CN117601513A - 一种绝热保温纤维棉及其制备方法 - Google Patents

一种绝热保温纤维棉及其制备方法 Download PDF

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CN117601513A
CN117601513A CN202311671862.2A CN202311671862A CN117601513A CN 117601513 A CN117601513 A CN 117601513A CN 202311671862 A CN202311671862 A CN 202311671862A CN 117601513 A CN117601513 A CN 117601513A
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nanofiber membrane
graphene
heat
preparation
polyacrylonitrile
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CN117601513B (zh
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李冬至
高培尧
高贺伟
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Huamei Energy Saving Technology Group Co ltd
Langfang Gerui Giass Wooi Products Co ltd
North China Institute of Aerospace Engineering
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Huamei Energy Saving Technology Group Co ltd
Langfang Gerui Giass Wooi Products Co ltd
North China Institute of Aerospace Engineering
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Abstract

本发明提供了一种绝热保温纤维棉及其制备方法，属于纺织品技术领域。本发明将聚丙烯腈/热塑性聚氨酯共混物与发泡剂混合后获得前驱体纺丝液，进行湿法静电纺丝，得到北极熊毛状蜂窝中空纳米纤维膜；将纳米纤维膜浸渍在石墨烯分散液中，得到石墨烯修饰纳米纤维膜；将石墨烯修饰纳米纤维膜与玻璃棉复合，得到绝热保温纤维棉。本发明制备的纤维棉具备出色的力学性能及优异的绝热保温性能，具有广阔应用前景。

Description

一种绝热保温纤维棉及其制备方法
技术领域
本发明涉及纺织品技术领域，尤其涉及一种绝热保温纤维棉及其制备方法。
背景技术
保持恒定的体温是哺乳动物生存的关键条件之一。动物主要依靠皮毛来抵御严寒。经过时间的更迭，一些动物(如安哥拉兔)的毛发已经进化出惊人的多腔结构特征。头发中的这些空腔充满了静止的空气，使其具有低导热性和优异的绝缘性能。早期，人类直接利用动物的毛或棉花制衣御寒。如今，人们对开发被动式保温纺织品产生了极大的兴趣。保暖纺织品主要通过设计纤维形貌如增加织物的多孔结构，改善织物蓬松度，减少空气流通，降低热传导，从而达到良好的保温效果。
