CN113308882A - 一种基于短纤维改性碳纤维的制备方法 - Google Patents
一种基于短纤维改性碳纤维的制备方法 Download PDFInfo
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Abstract
本发明公开了一种基于短纤维改性碳纤维的制备方法,包括:首先对碳纤维进行去剂处理,其次配置短纤维分散液,最后采用真空抽滤法抽滤短纤维分散液使其沉积在均匀铺放的碳纤维丝束表面,然后将沉积有短纤维分散液的碳纤维丝束翻转180°,再真空抽滤短纤维分散液使其沉积在均匀铺放的碳纤维丝束的另一表面,真空干燥得到短纤维改性碳纤维。本发明的制备方法开创了真空抽滤技术在具有圆周结构高性能纤维表面改性的应用,具有设备简单、反应条件温和、无毒、环保、低成本和高效的优点,制备的短纤维改性碳纤维使复合材料的界面粘结性能提高。
Description
技术领域
本发明属于材料的表面与界面改性应用技术领域,具体涉及一种基于短纤维改性碳纤维的制备方法。
背景技术
碳纤维增强树脂基复合材料由于其轻质高强、耐腐蚀和可设计性等优异特性被广泛用于航空航天、船舶、能源和体育休闲等领域。然而,碳纤维表面缺少活性官能团,惰性大,导致其与树脂的浸润性差,界面强度低,限制了碳纤维增强树脂基复合材料的广泛和深入应用。短纤维有天然短纤维和人工短纤维两种,天然短纤维包括多种植物短纤维和玄武岩短纤维,具有绿色环保和来源广泛等突出优点;人工短纤维包括短碳纤维、玻璃短纤维、芳纶短纤维、金属短纤维、聚苯并恶唑短纤维等,具有超高的力学强度和抗疲劳特性等。若将长短纤维相结合将有利于提高复合的界面粘结强度。然而,目前就短纤维改性碳纤维的报道并不多见,亟待深入研究。
发明内容
本发明的目的是提供一种具有操作简单、高效、绿色和成本低的基于短纤维改性碳纤维的制备方法。
为实现上述目的,本发明采用的技术方案如下:
(1)将碳纤维丝束在丙酮溶液中冷凝回流,然后用去离子水清洗干净并真空干燥;
(2)将短纤维分散在水或有机溶剂中,搅拌使其分散均匀,得到质量分数为0.01%~3%的短纤维分散液;
(3)将步骤(1)处理得到的碳纤维丝束均匀铺放在滤膜上,真空抽滤短纤维分散液使其沉积在均匀铺放的碳纤维丝束表面,然后将沉积有短纤维分散液的碳纤维丝束翻转180°,再真空抽滤短纤维分散液使其沉积在均匀铺放的碳纤维丝束另一表面,真空干燥后得到短纤维改性碳纤维。
所述步骤(1)的碳纤维为长碳纤维。
所述步骤(1)的冷凝回流温度为80~100℃,时间为12~48h。
所述步骤(2)的短纤维采用直径为500nm~20μm,长度为0.5~10mm的短碳纤维、玻璃短纤维、芳纶短纤维、玄武岩短纤维、聚酯短纤维、聚苯并恶唑短纤维及植物短纤维中的一种或两种以上混合物。
所述步骤(2)的有机溶剂为丙酮、乙醇、四氢呋喃、二甲基甲酰胺、二氯甲烷或二甲亚砜。
所述步骤(2)的搅拌采用转速为500~1000rpm/min的磁力搅拌,搅拌时间为30~120min。
所述步骤(3)真空抽滤短纤维分散液,抽滤短纤维分散液体积(ml):滤膜直径(cm)=(0.1~5):1。
所述步骤(1)和(3)的真空干燥采用真空干燥箱干燥,其温度为40~80℃,时间为2~5h。
与现有技术相比,本发明具有以下有益技术效果:
(1)采用真空抽滤法在圆周结构的碳纤维丝束表面实现短纤维的均匀沉积,开创了真空抽滤技术在具有圆周结构高性能纤维表面改性的应用。
(2)本发明的制备方法设备简单、反应条件温和、无毒、环保、低成本和高效。
(3)碳纤维表面的短纤维增加了纤维与树脂的机械咬合作用,提高了复合材料的界面粘结强度。
具体实施方式
下面结合具体实施例对本发明作进一步详细说明。
实施例1
