CN1694984A - 芳族聚酰胺纸层压材料 - Google Patents

芳族聚酰胺纸层压材料 Download PDF

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CN1694984A
CN1694984A CNA2003801008091A CN200380100809A CN1694984A CN 1694984 A CN1694984 A CN 1694984A CN A2003801008091 A CNA2003801008091 A CN A2003801008091A CN 200380100809 A CN200380100809 A CN 200380100809A CN 1694984 A CN1694984 A CN 1694984A
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laminated material
aramid
paper
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mill
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CN100557109C (zh
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D·W·考卡
D·W·安德森
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EIDP Inc
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EI Du Pont de Nemours and Co
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Abstract

一种含有芳族聚酰胺非织造片材和聚酯树脂的层压材料，其总厚度是5－25密尔(0.13－0.64mm)，横向和纵向断裂伸长率至少40％，横向和纵向平均撕裂负荷1.5磅－力(6.7牛顿)以上。

Description

芳族聚酰胺纸层压材料
相关申请
本专利申请是2002年10月1日申请的序号10/261850的部分继续申请。
技术领域
本发明涉及一种有芳族聚酰胺纸和聚酯聚合物层的改进层压材料，优选地，涉及一种用一层聚酯聚合物分隔的两层芳族聚酰胺纸的层压材料。
背景技术
日本专利公开8-99389公开了采用压延和快速冷却形成层压材料的方法生产间-芳族聚酰胺纸和聚酯薄膜的层压片材。
英国专利1 486 372公开了一种与不同人造短纤维掺合物非织造纤维网粘着的金属层，这些纤维已压实并用成膜高分子聚合物粘结剂材料基料保持在一起。
Hendren等人的US5 320 892公开了一种用于蜂巢结构的层压材料，这些结构由含有聚(间苯二甲酰间苯二胺)纤条体的芯和聚(间苯二甲酰间苯二胺)絮状物和纤条体的外层构成。
Ootuka等人的US5 948 543公开了使用树脂粘结剂将对-芳族聚酰胺和间-芳族聚酰胺纤维粘结而制成芳族聚酰胺纤维非织造织物的层压基础材料。
由一层或多层芳族聚酰胺片材或纸和一层或多层聚酯聚合物制成的层压材料用于变压器，其中这种层压材料用作电介质绝缘材料。对这种层压材料内粘合性或这样一些层压材料的撕裂或断裂伸长率性能所作的任何改进都是人们所希望的。
发明内容
本发明涉及一种非织造芳族聚酰胺片材和聚酯树脂的层压材料，其总厚度是5-25密尔(0.13-0.64mm)，优选地5-20密尔(0.13-0.51mm)，横向和纵向断裂伸长率至少40％，横向和纵向平均撕裂负荷1.5磅-力(6.7牛顿)以上。该层压材料中树脂层厚度优选地大于该层压材料中任何单个非织造片材的厚度。优选的是非织造芳族聚酰胺片材为纸，并且其纸包括芳族聚酰胺、聚(间苯二甲酰间苯二胺)。在该层压材料中使用的优选聚酯树脂是聚(对苯二甲酸乙二酯)，可以含有其它的共聚单体或支化剂。
附图说明
图1是简化表示用于生产本发明层压材料的挤塑层压方法。
图2是表示本发明挤塑层压材料的初始撕裂强度比现有技术胶粘层压材料的改进。
具体实施方式
