CN106587059A - 一种用于电化学储能器件的活性炭改性方法 - Google Patents
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Abstract
本发明提出了一种用于电化学储能器件的活性炭改性方法,包括以下步骤:将活性炭粉末与含氮活化液混合后,置于耐压反应釜中,于80~150oC活化处理,经过滤、烘干,获得高性能电化学储能器件用改性活性炭材料。本发明工艺简便,无污染,制备出的产品具有大的比表面积和优良的电化学性能。
Description
技术领域
本发明涉及一种用于电化学储能器件的活性炭改性方法,属于电化学储能器件中电极材料领域。
技术背景
电化学储能器件具有寿命长、功率大、绿色环保和便于携带等特点,作为电子设备和汽车的电源具有广泛的应用前景。电池和超级电容器作为重要的电化学储能器件主要由电极、电解质、隔膜、端板、引线和封装组成,其电化学性能主要由电极材料的性能决定,其中活性碳材料是最常用的负极材料之一。
活性碳材料是由众多不定域碳原子组成的疏水性大分子,不利于在溶剂中分散,这就限制了该材料本身所具有的用作电极材料的优良特性。此外,因原材料及制备工艺不同,导致商用活性碳材料性能参差不齐。因此,对活性碳进行改性,即在活性碳表面引入新的亲水性的含氮、氧官能团,不但可以改善碳的浸润性还可以赋予其额外的物理化学功能,提高它们实际应用性能。
当前对活性碳进行改性处理的方法,主要有(1)加热法,在300~350℃中低温空气中进行氧化或在800~1000℃高温惰性氛围中处置;(2)等离子体处理法;(3)微波法;(4)添加活化剂,活化剂主要有浓硝酸,浓氨水,尿素、三聚氰胺等。以上方法存在设备昂贵、能耗高、有一定环境污染或性能提高不明显等各种问题,限制其在工业上的应用。因此,克服现有技术的不足,发展一种用于电化学储能器件的活性炭的改性方法具有重要的作用。
发明内容
本发明提供一种用于电化学储能器件的活性炭改性方法,将活性炭粉末为原料经含氮官能团改性后,制备出的产品具有大的比表面积和优良的电化学性能,适于电化学储能器件的电极材料使用。
本发明采用的技术方案为:一种用于电化学储能器件的活性炭的改性方法,包括以下步骤:
(1)配制含氮活化液:向盛有质量百分比浓度为15~25%氨水的容器中加入无机铵盐并搅拌,待固体完全溶解即可;其中氨水与铵盐的质量比为1∶(0.05~0.2);注意铵盐的加入量不能大于其在配置温度时的溶解度;
(2)将活性炭原料粉末与步骤(1)含氮活化液的体积按1 kg∶(3~8)L的比例混合均匀,随后将混合物置于真空度为-0.1MPa的真空箱中10~20分钟;
(3)将步骤(2)的活性炭混合液转移到耐压反应釜中,于80~150℃下进行活化,保温时间2~4小时,然后冷却至室温;
(4)将步骤(3)所得混合液经过滤后,对滤饼进行干燥,即得用于电化学储能器件的活性炭。
上述技术方案中,步骤(4)得到的滤液经浓度调配后,可反复使用。
上述技术方案中,所述无机铵盐是助活化剂,优先硫酸铵或氯化铵。
有益效果:与现有技术相比,本发明的优点在于:
(1)本发明采用无机铵盐作为助活化剂可大幅降低氨水的用量并提高溶液中的氮含量,进而减轻后续活化过程中碱对设备的腐蚀及环境污染问题;采用含氮溶液真空浸渍活性炭,提高了活化液与活性颗粒接触程度及分布的均匀性,加快溶液在活性炭中的扩散吸附过程;第三,浸泡活性炭的混合溶液经过滤分离后,滤液可多次反复使用;
(2)本发明采用含氮活化液-水热联合法来强化活化改性过程,改进生产工艺,节约能耗,降低污染,制得高比面积的活性碳材料孔隙结构发育更为成熟,用于电化学储能器件的电极材料时电化学性能好。
综上所述,本发明以活性炭为原料,通过活化液真空浸渍、含氮活化液-水热法活化改性的技术,制备出的含氮活性炭材料具有大的比表面积和优良的电化学性能,在电化学储能器件领域具有广泛应用前景。
附图说明
图1 活性炭原料(a)及本发明实施例3制备的改性活性炭(b)的扫描电镜对比照片;
图2 活性炭原料(a)、活性炭在室温下经氨水活化改性(b)及本发明实施例3制备的改性活性炭(c)的红外光谱对比图;
图3 为本发明实施例1 制备的活性炭电极的循环伏安曲线;
