CN1325250C - 具有交联聚合物层的多层聚合物制品及其制造方法 - Google Patents
具有交联聚合物层的多层聚合物制品及其制造方法 Download PDFInfo
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- CN1325250C CN1325250C CNB028140389A CN02814038A CN1325250C CN 1325250 C CN1325250 C CN 1325250C CN B028140389 A CNB028140389 A CN B028140389A CN 02814038 A CN02814038 A CN 02814038A CN 1325250 C CN1325250 C CN 1325250C
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Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Laminated Bodies (AREA)
Abstract
公开了一种相互交联的多层聚合物制品,其包括:(A)至少一种热塑聚合物层,与之相接触的是(B)至少一种可交联聚合物层,其中(A)和(B)彼此不相容,而且(A)和(B)通过相互交联固定在一起。还公开了一种制备相互交联多层聚合物制品的方法。
Description
发明领域
本发明涉及如薄膜,片材,管材,软管,中空体等聚合物多层制品,将热塑性聚合物作为其中的一层。
发明背景
例如热塑性氟聚合物的高性能热塑性塑料,具有高热稳定性,化学惰性和不粘剥离性等多种独特性能。因此,它们被广泛用于涉及高温,侵蚀性化学品和剥离应用中。但是,这些聚合物与许多其他聚合物相比,价格昂贵。多层结构是降低氟聚合物制成的制品成本的一种合适方法,这种制品中,氟聚合物与其他具有低密度,弹性,密封性,抗刮性等多项优点的聚合物复合在一起。在制造含有氟聚合物的多层结构时,一直存在获得与氟聚合物层合适的层间粘合性的问题。许多氟聚合物是非极性的且具有很低的表面能(非润湿表面)。层间润湿可以通过熔融氟聚合物而获得;但是,在固化时,获得的多层产品层能很容易地被分离(脱层)。在许多情况下,层间粘合性是不够的,除非氟聚合物用化学方法官能化或采用特殊处理技术对其表面进行化学改性,这两种方法都是高成本和复杂的。如果目的是制造一种具有很薄氟聚合物层的多层制品,则中间层表面改性的成本会变得很高,或甚至是无法操作的。用化学方法官能化的氟聚合物是昂贵的,它们被用来粘合如尼龙等特殊聚合物,而不是聚烯烃。基于许多热塑性氟聚合物的官能化形式的材料,比如乙烯和丙烯的全氟化共聚物(FEP),四氟乙烯和全氟甲基乙烯基醚的共聚物(MFA)或全氟烷氧基树脂(PFA),都不是市售的。
美国专利3650827(Brown等,1972年3月21日)描述了一种具有聚乙烯组合物涂层中央铜导体的电缆。对该控制电缆施加的辐射剂量是约10兆拉德。该涂层电缆上挤出有四氟乙烯和六氟丙烯共聚物(FEP)的薄层。挤出后,用高能电子,X射线或紫外光在高于FEP玻璃化转变温度的温度下,引发FEP护套中的交联。
美国专利4155823(Gotcher等,1979年5月22日)涉及可熔融加工的氟碳聚合组合物,该组合物的加工温度要求超过200℃,而且由于氟碳聚合物中掺入了交联剂,因此是可辐射交联的。氟碳聚合物暴露于足以产生令人满意的交联而不会使其裂解的辐射剂量下。
美国专利4677017(DeAntonis,1987年6月30日)涉及一种多层薄膜及其共挤出方法。该共挤出薄膜具有至少一层热塑性氟聚合物层和至少一层与其相相邻的热塑性聚合物层。在每层热塑性氟聚合物层和每层热塑性聚合物层之间,存在有一种改性的聚烯烃粘合剂。
美国专利5480721(Pozzoli等,1996年1月2日)涉及使用一种粘合剂中间层粘合氟化聚合物和非氟化热塑性材料,该粘合剂中间层包含一种含氟化和非氟化热塑性塑料和一种离聚物的共混物或包含具有能或不能成盐的活性基团的共聚物的多种离聚物的共混物。
美国专利5578681(Tabb,1996年11月26日)公开了氟弹性体和乙烯共聚弹性体的可固化弹性混合物,其中至少一种氟弹性体和乙烯共聚弹性体包含一种固化位单体。
美国专利5916659(Koerber等,1999年6月29日)涉及包含在热量或压力影响下不易彼此粘合的聚合物的层状复合物。特别涉及由氟聚合物和非氟聚合物材料的分离层构成的复合物,该复合物由于创新地使用了纤维状粘合剂,因此具有提高的剥离粘合特性。
专利WO98/05493(Spohn,E.I.DuPont de Nemour and Copmany,国际公开日1998年2月12日)提出了一种包含氟聚合物和聚酰胺层的层压材料,该层压材料能通过共挤出单个挤出步骤而形成,其中的氟聚合物层和聚酰胺层在没有粘合剂粘结层存在时也能彼此粘合。