由芳族聚酰胺片材或纸和聚酯树脂薄膜制成的层压材料已用于变压器，其中这种层压材料用作电介质绝缘材料。希望这种绝缘层压材料具有特别适合于变压器生产要求的多个物理性能的组合。除绝缘性能外，这些性能包括其它的机械性能，它们包括初始撕裂强度(用断裂伸长率度量)和高抗撕裂蔓延性(用平均撕裂负荷度量)。这些性能尤其用于评价绝缘的层压材料，因为在生产变压器时有可能绝缘层压材料在装配时会受到损伤。
已发现，通过更换层压材料中使用的聚酯形态可以改进芳族聚酰胺绝缘层压材料的伸长率和撕裂性能。特别地，已发现，使用熔融聚酯树脂制成的层压材料比使用薄膜制成的层压材料具有改进的伸长率和撕裂性能。
典型地，现有电绝缘技术中使用的层压材料利用了聚酯薄膜。由于聚酯薄膜本身与芳族聚酰胺纸粘合不好(因为芳族聚酰胺纸表面光滑)，所以使用粘合剂将这些薄膜与芳族聚酰胺纸压实起来。首先把一种粘合剂涂布到这种薄膜上，然后在高温下把涂布的薄膜层压在芳族聚酰胺纸上，这样可将这些薄膜与芳族聚酰胺纸压实起来。人们认为，在这种层压材料中使用薄膜形式的聚酯制约了最后层压材料的伸长率和撕裂性能，还认为生产固体薄膜的典型方法可使聚酯层有一定结晶度和尺寸稳定性。认为这样会降低最后层压材料的弹性。
本发明层压材料优选地利用了芳族聚酰胺纸。在这里使用的术语纸用其标准意义，可以采用通常的制纸工艺和设备与方法生产纸。芳族聚酰胺纤维材料，例如纤条体和短纤维可以一起制成浆，形成一种混合物，它再转化成纸，例如使用Fourdrinier机或使用有成筛的手抄纸模具用手转化成纸。有关将芳族聚酰胺制成纸的方法可以参看Gross的US3 756 908和Hesler等人的US5 026 456。一般地，一旦制成芳族聚酰胺纸，就让其在两个具有高温度和压力的加热压延辊之间进行压延，这些辊可提高纸的结合强度。采用这种方式压延芳族聚酰胺纸也会降低纸的孔隙率，据认为这是造成层压材料中纸与聚合物层粘合不好的原因。
芳族聚酰胺纸的厚度不是关键，取决于最后使用的层压材料以及在最后层压材料中使用的芳族聚酰胺层数。尽管本发明可以使用两层，即一层芳族聚酰胺和一层聚合物层，优选地使用三层，即两层芳族聚酰胺纸和一层聚合物，但应该理解在最后物品中可能有的层数或其它材料没有任何上限。但是，该层压材料应具有如前面提出的总厚度上限。
在这里使用的术语芳族聚酰胺系指聚酰胺，其中至少85％酰胺(-CONH-)键是直接与两个芳族环压实。可以随芳族聚酰胺使用添加剂，可以将高达10重量％其它聚合物材料与这种芳族聚酰胺掺合，或可以使用用高达10重量％其它二胺取代该芳族聚酰胺二胺的共聚合物，或可以使用用高达10重量％其它二酰基氯取代该芳族聚酰胺二酰基氯的共聚合物。在实施本发明时，最常使用的芳族聚酰胺是：聚对苯二甲酰对苯二胺和聚(间苯二甲酰间苯二胺)，而聚(间苯二甲酰间苯二胺)是优选的芳族聚酰胺。
本发明中贴到这种芳族聚酰胺纸的优选聚酯树脂，即聚合物，是聚(对苯二甲酸乙二酯)(PET)。使用的PET可以包括多种共聚单体，其中包括二甘醇、环己烷二甲醇、聚(乙二醇)、戊二酸、壬二酸、癸二酸、间苯二甲酸等。除了这些共聚单体外，还可以使用支化剂，像苯均三酸、苯均四酸、三羟甲基丙烷、三羟甲基乙烷和季戊四醇。采用已知的聚合技术，使用对苯二甲酸或其低级烷基酯(例如对苯二甲酸二甲酯)和乙二醇或这些化合物的掺合物或混合物可以得到PET。在本发明中可以使用另外的聚酯树脂是聚萘二甲酸乙二酯(PEN)。可以采用已知的聚合技术使用2,6-萘二甲酸与乙二醇得到PEN。
曾采用不同的压延技术制得本发明中使用的优选压延芳族聚酰胺纸。在具有不同温度的加热辊之间采用单个压延步骤压延这些纸可以生产出这样一些纸，或采用首先在一个温度下压延片材的一个表面，然后在第二个温度下压延其相对面，这样也可以生产出这样一些纸。这种温差可直接造成芳族聚酰胺纸相对表面的孔隙率不同，这会转化成改进熔融树脂与芳族聚酰胺纸的粘合。温差至少20℃对获得本发明的优点是必不可少的，温差至少50℃至100℃，或更高是优选的。应理解到，加热辊的温度可以低于纸中芳族聚酰胺组分的玻璃化温度。但是，在一种优选的方式中，至少一个加热辊应是在芳族聚酰胺组分的玻璃化温度附近或高于这个温度。
