CN108018719A - 一种水分散性短切碳纤维及其制备方法 - Google Patents

一种水分散性短切碳纤维及其制备方法 Download PDF

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CN108018719A
CN108018719A CN201610963453.3A CN201610963453A CN108018719A CN 108018719 A CN108018719 A CN 108018719A CN 201610963453 A CN201610963453 A CN 201610963453A CN 108018719 A CN108018719 A CN 108018719A
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邓文彬
黄翔宇
王彪
王永梅
沈海娟
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China Petroleum and Chemical Corp
Sinopec Shanghai Petrochemical Co Ltd
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Sinopec Shanghai Petrochemical Co Ltd
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Abstract

本发明公开了一种水分散性短切碳纤维及其制备方法。本发明通过将碳纤维依次进行电化学阳极氧化处理、上浆、干燥及切断而成。本发明的碳纤维具有良好的集束性、可切割性和水分散性，与水的接触角为60°～80°，碳纤维长度2～12mm。本发明水分散性碳纤维处理方法简单，生产成本低，具有很高的市场应用价值。该短切碳纤维可用于湿法抄纸工艺，制备的碳纤维纸或碳纤维复合纸可应用于燃料电池的电极材料、电磁屏蔽材料、电发热材料和复合材料等领域。

Description

一种水分散性短切碳纤维及其制备方法
技术领域
本发明碳纤维处理技术领域，具体的说，涉及一种水分散性短切碳纤维及其制备方法。
背景技术
通过将碳纤维分散在基体树脂中来制备的碳纤维增强复合材料，在轻质、机械性能、尺寸稳定性、导电性等方面具有良好的性能。因此，这种复合材料被广泛应用在比如汽车、飞机、电气或电子装置、光学仪器、精密仪器、娱乐玩具和游戏、家庭或办公用品、建筑材料等领域。对这种复合材料的需求逐年上涨。同时含有碳纤维的纸或复合纸在电发热、电磁波屏蔽等领域也得到快速发展。获得这种碳纤维增强复合材料或纸的方法之一是在水中处理碳纤维比如运用湿法抄纸工艺，比如将短切碳纤维分散在水中，然后通过粘合、缠绕或缝合将短切碳纤维凝固在基体树脂或其它纤维(如木浆纤维)中。另外在最近几年，抄纸法被作为一种方法来获得用在燃料电池中的气体扩散层。
在造纸过程中，碳纤维被提前切成短切碳纤维，然后被分散在分散介质中，最后进行抄纸。当集束性能和纤维硬挺度差的时候，碳纤维切断可操作性差，导致纤维长度短于预定的长度。另外，在抄纸过程中碳纤在水中必须具有极好的分散性。用在电极气体扩散层时，分散性越好，导电性越好。
因此，碳纤维被应用到抄纸过程中时需要同时具有(1)集束性；(2)可切割性，即需要一定的硬挺度，(3)极好的分散性：在抄纸过程中，当碳纤维进入到水中时，可以迅速的分散成单纤的形式，并且抑制碳纤维二次聚集。
环氧树脂类的上浆剂是碳纤维常用上浆材料，对于抄纸过程来说，其集束性能太高，不适合用于抄纸工艺。涂覆水性化合物上浆剂的碳纤维分散性有提高，但切割性能差。本发明采用电化学处理与表面上浆相结合的方法，工艺简单且连续性强，使碳纤维具有了良好切割性和水分散性，可广泛应用于抄纸过程。
发明内容
为了克服现有技术的不足，本发明的目的在于提供一种水分散性碳纤维及其制备方法。其目的在于使碳纤维具有良好的水分散性。本发明制备方法包括了电化学氧化及上浆的处理过程；得到的水分散性碳纤维同时具有良好集束性、可切割性和极好的水分散性。
为实现上述发明目的，本发明采用的技术方案具体如下。
本发明提供一种水分散性短切碳纤维的制备方法，具体步骤如下：
1)对碳纤维进行电化学阳极氧化处理；
2)将电化学阳极氧化处理后的碳纤维上浆；
3)上浆后的碳纤维进行干燥、短切。
上述步骤1)中，所述碳纤维的单丝含量为1K-48K。
上述步骤1)中，电化学阳极氧化处理时，以铵盐为电解质，碳纤维为正极，石墨棒为负极，电解质浓度为0.5～1.5mol/L，电流密度为0.3～3mA/cm2，电解时间为2～3min。优选的，铵盐为磷酸氢二铵或者碳酸氢铵。
上述步骤2)中，所述上浆过程所用的上浆剂是包括表面活性剂、成膜剂、抗静电剂和扩散剂的水性乳液；上浆剂的固含量为0.5wt％～5wt％。优选的，表面活性剂为聚乙二醇、聚丙烯酰胺、聚氧乙烯月桂醇醚、吐温60、椰油酰胺丙基甜菜碱CAB-35中的一种或几种，其用量为上浆剂质量的0.02-5％；成膜剂为环氧树脂乳液、聚乙酸乙烯酯乳液、聚氨酯乳液或淀粉溶液中的一种或几种，其用量为上浆剂质量的2-15％；所述抗静电剂和扩散剂选自烷基三甲基氯化铵、壬酸酰胺、磷酸酯类、四乙烯戊胺及其衍生物、小苏打等中的一种或几种，其用量分别为上浆剂的0.01-1.5％。
上述步骤2)中，碳纤维的上浆率在0.2wt％-5wt％之间。
上述步骤2)中，上浆后的干燥方式为热辊、热风或红外，温度为80～100℃。
上述步骤3)中，短切后的碳纤维长度2～12mm。
本发明还提供一种上述制备方法得到的水分散性短切碳纤维，碳纤维表面氧含量O/C在0.16-0.32；与水的接触角为60°-80°；分散时间为5-35s。
和现有技术相比，本发明的有益效果在于：
1)本发明方法操作简单，可连续性操作，得到的碳纤维可大幅改善碳纤维的水分散性。
2)本发明所用原料便宜易得，具有很高的市场应用价值。
具体实施方式
下面结合具体实施方式，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例中，分散性评价标准是：一束碳纤维被切成长度约为2～12mm。这个短切碳纤维用来作为评价的样品。首先，在直径约为150mm高度约为300mm的烧杯中加入2000cc的水。以约0.01g短切碳纤维作为样品，加入盛水的烧杯中。同时，用搅拌器在200rpm下持续搅拌样品。随着时间的变化，可以看到短切碳纤维沉到水下。结合评价标准，测量碳纤维束在水中充分分散的时间(s)。当碳纤维束包含少于10根单纤的时候可以视其为充分分散。在本发明中，以上过程重复20次，总时间除以20得到平均值(分散时间)。分散时间越短，分散性越好。另外，300s后还未分散的话，实验可以停止。
实施例1
一种水分散性碳纤维的制备方法，将碳纤维直接进入电解池，电解液为1mol/L的碳酸氢铵，电流密度为0.3mA/cm2，石墨棒作为负极，碳纤维作为正极，电解时间为90s。电化学处理后的碳纤维通过水洗槽，水为常温下的自来水，然后通过100℃的干燥炉进行干燥，接着通过上浆槽进行上浆，采用浸渍上浆的方法，上浆剂固含量为5wt％，表面活性剂为聚乙二醇和聚氧乙烯月桂醇醚(3：2，占上降剂含量的2.5％)，成膜剂为淀粉水溶液(占上降剂含量为10％)，抗静电剂和扩散剂为烷基三甲基氯化铵、壬酸酰胺的混合液(占上降剂含量为0.05％％),然后通过干燥箱进行干燥，干燥温度为80℃。将处理好的碳纤维切成长度为4mm，进行水分散性实验。通过上述方式接入碳纤维表面上的氧含量(O)与碳(C)之比与碳纤维的亲水性密切相关，其中(O)的含量通过以光电子能谱(XPS)测定。本制备方法制得的碳纤维(O/C)含量为0.25，与水的接触角为65°，分散时间为25s。
实施例2
一种水分散性碳纤维的制备方法，一种水分散性碳纤维的制备方法，将碳纤维直接进入电解池，电解液为1mol/L的磷酸氢二铵，电流密度为0.3mA/cm2，石墨棒作为负极，碳纤维作为正极，电解时间为90s。电化学处理后的碳纤维通过水洗槽，水为常温下的自来水，然后通过100℃的干燥炉进行干燥，接着通过上浆槽进行上浆，上浆剂固含量为5wt％，采用浸渍上浆的方法，表面活性剂为吐温60(占上降剂含量的2.0％)，成膜剂为聚乙酸乙烯酯乳液(占上降剂含量为12％)，抗静电剂和扩散剂为四乙烯戊胺和小苏打的混合液(占上降剂含量为0.1％)然后通过干燥箱进行干燥，干燥温度为100℃。将处理好的碳纤维切成长度为4mm，进行水分散性实验。制得的碳纤维表面氧O/C含量为0.28，与水的接触角为60°，分散时间为20s。