发明概述
本发明公开了一种相互交联多层聚合物制品,其包括:
(A)至少一种热塑性聚合物层,与之接触的是
(B)至少一种可交联聚合物层,其中(A)和(B)彼此不相容,而且(A)和(B)通过相互交联固定在一起。
本发明的另一个实例涉及制备相互交联多层聚合物制品的方法,该制品包括:
(A)至少一种热塑性聚合物层,与之接触的是
(B)至少一种可交联热塑性聚合物层,其中(A)和(B)彼此不相容,该方法包括以下步骤:
将(A)和(B)在超过(A)和(B)两者熔点的温度和0.1到80兆帕压力下彼此直接接触,形成多层制品;和
保持(A)和(B)接触的同时,使多层制品交联,制成相互交联多层聚合物制品。
发明详述
相互交联多层聚合物制品包含至少一种热塑性聚合物层(A),与至少一种可交联聚合物层(B)接触。重要的是,(A)和(B)聚合物层是彼此不相容的。(A)与(B)的直接接触在高于它们的熔点的温度和0.1到80兆帕压力下进行,并形成多层制品。通过交联多层制品,在(A)和(B)之间产生键合,形成相互交联多层聚合物制品。
(A)热塑性聚合物层
热塑性聚合物层是从包含聚烯烃,聚酰胺,聚酯或氟聚合物树脂的热塑性树脂制备的。优选氟聚合物树脂。通常,热塑性树脂在加热时不会发生化学反应,但是会发生熔融和流动,因此能以薄膜或片材形式被挤出。可被用做组分(A)的热塑性氟聚合物包括乙烯和丙烯的氟化共聚物(FEP),四氟乙烯和全氟丙基乙烯基醚的氟化共聚体(PFA),乙烯和四氟乙烯的共聚物(ETFE),乙烯和三氟氯乙烯的共聚物(ECTFE),聚三氟氯乙烯(PCTFE),聚偏二氟乙烯(PVDF),含有四氟乙烯,六氟丙烯和偏二氟乙烯链段的三元共聚物(THV),它们的共混物和合金,或它们的共混物或合金。优选的氟聚合物是FEP。THV树脂可以从Dyneon 3M CorporationMinneapolis,Minn.获得。ECTFE聚合物可以从Ausimont Corporation(意大利)获得,商品名为Halar。其他所用的氟聚合物可以从Daikin(日本),DuPont(美国)和Hoechst(德国)获得。
而且,(A)自身可以是可交联聚合物。可用做(A)的可交联聚合物包括聚酰胺,聚酯和它们的共聚物,以及包括聚乙烯的聚烯烃。在以上热塑性氟聚合物中,注意,ETFE,THV和PVDF可以用如电子束等辐射而交联。
(B)可交联热塑性聚合物层
本发明中可以用做可交联热塑性聚合物层(B)的材料是聚烯烃,它们为均聚物,共聚物,三元共聚物或它们的混合物。本发明中的聚烯烃类型是高密度聚乙烯(PE),中密度PE,低密度PE,超低密度PE,乙烯丙烯共聚物,乙烯-1-丁烯共聚物,聚丙烯(PP),聚1-丁烯,聚1-戊烯,聚-4-甲基-1-戊烯,聚苯乙烯,乙烯-丙烯橡胶(EPR),乙烯-丙烯-二烯聚合物(EPDM)等。本发明优选的聚烯烃类型是EPDM。
所用的EPDM聚合物包括乙烯,丙烯和二烯单体的共聚单元。乙烯占EPDM聚合物总重量的约63-95重量%,丙烯约为5-37重量%,二烯约为0.2-15重量%。优选的乙烯含量约为EPDM聚合物的70-90重量%,丙烯约17-31重量%,二烯约10重量%。合适的二烯单体包括如丁二烯,异戊二烯,氯丁二烯等的共轭二烯;如1,4-戊二烯,1,4-己二烯,1,5-己二烯,2,5-二甲基-1,5-己二烯,1,4-辛二烯等具有5到约25个碳原子的非共轭二烯;如环戊二烯,环己二烯,环辛二烯,双环戊二烯等的环二烯;如1-乙烯基-1-环戊烯,1-乙烯基-1-环己烯等的乙烯基环烯;如3-甲基二环-(4,2,1)-3,7-壬二烯等的烷基二环壬二烯;如甲基四氢茚等的茚;如5-亚乙基-2-降冰片烯,5-亚丁基-2-降冰片烯,2-甲代烯丙基-5-降冰片烯,2-异丙烯基-5-降冰片烯,5-(1,5-己二烯基)-2-降冰片烯,5-(3,7-辛二烯基)-2-降冰片烯等的链烯基降冰片烯;和如3-甲基三环-(5,2,1,0.sup.2,6)-3,8-癸二烯等的三环二烯。更优选的二烯包括非共轭二烯。可以采用下面已知的悬浮和溶液技术容易制得EPDM聚合物,如美国专利3646169和Friedlander所著《聚合物科学技术百科全书》(Encyclopedia of Polymer Science andTechnology)(New York,1967)第六卷第338-386页中所述。EPDM聚合物是高分子量的固体弹性体。它们的门尼粘度通常至少是约20,优选约25到约150(在125℃ML1+8),每分升甲苯含0.1克EPDM聚合物的稀溶液粘度(DSV)在25℃的测量值至少是约1,优选约1.3到约3。原料聚合物通常具有约800到约1800,更典型为约900到约1600磅/平方英寸的原始拉伸强度,而且断裂伸长至少是约600%。EPDM聚合物通常是用少量的如二环戊二烯,乙基降冰片烯,甲基降冰片烯,非共轭己二烯等的二烯单体制造的,而且数均分子量是约50,000到约100,000。
