二甲基辛稀、乙基-1-辛稀、甲基-1-壬烯、乙烯基环戊烯、乙烯基环己烯和乙烯基降冰片烯，其中烷基支化位不定，其通常在烯烃的位3或更高的位置上。
可用于本发明的聚丙烯的熔体流动速率(MFR)通常大于或等于1克/10分钟(克/10分钟)，优选大于或等于5克/10分钟，更优选大于或等于10克/10分钟，甚至更优选大于或等于15克/10分钟，最优选大于或等于20克/10分钟。此处可用的聚丙烯的熔体流动速率通常小于或等于100克/10分钟，优选小于或等于80克/10分钟，更优选小于或等于70克/10分钟，甚至更优选小于或等于60克/10分钟，最优选小于或等于50克/10分钟。除非另行说明，按照ISO 1133在230℃和2.1 6千克(kg)的施加载荷下测定熔体流动速率。
本发明的部分或全部聚丙烯是接枝改性的。使用除至少一个烯键式不饱和基(例如至少一个双键)外还含有至少一个羰基(-C＝O)而且接枝到如上所述的聚丙烯上的任何不饱和有机化合物实现聚丙烯的优选接枝改性。含至少一个羰基的不饱和有机化合物的典型代表是羧酸、酐、酯及其盐，可以是金属的和非金属的。优选地，有机化合物含有与羰基共轭的烯键式不饱和基。典型化合物包括顺丁烯二酸、反丁烯二酸、丙烯酸、甲基丙烯酸、衣康酸、巴豆酸、甲基巴豆酸和肉桂酸、及其酸酐、酯和盐衍生物。顺丁烯二酸酐是优选的含至少一个烯键式不饱和基和至少一个羰基的不饱和化合物。
可以通过任何已知的技术，例如USP 3,236,917、USP5,194,509和USP4,905,541中所述技术，将含至少一个羰基的不饱和有机化合物接枝到聚丙烯上。
接枝聚丙烯的不饱和有机化合物含量至少为聚丙烯和有机化合物总重量的0.01wt％，优选至少0.1wt％，最优选至少0.5wt％。不饱和有机化合物含量的最大值可以为方便使用而进行变动，但典型地不超过聚丙烯和有机化合物总重量的10wt％，优选不超过5wt％，最优选不超过2wt％。
一般而言，热塑性聚合物的用量为组合物总重量的至少20重量份，优选至少30重量份，更优选至少40重量份，最优选至少50重量份。一般而言，热塑性聚合物的用量小于或等于组合物总重量的94重量份，优选小于或等于90重量份，更优选小于或等于80重量份，甚至更优选小于或等于75重量份，最优选小于或等于70重量份。
本发明的纤维增强热塑性聚合物组合物中的弹性体组分是在相对较低的应力下经受较大可逆变形的材料。弹性体的典型特征是在聚合物链中具有结构不规则性、非极性结构或柔性单元。优选地，在应力下，弹性聚合物可以拉伸至其松弛长度的至少两倍，在应力释放后，可以恢复到接近其最初尺寸和形状。可购得的弹性体的一些例子包括天然橡胶、聚烯烃橡胶(POE)、氯化聚乙烯(CPE)、硅橡胶、苯乙烯/丁二烯(SB)共聚物、苯乙烯/丁二烯/苯乙烯(SBS)三元共聚物、苯乙烯/乙烯/丁二烯/苯乙烯(SEBS)三元共聚物和氢化SBS或SEBS。
优选的弹性体是聚烯烃橡胶。适用于本发明的聚烯烃橡胶含有一种或多种聚合形式的C2至C20烯烃，玻璃化转变温度(Tg)小于25℃，优选小于0℃，更优选小于-25℃。Tg是聚合物材料在物理性质(包括，例如机械强度)上表现出突变时的温度或温度范围。可以通过差示扫描量热法测定Tg。本发明的聚烯烃弹性体可以从中选择的聚合物类型的例子包括聚乙烯和α烯烃共聚物，例如乙烯和丙稀(EPM)共聚物、乙烯和1-丁烯共聚物、乙烯和1-己烯共聚物、或乙烯和1-辛稀共聚物、乙烯/丙稀/二烯共聚单体(例如己二烯或亚乙基降冰片烯)的三元共聚物(EPDM)
优选的聚烯烃弹性体是一种或多种基本线型的乙烯聚合物、或一种或多种线型乙烯聚合物(S/LEP)、或其中一种或多种的混合物。基本线型的乙烯聚合物和线型乙烯聚合物都是公知的。在USP 5,272,236和USP 5,278,272中有充分描述了基本线型的乙烯聚合物及其制备方法，在USP 3,645,992、USP 4,937,299、USP 4,701,432、USP 4,937,301、USP 4,935,397、USP 5,055,438、EP 129,368、EP 260,999和WO90/07526中充分公开了线型乙烯聚合物及其制备方法。
