CN114023573B - 一种三嗪基氮杂二维电极材料的制备方法 - Google Patents
一种三嗪基氮杂二维电极材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种三嗪基氮杂二维电极材料的制备方法,该方法先将对苯二胺与三聚氰酸利用Schiff Base反应合成富氮材料;然后利用凹凸棒土将合成的富氮材料诱导为二维结构,得到二维平面结构的富氮材料。该二维平面结构富氮电极材料富含杂原子,具有高比电容,比表面积大,且该材料是多孔道结构,既有利于离子的进出,又能在膨胀或收缩时稳固结构,不易崩塌,具有很好的稳定性,可以替代石墨烯作为一种良好的负极材料。
Description
技术领域
本发明涉及一种三嗪基氮杂二维电极材料的制备方法。属于电池电极材料技术领域。
背景技术
锂离子电池的性能很大程度上取决于负极材料,现有的商业化锂离子电池负极使用石墨类碳作为负极材料,其较低的理论容量远不能适应相关产业的发展。因此,开发具有低成本,高性能的负极材料是当前的主要内容之一。
石墨烯是目前所发现的最薄的二维材料,其拥有独特的晶体结构,丰富的C杂化结构和界面性能,表现出了优异的电化学性质。例如,高的比表面积,室温下优良的导电性能以及稳定的电化学性能。但是石墨烯片层之间存在较强的范德华力,容易产生团聚,使其难溶于水和常用有机溶剂,因而限制了其应用研究和发展。因此,开发新型具有特殊性能的类石墨烯二维晶体材料成为研究热点,如单原子层六方氮化硼、过渡金属硫化物、磷烯和硼烯等。
聚苯胺被视为可应用与超级电容器电极材料中最具有前景的导电聚合物,具有诸多的优良性质。例如,聚苯胺有多种氧化还原态,在诸多导电聚合物中理论赝电容最大,拥有良好稳定性以及易于合成、处理,而且聚苯胺酸掺杂后具有较高的电导率,大大地提高了充放电过程中电子的传导速率,以上特点使得聚苯胺在电极材料方面有着传统材料不可匹敌的优势。
发明内容
本发明为了解决现有技术中存在的问题,提供一种可以替代石墨烯的类石墨烯电极材料。
为了达到上述目的,本发明提出的技术方案为:一种三嗪基氮杂二维电极材料的制备方法,包括如下步骤:
步骤一、将对苯二胺与三聚氰酸利用Schiff Base反应合成富氮材料;
步骤二、利用凹凸棒土将合成的富氮材料诱导为二维结构,得到三嗪基氮杂二维电极材料。
对上述技术方案的进一步设计为:所述步骤一中,先将对苯二胺与碘在乙醇溶剂中混合,采用冰水浴并搅拌30min,得到处理过的对苯二胺待用;
然后将上述处理过的对苯二胺与三聚氰酸在甲苯溶剂中混合,在油浴加热下进行Schiff Base反应,并回流8h后,得到富氮材料混合物。
所述步骤一中,对苯二胺与碘的物质的量比为1:2。
所述步骤一中,对苯二胺与三聚氰酸物质的量比应为2:3。
所述步骤二中,先将凹凸棒土与1mol/L盐酸混合搅拌30min,抽滤后得到干燥凹凸棒土;
然后将上述干燥凹凸棒土加入步骤一得到的富氮材料混合物中,连接玻璃分水器分水,抽滤后用乙醇重结晶,并干燥处理;
最后向干燥后的产品中加入盐酸,搅拌8h,溶解其中的凹凸棒土,得到最终产品-三嗪基氮杂二维电极材料。
重结晶时使用的为无水乙醇。
本发明的有益效果在于:
本发明产品是一种可以替代石墨烯的类石墨烯材料,用化学方法合成负极材料能有效降低成本,且该材料的合成方法不产生大量废物,保护环境。该二维平面结构富氮电极材料富含杂原子,具有高比电容,比表面积大,且该材料是多孔道结构,既有利于离子的进出,又能在膨胀或收缩时稳固结构,不易崩塌,具有很好的稳定性,可以替代石墨烯作为一种良好的负极材料。
附图说明
图1为本发明三嗪基氮杂二维电极材料制备过程反应式;
图2为本实施例制成的电极材料的红外吸收图谱一;
图3为本实施例制成的电极材料的红外吸收图谱二。
具体实施方式
下面结合附图以及具体实施例对本发明进行详细说明。
实施例
本实施例的二维平面结构富氮电极材料的制备方法,包括如下步骤:
步骤一、利用Schiff Base反应合成富氮材料;
1.1、将对苯二胺与碘在乙醇溶剂中混合,采用冰水浴并搅拌30min待用,其中对苯二胺与碘的物质的量比为1:2;
1.2、将处理过的对苯二胺与三聚氰酸在甲苯溶剂中混合,其中对苯二胺与三聚氰酸物质的量比应为2:3,将上述混合物在90℃油浴加热下进行Schiff Base反应,并回流8h后,得到富氮材料混合物。