探索具有功能性优势的保暖纺织品，北极熊毛的结构成为研究人员关注的焦点之一。北极熊的毛发有一种独特的结构，由一个中空的核心和一个排列整齐的多孔壳组成，这种中空多孔结构使其具有独特的光学性能，并允许大量静止空气进入，可以有效地减少热量损失，这极大地有助于抵抗热量的传递。现阶段，北极熊的皮毛保暖效果最好，人们对这种仿生结构的隔热纺织品的开发产生了极大的兴趣。冬装里填充的保暖棉，羽绒服和棉服的热反射技术，都采用了北极熊皮毛有关的仿生科技。因此，开发新型绝热保温纺织品，仍具有重要的实用价值。
发明内容
本发明的目的在于提供一种绝热保温纤维棉及其制备方法，所制备的绝热保温纤维棉具备出色的力学性能及优异的绝热保温性能，具有广阔应用前景。
为了实现上述发明目的，本发明提供以下技术方案：
本发明提供了一种绝热保温纤维棉的制备方法，包括以下步骤：
将聚丙烯腈-热塑性聚氨酯共混物、发泡剂和有机溶剂混合，得到前驱体纺丝液；
将所述前驱体纺丝液进行湿法静电纺丝，得到北极熊毛状蜂窝中空纳米纤维膜；
将石墨、分散剂和水混合，将所得混合分散液进行液相剪切剥离，得到石墨烯分散液；
将所述北极熊毛状蜂窝中空纳米纤维膜浸渍在所述石墨烯分散液中，干燥后，得到石墨烯修饰纳米纤维膜；
将所述石墨烯修饰纳米纤维膜与玻璃棉复合，得到绝热保温纤维棉。
优选的，所述聚丙烯腈-热塑性聚氨酯共混物中聚丙烯腈与热塑性聚氨酯的质量比为2～4:1。
优选的，所述有机溶剂包括氯仿、丙酮、乙酸乙酯、二甲基甲酰胺、二氯甲烷、三氯甲烷和乙醇中的至少一种，所述前驱体纺丝液中聚丙烯腈-热塑性聚氨酯共混物的质量分数为10～30wt％。
优选的，所述发泡剂包括MDI；所述发泡剂与聚丙烯腈-热塑性聚氨酯共混物的质量比为1:2～15。
优选的，所述湿法静电纺丝时，前驱体纺丝液的注射速率为20～40mL/h，光纤缠绕速度为20～50cm/min，接收距离为60～120cm。
优选的，所述石墨包括微晶石墨、热膨胀石墨和高定向热解石墨中的至少一种。
优选的，所述分散剂包括N-甲基吡咯烷酮、十二烷基苯磺酸钠、牛黄脱氧胆酸钠和泊洛沙姆中的至少一种，所述分散剂在混合分散液中的质量浓度为0.004～5％。
优选的，所述石墨烯分散液中石墨烯的平均层数为1～20层，所述石墨烯分散液的质量浓度为0.5～15％。
优选的，所述浸渍的时间为10～60min，温度为20～50℃，所述干燥的时间为1～6h，温度为25～70℃；所述玻璃棉的厚度为1mm～1cm。
本发明提供了上述技术方案所述制备方法制备得到的绝热保温纤维棉。
本发明以聚丙烯腈-热塑性聚氨酯共混物作为纺丝前驱体，采用PAN提高TPU纤维的可纺性和力学性能，同时采用湿法纺丝和聚合物溶液发泡相结合的方法制备中空多孔TPU/PAN纤维；在旋转射流中，气泡的扩散和成核在聚合物纤维中形成多腔结构；即当纺丝纤维被挤进凝浴池中时，H2O开始扩散到湿射流中并与发泡剂发生反应，在聚合物溶液的相分离过程中产生CO2，从而形成中空多孔纤维，提高绝热性和保温性能。同时本发明将具有卓越热导性能的二维石墨烯纳米片通过浸涂工艺附着于中空多孔纳米纤维上提升纳米纤维膜的绝热保温性能，且制备的北极熊毛发状纤维具有良好的延展性，可用于具有优异保温性能的纺织品。
