CN107344440B - 一种阻燃防火聚酰亚胺泡沫复合毡材料及其制备方法 - Google Patents
一种阻燃防火聚酰亚胺泡沫复合毡材料及其制备方法 Download PDFInfo
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Abstract
一种阻燃防火聚酰亚胺泡沫复合毡材料及其制备方法，其特征在于是由反射型阻燃复合结构和聚酰亚胺泡沫复合而成，聚酰亚胺泡沫位于两层反射型阻燃复合结构的中间层位置，其中反射型阻燃复合结构由玻璃纤维、铝箔、聚酰胺类薄膜、聚酯薄膜组成；本发明还提供了阻燃防火聚酰亚胺泡沫复合毡的制备防范，该复合毡具有阻燃防火的功能，同时具有一定的耐温性，复合毡A级不燃，导热系数为0.02～0.05W/(m·K)，厚度为0～25mm，容重为3～25Kg/m3；所述的泡沫复合材料中聚酰亚胺泡沫结构均匀，泡孔细腻。本发明的阻燃防火聚酰亚胺泡沫复合材料可长期耐温200℃，阻燃等级且聚酰亚胺泡沫中可含有不同的填充气体(CO2、N2、NH3)，主要用于航空航天、高铁、舰船及潜艇等保温领域。
Description
技术领域
本发明涉及耐高温技术领域，尤其涉及一种阻燃防火聚酰亚胺泡沫复合毡材料及其制备方法。
背景技术
随着社会的发展，工业的进步，人们对能源的需求不断增加，尤其是我国能源长期存在不足，能源紧张成为严重困扰国民经济发展的重大问题，这迫使工业各部门重新考虑能源的开发利用方式和节能的措施。目前用于保温隔热的主要材料是聚氨酯泡沫和酚醛泡沫。但聚氨酯泡沫不阻燃，且在燃烧时产生大量低落物和大量的烟雾，烟密度达到了80％以上；酚醛泡沫具有良好的阻燃性能，但是该泡沫没有强度，易粉化，且密度太高。而聚酰亚胺泡沫燃烧时没有滴落，其烟密度仅有8％。
聚酰亚胺是一种耐热性极好的聚合物，具有良好的力学、耐腐蚀和耐辐射性能，广泛应用于航空航天、军事等领域。泡沫的聚酰亚胺材料不仅保持了原数值优异的耐温、阻燃等性能，还具有突出的透波特性以及质量轻、柔性回弹性好、使用方便等综合性能，因此在军事装备上有着极其重要的用途。
聚酰亚胺分为硬质聚酰亚胺和软质聚酰亚胺，其中软质热塑性聚酰亚胺泡沫使用热塑性聚酰亚胺粉末在高温发泡而成，利用聚酰亚胺泡沫材料与其他材料制备形成复合结构，充分发挥材料和复合结构的性能优势。
US 5298531中公开的专利中，是采用生成预聚体，在再加入芳香族或脂肪族二胺，待反应完全后去除溶液中的小分子成粉末，通过高温使其放出水和甲醇等小分子的方法发泡，缺点是具体干燥复杂。
CN101402895A公开的一种新型耐高温聚酰亚胺泡沫的合成方法，其也是通过双酐酯化，于溶液中加入双胺的防范产生粉末预聚体，通过两步法产生聚酰亚胺泡沫塑料，但是得到的是硬质泡沫材料。
发明内容
本发明公开了一种阻燃防火聚酰亚胺泡沫复合材料及其制备方法，该方法阻燃防火聚酰亚胺泡沫复合毡材料，其结构是由反射型阻燃复合结构和聚酰亚胺泡沫复合而成，聚酰亚胺泡沫位于两层反射型阻燃复合结构的中间层位置，复合毡A级不燃，导热系数为0.02～0.05W/(m·K)，厚度为0～25mm，容重为3～25Kg/m3；
