CN1370203A - 新型聚酰亚胺共聚物和使用了该共聚物的金属层压品 - Google Patents

新型聚酰亚胺共聚物和使用了该共聚物的金属层压品 Download PDF

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CN1370203A
CN1370203A CN00811810A CN00811810A CN1370203A CN 1370203 A CN1370203 A CN 1370203A CN 00811810 A CN00811810 A CN 00811810A CN 00811810 A CN00811810 A CN 00811810A CN 1370203 A CN1370203 A CN 1370203A
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林正添
关根博行
A·L·鲁萨诺
L·B·埃奇纳
C·V·卡扎科瓦
Y·S·维戈德斯
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Abstract

一种新型聚酰亚胺共聚物,该共聚物是异亚丙基双(4－亚苯基氧基－4－邻苯二甲酸)二酐与6－氨基－2－(对氨基苯基)苯并咪唑的共聚物,或者是由异亚丙基双(4－亚苯基氧基－4－邻苯二甲酸)二酐和3,3′,4,4′－二苯甲酮四酸二酐形成的2种四酸二酐与6－氨基－2－(对氨基苯基)苯并咪唑的共聚物。该聚酰亚胺共聚物可被直接层压于金属箔上形成金属层压品,所形成的金属层压品具有完全令人满意的剥离强度。

