CN107240720A - 一种改性碳纳米管掺杂固体聚合物电解质的制备方法 - Google Patents
一种改性碳纳米管掺杂固体聚合物电解质的制备方法 Download PDFInfo
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Abstract
本发明公开了一种改性碳纳米管掺杂固体聚合物电解质的制备方法，具体是先将羟基碳纳米管、乙烯基硅烷偶联剂、氨水、无水乙醇与去离子水按一定比例混合，加热至80℃并磁力搅拌8~12小时，抽滤洗涤干燥后将得到的改性碳纳米管、甲基丙烯酸聚乙二醇酯、锂盐、过硫酸钾、去离子水按一定比例在室温下超声半小时，磁力搅拌直至形成分散良好的悬浊液，再将其浇注至聚四氟乙烯模具中，放入烘箱70℃反应6~10小时，然后升温至80℃保持24小时烘干得到改性碳纳米管掺杂固体聚合物电解质膜。本方法生产过程简单，生产效率高；制备得到的改性碳纳米管掺杂固体聚合物电解质室温下离子电导率高，机械强度好，能够满足锂电池的应用需求。
Description
技术领域
本发明属于电池技术领域，具体为锂离子二次电池固体聚合物电解质的制备方法。
背景技术
锂离子电池是商用最为广泛的储能设备。传统的锂离子电池因其使用电解液容易泄露，以及锂枝晶的生长会导致短路，从而引起安全事故。而采用凝胶聚合物电解质，虽然能够保证较高的离子电导率，但是其机械强度低，不能抑制锂枝晶的生长，导致电池循环性能不佳。因此需要开发电导率高、机械强度好的聚合物电解质。
聚氧化乙烯基固体聚合物电解质虽然由于其链段结晶性从而导致其室温下电导率低，但机械性能相较于凝胶电解质有很大提高，而且其不使用电解液，不会出现电解液泄露导致的安全事故。L. Porcarelli等研究了部分交联的聚氧化乙烯基固体聚合物电解质，其室温下的离子电导率达到了0.1mS·cm-1，工作电压达到5V（Scientific Reports, 2016,6, 19892）。Q.W Pan等研究了可控交联的聚氧化乙烯基固体聚合物电解质，其室温下锂离子电导率能够达到接近1×10-4 S·cm-1，在0.3 mA cm-2的电流密度下，可循环使用2600小时以上（Advanced Materials, 2015, 27, 5995-6001）。
碳纳米管的加入可以限制聚氧化乙烯链段的结晶行为，改性后的碳纳米管既可以充当填料也可以作为交联剂，同时，碳纳米管具有优良的机械性能和热稳定性，能够提高所制膜材料的机械强度和热稳定性。
本发明是利用改性碳纳米管和甲基丙烯酸聚乙二醇酯与锂盐配成分散良好的悬浊液在过硫酸钾引发下直接聚合得到固体聚合物电解质膜。该方法过程简单，得到的固体聚合物电解质膜室温下电导率高，机械强度好。
发明内容
为实现本发明的目的，提供以下技术方案：
一种改性碳纳米管掺杂固体聚合物电解质的制备方法，其特征在于，包括如下步骤：
（1）将羟基碳纳米管、乙烯基硅烷偶联剂、氨水、无水乙醇与去离子水按质量比0.1:1~5:0.5~2.5:60~300:0.5~2.5在室温下超声分散半小时，加热至80℃并磁力搅拌8~12小时，抽滤洗涤干燥后得到乙烯基改性的碳纳米管；
（2）将步骤（1）所得表面修饰乙烯基的碳纳米管，与甲基丙烯酸聚乙二醇酯、锂盐、过硫酸钾、去离子水按照质量比0.1~0.3:1.5:0.075~0.375:0.015:15在室温下超声半个小时，磁力搅拌直至形成分散良好的悬浊液，再将其浇注至聚四氟乙烯模具中，放入烘箱70℃反应6~10小时，然后升温至80℃保持24小时烘干水分，得到改性碳纳米管掺杂固体聚合物电解质膜；
进一步的，所述一种改性碳纳米管掺杂固体聚合物电解质膜中改性碳纳米管含量为5~16 wt%。
进一步的，所述步骤中乙烯基硅烷偶联剂为乙烯基三氯硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷的一种。
进一步的，所述步骤中锂盐为氯化锂、硝酸锂、高氯酸锂、二草酸硼酸锂、双三氟甲烷磺酰亚胺锂的一种。
本发明的特点是：生产过程简单，生产效率高；制备得到的改性碳纳米管掺杂固体聚合物电解质室温下离子电导率高，机械强度好，能够满足锂电池的应用需求。
具体实施方式
以下实施例旨在说明本发明而不是对本发明的进一步限定。
实施例1：
（1）将0.1g羟基碳纳米管、1g乙烯基三氯硅烷、0.5g氨水、0.5g去离子水和60g无水乙醇混合室温下超声分散半小时，加热至80℃并磁力搅拌8小时，抽滤洗涤干燥后得到乙烯基改性的碳纳米管；
