CN116103838A - 一种再生碳纤维/热塑性纤维混合毡及其制备方法 - Google Patents

一种再生碳纤维/热塑性纤维混合毡及其制备方法 Download PDF

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CN116103838A
CN116103838A CN202211739587.9A CN202211739587A CN116103838A CN 116103838 A CN116103838 A CN 116103838A CN 202211739587 A CN202211739587 A CN 202211739587A CN 116103838 A CN116103838 A CN 116103838A
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杨斌
李鑫
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Nantong Fuyuan New Mstar Technology Ltd
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Abstract

本发明涉及碳纤维回收再利用技术领域，提供了性能优异一种再生碳纤维/热塑性纤维混合毡及其制备方法，包括：S1、本发明首先在回收过程中对再生碳纤维表面预活性化处理；S2、在使用非织造技术制备混合毡的铺网过程中，以雾状逐层向网胎喷洒上浆剂的0.1‑0.5％稀的水溶液，然后趁湿针刺，避免了再生碳纤维发生断裂；S3、利用安装在收卷机之前的红外干燥设备干燥，最后收卷、包装。该制备方法能大幅度提高再生碳纤维和热塑纤维树脂的界面结合力，且碳纤维断裂损伤率低，系统内不引入第三种杂质粘结剂，可制备力学性能优异的再生碳纤维增强热塑性复合材料，该制备方法成本低且易于工业化生产。

