CN108049182A - 一种碳纤维增强树脂基复合材料阻燃表面膜及其制备方法 - Google Patents

一种碳纤维增强树脂基复合材料阻燃表面膜及其制备方法 Download PDF

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CN108049182A
CN108049182A CN201711038204.4A CN201711038204A CN108049182A CN 108049182 A CN108049182 A CN 108049182A CN 201711038204 A CN201711038204 A CN 201711038204A CN 108049182 A CN108049182 A CN 108049182A
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retardant
carbon fiber
composite material
epoxy resin
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李志涛
单瑞俊
孙永锋
朱珊珊
雷攀
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Jiangsu Hengshen Co Ltd
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Abstract

本发明公开一种碳纤维增强树脂基复合材料阻燃表面膜以及制备方法，表面膜材料由如下重量份的原料组成：60‑100份环氧树脂，15‑25份增韧剂，4‑8份固化剂，2‑4份促进剂，40‑0份的阻燃剂以及载体，其制备方法包括(1)称量，(2)制备树脂混合物，(3)共混出料，(4)压延成膜。本表面膜不仅能够提高制件表观质量，同时解决了普通环氧树脂体系无法满足EN45545‑2阻燃标准的问题。

Description

一种碳纤维增强树脂基复合材料阻燃表面膜及其制备方法
技术领域
本发明涉及一种用于碳纤维增强环氧树脂基复合材料的阻燃表面膜及其制备方法，属于纤维技术领域。
背景技术
随着国家大力提倡节能减排，各个领域都大力的投入和研发能够节能减排的材料及方法，轨道交通领域也不例外。众所周知，碳纤维增强树脂基复合材料作为高强高模材料的典型代表，由于其质量轻于铝合金，同时力学强度却不低于铝合金，而使其成为了“节能减排”旗帜下的宠儿，被广泛应用于航空航天等领域，但若想将碳纤维增强树脂基复合材料很好的引入轨道交通领域来节能减排，绕不开的问题就是替代铝合金的碳纤维增强树脂基复合材料的阻燃性能，由于碳纤维增强树脂基复合材料的连续相大多都是环氧树脂，它的阻燃等级不高，需要对其进行改性，以满足阻燃使用要求。但目前这种阻燃改性大多停留在本体添加型，很难在不影响板材力学性能的前提下，满足EN45545-2的阻燃标准，因此急需寻找一种高效阻燃方法来提高碳纤维增强环氧树脂基复合材料的阻燃级别，同时对最终制件板材的力学性能基本不产生影响。
发明内容
为了解决上述问题，本发明提供了一种用于碳纤维增强环氧树脂基复合材料的阻燃表面膜及其制备方法，它不仅能够提高制件表观质量，同时解决了普通环氧树脂体系无法满足EN45545-2阻燃标准的问题。
