CN115274314A - 一种三苯基苯-酰亚胺类cof/碳纳米管复合材料及其制备方法和应用 - Google Patents
一种三苯基苯-酰亚胺类cof/碳纳米管复合材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种三苯基苯‑酰亚胺类COF/碳纳米管复合材料及其制备方法和应用,操作过程如下:将三(4‑氨基苯基)苯(TAPB)、1,4,5,8‑萘四甲酸酐、氨基化多壁碳纳米管、1,3‑二甲基‑2‑咪唑啉酮、均三甲苯和异喹啉混合,超声匀质,冷冻抽气,火焰封管,于150‑250℃下反应2‑6d,之后反应物经后处理,得到三苯基苯‑酰亚胺类COF/碳纳米管复合材料,通过调节氨基化多壁碳纳米管的加入量得到含不同比例CNT的复合材料。本发明制备得到的活性物质作为电极材料时具有较宽的电势窗口,优良的比电容,良好的电化学稳定性等优异的性能。
Description
技术领域
本发明属于电极材料制备技术领域,具体涉及一种三苯基苯-酰亚胺类COF/碳纳米管复合材料及其制备方法和应用。
背景技术
通过研究和开发可再生以及可持续的电化学储能系统是用于解决当前能源危机和环境污染问题的一种重要方法途径。超级电容器是近几年逐渐发展批量生产的一种无源器件,介于电池与普通电容之间,超级电容器极长的工作寿命和快速充放电特性,也在电动车辆、混合动力车辆、电动工具、铁路系统、电力系统等广泛的领域得到应用。
由于目前用于超级电容器的电极材料的能量密度相对较低,循环稳定性还不够乐观,超级电容器的导电性能还不能满足大型储能系统的应用要求。为了满足大型储能系统的要求,所需理想的电极材料应该具有高的电导率、较大的有效表面积和快速的离子输运速率。基于该需要,电极材料的制备已经采用了许多改进方法,如形态控制、结构调节和成分匹配等。
共价有机框架COF是一类多晶、高比表面积、可原子设计结构的孔结构规整聚合物,由于其π共轭骨架和丰富的离子传输纳米孔,在能量存储中受到越来越多的关注。
三苯基苯-酰亚胺类共价有机框架材料中,酰亚胺具备典型的氧化还原位点,中心可进行孔结构调整;碳纳米管是一类一维的sp2杂化碳材料,有着非常好的导电性,在储能等相关领域有着非常广泛的应用。
发明内容
针对上述问题,本发明的目的在于提供一种三苯基苯-酰亚胺类COF/碳纳米管复合材料及其制备方法和应用。
为达到上述目的,提出以下技术方案:
一种三苯基苯-酰亚胺类COF/碳纳米管复合材料的制备方法,包括如下步骤:将固体物料三(4-氨基苯基)苯(TAPB)、1,4,5,8-萘四甲酸酐、氨基化多壁碳纳米管与液体物料1,3-二甲基-2-咪唑啉酮、均三甲苯和异喹啉混合,超声匀质,冷冻抽气,火焰封管,于150-250℃下反应2-6d,之后反应物经后处理,得到三苯基苯-酰亚胺类COF/碳纳米管复合材料。
三苯基苯-酰亚胺类COF(pNTCDA-TAPB)的结构式如式(I)所示
(I),
进一步地,氨基化多壁碳纳米管(CNT)的添加量为固体物料总质量的5~50%。
进一步地,后处理的操作过程为反应结束后,冷却至室温,粗产物依次用四氢呋喃、N,N-二甲基乙酰胺、丙酮洗涤;再依次使用四氢呋喃、N,N-二甲基乙酰胺、甲醇作为溶剂对粗产物进行索氏提取;最后使用四氢呋喃进行索氏提取至虹吸液为无色,产物在100-140℃下减压烘干。
进一步地,三(4-氨基苯基)苯和1,4,5,8-萘四甲酸酐的投料摩尔比为1:1-5。
进一步地,异喹啉、均三甲苯和1,3-二甲基-2-咪唑啉酮的投料体积比为1:3:3-8。
一种采用上述制备方法制备得到的三苯基苯-酰亚胺类COF/碳纳米管复合材料。
一种三苯基苯-酰亚胺类COF/碳纳米管复合材料作为电极材料的应用,包括如下步骤:将制备得到的三苯基苯-酰亚胺类COF/碳纳米管复合材料、聚氟乙烯、导电炭黑以质量比为8:1:0.5-5混合,加入N-甲基吡咯烷酮混合摇匀1-5h,滴铸在处理好的泡沫镍上,干燥1-10h后在5-30MPa压力下机械压制5-60min,作为电极进行电化学测试。