此外，玻璃棉具有高隔热性能，不易燃烧，不会随着时间的推移而变质，对身体友好；本发明将纺丝织物与玻璃棉结合，可以在使用相对较薄的玻璃棉的情况下大幅提升纤维棉的绝热保温效果。
附图说明
图1为本发明制备绝热保温纤维棉的流程图。
具体实施方式
如图1所示，本发明提供了一种绝热保温纤维棉的制备方法，包括以下步骤：
将聚丙烯腈-热塑性聚氨酯共混物、发泡剂和有机溶剂混合，得到前驱体纺丝液；
将所述前驱体纺丝液进行湿法静电纺丝，得到北极熊毛状蜂窝中空纳米纤维膜；
将石墨、分散剂和水混合，将所得混合分散液进行液相剪切剥离，得到石墨烯分散液；
将所述北极熊毛状蜂窝中空纳米纤维膜浸渍在所述石墨烯分散液中，干燥后，得到石墨烯修饰纳米纤维膜；
将所述石墨烯修饰纳米纤维膜与玻璃棉复合，得到绝热保温纤维棉。
在本发明中，若无特殊说明，所需制备原料均为本领域技术人员熟知的市售商品。
本发明将聚丙烯腈-热塑性聚氨酯共混物、发泡剂和有机溶剂混合，得到前驱体纺丝液。
在本发明中，所述聚丙烯腈-热塑性聚氨酯共混物(PAN/TPU)中聚丙烯腈与热塑性聚氨酯的质量比优选为2～4:1，更优选为3:1。本发明对所述聚丙烯腈-热塑性聚氨酯共混物的制备方法没有特殊的限定，将聚丙烯腈和热塑性聚氨酯混合即可。
TPU是一种线状嵌段聚合物，具有优异的回弹性、高耐磨性和耐低温性，然而，TPU溶液在水中的相变速率较慢，相应的纤维通常具有较低的结晶性和机械强度；本发明掺入PAN聚合物提高TPU纤维的可纺性和力学性能。
在本发明中，所述发泡剂优选包括二苯基甲烷二异氰酸酯(MDI)；所述发泡剂与聚丙烯腈-热塑性聚氨酯共混物的质量比优选为1:2～15，更优选为1:5～10。
在本发明中，所述有机溶剂优选包括氯仿、丙酮、乙酸乙酯、二甲基甲酰胺、二氯甲烷、三氯甲烷和乙醇中的至少一种，当所述有机溶剂为上述中两种以上时，本发明对不同种类有机溶剂的配比没有特殊的限定，根据实际需求调整即可；所述前驱体纺丝液中聚丙烯腈-热塑性聚氨酯共混物的质量分数优选为10～30wt％，更优选为15～25wt％，进一步优选为20wt％。
本发明优选将聚丙烯腈-热塑性聚氨酯共混物溶于有机溶剂中后，加入发泡剂；所述混合的温度优选为40～50℃，时间优选为5～6h，更优选为5.5h；所述混合优选在搅拌条件下进行；本发明对所述搅拌没有特殊限定，按照本领域熟知的过程进行即可。
得到前驱体纺丝液后，本发明将所述前驱体纺丝液进行湿法静电纺丝，得到北极熊毛状蜂窝中空纳米纤维膜。
在本发明中，所述湿法静电纺丝时，前驱体纺丝液的注射速率优选为20～40mL/h，更优选为25～30mL/h；光纤缠绕速度优选为20～50cm/min，更优选为25～40cm/min；接收距离优选为60～120cm，更优选为70～100cm。
本发明优选将所述前驱体纺丝液装入注射泵中进行湿法静电纺丝，凝浴池所用试剂优选为水，将所得纤维膜进行常温干燥后，得到北极熊毛状蜂窝中空纳米纤维膜。
本发明通过静电纺丝制备的北极熊毛状蜂窝中空纳米纤维膜，具有较高的比表面积，浸渍石墨烯纳米片的中空纤维比表面积大，中空纤维间的空隙较多，含气量大，因而绝热性好，具有优异的保温性能。
本发明将石墨、分散剂和水混合，将所得混合分散液进行液相剪切剥离，得到石墨烯分散液。
在本发明中，所述石墨优选包括微晶石墨、热膨胀石墨和高定向热解石墨中的至少一种，当所述石墨为上述两种以上时，本发明对不同种类石墨的配比没有特殊的限定，根据实际需求调整即可。