组分(A)和(B)是彼此不相容的,而且两种组分在高于两者熔点的温度,优选不超过400℃和0.1到80兆帕,优选不超过40兆帕压力的条件下彼此直接接触,预先形成多层制品。“不相容”是指(A)和(B)甚至在高于其熔点温度下彼此接触时也不会互相混合或溶解。在(A)和(B)之间没有化学相互作用发生,而且这些组分间事实上没有键合。存在(A)和(B)各一层。在其他实例中,两层(A)分别与一层(B)的各面接触,或两层(B)分别与一层(A)的各面接触。在另一个实例中,若干层(A)与若干层(B)相邻排列,其中(A)和(B)相互逐一交替,当(A)和(B)的层数为奇数时,终端层是两个(A)或两个(B),当(A)和(B)的层数为偶数时,一个外层是(A)且另一个外层是(B)。另外,还可有其他除(A)和(B)之外的层存在,只要至少有一对(A)层和(B)层彼此接触。
有多种方法使(A)和(B)接触。这些方法是共挤出,共层压,挤出-层压,预制层的熔融涂布和共模塑。对共模塑而言,可以是共注塑,多材料模塑,多注射模塑,压铸,吹塑和包括多层压塑的压塑。通过共模塑方法,能够制成如容器等的多层制品。通过共挤出方法,能够制成薄膜,片材,软管或型材。
模塑通常是经三种基本模塑技术完成的:压塑,压铸和共注塑。这些模塑技术的说明可参见Wright,Ralph E.所著《模塑热固性塑料》(Molded Thermosets);《塑料工程师,模塑师和设计师手册》(A Handbook for Plastics Engineers,Molders,and Designers),Hanser Publishers,Oxford University Press,NewYork,1991。
对模塑技术的选择很大程度上取决于模塑制品设计和功能上的要求及其生产经济性的要求。虽然每种方法都有一些相似处,但仍具有其自身的设计和操作要求。在选择模塑技术用于制造制品时要考虑的因素包括,例如制品设计特点,模具设计,模塑过程,压机选择和操作以及模塑后工具和夹具。
压塑通常使用一个立式液压操作的压机,该压机具有两块压板,一块固定,另一块可移动。半模固定在压板上。将预先计量好的模塑料采用手动或自动方式置于加热的模腔中。自动装料包括使用过程控制,使模塑方法应用更广。然后用合适的压力和温度将模具闭合。在模塑周期的结束时,用液压方式打开模具并取出模塑好的部件。
压塑的模具结构基本上由一个模腔和一个柱塞构成。根据最终部件设计,模具可以具有各种滑块,顶出销和/或移动板,以帮助模具操作和取出模塑制品。可以调整模具的溢料间隙和尺寸公差,以适应配混料的特性和部件要求。
压铸类似于压塑,区别在于物料加入模腔的方法不同。该技术典型适用于多模腔模具。在这个方法中,物料以手动或自动方式通过流道***被加入与模腔相连的圆筒中。可以使用螺杆将物料加入压铸压缸中。用第二液压单元对柱塞提供动力,使模塑料经流道注入闭合模具的模腔中。然后用立式液压压机在合适的温度下施加要求的压力,压塑出要求的部件。压铸模具设计比压模模具的设计更复杂一些,因为其内部存在压铸压缸和流道,还要考虑模具内部的流动,但一般部分是相似的。可以使用梭式压机使埋塑嵌件封铸。
总的来说,共注塑与压铸有关,区别在于其液压压机通常是水平方向的,而且模塑料是经注道衬套,浇口和流道***被螺杆注入闭合模腔中的。然后在合适的温度下施加压力,使部件固化。打开模具进行部件顶出和取出,闭合模具,通过螺杆注射再次加料。注塑技术相对其他上述技术的显著优点是循环时间。因此,在多模腔模塑中有广泛应用。注射模具设计更复杂,对模塑料的模具内流动要特别注意。在注塑的扩展应用中,可以使用一个梭式压机使埋塑嵌件封铸。
总之,压塑技术主要是一种半间歇方法,通常产生最小的部件收缩和最高的部件密度,但是循环时间最长,生产受埋塑嵌件的能力和模具设计复杂性的限制,需要最大的工作量完成模塑成品(除去溢料)。压铸和注塑分别是半自动和自动方法,具有更短的循环时间,制造埋塑嵌件时极佳的操作性,和较小的工作量完成模塑部件。与压缩模塑相比,这两种技术通常都产生较低的部件密度和增大收缩。
可以采用本领域技术人员公知的任何共挤出方法制备本发明的片材或薄膜。比如,可以先分别挤出含组分(A)和(B)的片,然后放在一起在共挤出模头的热软化条件下或模头出口处,形成预成型制品。如果存在化学交联剂,则发生交联。如果没有,则可以对该片进行辐射交联。或者,可以形成熔融的聚合复合流,一面是(A)层,另一面是(B)层。然后将该复合流送入挤出模头,在模头中复合流横向扩展或再成型成复合片或复合薄膜。要制造具有要求的层排列和厚度的共挤出复合产品,可以分别控制共挤出单元的每个进料管线的进料速度,这对本领域技术人员是公知的。