Description

新型聚酰亚胺共聚物和使用了该共聚物的金属层压品
技术领域
本发明涉及新型聚酰亚胺共聚物和使用了该共聚物的金属层压品。更详细地说，涉及可有效用于与金属箔的粘接等的新型聚酰亚胺共聚物和使用了该共聚物的金属层压品。
背景技术
柔性(flexible)配线基板等的金属层压品历来是通过用环氧树脂、聚氨酯树脂等粘结剂将铜箔等金属箔和芳族聚酰亚胺薄膜粘接来制造的。但是，这种使用粘结剂制造的柔性配线基板存在由所用粘结剂引起的各种问题，如在焊接步骤中由于高温、用于高温环境而引起的粘结剂层剥落，在钻孔步骤中产生污点等。
为了从根本上解决这些问题，虽然可以不用粘结剂，将芳族聚酰亚胺直接层压在金属箔上，但是很多由此得到的金属层压品不能满足剥离强度。
发明的公开
本发明的目的是提供一种可以直接层压于金属箔上形成金属层压品的芳族聚酰亚胺，该聚酰亚胺可充分满足由此形成的金属层压品的剥离强度。
所述本发明的目的可通过新型聚酰亚胺共聚物来实现，该新型聚酰亚胺是异亚丙基双(4-亚苯基氧基-4-邻苯二甲酸)二酐与6-氨基-2-(对氨基苯基)苯并咪唑的共聚物，或者是由异亚丙基双(4-亚苯基氧基-4-邻苯二甲酸)二酐和3，3′，4，4′-二苯甲酮四酸二酐构成的2种四酸二酐与6-氨基-2-(对氨基苯基)苯并咪唑的共聚物。
作为本发明所用新型聚酰亚胺共聚物的四酸二酐，可以使用异亚丙基双(4-亚苯基氧基-4-邻苯二甲酸)二酐
Figure A0081181000041
或者上述(A)与3，3′，4，4′-二苯甲酮四酸二酐
Figure A0081181000042
的混合物。
当(A)成分与(B)成分并用时，可以按(B)成分在与(A)成分的混合物中占约90％摩尔或以下，优选约80％摩尔或以下的比例使用。如果按高于上述比例的量使用(B)成分，则(A)成分的量相应地变为约10％摩尔或以下，得到的聚酰亚胺共聚物在有机溶剂中的溶解性降低。
作为与上述四酸二酐反应的二胺，可以使用6-氨基-2-(对氨基苯基)苯并咪唑
Figure A0081181000043
虽然四酸二酐与二胺的反应可以在二甲基甲酰胺、二甲基乙酰胺、N-甲基-2-吡咯烷酮等非质子性极性溶剂中进行，但优选在间甲酚等极性溶剂中进行。实际上，在四酸二酐的极性溶剂溶液中，保持约0-60℃的温度，一边搅拌，一边滴加二胺的极性溶剂溶液，滴加结束后，在约0-60℃的温度、搅拌约0.5-5小时的条件下，使其发生反应。认为由这样的反应可生成聚酰胺酸，为了通过环化脱水反应使聚酰亚胺化反应结束，在反应的后半阶段，在搅拌条件下，在约100-250℃，优选150-200℃加热约2-8小时。另外，在四酸二酐溶液中，可以添加苯甲酸等作为催化剂用于反应。
将反应混合物注入甲醇等不溶性有机溶剂中，得到白色聚酰亚胺共聚物。所得共聚物具有约250-330℃的玻璃化转变点(Tg)和约0.2-3.0dl的比浓粘度ηred(N-甲基-2-吡咯烷酮)。当将该共聚物用于与金属箔的层压时，可以不必从上述反应混合物即聚酰亚胺共聚物溶液中分离聚酰亚胺共聚物，直接以溶液的状态用于与金属箔的层压。
通过四酸二酐(A)与二胺(C)的反应，可以得到具有下述重复单元的聚酰亚胺共聚物。
Figure A0081181000051
当将四酸二酐(A)与(B)一起使用时，通过与二胺(C)的反应，可以得到在上述重复单元的基础上还具有下述重复单元的聚酰亚胺共聚物。
Figure A0081181000052
用所述新型聚酰亚胺共聚物制造金属层压品时，用浇铸法等将聚酰亚胺共聚物溶液涂在以铜箔为代表的金属箔上，再在约60-200℃、优选约80-120℃以及约150-200℃的两个温度阶段分别加热约5-60分钟左右，形成约3-75μm膜厚的聚酰亚胺共聚物层，在共聚物层的一面形成层压了金属箔的金属层压体。在共聚物层的另一面再叠放金属箔，使其在加压下从加热至约150-400℃、优选约200-350℃温度的层压辊间通过，从而可以容易地接合复印所用的金属箔，可以形成贴有铜的材料等的两面层压品。
下面结合实施例对本发明进行说明。
实施例1
在配备有搅拌装置的容量1L的四颈烧瓶中，装入将异亚丙基双(4-亚苯基氧基-4-邻苯二甲酸)二酐26g(0.05摩尔)、3，3′，4，4′-二苯甲酮四酸二酐16.1g(0.05摩尔)以及苯甲酸12.2g溶解于间甲酚500ml中所形成的溶液，在将其保持在30℃或以下温度的同时，向其中加入6-氨基-2-(对氨基苯基)苯并咪唑22.4g(0.1摩尔)，在室温下搅拌1小时，得到聚酰胺酸溶液。将该溶液保持原样升温至200℃，在该温度下继续搅拌5小时。将反应混合物注入甲醇500ml中，将沉淀物过滤、干燥，得到61g聚酰亚胺共聚物。
所得聚酰亚胺共聚物的Tg为308℃，ηred(N-甲基-2-吡咯烷酮)为1.20dl，在二甲基甲酰胺、二甲基乙酰胺、N-甲基-2-吡咯烷酮、间甲酚中具有可溶性。
用浇铸法将上述聚酰亚胺共聚物的15％重量N-甲基-2-吡咯烷酮溶液涂在铜箔(厚18μm)上，将涂层在80℃加热30分钟，再在180℃加热30分钟，使铜箔上形成膜厚25μm的层压薄片，在260℃老化2小时，得到没有卷曲的单面层压体。再在该层压薄片上叠放铜箔(厚18μm)，使其在加压下从加热至330℃的层压辊间通过，进行压制，得到两面层压品。
按照JIS C-6481法测定所得铜箔/聚酰亚胺共聚物/铜箔层压品的剥离强度，在室温条件下为2.1Kg/cm，在150℃的热条件下为1.4Kg/cm。进而，在300℃、1分钟条件下观察其焊接耐热性，未观察到聚酰亚胺共聚物层有膨胀。实施例2
将实施例1中的3，3′，4，4′-二苯甲酮四酸二酐换成52g(0.1摩尔)异亚丙基双(4-亚苯基氧基-4-邻苯二甲酸)二酐，得到71g聚酰亚胺共聚物。
所得聚酰亚胺共聚物的Tg为275℃，ηred(N-甲基-2-吡咯烷酮)为1.20dl，在二甲基甲酰胺、二甲基乙酰胺、N-甲基-2-吡咯烷酮、苯酚、间甲酚中具有可溶性。
使用上述聚酰亚胺共聚物的15％重量N-甲基-2-吡咯烷酮溶液，与实施例1一样，制造铜箔(18μm)/聚酰亚胺共聚物(25μm)/铜箔(18μm)层压品，测定其剥离强度，在室温条件下为1.8Kg/cm，在300℃、1分钟的热条件下为1.6Kg/cm。进而，在焊接耐热性试验中未观察到膨胀。对照例
将实施例1中的异亚丙基(4-亚苯基氧基-4-邻苯二甲酸)二酐换成32.2g(0.1摩尔)3，3′，4，4′-二苯甲酮四酸二酐，得到50g聚酰亚胺共聚物。
所得聚酰亚胺共聚物的Tg为390℃，由于其在二甲基甲酰胺、二甲基乙酰胺、N-甲基-2-吡咯烷酮、间甲酚中不可溶，无法形成溶液，因而未能形成与铜箔的层压品。
工业上的可利用性
本发明的新型聚酰亚胺共聚物本身具有高粘接强度，即使不通过粘结剂层与金属箔粘接，也可以得到在剥离强度方面满足要求的金属层压品。而且，在焊接耐热性方面也表现优异，因而该金属层压品作为柔软的贴有金属箔的层压板，可以适当地用于无卷曲的柔性配线基板等。

Claims (11)

