CN109637828A - 石墨烯-聚苯胺-evoh纳米纤维膜的制备方法 - Google Patents

石墨烯-聚苯胺-evoh纳米纤维膜的制备方法 Download PDF

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CN109637828A
CN109637828A CN201811575734.7A CN201811575734A CN109637828A CN 109637828 A CN109637828 A CN 109637828A CN 201811575734 A CN201811575734 A CN 201811575734A CN 109637828 A CN109637828 A CN 109637828A
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赵妙妙
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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    • H01—ELECTRIC ELEMENTS
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    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

本发明涉及化工新型材料技术领域，具体地涉及一种石墨烯‑聚苯胺‑EVOH纳米纤维膜的制备方法。石墨烯‑聚苯胺‑EVOH纳米纤维膜的制备方法，包括如下步骤：（1）EVOH纳米纤维的制备；（2）石墨烯‑聚苯胺‑EVOH复合纳米纤维膜的制备。通过本发明提供的方法制备的石墨烯‑聚苯胺‑EVOH纳米纤维膜具有良好的柔性和电化学性能，可作为柔性超级电容器电极材料使用。

Description

石墨烯-聚苯胺-EVOH纳米纤维膜的制备方法
技术领域
本发明涉及化工新型材料技术领域，具体地涉及一种石墨烯-聚苯胺-EVOH纳米纤维膜的制备方法。
背景技术
石墨烯因具有独特的物理化学结构表现出优异的电化学性能。自验证了石墨烯在超级电容器电极材料领域的应用可行性后，其与碳材料、金属氧化物及导电高分子等的复合体系被大量报道。然而在实际应用中，由于石墨烯表面较好的稳定性导致其难以被电解液润湿，或者石墨烯片层之间较强的范德华力容易造成团聚导致电容量较低，这些均限制了石墨烯在超级电容器领域的应用。
聚苯胺(P苯胺)有多重氧化还原态，理论比电容高达2000F/g，经酸掺杂后具有较高的电导率，可提高充放电过程中电子的传导速率。然而P苯胺力学性能较差，循环寿命短。因此，将P苯胺与石墨烯进行复合，可弥补各自的缺点，发挥二者的协同作用，从而引起众多研究者的关注。用电化学聚合法制备了石墨烯/P苯胺复合材料，发现当电流密度为0.5A/g时，比电容达352F/g。
随着科学技术的进步，电子设备从“可使用”逐步向“便携化”方向迈进。要求电子设备具有超薄的电极材料和精简的组装过程，使器件更小型、轻质。传统的超级电容器多为平面状，刚性有余柔性不足，无法满足可穿戴的需求。高聚物纳米纤维有比表面积大、长径比高、孔径小、柔性好等诸多优点，是颇具潜力的柔性超级电容器电极基底材料。将P苯胺/碳纳米管复合膜粘附在弹性纤维表面作为电极、以聚乙烯醇一磷酸作为凝胶电解质构建了纤维状智能超级电容器，其电化学储能性能在弯曲和拉伸过程中均保持着良好的稳定性。
发明内容
本发明旨在针对上述问题，提出一种石墨烯-聚苯胺-EVOH纳米纤维膜的制备方法。
本发明的技术方案在于：
石墨烯-聚苯胺-EVOH纳米纤维膜的制备方法，包括如下步骤：
（1）EVOH纳米纤维的制备；
将EVOH 和CAB置于8O℃真空烘箱干燥24h，将干燥好的EVOH 和CAB混合均匀，然后进行熔融挤出，熔融挤出所得试样以丙酮为溶剂，萃取，去除基体材料CAB，获得EVOH纳米纤维；
（2）石墨烯-聚苯胺-EVOH复合纳米纤维膜的制备；
将20mg 石墨烯分散到20mL去离子水中形成1mg/mL 石墨烯分散液，超声波和细胞粉碎机分别分散0.5h待用；将经高速分散剂剪切分散30min形成的EVOH 纳米纤维悬浮液加入其中，再添加稀盐酸后搅拌30min；取200mg经减压蒸馏纯化的苯胺分散于HC1溶液中，超声分散后加入上述混合液；0℃反应槽中磁力搅拌，同时滴加HC1溶液中所溶解的APS，滴加速度为ld/s；持续反应12h，所得产物经真空抽滤成膜，用去离子水和无水乙醇反复洗涤至无色，过滤、冷冻真空干燥48h。
所述的EVOH 和CAB的混合质量比为20：8O。
所述的APS与苯胺的质量比为1：1.25。
所述的熔融挤出采用双螺杆共混挤出机，其螺杆转速为50r/min，温度为200~225℃。
所述的萃取采用索式萃取器，萃取的温度为8O℃，萃取时间为72h。
所述的HC1溶液的浓度为lmol/L，体积为10mL。
本发明的技术效果在于：
通过本发明提供的方法制备的石墨烯-聚苯胺-EVOH纳米纤维膜具有良好的柔性和电化学性能，可作为柔性超级电容器电极材料使用。
具体实施方式
实施例1
石墨烯-聚苯胺-EVOH纳米纤维膜的制备方法，包括如下步骤：
（1）EVOH纳米纤维的制备；
将EVOH 和CAB置于8O℃真空烘箱干燥24h，将干燥好的EVOH 和CAB按质量比20：8O混合均匀，然后利用双螺杆共混挤出机进行熔融挤出，螺杆转速为50r/min，温度为200~225℃ ，熔融挤出所得试样以丙酮为溶剂，经索式萃取器在8O℃萃取72h，去除基体材料CAB，获得EVOH纳米纤维；
（2）石墨烯-聚苯胺-EVOH复合纳米纤维膜的制备；
将20mg 石墨烯 分散到20mL去离子水中形成1mg/mL 石墨烯分散液，超声波和细胞粉碎机分别分散0.5h待用；将经高速分散剂剪切分散30min形成的EVOH 纳米纤维悬浮液加入其中，再添加稀盐酸后搅拌30min；取200mg经减压蒸馏纯化的苯胺分散于10mL浓度为lmol/L的HC1溶液中，超声分散后加入上述混合液；0℃反应槽中磁力搅拌，同时滴加10mL浓度为lmol/L HC1所溶解的APS，其中，APS与苯胺的质量比为1：1.25；滴加速度为ld/s；持续反应12h，所得产物经真空抽滤成膜，用去离子水和无水乙醇反复洗涤至无色，过滤、冷冻真空干燥48h。
实施例2
石墨烯-聚苯胺-EVOH纳米纤维膜的制备方法，包括如下步骤：
（1）EVOH纳米纤维的制备；
将EVOH 和CAB置于8O℃真空烘箱干燥24h，将干燥好的EVOH 和CAB按质量比20：8O混合均匀，然后利用双螺杆共混挤出机进行熔融挤出，螺杆转速为50r/min，温度为200~225℃ ，熔融挤出所得试样以丙酮为溶剂，经索式萃取器在8O℃萃取72h，去除基体材料CAB，获得EVOH纳米纤维；
（2）石墨烯-聚苯胺-EVOH复合纳米纤维膜的制备；
将20mg 石墨烯 分散到20mL去离子水中形成1mg/mL 石墨烯分散液，超声波和细胞粉碎机分别分散0.5h待用；将经高速分散剂剪切分散30min形成的EVOH 纳米纤维悬浮液加入其中，再添加稀盐酸后搅拌30min；取200mg经减压蒸馏纯化的苯胺分散于10mL浓度为lmol/L的HC1溶液中，超声分散后加入上述混合液；0℃反应槽中磁力搅拌，同时滴加10mL浓度为lmol/L HC1所溶解的APS，其中，APS与苯胺的质量比为1：1.32；滴加速度为ld/s；持续反应12h，所得产物经真空抽滤成膜，用去离子水和无水乙醇反复洗涤至无色，过滤、冷冻真空干燥48h。

