CN114575165A - 一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法 - Google Patents

一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法 Download PDF

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CN114575165A
CN114575165A CN202210219554.5A CN202210219554A CN114575165A CN 114575165 A CN114575165 A CN 114575165A CN 202210219554 A CN202210219554 A CN 202210219554A CN 114575165 A CN114575165 A CN 114575165A
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glass fiber
polytetrafluoroethylene
composite material
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fiber
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王健
王晓连
吴闯
王春霞
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Jiangsu Bocheng New Technology Material Co ltd
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Abstract

本发明涉及复合材料技术领域，本发明公开了一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，包括以下步骤；步骤(1)、纤维复合材料制备：步骤(2)、纤维复合材料预处理：步骤(3)、将预处理好的纤维复合材料通过绞织机进行纺纱，形成经纱层和纬纱层，并制备成玻纤布；步骤(4)、将聚偏氟乙烯和硅烷偶联剂溶于DMF，完全溶解后均匀涂覆到玻纤布上，自然晾干后进行热压处理。本发明制备的聚四氟乙烯玻璃纤维布可增强抗拉伸性能，通过改良了聚四氟乙烯复合材料中的填料，大大提高了材料的拉伸强度，并一定程度的降低了最大收缩率和相对伸长率，且大大提高了聚四氟乙烯玻璃纤维布的耐折叠性和柔韧性，满足目前的材料性能需求。