在本发明中，所述分散剂优选包括N-甲基吡咯烷酮、十二烷基苯磺酸钠、牛黄脱氧胆酸钠和泊洛沙姆中的至少一种，当所述分散剂为上述两种以上时，本发明对不同种类分散剂的配比没有特殊的限定，根据实际需求调整即可；所述分散剂在混合分散液中的质量浓度优选为0.004～5％，更优选为0.06～0.5％。
在本发明中，所述水优选为超纯水；本发明对所述水的用量没有特殊的限定，根据实际需求调整保证液相剪切分散顺利进行即可。
在本发明中，所述液相剪切剥离所用仪器优选为纳米珠磨机、棒销式砂磨机、涡轮式砂磨机和高压均质机中的至少一种，所述液相剪切剥离的时间优选为10～90min，更优选为30～80min，进一步优选为40～60min；研磨转速优选为600～3200r/min，更优选为800～2500r/min，进一步优选为1000～2000r/min，研磨时间优选为0.5～5h，更优选为1～3h，进一步优选为1.2～1.5h。
在本发明中，所述石墨烯分散液中石墨烯的平均层数优选为1～20层，更优选为8～15层，进一步优选为10～12层，所述石墨烯分散液的质量浓度优选为0.5～15％，更优选为2～12％，进一步优选为3～8％。
得到石墨烯分散液后，本发明将所述北极熊毛状蜂窝中空纳米纤维膜浸渍在所述石墨烯分散液中，干燥后，得到石墨烯修饰纳米纤维膜。
在本发明中，所述浸渍的时间优选为10～60min，更优选为30～40min；温度优选为20～50℃，更优选为30～40℃；所述干燥的时间优选为1～6h，更优选为2～4h，温度优选为25～70℃，更优选为30～60℃。本发明对所述北极熊毛状蜂窝中空纳米纤维膜与石墨烯分散液的用量比没有特殊的限定，根据实际浸渍条件确定负载量即可。
得到石墨烯修饰纳米纤维膜后，本发明将所述石墨烯修饰纳米纤维膜与玻璃棉复合，得到绝热保温纤维棉；所述石墨烯修饰纳米纤维膜与玻璃棉的厚度比优选为1:10～30，更优选为1:15～25，进一步优选为1:20。
本发明优选通过喷涂热固性树脂将石墨烯修饰纳米纤维膜与玻璃棉复合；所述热固性树脂优选为酚醛树脂、脲醛树脂或三聚氰胺-甲醛树脂。本发明对所述喷涂以及热固性树脂的用量没有特殊的限定，按照本领域熟知的过程喷涂实现复合即可。
在本发明中，所述玻璃棉的厚度优选为1mm～1cm，更优选为5～7mm。
本发明提供了上述技术方案所述制备方法制备得到的绝热保温纤维棉。
本发明将石墨烯纳米片锚定于纤维表面，能够提高纤维的比表面积，同时石墨烯材料拥有优异的保温性能，因而将石墨烯纳米片锚定于纤维表面能极大提升纳米纤维膜整体的绝热保温性能，而与玻璃棉结合后其绝热保温效果更佳。
下面结合实施例对本发明提供的技术方案进行详细的说明，但是不能把它们理解为对本发明保护范围的限定。
实施例1
本实施例中绝热保温纤维棉的制备方法，包括以下步骤：
S1.制备前驱体纺丝液：将2gPAN/TPU共混物(所述PAN与TPU的质量比为3:1)于18g二甲基甲酰胺中溶解后，形成质量分数为10wt％的溶液，后加入1gMDI，在40℃下磁力搅拌6h后，得到前驱体纺丝液；
S2.制备北极熊毛状蜂窝中空纳米纤维膜：将所得前驱体纺丝液装入注射泵中进行湿法静电纺丝，注射速率为20mL/h，光纤缠绕速度为20cm/min，接收距离为60cm，凝浴池中为去离子水，将所得纤维膜进行常温干燥后，得到北极熊毛状蜂窝中空纳米纤维膜；
