CN108192115A - 一种改性芳纶纤维提高其与环氧树脂界面粘结性的方法 - Google Patents
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Abstract
本发明针对芳纶纤维与环氧树脂界面粘结性差的问题，提供了一种改性芳纶纤维从而提高其与环氧树脂界面粘结力的方法，其特点在于用LiCl乙醇溶液与超声联合改性。所述LiCl乙醇溶液浓度为5wt％，超声联合改性的时间为120分钟。将芳纶纤维在丙酮溶液中进行预处理去除表面杂质后，用去离子水冲洗、烘箱干燥。再经过LiCl乙醇溶液超声联合处理一定时间，再次经过去离子水冲洗、烘箱干燥。最后处理后的纤维进行测试。该改性方法处理后的纤维强力仅下降13.8％，与树脂的粘结力提高39.69％，以其高强度、高模量等优点广泛的应用于军事、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，是一种新型高科技合成纤维，具有超高强度、高模量和耐高温、耐酸耐碱、重量轻、绝缘、抗老化、生命周期长等优良性能，广泛应用于复合材料、防弹制品、建材、特种防护服装、电子设备等领域。芳纶纤维在复合材料领域应用是主要作为复合材料的增强体。但由于芳纶纤维表面比较光滑，纤维表面活性基团少，故与基体复合时其界面的粘结性比较差。复合材料受到拉伸等外界作用力时，纤维易从复合材料中抽拔出来，故对纤维表面进行改性处理，提高其与基体的结合能力显得尤为重要，
目前，纤维改性方法按原理可以分为3种：化学改性、物理改性、表面涂层改性。
化学改性是通过化学试剂的刻蚀作用，对纤维表面实施刻蚀。这种方法反应程度和反应速率不易控制，极易对纤维造成破坏，使纤维的力学性能损失较大，进而影响复合材料的力学性能。另一方面，此类化学试剂具有氧化性和腐蚀性，可能对人体造成伤害，对实验环境要求较高，且不利于企业的规模化生产。
物理改性有超声波处理、高能射线辐射、等离子技术处理等方法，这些方法应用简单，无污染，无腐蚀，实验条件能最大满足。但是物理改性和化学改性方法一样，会对纤维的力学性能造成伤害。例如利用等离子体处理法对纤维表面的刻蚀和接枝反应，会破坏纤维表面的完整性，同时存在活性退化效果，对设备和环境要求较高。
表面涂层改性同样简单可行，但涂层和纤维只是物理性的结合，与材料共混时还存在一定的缺陷。
本发明采用了丙酮预处理，LiCl乙醇溶液超声联合改性的方法，使纤维表面粗糙，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，证实该方法在芳纶纤维强力下降不大的情况下，对于芳纶和环氧树脂的粘结力有了很大的提高，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：
一种增强芳纶纤维和环氧树脂粘结性的方法有以下步骤：
(1)将芳纶纤维在丙酮溶液中进行预处理，去除纤维表面的杂质，用去离子水反复清洗，60℃烘干备用；
(2)用一定浓度LiCl乙醇溶液超声联合处理60、90、120、180分钟后，用去离子水反复清理，60℃烘干。
(3)测试纤维改性后的强力以及改性后纤维在树脂中的抽拔力。
优选的LiCl乙醇溶液浓度为5wt％。
超声震荡频率为40KHz，温度为40℃。
烘箱干燥温度为60℃，时间为3-4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，纤维的强力下降13.8％粘结力提高39.69％，使后续复合材料性能更优。
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4小时，用去离子水反复清洗，在干燥箱内60℃烘干，密封备用。将预处理的纤维分别放入质量浓度为0wt％的LiCl乙醇溶液中，分别超声处理60分钟、90分钟、120分钟、180分钟，用去离子水反复清洗，在干燥箱内60℃烘干，保存。
(2)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。
(3)纤维强力测试
使用万能强力机测试纤维的强力，5组取平均值。
表1为纤维抽拔力测试结果
实施例2
(1)纤维改性处理
将芳纶纤维在丙酮溶液中浸泡4小时，用去离子水反复清洗，在干燥箱内60℃烘干，密封备用。将预处理的纤维分别放入质量浓度为3wt％的LiCl乙醇溶液中，分别超声处理60分钟、90分钟、120分钟、180分钟，用去离子水反复清洗，在干燥箱内60℃烘干，保存。
