CN112853547A - 静电纺丝处理沥青进一步制备超级电容器电极材料的方法 - Google Patents
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Abstract
本发明提供了一种超级电容器电极材料的制备方法，特别涉及一种利用静电纺丝技术处理沥青进一步制备超级电容器电极材料的方法。其具体制备方法为：步骤一：将沥青溶解在有机溶剂（四氢呋喃、甲苯等）混合PVP等助纺剂；步骤二：碳化；步骤三：利用静电纺丝制备沥青纤维；步骤四：利用二氧化碳活化得到高比表面积的沥青基碳纳米纤维，用作超级电容器电极材料。本发明的制备工艺简单，原料价格低廉，可以实现工业化生产。
Description
技术领域
本发明涉及一种制备超级电容器电极材料的方法，特别是利用静电纺丝技术处理沥青进一步制备超级电容器电极材料的方法，属于电池材料制备技术领域。
背景技术
高压静电纺丝技术是采用高压静电场PVP、PVN、PVA等高分子溶液的击穿作用来制备纳米或微米纤维材料的方法，其基本原理是在喷射枪和接收板之间施加上超高压的静电场，从锥体端喷射的纺丝液的形成射流状，通过电场作用被拉伸，最终在接收板上形成均匀的纳米纤维。该方法可以得到纤维直径达纳米级，并且其延展性和柔韧性都较好。
超级电容器也被称为电化学电容器，是基于诸如多孔碳和一些金属氧化物这样的高比表面材料的电极-电解液界面上进行充放电的一类特殊的电容器。碳材料应用于超级电容器材料，在反复的充放电循环过程中表现出可逆性较高，寿命较长。而煤沥青作为煤焦油减压蒸馏的副产品（约占 45％-50％），价格低廉，丰富且产量高。煤沥青由多环芳烃和多环碳化合物组成，是合成高性能多孔碳材料有利碳前驱体。近年来，煤沥青是一种非常优秀的碳源作为制备高性能多孔碳材料。
超级电容器用炭材料的制备方法有物理活化法、化学活化法、模板法等，物理活化法成本低且无污染，避免了对活化产物繁琐的清洗过程。气体活化剂一般是 CO2、水蒸气和空气，活化温度一般在800 ℃~1000 ℃。
本发明创造性地提出了利用静电纺丝技术处理沥青进一步制备超级电容器电极材料的方法，本方法的制备工艺简单、成本低、产量高、生产安全性强，可以实现工业化生产。
发明内容
本发明涉及一种以静电纺丝技术处理沥青进一步制备超级电容器电极材料的方法，该制备方法简单，且易于操作控制，成本低廉，是提高超级电容器电极材料电化学性能的有效方法。制备步骤为：
步骤一：将沥青溶解在有机溶剂中配成不同浓度溶液，将其与PVP等助纺剂按不同配比进行混合，搅拌10 h；
步骤二：将步骤一得到的混合物进行静电纺丝，先在260 o C氩气下进行预处理处理1h，然后再经过650 o C高温处理2 h，制得沥青纤维；
步骤三：碳化：将所述步骤二得到的所述沥青纤维放入氩气环境下，以5 o C/min升温速率加热至800 o C，使其碳化2 h，制得具有一定初始孔隙的炭化物；
步骤四：利用活化剂CO2将步骤三得到的炭化物进行活化，得到高比表面积的沥青基碳纳米纤维，用作超级电容器电极材料。
进一步的，所述步骤一中的：所述有机溶剂为四氢呋喃、甲苯中的一种。
进一步的，所述步骤一中的：所述浓度为10%，20%，30%。
进一步的，所述步骤一中的：所述助纺剂与溶液配比为5%，10%，15%。
进一步的，所述步骤四中调变活化温度：活化时间是2 h；活化温度是800 o C，900o C，1000 o C。
进一步的，所述步骤四中调变活化时间：活化温度是900 o C；活化时间是1.5 h，2h，2.5 h。
本发明的有益效果为：采用从来源广泛、价廉的沥青为原料制备超级电容器， 在提高产量的同时降低了生产成本。通过改变反应条件，可以得到不同性质的沥青碳纳米片。本发明生产安全性高，易于实现工业化生产。
附图说明
图1是本发明中制备高比表面积的沥青基碳纳米纤维的工艺流程示意图。
图2是实施例1制备的高比表面积沥青基碳纳米纤维的扫描电镜图。
具体实施方式
下文将结合附图详细描述本发明的实施例。应当注意的是，下述实施例中描述的技术特征或者技术特征的组合不应当被认为是孤立的，它们可以被相互组合从而达到更好的技术效果。
图1是本发明中制备高比表面积的沥青碳纳米片的工艺流程示意图。从图中可以看出利用静电纺丝技术处理沥青进一步制备超级电容器电极材料的具体工艺流程为：S1：沥青溶解在有机溶剂并混合PVP等助纺剂；S2：静电纺丝制备沥青纤维；S3：碳化；S4：利用二氧化碳活化得到高比表面积的沥青基碳纳米纤维，用作超级电容器电极材料。