当多层制品预成型后,要进行交联,使(A)和(B)键合在一起。如果没有这交联,(A)和(B)层很容易分离。通过相互交联,(A)和(B)层就不会彼此分离,或只能很困难地并破坏多层制品,才能使其分离。因此,本发明在交联前的剥离强度很低,而交联后,就具有很高的剥离强度。
交联可以通过辐射进行。辐射包括X射线,γ射线,紫外光,可见光或也称为e-beam的电子束。“紫外”或“UV”是指波长或多数波长在170到400纳米范围内的辐射。“电离辐射”是指能产生离子的高能辐射,包括电子束辐射,γ射线和X射线。术语“e-beam”是指由Van de Graaff发生器,电子加速器或X射线产生的电子束的电离辐射。
辐射交联可以在升高的温度下发生,比如当(A)和(B)被一起置于高于任一组分熔点温度时,或在室温或其间的任一温度下发生。
在辐射交联的时间安排上,也有时机时间。在多层制品仍然处于升高的温度时,(A)和(B)一贴近,就可能立刻发生交联。在这种情况下,这样就制得最终产品。在另一种情况下,将(A)和(B)置于一起,在升高温度下形成非交联制品,待非交联制品冷却至或接近室温时,过后才发生交联。这里所指的辐射剂量是以辐射单位,“拉德”,表示一百万拉德或兆拉德被称为“Mrad”。分子交联度取决于辐射剂量,通常,辐射剂量越高,交联度越大。
这里所说的“辐射”通常是指电离辐射,比如X射线,γ射线和能直接引发分子交联的高能电子。(但是,当与分散在材料中的交联剂共同使用时,热量和光也被视为能引发交联的辐射能量形式。)电子是优选的辐射能量形式,优选由0.1到2.0兆电子伏特的市售加速器产生。
优选的交联方法是通过电离辐射。因此,在优选方法中,使多层制品通过由电子加速器产生的电子束而受到辐射。在典型的加速器中,电子束对多层制品的宽度进行扫描,多层制品多次通过电子束,直至获得要求的辐射剂量。电子能量范围是0.1到2.0兆电子伏特,据发现,本发明优选的剂量水平在1.0到12.0兆拉德(Mrad)范围内。当然,任何能在长链烯烃聚合物分子间引发交联的电离辐射都是合适的。足以加强多层结构所需的剂量随分子量,密度和可交联材料的组成不同而不同,对某些如聚乙烯的结构,低至1.0兆拉德。另一方面,在大于12兆拉德的剂量水平下,某些共聚物被交联成坚硬而难于处理的程度。因此,对大多数结构而言,最佳的剂量水平范围介于4和8兆拉德之间。辐射之后,形成多层制品。
在某些辐射形式中,最好使用光引发剂或敏化剂组合物。因此,组分(B)可进一步包括光引发化合物。这种化合物与(B)混合形成一种基本均匀的组合物。当考虑紫外辐射作为辐射形式时,(B)优选应包含光引发剂,以提高交联效率,即每单位辐射剂量的交联度,当考虑电子束辐射作为辐射形式时,(B)可以任选包含光引发剂。虽然电子束辐射通常并不与光引发剂一起使用,因为不含这种化合物时也能容易地发生交联,据报道,当使用含有这种光引发剂组合物的(B)时,交联效率提高,由此可获得更高程度的交联,可使用更低剂量的电子束辐射或它们的组合。
合适的光引发剂包括但并不限于二苯甲酮,邻-和对-甲氧基二苯甲酮,二甲基二苯甲酮,二甲氧基二苯甲酮,二苯氧基二苯甲酮,苯乙酮,邻-甲氧基-苯乙酮,二氢苊醌,丁酮,戊酰苯酮,己酰苯,α-苯基-丁酰苯,对-吗啉代丙酰苯,二苯并环庚酮,4-吗啉代二苯甲酮,苯偶姻,苯偶姻甲基醚,3-邻-吗啉代脱氧苯偶姻,对-二乙酰基苯,4-氨基二苯甲酮,4′-甲氧基苯乙酮,α-四氢萘酮,9-乙酰基菲,2-乙酰基菲,10-噻吨酮,3-乙酰基菲,3-乙酰基吲哚,9-芴酮,2,3-二氢-1-茚酮,1,3,5-三乙酰基苯,9-噻吨酮,9-占吨酮,7-H-苯并[de]蒽-7-酮,苯偶姻四氢吡喃醚,4,4’-二(二甲氨基)-二苯甲酮,1’-萘乙酮,2’-萘乙酮,萘乙酮和2,3-丁二酮,苯并[a]蒽-7,12-二酮,2,2-二甲氧基-2-苯基苯乙酮,α,α-二乙氧基苯乙酮,α,α-二丁氧基苯乙酮,蒽醌,异丙基噻吨酮等。聚合引发剂包括聚(乙烯/一氧化碳),低聚[2-羟基-2-甲基-1-[4-(1-甲基乙烯基)-苯基]丙酮],聚甲基乙烯基酮和聚乙烯基芳基酮。光引发剂优选与紫外辐射共同使用,因为它通常能提供更快和更有效的交联。
优选的市售光引发剂包括二苯甲酮,蒽酮,占吨酮及其它,从Ciba-Geigy Corp.购得的IrgacureTM系列光引发剂包括2,2-二甲氧基-2-苯基苯乙酮,(IrgacureTM651);1-羟基环己基苯基酮(IrgacureTM184)和2-甲基-1-[4-(甲硫基)苯基]-2-吗啉代-1-丙酮(IrgacureTM907)。最优选的光引发剂具有从配制树脂的迁移低,在挤出温度的低蒸汽压和在聚合物或聚合物共混物中的足够溶解度,能够产生良好的交联效率。很多常用光引发剂的蒸汽压和溶解度或聚合物相容性能够通过连接衍生基团而容易得到提高。衍生的光引发剂包括,例如更高分子量的二苯甲酮衍生物,如4-苯基二苯甲酮,4-烯丙氧基二苯甲酮,4-十二烷氧基二苯甲酮和类似物。可以将光引发剂与(B)共价键合。因此,最优选的光引发剂是基本上从组装结构无迁移的。