弹性体的用量大于或等于纤维增强热塑性聚合物组合物重量的1重量份，优选大于或等于2重量份，更优选大于或等于4重量份，甚至更优选大于或等于6重量份，最优选大于或等于10重量份。一般而言，弹性体的用量小于等于纤维增强热塑性聚合物组合物重量的70重量份，优选小于或等于50重量份，更优选小于或等于40重量份，甚至更优选小于或等于30重量份，最优选小于或等于20重量份。
本发明的加工制品包含热塑性聚合物、弹性体和增强纤维的纤维增强热塑性聚合物组合物。此外，本发明的纤维增强热塑性聚合物组合物也可以(任选)包含一种或多种额外的聚合物和/或也可以(任选)包含这类热塑性组合物中常用的一种或多种添加剂。额外的聚合物可以是一种或多种上述热塑性聚合物而且可以与纤维增强的热塑性聚合物组合物中的热塑性聚合物组分相同或不同。典型添加剂的例子是不同于增强纤维组分的填料，例如但不限于，滑石、粘土、硅灰石、云母、碳酸钙或其混合物；热稳定剂；紫外(UV)线稳定剂；偶联剂；色料；抗氧化剂；抗静电剂；脱模剂、澄清剂、成核剂、阻燃剂，例如但不限于，卤代烃、卤代碳酸酯低聚物、卤代二环氧甘油醚、有机磷化合物(例如单、二或低聚磷酸酯)、氟化烯烃、氧化锑、和芳族硫的金属盐、或其混合物。
根据添加剂和所需效用，这些添加剂的含量是组合物总重量的至少0.01重量份，优选至少0.1重量份，更优选至少1重量份，更优选至少2重量份，最优选至少5重量份。通常，添加剂的含量小于或等于组合物总重量的25重量份，优选小于或等于20重量份，更优选小于或等于15重量份，更优选小于或等于12重量份，最优选小于或等于10重量份。
在本发明的方法中，任何额外的聚合物和/或添加剂优选与弹性体一起作为母炼胶加入。母炼胶是指两种或多种组分的混合物。构成母炼胶的各组分可以以任何合适的方式结合，使其在最终的纤维增强热塑性聚合物组合物中充分分散，例如，其可以干混和/或熔体混合，其可以以粉末和/或丸粒的形式混合，其可以以纯净形式加入也可以以载体(例如热塑性聚合物、蜡或油)中的浓缩液形式加入，或者结合使用这些方式。优选地，除大多数至所有的热塑性聚合物组分和增强纤维材料外，弹性体和其它组分总数中至少一半至所有的组分(例如添加剂)作为母炼胶加入。更优选地，除大多数至所有的热塑性聚合物组分和增强纤维材料外，弹性体和至少2/3至所有的其它组分作为母炼胶加入。再优选地，除大多数至所有的热塑性聚合物组分和增强纤维材料外，弹性体和至少3/4至所有的其它组分作为母炼胶加入。更优选地，除大多数至所有的热塑性聚合物组分和增强纤维材料外，弹性体和所有的其它组分作为母炼胶加入。在某些情况下，优选在母炼胶中加入高达49wt％的热塑性聚合物组分。
为了举例说明本发明的实践，下文列举优选实施方式的实施例。然而，这些实施例不以任何方式限制本发明的范围。
实施例
在下列实施例中，重量百分比是以纤维增强丙稀聚合物组合物的总重量为基础的。
将耐冲击聚丙烯和含聚烯烃橡胶、胶粘剂和浓色母料的母炼胶加入机筒温度约为240℃的Dieffenbacher单螺杆压出机中并在此塑炼，形成熔融的丙稀聚合物组合物。将熔融的丙稀聚合物组合物输送到Dieffenbacher双螺杆压出机(在此，在输送开始时加入大约48玻璃粗纱(30wt％))和设定为大约210℃的混合区中。当纤维增强的熔融丙稀聚合物组合物通过双螺杆压出机从熔体区输送到模头区(两个区域都设为240℃)时，将连续纤维切短至1英寸(2.54厘米)至4英寸(10.16厘米)内的所需长度。双螺杆以每分钟55转的速度运转，处理量为每小时300磅(136.08千克)。
