CN107761195B - 一种用于超级电容器电极的木质素基纳米碳纤维制备方法 - Google Patents
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Abstract
本发明公开了一种用于超级电容器电极的木质素基纳米碳纤维制备方法,在海藻酸钠水溶液中加入纳米级二氧化锰,超声搅拌后加入氧化石墨烯,随后调整溶液pH值至10~11,加入纯化木质素,经减压旋蒸后得到杂化材料;将所得杂化材料加入到离心纺丝机中在200~250℃下进行熔融离心纺丝,得到杂化纤维;将杂化纤维置于高温炉中,以0.01~3℃/min的升温速率升至280~300℃,恒温1~6h;然后升温至1000~2000℃,进行碳化,时间为0.5~12h,得到用于超级电容器电极的纳米碳纤维。本发明的有益效果是制备出的用于超级电容器电极的木质素基纳米碳纤维具有较大的能量密度。
Description
技术领域
本发明属于纳米碳纤维的制备技术领域,涉及一种用于超级电容器电极的木质素基纳米碳纤维制备方法。
背景技术
随着便携式及可穿戴电子设备的快速发展,开发与之相适应的柔性、轻质、高效储能设备变得尤为迫切。超级电容器由于具有高功率密度、长循环寿命和超快的充放电能力而被认为颇有前景的储能设备。构筑柔性超级电容器的核心问题是研究和开发具有高能量密度和功率密度的电极。目前柔性超级电容器的电极多采用一维碳纳米管和二维石墨烯来制备,生产成本高,同时难以规模化生产。相比之下活性碳纤维由于具有价格低廉、比表面积大等优点而颇受关注。而在活性碳纤维的所有前驱体中,木质素由于具有含碳量高、资源可再生、价格低廉等优点而成为制备低成本活性碳纤维的较佳选择。专利CN 106744793 A公布了一种碱木质素基超级电容器用多孔碳材料及其制备方法和应用,通过将碱木质素与三嵌段共聚物和乙酸镁混合后加入甲醛和盐酸,经碳化、酸洗和水洗后得到多孔碳材料。然而所得到的碳材料为块状材料,很难进行编织应用于可穿戴领域。同时所得到的电极材料的能量密度较低。
针对上述问题,本专利在木质素中原位引入海藻酸钠、石墨烯和赝电容二氧化锰,采用熔融离心纺丝的方法得到木质素基杂化纳米纤维,并经预氧化、碳化等过程得到了木质素基多孔纳米碳纤维。本专利所制备的多孔纳米碳纤维可用作超级电容器电极,具有比表面积大、孔洞结构可控、能量密度高等优点,便于规模化生产,在纤维状超级电容器领域具备较大的潜在应用,市场前景广阔。
发明内容
本发明的目的在于提供一种用于超级电容器电极的木质素基纳米碳纤维制备方法,解决了目前的木质素基纳米碳纤维能量密度低的问题。
本发明所采用的技术方案是按照以下步骤进行:
步骤1:在海藻酸钠水溶液中加入纳米级二氧化锰,超声搅拌后加入氧化石墨烯,随后调整溶液pH值至10~11,加入纯化木质素,经减压旋蒸后得到杂化材料;将所得杂化材料加入到离心纺丝机中在200~250℃下进行熔融离心纺丝,得到杂化纳米纤维;
步骤2:将步骤1所得杂化纳米纤维置于高温炉中,以0.01~3℃/min的升温速率升至280~300℃,恒温1~6h;然后升温至1000~2000℃,进行碳化,时间为0.5~12h,得到用于超级电容器电极的纳米碳纤维。
进一步,步骤1中的纯化木质素为富含羟基的木质素(羟基含量大于6mmol/g),其结构单元间的连接方式主要为β-β和β-1。
进一步,步骤1中的海藻酸钠的重均分子量低于8万,添加量为总质量的0.05~10%。
进一步,步骤1中的纳米二氧化锰的添加量为总质量的0.1~20%。
进一步,步骤1中的氧化石墨烯的添加量为总质量的0.1~10%。
进一步,步骤1中离心纺丝机的转盘旋转速度为1000~20000转/分钟。
进一步,步骤2中的多孔纳米碳纤维直径为100~900nm,为连续多级孔结构,孔径为1~80nm。
本发明的有益效果是制备出的用于超级电容器电极的木质素基纳米碳纤维具有较大的能量密度。
具体实施方式
下面结合具体实施方式对本发明进行详细说明。
以下实施例中所用的木质素为购自(Suzano Papel e Celulose S.A.)公司的硫酸盐木质素,采用陶瓷膜过滤设备进行纯化,纯化精度为5kDa。
实施例1:将0.5g纳米二氧化锰加入到盛有200ml质量分数为0.5wt.%的海藻酸钠水溶液中,超声分散30min(超声功率120W,超声频率40KHz)后加入1g氧化石墨烯,搅拌均匀。随后调整溶液pH值至11,加入97g纯化木质素。在80℃下采用旋转蒸发仪旋转蒸发后得到木质素/氧化石墨烯/海藻酸钠/二氧化锰杂化材料;将所得杂化材料加入到离心纺丝机中在230℃下进行熔融离心纺丝,得到木质素/氧化石墨烯/海藻酸钠/二氧化锰纳米杂化纤维,其中转盘旋转速度为6000转/分钟。将所得杂化纳米纤维置于高温炉中,以0.01℃/min的升温速率升至280℃,恒温1h;然后升温至1000℃,进行碳化,时间为0.5h,得到木质素基纳米碳纤维。所得纳米碳纤维具有多级孔结构,直径为900nm,比表面积为1100m2/g,介孔孔容为0.13cm3/g。