并不试图进行限制时，一种生产本发明层压材料的方法是将熔融聚合物挤塑在两片压延芳族聚酰胺纸之间，接着加压与骤冷形成层压材料。可以采用许多方式将这种熔融树脂挤塑成芳族聚酰胺片材。例如该树脂可以挤塑成一种压延芳族聚酰胺片材，然后覆盖第二种芳族聚酰胺片材，再用压力机和层压辊进行层压。参看图1，在一种优选的方法中，这种熔融树脂从挤塑机加到缝口模头1。这种缝口模头如此取向，使熔融树脂片材以向下方式挤塑到一组水平层压辊2。两个芳族聚酰胺纸供料辊3将两个分开的芳族聚酰胺卷筒纸4提供给层压辊，卷筒纸和熔融树脂片材都汇集于层压辊辊隙，同时这种树脂定位于两个卷筒纸之间。这些辊将这种卷筒纸与树脂压实在一起；压实的层压材料再使用一组冷却辊5骤冷。或者，可以冷却水平层压辊2，以压实层压材料并使其骤冷。这种层压材料可以再切成这种应用所需要的适当粒度。
在本发明的另一个具体实施方案中，可以采用将这些不同聚合物成层置于两片芳族聚酰胺纸之间的方式挤塑这种熔融聚合物组合。例如，这种聚合物层可以由三层组成，例如依次是有第一特性粘度的PET聚合物层，有第二特性粘度的PET聚合物层，和有与第一层同样特性粘度的第三PET聚合物层。采用这种方式，可以使用对芳族聚酰胺片材有较大亲合性的PET聚合物，将对芳族聚酰胺片材有较低亲合性的PET聚合物加到这种层压材料中。
本发明层压材料的厚度是5-25密尔，例如5-20密尔，横向和纵向断裂伸长率是至少40％。另外，这些层压材料的横向和纵向平均撕裂负荷是1.5磅-力以上。优选的是这样的层压材料的树脂厚度大于该层压材料中任何一种非织造片材的厚度。
在下面的实施例中，所有的份和百分数都是以重量表示的，除非另外指出。根据ASTM D1004通过断裂伸长率测定了初始撕裂强度。根据ASTM D1938通过平均撕裂负荷测定了抗撕裂蔓延性。
实施例
这个实施例说明采用挤塑层压法制成的本发明层压材料性能，而对比为采用胶粘层压法制成的层压材料性能。挤塑层压材料按如下方法生产。由45％聚(间苯二甲酰间苯二胺)絮状物和55％聚(间苯二甲酰间苯二胺)纤条体组成的芳族聚酰胺纸，可以采用通常的Fourdrinier制纸方法和设备制得。这种纸然后在两个辊之间在800普兰(1400n/cm)与两个表面温度，特别地360℃和250℃的条件下压延，得到用于层压材料的不同压延纸。通过在两片纸之间挤塑层压聚(对苯二甲酸乙二酯)(PET)聚酯聚合物，可将聚合物贴合到芳族聚酰胺片材的较多孔表面上。将这些挤塑层压材料与电绝缘中使用的市售胶粘层压材料进行了比较，这些市售胶粘层压材料在两层NomexType416芳族聚酰胺纸之间有胶粘层压的聚酯薄膜。
得到的数据说明了采用挤塑层压法制得的本发明层压材料具有改进的初始撕裂强度，采用断裂伸长率测定的初始撕裂强度在横向和纵向都大于40％，而采用平均撕裂负荷测定的改进抗撕裂蔓延性大于1.5lb-力(6.7牛顿)。下面使用的EL代表挤塑层压，AL代表胶粘层压，MD代表纵向，而XD代表横向。图2说明了这些层压材料断裂伸长率的改进，线10和15是挤塑层压材料的MD和XD值，而线20和25是胶粘层压材料的MD和XD值。
层压材料类型              AL    EL    AL    EL    AL    EL
芳族聚酰胺片材厚度(密尔)  3     3     3     3     3     3
                  (mm)    0.076 0.076 0.076 0.076 0.076 0.076
聚合物厚度        (密尔)  5     5     7.5   7.5   10    10
                  (mm)    0.127 0.127 0.191 0.191 0.254 0.254
MD断裂伸长率      (％)    25    50    28    52    31    55
XD断裂伸长率      (％)    26    52    27    54    29    58
MD平均撕裂负荷    (lb-f)  1.1   1.9   1.2   2.2   1.9   3.5
                  (N)     4.9   8.5   5.3   9.8   8.5   15.6
XD平均撕裂负荷    (lb-f)  1.4   3.0   1.7   3.3   2.0   4.8
                  (N)     6.2   13.4  7.6   14.7  8.9   21.4
MD是纵向
XD是横向。

