CN111778714B - 一种高性能纤维三相复合材料制备工艺 - Google Patents
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Abstract
本发明公开了一种高性能纤维三相复合材料制备工艺，包括以下步骤：将碳纤维加入到80℃的浓硝酸中400W超声氧化5小时，然后过滤水洗至中性，得到氧化碳纤维；将氧化碳纤维分散到乙氧基化聚乙烯亚胺溶液中，加热至80℃，搅拌反应5小时，过滤水洗，然后得到聚乙烯亚胺枝化碳纤维；将聚乙烯亚胺枝化碳纤维浸入胶液中，取出，然后60℃固化1min，得到浸胶纤维；在浸胶纤维的表面立即包覆一层厚度为20um的三元乙丙橡胶层，然后80℃固化5小时，得到三相复合材料，本发明克服了现有技术的不足，提高了碳纤维复合材料的界面结合强度和力学性能。
Description
技术领域
本发明涉及高性能纤维复合材料技术领域，具体属于一种高性能纤维三相复合材料制备工艺。
背景技术
碳纤维是含碳量在90％以上的高强度高模量纤维，在碳纤维复合材料中，碳纤维与复合相之间的界面结合强度，是影响碳纤维复合材料力学性能的关键因素，只有碳纤维与复合相之间实现较好的界面结合，碳纤维才可能有效的传递外界应力，从而提高复合材料的力学性能。而碳纤维由于表面官能团数量少，界面结合强度低，因此很难与其他材料进行有效的复合，导致单一的碳纤维材料存在整体力学性能差的问题，无法满足材料的使用要求。
发明内容
本发明的目的是提供一种高性能纤维三相复合材料制备工艺，克服了现有技术中碳纤维复合材料界面结合强度低和力学性能不足的问题。
为解决上述问题，本发明所采取的技术方案如下：
一种高性能纤维三相复合材料制备工艺，包括以下步骤：
S1，将碳纤维加入到80℃的浓硝酸中400W超声氧化5小时，然后过滤水洗至中性，得到氧化碳纤维；
S2，将氧化碳纤维分散到乙氧基化聚乙烯亚胺溶液中，加热至80℃，搅拌反应5小时，过滤水洗，然后得到聚乙烯亚胺枝化碳纤维；
S3，将聚乙烯亚胺枝化碳纤维浸入胶液中，取出，然后60℃固化1min，得到浸胶纤维；
S4，在浸胶纤维的表面立即包覆一层厚度为20um的三元乙丙橡胶层，然后80℃固化5小时，得到三相复合材料。
其中，所述的乙氧基化聚乙烯亚胺溶液中乙氧基化聚乙烯亚胺的浓度为37wt％。
其中，所述的乙氧基化聚乙烯亚胺的乙氧基化程度为80％。
其中，所述的胶液的制备方法为：在乙醇溶液中加入二烯丙基双酚A和甲基丙烯酰胺，加热至60℃搅拌反应4小时，然后将乙醇蒸干，加入过氧化二异丙苯和3-异氰酸酯基-4-甲苯氨基甲酸烯丙酯搅拌混合均匀，得到胶液。
其中，所述的三元乙丙橡中的硫化剂为1,1-二(叔丁基过氧)-3,3,5三甲基环己烷。
本发明与现有技术相比较，本发明的实施效果如下：
1、本发明使用浓硝酸对碳纤维的表面进行氧化，使碳纤维的表面产生-OH和-COOH；同时在氧化的过程中，使用超声辅助，使浓硝酸对碳纤维表面氧化更加彻底。
2、将氧化后的碳纤维与乙氧基化聚乙烯亚胺混合并加热，使亚胺基与羧基发生脱水反应，实现了对碳纤维表面的枝化，使碳纤维更容易与胶液反应，同时，接枝后的碳纤维表面存在大量的乙氧基官能团，乙氧基官能团在过氧化二异丙苯引发剂的作用下，与3-异氰酸酯基-4-甲苯氨基甲酸烯丙酯发生接枝反应，而二烯丙基双酚A和甲基丙烯酰胺在过氧化二异丙苯引发剂的作用下生成甲基丙烯酰胺-二烯丙基双酚A接枝聚合物，起到基体作用，而甲基丙烯酰胺-二烯丙基双酚A接枝聚合物具有较强的韧性和抗拉伸性能，与碳纤维复合后提高了纤维的力学性能。
3、本发明采用乙氧基化程度为80％的乙氧基化聚乙烯亚胺，使接枝后的碳纤维与3-异氰酸酯基-4-甲苯氨基甲酸烯丙酯的接枝反应程度更高，有效的增强了甲基丙烯酰胺-二烯丙基双酚A接枝聚合物与碳纤维的结合强度。