将纤维增强丙稀聚合物组合物通过模头压出，形成大约7英寸(17.78厘米)宽×大约1.25英寸(3.18厘米)高的带状物。由第一输送带将熔融的带状物穿过175℃的温度受控罩壳输送到切刀处，将带状物切成预成型坯(称作原材)并在设为240℃的温度受控罩壳中的第二输送带上运离切刀，然后由第三输送带经过设为200℃的温度受控管道输送带压塑模中。在每个模制周期的塑模中需要三个原材，第一个和第二个约为28.5英寸(72.39厘米)长，第三个约为5.9英寸(65.79厘米)长。
将这些原材用手放置在模腔温度为180℃且中心温度为170℃的3000吨压模机的塑模中。缓慢关闭时间约为9秒，吨位(tonnage)时间约为1.5分钟，硫化时间约为0.5分钟。加工制品是车辆底板，其具有在0.125英寸(0.32厘米)至0.2英寸(0.51厘米)之间的可变壁厚，大约3.5英尺(1.07米)长×2.5英尺(0.76米)宽×2英尺(0.61米)深，且重量约为19磅(8.62千克)。
表1给出了实施例1至4的组成(重量份以总组合物重量为基础)。
在表1中：
“PP”是一种含大约12％乙烯且熔体流动速率为35克/分钟的耐冲击聚丙烯共聚物，按照ISO 1133在230℃和2.16千克的施加载荷下测定熔体流动速率。
“POE”是可得自陶氏化学公司的AFFINITYTM 8200聚烯烃的基本线型乙烯聚合物，其具有大约0.87克/平方厘米(g/cm2)的密度、5克/10分钟的熔体流度速率(按照ISO 1133在190℃和2.16千克的施加载荷下测定)、2.1的分子量分布；
“玻璃”是可得自PPG的TUFROVTM的连续玻璃纤维，其具有2205的纤度单位值和大约17微米的直径；
“色料”是可得自Americhem的Product Code 52480-H1的黑灰色浓色母料。
“SA”是可得自Crompton的POLYBNDTM 3200的马来酸聚丙烯胶粘剂，其具有1至1.5％的马来酐接枝度。
在从加工制品上切下的试样上进行下列测试，测试结果记录在表1中：
弯曲性能，“FM”(弯曲模量)和“FS”(弯曲强度)，在0.2英寸(0.51厘米)× 1英寸(2.54厘米)×8英寸(20.32厘米)的试样上按照ISO178以2毫米(mm)/分钟进行测试，所得值的单位是兆帕(MPa)；
抗张性能，“TS”(抗张强度)和“TE”(致断拉伸长度)，在0.2英寸(0.5 1厘米)×1英寸(2.54厘米)×8英寸(20.32厘米)的试样上按照ISO 527以5毫米(mm)/分钟进行测试，所得值的单位分别是MPa和％；
仪器化落镖冲击，“IDI”，在3、4和5毫米厚的3英寸(7.62厘米)×3英寸(7.62厘米)试样上按照ISO 6603/2以4.4米/秒(m/s)在73℃下进行测试，其中落镖半径为20毫米，环形开口为40毫米，在用相当于下环的40毫米环冲击的过程中没有靠气动夹住的润滑样品，所得值的单位是焦耳(J)；
                                表1
  组合物     1     2     3     4
  PP     67     65     63     61
  POE     0     2     4     6
  玻璃     30     30     30     30
  色料     2     2     2     2
  SA     1     1     1     1
  性能
  FM，MPa     4760     5330     5000     4820
  FS，MPa     97     113     115     108
  TS，MPa     52     55     53     58
  TE，％     1.4     1.6     1.4     1.5
  IDI@3毫米，J     15     14     14     17
  IDI@4毫米，J     18     20     22     24
  IDI@5毫米，J     29     33     33     34

