CN110205709A - 一种高性能中间相沥青基碳纤维的制备方法 - Google Patents
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Abstract
本发明涉及一种高性能中间相沥青基碳纤维的制备方法，用恒电位电解法制备磷掺杂碳烯量子点，电解体系的阳极是石墨棒，阴极为Pt电极，电解后通过微孔过滤膜过滤，得到滤液，经去离子水水洗干燥、真空干燥得到磷掺杂碳烯量子点的固体。通过磷掺杂碳烯量子点对中间相沥青进行修饰，用甲苯分散磷掺杂碳烯量子点配置浓度，再和中间相沥青在280‑350ºC混合惰性气氛下搅拌后进行纺丝。纺丝后进行预氧化处理、低温炭化处理和连续石墨化处理得到中间相沥青基碳纤维。本发肯制备的碳纤维的模量为800‑960GPa，导热率为600‑900W/m·K，纤维界面为典型的辐射状结构，不存在劈裂，工艺性能好，是一种良好的“碳转辊”增强材料。
Description
技术领域
本发明涉及一种可用于功能性薄膜制造领域所需转辊的高性能中间相沥青基碳纤维的制备方法。
背景技术
新一代大尺寸薄膜制造用的转辊，搭载机器后转速高达800m/min，需要在100-200℃高温下具有和室温下相同精度。中间相沥青基碳纤维具备高强高模和高导热的特点，近几年成为LCD制造的各种功能性薄膜制造领域最有潜力的材料之一。以中间相沥青基碳纤维为增强体的碳纤维转辊具有高强度高模量的特点，搭载机器后可以800r/min的超高转速运转，尺寸稳定性高；同时，由于导热系数高，可以规避由于热膨胀导致的转辊精度下降，成功地克服了铝、铁等金属转辊的热变形问题，是新一代的高性能转辊。辐射状结构是高性能中间相沥青基碳纤维的常见结构之一，这种结构往往伴随着劈裂状的缺陷，这大大削弱了纤维的工艺性能。因此，在保证辐射状中间相沥青基碳纤维高导热和高模量特性的同时，规避劈裂状结构的产生从而优化其工艺性能具有重要意义。
发明内容
本发明的目的是提供一种高性能中间相沥青基碳纤维的制备方法。
本发明利用恒电位电解法制备磷掺杂碳烯量子点，电解体系的阳极是高纯碳棒，阴极为Pt电极，电解后通过微孔过滤膜过滤，得到滤液，经过去离子水水洗干燥、真空干燥得到磷掺杂碳烯量子点的固体。通过磷掺杂碳烯量子点对中间相沥青进行修饰，利用甲苯分散磷掺杂碳烯量子点配置浓度，随后和中间相沥青在280-350ºC混合惰性气氛下搅拌后进行纺丝。纺丝后进行预氧化处理、低温炭化处理和连续牵伸石墨化处理得到中间相沥青基碳纤维。
具体过程如下：
一种高性能中间相沥青基碳纤维的制备方法，通过磷掺杂碳烯量子点对中间相沥青进行修饰，中间相沥青的原料种类包括石油焦油、煤焦油和合成化工原料，中间相的含量≥98%，灰分≤50ppm，软化点为240-300ºC。磷掺杂碳烯量子点通过恒电位电解法制备，电压为5V，电解液为0.05-5mol/L的磷酸溶液，电解体系的阳极是高纯碳棒，阴极为Pt电极，电流强度为0.01-1mA，电解时间为1-3h，电解后通过10nm微孔过滤膜过滤，得到滤液，经过去离子水水洗干燥、真空干燥得到磷掺杂碳烯量子点的固体。所制备的磷掺杂碳烯量子点粒径在5-20nm。利用甲苯分散磷掺杂碳烯量子点，甲苯中磷掺杂碳烯量子点的浓度为0.5-5g/L，利用超声搅拌0.5-5h在真空条件下混合均匀；随后和中间相沥青在280-350ºC混合惰性气氛下搅拌1-5h后进行纺丝。通过熔融纺丝纺成直径10-20µm的中间相沥青纤维，纺丝温度为280-350ºC。纺丝后进行预氧化处理，中间相沥青纤维在氧化气氛下由室温升温至240-300ºC，进行预氧化处理，氧化增重3%-8%，升温速率0.5-3ºC/min；氧化性气氛包括空气、氧气或二者的混合气体。预氧化后进行炭化处理，在惰性气氛下，升温至500-700ºC进行低温炭化处理，升温速率5-15ºC/min；惰性气氛包括氮气或氩气。炭化后进行石墨化处理，石墨化工艺为在氮气气氛下，由室温升温至2400-2800ºC进行连续牵伸石墨化处理，牵伸比为1.01-1.26，得到中间相沥青基碳纤维。
