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CN106947215A - 一种氧化石墨烯丙纶耐热高强复合型材及其制备方法 - Google Patents

一种氧化石墨烯丙纶耐热高强复合型材及其制备方法 Download PDF

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CN106947215A
CN106947215A CN201710138429.0A CN201710138429A CN106947215A CN 106947215 A CN106947215 A CN 106947215A CN 201710138429 A CN201710138429 A CN 201710138429A CN 106947215 A CN106947215 A CN 106947215A
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graphene oxide
polypropylene fibre
plain weave
composite
oxide polypropylene
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黄旭
张炜栋
陈志华
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Nantong Textile Vocational Technology College
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Nantong Textile Vocational Technology College
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Priority to CN201710138429.0A priority Critical patent/CN106947215A/zh
Publication of CN106947215A publication Critical patent/CN106947215A/zh
Priority to PCT/CN2017/108498 priority patent/WO2018161612A1/zh
Priority to US16/300,659 priority patent/US11041261B2/en
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Abstract

本发明公开了一种氧化石墨烯丙纶耐热高强复合型材及其制备方法，所述复合型材是氧化石墨烯丙纶基增强平纹组织复合树脂材料，是氧化石墨烯丙纶基机平纹组织织布与纤维隔热材料制成层连间隔结构复合平网，最终与树脂复合材料制成的耐热高强复合型材。其制备方法包括如下步骤：氧化石墨烯丙纶基机平纹组织织布制备；氧化石墨烯丙纶基增强平纹组织复合材料制备；多层氧化石墨烯丙纶基增强平纹组织复合材料制备；树脂复合材料制备。本发明操作方便，性能优异，由于氧化石墨烯丙纶具有优异耐温性和传热性，耐温温度进一步提高，抗冲击性能也同时提高，从而获得性能优异的复合型材。

Description