1.新型聚酰亚胺共聚物，该共聚物是异亚丙基双(4-亚苯基氧基-4-邻苯二甲酸)二酐与6-氨基-2-(对氨基苯基)苯并咪唑的共聚物。
2.新型聚酰亚胺共聚物，该共聚物是由异亚丙基双(4-亚苯基氧基-4-邻苯二甲酸)二酐和3，3′，4，4′-二苯甲酮四酸二酐形成的2种四酸二酐与6-氨基-2-(对氨基苯基)苯并咪唑的共聚物。
3.新型聚酰亚胺共聚物的制造方法，其特征在于使异亚丙基双(4-亚苯基氧基-4-邻苯二甲酸)二酐或者由其和3，3′，4，4′-二苯甲酮四酸二酐形成的2种四酸二酐与6-氨基-2-(对氨基苯基)苯并咪唑在极性溶剂中反应，形成聚酰胺酸之后，进行环化脱水反应。
4.权利要求3的新型聚酰亚胺共聚物的制造方法，其中所述极性溶剂为间甲酚。
5.权利要求3的新型聚酰亚胺共聚物的制造方法，其中所述反应是在苯甲酸催化剂的存在下进行的。
6.权利要求1的新型聚酰亚胺共聚物，其中所述共聚物被用于与金属箔的粘接。
7.权利要求2的新型聚酰亚胺共聚物，其中所述共聚物被用于与金属箔的粘接。
8.金属层压品，该层压品是在权利要求1的聚酰亚胺共聚物层的一面上层压了金属箔而形成的。
9.金属层压品，该层压品是在权利要求2的聚酰亚胺共聚物层的一面上层压了金属箔而形成的。
10.金属层压品，该层压品是在权利要求1的聚酰亚胺共聚物层的两面上层压了金属箔而形成的。
11.金属层压品，该层压品是在权利要求2的聚酰亚胺共聚物层的两面上层压了金属箔而形成的。
CNB008118108A 1999-10-18 2000-10-11 新型聚酰亚胺共聚物和使用了该共聚物的金属层压品 Expired - Fee Related CN1150277C (zh)

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CN1976977B (zh) * 2003-06-03 2010-05-26 沙伯基础创新塑料知识产权有限公司 苯并咪唑二胺-基聚醚酰亚胺组合物和制造它们的方法
CN102838745A (zh) * 2012-09-19 2012-12-26 中国科学院长春应用化学研究所 一种聚酰亚胺泡沫的制备方法
CN103992478A (zh) * 2014-05-29 2014-08-20 江苏尚莱特医药化工材料有限公司 耐高温的可溶可熔聚酰亚胺树脂及其制备方法
CN104130412A (zh) * 2014-07-11 2014-11-05 西南科技大学 一种n取代聚苯并咪唑酰亚胺及其制备方法
CN112679733A (zh) * 2020-12-11 2021-04-20 东华大学 一种含n取代双苯并咪唑聚酰亚胺和聚酰亚胺薄膜及其制备方法和应用

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JP3982296B2 (ja) * 2002-03-27 2007-09-26 日本メクトロン株式会社 新規ポリイミド共重合体
EP1533332B1 (en) * 2002-08-20 2011-05-18 Nippon Mektron, Limited Novel polyimide copolymer and metal laminate comprising the same
CN1305933C (zh) * 2004-12-07 2007-03-21 长春人造树脂厂股份有限公司 聚酰亚胺的制法
JP2010105258A (ja) * 2008-10-30 2010-05-13 Unimatec Co Ltd チューブ状ポリイミドベルトの製造法
JP7079076B2 (ja) 2016-08-10 2022-06-01 日鉄ケミカル＆マテリアル株式会社 ポリイミド前駆体及びそれから生じるポリイミド

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* Cited by examiner, † Cited by third party
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CN1976977B (zh) * 2003-06-03 2010-05-26 沙伯基础创新塑料知识产权有限公司 苯并咪唑二胺-基聚醚酰亚胺组合物和制造它们的方法
CN102838745A (zh) * 2012-09-19 2012-12-26 中国科学院长春应用化学研究所 一种聚酰亚胺泡沫的制备方法
CN102838745B (zh) * 2012-09-19 2014-11-26 中国科学院长春应用化学研究所 一种聚酰亚胺泡沫的制备方法
CN103992478A (zh) * 2014-05-29 2014-08-20 江苏尚莱特医药化工材料有限公司 耐高温的可溶可熔聚酰亚胺树脂及其制备方法
CN104130412A (zh) * 2014-07-11 2014-11-05 西南科技大学 一种n取代聚苯并咪唑酰亚胺及其制备方法
CN112679733A (zh) * 2020-12-11 2021-04-20 东华大学 一种含n取代双苯并咪唑聚酰亚胺和聚酰亚胺薄膜及其制备方法和应用

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KR100556069B1 (ko) 2006-03-07
CN1500821A (zh) 2004-06-02
EP1229081A1 (en) 2002-08-07
CN1150277C (zh) 2004-05-19
JP4433655B2 (ja) 2010-03-17
US6489436B1 (en) 2002-12-03
EP1229081A4 (en) 2002-12-04
DE60016963T2 (de) 2005-12-22
CN1219808C (zh) 2005-09-21
DE60016963D1 (de) 2005-01-27
EP1229081B1 (en) 2004-12-22
WO2001029136A1 (fr) 2001-04-26
KR20020013931A (ko) 2002-02-21
RU2238285C2 (ru) 2004-10-20

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