进一步地,三苯基苯-酰亚胺类COF/碳纳米管复合材料的质量与N-甲基吡咯烷酮的体积之比为1:10-50,质量单位为g,体积单位为mL。
进一步地,泡沫镍的处理过程为将泡沫镍剪成旗形,涂料面积为1×1 cm,在盐酸中超声5-60min,再用去离子水和丙酮清洗三次,放入60-100℃烘箱中烘干20-200min。
本发明的有益效果在于:制备得到的活性物质作为电极材料时具有较宽的电势窗口,优良的比电容,良好的电化学稳定性等优异的性能,可应用于超级电容器等领域。
附图说明
图1为本发明实施例1中TAPB、1,4,5,8-萘四甲酸酐以及pNTCDA-TAPB的红外光谱;
图2为本发明实施例1中pNTCDA-TAPB、CNT、实施例4中pNTCDA-TAPB@20%CNT的SEM和TEM图;
图3为本发明实施例1-7的产物在10mV/s扫速下的循环伏安曲线
图4为本发明实施例1-7的产物在0.5A/g的电流密度下的恒流充放电曲线
图5为本发明实施例4中pNTCDA-TAPB@20%CNT在不同扫速下的循环伏安曲线;
图6为本发明实施例4中pNTCDA-TAPB@20%CNT在不同电流下的恒流充放电曲线。
具体实施方式
下面以具体实施例对本发明的技术方案作进一步说明,但本发明的保护范围并不限于此。
实施例1 pNTCDA-TAPB的合成
向安瓿瓶中加入三(4-氨基苯基)苯(48.5mg,0.138mmol)、1,4,5,8-萘四甲酸酐(55.41mg,0.207mmol)、1,3-二甲基-2-咪唑啉酮(1.5 mL)、均三甲苯(0.5mL)、异喹啉(0.2mL),超声匀质30min,反应物液氮冷冻15min,真空脱气15min,在真空条件下火焰封管,200℃下反应5天后冷至室温,取出底部粗产物后,依次以THF、DMAc、丙酮洗涤,然后以THF、DMAc、甲醇为溶剂进行索氏提取,最后用THF进行索氏提取至滤液为无色,经120℃减压烘干得褐色产物59.5mg,产率为57.3%。
实施例2 pNTCDA-TAPB@5%CNT的合成
合成方法和操作条件同实施例1,不同之处在于,在添加三(4-氨基苯基)苯、1,4,5,8-萘四甲酸酐同时添加氨基化多壁碳纳米管5.47mg (5%),最终得到目标产物64.4mg,产率为58.9%。
实施例3 pNTCDA-TAPB@10%CNT的合成
合成方法同实施例1,不同之处在于,在添加三(4-氨基苯基)苯、1,4,5,8-萘四甲酸酐同时添加氨基化多壁碳纳米管11.54mg(10%),最终得到目标产物69.8mg,产率为60.5%。
实施例4 pNTCDA-TAPB@20%CNT的合成
合成方法同实施例1,不同之处在于,在添加三(4-氨基苯基)苯、1,4,5,8-萘四甲酸酐同时添加氨基化多壁碳纳米管25.98mg(20%),最终得到目标产物79.55mg,产率为61.2%。
实施例5 pNTCDA-TAPB@30%CNT的合成
合成方法同实施例1,不同之处在于,在添加三(4-氨基苯基)苯、1,4,5,8-萘四甲酸酐同时添加氨基化多壁碳纳米管44.53mg(30%),最终得到目标产物110.54mg,产率为74.5%。
实施例6 pNTCDA-TAPB@40%CNT的合成
合成方法同实施例1,不同之处在于,在添加三(4-氨基苯基)苯、1,4,5,8-萘四甲酸酐同时添加氨基化多壁碳纳米管69.27mg(40%),最终得到目标产物132.3mg,产率为76.4%。
实施例7 pNTCDA-TAPB@50%CNT的合成
合成方法同实施例1,不同之处在于,在添加三(4-氨基苯基)苯、1,4,5,8-萘四甲酸酐同时添加氨基化多壁碳纳米管103.91mg(50%),最终得到目标产物168.11mg,产率为80.9%。
实施例8 电化学性能测试
(1)将泡沫镍剪成具备1×1cm正方形的旗状,在16%盐酸中超声10min,然后用去离子水和丙酮清洗,干燥20min,称重;