一种氧化石墨烯丙纶耐热高强复合型材及其制备方法
技术领域
本发明属于复合型材领域，具体涉及一种氧化石墨烯丙纶耐热高强复合型材及其制备方法。
背景技术
从石墨烯发现那一天起，已经成为研究热点，在超级电容、透明电极、海水淡化、太阳能电池、复合材料等领域有广泛应用。石墨烯由碳原子以sp2杂化轨道组成六角型蜂巢晶格，其结构单元为碳六元环，是一种只有单层碳原子厚度的二维材料。石墨烯具有优异的机械、电学和热学性能。氧化石墨烯是石墨烯派生物，与石墨烯结构大体相同，氧化石墨烯含有羟基—OH、羧基—COOH、羰基C＝O等官能团，可以与其它化学基团进行共价反应。
聚丙烯纤维，简称丙纶，具有熔点低、耐化学腐蚀、热变形温度高等特点，是热塑性复合材料的常用基体材料。氧化石墨烯丙纶耐热高强复合型材可以克服单一聚合物的一些缺陷，赋予聚合物特殊的物化性能，改善聚合物的综合性能，扩宽聚合物的应用领域。以期得到成型效果良好的丙纶基连续纤维增强机织复合材料。
发明内容
发明目的：本发明提供一种氧化石墨烯丙纶耐热高强复合型材及其制备方法。
技术方案：一种氧化石墨烯丙纶耐热高强复合型材，所述复合型材是氧化石墨烯丙纶基增强平纹组织复合树脂材料，是氧化石墨烯丙纶基机平纹组织织布与纤维隔热材料制成层连间隔结构复合平网，最终与树脂复合材料制成的耐热高强复合型材，其中，所述氧化石墨烯丙纶基机平纹组织织布采用氧化石墨烯丙纶长丝纤维，丙纶长丝纤维中氧化石墨烯重量百分比含量0.3-0.7％。
一种根据所述的氧化石墨烯丙纶耐热高强复合型材的制备方法，包括如下步骤：
步骤一、氧化石墨烯丙纶基机平纹组织织布制备：所述氧化石墨烯丙纶基机平纹组织织布采用氧化石墨烯丙纶长丝纤维，丙纶纤维中氧化石墨烯重量百分比含量0.3-0.7％，210D，24F；通过络筒、并丝、捻丝、定型、整经、浆丝、并轴、穿结经、机织织造工序，以氧化石墨烯丙纶复丝为经纬纱线，织造经密45-55根/5cm，纬密30-40根/5cm的平纹组织，平方米克重为500-700g/㎡,厚度0.06-0.20mm；
步骤二、氧化石墨烯丙纶基增强平纹组织复合材料制备：将隔热材料，制成几种不同厚度与密度的平网，隔热层平方米克重为150-220g/㎡,厚度0.10-0.25mm；将氧化石墨烯丙纶基机平纹组织织布覆于其上，采用干法成网、针刺加固的方法非织造网材；所述隔热层材料为石棉、岩棉、玻璃纤维、硅酸铝纤维、高硅氧纤维和氧化铝纤维中的一种或几种；
步骤三、多层氧化石墨烯丙纶基增强平纹组织复合材料制备：所述多层氧化石墨烯丙纶基增强平纹组织复合材料为两层或两层以上，主要目的为增加复合材料内部氧化石墨烯丙纶含量；通过针刺加固将氧化石墨烯丙纶基增强平纹组织复合材料进行正反2次针刺加固，针刺密度为90-130刺/cm2，针刺频率220-280刺/min，第一次植针密度为2500枚/m，第二次植针密度为2500枚/m，针刺纤网的速度分别为1.8-2.0m/min；
步骤四、树脂复合材料制备：所述树脂复合材料为环氧树脂，将环氧树脂和固化剂按照质量比2：1称取，在45-60℃下预热10min，加入环氧树脂质量分数3-5％硅烷偶合剂及质量分数3-5％氧化石墨烯N-甲基吡咯烷酮分散液(0.5％)，搅拌10min，45-60℃抽真空30-40min，去除环氧树脂中气泡；在环氧树脂中依次加入环氧树脂质量分数1-2％的促进剂、丙酮，搅拌混合均匀，将多层氧化石墨烯丙纶基增强平纹组织复合材料浸入，加入环氧树脂质量分数40％的固化剂，充分搅拌均匀，45-60℃抽真空30-40min，去除气泡；放入鼓风干燥箱中：常温2h,然后温度为95℃-120℃下4h进行固化,最终得到氧化石墨烯丙纶耐热高强复合型材。