Description

一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法
技术领域
本发明涉及复合材料技术领域，具体为一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法。
背景技术
聚四氟乙烯(PTFE)，以碳原子为骨架，氟原子对称而均匀地分布在它的周围，构成严密的屏障，使它具有非常宝贵的综合物理机械性能。聚四氟乙烯对强酸、强碱、强氧化剂有很高的抗蚀性，即使温度较高，也不会发生作用，其耐腐蚀性能甚至超过玻璃、陶瓷、不锈钢以至金、铂，所以，素有“塑料王”之称。聚四氟乙烯因其具有一系列优异的综合性能，宽广的耐高低温(-180～260℃)，高度的化学稳定性，卓越的电绝缘性，理想的耐腐蚀性，异常的自润滑性，长期的耐候性和适中的机械强度等，在化工、石油、机械、矿山、冶金、电子、医药、建筑、交通运输、轻纺、食品等各个行业中广泛运用，并已成为尖端科学和现代工业不可缺少的重要材料之一，也是目前材料学中研究的热点之一；
聚四氟乙烯玻璃纤维布是以悬浮聚四氟乙烯(俗称塑料王)乳液为原料，浸渍高性能玻璃纤维布而成的纤维布，是一种高性能，多用途的复合材料新产品，可用于防腐包覆、内衬及衬垫、防粘运输带、高频覆铜板、建筑膜材、绝缘材料、微波干燥输送带、柔性补偿器、摩擦材料等；
但是聚四氟乙烯玻璃纤维布也存在一些不足之处，如：强度较小、柔性差、磨损率高、在外力作用下有较大的粘弹性变形和导热性差等，这些缺点限制了聚四氟乙烯玻璃纤维布在实际生产生活中的应用，为了提高聚四氟乙烯玻璃纤维布的性能，应对聚四氟乙烯玻璃纤维布进行适当增强改性，鉴于此，提出一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法。
发明内容
本发明的目的在于提供一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，以解决上述背景技术中提出聚四氟乙烯玻璃纤维布强度较小、柔性差、磨损率高、在外力作用下有较大的粘弹性变形和导热性差的问题。
为实现上述目的，本发明提供如下技术方案：一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，包括以下步骤；
步骤(1)、纤维复合材料制备：
A1、将玻璃纤维、聚丙烯纤维、马来酸酐纤维和聚四氟乙烯纤维在高速混合机中搅拌均匀得到混合纤维；
A2、将混合纤维投入同向双螺杆挤出机中，经熔融挤出、造粒，制备出纤维复合材料；
步骤(2)、纤维复合材料预处理：
B1、先将纤维复合材料浸入甲醇中浸泡洗涤，进行干燥，而后浸入一定比例的甲醇/硅烷偶联剂溶剂中，40～45℃经1.5～2h的偶联反应，自然晾干后，在120～130℃环境中干燥30～40min；
B2、将上述干燥后的纤维复合材料，与聚四氟乙烯乳液浸渍30～45min，表面经滚压除去气泡，晾干；
B3、经鼓风烘箱梯度烘焙，在120℃的环境下，每分钟升高1～1.5℃干燥30min，然后在炉中380～400℃烧结30～35min，冷却后取出；
步骤(3)、将预处理好的纤维复合材料通过绞织机进行纺纱，形成经纱层和纬纱层，并制备成玻纤布；
步骤(4)、将聚偏氟乙烯和硅烷偶联剂溶于DMF，完全溶解后均匀涂覆到玻纤布上，自然晾干后进行热压处理。
优选的，步骤(1)，A1中，玻璃纤维、聚丙烯纤维、马来酸酐纤维和聚四氟乙烯纤维质量份数为：玻璃纤维100～120份、聚丙烯纤维20～30份、马来酸酐纤维15～20份和聚四氟乙烯纤维10～15份。
优选的，步骤(1)，A2中，挤出机挤出温度230～260℃，螺杆转速350～380r/min，真空度-0.06～-0.08MPa。
优选的，步骤(2)，B1中，对纤维复合材料水洗多次，并在100～120℃的环境下干燥。
优选的，步骤(2)，B2中，聚四氟乙烯乳液需预搅拌35～40min。
优选的，步骤(4)中，聚偏氟乙烯和硅烷偶联剂的质量比为9∶1。
优选的，步骤(4)中，热压处理的具体步骤为：
S1、将PVDF溶于DMF和丙酮的溶液中，配制成浓度为12wt％的纺丝液；
S2、通过调整纺丝时间控制玻纤布上的复合隔膜厚度在150μm以下；
S3、在真空70～75℃真空干燥10～12h除去剩余的溶剂，将玻纤布至于两块平板间，在0.01～0.02MPa、140～150℃环境下热压处理1.5～2h后，取出室温自然冷却。
优选的，所述DMF和丙酮的体积比8:2。
本发明提出的一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，有益效果在于：本发明制备的聚四氟乙烯玻璃纤维布可增强抗拉伸性能，通过改良了聚四氟乙烯复合材料中的填料，大大提高了材料的拉伸强度，并一定程度的降低了最大收缩率和相对伸长率，且大大提高了聚四氟乙烯玻璃纤维布的耐折叠性和柔韧性，满足目前的材料性能需求。
具体实施方式
下面将结合本发明的实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1、本发明提供一种技术方案：一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，包括以下步骤；
步骤(1)、纤维复合材料制备：
A1、将玻璃纤维100份、聚丙烯纤维20份、马来酸酐纤维15份和聚四氟乙烯纤维10份在高速混合机中搅拌均匀得到混合纤维；
A2、将混合纤维投入同向双螺杆挤出机中，经熔融挤出、造粒，制备出纤维复合材料，挤出机挤出温度230℃，螺杆转速350r/min，真空度～0.06MPa；
步骤(2)、纤维复合材料预处理：
B1、先将纤维复合材料浸入甲醇中浸泡洗涤，对纤维复合材料水洗多次，并在100℃的环境下干燥，而后浸入一定比例的甲醇/硅烷偶联剂溶剂中，40℃经1.5h的偶联反应，自然晾干后，在120℃环境中干燥30min；
B2、将上述干燥后的纤维复合材料，与聚四氟乙烯乳液浸渍30min，，聚四氟乙烯乳液需预搅拌35min，表面经滚压除去气泡，晾干；
B3、经鼓风烘箱梯度烘焙，在120℃的环境下，每分钟升高1℃干燥30min，然后在炉中380℃烧结30min，冷却后取出；
步骤(3)、将预处理好的纤维复合材料通过绞织机进行纺纱，形成经纱层和纬纱层，并制备成玻纤布；
步骤(4)、将聚偏氟乙烯和硅烷偶联剂溶于DMF，聚偏氟乙烯和硅烷偶联剂的质量比为9∶1，完全溶解后均匀涂覆到玻纤布上，自然晾干后进行热压处理；
热压处理的具体步骤为：
S1、将PVDF溶于DMF和丙酮的溶液中，DMF和丙酮的体积比8:2，配制成浓度为12wt％的纺丝液，电压20kv，距离18cm，湿度35％％，温度45℃；
S2、通过调整纺丝时间控制玻纤布上的复合隔膜厚度在150μm以下；
S3、在真空70℃真空干燥10h除去剩余的溶剂，将玻纤布至于两块平板间，在0.01MPa、140℃环境下热压处理1.5h后，取出室温自然冷却。
实施例2、本发明提供另一种技术方案：一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，包括以下步骤；
步骤(1)、纤维复合材料制备：
A1、将玻璃纤维120份、聚丙烯纤维30份、马来酸酐纤维20份和聚四氟乙烯纤维15份在高速混合机中搅拌均匀得到混合纤维；
A2、将混合纤维投入同向双螺杆挤出机中，经熔融挤出、造粒，制备出纤维复合材料，挤出机挤出温度260℃，螺杆转速380r/min，真空度-0.08MPa；
步骤(2)、纤维复合材料预处理：
B1、先将纤维复合材料浸入甲醇中浸泡洗涤，对纤维复合材料水洗多次，并在1120℃的环境下干燥，而后浸入一定比例的甲醇/硅烷偶联剂溶剂中，45℃经2h的偶联反应，自然晾干后，在130℃环境中干燥40min；
B2、将上述干燥后的纤维复合材料，与聚四氟乙烯乳液浸渍45min，，聚四氟乙烯乳液需预搅拌40min，表面经滚压除去气泡，晾干；
B3、经鼓风烘箱梯度烘焙，在120℃的环境下，每分钟升高1.5℃干燥30min，然后在炉中400℃烧结35min，冷却后取出；
步骤(3)、将预处理好的纤维复合材料通过绞织机进行纺纱，形成经纱层和纬纱层，并制备成玻纤布；
步骤(4)、将聚偏氟乙烯和硅烷偶联剂溶于DMF，聚偏氟乙烯和硅烷偶联剂的质量比为9∶1，完全溶解后均匀涂覆到玻纤布上，自然晾干后进行热压处理；
热压处理的具体步骤为：
S1、将PVDF溶于DMF和丙酮的溶液中，DMF和丙酮的体积比8:2，配制成浓度为12wt％的纺丝液，电压20kv，距离18cm，湿度45％，温度50℃；
S2、通过调整纺丝时间控制玻纤布上的复合隔膜厚度在150μm以下；
S3、在真空75℃真空干燥12h除去剩余的溶剂，将玻纤布至于两块平板间，在0.02MPa、150℃环境下热压处理2h后，取出室温自然冷却。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。