S3.制备石墨烯分散液：将石墨(微晶石墨，5g)与0.05g分散剂(N-甲基吡咯烷酮/十二烷基苯磺酸钠的质量比为2:1)置于1L的超纯水中搅拌均匀，采用液相剪切剥离(纳米珠磨机，搅拌处理时间为30min，研磨转速为800r/min，研磨时间为1.5h)制备石墨烯分散液，所得石墨烯分散液中石墨烯平均层数为10层，石墨烯分散液的质量浓度为3％；
S4.制备石墨烯修饰的仿生结构纳米纤维膜：将所得纳米纤维膜浸渍在所得石墨烯分散液中(浸渍处理时间为10min，处理温度为50℃)，浸渍处理后放置于25℃烘箱中干燥6h，得到石墨烯修饰的仿生结构纳米纤维膜；
S5.制备绝热保温纤维棉：将所得石墨烯修饰的仿生结构纳米纤维膜通过喷涂10mL酚醛树脂与厚度为1cm的玻璃棉复合，石墨烯修饰纳米纤维膜与玻璃棉的厚度比为1:30，得到绝热保温纤维棉。
实施例2
本实施例中绝热保温纤维棉的制备方法，包括以下步骤：
S1.制备前驱体纺丝液：将2gPAN/TPU共混物(所述PAN与TPU的质量比为3:1)于11.3g二氯甲烷中溶解后，形成质量分数为15wt％的溶液，后加入0.4gMDI，在40℃下磁力搅拌6h后，得到前驱体纺丝液；
S2.制备北极熊毛状蜂窝中空纳米纤维膜：将所得前驱体纺丝液装入注射泵中进行湿法静电纺丝，注射速率为25mL/h，光纤缠绕速度为25cm/min，接收距离为70cm，凝浴池中为去离子水，将所得纤维膜进行常温干燥后，得到北极熊毛状蜂窝中空纳米纤维膜；
S3.制备石墨烯分散液：将石墨(热膨胀石墨，10g)与0.125g分散剂(牛黄脱氧胆酸钠)置于1L的超纯水中搅拌均匀，采用液相剪切剥离(纳米珠磨机，搅拌处理时间为40min，研磨转速为1000r/min，研磨时间为1.2h)制备石墨烯分散液，所得石墨烯分散液中石墨烯平均层数为12层，石墨烯分散液的质量浓度为8％；
S4.制备石墨烯修饰的仿生结构纳米纤维膜：将所得纳米纤维膜浸渍在所得石墨烯分散液中(浸渍处理时间为60min，处理温度为20℃)，浸渍处理后放置于30℃烘箱中干燥4h，得到石墨烯修饰的仿生结构纳米纤维膜；
S5.制备绝热保温纤维棉：将所得石墨烯修饰的仿生结构纳米纤维膜通过喷涂10mL脲醛树脂与厚度为7mm的玻璃棉复合，石墨烯修饰纳米纤维膜与玻璃棉的厚度比为1:25，得到绝热保温纤维棉。
实施例3
本实施例中绝热保温纤维棉的制备方法，包括以下步骤：
S1.制备前驱体纺丝液：将2gPAN/TPU共混物(所述PAN与TPU的质量比为2:1)于8g二甲基甲酰胺/二氯甲烷(体积比为3:7)共混物中溶解后，形成质量分数为20wt％的溶液，后加入0.2gMDI，在50℃下磁力搅拌5.5h后，得到前驱体纺丝液；
S2.制备北极熊毛状蜂窝中空纳米纤维膜：将所得前驱体纺丝液装入注射泵中进行湿法静电纺丝(注射速率为30mL/h，光纤缠绕速度为40cm/min，接收距离为100cm)，凝浴池中为去离子水，将所得纤维膜进行常温干燥后，得到北极熊毛状蜂窝中空纳米纤维膜；
S3.制备石墨烯分散液：将石墨(高定向热解石墨，10g)与0.1g分散剂(十二烷基苯磺酸钠)置于1L的超纯水中搅拌均匀，采用液相剪切剥离技术(涡轮式砂磨机，搅拌处理时间为60min，研磨转速为800r/min，研磨时间为5h)制备石墨烯分散液，所得石墨烯分散液中石墨烯平均层数为20层，石墨烯分散液的质量浓度为2％；