光引发剂以(B)的0到约3重量%,优选0.1%到2重量%的浓度添加。
还可以使用含有过氧化物,胺和硅烷的化学交联剂进行交联。
对于化学交联,将(B)与一种交联剂混合制备成基本均匀或均相的(B)混合物。每种化学交联剂将在下文更详细说明。通常(B)和交联剂的混合料是通过将固体状态的(B)与粉末状态的交联剂干混而制备的。但是,可以采用任何用来制备简单混合料的本领域公知技术来制备该混合料,比如由液体状态的组分制备混合料,吸附在惰性粉末载体上以及制备带涂层粒料等方法。
可用于本发明的可热活化交联剂包括本领域公知的任何能产生自由基的化学品。这些化学品受到热量作用时,会分解形成至少一种,通常是两种或更多的自由基,从而引发交联。本领域公知的任何交联剂都可以用于本发明,但优选的交联剂是一种含有机过氧化物,胺和硅烷的有机交联剂。
可用于本发明的有机过氧化物的例子包括但并不限于2,7-二甲基-2,7-二(叔丁基过氧)-3,5-辛二炔;2,7-二甲基-2,7-二(过氧碳酸乙酯)-3,5-辛二炔;3,6-二甲基-3,6-二(过氧碳酸乙酯)-4-辛炔;3,6-二甲基-3,6-(叔丁基过氧)-4-辛炔;2,5-二甲基-2,5-二(过氧苯甲酸酯)-3-己炔;2,5-二甲基-2,5-二(过氧碳酸正丙酯)-3-己炔;2,5-二甲基-2,5-二(过氧碳酸异丁酯)-3-己炔;2,5-二甲基-2,5-二(过氧碳酸乙酯)-3-己炔;2,5-二甲基-2,5-二(α-异丙苯基过氧)-3-己炔;2,5-二甲基-2,5-二(过氧碳酸β-氯乙酯)-3-己炔和2,5-二甲基-2,5-二(叔丁基过氧)-3-己炔。目前优选交联剂是2,5-二甲基-2,5-二(叔丁基过氧)-3-己炔,从ElfAtochem购得,商品名为Lupersol 130。另一种交联剂是过氧化二异丙苯基,从Elf Atochem购得,商品名为Luperox 500R。优选聚合物中的交联剂浓度是(B)重量的0.1%到5%,优选0.5%到2重量%。
合适的硅烷交联剂具有以下通式,
其中R1是氢原子或甲基;X和Y是0或1,条件是当X是1,Y是1;n是1到12(包括1和12),优选1到4的整数,每个R分别是可水解的有机基团,比如具有1到12个碳原子的烷氧基(例如甲氧基,乙氧基,丁氧基),芳氧基(例如苯氧基),芳烷氧基(例如苄氧基),具有1到12个碳原子的脂肪族酰氧基(例如甲酰氧基,乙酰氧基,丙酰氧基),氨基或取代的氨基(烷氨基,芳氨基)或具有1到6个碳原子的低级烷基,条件是三个R基团中不超过一个是烷基。这种硅烷可以通过使用适量的有机过氧化物,在成型或模塑操作前或过程之中,被接枝到合适的聚烯烃中。如热稳定剂,光稳定剂,颜料等其它配料也可以加入配方中。在任何情况下,交联反应都是在成型或模塑步骤后,通过接枝的硅烷基团和水的反应而发生的,水从大气或水浴或“桑拿”渗入聚合物主体中。产生交联的阶段通常是指“固化阶段”,通常称为“固化”。
任何能被有效接枝并与(B)交联的硅烷都能用于本发明。合适的硅烷包括不饱和硅烷,其含有一种乙烯基不饱和烃基,如乙烯基,烯丙基,异丙烯基,丁烯基,环己烯基或γ-(甲基)丙烯酰氧烯丙基和可水解基团,如烃氧基,酰氧基或烃氨基。可水解基团的例子包括甲氧基,乙氧基,甲酰氧基,乙酰氧基,丙酰氧基和烷氨基或芳氨基。优选的硅烷是能接枝聚合物的不饱和烷氧基硅烷。这些硅烷及其制备方法在Meverden等的美国专利5266627中有详细说明。用于本发明的优选硅烷交联剂是乙烯基三甲氧基硅烷,乙烯基三乙氧基硅烷,γ-(甲基)丙烯酰氧丙基三甲氧基硅烷和这些硅烷的混合物。如果存在填料,则优选交联剂包括乙烯基三乙氧基硅烷。
本发明的硅烷交联剂的用量可根据热塑性聚合物的性质,硅烷,加工条件,接枝效率,最终应用和类似因素有很大变化,通常至少是0.5份/百份树脂(phr),优选至少0.7phr。简便性和经济性也是本发明中硅烷交联剂最大用量的两个主要限制因素,通常硅烷交联剂的最大用量不超过5phr,优选不超过2phr。
硅烷交联剂通过任何传统方法接枝(B),通常是在例如过氧化物和偶氮化合物自由基引发剂存在下或通过电子辐射等进行的。优选有机引发剂,比如任何一种过氧化物引发剂,例如过氧化二异丙苯基,过氧化二叔丁基,过苯甲酸叔丁酯,过氧化苯甲酰,氢过氧化异丙基苯,过辛酸叔丁酯,甲基乙基酮过氧化物,2,5-二甲基-2,5-二(叔丁基过氧)己烷,过氧化月桂酰和过乙酸叔丁酯。合适的偶氮化合物是偶氮二异丁腈。引发剂含量各不相同,但其量通常至少为0.04,优选至少0.06phr。通常,引发剂含量不超过0.15,优选不超过约0.10phr。硅烷交联剂与引发剂的比值也可以有很大的不同,但通常交联剂:引发剂比值在10∶1到30∶1之间,优选18∶1和24∶1。
虽然任何传统方法都能用来将硅烷交联剂接枝(B),但优选的方法是,将这两种组分与引发剂在如Buss捏合机等反应挤出机的第一阶段中混合。接枝条件可以各不相同,但熔体温度通常介于160℃和260℃之间,优选介于190℃和230℃之间,取决于引发剂的停留时间和半衰期。
