CN111979766A - 一种增强芳纶纤维与环氧树脂界面粘结性能的方法 - Google Patents
一种增强芳纶纤维与环氧树脂界面粘结性能的方法 Download PDFInfo
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Abstract
本发明针对芳纶纤维表面呈现惰性,与环氧树脂之间界面粘结性差的问题,提供了一种增强芳纶纤维与环氧树脂界面粘结性能的方法,其特点在于用碳纳米管掺杂多巴胺二次接枝硅烷偶联剂改性芳纶纤维。所述硅烷偶联剂浓度为2%,多巴胺溶液浓度为2g/L。用丙酮溶液去除芳纶纤维表面杂质后烘干;将处理后的芳纶纤维在多巴胺+羟基碳纳米管混合溶液中浸渍,表面形成聚多巴胺涂层,后二次接枝硅烷偶联剂KH560。利用本发明方法制备的改性芳纶纤维强力增强了35.5%,在环氧树脂复合材料抽拔实验中,纤维界面剪切强度提高了41.2%。该改性方法处理后的纤维有效的改善了芳纶树脂基复合材料的力学性能,在军事、建筑产业等各个领域,具有广泛的应用前景。
Description
技术领域
本发明涉及改性芳纶纤维以提高其与环氧树脂界面粘结性的方法,为后续芳纶复合材料力学性能研究提供理论基础,属于芳纶纤维复合材料科学技术领域。
背景技术
芳纶纤维各个品种中,对位芳纶(芳纶1414)综合性能最优异,刚性大分子结构赋予了芳纶高强高模,耐高温,耐化学腐蚀等优异性能,常作为复合材料增强体,广泛应用于航空航天,军事,交通,防护用品等领域。
由于芳纶的分子连段之间的共轭效应和苯环的位阻效应,表面基团的活性低,分子链呈刚性伸直状态,这种结构特点导致纤维表面光滑,在复合材料制备过程中,不易与基体结合,纤维的界面性能影响了复合材料的整体性能,限制了芳纶纤维优异性能的发挥。因此,芳纶纤维表面改性至关重要。
多巴胺分子中含有活性较高的邻苯二酚基团和氨基,在常温下氧化自聚,可以在纤维表面沉积一层聚多巴胺涂层,充当纤维与基体之间的桥梁。掺杂0.03%的羟基碳纳米管作为纳米填料,改善多巴胺在纤维表面涂敷效果,提高涂层的牢固度和均匀致密程度。聚多巴胺层分子中含有大量活性亲水基团,氨基和羟基,不仅能改善基体材料的表面性能,还可作为过渡层,进一步与其他官能团发生接枝,使材料功能化,采用硅烷偶联剂KH560作为接枝剂,在纤维表面进行二次接枝。
本发明采用了多巴胺涂覆改性的方法,掺杂碳纳米管,使纤维表面聚多巴胺涂层牢固度提高,分布均匀致密,接着利用硅烷偶联剂KH560进行二次功能化处理,改性后的纤维表面基团增加从而使表面能增加,进而纤维与环氧树脂的表面粘结性提高。在纤维拉伸、接触角测试和纤维的抽拔试验之后,证实改性后芳纶强力提高,芳纶和环氧树脂的粘结力也有了很大的提高,该方法可以较为简单的实现对复合材料的增强,亦可为复合材料的力学性能的基础进行后续的分析研究。
发明内容
本发明针对芳纶纤维与环氧树脂粘结性差的问题,提供了一种改性芳纶纤维提高其与环氧树脂界面粘结性的方法。为了实现本发明的目的,发明人通过大量的实验研究与不断探索,最终获得如下技术方案:
一种增强芳纶纤维与环氧树脂界面粘结性能的方法有以下步骤:
(1)将芳纶纤维在丙酮溶液中进行超声处理,去除纤维表面的杂质,用去离子水反复清洗,在60℃烘干2h备用;
(2)配制2g/l的盐酸多巴胺溶液,用Tris(三羟甲基氨基甲烷)缓冲剂调节溶液PH到8.5。然后加入质量分数为0.03%的羟基碳纳米管,充分混合后,将芳纶纤维放入,浸渍4h,在浸泡溶液中加入一定质分数的硅烷偶联剂KH560,继续浸泡反应20h,之后取出纤维,用去离子水清洗3-5次,在60℃下烘干2h。
(3)测试纤维改性后的强力、纤维表面的接触角、表面自由能以及改性后纤维在树脂中的抽拔力。
优选的硅烷偶联剂KH560质量分数为2%。
添加羟基碳納米管浓度为0.03%。
多巴胺溶液浓度为2g/L。
烘箱干燥温度为60℃,时间为2小时。
所述的树脂是环氧树脂GCC-135,固化剂为GCC-137固化剂。
本发明的芳纶纤维改性后与未改性芳纶纤维相比,纤维的强力提高35.5%,界面剪切强度提高41.2%,有效改善纤维与树脂之间的界面粘结性,使后续复合材料性能更优。
附图说明
图1为不同硅烷偶联剂浓度改性的芳纶纤维表面SEM图,图2为改性纤维的接触角及表面自由能,图3为改性纤维的拉伸性能参数,图4为改性纤维的抽拔性能参数.