S4.制备石墨烯修饰的仿生结构纳米纤维膜：将所得纳米纤维膜浸渍在所得石墨烯分散液中(浸渍处理时间为40min，处理温度为30℃)，浸渍处理后放置于40℃烘箱中干燥2h，得到二维纳米片修饰的仿生结构纳米纤维膜；
S5.制备绝热保温纤维棉：将所得二维纳米片修饰的仿生结构纳米纤维膜通过喷涂10mL三聚氰胺-甲醛树脂与厚度为5mm的玻璃棉复合，石墨烯修饰纳米纤维膜与玻璃棉的厚度比为1:20，得到绝热保温纤维棉。
实施例4
本实施例中绝热保温纤维棉的制备方法，包括以下步骤：
S1.制备前驱体纺丝液：将2gPAN/TPU共混物(所述PAN与TPU的质量比为4:1)于4.66g二甲基甲酰胺中溶解后，形成质量分数为30wt％的溶液，后加入0.135gMDI，在50℃下磁力搅拌5h后，得到前驱体纺丝液；
S2.制备北极熊毛状蜂窝中空纳米纤维膜：将所得前驱体纺丝液装入注射泵中进行湿法静电纺丝，注射速率为40mL/h，光纤缠绕速度为50cm/min，接收距离为120cm，凝浴池中为去离子水，将所得纤维膜进行常温干燥后，得到北极熊毛状蜂窝中空纳米纤维膜；
S3.制备石墨烯分散液：将石墨(热膨胀石墨，20g)与0.6g分散剂(泊洛沙姆)置于1L的超纯水中搅拌均匀，采用液相剪切剥离(纳米珠磨机，搅拌处理时间为30min，研磨转速为2000r/min，研磨时间为1h)制备石墨烯分散液，所得石墨烯平均层数为8层，石墨烯分散液的质量浓度为15％；
S4.制备石墨烯修饰的仿生结构纳米纤维膜：将所得纳米纤维膜浸渍在所得石墨烯分散液中(浸渍处理时间为30min，处理温度为40℃)，浸渍处理后放置于70℃烘箱中干燥1h，得到石墨烯修饰的仿生结构纳米纤维膜；
S5.制备绝热保温纤维棉：将所得石墨烯修饰的仿生结构纳米纤维膜通过喷涂10mL酚醛树脂与厚度为1mm的玻璃棉复合，石墨烯修饰纳米纤维膜与玻璃棉的厚度比为1:10，得到绝热保温纤维棉。
对比例1(不浸渍石墨烯分散液)
将2gPAN/TPU共混物(所述PAN与TPU的质量比为3:1)于18g二甲基甲酰胺中溶解后，形成质量分数为10wt％的溶液，后加入1gMDI，在40℃下磁力搅拌6h后，得到前驱体纺丝液；
将所得前驱体纺丝液装入注射泵中进行湿法静电纺丝(注射速率为20mL/h，光纤缠绕速度为20cm/min，接收距离为60cm)，凝浴池中为去离子水，常温干燥后，得到北极熊毛状蜂窝中空纳米纤维膜；
通过喷涂10mL酚醛树脂将纳米纤维膜与厚度为1cm的玻璃棉复合，纳米纤维膜与玻璃棉的厚度比为1:30，得到绝热保温纤维棉。
对比例2(不添加MDI，即不形成北极熊毛状蜂窝中空纤维)
将2gPAN/TPU共混物(所述PAN与TPU的质量比为3:1)于11.3g二氯甲烷中溶解，在40℃下磁力搅拌6小时后，得到质量分数为15wt％的前驱体纺丝液；
将所得前驱体纺丝液装入注射泵中进行湿法静电纺丝(注射速率为25mL/h，光纤缠绕速度为25cm/min，接收距离为70cm)，凝浴池中为去离子水，将所得纤维膜进行常温干燥后，得到纳米纤维膜；
将石墨(热膨胀石墨，10g)与0.125g分散剂(牛黄脱氧胆酸钠)置于1L的超纯水中搅拌均匀，采用液相剪切剥离(纳米珠磨机，搅拌处理时间为40min，研磨转速为1000r/min，研磨时间为1.2h)制备石墨烯分散液，所得石墨烯平均层数为12层，石墨烯分散液的质量浓度为8％；