作为优化：所述步骤四中，加入的固化剂为脂肪胺类、芳香族、脂肪环类、改性胺类、酸酐类、低分子聚酰胺和潜伏性胺固化剂其中一种或几种。
作为优化：所述步骤四中，加入的硅烷偶合剂为硅烷偶联剂KH-560、硅烷偶联剂A-172、复合型铝钛偶联剂其中一种或几种。
作为优化：所述步骤四中，加入的环氧促进剂为环氧促进剂XH-610、环氧促进剂DMP-30、巴斯夫E-6623、环氧固化促进剂EM-7604H其中一种或几种。
有益效果：本发明的具体优势如下：
1、本发明中的氧化石墨烯丙纶与传统丙纶相比具有优异耐温、传热、高强效果，抗冲击性能也同时提高。
2、本发明氧化石墨烯丙纶纤维中含有氧化石墨烯，纤维表面氧化石墨烯易与环氧树脂锚定，从而强化多层氧化石墨烯丙纶基增强平纹组织复合材料与树脂的结合。
3、本发明在环氧树脂中加入硅烷偶合剂及氧化石墨烯N-甲基吡咯烷酮分散液对树脂中的氧化石墨烯进行硅烷修饰，从而增强树脂中的硅烷修饰氧化石墨烯与多层氧化石墨烯丙纶基增强平纹组织复合材料锚定，起到协同双锚定的效果。
具体实施方式
下面结合具体实施例对本发明进行详细阐述。
具体实施例一：
一种氧化石墨烯丙纶耐热高强复合型材，所述复合型材是氧化石墨烯丙纶基增强平纹组织复合树脂材料，是氧化石墨烯丙纶基机平纹组织织布与纤维隔热材料制成层连间隔结构复合平网，最终与树脂复合材料制成的耐热高强复合型材，其中，所述氧化石墨烯丙纶基机平纹组织织布采用氧化石墨烯丙纶长丝纤维，丙纶长丝纤维中氧化石墨烯重量百分比含量0.3％。
一种根据所述的氧化石墨烯丙纶耐热高强复合型材的制备方法，包括如下步骤：
步骤一、氧化石墨烯丙纶基机平纹组织织布制备：所述氧化石墨烯丙纶基机平纹组织织布采用氧化石墨烯丙纶长丝纤维，丙纶纤维中氧化石墨烯重量百分比含量0.3％，210D，24F；通过络筒、并丝、捻丝、定型、整经、浆丝、并轴、穿结经、机织织造工序，以氧化石墨烯丙纶复丝为经纬纱线，织造经密45根/5cm，纬密30根/5cm的平纹组织，平方米克重为500g/㎡,厚度0.06mm。
步骤二、氧化石墨烯丙纶基增强平纹组织复合材料制备：将隔热材料，制成几种不同厚度与密度的平网，隔热层平方米克重为150g/㎡,厚度0.10mm；将氧化石墨烯丙纶基机平纹组织织布覆于其上，采用干法成网、针刺加固的方法非织造网材；所述隔热层材料为石棉、岩棉、玻璃纤维、硅酸铝纤维、高硅氧纤维和氧化铝纤维中的一种或几种。
步骤三、多层氧化石墨烯丙纶基增强平纹组织复合材料制备：所述多层氧化石墨烯丙纶基增强平纹组织复合材料为两层或两层以上，主要目的为增加复合材料内部氧化石墨烯丙纶含量；通过针刺加固将氧化石墨烯丙纶基增强平纹组织复合材料进行正反2次针刺加固，针刺密度为90刺/cm2，针刺频率220刺/min，第一次植针密度为2500枚/m，第二次植针密度为2500枚/m，针刺纤网的速度分别为1.8m/min。