具体实施方式
下面结合具体实施例对本发明做进一步详细描述。
实施例1
(1)纤维改性处理
将芳纶纤维在丙酮溶液中浸泡2小时,用去离子水反复清洗,在干燥箱内60℃烘干2h,密封备用。配制2g/L的盐酸多巴胺溶液,用TRIS缓冲剂调节溶液的PH到8.5,加入质量分数为0.03%的羟基碳納米管,混合充分后,将芳纶纤维放入多巴胺混合溶液中,浸渍4h,后加入质量分数为1%的硅烷偶联剂KH560,浸泡反应20h,最后用去离子水清洗3-5次,60℃烘箱干燥2h。
(2)纤维表面接触角测试
利用Sigma 700/701表面张力仪测试纤维表面接触角和自由能。每组5个样,取平均值。
(3)纤维在树脂中的拔出实验
按照环氧树脂GCC-135∶固化剂GCC-137=100∶30的比例配置树脂,将其注入纤维抽拔装置,测试抽拔力。
(4)纤维强力测试
使用单纤维强力仪测试纤维的强力,5组取平均值。
实施例2
(1)纤维改性处理
将芳纶纤维在丙酮溶液中浸泡2小时,用去离子水反复清洗,在干燥箱内60℃烘干2h,密封备用。配制2g/L的盐酸多巴胺溶液,用TRIS缓冲剂调节溶液的PH到8.5,加入质量分数为0.03%的羟基碳納米管,混合充分后,将芳纶纤维放入多巴胺混合溶液中,浸渍4h,后加入质量分数为1.5%的硅烷偶联剂KH560,浸泡反应20h,最后用去离子水清洗3-5次,60℃烘箱干燥2h。
(3)纤维表面接触角测试
利用Sigma 700/701表面张力仪测试纤维表面接触角和自由能。每组5个样,取平均值。
(3)纤维在树脂中的拔出实验
按照环氧树脂GCC-135∶固化剂GCC-137=100∶30的比例配置树脂,将其注入纤维抽拔装置,测试抽拔力。
(4)纤维强力测试
使用单纤维强力仪测试纤维的强力,5组取平均值。
实施例3
(1)纤维改性处理
将芳纶纤维在丙酮溶液中浸泡2小时,用去离子水反复清洗,在干燥箱内60℃烘干2h,密封备用。配制2g/L的盐酸多巴胺溶液,用TRIS缓冲剂调节溶液的PH到8.5,加入质量分数为0.03%的羟基碳納米管,混合充分后,将芳纶纤维放入多巴胺混合溶液中,浸渍4h,后加入质量分数为2%的硅烷偶联剂KH560,浸泡反应20h,最后用去离子水清洗3-5次,60℃烘箱干燥2h。
(4)纤维表面接触角测试
利用Sigma 700/701表面张力仪测试纤维表面接触角和自由能。每组5个样,取平均值。
(3)纤维在树脂中的拔出实验
按照环氧树脂GCC-135∶固化剂GCC-137=100∶30的比例配置树脂,将其注入纤维抽拔装置,测试抽拔力。
(4)纤维强力测试
使用单纤维强力仪测试纤维的强力,5组取平均值。
实施例4
(1)纤维改性处理
将芳纶纤维在丙酮溶液中浸泡2小时,用去离子水反复清洗,在干燥箱内60℃烘干2h,密封备用。配制2g/L的盐酸多巴胺溶液,用TRIS缓冲剂调节溶液的PH到8.5,加入质量分数为0.03%的羟基碳納米管,混合充分后,将芳纶纤维放入多巴胺混合溶液中,浸渍4h,后加入质量分数为2.5%的硅烷偶联剂KH560,浸泡反应20h,最后用去离子水清洗3-5次,60℃烘箱干燥2h。
(5)纤维表面接触角测试
利用Sigma 700/701表面张力仪测试纤维表面接触角和自由能。每组5个样,取平均值。
(3)纤维在树脂中的拔出实验
按照环氧树脂GCC-135∶固化剂GCC-137=100∶30的比例配置树脂,将其注入纤维抽拔装置,测试抽拔力。
(4)纤维强力测试
使用单纤维强力仪测试纤维的强力,5组取平均值。
实施例5
(1)纤维改性处理
将芳纶纤维在丙酮溶液中浸泡2小时,用去离子水反复清洗,在干燥箱内60℃烘干2h,密封备用。配制2g/L的盐酸多巴胺溶液,用TRIS缓冲剂调节溶液的PH到8.5,加入质量分数为0.03%的羟基碳納米管,混合充分后,将芳纶纤维放入多巴胺混合溶液中,浸渍4h,后加入质量分数为3%的硅烷偶联剂KH560,浸泡反应20h,最后用去离子水清洗3-5次,60℃烘箱干燥2h。
(6)纤维表面接触角测试
利用Sigma 700/701表面张力仪测试纤维表面接触角和自由能。每组5个样,取平均值。
(3)纤维在树脂中的拔出实验
按照环氧树脂GCC-135∶固化剂GCC-137=100∶30的比例配置树脂,将其注入纤维抽拔装置,测试抽拔力。
(4)纤维强力测试
使用单纤维强力仪测试纤维的强力,5组取平均值。
表1纤维性能测试
Claims (4)
1.用丙酮溶液去除芳纶纤维表面杂质后烘干,配置2g/L,PH8.5的多巴胺溶液,掺加浓度为0.03%的羟基碳纳米管,将芳纶纤维放入改性溶液中,在室温下氧化自聚4h,然后添加浓度为2%的硅烷偶联剂KH560,浸渍反应20h,60℃下真空干燥2h。
2.根据权利要求1所述一种增强芳纶纤维与环氧树脂界面粘结性能的方法,其特征在于,所述的羟基碳纳米管浓度为0.03%。
3.据权利要求1所述一种增强芳纶纤维与环氧树脂界面粘结性能的方法,其特征在于,所述的硅烷偶联剂浓度为2%。
4.根据权利要求1所述一种增强芳纶纤维与环氧树脂界面粘结性能的方法,其特征在于,芳纶纤维在多巴胺+碳纳米管混合溶液中浸泡4h,添加硅烷偶联剂继续浸泡20h。
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