(2)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。
(3)纤维强力测试
使用万能强力机测试纤维的强力，5组取平均值。
表2为纤维抽拔力测试结果
实施例3
(1)纤维改性处理
将芳纶纤维在丙酮溶液中浸泡4小时，用去离子水反复清洗，在干燥箱内60℃烘干，密封备用。将预处理的纤维分别放入质量浓度为5wt％的LiCl乙醇溶液中，分别超声处理60分钟、90分钟、120分钟、180分钟，用去离子水反复清洗，在干燥箱内60℃烘干，保存。
(2)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。
(3)纤维强力测试
使用万能强力机测试纤维的强力，5组取平均值。
表3为纤维抽拔力测试结果
实施例4
(1)纤维改性处理
将芳纶纤维在丙酮溶液中浸泡4小时，用去离子水反复清洗，在干燥箱内60℃烘干，密封备用。将预处理的纤维分别放入质量浓度为7wt％的LiCl乙醇溶液中，分别超声处理60分钟、90分钟、120分钟、180分钟，用去离子水反复清洗，在干燥箱内60℃烘干，保存。
(2)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。
(3)纤维强力测试
使用万能强力机测试纤维的强力，5组取平均值。
表3为纤维抽拔力测试结果
Claims (4)
1.一种改性芳纶纤维进而提高其与环氧树脂界面粘结力的方法，其主要特点是LiCl乙醇溶液超声联合对芳纶纤维改性处理。将芳纶纤维在丙酮溶液中预处理浸泡4小时，预处理后的纤维经过去离子水反复清洗，在烘箱中干燥。干燥后的芳纶纤维用一定浓度的LiCl乙醇溶液超声联合改性一定的时间，然后用去离子水反复冲洗，在烘箱中干燥，最后密封保存。
2.根据权利要求1所述一种芳纶纤维与环氧树脂结合，并提高其界面粘结力的方法，其特征在于，所述的LiCl乙醇溶液浓度为5wt％，超声处理时间为60、90、120、180分钟。
3.根据权利要求1所述一种芳纶纤维与环氧树脂结合，并提高其界面粘结力的方法，超声震荡频率为40KHz，温度为40℃。
4.根据权利要求1所述一种芳纶纤维与环氧树脂结合，并提高其界面粘结力的方法，烘箱干燥温度为60℃，时间为3-4小时。
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| CN110372998A (zh) * | 2019-07-30 | 2019-10-25 | 山东大学 | 一种芳纶纤维增强环氧树脂基体复合材料及其制备方法 |
| CN110424150A (zh) * | 2019-07-31 | 2019-11-08 | 山东大学 | 一种芳纶纤维表面改性方法 |
| CN111533930A (zh) * | 2020-05-11 | 2020-08-14 | 哈尔滨工业大学 | 一种微纤化纤维增强复合材料的制备方法 |
| CN113234314A (zh) * | 2021-04-14 | 2021-08-10 | 电子科技大学 | 一种芳纶纤维增强聚芳醚腈复合材料的制备方法 |
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2018
- 2018-01-24 CN CN201810070950.XA patent/CN108192115A/zh active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110372998A (zh) * | 2019-07-30 | 2019-10-25 | 山东大学 | 一种芳纶纤维增强环氧树脂基体复合材料及其制备方法 |
| CN110424150A (zh) * | 2019-07-31 | 2019-11-08 | 山东大学 | 一种芳纶纤维表面改性方法 |
| CN111533930A (zh) * | 2020-05-11 | 2020-08-14 | 哈尔滨工业大学 | 一种微纤化纤维增强复合材料的制备方法 |
| CN113234314A (zh) * | 2021-04-14 | 2021-08-10 | 电子科技大学 | 一种芳纶纤维增强聚芳醚腈复合材料的制备方法 |
| CN113234314B (zh) * | 2021-04-14 | 2022-04-15 | 电子科技大学 | 一种芳纶纤维增强聚芳醚腈复合材料的制备方法 |
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