本发明碳烯量子点粒径在100nm以下，厚度在0.5-1.0nm，表面存在大量的含氧官能团，在嵌入磷原子后形成磷掺杂碳烯量子点。本发明通过磷掺杂碳烯量子点对中间相沥青分子结构进行修饰，在纺丝过程中，中间相沥青分子受到喷丝孔的剪切作用而进行定向排列，取向度很高，中间相沥青分子之间通过磷掺杂石墨烯量子点形成化学键合，在后续的预氧化过程中强化沥青分子的热稳定性和分子取向，在后续的石墨化过程中，分散在乱层炭结构中的磷原子随着无定形碳的晶格转变扩散固溶，打开交叉键并消除缺陷，催化沥青基碳纤维的石墨化过程。由于磷掺杂石墨烯量子点在纺丝和预氧化时固定中间相分子取向并强化中间相沥青分子之间的连接，在石墨化时通过固溶析出催化石墨化，最终可形成无劈裂结构、石墨化程度高的中间相沥青基碳纤维。所制备的高性能碳纤维的模量为800-960GPa，导热率为600-900W/m·K，纤维界面为典型的辐射状结构工艺性能好，是一种具有良好应用前景的“碳转辊”增强材料。
具体实施方式
实施例1
通过磷掺杂碳烯量子点对中间相沥青进行修饰，中间相沥青的原料种类包括石油焦油、煤焦油和合成化工原料，中间相的含量为98%，灰分为50ppm，软化点为240ºC。磷掺杂碳烯量子点通过恒电位电解法制备，电压为5V，电解液为0.05mol/L的磷酸溶液，电解体系的阳极是高纯碳棒，阴极为Pt电极，电流强度为0.1mA，电解时间为1h，电解后通过10nm微孔过滤膜过滤，得到滤液，经过去离子水水洗干燥、真空干燥得到磷掺杂碳烯量子点的固体。所制备的磷掺杂碳烯量子点粒径在16-20nm。利用甲苯分散磷掺杂碳烯量子点，甲苯中磷掺杂碳烯量子点的浓度为0.5g/L，利用超声搅拌0.5h在真空条件下混合均匀；随后和中间相沥青在280ºC混合惰性气氛下搅拌1h后进行纺丝。通过熔融纺丝纺成直径20µm的中间相沥青纤维，纺丝温度为280ºC。纺丝后进行预氧化处理，中间相沥青纤维在氧化气氛下由室温升温至240ºC，进行预氧化处理，氧化增重3%，升温速率0.5ºC/min；氧化性气氛为空气。预氧化后进行炭化处理，在氮气气氛下，升温至500ºC进行低温炭化处理，升温速率5ºC/min。炭化后进行石墨化处理，石墨化工艺为在氮气气氛下，由室温升温至2600ºC进行连续牵伸石墨化处理，牵伸比为1.01，得到中间相沥青基碳纤维模量为800GPa，导热为600W/mK。
实施例2
一种高性能中间相沥青基碳纤维的制备方法，其特征在于：通过磷掺杂碳烯量子点对中间相沥青进行修饰，中间相沥青的原料种类包括石油焦油、煤焦油和合成化工原料，中间相的含量为99%，灰分为35ppm，软化点为270ºC。磷掺杂碳烯量子点通过恒电位电解法制备，电压为5V，电解液为3mol/L的磷酸溶液，电解体系的阳极是高纯碳棒，阴极为Pt电极，电流强度为0.5mA，电解时间为2h，电解后通过10nm微孔过滤膜过滤，得到滤液，经过去离子水水洗干燥、真空干燥得到磷掺杂碳烯量子点的固体。所制备的磷掺杂碳烯量子点粒径在10-14nm。利用甲苯分散磷掺杂碳烯量子点，甲苯中磷掺杂碳烯量子点的浓度为2.5g/L，利用超声搅拌2.5h在真空条件下混合均匀；随后和中间相沥青在310ºC混合惰性气氛下搅拌2.5h后进行纺丝。通过熔融纺丝纺成直径15µm的中间相沥青纤维，纺丝温度为310ºC。纺丝后进行预氧化处理，中间相沥青纤维在氧化气氛下由室温升温至270ºC，进行预氧化处理，氧化增重5%，升温速率1.5ºC/min；氧化性气氛为氧气。预氧化后进行炭化处理，在氮气气氛下，升温至500-700ºC进行低温炭化处理，升温速率5-15ºC/min。炭化后进行石墨化处理，石墨化工艺为在氩气气氛下，由室温升温至2600-3000ºC进行连续牵伸石墨化处理，牵伸比为1.12，得到中间相沥青基碳纤维模量为900GPa，导热为710W/mK。
实施例3