将所得纳米纤维膜浸渍在石墨烯分散液中(浸渍处理时间为60min，处理温度为20℃)，浸渍处理后放置于30℃烘箱中干燥4h，得到石墨烯修饰的纳米纤维膜；
通过喷涂10mL脲醛树脂将该纳米纤维膜与厚度为7mm的玻璃棉复合，纳米纤维膜与玻璃棉的厚度比为1:25，得到绝热保温纤维棉。
对比例3(不与玻璃棉复合)
将2gPAN/TPU共混物(所述PAN与TPU的质量比为2:1)于8g二甲基甲酰胺/二氯甲烷(体积比为3:7)共混物中溶解后，形成质量分数为20wt％的溶液，后加入0.2gMDI，在50℃下磁力搅拌5.5h后，得到前驱体纺丝液；
将所得前驱体纺丝液装入注射泵中进行湿法静电纺丝(注射速率为30mL/h，光纤缠绕速度为40cm/min，接收距离为100cm)，凝浴池中为去离子水，将所得纤维膜进行常温干燥后，得到北极熊毛状蜂窝中空纳米纤维膜；
将石墨(高定向热解石墨，10g)与0.1g分散剂(十二烷基苯磺酸钠)置于1L的超纯水中搅拌均匀，采用液相剪切剥离技术(涡轮式砂磨机，搅拌处理时间为60min，研磨转速为800r/min，研磨时间为5h)制备石墨烯分散液，所得石墨烯分散液中石墨烯平均层数为20层，石墨烯分散液的质量浓度为2％；
将所得纳米纤维膜浸渍在所得石墨烯分散液中(浸渍处理时间为40min，处理温度为30℃)，浸渍处理后放置于40℃烘箱中干燥2h，得到石墨烯修饰的仿生结构纳米纤维膜。
结构表征和性能测试
比表面积测试：采用气体吸附仪(ASAP 2060，美国Micromeritics公司)在77K下测量氮气吸附等温线。
拉伸性能测试：将所得材料裁剪后获得拉伸样条，根据美国材料试验协会的ASTMD638-2003中塑料拉伸性能测试标准，使用美国Instron公司的万能拉伸机(型号4403，传感器100N)对复合材料的拉伸性能进行测试。每组至少保证3个平行的测试样品，结果取其平均值。
绝热性能评价：采用热导率测试仪(Hot DiskTPS2500S，瑞典)，根据ISO 22007-2:2015的测试标准，采用瞬态平面源法在Ar气氛中测量样品在室温下的导热系数λ。根据ASTM-E1461-13的测试标准，采用激光闪光法，用导热分析仪(LFA427,Netzsch,Germany)在Ar气氛中测量高温(50～150℃)的λ。
λ的计算公式如下:
λ＝α×ρ×Cp
其中α为热扩散系数，ρ为样品密度，Cp为比热容。
保温性能测试：通过YG 606平板式织物保温仪测定其保温性能；将30mm×30mm的试样包覆在试样架上，盖上外罩，使加热管升温一定时间，然后再定时降温散热，测试过程采用计算机进行控制和数据处理，直接测定并自动计算显示保温率。
以上测试结果见表1和表2。
表1实施例1～4和对比例1～3制备的石墨烯修饰的仿生结构纳米纤维膜的比表面积测试结果
由表1可知，实施例1～4制备得到的石墨烯修饰的仿生结构纳米纤维膜均展现了较高的比表面积，最高可达380.5m2/g，而未浸渍石墨烯纳米片的纤维膜的比表面积仅为70.6m2/g(对比例1)。比表面积越大，静止空气层的表面积也大，因此绝热性能较好。另外，具有中空多孔结构的纤维，纤维间的空隙较多，含气量大，因此具备中空多孔结构的纤维其绝热性能较对比例2中一般纤维会更好。
表2实施例1～4和对比例1～3制备的绝热保温纤维棉的力学性能及保温性能测试结果