固化用交联催化剂促进,任何能起到这种作用的催化剂都能用于本发明。这些催化剂通常包括有机碱,羧酸和包括有机钛酸酯的有机金属化合物和铅,钴,铁,镍,锌和锡的配合物或羧酸盐。二月桂酸二丁基锡,马来酸二辛基锡,二乙酸二丁基锡,二辛酸二丁基锡,乙酸亚锡,辛酸亚锡,环烷酸铅,辛酸锌,环烷酸钴等。本发明特别优选羧酸锡,特别是二月桂酸二丁基锡和马来酸二辛基锡。催化剂(或催化剂混合物)的含量是催化剂量,通常约为树脂的0.015和约0.035phr之间。
可以用于本发明的胺交联剂包括单烷基,双烷基和三烷基单胺,其中的烷基包含约2到约14个碳原子,分子式为N(R2)3N的三亚烷基二胺,分子式为HN(R2)2NH的二亚烷基二胺,分子式为H2NR2NH2的亚烷基二胺,分子式为H2NR2NHR2NH2的二亚烷基三胺和具有4到6个碳原子的环链的脂肪胺。以上分子式中的亚烷基R2优选含有约2到约14个碳原子。环胺可以含有如氧等杂原子,如N-烷基吗啉。其它可用的环胺包括吡啶和N,N-二烷基环己胺。以上这些胺是相对不挥发的,不能通过产生的热量被除去。合适的胺的例子包括三乙胺;二正丙胺;三正丙胺;正丁胺;环己胺;三亚乙基二胺,亚乙基二胺;亚丙基二胺;六亚甲基二胺;N,N-二乙基环己胺和吡啶。如果需要,胺可以溶解于合适的溶剂中。比如,三亚乙基二胺可以溶于多羟基叔胺中。以(B)的重量计,胺的用量应约为0.5%到10%。不能使用芳香胺,因为它们是毒性的,而且会使交联产物变色。
化学交联剂与(B)混合后,(A)和(B)彼此接触并交联形成多层制品。化学交联反应中,交联剂分解产生自由基,使(A)和(B)交联并形成多层制品。交联剂的分解是一个与时间相关的反应,温度越高,交联剂分解产生自由基越快。交联剂的半衰期是指交联剂分解一半需要的时间。对于过氧化二异丙苯基,半衰期是100℃时约100小时,120℃时约10小时,138℃时约1小时,182℃时30秒。其它交联剂的半衰期也类似。
混合的一种形式是干混,其中(B)和化学交联剂被同时送入挤出机。(B)和交联剂可以被预混合或最终在挤出机中混合,制成聚合物-交联剂共混料。(B)和交联剂被分别通过输送管线进入螺杆挤出机进行混合。或者,(B)和交联剂也可以被直接送入本领域公知的混合设备中,制成一种简单的混合料,然后被送入挤出机,进一步混合和加热。
在应用交联剂的另一个实例中,当(A)是一种可交联聚合物时,交联剂可以被加入(A)而不是(B)。而且,当(A)是一种可交联聚合物时,(A)和(B)中可以都加入交联剂。
上述使(A)和(B)接触的一种方法是共挤出。以下将讨论用辐射进行交联的共挤出方法。
要说明辐射交联,通过挤出方法制备进行薄膜。在挤出过程中,(A)和(B)被分别熔融并分开供料,或者共熔融并送入共挤出供料头和模头中,形成(A)和(B)的薄膜。优选的挤出模头结构是,能形成沿模头均匀分布的基本均匀的聚合物流。目前优选模头采用了本领域公知的一种“衣架”型结构。一种典型线性衣架型模头可以从Extrusion Dies,Inc.和Cloereu Die Corp.购得,尽管如本领域技术人员所知,也可以使用其它模头和结构,使基本均匀的聚合物流能沿模头均匀分布。使用挤出机和线性模头以及引出设备,能从熔融的聚乙烯制成连续的片。要注意必须小心地控制聚合物送入模头和在压力下通过模头挤出的温度。这个温度应保持低于交联剂的分解温度,但又要足够高,即至少是聚合物的熔融温度,这样才能使组合物流动并形成片状材料。当向模头送入聚合物时,优选将聚合物温度保持在设定平均值的上下约5℃的范围内,并且当聚合物通过模头时,优选将聚合物的温度保持在设定平均值的上下约5℃的范围内。通过调整模头的间隙或通过调整使薄膜牵伸的引出辊的速度,能够获得各种厚度的熔融薄膜。也可以将上述调整手段结合使用。
形成薄膜后,可以立刻进行辐射交联,然后卷起薄膜。或者,可以将未交联的薄膜卷起,然后再解卷进行辐射交联。
在下表中,列出了对由不同材料平挤-共挤出的三层薄膜(A)/(B)/(A)的数据。共挤出时,对(B)使用了一英寸Killoin挤出机,对(A)使用了3/4英寸Brabender挤出机以及一种(A)/(B)/(A)供料头和8英寸宽模头。层厚度比是约15%∶70%∶15%。挤出温度列在表1中。
表1.挤出机各段的温度(℃)
实施例号 | 皮层/芯层/皮层 | Brabender挤出机段(聚合物A) | Killion挤出机段(聚合物B) | ||||||||
A/B/A | 1 | 2 | 3 | 模头接套 | 1 | 2 | 3 | 模头接套 | 供料区 | 冲模头 | |
1 | FEP/LDPE/FEP | 260 | 290 | 300 | 300 | 170 | 250 | 250 | 250 | 290 | 270 |