Claims (10)

1.一种水分散性短切碳纤维的制备方法，其特征在于，具体步骤如下：
1)对碳纤维进行电化学阳极氧化处理；
2)将电化学阳极氧化处理后的碳纤维上浆；
3)上浆后的碳纤维进行干燥、短切，得到水分散性短切碳纤维。
2.根据权利要求1所述的制备方法，其特征在于，步骤1)中，碳纤维的单丝含量为1K-48K。
3.根据权利要求1所述的制备方法，其特征在于，步骤1)中，电化学阳极氧化处理时，以铵盐为电解质，碳纤维为正极，石墨棒为负极，电解质浓度为0.5～1.5mol/L，电流密度为0.3～3mA/cm2，电解时间为2～3min。
4.根据权利要求3所述的制备方法，其特征在于，铵盐为磷酸氢二铵或者碳酸氢铵。
5.根据权利要求1所述的制备方法，其特征在于，步骤2)中，上浆过程所用的上浆剂是包括表面活性剂、成膜剂、抗静电剂和扩散剂的水性乳液；上浆剂的固含量为0.5wt％～5wt％。
6.根据权利要求5所述的制备方法，其特征在于，表面活性剂为聚乙二醇、聚丙烯酰胺、聚氧乙烯月桂醇醚、吐温60或椰油酰胺丙基甜菜碱CAB-35中的一种或几种，其用量为上浆剂质量的0.02-5％；成膜剂为环氧树脂乳液、聚乙酸乙烯酯乳液、聚氨酯乳液或淀粉溶液中的一种或几种，其用量为上浆剂质量的2-15％；所述抗静电剂和扩散剂选自烷基三甲基氯化铵、壬酸酰胺、磷酸酯类、四乙烯戊胺及其衍生物或小苏打中的一种或几种，其用量分别为上浆剂质量的0.01-1.5％。
7.根据权利要求1所述的制备方法，其特征在于，步骤2)中，碳纤维的上浆率在0.2wt％-5wt％之间。
8.根据权利要求1所述的制备方法，其特征在于，步骤2)中，上浆后的干燥方式为热辊、热风或红外，温度为80～100℃。
9.根据权利要求1所述的制备方法，其特征在于，步骤3)中，短切后的碳纤维长度2～12mm。
10.一种根据权利要求1-9之一所述的制备方法得到的水分散性短切碳纤维，其特征在于，碳纤维表面氧含量O/C在0.16-0.32；与水的接触角为60°-80°；分散时间为5-35s。
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