为了达到上述目的，本发明是通过以下技术方案实现的：
本发明是一种碳纤维增强树脂基复合材料阻燃表面膜，表面膜材料由如下重量份的原料组成：60-100份环氧树脂，15-25份增韧剂，4-8份固化剂，2-4份促进剂，40-0份的阻燃剂以及载体。
本发明的进一步改进在于：环氧树脂由低粘度双酚A型环氧树脂、中等粘度双酚A型环氧树脂、酚醛环氧树脂以及多官能团环氧树脂组成。
本发明的进一步改进在于：增韧剂由聚砜、聚醚砜、聚芳醚酮、端羟基丁腈橡胶、端羧基丁腈橡胶中的一种或多种组成。
本发明的进一步改进在于：固化剂由双氰胺、4，4’-二氨基二苯砜的一种或者两种组成。
本发明的进一步改进在于：促进剂由有机脲类，硫脲类，咪唑类化合物或者路易斯酸类中的一种或多种组成。
本发明的进一步改进在于：阻燃剂由添加型阻燃剂磷酸三苯酯、甲苯基磷酸二苯酯、季戊四醇、氢氧化铝、三聚氰胺磷酸酯、聚磷酸铵、硼酸锌中的一种或者多种组成。
本发明的进一步改进在于：载体为聚酯毡或玻纤毡。
本发明是一种碳纤维增强树脂基复合材料阻燃表面膜的制备方法，制备方法包括如下步骤：
(1)称量：按照重量份数称取60-100份环氧树脂，15-25份增韧剂，4-8 份固化剂，2-4份促进剂和40-70份的阻燃剂；
(2)制备树脂混合物：将步骤(1)中称取的环氧树脂按质量分为3 份，第一份与增韧剂热熔制备成增韧浓缩液或糊，第二份与阻燃剂采用三辊碾磨机进行研磨共混做成阻燃剂糊，第三份与固化剂及促进剂采用Speed Mixer 混合成为固化剂糊；
(3)共混出料：将步骤(2)中的增韧浓缩液或糊与阻燃剂糊在75℃反应釜中搅拌1h至体系均匀，将釜温降低到60℃以下，加入步骤(2)的固化剂糊，搅拌15min至体系均匀，出料；
(4)压延成膜：将步骤(3)中的出料通过涂膜机涂膜，然后与载体支撑物在含浸机上含浸，制成高效阻燃表面膜。
本发明的进一步改进在于：在所述步骤(4)中，涂膜温度75℃-85℃，含浸温度80℃-85℃，表面膜克重控制在140gsm-300gsm。
本发明的有益效果是：本发明的阻燃表面膜可以在碳纤维复材表面形成一层稳定且具有膨胀型的阻燃炭层，可以有效的阻燃，隔热，抑烟，满足EN45545-2 的阻燃标准。
具体实施方式
为了加深对本发明的理解，下面将结合实施例对本发明做进一步详细描述，该实施例仅用于解释本发明，并不对本发明的保护范围构成限定。
如实施例所示，本发明是一种碳纤维增强树脂基复合材料阻燃表面膜，表面膜材料由如下重量份的原料组成：60-100份环氧树脂，15-25份增韧剂，4-8份固化剂，2-4份促进剂，40-0份的阻燃剂以及载体；
其中：所述环氧树脂由低粘度双酚A型环氧树脂、中等粘度双酚A型环氧树脂、酚醛环氧树脂以及多官能团环氧树脂组成；
所述增韧剂由聚砜、聚醚砜、聚芳醚酮、端羟基丁腈橡胶、端羧基丁腈橡胶中的一种或多种组成；
固化剂由双氰胺、4，4’-二氨基二苯砜的一种或者两种组成；
促进剂由有机脲类，硫脲类，咪唑类化合物或者路易斯酸类中的一种或多种组成；
阻燃剂由添加型阻燃剂磷酸三苯酯、甲苯基磷酸二苯酯、季戊四醇、氢氧化铝、三聚氰胺磷酸酯、聚磷酸铵、硼酸锌中的一种或者多种组成；
所述载体为聚酯毡或玻纤毡。
本发明是一种碳纤维增强树脂基复合材料阻燃表面膜的制备方法，所述制备方法包括如下步骤：