Claims (20)

1.一种层压材料，它含有芳族聚酰胺非织造片材和聚酯树脂，其总厚度是5-25密尔(0.13-0.64mm)，横向和纵向断裂伸长率至少40％，横向和纵向平均撕裂负荷1.5磅-力(6.7牛顿)以上。
2.根据权利要求1所述的层压材料，其中其厚度是5-20密尔(0.13-0.51mm)。
3.根据权利要求1所述的层压材料，该材料有一块以上的芳族聚酰胺非织造片材。
4.根据权利要求3所述的层压材料，其中该层压材料中聚酯树脂的厚度大于该层压材料中任何单个非织造片材的厚度。
5.根据权利要求1所述的层压材料，其中非织造芳族聚酰胺片材包括纸。
6.根据权利要求5所述的层压材料，其中芳族聚酰胺非织造片材是芳族聚酰胺纸，它含有芳族聚酰胺纤维和纤条体。
7.根据权利要求5所述的层压材料，其中芳族聚酰胺纸包括聚间苯二甲酰间苯二胺絮状物。
8.根据权利要求1所述的层压材料，其中聚酯树脂是聚对苯二甲酸乙二酯。
9.根据权利要求8所述的层压材料，其中聚对苯二甲酸乙二酯包含选自二甘醇、环己烷二甲醇、聚乙二醇、戊二酸、壬二酸、癸二酸、间苯二甲酸的共聚单体。
10.根据权利要求8所述的层压材料，其中聚对苯二甲酸乙二酯包含选自苯均三酸、苯均四酸、三羟甲基丙烷、三羟甲基乙烷和季戊四醇的支化剂。
11.根据权利要求1所述的层压材料，其中该聚酯树脂夹在两块非织造芳族聚酰胺纸片材之间。
12.根据权利要求11所述的层压材料，其中夹在两块非织造芳族聚酰胺纸片材之间的聚酯树脂包括一层树脂。
13.一种用于电绝缘的层压材料的生产方法，该方法包括：
a)将两块非织造芳族聚酰胺片材加到一对辊之间的辊隙中，
b)在前将熔融聚酯聚合物挤塑到两块芳族聚酰胺片材之间，或将熔融聚酯聚合物挤塑到一对辊之间的辊隙中，
c)把芳族聚酰胺片材与在这些辊之间的熔融聚合物压实，形成未骤冷的层压材料，以及
d)冷却未骤冷的层压材料。
14.根据权利要求13所述的方法，其中压实并骤冷层压材料，使其总厚度是5-25密尔(0.13-0.64mm)。
15.根据权利要求13所述的方法，其中让熔融的聚酯聚合物挤塑通过缝口模头。
16.一种用于电绝缘的层压材料的生产方法，该方法包括
a)将两块芳族聚酰胺片材加到一对辊之间的辊隙中，
b)在前将熔融聚酯聚合物挤塑到两块芳族聚酰胺片材之间，或将熔融聚酯聚合物挤塑到一对辊之间的辊隙中，
c)将芳族聚酰胺卷筒纸与在这些辊之间的熔融聚合物压实与骤冷，形成该层压材料。
17.根据权利要求16所述的方法，其中压实并骤冷层压材料，使其总厚度是5-25密尔(0.13-0.64mm)。
18.根据权利要求16所述的方法，其中让熔融的聚酯聚合物挤塑通过缝口模头。
19.一种有介电绝缘层压材料的变压器，该材料含有芳族聚酰胺非织造片材和聚酯树脂，其总厚度是5-25密尔(0.13-0.64mm)，横向和纵向断裂伸长率至少40％，横向和纵向平均撕裂负荷1.5磅-力(6.7牛顿)以上。
20.根据权利要求19所述的变压器，其中厚度是5-20密尔(0.13-0.51mm)。
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CN103477401B (zh) * 2011-04-18 2016-04-20 日东新兴有限公司 电绝缘用立体形状物及电绝缘性片材
CN104395079A (zh) * 2012-04-20 2015-03-04 杜邦帝人先进纸（日本）有限公司 芳族聚酰胺树脂薄膜层压体及其制备方法
US10173403B2 (en) 2012-04-20 2019-01-08 Dupont Teijin Advanced Papers (Japan), Ltd. Aramid resin film laminate and method for producing the same

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MXPA05003383A (es) 2005-06-22
US20060003659A1 (en) 2006-01-05
BR0314492A (pt) 2005-08-02
CN100557109C (zh) 2009-11-04
US20040072000A1 (en) 2004-04-15
KR20050055738A (ko) 2005-06-13
US20040071952A1 (en) 2004-04-15
JP2006501091A (ja) 2006-01-12
AU2003277302A1 (en) 2004-04-23
CA2500525A1 (en) 2004-04-15
WO2004031466A1 (en) 2004-04-15

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