通过磷掺杂碳烯量子点对中间相沥青进行修饰，中间相沥青的原料种类包括石油焦油、煤焦油和合成化工原料，中间相的含量为100%，灰分为15ppm，软化点为300ºC。磷掺杂碳烯量子点通过恒电位电解法制备，电压为5V，电解液为5mol/L的磷酸溶液，电解体系的阳极是高纯碳棒，阴极为Pt电极，电流强度为1mA，电解时间为3h，电解后通过10nm微孔过滤膜过滤，得到滤液，经过去离子水水洗干燥、真空干燥得到磷掺杂碳烯量子点的固体。所制备的磷掺杂碳烯量子点粒径在5-9nm。利用甲苯分散磷掺杂碳烯量子点，甲苯中磷掺杂碳烯量子点的浓度为5g/L，利用超声搅拌5h在真空条件下混合均匀；随后和中间相沥青在350ºC混合惰性气氛下搅拌5h后进行纺丝。通过熔融纺丝纺成直径10µm的中间相沥青纤维，纺丝温度为350ºC。纺丝后进行预氧化处理，中间相沥青纤维在氧化气氛下由室温升温至240-300ºC，进行预氧化处理，氧化增重8%，升温速率3ºC/min；氧化性气氛为空气和氧气的混合气体。预氧化后进行炭化处理，在氩气气氛下，升温至500-700ºC进行低温炭化处理，升温速率5-15ºC/min。炭化后进行石墨化处理，石墨化工艺为在氮气气氛下，由室温升温至2800ºC进行连续牵伸石墨化处理，牵伸比为1.26，得到中间相沥青基碳纤维模量为960GPa，导热为800W/mK。
Claims (10)
1.一种高性能中间相沥青基碳纤维的制备方法，其特征在于：通过磷掺杂碳烯量子点对中间相沥青进行修饰，磷掺杂碳烯量子点通过恒电位电解法制备，电压为5V，电解液为0.05-5mol/L的磷酸溶液，电解体系的阳极是高纯碳棒，阴极为Pt电极，电流强度为0.01-1mA，电解时间为1-3h，电解后通过10nm微孔过滤膜过滤，得到滤液，经过去离子水水洗干燥、真空干燥得到磷掺杂碳烯量子点的固体，所制备的磷掺杂碳烯量子点粒径在5-20nm，利用甲苯分散磷掺杂碳烯量子点，甲苯中磷掺杂碳烯量子点的浓度为0.5-5g/L，利用超声搅拌0.5-5h在真空条件下混合均匀；随后和中间相沥青在280-350ºC混合惰性气氛下搅拌1-5h后进行纺丝；通过熔融纺丝纺成直径10-20µm的中间相沥青纤维，纺丝温度为280-350ºC；纺丝后进行预氧化处理，中间相沥青纤维在氧化气氛下由室温升温至240-300ºC，进行预氧化处理；预氧化后升温至500-700ºC进行低温炭化处理；炭化后进行石墨化处理，石墨化工艺为在氮气气氛下，由室温升温至2400-2800ºC进行连续牵伸石墨化处理，牵伸比为1.01-1.26，得到中间相沥青基碳纤维。
2.根据权利要求1所述的一种高性能中间相沥青基碳纤维的制备方法，其特征在于：所述的中间相沥青的原料来自石油焦油、煤焦油或合成化工原料，中间相的含量≥98%，灰分≤50ppm，软化点为240-300ºC。
3.根据权利要求1所述的一种高性能中间相沥青基碳纤维的制备方法，其特征在于：纺丝后进行预氧化处理，中间相沥青纤维在氧化气氛下由室温升温至240-300ºC，进行预氧化处理，氧化增重3%-8%，升温速率0.5-3ºC/min。
4.根据权利要求3所述的一种高性能中间相沥青基碳纤维的制备方法，其特征在于：所述的预氧化处理的氧化性气氛为空气、氧气或二者的混合气体。
5.根据权利要求3或者4所述的一种高性能中间相沥青基碳纤维的制备方法，其特征在于：纺丝后进行预氧化处理，中间相沥青纤维在氧化气氛下由室温升温至240-300ºC，进行预氧化处理，氧化增重5%-8%。
6.根据权利要求1所述的一种高性能中间相沥青基碳纤维的制备方法，其特征在于：预氧化后进行炭化处理，在惰性气氛下，升温至600-700ºC进行低温炭化处理，升温速率5-15ºC/min；惰性气氛为氮气或氩气。
7.根据权利要求1所述的一种高性能中间相沥青基碳纤维的制备方法，其特征在于：所述的电解液为0.10-5mol/L的磷酸溶液。
8.根据权利要求1所述的一种高性能中间相沥青基碳纤维的制备方法，其特征在于：甲苯中磷掺杂碳烯量子点的浓度为0.5-5g/L。
9.根据权利要求5所述的一种高性能中间相沥青基碳纤维的制备方法，其特征在于：进行预氧化处理，氧化增重6%-8%，升温速率1.0-3ºC/min。
10.根据权利要求1所述的一种高性能中间相沥青基碳纤维的制备方法，其特征在于：炭化后进行石墨化处理，石墨化工艺为在氮气气氛下，由室温升温至2500-2800ºC进行连续牵伸石墨化处理，牵伸比为1.01-1.25。
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