(1)称量：按照重量份数称取60-100份环氧树脂，15-25份增韧剂，4-8 份固化剂，2-4份促进剂和40-70份的阻燃剂；
(2)制备树脂混合物：将步骤(1)中称取的环氧树脂按质量分为3 份，第一份与增韧剂热熔制备成增韧浓缩液或糊，第二份与阻燃剂采用三辊碾磨机进行研磨共混做成阻燃剂糊，第三份与固化剂及促进剂采用Speed Mixer 混合成为固化剂糊；
(3)共混出料：将步骤(2)中的增韧浓缩液或糊与阻燃剂糊在75℃反应釜中搅拌1h至体系均匀，将釜温降低到60℃以下，加入步骤(2)的固化剂糊，搅拌15min至体系均匀，出料；
(4)压延成膜：将步骤(3)中的出料通过涂膜机涂膜，然后与载体支撑物在含浸机上含浸，制成高效阻燃表面膜，所述涂膜温度75℃-85℃，含浸温度 80℃-85℃，表面膜克重控制在140gsm-300gsm。
实施例一
本发明是碳纤维增强树脂基复合材料阻燃表面膜，表面膜材料由如下重量份的原料组成：
环氧树脂：75份
聚醚砜：15份
阻燃剂：40份
固化剂及促进剂：6份
将称取的环氧树脂按质量分为3份，第一份与聚醚砜热熔制备成增韧浓缩液，第二份与阻燃剂采用三辊碾磨机进行研磨共混做成阻燃剂糊，第三份与固化剂及促进剂采用Speed Mixer混合成为固化剂糊；然后，将增韧浓缩液与阻燃剂糊在75℃反应釜中均匀搅拌1h后，将釜温降低到60℃以下，加入固化剂糊，均匀搅拌15min，出料；最后，将所出料通过涂膜机涂膜，然后在含浸机上与载体支撑物含浸制成高效阻燃表面膜。
将江苏恒神公司EM112-42％-HFW220T-1000预浸料单独热压罐固化后得到的板材和江苏恒神公司EM112-42％-HFW220T-1000碳纤维预浸料与阻燃表面膜进行共固化后得到的板材分别记为1#和2#，得到的表面膜基本性能及板材阻燃性能如下：
表1碳纤维复材表面膜固化后性能
表2无阻燃表面膜和有阻燃表面膜的碳纤维复合材料阻燃性能对比
其中：2#满足EN45545-2中HL1的阻燃标准(临界辐射能量CFE值>20，4min 时的烟密度Ds(4)值<600，4min时的烟毒性VOF4值<1200)
实施例二
本发明是一种用于碳纤维增强环氧树脂基复材的阻燃表面膜材料，按照质量分数称取：
环氧树脂：80份
端羧基丁腈橡胶：10份
阻燃剂：60份
固化剂及促进剂：7份
将称取的环氧树脂按质量分为3份，第一份与端羧基丁腈橡胶制备成增韧糊，第二份与阻燃剂采用三辊碾磨机进行研磨共混做成阻燃剂糊，第三份与固化剂及促进剂采用Speed Mixer混合成为固化剂糊；然后，将增韧糊与阻燃剂糊在75℃反应釜中均匀搅拌1h后，将釜温降低到60℃以下，加入固化剂糊，均匀搅拌15min，出料；最后，将所出料通过涂膜机涂膜，然后在含浸机上与载体支撑物含浸制成高效阻燃表面膜。
将江苏恒神公司EM112-42％-HFW200T-1000碳纤维预浸料与阻燃表面膜进行共固化后得到的板材记为3#，得到的表面膜基本性能及板材阻燃性能如下：
表3碳纤维复材表面膜固化后性能
表4无阻燃表面膜和有阻燃表面膜的碳纤维复合材料阻燃性能对比
其中：3#满足EN45545-2中HL2的阻燃标准(临界辐射能量CFE值>20，最大平均热释放速率MARHE值<90，4min时的烟密度Ds(4)值<300，4min时的烟毒性VOF4值<600) 。