本发明同时还公开了不同填充气体的聚酰亚胺泡沫，通过反应原料的自身反应，产生不同的气体，进行发泡，得带不同填充气体的软质聚酰亚胺泡沫材料。
本发明采用在保证阻燃防火隔热材料具有较好阻燃性能的同时又能够满足良好的耐温性要求。聚酰亚胺泡沫材料主要是通过原料自身反应进行发泡，并辅助以催化剂，得到填充不同的气体的聚酰亚胺泡沫，所得到的聚酰亚胺泡沫材料与反射型复合结构进行复合，两者之间采用树脂材料进行粘结。所述阻燃防火聚酰亚胺泡沫复合毡材料阻燃性A级不燃，具有一定的耐温性。用于制造车辆、船舶、飞行器和火箭的构造材料、用于制造飞行器内部和外部零件、用于制造任何类型的绝缘材料、用于制造绝缘面板、管道和容器绝缘体、用于制造吸声材料、用于发动机舱、用于制造磨盘等，主要用于航空航天、高铁、舰船及潜艇等保温领域。
为了实现本发明的目的，采用如下技术方案：一种阻燃防火聚酰亚胺泡沫复合毡材料及其制备方法，结构中泡沫复合材料中聚酰亚胺泡沫结构均匀，泡孔细腻，复合材料导热系数为0.02～0.05W/(m·K)，厚度为0～25mm，容重为3～25Kg/m3。
本发明的阻燃防火聚酰亚胺泡沫复合毡材料，阻燃等级为A级不燃，且聚酰亚胺泡沫中填充不同的气体(CO2、N2、NH3)，其制备过程：采用热压法将玻璃纤维布和铝箔进行复合，形成铝箔复合玻璃纤维布，其特征在于热压温度在180～250℃，复合辊压力为0.4MPa～0.8MPa，玻璃纤维布和铝箔运转的线速度为10～20m/min；将得到的铝箔复合玻璃纤维布与聚酰胺类薄膜干式复合方法进行复合，每层通过粘结剂粘合一起，经热压辊压合并经冷却辊冷却，得到三层复合薄膜结构，其特征在于复合辊压力为0.4MPa～0.8MPa，铝箔复合玻璃纤维布和聚酰胺薄膜运转的线速度为15～25m/min，热压辊的温度为80～110℃，冷却辊的温度为30～50℃；将三层复合结构与聚酯薄膜进行复合，通过改性酚醛树脂或邻苯二甲酸酐环氧树脂粘结剂进行粘合，经热压辊压合并经冷却辊冷却，得到四层复合结构，复合辊压力为0.4～0.8MPa，三层复合结构和聚酯薄膜运转的线速度为15～25m/min，熟化温度为40～60℃，时间为1～3小时。
在极性溶剂DMAC中加入一种或两种以上二元酐或多元酸和多异氰酸酯等原材料，使其完全溶解，缓慢加热至80～130℃，极性溶剂与原料的配比为5∶1～1∶1；将得到的溶液温度降至30～60℃，加入催化剂所加催化剂含量为原料量的1/1000～1/500，预加热温度在100～250℃；温度降至室温状态下，开始自由发泡产生气体，生成聚酰亚胺泡沫材料，气体为CO2、N2、NH3中的一种；将得到的泡沫材料先在100～200℃中处理10～15min，然后在180～250℃中处理10～15min；将得到的薄膜结构与得到的泡沫材料进行复合，薄膜结构通过粘结剂与中间层泡沫结构复合在一起；将得到的成品置于常温下熟化30～45min，得到阻燃防火聚酰亚胺泡沫复合材料。