步骤四、树脂复合材料制备：所述树脂复合材料为环氧树脂，将环氧树脂和固化剂按照质量比2：1称取，在45℃下预热10min，加入环氧树脂质量分数3％硅烷偶合剂及质量分数3％氧化石墨烯N-甲基吡咯烷酮分散液(0.5％)，搅拌10min，45℃抽真空30min，去除环氧树脂中气泡；在环氧树脂中依次加入环氧树脂质量分数1％的促进剂、丙酮，搅拌混合均匀，将多层氧化石墨烯丙纶基增强平纹组织复合材料浸入，加入环氧树脂质量分数40％的固化剂，充分搅拌均匀，45℃抽真空30min，去除气泡；放入鼓风干燥箱中：常温2h,然后温度为95℃下4h进行固化,最终得到氧化石墨烯丙纶耐热高强复合型材；加入的固化剂为脂肪胺类、芳香族、脂肪环类、改性胺类、酸酐类、低分子聚酰胺和潜伏性胺固化剂其中一种或几种；加入的硅烷偶合剂为硅烷偶联剂KH-560、硅烷偶联剂A-172、复合型铝钛偶联剂其中一种或几种；加入的环氧促进剂为环氧促进剂XH-610、环氧促进剂DMP-30、巴斯夫E-6623、环氧固化促进剂EM-7604H其中一种或几种。
具体实施例二：
一种氧化石墨烯丙纶耐热高强复合型材，所述复合型材是氧化石墨烯丙纶基增强平纹组织复合树脂材料，是氧化石墨烯丙纶基机平纹组织织布与纤维隔热材料制成层连间隔结构复合平网，最终与树脂复合材料制成的耐热高强复合型材，其中，所述氧化石墨烯丙纶基机平纹组织织布采用氧化石墨烯丙纶长丝纤维，丙纶长丝纤维中氧化石墨烯重量百分比含量0.7％。
一种根据所述的氧化石墨烯丙纶耐热高强复合型材的制备方法，包括如下步骤：
步骤一、氧化石墨烯丙纶基机平纹组织织布制备：所述氧化石墨烯丙纶基机平纹组织织布采用氧化石墨烯丙纶长丝纤维，丙纶纤维中氧化石墨烯重量百分比含量0.7％，210D，24F；通过络筒、并丝、捻丝、定型、整经、浆丝、并轴、穿结经、机织织造工序，以氧化石墨烯丙纶复丝为经纬纱线，织造经密55根/5cm，纬密40根/5cm的平纹组织，平方米克重为700g/㎡,厚度0.20mm。
步骤二、氧化石墨烯丙纶基增强平纹组织复合材料制备：将隔热材料，制成几种不同厚度与密度的平网，隔热层平方米克重为220g/㎡,厚度0.25mm；将氧化石墨烯丙纶基机平纹组织织布覆于其上，采用干法成网、针刺加固的方法非织造网材；所述隔热层材料为石棉、岩棉、玻璃纤维、硅酸铝纤维、高硅氧纤维和氧化铝纤维中的一种或几种。
步骤三、多层氧化石墨烯丙纶基增强平纹组织复合材料制备：所述多层氧化石墨烯丙纶基增强平纹组织复合材料为两层或两层以上，主要目的为增加复合材料内部氧化石墨烯丙纶含量；通过针刺加固将氧化石墨烯丙纶基增强平纹组织复合材料进行正反2次针刺加固，针刺密度为130刺/cm2，针刺频率280刺/min，第一次植针密度为2500枚/m，第二次植针密度为2500枚/m，针刺纤网的速度分别为2.0m/min。
步骤四、树脂复合材料制备：所述树脂复合材料为环氧树脂，将环氧树脂和固化剂按照质量比2：1称取，在60℃下预热10min，加入环氧树脂质量分数3-5％硅烷偶合剂及质量分数5％氧化石墨烯N-甲基吡咯烷酮分散液(0.5％)，搅拌10min，45-60℃抽真空40min，去除环氧树脂中气泡；在环氧树脂中依次加入环氧树脂质量分数2％的促进剂、丙酮，搅拌混合均匀，将多层氧化石墨烯丙纶基增强平纹组织复合材料浸入，加入环氧树脂质量分数40％的固化剂，充分搅拌均匀，60℃抽真空40min，去除气泡；放入鼓风干燥箱中：常温2h,然后温度为120℃下4h进行固化,最终得到氧化石墨烯丙纶耐热高强复合型材；加入的固化剂为脂肪胺类、芳香族、脂肪环类、改性胺类、酸酐类、低分子聚酰胺和潜伏性胺固化剂其中一种或几种；加入的硅烷偶合剂为硅烷偶联剂KH-560、硅烷偶联剂A-172、复合型铝钛偶联剂其中一种或几种；加入的环氧促进剂为环氧促进剂XH-610、环氧促进剂DMP-30、巴斯夫E-6623、环氧固化促进剂EM-7604H其中一种或几种。