实施例2:将1g纳米二氧化锰加入到盛有200ml质量分数为1wt.%的海藻酸钠水溶液中,超声分散30min(超声功率120W,超声频率40KHz)后加入2g氧化石墨烯,搅拌均匀。随后调整溶液pH值至12,加入96g纯化木质素。在80℃下采用旋转蒸发仪旋转蒸发后得到木质素/氧化石墨烯/海藻酸钠/二氧化锰杂化材料;将所得杂化材料加入到离心纺丝机中在240℃下进行熔融离心纺丝,得到木质素/氧化石墨烯/海藻酸钠/二氧化锰纳米杂化纤维,其中转盘旋转速度为8000转/分钟。将所得杂化纳米纤维置于高温炉中,以0.03℃/min的升温速率升至280℃,恒温2h;然后升温至1200℃,进行碳化,时间为1h,得到木质素基纳米碳纤维。所得纳米碳纤维具有多级孔结构,直径为810nm,比表面积为1900m2/g,介孔孔容为0.21cm3/g。
实施例3:将2g纳米二氧化锰加入到盛有200ml质量分数为2wt.%的海藻酸钠水溶液中,超声分散30min(超声功率120W,超声频率40KHz)后加入4g氧化石墨烯,搅拌均匀。随后调整溶液pH值至11,加入90g纯化木质素。在80℃下采用旋转蒸发仪旋转蒸发后得到木质素/氧化石墨烯/海藻酸钠/二氧化锰杂化材料;将所得杂化材料加入到离心纺丝机中在250℃下进行熔融离心纺丝,得到木质素/氧化石墨烯/海藻酸钠/二氧化锰纳米杂化纤维,其中转盘旋转速度为12000转/分钟。将所得杂化纳米纤维置于高温炉中,以0.03℃/min的升温速率升至280℃,恒温3h;然后升温至1000℃,进行碳化,时间为3h,得到木质素基纳米碳纤维。所得纳米碳纤维具有多级孔结构,直径为610nm,比表面积为2500m2/g,介孔孔容为0.32cm3/g。
实施例4:将5g纳米二氧化锰加入到盛有200ml质量分数为3wt.%的海藻酸钠水溶液中,超声分散50min(超声功率120W,超声频率40KHz)后加入5g氧化石墨烯,搅拌均匀。随后调整溶液pH值至10,加入84g纯化木质素。在80℃下采用旋转蒸发仪旋转蒸发后得到木质素/氧化石墨烯/海藻酸钠/二氧化锰杂化材料;将所得杂化材料加入到离心纺丝机中在250℃下进行熔融离心纺丝,得到木质素/氧化石墨烯/海藻酸钠/二氧化锰纳米杂化纤维,其中转盘旋转速度为15000转/分钟。将所得杂化纳米纤维置于高温炉中,以0.02℃/min的升温速率升至280℃,恒温3h;然后升温至1200℃,进行碳化,时间为3h,得到木质素基纳米碳纤维。所得纳米碳纤维具有多级孔结构,直径为500nm,比表面积为3200m2/g,介孔孔容为0.46cm3/g。
本发明还具有以下优点:
(1)本发明中所提供的木质素基多孔纳米碳纤维电极具备生产成本低、能量密度高、孔洞结构可控、便于工业化生产等优点。
(2)本发明中所提供的木质素基多孔纳米碳纤维电极采用的是熔融离心纺丝方法,可纺性好,纤维品质优良,生产成本大幅降低,可进行连续化生产。
(3)本发明中所提供的木质素基多孔纳米碳纤维电极具备多级孔结构,孔道直径大,有望广泛应用于智能服装等领域,市场前景广阔。
以上所述仅是对本发明的较佳实施方式而已,并非对本发明作任何形式上的限制,凡是依据本发明的技术实质对以上实施方式所做的任何简单修改,等同变化与修饰,均属于本发明技术方案的范围内。
Claims (1)
1.一种用于超级电容器电极的木质素基纳米碳纤维制备方法,其特征在于:将0.5g纳米二氧化锰加入到盛有200mL 质量分数为0.5wt.%的海藻酸钠水溶液中,超声分散30min,超声功率120W,超声频率40KHz,然加入1g氧化石墨烯,搅拌均匀,随后调整溶液pH值至11,加入97g纯化木质素,在80℃下采用旋转蒸发仪旋转蒸发后得到木质素/氧化石墨烯/海藻酸钠/二氧化锰杂化材料;将所得杂化材料加入到离心纺丝机中在230℃下进行熔融离心纺丝,得到木质素/氧化石墨烯/海藻酸钠/二氧化锰纳米杂化纤维,其中转盘旋转速度为6000转/分钟,将所得杂化纳米纤维置于高温炉中,以0.01℃/min的升温速率升至280℃,恒温1h;然后升温至1000℃,进行碳化,时间为0.5h,得到木质素基纳米碳纤维。
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