(2)分别将通过实施例1到7制备得到的活性物质与导电炭黑,聚氟乙烯(PVDF)以质量比80:10:10混合,加入N-甲基吡咯烷酮(0.02g活性物质/0.5mLNMP)混合摇匀2h,滴铸在(1)中处理好的泡沫镍上,干燥2h后在20MPa压力下机械压制10min后继续干燥过夜,称重,活性物质量控制在1~3mg之间。
电化学性能测试采用三电极系统进行测试,参比电极为Ag/AgCl (3M KCl)电极,对电极为铂片电极,以上述涂覆了活性物质的泡沫镍作为工作电极,电解液为1 M Na2SO4溶液;分别进行测试,循环伏安法,恒流充放电法测试电势窗口为-0.3~-0.9V,得到如图3的pNTCDA-TAPB复合不同添加量氨基化多壁碳纳米管在10mV/s扫速下的循环伏安曲线,如图4所示的pNTCDA-TAPB复合不同添加量氨基化多壁碳纳米管在0.5A/g的电流密度下的恒流充放电曲线,结果表示材料具备良好的氧化还原性能,根据公式,其中I是电流,Δt是放电时间,m是活性物质的质量,ΔV是工作电压窗口,计算得pNTCDA-TAPB@20%CNT材料在0.5A/g电流密度下具备271.4F/g的优良比电容,表明该材料是一种非常潜在的超级电容器电极材料。
图5和6分别为pNTCDA-TAPB@20%CNT在不同扫速和不同电流下的循环伏安曲线和恒流充放电曲线。图5不同扫速下的循环伏安曲线表明复合电极材料具有较大的闭合曲线,具有较高的储存电荷能力,图6不同电流密度下的充放电曲线进一步说明复合电极材料具有较高的比电容,即储存电荷能力。
图1为三(4-氨基苯基)苯,1,4,5,8-萘四甲酸酐以及pNTCDA-TAPB的红外光谱图,证实反应发生了聚合反应,图2依次为pNTCDA-TAPB、CNT、pNTCDA-TAPB@20%CNT的扫描电镜以及透射电镜图,证明pNTCDA-TAPB材料成功在CNT上原位生长。
Claims (10)
1.一种三苯基苯-酰亚胺类COF/碳纳米管复合材料的制备方法,其特征在于包括如下步骤:将固体物料三(4-氨基苯基)苯、1,4,5,8-萘四甲酸酐、氨基化多壁碳纳米管与液体物料1,3-二甲基-2-咪唑啉酮、均三甲苯和异喹啉混合,超声匀质,冷冻抽气,火焰封管,于150-250℃下反应2-6d,之后反应物经后处理,得到三苯基苯-酰亚胺类COF/碳纳米管复合材料。
2.如权利要求1所述的制备方法,其特征在于氨基化多壁碳纳米管的添加量为添加的固体物料总质量的5~50%。
3.如权利要求1所述的制备方法,其特征在于后处理的操作过程为反应结束后,冷却至室温,粗产物依次用四氢呋喃、N,N-二甲基乙酰胺、丙酮洗涤;再依次使用四氢呋喃、N,N-二甲基乙酰胺、甲醇作为溶剂对粗产物进行索氏提取;最后使用四氢呋喃进行索氏提取至虹吸液为无色,产物在100-140℃下减压烘干。
4.如权利要求1所述的制备方法,其特征在于三(4-氨基苯基)苯和1,4,5,8-萘四甲酸酐的投料摩尔比为1:1-5。
5.如权利要求1所述的制备方法,其特征在于异喹啉、均三甲苯和1,3-二甲基-2-咪唑啉酮的投料体积比为1:3:3-8。
6.一种采用如权利要求2所述的制备方法制备得到的三苯基苯-酰亚胺类COF/碳纳米管复合材料。
7.一种如权利要求6所述的三苯基苯-酰亚胺类COF/碳纳米管复合材料作为电极材料的应用。
8.如权利要求7所述的应用,其特征在于包括如下步骤:将制备得到的三苯基苯-酰亚胺类COF/碳纳米管复合材料、聚氟乙烯、导电炭黑以质量比为8:1:0.5-5混合,加入N-甲基吡咯烷酮混合摇匀1-5h,滴铸在处理好的泡沫镍上,干燥1-10h后在5-30MPa压力下机械压制5-60min,作为电极进行电化学测试。
9.如权利要求8所述的应用,其特征在于三苯基苯-酰亚胺类COF/碳纳米管复合材料的质量与N-甲基吡咯烷酮的体积之比为1:10-50,质量单位为g,体积单位为mL。
10.如权利要求8所述的应用,其特征在于泡沫镍的处理过程为将泡沫镍剪成旗形,涂料面积为1×1 cm,在盐酸中超声5-60min,再用去离子水和丙酮清洗三次,放入60-100℃烘箱中烘干20-200min。
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