Claims (17)

1.一种制造纤维增强的热塑性聚合物组合物并由其形成加工制品的方法，包括下列步骤：
(1)在压出机中加入热塑性聚合物，
(2)在压出机中加入含弹性体的母炼胶，
(3)在压出机中塑炼热塑性聚合物和母炼胶以形成熔融的热塑性聚合物组合物，
(4)在熔融的热塑性聚合物组合物中加入增强纤维材料，
(5)将熔融的纤维增强热塑性聚合物组合物压出，并
(6)形成含有纤维增强热塑性聚合物组合物的加工制品。
2.根据权利要求1所述的方法，在步骤(5)和(6)之间进一步包括下列步骤：
(i)将熔融的纤维增强热塑性聚合物组合物通过模头压出，形成具有所需横截面形状的加热纤维增强热塑性聚合物组合物的连续挤压件，
(ii)将该加热纤维增强热塑性聚合物组合物的连续挤压件输送到切刀处，
(iii)将连续挤压件切成多个预成型坯，并
(iv)将这些预成型坯运离所述切刀并输送到压塑模、真空成型塑模或热成型塑模中。
3.根据权利要求2所述的方法，其中步骤(iv)中的塑模是压模。
4.根据权利要求1所述的方法，在步骤(5)和(6)之间进一步包括下列步骤：
(v)将熔融的纤维增强热塑性聚合物组合物输送到聚积器中；
(vi)聚积所需量的加热纤维增强热塑性聚合物组合物以形成颗粒并
(vii)将该颗粒注入注模中。
5.根据权利要求1所述的方法，在步骤(5)和(6)之间进一步包括下列步骤：
(viii)将熔融的纤维增强热塑性聚合物从挤压模头中压出，形成具有所需形状的型坯，
(ix)将所述型坯置于吹塑模中，
(x)封闭所述吹塑模，并
(xi)将气体注入所述吹塑模中。
6.根据权利要求1所述的方法，在步骤(5)和(6)之间进一步包括下列步骤：
(xii)将熔融的纤维增强热塑性聚合物组合物从具有所需形状的型材挤塑模中压出。
7.根据权利要求1所述的方法，其中压出机是单螺杆压出机或双螺杆压出机。
8.根据权利要求1所述的方法，其中弹性体是聚烯烃弹性体。
9.如权利要求1所述的方法，其中弹性体是含有乙烯和C3至C20α烯烃的基本线型的聚乙烯聚合物或线型乙烯聚合物。
10.根据权利要求1所述的方法，其中弹性体是含乙烯和选自丙稀、丁烯、己烯或1-辛稀的α-烯烃的基本线型的聚乙烯聚合物或线型乙烯聚合物。
11.根据权利要求1所述的方法，其中弹性体是含乙烯和1-辛稀的基本线型的聚乙烯聚合物。
12.根据权利要求1所述的方法，其中母炼胶进一步包括滑石、粘土、硅灰石、云母、碳酸钙、热稳定剂、紫外(UV)线稳定剂、偶联剂、着色剂、抗氧化剂、抗静电剂、澄清剂、成核剂、阻燃剂，或其混合物。
13.根据权利要求1所述的方法，其中增强纤维材料是连续或不连续的，并且是玻璃纤维、碳石墨纤维、聚酯纤维、聚芳酰胺纤维、大麻纤维、金属纤维或镀金属纤维。
14.根据权利要求1所述的方法，其中增强纤维材料是连续的。
15.根据权利要求1所述的方法，其中增强纤维材料是大量的连续玻璃纤维。
16.根据权利要求1所述的方法，其中加工制品是车辆底座衬垫、车辆仪表盘、车辆整流罩、车辆挡泥板、车辆面板、车辆车体外壳、车辆底板、电子设备器件外壳、机箱、草坪和庭园用具、底板覆盖物或墙面覆盖物，其中车辆是小轿车、卡车、摩托雪橇、私人船只、所有的地面运动车辆、草坪和园艺拖拉机、农场设备或高尔夫球车。
17.根据权利要求1所述的方法，其中加工制品是高尔夫球车底板。
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CN110126323A (zh) * 2019-06-05 2019-08-16 无锡市荣允瓶盖有限公司 一种密封性好的塑料瓶盖生产方法
CN111688236A (zh) * 2020-06-12 2020-09-22 东北林业大学 一种引入连续纤维的分散型天然纤维增强热塑性树脂预浸带的制备方法

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