2 | FEP/EPDM/FEP | 260 | 290 | 300 | 300 | 170 | 250 | 250 | 250 | 290 | 270 |
3 | ECTFE/LDPE/ECTFE | 245 | 280 | 270 | 265 | 160 | 210 | 215 | 230 | 250 | 240 |
4 | ECTFE/EPDM/ECTFE | 245 | 280 | 270 | 265 | 170 | 290 | 300 | 250 | 250 | 240 |
5 | THV/LDPE/THV | 220 | 270 | 260 | 260 | 160 | 230 | 230 | 260 | 280 | 230 |
6 | THV/EPDM/THV | 220 | 270 | 260 | 260 | 160 | 240 | 285 | 280 | 280 | 220 |
7 | 共聚聚酯/LDPE/共聚聚酯 | 190 | 255 | 245 | 245 | 170 | 230 | 240 | 245 | 250 | 260 |
8 | 共聚聚酯/EPDM/共聚聚酯 | 190 | 255 | 245 | 245 | 170 | 230 | 240 | 245 | 250 | 260 |
用由Equistar制造的通用级为NA353000的LDPE作为奇数实施例样品的芯层。在偶数实施例样品中,用由DuPont Dow Elastomers L.L.C.制造的EPDM Nordel4920作为芯层。用三种氟聚合物和一种共聚聚酯作为多层薄膜中的皮层:
●由Daikin提供的FEP NP-12X
●由Ausimont提供的ECTFE Halar 300 LC
●由Dyneon提供的THV 500 G
●由DSM提供的共聚聚酯热塑性弹性体Arnitel EM 740
从挤出的薄膜上剪下6×10英寸的样品,用紫外或电子束进行处理,使聚合物层相互交联。用H-plus型紫外灯泡(由Fusion-UV Systems,Inc.制造)在300W/in功率50′/分的传动速度进行紫外处理。为了增加紫外照射,样品的每面都用紫外光照射32次。使样品通过175千伏加速电压下的处理机一次进行电子束处理。对所有处理样品的电子束辐射剂量都是12兆拉德。用T剥离测试方法测量层分离的力,对层间粘合性进行评价。从薄膜样品上切下1″宽的带状样品;两面各敷以遮蔽胶带,拉开一层皮层开始分层。用校准的砝码测定静态剥离力;最小重量是2.5克。对未处理的,紫外处理的或电子束处理的样品的层间粘合性数据列在表2中。
表2.多层体薄膜的层间静态T-剥离力(g/in)
实施例号 | 皮层/芯层/皮层 | 未处理的 | 紫外-32次300W/in-50′/分 | 电子束12兆拉德 |
1 | FEP/LDPE/FEP | <2.5克 | 4克 | 42克 |
2 | FEP/EPDM/FEP | <2.5 | >200,断裂 | 70 |
3 | ECTFE/LDPE/ECTFE | 8 | 150 | 40 |
4 | ECTFE/EPDM/ECTFE | 40 | >500 | 80 |
5 | THV/LDPE/THV | <2.5 | 4 | 75 |
6 | THV/EPDM/THV | 4 | 15 | 断裂 |
7 | Arnitel/LDPE/Arnitel | 12 | 7 | 22 |
8 | Arnitel/EPDM/Arnitel | 180 | >500 | 220 |
从表中可见,大多数未处理的薄膜样品的层间粘合性都很差。同时,在实施例4和8中,共挤出层间的相互作用甚至在处理前就很大。剥离力取决于层间粘合性和基片材料的机械性能,因为T-剥离同时有薄膜样品弯曲和拉伸。因此,对比只能在处理过的和未处理过的相同材料上进行。剥离力增大约一个数量级或更多表示层间粘合性显著增加。在某些样品的分层中,不使皮层断裂是不可能的(比如实施例6中用电子束处理的薄膜),其粘合力高于内聚力。
EPDM含有不饱和化学键,能被紫外线交联,而LDPE是不能被紫外线交联的。因此,在实施例1,5和7中,LDPE被用做芯层,紫外处理不会提高层间粘合性。有关EPDM的所有实施例都表现出紫外处理后剥离力提高。EPDM和LDPE都能被电子束交联,因此所有电子束处理的样品都表现出更高的层间粘合性。
表2中的两个实施例与其它实施例有所不同。在实施例3中,LDPE和ECTFE的强相互作用意外地通过紫外处理而获得。显然,ECTFE中的化学键被紫外光激活。在实施例8中,共挤出层间的大的相互作用甚至在处理前就能观察到。而且,紫外处理的确提高了实施例8样品中的层间粘合性。
从实施例中可以看出,粘合性提高从略微增加至显著增加有所不同。在此处列出的所有聚合物中,FEP是最难与其它聚合物键合的。选择FEP/EPDM的组合是优选的,因为这个组合表明在相互交联后能获得增加最大的相互粘合性。