（2）将0.1g步骤1所得的乙烯基改性碳纳米管、1.5g甲基丙烯酸聚乙二醇酯、0.075g氯化锂、0.015g过硫酸钾和15g去离子水混合，在室温下超声半小时，磁力搅拌直至形成分散良好的悬浊液，再将其浇注至聚四氟乙烯模具中，放入烘箱70℃反应6小时, 然后升温至80℃保持24小时烘干水分，得到改性碳纳米管掺杂固体聚合物电解质膜。
实施例2：
（1）将0.1g羟基碳纳米管、2g乙烯基三甲氧基硅烷、1g氨水、1g去离子水和120g无水乙醇混合室温下超声分散半小时，加热至80℃并磁力搅拌9小时，抽滤洗涤干燥后得到乙烯基改性的碳纳米管；
（2）将0.1g步骤1所得的乙烯基改性碳纳米管、1.5g甲基丙烯酸聚乙二醇酯、0.15g硝酸锂、0.015g过硫酸钾和15g去离子水混合，在室温下超声半小时，磁力搅拌直至形成分散良好的悬浊液，再将其浇注至聚四氟乙烯模具中，放入烘箱70℃反应7小时, 然后升温至80℃保持24小时烘干水分，得到改性碳纳米管掺杂固体聚合物电解质膜。
实施例3：
（1）将0.1g羟基碳纳米管、3g乙烯基三甲氧基硅烷、1.5g氨水、1.5g去离子水和180g无水乙醇混合室温下超声分散半小时，加热至80℃并磁力搅拌10小时，抽滤洗涤干燥后得到乙烯基改性的碳纳米管；
（2）将0.2g步骤1所得的乙烯基改性碳纳米管、1.5g甲基丙烯酸聚乙二醇酯、0.225g高氯酸锂、0.015g过硫酸钾和15g去离子水混合，在室温下超声半小时，磁力搅拌直至形成分散良好的悬浊液，再将其浇注至聚四氟乙烯模具中，放入烘箱70℃反应8小时, 然后升温至80℃保持24小时烘干水分，得到改性碳纳米管掺杂固体聚合物电解质膜。
实施例4：
（1）将0.1g羟基碳纳米管、4g乙烯基三乙氧基硅烷、2g氨水、2g去离子水和240g无水乙醇混合室温下超声分散半小时，加热至80℃并磁力搅拌11小时，抽滤洗涤干燥后得到乙烯基改性的碳纳米管；
（2）将0.2g步骤1所得的乙烯基改性碳纳米管、1.5g甲基丙烯酸聚乙二醇酯、0.3g二草酸硼酸锂、0.015g过硫酸钾和15g去离子水混合，在室温下超声半小时，磁力搅拌直至形成分散良好的悬浊液，再将其浇注至聚四氟乙烯模具中，放入烘箱70℃反应9小时, 然后升温至80℃保持24小时烘干水分，得到改性碳纳米管掺杂固体聚合物电解质膜。
实施例5：
（1）将0.1g羟基碳纳米管、5g乙烯基三乙氧基硅烷、2.5g氨水、2.5g去离子水和300g无水乙醇混合室温下超声分散半小时，加热至80℃并磁力搅拌12小时，抽滤洗涤干燥后得到乙烯基改性的碳纳米管；
（2）将0.3g步骤1所得的乙烯基改性碳纳米管、1.5g甲基丙烯酸聚乙二醇酯、0.375g双三氟甲烷磺酰亚胺锂、0.015g过硫酸钾和15g去离子水混合，在室温下超声半小时，磁力搅拌直至形成分散良好的悬浊液，再将其浇注至聚四氟乙烯模具中，放入烘箱70℃反应10小时, 然后升温至80℃保持24小时烘干水分，得到改性碳纳米管掺杂固体聚合物电解质膜。
Claims (2)
1.一种改性碳纳米管掺杂固体聚合物电解质的制备方法，其特征在于，包括如下步骤：
（1）将羟基碳纳米管、乙烯基硅烷偶联剂、氨水、无水乙醇与去离子水按质量比0.1:1~5:0.5~2.5:60~300:0.5~2.5在室温下超声分散半小时，加热至80℃并磁力搅拌8~12小时，抽滤洗涤干燥后得到乙烯基改性的碳纳米管，其中所用乙烯基硅烷偶联剂为乙烯基三氯硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷的一种。
（2）将步骤（1）所得表面修饰乙烯基的碳纳米管，与甲基丙烯酸聚乙二醇酯、锂盐、过硫酸钾、去离子水按照质量比0.1~0.3:1.5:0.075~0.375:0.015:150在室温下超声分散半小时，磁力搅拌直至形成分散良好的悬浊液，再将其浇注至聚四氟乙烯模具中，放入烘箱70℃反应6~10小时，然后升温至80℃保持24小时烘干水分，得到改性碳纳米管掺杂固体聚合物电解质膜，其中所用锂盐为氯化锂、硝酸锂、高氯酸锂、二草酸硼酸锂、双三氟甲烷磺酰亚胺锂的一种。
2.根据权利要求1所述一种改性碳纳米管掺杂固体聚合物电解质的制备方法，其特征在于所述电解质膜中改性碳纳米管的含量为5~16 wt%。
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