Description

一种再生碳纤维/热塑性纤维混合毡及其制备方法
技术领域
本发明涉及碳纤维回收再利用技术领域，具体涉及一种界面结合性优异的再生碳纤维/热塑性纤维混合毡及其制备方法。
背景技术
具有足够长度的再生碳纤维能够和热塑性纤维混合通过针刺工艺制备混合毡，再模压得到力学性能优异的再生碳纤维毡/热塑性复合材料，可以再利用到航空、汽车、高铁的次承力结构部件上，有极高的二次利用价值。影响再生碳纤维毡/热塑性复合材料力学性能的有两个关键因素：一、碳纤维长度；二，碳纤维与热塑性纤维树脂的界面结合性。
常规针刺法容易使碳纤维断裂，为了避免断裂有人采用热熔胶粘结，这样引入了第三种杂质成分，带来力学性能下降、成本增加、且过程不环保。在提高碳纤维与热塑性纤维树脂的界面结合性方面，已有电化学氧化、等离子辐照等技术，这些并不适合非连续的再生碳纤维，带来操作复杂、成本增加或无法满足均匀性；而有人提出先上浆或者事先用某种化合物处理、再制毡，这种方法完全不可行，因为直径仅5-7微米的碳纤维将被上浆剂粘结成团簇状，无法在制毡过程中被分散成单纤维形态，如果强行拆分将导致纤维断裂。
因此，需要开发一种新的混合毡制备技术，该技术能大幅度提高再生碳纤维和热塑纤维树脂的界面结合力，且碳纤维断裂损伤率低，且系统内不引入第三种杂质粘结剂。
发明内容
本发明提供一种界面结合性优异的再生碳纤维/热塑性纤维混合毡及其制备方法，以期解决现有技术中的一个或多个技术问题。
本发明采用如下技术方案：
一种再生碳纤维/热塑性纤维混合毡的制备方法，包括以下步骤：
S1、在回收过程中对再生碳纤维表面预活性化处理；
S2、在使用非织造技术制备混合毡的铺网过程中，以雾状逐层向网胎喷洒上浆剂的0.1％-0.5％稀释水溶液，趁湿针刺；
S3、使用安装在收卷机之前的红外干燥设备对产品进行干燥，最后收卷、包装。
所述的在回收过程中对再生碳纤维表面预活性化处理过程，具体包括：在通过热解回收工艺从废弃碳纤维复合材料中回收提取碳纤维的生产过程后段，垂直于纤维床层移动方向，以1-30m/s的气速连续吹入常温空气1-30min；进行活化的区域为当再生纤维表层温度降到100-200℃的区域。
其中：预活性化处理过程中，氧化性气体常温空气要垂直吹过碳纤维床层，一方面使气体充分渗透到每一根碳纤维使其充分活性化，另一方面还能够将内部的热气流带入到较低温度的表层，加热表层碳纤维使其也能充分活性化。
其次，控制垂直吹入氧化性气体的气速为1-30m/s，优选5-20m/s；吹入常温空气1-30min；优选2-20min，再优选为3-10min。要控制在再生碳纤维表层温度降到100-200℃的区域内，优选120-180℃。
该预活性化处理的原理为：再生碳纤维经过充分和氧化性气体接触反应后，在表面易生成大量羧基(—COOH)和羟基(—OH)官能团，使其非常容易地与后续上浆剂中的酰胺键、异氰酸酯等基团发生化学反应，形成牢固的化学键合。
在使用非织造技术制备混合毡的铺网过程中，以雾状逐层向网胎喷洒上浆剂的0.1-0.5％稀的水溶液，然后趁湿针刺，可避免碳纤维发生断裂。；
上浆剂的喷洒装置是自行安装在铺网机上部、能够来回自动移动的细孔花洒，通过调节出口剂量喷出上浆剂呈雾状。对每一层网胎喷淋上浆剂，喷洒一层、叠合一层，然后趁湿进行针刺，极大减少了针刺中引起的再生碳纤维断裂。这也是本发明的意外收获。
所述上浆剂种类可根据热塑纤维种类决定，优先选择与热塑纤维亲和性好、相容性高或者/和反应活性高的商品化化合物。比如对于尼龙纤维，可选水性聚氨酯、水性聚酰胺等；对于PP纤维，可选马来酸酐接枝PP的水性乳液；对于PBT或PET纤维，可选择水性聚氨酯、水性环氧乳液等。
S2中所述的在使用非织造技术制备混合毡过程，包括将预活性化的再生碳纤维和热塑性纤维先切割成38-100毫米，按照所需比例进行预混合，通过预开松、混合、二次开松、梳理、铺网、针刺成毡。所述的再生碳纤维质量含量为1-99％。混合毡面密度为50-2000gsm。
再生碳纤维和热塑性纤维先切割成38-100毫米，优选切割长度为70-100毫米。如果纤维长度小于38毫米，常规的针刺法无法制毡，尤其对于碳纤维难度更大，因碳纤维模量高、报合力差；如果纤维长度大于100毫米，难以均匀分散，常规的针刺法无法制毡。
再生碳纤维质量含量为0.1-99.9％，还可以制备100％碳纤维毡，这只代表了技术能力。再生碳纤维含量越高，针刺毡越难制备。实际混合毡中再生碳纤维/热塑纤维的比例，会根据性能和成本综合决定，一般优选再生碳纤维含量为10-50％。
混合毡面密度为50-2000gsm；优选100-1000gsm；再优选200-800gsm。
步骤S3中，所述的红外干燥设备为大功率快干外红灯光源，功率1000-2000W，工作温度40-200℃，带有温控装置。干燥时间为5-60秒。