具体实施例三：
一种氧化石墨烯丙纶耐热高强复合型材，所述复合型材是氧化石墨烯丙纶基增强平纹组织复合树脂材料，是氧化石墨烯丙纶基机平纹组织织布与纤维隔热材料制成层连间隔结构复合平网，最终与树脂复合材料制成的耐热高强复合型材，其中，所述氧化石墨烯丙纶基机平纹组织织布采用氧化石墨烯丙纶长丝纤维，丙纶长丝纤维中氧化石墨烯重量百分比含量0.4％。
一种根据所述的氧化石墨烯丙纶耐热高强复合型材的制备方法，包括如下步骤：
步骤一、氧化石墨烯丙纶基机平纹组织织布制备：所述氧化石墨烯丙纶基机平纹组织织布采用氧化石墨烯丙纶长丝纤维，丙纶纤维中氧化石墨烯重量百分比含量0.4％，210D，24F；通过络筒、并丝、捻丝、定型、整经、浆丝、并轴、穿结经、机织织造工序，以氧化石墨烯丙纶复丝为经纬纱线，织造经密49根/5cm，纬密36根/5cm的平纹组织，平方米克重为600g/㎡,厚度0.10mm。
步骤二、氧化石墨烯丙纶基增强平纹组织复合材料制备：将隔热材料，制成几种不同厚度与密度的平网，隔热层平方米克重为190g/㎡,厚度0.20mm；将氧化石墨烯丙纶基机平纹组织织布覆于其上，采用干法成网、针刺加固的方法非织造网材；所述隔热层材料为石棉、岩棉、玻璃纤维、硅酸铝纤维、高硅氧纤维和氧化铝纤维中的一种或几种。
步骤三、多层氧化石墨烯丙纶基增强平纹组织复合材料制备：所述多层氧化石墨烯丙纶基增强平纹组织复合材料为两层或两层以上，主要目的为增加复合材料内部氧化石墨烯丙纶含量；通过针刺加固将氧化石墨烯丙纶基增强平纹组织复合材料进行正反2次针刺加固，针刺密度为110刺/cm2，针刺频率270刺/min，第一次植针密度为2500枚/m，第二次植针密度为2500枚/m，针刺纤网的速度分别为1.9m/min。
步骤四、树脂复合材料制备：所述树脂复合材料为环氧树脂，将环氧树脂和固化剂按照质量比2：1称取，在52℃下预热10min，加入环氧树脂质量分数4％硅烷偶合剂及质量分数4％氧化石墨烯N-甲基吡咯烷酮分散液(0.5％)，搅拌10min，52℃抽真空36min，去除环氧树脂中气泡；在环氧树脂中依次加入环氧树脂质量分数1.5％的促进剂、丙酮，搅拌混合均匀，将多层氧化石墨烯丙纶基增强平纹组织复合材料浸入，加入环氧树脂质量分数40％的固化剂，充分搅拌均匀，54℃抽真空37min，去除气泡；放入鼓风干燥箱中：常温2h,然后温度为110℃下4h进行固化,最终得到氧化石墨烯丙纶耐热高强复合型材；加入的固化剂为脂肪胺类、芳香族、脂肪环类、改性胺类、酸酐类、低分子聚酰胺和潜伏性胺固化剂其中一种或几种；加入的硅烷偶合剂为硅烷偶联剂KH-560、硅烷偶联剂A-172、复合型铝钛偶联剂其中一种或几种；加入的环氧促进剂为环氧促进剂XH-610、环氧促进剂DMP-30、巴斯夫E-6623、环氧固化促进剂EM-7604H其中一种或几种。
本发明不局限于上述最佳实施方式，任何人在本发明的启示下都可得出其他各种形式的产品，但不论在其形状或结构上作任何变化，凡是具有与本申请相同或相近似的技术方案，均落在本发明的保护范围之内。

Claims (5)

1.一种氧化石墨烯丙纶耐热高强复合型材，其特征在于：所述复合型材是氧化石墨烯丙纶基增强平纹组织复合树脂材料，是氧化石墨烯丙纶基机平纹组织织布与纤维隔热材料制成层连间隔结构复合平网，最终与树脂复合材料制成的耐热高强复合型材，其中，所述氧化石墨烯丙纶基机平纹组织织布采用氧化石墨烯丙纶长丝纤维，丙纶长丝纤维中氧化石墨烯重量百分比含量0.3-0.7％。