虽然已通过优选实施例对本发明进行说明,但要理解在阅读了本说明书后各种改进对本领域技术人员而言都是显而易见的。因此,此处公开的发明包括这些在所附的权利要求书范围内的改进。
Claims (18)
1.一种相互交联多层聚合物制品,其包括:
(A)至少一种聚合物层,包含选自FEP,PFA,ETFE,ECTFE,PCTFE,PVDF,THV和其共混料和/或合金的氟聚合物,与之接触的是
(B)至少一种基本上由EPDM组成的可交联的聚合物层,其中,(A)和(B)是彼此不相容的,而且(A)和(B)通过相互交联固定在一起。
2.如权利要求1所述的制品,其中,聚合物层(A)是可交联的聚合物。
3.如权利要求1所述的制品,其中,氟聚合物是FEP。
4.如权利要求1所述的制品,其中该多层制品是由共挤出,共层压或挤出-层压而制成的。
5.如权利要求4所述的制品,其特征在于该共挤出形成薄膜或片材。
6.如权利要求4所述的制品,其特征在于该共挤出形成软管或型材。
7.如权利要求1所述的制品,其中该多层制品是由共模塑而制成的。
8.如权利要求7所述的制品,其中该共模塑包括注塑。
9.如权利要求7所述的制品,其中该共模塑包括共注塑,多材料模塑,多注射模塑,转压铸,压塑或吹塑。
10.如权利要求7所述的制品,其中该共模塑形成容器。
11.如权利要求1所述的制品,其中多层制品的相互交联使用了X射线。
12.如权利要求1所述的制品,其中多层制品的相互交联使用了γ射线。
13.如权利要求1所述的制品,其中多层制品的相互交联使用了紫外光或可见光。
14.如权利要求1所述的制品,其特征在于多层制品的相互交联使用了电子束。
15.如权利要求1所述的制品,其中多层制品的相互交联使用了包含过氧化物,胺和硅烷的化学交联剂。
16.如权利要求15所述的制品,其中该化学交联剂是一种有机过氧化物。
17.如权利要求1所述的制品,其中存在(A)和(B)各一层。
18.如权利要求1所述的制品,其中层(A)与一层(B)的各面邻接。
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US09/873,612 US6652943B2 (en) | 2001-06-04 | 2001-06-04 | Multilayer polymeric article with intercrosslinked polymer layers and method of making same |
US09/873,612 | 2001-06-04 |
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CN1325250C true CN1325250C (zh) | 2007-07-11 |
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CNB028140389A Expired - Fee Related CN1325250C (zh) | 2001-06-04 | 2002-06-04 | 具有交联聚合物层的多层聚合物制品及其制造方法 |
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US (2) | US6652943B2 (zh) |
EP (1) | EP1401654B1 (zh) |
JP (3) | JP2005517549A (zh) |
CN (1) | CN1325250C (zh) |
AU (1) | AU2002318176A1 (zh) |
DE (1) | DE60208795T2 (zh) |
TW (1) | TWI227195B (zh) |
WO (1) | WO2002098657A2 (zh) |
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CN1533329A (zh) | 2004-09-29 |
US6652943B2 (en) | 2003-11-25 |
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TWI227195B (en) | 2005-02-01 |
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WO2002098657A3 (en) | 2003-04-24 |
WO2002098657A2 (en) | 2002-12-12 |
JP2005517549A (ja) | 2005-06-16 |
JP2012245790A (ja) | 2012-12-13 |
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