外红灯光源功率为1000-2000W，功率高是为了加速干燥时间，功率如果小于1000W，干燥慢、时间长、影响生产效率；功率如果大于2000W，则费电且设备容易坏。所以功率为1000-2000W，优选功率为1200-1800W。
工作温度40-200℃，上浆剂干燥主要去除的是水溶液，原则上温度大于100度即可。工作温度如果小于40℃，则干燥慢、时间长、影响生产效率；工作温度如果大于200℃，则容易引起某些种类的上浆剂变质。
干燥时间为5-60秒。如果小于5秒，容易干燥不够均匀；如果大于60秒，干燥时间长、影响生产效率。优选干燥时间为10-40秒。
所述基体树脂为热固性树脂或热塑性树脂中的一种或多种；所述热固性树脂包括环氧树脂、不饱和聚酯树脂、聚氨酯树脂、酚醛树脂、聚酰亚胺树脂、脲醛树脂、三聚氰胺甲醛树脂、有机硅树脂或呋喃树脂；所述热塑性树脂包括聚苯硫醚、聚醚醚酮、聚砜、热塑性聚酰亚胺、聚芳酯、液晶聚合物、聚四氟乙烯、聚碳酸酯、聚对苯二甲酸乙二醇酯、聚对苯二甲酸工二醇酯、聚甲醛、聚酰胺、聚苯醚、聚乙烯、聚丙烯、聚氯乙烯或聚苯乙烯及丙烯腈-丁二烯-苯乙烯共聚物；所述碳纤维包括聚丙烯腈基碳纤维、沥青基碳纤维或黏胶基碳纤维中的一种或多种。
所述热解回收工艺包括常规高温热解法和微波热解法；所述热解法的氛围气包括氮气、水蒸气、二氧化碳气体；所述常规高温热解法包括一步法和两步法。
所述回收生产的再生碳纤维是表面无积炭残留的柔软质感再生碳纤维。
本发明的有益效果是：与现有技术相比，本发明的制备方法能大幅度提高再生碳纤维和热塑纤维树脂的界面结合力，且碳纤维断裂损伤率低，系统内不引入第三种杂质粘结剂，可制备力学性能优异的再生碳纤维增强热塑性复合材料，该制备方法成本低且易于工业化生产。
附图说明
图1是本发明实施例1提供的复合材料的SEM照片，
图2是本发明对比例1提供的复合材料的SEM照片。
具体实施方式
下面通过实施方式对本发明进行进一步详细的说明。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
实施例1
一种再生碳纤维/热塑性纤维混合毡，其由以下方法制得：
S1、在回收生产再生碳纤维过程中对再生碳纤维进行预活性化处理，具体包括在通过热解回收工艺从废弃碳纤维复合材料中回收提取碳纤维的生产过程后段，即在该再生纤维出炉前的阶段、当再生纤维表层温度降到200℃的区域，垂直于纤维床层移动方向，以5m/s的气速连续吹入空气5min，得到预活性化再生碳纤维；
S2、将再生碳纤维(RCF)和热塑性纤维(PP纤维)短切成80毫米，制备RCF与PP的质量比为40/60，按照常规针刺工艺预混合、预开松、混合、二次开松、梳理、铺网、针刺成毡，面密度270gsm，其中在铺网过程中雾状喷洒浓度为0.5％的马来酸酐接枝PP(MAH-PP)水性乳液上浆剂；
S3、红外干燥条件是红外干燥设备功率1500W，工作温度100℃，干燥时间为40秒；
S4、碳纤维增强聚丙烯树脂基复合材料的制备：将RCF/PP纤维毡分别沿纵向(MD)和横向(TD)裁剪成热压成型的试样，将8层剪好的CF/PP纤维毡试样顺序铺层，之后在230℃、10MPa下进行180s的热压，然后在压力为8MPa下冷压90s，得到碳纤维增强聚丙烯树脂基复合材料。
实施例2
该实施例的制备过程与实施例1大体相同，区别仅在于，将步骤S1中预活性化的操作调整为：垂直于纤维床层移动方向以15m/s的气速连续吹入空气10min。
实施例3
该实施例的制备过程与实施例1大体相同，区别仅在于，将步骤S2中上浆剂的浓度调整为0.1％。
对比例1
该对比例的制备过程与实施例1大体相同，区别仅在于，不包括步骤S1，其将未经过表面活化的再生碳纤维直接与热塑性纤维进行混合加工，依照步骤S2-S4，制得复合材料。
对比例2
该对比例的制备过程与实施例1大体相同，区别仅在于，不包括步骤S2及S3，其将经过表面活化的再生碳纤维直接热压，制备得到复合材料。
对比例3
取再生碳纤维直接热压，制备得到复合材料。
取实施例1-3和对比例1-3提供的复合材料，对其分别进行力学性能测试，结果如下表所示。
Figure BDA0004032249190000061
根据表中数据可知，本发明实施例1-3由于再生碳纤维/PP之间优异的界面结合性能，制备的混合毡复合材料力学性能优异，拉伸强度达到526-560.4MPa，模量38.32-41.3GPa，弯曲强度435.6-480.8MPa，弯曲模量30.9-32.45GPa；相关性能远高于对比例，且几乎是对比例3的3-4倍。
本领域的技术人员可以明确，在不脱离本发明的总体精神以及构思的情形下，可以做出对于以上实施例的各种变型。其均落入本发明的保护范围之内。本发明的保护方案以本发明所附的权利要求书为准。