Claims (8)

1.一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，其特征在于：包括以下步骤；
步骤(1)、纤维复合材料制备：
A1、将玻璃纤维、聚丙烯纤维、马来酸酐纤维和聚四氟乙烯纤维在高速混合机中搅拌均匀得到混合纤维；
A2、将混合纤维投入同向双螺杆挤出机中，经熔融挤出、造粒，制备出纤维复合材料；
步骤(2)、纤维复合材料预处理：
B1、先将纤维复合材料浸入甲醇中浸泡洗涤，进行干燥，而后浸入一定比例的甲醇/硅烷偶联剂溶剂中，40～45℃经1.5～2h的偶联反应，自然晾干后，在120～130℃环境中干燥30～40min；
B2、将上述干燥后的纤维复合材料，与聚四氟乙烯乳液浸渍30～45min，表面经滚压除去气泡，晾干；
B3、经鼓风烘箱梯度烘焙，在120℃的环境下，每分钟升高1～1.5℃干燥30min，然后在炉中380～400℃烧结30～35min，冷却后取出；
步骤(3)、将预处理好的纤维复合材料通过绞织机进行纺纱，形成经纱层和纬纱层，并制备成玻纤布；
步骤(4)、将聚偏氟乙烯和硅烷偶联剂溶于DMF，完全溶解后均匀涂覆到玻纤布上，自然晾干后进行热压处理。
2.根据权利要求1所述的一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，其特征在于：步骤(1)，A1中，玻璃纤维、聚丙烯纤维、马来酸酐纤维和聚四氟乙烯纤维质量份数为：玻璃纤维100～120份、聚丙烯纤维20～30份、马来酸酐纤维15～20份和聚四氟乙烯纤维10～15份。
3.根据权利要求1所述的一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，其特征在于：步骤(1)，A2中，挤出机挤出温度230～260℃，螺杆转速350～380r/min，真空度-0.06～-0.08MPa。
4.根据权利要求1所述的一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，其特征在于：步骤(2)，B1中，对纤维复合材料水洗多次，并在100～120℃的环境下干燥。
5.根据权利要求1所述的一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，其特征在于：步骤(2)，B2中，聚四氟乙烯乳液需预搅拌35～40min。
6.根据权利要求1所述的一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，其特征在于：步骤(4)中，聚偏氟乙烯和硅烷偶联剂的质量比为9∶1。
7.根据权利要求1所述的一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，其特征在于：步骤(4)中，热压处理的具体步骤为：
S1、将PVDF溶于DMF和丙酮的溶液中，配制成浓度为12wt％的纺丝液；
S2、通过调整纺丝时间控制玻纤布上的复合隔膜厚度在150μm以下；
S3、在真空70～75℃真空干燥10～12h除去剩余的溶剂，将玻纤布至于两块平板间，在0.01～0.02MPa、140～150℃环境下热压处理1.5～2h后，取出室温自然冷却。
8.根据权利要求7所述的一种高柔性耐折叠聚四氟乙烯玻璃纤维材料的制备方法，其特征在于：所述DMF和丙酮的体积比8:2。
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