图4 为本发明实施例2 制备的活性炭(b)与活性炭原料(a)的电化学交流阻抗对比图。
具体实施方式
下面的实施例将对本发明予以进一步的说明,但并不因此而限制本发明。
以下实施例中,涉及到的氨水浓度是指质量百分比浓度。
实施例1
配置质量之比为1(15%氨水)∶0.2(助活化剂硫酸铵)的活化液,搅拌,待固体完全溶解即可;以市售活性炭为原料,按质量(kg)与活化液的体积(L)之比为1∶4 搅拌混合均匀后,置于真空度为-0.1MPa的真空箱中10分钟,随后将混合物转移至耐高压反应釜中,于100℃保温 120 min;最终将活化产物过滤,滤饼在100℃ 干燥 2h。
实施例2
配置物质的量之比为1(20%氨水)∶0.15(助活化剂硫酸铵)的活化液,搅拌,待固体完全溶解即可;将市售活性炭原料,按质量(kg)与活化液的体积(L)之比为1∶4 搅拌混合均匀后,置于真空度为-0.1MPa的真空箱中15分钟,随后将混合物转移至耐高压反应釜中,于80℃保温 180 min;最终将活化产物过滤,滤饼在100℃ 干燥 2h。
实施例3
配置物质的量之比为1(25%氨水)∶0.1(助活化剂硫酸铵)的活化液,搅拌,待固体完全溶解即可;将市售活性炭原料,按质量(kg)与活化液的体积(L)之比为1∶6 搅拌混合均匀后,于真空度为-0.1MPa的真空箱中放置10分钟,随后将混合物转移至耐高压反应釜中,于150℃保温 120 min;最终将活化产物过滤,滤饼在100℃干燥 2h。
如图1所示,是活性炭原料(a)及本发明实施例3制备的改性活性炭(b)的扫描电镜对比照片。
实施例4
配置质量之比为1(25%氨水)∶0.05(助活化剂硫酸铵)的活化液,搅拌,待固体完全溶解即可;将市售活性炭原料,按质量(kg)与活化液的体积(L)之比为1∶8 搅拌混合均匀后,于真空度为-0.1MPa的真空箱中放置20分钟,随后将混合物转移至耐高压反应釜中,于150℃保温 240 min;最终将活化产物过滤,滤饼在100℃干燥 2h。
本发明中,助活化剂不只局限于硫酸铵,与活性炭不发生剧烈化学反应且能提供氮原子的铵盐都可使用。
应用例1
将上述例3 制备的活性炭按活性物质∶乙炔黑∶PVDF =85∶10∶5 的比例进行混合,制备成电极片,以6M KOH 溶液为电解液,采用在公知双电层电容器中使用的隔膜共同组装成纽扣式超级电容器。采用循环伏安法在不同扫描速率下进行测试,结果如图 3 所示。该石墨化活性炭电极的循环伏安曲线在50 mV/s的高扫速下仍然能够保持较好的矩形,说明其具有很高的倍率性能。
应用例2
将上述例4 制备的活性炭按活性物质∶乙炔黑∶PVDF =85∶10∶5 的比例进行混合,制备成电极片,以6M KOH 溶液为电解液,采用在公知双电层电容器中使用的隔膜共同组装成纽扣式超级电容器。常温下在CHI660D电化学工作站进行交流阻抗的测试,其测试结果见图4。经过本发明制备的活性炭与未经改性的原料相比,其阻抗值明显降低。
以上实施例说明,采用本发明以市售活性炭为原料可以制备出具有优异电化学性能的改性活性炭材料。
Claims (2)
1.一种用于电化学储能器件的活性炭改性方法,包括以下步骤:
(1)配制含氮活化液:向盛有质量百分比浓度为15~25%氨水的容器中加入无机铵盐并搅拌,待固体完全溶解即可;其中氨水与铵盐的质量比为1∶(0.05~0.2);
(2)将活性炭原料粉末与步骤(1)含氮活化液的体积按1 kg∶(3~8)L的比例混合均匀,随后将混合物置于真空度为-0.1MPa的真空箱中10~20分钟;
(3) 将步骤(2)的活性炭混合液转移到耐压反应釜中,于80~150oC下进行活化,保温时间2~4小时,然后冷却至室温;
(4)将步骤(3)所得混合液经过滤后,对滤饼进行干燥,即得用于电化学储能器件的活性炭。
2.根据权利要求1所述的一种用于电化学储能器件的活性炭改性方法,其特征在于:所述无机铵盐是硫酸铵或氯化铵。
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Citations (6)
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