Claims (8)

1.一种再生碳纤维/热塑性纤维混合毡的制备方法，其特征在于，包括以下步骤：
S1、在回收过程中对再生碳纤维表面预活性化处理；
S2、在使用非织造技术制备混合毡的铺网过程中，以雾状逐层向网胎喷洒上浆剂的0.1％-0.5％稀释水溶液，趁湿针刺；
S3、使用安装在收卷机之前的红外干燥设备对产品进行干燥，最后收卷、包装。
2.根据权利要求1所述再生碳纤维/热塑性纤维混合毡的制备方法，其特征在于，步骤S1具体包括：在通过热解回收工艺从废弃碳纤维复合材料中回收提取碳纤维的生产过程后段，垂直于纤维床层移动方向，以1-30m/s的气速连续吹入常温空气1-30min，当再生纤维表面温度降到100-200℃时，对其进行预活化处理。
3.根据权利要求1所述再生碳纤维/热塑性纤维混合毡的制备方法，其特征在于，步骤S2中，所述使用非织造技术制备混合毡的铺网过程具体为：包括将预活性化的再生碳纤维和热塑性纤维先切割成38-100毫米，进行预混合后，通过预开松、混合、二次开松、梳理、铺网、针刺成毡；其中，所述再生碳纤维的重量占比为0.1-99.9％，混合毡的面密度为50-2000gsm。
4.根据权利要求1所述再生碳纤维/热塑性纤维混合毡的制备方法，其特征在于，步骤S3中，所述红外干燥装置为大功率快干外红灯光源，其功率为1000-2000W，工作温度为40-200℃，且具有温控功能；步骤S3中的干燥时间为5-60秒。
5.根据权利要求2所述再生碳纤维/热塑性纤维混合毡的制备方法，其特征在于，所述废弃碳纤维复合材料包括基体树脂和碳纤维；所述基体树脂为热固性树脂或热塑性树脂中的一种或多种；所述热固性树脂为环氧树脂、不饱和聚酯树脂、聚氨酯树脂、酚醛树脂、聚酰亚胺树脂、脲醛树脂、三聚氰胺甲醛树脂、有机硅树脂、呋喃树脂中的一种或多种；所述热塑性树脂包括聚苯硫醚、聚醚醚酮、聚砜、热塑性聚酰亚胺、聚芳酯、液晶聚合物、聚四氟乙烯、聚碳酸酯、聚对苯二甲酸乙二醇酯、聚对苯二甲酸工二醇酯、聚甲醛、聚酰胺、聚苯醚、聚乙烯、聚丙烯、聚氯乙烯、聚苯乙烯及丙烯腈-丁二烯-苯乙烯共聚物中的一种或多种；所述碳纤维为聚丙烯腈基碳纤维、沥青基碳纤维、黏胶基碳纤维中的一种或多种。
6.根据权利要求2所述再生碳纤维/热塑性纤维混合毡的制备方法，其特征在于，所述热解回收工艺为常规高温热解法或微波热解法；所述微波热解法的氛围气为氮气、水蒸气或二氧化碳气体；所述常规高温热解法为一步热解法或两步热解法。
7.根据权利要求1所述再生碳纤维/热塑性纤维混合毡的制备方法，其特征在于，所述再生碳纤维为表面无积炭残留的柔软质感再生碳纤维。
8.一种再生碳纤维/热塑性纤维混合毡，其特征在于，其按照权利要求1-7任一项所述的制备方法制备而得。
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