Claims (9)

1.碳纤维增强树脂基复合材料阻燃表面膜，其特征在于：表面膜材料由如下重量份的原料组成：60-100份环氧树脂，15-25份增韧剂，4-8份固化剂，2-4份促进剂，40-0份的阻燃剂以及载体。
2.根据权利要求1所述碳纤维增强树脂基复合材料阻燃表面膜，其特征在于：所述环氧树脂由低粘度双酚A型环氧树脂、中等粘度双酚A型环氧树脂、酚醛环氧树脂以及多官能团环氧树脂组成。
3.根据权利要求1所述碳纤维增强树脂基复合材料阻燃表面膜，其特征在于：所述增韧剂由聚砜、聚醚砜、聚芳醚酮、端羟基丁腈橡胶、端羧基丁腈橡胶中的一种或多种组成。
4.根据权利要求1所述碳纤维增强树脂基复合材料阻燃表面膜，其特征在于：所述固化剂由双氰胺、4，4’-二氨基二苯砜中的一种或者两种组成。
5.根据权利要求1所述碳纤维增强树脂基复合材料阻燃表面膜，其特征在于：所述促进剂由有机脲类，硫脲类，咪唑类化合物或者路易斯酸类中的一种或多种组成。
6.根据权利要求1所述碳纤维增强树脂基复合材料阻燃表面膜，其特征在于：所述阻燃剂由添加型阻燃剂磷酸三苯酯、甲苯基磷酸二苯酯、季戊四醇、氢氧化铝、三聚氰胺磷酸酯、聚磷酸铵、硼酸锌中的一种或者多种组成。
7.根据权利要求1所述碳纤维增强树脂基复合材料阻燃表面膜，其特征在于：所述载体为聚酯毡或玻纤毡。
8.一种碳纤维增强树脂基复合材料阻燃表面膜的制备方法，其特征在于：所述制备方法包括如下步骤：
(1)称量：按照重量份数称取60-100份环氧树脂，15-25份增韧剂，4-8份固化剂，2-4份促进剂和40-70份的阻燃剂；
(2)制备树脂混合物：将步骤(1)中称取的环氧树脂按质量分为3份，第一份与增韧剂热熔制备成增韧浓缩液或糊，第二份与阻燃剂采用三辊碾磨机进行研磨共混做成阻燃剂糊，第三份与固化剂及促进剂采用Speed Mixer混合成为固化剂糊；
(3)共混出料：将步骤(2)中的增韧浓缩液或糊与阻燃剂糊在75℃反应釜中搅拌1h至体系均匀，将釜温降低到60℃以下，加入步骤(2)的固化剂糊，搅拌15min至体系均匀，出料；
(4)压延成膜：将步骤(3)中的出料通过涂膜机涂膜，然后与载体支撑物在含浸机上含浸，制成高效阻燃表面膜。
9.根据权利要求8所述碳纤维增强树脂基复合材料阻燃表面膜的制备方法，其特征在于：在所述步骤(4)中，所述涂膜温度75℃-85℃，含浸温度80℃-85℃，表面膜克重控制在140gsm-300gsm。
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110713697A (zh) * 2019-09-26 2020-01-21 江苏恒神股份有限公司 一种满足EN45545阻燃标准的OoA工艺用预浸料
CN114015200A (zh) * 2021-10-12 2022-02-08 许继集团有限公司 一种阻燃型环氧树脂绝缘材料及其制备方法与应用
CN116874988A (zh) * 2023-08-02 2023-10-13 常州天启新新科技有限公司 一种高阻燃中温固化环氧树脂预混物及其制备方法和应用

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110713697A (zh) * 2019-09-26 2020-01-21 江苏恒神股份有限公司 一种满足EN45545阻燃标准的OoA工艺用预浸料
CN110713697B (zh) * 2019-09-26 2022-05-31 江苏恒神股份有限公司 一种满足EN45545阻燃标准的OoA工艺用预浸料
CN114015200A (zh) * 2021-10-12 2022-02-08 许继集团有限公司 一种阻燃型环氧树脂绝缘材料及其制备方法与应用
CN116874988A (zh) * 2023-08-02 2023-10-13 常州天启新新科技有限公司 一种高阻燃中温固化环氧树脂预混物及其制备方法和应用
CN116874988B (zh) * 2023-08-02 2024-01-26 常州天启新新科技有限公司 一种高阻燃中温固化环氧树脂预混物及其制备方法和应用

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