(1)将长碳纤维丝束在80℃的丙酮溶液中冷凝回流48h,然后用去离子水清洗干净并在真空干燥箱中60℃真干燥3h;
(2)将直径为5~6μm、长度约为3mm的短碳纤维分散在丙酮中,500rpm/min磁力搅拌30min使其分散均匀,得到质量分数为0.01%的短碳纤维分散液;
(3)将步骤(1)处理得到的碳纤维丝束均匀铺放在滤膜上,按短碳纤维分散液体积(ml):滤膜直径(cm)=0.4:1真空抽滤短碳纤维分散液使其沉积在均匀铺放的碳纤维丝束表面,然后将沉积有短碳纤维分散液的碳纤维丝束翻转180°,再真空抽滤同样量的短碳纤维分散液使其沉积在均匀铺放的碳纤维丝束另一表面,在真空箱中60℃干燥3h后得到短碳纤维改性碳纤维。
实施例2
(1)将长碳纤维丝束在90℃的丙酮溶液中冷凝回流24h,然后用去离子水清洗干净并在真空干燥箱中60℃真干燥3h;
(2)将直径为500nm~2μm、长度约为0.5~2mm的聚酯短纤维分散在二甲基甲酰胺中,500rpm/min磁力搅拌40min使其分散均匀,得到质量分数为0.05%的聚酯短纤维分散液;
(3)将步骤(1)处理得到的碳纤维丝束均匀铺放在滤膜上,按聚酯短纤维分散液体积(ml):滤膜直径(cm)=2:1真空抽滤聚酯短纤维分散液使其沉积在均匀铺放的碳纤维丝束表面,然后将沉积有聚酯短纤维分散液的碳纤维丝束翻转180°,再真空抽滤同样量的的聚酯短纤维分散液使其沉积在均匀铺放的碳纤维丝束另一表面,在真空箱中60℃干燥3h后得到聚酯短纤维改性的碳纤维。
实施例3
(1)将长碳纤维丝束在100℃的丙酮溶液中冷凝回流12h,然后用去离子水清洗干净并在真空干燥箱中50℃真干燥4h;
(2)将直径为12~15μm、长度约为8~10mm的植物短纤维分散在水中,500rpm/min磁力搅拌50min使其分散均匀,得到质量分数为0.5%的植物短纤维分散液。
(3)将步骤(1)处理得到的碳纤维丝束均匀铺放在滤膜上,按植物短纤维分散液体积(ml):滤膜直径(cm)=1:1真空抽滤植物短纤维分散液使其沉积在均匀铺放的碳纤维丝束表面,然后将沉积有植物短纤维分散液的碳纤维丝束翻转180°,再真空抽滤同样量的植物短纤维分散液使其沉积在均匀铺放的碳纤维丝束另一表面,在真空箱中50℃干燥4h后得到植物短纤维改性碳纤维。
实施例4
(1)将长碳纤维丝束在80℃的丙酮溶液中冷凝回流24h,然后用去离子水清洗干净并在真空干燥箱中40℃真干燥5h;
(2)将直径约为12μm、长度约为2~7mm的芳纶短纤维分散在二甲亚砜中,800rpm/min磁力搅拌80min使其分散均匀,得到质量分数为2%的芳纶短纤维分散液;
(3)将步骤(1)处理得到的碳纤维丝束均匀铺放在滤膜上,按植物短纤维分散液体积(ml):滤膜直径(cm)=0.5:1真空抽滤芳纶短纤维分散液使其沉积在均匀铺放的碳纤维丝束表面,然后将沉积有芳纶短纤维分散液的碳纤维丝束翻转180°,再真空抽滤同样量的芳纶短纤维分散液使其沉积在均匀铺放的碳纤维丝束另一表面,在真空箱中40℃干燥5h后得到芳纶短纤维改性碳纤维。
实施例5
(1)将长碳纤维丝束在90℃的丙酮溶液中冷凝回流48h,然后用去离子水清洗干净并在真空干燥箱中80℃真干燥2h;
(2)将直径约为8~11μm、长度约为1~5mm的玻璃短纤维分散在四氢呋喃中,600rpm/min磁力搅拌30min使其分散均匀,得到质量分数为0.08%的玻璃短纤维分散液;
(3)将步骤(1)处理得到的碳纤维丝束均匀铺放在滤膜上,按玻璃短纤维分散液体积(ml):滤膜直径(cm)=0.1:1真空抽滤玻璃短纤维分散液使其沉积在均匀铺放的碳纤维丝束表面,然后将沉积有玻璃短纤维分散液的碳纤维丝束翻转180°,再真空抽滤同样量的玻璃短纤维分散液使其沉积在均匀铺放的碳纤维丝束另一表面,在真空箱中80℃干燥2h后得到玻璃短纤维改性碳纤维。