Claims (6)

1.石墨烯-聚苯胺-EVOH纳米纤维膜的制备方法，其特征在于：包括如下步骤：
（1）EVOH纳米纤维的制备；
将EVOH 和CAB置于8O℃真空烘箱干燥24h，将干燥好的EVOH 和CAB混合均匀，然后进行熔融挤出，熔融挤出所得试样以丙酮为溶剂，萃取，去除基体材料CAB，获得EVOH纳米纤维；
（2）石墨烯-聚苯胺-EVOH复合纳米纤维膜的制备；
将20mg 石墨烯分散到20mL去离子水中形成1mg/mL 石墨烯分散液，超声波和细胞粉碎机分别分散0.5h待用；将经高速分散剂剪切分散30min形成的EVOH 纳米纤维悬浮液加入其中，再添加稀盐酸后搅拌30min；取200mg经减压蒸馏纯化的苯胺分散于HC1溶液中，超声分散后加入上述混合液；0℃反应槽中磁力搅拌，同时滴加HC1溶液中所溶解的APS，滴加速度为ld/s；持续反应12h，所得产物经真空抽滤成膜，用去离子水和无水乙醇反复洗涤至无色，过滤、冷冻真空干燥48h。
2.根据权利要求1所述的石墨烯-聚苯胺-EVOH纳米纤维膜的制备方法，其特征在于：所述的EVOH 和CAB的混合质量比为20：8O。
3.根据权利要求2所述的石墨烯-聚苯胺-EVOH纳米纤维膜的制备方法，其特征在于：所述的APS与苯胺的质量比为1：1.25~1.32。
4.根据权利要求3所述的石墨烯-聚苯胺-EVOH纳米纤维膜的制备方法，其特征在于：所述的熔融挤出采用双螺杆共混挤出机，其螺杆转速为50r/min，温度为200~225℃。
5.根据权利要求4所述的石墨烯-聚苯胺-EVOH纳米纤维膜的制备方法，其特征在于：所述的萃取采用索式萃取器，萃取的温度为8O℃，萃取时间为72h。
6.根据权利要求5所述的石墨烯-聚苯胺-EVOH纳米纤维膜的制备方法，其特征在于：所述的HC1溶液的浓度为lmol/L，体积为10mL。
CN201811575734.7A 2018-12-22 2018-12-22 石墨烯-聚苯胺-evoh纳米纤维膜的制备方法 Pending CN109637828A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114743809A (zh) * 2022-04-29 2022-07-12 晋江瑞碧科技有限公司 一种纤维素纳米纤维膜基柔性电极材料的制备方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114743809A (zh) * 2022-04-29 2022-07-12 晋江瑞碧科技有限公司 一种纤维素纳米纤维膜基柔性电极材料的制备方法
CN114743809B (zh) * 2022-04-29 2023-08-18 武夷学院 一种纤维素纳米纤维膜基柔性电极材料的制备方法

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