在上述所选材料中，玻璃纤维布面密度为100～200g/m2，铝箔厚度为0.1～8μm，聚酰胺类薄膜重量为15～20g/m2，聚酯类薄膜重量为15～21g/m2；聚酰亚胺泡沫厚度为0～20mm，容重为3～20Kg/m3，泡沫中含CO2、N2、NH3气体中的一种；聚酰亚胺泡沫复合材料的原料为二酸、二胺、二酐或四酸、多异氰酸酯、小分子羧酸、多聚甲醛、P，P’一氧双(苯磺酰肼)、偶氮二酰胺中的一种或多种；并在制备过程中添加了催化剂，催化剂为杂环胺、叔胺如三亚乙基二胺、二甲基羟乙胺、异喹啉，辛酸亚锡、辛酸铝、辛酸铁；粘结剂为改性酚醛树脂和邻苯二甲酸酐环氧树脂粘结剂中的一种。
具体实施方式
下面结合具体实施例，进一步阐明本发明，应理解这些实施例仅用于说明本发明而不用于限制本发明的范围，在阅读了本发明之后，本领域技术人员对本发明的各种等价形式的修改均落于本申请所附权利要求所限定。
实施例1
本发明提供一种阻燃防火聚酰亚胺泡沫复合毡材料，首先采用热压法将玻璃纤维布和铝箔进行复合，铝箔复合玻璃纤维布；添加粘结剂，将得到的反射型复合璃纤维布与聚酰胺类薄膜进行复合，得到三层复合薄膜结构，其特征在于通过干式复合的方式进行复合，每层通过粘结剂粘合一起，经热压辊压合并经冷却辊冷却；冷却后放入熟化室内，熟化温度为40℃，时间为15min；在极性溶剂DMAC中加入二元酐或四元酸，充分溶解后再加入多异氰酸酯，待两者完全溶解后，生成不稳定的中间体，氨基甲酸，此时加入催化剂杂环胺，并进行预加热处理；加热开始后开始发泡产生CO2气体，生成聚酰亚胺泡沫材料；预固化是在固化炉中150℃中固化10分钟，后固化是在高温炉中220℃中固化10min。将步骤(3)得到的薄膜结构与得到的中间层泡沫材料进行复合，薄膜结构通过粘结剂与中间层泡沫结构复合再一起；将得到的成品置于常温下熟化30min，得到阻燃防火聚酰亚胺泡沫复合材料。
阻燃防火聚酰亚胺泡沫复合毡材料的制备方法，包括以下步骤：
(1)采用热压法将玻璃纤维布布110g/m2和5μm铝箔进行复合，铝箔复合玻璃纤维布；
(2)将步骤(1)得到的铝箔复合玻璃纤维布与18g/m2聚酰亚胺薄膜进行复合，得到三层复合薄膜结构，其特征在于通过干式复合的方式进行复合，每层通过粘结剂粘合一起，经热压辊压合并经冷却辊冷却，热辊温度为200℃，冷却辊温度为50℃；
(3)与18g/m2的PET薄膜进行复合，通过改性酚醛树脂或邻苯二甲酸酐环氧树脂粘结剂进行粘合，经热压辊压合并经冷却辊冷却，得到四层复合结构，复合辊压力为0.6MPa，三层复合结构和聚酯薄膜运转的线速度为15m/min，熟化温度为60℃，时间为1小时；
(4)在200g极性溶剂DMAC中加入75g四元酸和40g多异氰酸酯材料，使其完全溶解，并缓慢加热至100℃；
(5)将上述得到的溶液温度降低至40℃，加入0.1g催化剂杂环胺；
(6)温度降至室温下，开始自由发泡15min，产生CO2气体，生成聚酰亚胺泡沫材料；
(7)将上述所得聚酰亚胺泡沫材料进行固化处理，预固化是在固化炉中150℃中固化10min，后固化是在高温炉中220℃中固化10min；
(8)将固化完成的聚酰亚胺泡沫材料与反射型复合结构通过粘结剂邻苯二甲酸酐环氧树脂复合在一起，常温下熟化30min，即可获得阻燃防火聚酰亚胺泡沫复合材料。
所得的阻燃防火聚酰亚胺泡沫复合材料A级不燃，容重为21Kg/m3，导热系数为0.021W/(m·K)，厚度为15mm，其中聚酰亚胺泡沫材料发泡均匀，泡孔细腻。