实施例6
(1)将长碳纤维丝束在100℃的丙酮溶液中冷凝回流24h,然后用去离子水清洗干净并在真空干燥箱中70℃干燥2h;
(2)将直径约为20μm、长度约为4~6mm的聚苯并恶唑短纤维分散在二氯甲烷中,1000rpm/min磁力搅拌60min使其分散均匀,得到质量分数为1%的聚苯并恶唑短纤维分散液;
(3)将步骤(1)处理得到的碳纤维丝束均匀铺放在滤膜上,按聚苯并恶唑短纤维分散液体积(ml):滤膜直径(cm)=0.2:1真空抽滤聚苯并恶唑短纤维分散液使其沉积在均匀铺放的碳纤维丝束表面,然后将沉积有聚苯并恶唑短纤维分散液的碳纤维丝束翻转180°,再真空抽滤同样量的聚苯并恶唑短纤维分散液使其沉积在均匀铺放的碳纤维丝束另一表面,在真空箱中70℃干燥2h后得到聚苯并恶唑短纤维改性碳纤维。
实施例7
(1)将长碳纤维丝束在100℃的丙酮溶液中冷凝回流48h,然后用去离子水清洗干净并在真空干燥箱中60℃干燥5h;
(2)将直径约为12~16μm、长度约为2~5mm的玄武岩短纤维分散在二氯甲烷中,700rpm/min磁力搅拌120min使其分散均匀,得到质量分数为3%的玄武岩短纤维分散液;
(3)将步骤(1)处理得到的碳纤维丝束均匀铺放在滤膜上,按玄武岩短纤维分散液体积(ml):滤膜直径(cm)=5:1真空抽滤玄武岩短纤维分散液使其沉积在均匀铺放的碳纤维丝束表面,然后将沉积有玄武岩短纤维分散液的碳纤维丝束翻转180°,再真空抽滤同样量的玄武岩短纤维分散液使其沉积在均匀铺放的碳纤维丝束另一表面,在真空箱中60℃干燥5h后得到玄武岩短纤维改性碳纤维。
Claims (8)
1.一种基于短纤维改性碳纤维的制备方法,其特征在于,包括如下步骤:
(1)将碳纤维丝束在丙酮溶液中冷凝回流,然后用去离子水清洗干净并真空干燥;
(2)将短纤维分散在水或有机溶剂中,搅拌使其分散均匀,得到质量分数为0.01%~3%的短纤维分散液;
(3)将步骤(1)处理得到的碳纤维丝束均匀铺放在滤膜上,真空抽滤短纤维分散液使其沉积在均匀铺放的碳纤维丝束表面,然后将沉积有短纤维分散液的碳纤维丝束翻转180°,再真空抽滤短纤维分散液使其沉积在均匀铺放的碳纤维丝束另一表面,真空干燥后得到短纤维改性碳纤维。
2.根据权利要求1所述的基于短纤维改性碳纤维的制备方法,其特征在于,所述步骤(1)的碳纤维为长碳纤维。
3.根据权利要求1所述的基于短纤维改性碳纤维的制备方法,其特征在于,所述步骤(1)的冷凝回流温度为80~100℃,时间为12~48h。
4.根据权利要求1所述的基于短纤维改性碳纤维的制备方法,其特征在于,所述步骤(2)的短纤维采用直径为500nm~20μm,长度为0.5~10mm的短碳纤维、玻璃短纤维、芳纶短纤维、玄武岩短纤维、聚酯短纤维、聚苯并恶唑短纤维及植物短纤维中的一种或两种以上混合物。
5.根据权利要求1所述的基于短纤维改性碳纤维的制备方法,其特征在于,所述步骤(2)的有机溶剂为丙酮、乙醇、四氢呋喃、二甲基甲酰胺、二氯甲烷或二甲亚砜。
6.根据权利要求1所述的基于短纤维改性碳纤维的制备方法,其特征在于,所述步骤(2)的搅拌采用转速为500~1000rpm/min的磁力搅拌,搅拌时间为30~120min。
7.根据权利要求1所述的基于短纤维改性碳纤维的制备方法,其特征在于,所述步骤(3)真空抽滤短纤维分散液,抽滤短纤维分散液体积(ml):滤膜直径(cm)=(0.1~5):1。
8.根据权利要求1所述的基于短纤维改性碳纤维的制备方法,其特征在于,所述步骤(1)和(3)的真空干燥采用真空干燥箱干燥,其温度为40~80℃,时间为2~5h。
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