由表2可以看出，与玻璃棉复合后，绝热保温纤维棉均展现了极高的抗拉强度(32.5～43.2MPa)，具有优异的力学强度。尤其是实施例1的抗拉强度高至43.2MPa，相较于对比例3，显示出该纤维棉出色的力学性能。
纤维导热性能用导热系数来衡量，导热系数愈大，热传递性愈好，织物的保暖性愈差。导热系数愈小，织物保暖性愈好。从表2可以看出，对比例1和对比例2制备的纤维棉具有较高的导热系数，分别为0.042W/(m·K)和0.045W/(m·K)，均高于实施例1～4，因此保温效果较差。另外，实施例1制备的纤维棉的保温率达到了40.5％，远高于对比例1和对比例2。
综上所述，本发明制备的绝热保温纤维棉具备优异的力学性能和出色的绝热保温性能。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (10)

1.一种绝热保温纤维棉的制备方法，其特征在于，包括以下步骤：
将聚丙烯腈-热塑性聚氨酯共混物、发泡剂和有机溶剂混合，得到前驱体纺丝液；
将所述前驱体纺丝液进行湿法静电纺丝，得到北极熊毛状蜂窝中空纳米纤维膜；
将石墨、分散剂和水混合，将所得混合分散液进行液相剪切剥离，得到石墨烯分散液；
将所述北极熊毛状蜂窝中空纳米纤维膜浸渍在所述石墨烯分散液中，干燥后，得到石墨烯修饰纳米纤维膜；
将所述石墨烯修饰纳米纤维膜与玻璃棉复合，得到绝热保温纤维棉。
2.根据权利要求1所述的制备方法，其特征在于，所述聚丙烯腈-热塑性聚氨酯共混物中聚丙烯腈与热塑性聚氨酯的质量比为2～4:1。
3.根据权利要求1或2所述的制备方法，其特征在于，所述有机溶剂包括氯仿、丙酮、乙酸乙酯、二甲基甲酰胺、二氯甲烷、三氯甲烷和乙醇中的至少一种，所述前驱体纺丝液中聚丙烯腈-热塑性聚氨酯共混物的质量分数为10～30wt％。
4.根据权利要求1所述的制备方法，其特征在于，所述发泡剂包括MDI；所述发泡剂与聚丙烯腈-热塑性聚氨酯共混物的质量比为1:2～15。
5.根据权利要求1所述的制备方法，其特征在于，所述湿法静电纺丝时，前驱体纺丝液的注射速率为20～40mL/h，光纤缠绕速度为20～50cm/min，接收距离为60～120cm。
6.根据权利要求1所述的制备方法，其特征在于，所述石墨包括微晶石墨、热膨胀石墨和高定向热解石墨中的至少一种。
7.根据权利要求1所述的制备方法，其特征在于，所述分散剂包括包括N-甲基吡咯烷酮、十二烷基苯磺酸钠、牛黄脱氧胆酸钠和泊洛沙姆中的至少一种，所述分散剂在混合分散液中的质量浓度为0.004～5％。
8.根据权利要求1所述的制备方法，其特征在于，所述石墨烯分散液中石墨烯的平均层数为1～20层，所述石墨烯分散液的质量浓度为0.5～15％。
9.根据权利要求1所述的制备方法，其特征在于，所述浸渍的时间为10～60min，温度为20～50℃，所述干燥的时间为1～6h，温度为25～70℃；所述玻璃棉的厚度为1mm～1cm。
10.权利要求1～9任一项所述制备方法制备得到的绝热保温纤维棉。
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JP2003193359A (ja) * 2001-12-20 2003-07-09 Kanebo Ltd 断熱材
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