上述仅为本发明的具体实施方式，但本发明的设计构思并不局限于此，凡利用此构思对本发明进行非实质性的改动，均应属于侵犯本发明保护的范围的行为。但凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所作的任何形式的简单修改、等同变化与改型，仍属于本发明技术方案的保护范围。
Claims (1)
1.一种阻燃防火聚酰亚胺泡沫复合毡材料，其特征在于，复合毡结构是由反射型阻燃复合结构和聚酰亚胺泡沫复合而成，聚酰亚胺泡沫位于两层反射型阻燃复合结构的中间层位置，复合毡A级不燃，导热系数为0.02～0.05W/(m·K)，厚度为0～25mm，容重为3～25Kg/m3；其中反射型阻燃复合结构由玻璃纤维、铝箔、聚酰胺类薄膜、聚酯薄膜组成，玻璃纤维布面密度为100～200g/m2，铝箔厚度为0.1～8μm，聚酰胺类薄膜重量为12～20g/m2，聚酯类薄膜重量为13～21g/m2；聚酰亚胺泡沫厚度为0～20mm，容重为3～20Kg/m3，泡沫中含CO2、N2、NH3气体中的一种；其特征在于包括以下制备步骤：
(1)采用热压法通过聚醋酸乙烯乳液共聚物将玻璃纤维布和铝箔进行复合，形成铝箔复合玻璃纤维布，热压温度在180～250℃，复合辊压力为0.4MPa～0.8MPa，玻璃纤维布和铝箔运转的线速度为10～20m/min；
(2)将步骤(1)得到的铝箔复合玻璃纤维布与聚酰胺类薄膜干式复合方法进行复合，每层通过改性酚醛树脂或邻苯二甲酸酐环氧树脂粘结剂进行粘合，经热压辊压合并经冷却辊冷却，得到三层复合结构，复合辊压力为0.4～0.8MPa，铝箔复合玻璃纤维布和聚酰胺薄膜运转的线速度为15～25m/min，热压辊的温度为80～130℃，冷却辊的温度为30～50℃；
(3)将步骤(2)得到的三层复合结构与聚酯薄膜进行复合，通过改性酚醛树脂或邻苯二甲酸酐环氧树脂粘结剂进行粘合，经热压辊压合并经冷却辊冷却，得到四层复合结构，复合辊压力为0.4～0.8MPa，三层复合结构和聚酯薄膜运转的线速度为15～25m/min，熟化温度为40～60℃，时间为1～3小时；
(4)在极性溶剂DMAC中加入一种或两种以上二元酐或多元酸和多异氰酸酯原材料，使其完全溶解，缓慢加热至80～130℃，极性溶剂与原料的配比为1～5∶1，原料为多异氰酸酯；
(5)将步骤(4)中得到的溶液温度降低至30～60℃，加入催化剂，为杂环胺、叔胺、二甲基羟乙胺、异喹啉，辛酸亚锡、辛酸铝、辛酸铁中的一种，与原料的配比为1～2∶1000；
(6)将步骤(4)得到的溶液温度降至室温，开始自由发泡10～30min，产生CO2、N2、NH3气体中的一种，生成聚酰亚胺泡沫材料；
(7)将步骤(6)中得到的泡沫材料，在100～200℃中处理10～15min，后在180～250℃中处理10～15min；
(8)将步骤(3)得到的四层复合结构与步骤(7)得到的泡沫材料进行复合，通过改性酚醛树脂或邻苯二甲酸酐环氧树脂粘结剂将泡沫结构复合在中间层位置；
(9)将步骤(8)得到的成品置于常温下熟化30～45min，得到阻燃防火聚酰亚胺泡沫复合毡材料。
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