2.一种根据权利要求1所述的氧化石墨烯丙纶耐热高强复合型材的制备方法，其特征在于：包括如下步骤：
步骤一、氧化石墨烯丙纶基机平纹组织织布制备：所述氧化石墨烯丙纶基机平纹组织织布采用氧化石墨烯丙纶长丝纤维，丙纶纤维中氧化石墨烯重量百分比含量0.3-0.7％，210D，24F；通过络筒、并丝、捻丝、定型、整经、浆丝、并轴、穿结经、机织织造工序，以氧化石墨烯丙纶复丝为经纬纱线，织造经密45-55根/5cm，纬密30-40根/5cm的平纹组织，平方米克重为500-700g/㎡,厚度0.06-0.20mm；
步骤二、氧化石墨烯丙纶基增强平纹组织复合材料制备：将隔热材料，制成几种不同厚度与密度的平网，隔热层平方米克重为150-220g/㎡,厚度0.10-0.25mm；将氧化石墨烯丙纶基机平纹组织织布覆于其上，采用干法成网、针刺加固的方法非织造网材；所述隔热层材料为石棉、岩棉、玻璃纤维、硅酸铝纤维、高硅氧纤维和氧化铝纤维中的一种或几种；
步骤三、多层氧化石墨烯丙纶基增强平纹组织复合材料制备：所述多层氧化石墨烯丙纶基增强平纹组织复合材料为两层或两层以上，主要目的为增加复合材料内部氧化石墨烯丙纶含量；通过针刺加固将氧化石墨烯丙纶基增强平纹组织复合材料进行正反2次针刺加固，针刺密度为90-130刺/cm2，针刺频率220-280刺/min，第一次植针密度为2500枚/m，第二次植针密度为2500枚/m，针刺纤网的速度分别为1.8-2.0m/min；
步骤四、树脂复合材料制备：所述树脂复合材料为环氧树脂，将环氧树脂和固化剂按照质量比2：1称取，在45-60℃下预热10min，加入环氧树脂质量分数3-5％硅烷偶合剂及质量分数3-5％氧化石墨烯N-甲基吡咯烷酮分散液(0.5％)，搅拌10min，45-60℃抽真空30-40min，去除环氧树脂中气泡；在环氧树脂中依次加入环氧树脂质量分数1-2％的促进剂、丙酮，搅拌混合均匀，将多层氧化石墨烯丙纶基增强平纹组织复合材料浸入，加入环氧树脂质量分数40％的固化剂，充分搅拌均匀，45-60℃抽真空30-40min，去除气泡；放入鼓风干燥箱中：常温2h,然后温度为95℃-120℃下4h进行固化,最终得到氧化石墨烯丙纶耐热高强复合型材。
3.根据权利要求2所述的氧化石墨烯丙纶耐热高强复合型材的制备方法，其特征在于：所述步骤四中，加入的固化剂为脂肪胺类、芳香族、脂肪环类、改性胺类、酸酐类、低分子聚酰胺和潜伏性胺固化剂其中一种或几种。
4.根据权利要求2所述的氧化石墨烯丙纶耐热高强复合型材的制备方法，其特征在于：所述步骤四中，加入的硅烷偶合剂为硅烷偶联剂KH-560、硅烷偶联剂A-172、复合型铝钛偶联剂其中一种或几种。
5.根据权利要求2所述的氧化石墨烯丙纶耐热高强复合型材的制备方法，其特征在于：所述步骤四中，加入的环氧促进剂为环氧促进剂XH-610、环氧促进剂DMP-30、巴斯夫E-6623、环氧固化促进剂EM-7604H其中一种或几种。
CN201710138429.0A 2017-03-09 2017-03-09 一种氧化石墨烯丙纶耐热高强复合型材及其制备方法 Pending CN106947215A (zh)

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