实施例1：本实施例以静电纺丝技术处理沥青进一步制备超级电容器电极材料的方法是由下述步骤完成的：
步骤一：将沥青溶解在有机溶剂四氢呋喃中配成10 %浓度溶液，将其与PVP等助纺剂按配比5 %进行混合，搅拌10 h；
步骤二：将步骤一得到的混合物进行静电纺丝，先在260 o C氩气下进行预处理处理1h，然后再经过650 o C高温处理2 h，制得沥青纤维；
步骤三：碳化：将所述步骤二得到的所述沥青纤维放入氩气环境下，以5 o C/min升温速率加热至800 o C，使其碳化2 h，制得具有一定初始孔隙的炭化物；
步骤四：利用活化剂CO2将步骤三得到的炭化物进行活化，活化时间是2 h，活化温度是800 o C，得到高比表面积的沥青基碳纳米纤维，用作超级电容器电极材料。
实施例2：本实施例与实施例1不同的是：步骤一中所述的有机溶剂为甲苯。
实施例3：本实施例与实施例2不同的是：步骤一中所述沥青溶解在有机溶剂四氢呋喃中配成20 %浓度溶液。
实施例4：本实施例与实施例3不同的是：步骤一中所述沥青溶解在有机溶剂四氢呋喃中配成30 %浓度溶液。
实施例5：本实施例与实施例4不同的是：步骤一中所述与PVP等助纺剂按配比10 %进行混合。
实施例6：本实施例与实施例5不同的是：步骤一中所述与PVP等助纺剂按配比15 %进行混合。
实施例7：本实施例与实施例6不同的是：步骤六中所述的活化比例是1.5:1，活化温度是800 o C；活化时间是2 h。
实施例8：本实施例与实施例7不同的是：步骤四所述活化时间是2 h；活化温度是900 o C。
实施例9：本实施例与实施例8不同的是：步骤四所述活化时间是2 h；活化温度是1000 o C。
实施例10：本实施例与实施例9不同的是：步骤四所述活化时间是1.5 h；活化温度是900 o C。
实施例11：本实施例与实施例10不同的是：步骤四所述活化时间是2.5 h；活化温度是900 o C。
从上述实施例中可以看出：本发明采用来源广泛、价廉的沥青为原料制备超级电容电极材料，在提高产量的同时降低了生产成本。通过改变各种反应条件，可以得到不同性质的高比表面积的沥青基碳纳米纤维。本发明方法生产安全性高，易于实现工业化生产。
本文虽然已经给出了本发明的一些实施例，但是本领域的技术人员应当理解，在不脱离本发明精神的情况下，可以对本文的实施例进行改变。上述实施例只是示例性的，在不脱离本发明原理的范围下，本发明还会有各种变化和改进，这些变化和改进均落入本发明保护的范围内。
Claims (6)
1.一种用静电纺丝技术处理沥青进一步制备超级电容器电极材料的方法，其特征在于，所述的制备方法包括如下步骤：
步骤一：将沥青溶解在有机溶剂中配成不同浓度溶液，将其与PVP等助纺剂按不同配比进行混合，搅拌10 h；
步骤二：将步骤一得到的混合物进行静电纺丝，先在260 o C氩气下进行预处理处理1h，然后再经过650 o C高温处理2 h，制得沥青纤维；
步骤三：碳化：将所述步骤二得到的所述沥青纤维放入氩气环境下，以5 o C/min升温速率加热至800 o C，使其碳化2 h，制得具有一定初始孔隙的炭化物；
步骤四：利用活化剂CO2将步骤三得到的炭化物进行活化，得到高比表面积的沥青基碳纳米纤维，用作超级电容器电极材料。
2.根据权利要求1所述的静电纺丝技术处理沥青进一步制备超级电容器电极材料的方法，其特征在于，所述步骤一中的：所述有机溶剂为四氢呋喃、甲苯中的一种。
3.根据权利要求2所述的静电纺丝技术处理沥青进一步制备超级电容器电极材料的方法，其特征在于，所述步骤一中的：所述浓度为10%，20%，30%。
4.根据权利要求3所述的静电纺丝技术处理沥青进一步制备超级电容器电极材料的方法，其特征在于，所述步骤一中的：所述助纺剂与溶液配比为5%，10%，15%。
5.根据权利要求4所述的静电纺丝技术处理沥青进一步制备超级电容器电极材料的方法，其特征在于，所述步骤四中调变活化温度：活化时间是2 h；活化温度是800 o C，900 o C，1000 o C。
6.根据权利要求5任一项所述的静电纺丝技术处理沥青进一步制备超级电容器电极材料的方法，其特征在于，所述步骤四中调变活化时间：活化温度是900 o C；活化时间是1.5h，2 h，2.5 h。
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