步骤二、利用凹凸棒土将合成的富氮材料诱导为二维结构;
2.1、将凹凸棒土与1mol/L盐酸混合搅拌30min,抽滤后得到干燥凹凸棒土,待用;凹凸棒土用量应大于对苯二胺与三聚氰酸用量;
2.2、将上述干燥凹凸棒土加入步骤一得到的富氮材料混合物中,在温度115℃环境下连接玻璃分水器分水,抽滤后用乙醇重结晶,并做干燥处理;
2.3、最后向干燥后的产品中加入酸,搅拌8h,溶解其中的凹凸棒土,得到最终产品-三嗪基氮杂二维电极材料。
本实施例在分别采用三种酸溶液溶解凹凸棒土,结果如下:
酸处理1:取1.2g干燥粗产品于烧杯中,向产品中加入20% HF溶液,搅拌8h,溶解凹凸棒土,干燥后称重为0.29g。
酸处理2:取1.2g干燥粗产品于烧杯中,向产品中加入36.8% 盐酸溶液,搅拌8h,溶解凹凸棒土,干燥后称重为0.81g。
酸处理3:取0.15干燥粗产品于烧杯中,向产品中加入5% 盐酸溶液,搅拌8h,溶解凹凸棒土,干燥后称重为0.15g。由上述实例中可知,在HF溶液中去除凹凸棒土更为彻底。
席夫碱产物在有水存在时,在酸催化下易水解为原来的醛酮,所以上述实验应在无水条件下进行,重结晶应使用无水乙醇。
分别取两份本实施例制成的电极材料进行红外吸收图谱分析,红外吸收谱图分别如图2和图3所示,可以看出:产物在3422、3535cm-1处有N—H键的吸收峰,1645cm-1处有C=N键的吸收峰,而原本1720cm-1处的C=0键吸收峰消失,表面两个反应物已经接上。
本发明的技术方案不局限于上述各实施例,凡采用等同替换方式得到的技术方案均落在本发明要求保护的范围内。
Claims (4)
1.一种三嗪基氮杂二维电极材料的制备方法,其特征在于,包括如下步骤:
步骤一、将对苯二胺与三聚氰酸利用Schiff Base反应合成富氮材料;
步骤二、利用凹凸棒土将合成的富氮材料诱导为二维结构,得到三嗪基氮杂二维电极材料;
所述步骤二中,先将凹凸棒土与1mol/L盐酸混合搅拌30min,抽滤后得到干燥凹凸棒土;
然后将上述干燥凹凸棒土加入步骤一得到的富氮材料混合物中,连接玻璃分水器分水,抽滤后用乙醇重结晶,并干燥处理;
最后向干燥后的产品中加入盐酸,搅拌8h,溶解其中的凹凸棒土,得到最终产品-三嗪基氮杂二维电极材料;
重结晶时使用的为无水乙醇。
2.根据权利要求1所述三嗪基氮杂二维电极材料的制备方法,其特征在于:
所述步骤一中,先将对苯二胺与碘在乙醇溶剂中混合,采用冰水浴并搅拌30min,得到处理过的对苯二胺待用;
然后将上述处理过的对苯二胺与三聚氰酸在甲苯溶剂中混合,在油浴加热下进行Schiff Base反应,并回流8h后,得到富氮材料混合物。
3.根据权利要求2所述三嗪基氮杂二维电极材料的制备方法,其特征在于:所述步骤一中,对苯二胺与碘的物质的量比为1:2。
4.根据权利要求3所述三嗪基氮杂二维电极材料的制备方法,其特征在于:所述步骤一中,对苯二胺与三聚氰酸物质的量比应为2:3。
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CN107098910A (zh) * | 2017-04-12 | 2017-08-29 | 中国科学院青岛生物能源与过程研究所 | 一种新型三嗪富碳二维材料及其制备方法 |
CN108584944A (zh) * | 2018-06-26 | 2018-09-28 | 北京化工大学 | 一种超级电容器用高比表面积富氮分级多孔炭电极材料的制备方法 |
CN110090633A (zh) * | 2019-06-04 | 2019-08-06 | 东华理工大学 | 一种富氮的超交联多孔聚合物材料及其制备方法和应用 |
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CN107098910A (zh) * | 2017-04-12 | 2017-08-29 | 中国科学院青岛生物能源与过程研究所 | 一种新型三嗪富碳二维材料及其制备方法 |
CN108584944A (zh) * | 2018-06-26 | 2018-09-28 | 北京化工大学 | 一种超级电容器用高比表面积富氮分级多孔炭电极材料的制备方法 |
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