4、在甲基丙烯酰胺-二烯丙基双酚A接枝聚合物的外部包覆一层三元乙丙橡胶，提高了该纤维的抗氧化能力和耐腐蚀能力，且三元乙丙橡胶橡胶中的硫化剂为1,1-二(叔丁基过氧)-3,3,5三甲基环己烷，具有氧化和交联作用，使三元乙丙橡胶与3-异氰酸酯基-4-甲苯氨基甲酸烯丙酯发生接枝反应，增强了三元乙丙橡胶与甲基丙烯酰胺-二烯丙基双酚A接枝聚合物的结合强度。
具体实施方式
下面将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。
本发明的乙氧基化聚乙烯亚胺溶液中的乙氧基化聚乙烯亚胺浓度为37wt％，而三元乙丙橡胶来源于山东七同橡胶科技有限公司。
实施例1
高性能纤维三相复合材料制备工艺，包括以下步骤：
首先，将5g碳纤维加入到400g 80℃的浓硝酸中400W超声氧化5小时，然后过滤水洗至中性，得到氧化碳纤维。
然后，将5g氧化碳纤维分散到200g乙氧基化聚乙烯亚胺溶液中，乙氧基化聚乙烯亚胺的乙氧基化程度为80％，加热至80℃，搅拌反应5小时，过滤水洗，然后得到聚乙烯亚胺枝化碳纤维。
接着，将聚乙烯亚胺枝化碳纤维浸入100g的胶液中，胶液的制备方法为：在150g的乙醇溶液中加入二烯丙基双酚A 20g和甲基丙烯酰胺30g，加热至60℃搅拌反应4小时，然后将乙醇蒸干，加入过氧化二异丙苯1.2g和3-异氰酸酯基-4-甲苯氨基甲酸烯丙酯8g搅拌混合均匀，得到胶液。然后将浸胶后的纤维取出，然后60℃固化1min，得到浸胶纤维；紧接着，在浸胶纤维的表面立即包覆一层厚度为20um的三元乙丙橡胶层，其中，三元乙丙橡层中的硫化剂为1,1-二(叔丁基过氧)-3,3,5三甲基环己烷，然后80℃固化5小时，得到三相复合材料。
对照例1
与实施例1的区别在于，将乙氧基化聚乙烯亚胺溶液替换为相同浓度的聚乙烯亚胺溶液。
对照例2
与实施例1的区别在于，3-异氰酸酯基-4-甲苯氨基甲酸烯丙酯的加入量为0。
对照例3
与实施例1的区别在于，将1,1-二(叔丁基过氧)-3,3,5三甲基环己烷替换为过氧化二异丙苯。
将实施例1和对照例1-3中的三相复合材料按照GB/T 26749-2011中的测试方法测试拉伸性能，结果如下表所示：
| 实施例1 | 对照例1 | 对照例2 | 对照例3 | |
| 拉伸模量(GPa) | 27.4 | 7.5 | 6.2 | 19.4 |
由拉伸模量的数据变化可以明显看出，碳纤维接枝乙氧基化聚乙烯亚胺后的三相复合材料的拉伸模量最大，达到了27.4GPa，同时3-异氰酸酯基-4-甲苯氨基甲酸烯丙酯与乙氧基官能团的交联作用对碳纤维与甲基丙烯酰胺-二烯丙基双酚A接枝聚合物的界面结合强度起主要作用。
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 (2)
1.一种高性能纤维三相复合材料制备工艺，其特征在于，包括以下步骤：
S1，将碳纤维加入到80℃的浓硝酸中400W超声氧化5小时，然后过滤水洗至中性，得到氧化碳纤维；
S2，将氧化碳纤维分散到乙氧基化聚乙烯亚胺溶液中，加热至80℃，搅拌反应5小时，过滤水洗，然后得到聚乙烯亚胺枝化碳纤维；
S3，将聚乙烯亚胺枝化碳纤维浸入胶液中，取出，然后60℃固化1min，得到浸胶纤维；
S4，在浸胶纤维的表面立即包覆一层厚度为20um的三元乙丙橡胶层，然后80℃固化5小时，得到三相复合材料；
所述的乙氧基化聚乙烯亚胺的乙氧基化程度为80%；
所述的胶液的制备方法为：在乙醇溶液中加入二烯丙基双酚A和甲基丙烯酰胺，加热至60℃搅拌反应4小时，然后将乙醇蒸干，加入过氧化二异丙苯和3-异氰酸酯基-4-甲苯氨基甲酸烯丙酯搅拌混合均匀，得到胶液；
所述的三元乙丙橡胶中的硫化剂为1,1-二(叔丁基过氧)-3,3,5三甲基环己烷。
2.根据权利要求1所述的一种高性能纤维三相复合材料制备工艺，其特征在于，所述的乙氧基化聚乙烯亚胺溶液中乙氧基化聚乙烯亚胺的浓度为37wt%。
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