CN113527161B - 一种阻燃凝胶聚合物及其制备方法与应用 - Google Patents

一种阻燃凝胶聚合物及其制备方法与应用 Download PDF

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CN113527161B
CN113527161B CN202110732658.1A CN202110732658A CN113527161B CN 113527161 B CN113527161 B CN 113527161B CN 202110732658 A CN202110732658 A CN 202110732658A CN 113527161 B CN113527161 B CN 113527161B
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邓魁荣
徐泽林
周素萍
赵正
曾康龙
关天瑜
曾庆光
汪达
刘争
王光霞
邱振平
张业龙
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Abstract

本发明提供了一种阻燃凝胶聚合物及其制备方法与应用，属于锂离子电池技术领域。本发明公开了式1所示阻燃凝胶聚合物的制备方法，(1)将乙氧基化三羟甲基丙烷三丙烯酸酯和3,6‑二氧杂‑1,8‑辛二硫醇溶解于溶剂中，配置成溶液，将光引发剂加入上述溶液中，搅拌均匀后得到前驱体溶液；(2)将前驱体溶液置于聚偏氟乙烯纤维骨架中，然后在紫外光照射下进行反应，得到聚合物膜；(3)将步骤(2)所得聚合物膜置于电解液中浸泡，即得阻燃凝胶聚合物；其中，步骤(1)中乙氧基化三羟甲基丙烷三丙烯酸酯和3,6‑二氧杂‑1,8‑辛二硫醇的摩尔比为2:3。本发明还提供了阻燃凝胶聚合物在锂离子电池中的应用。

Description

一种阻燃凝胶聚合物及其制备方法与应用
技术领域
本发明涉及一种阻燃凝胶聚合物及其制备方法与应用，属于锂离子电池技术领域。
背景技术
随着智能手机、智能移动设备、电动汽车、混合动力汽车的快速发展，对锂电池的能量密度，安全性能要求越来越高。电解质作为锂电池的一个重要组成部分，对电池性能有重要影响。理想的电解质要求具有离子电导率高，锂离子迁移数高，电化学窗口宽，热稳定性好、机械强度高、安全性好等特性。
传统的锂离子电池使用的是液体电解质，通常由有机液体与锂盐组成。而这些有机液体如碳酸二甲酯(DMC)、碳酸二乙酯(DEC)、乙烯碳酸酯(EC)等是易燃易爆物质，在锂离子电池的使用中存在诸多安全隐患(如燃烧、爆炸、泄漏等)。
聚合物电解质由具有离子传导能力的聚合物与锂盐复合而成，比液体电解质具有更好的安全性，而且可以同时作为电解质和隔膜使用。
发明内容
本发明的目的在于克服现有技术的不足，提供一种阻燃凝胶聚合物电解质及其制备方法与应用，所述阻燃凝胶聚合物电解质室温电导率高、锂离子迁移数高、电化学窗口宽优点，用本发明提供的电解质组装的锂电池安全性好，倍率性能好，循环寿命高且稳定。
为实现上述目的，本发明采取的技术方案为：一种阻燃凝胶聚合物电解质，其化学结构如式1所示：
第二方面，本发明提供了一种阻燃凝胶聚合物的制备方法，包括以下步骤：
(1)将乙氧基化三羟甲基丙烷三丙烯酸酯和3,6-二氧杂-1,8-辛二硫醇溶解于溶剂中，配置成溶液，将光引发剂加入上述溶液中，搅拌均匀后得到前驱体溶液；
(2)将前驱体溶液置于聚偏氟乙烯纤维骨架中，然后在紫外光照射下进行反应，得到聚合物膜；
(3)将步骤(2)所得聚合物膜置于电解液中浸泡，即得阻燃凝胶聚合物；
其中，步骤(1)中乙氧基化三羟甲基丙烷三丙烯酸酯和3,6-二氧杂-1,8-辛二硫醇的摩尔比为2:3。
本发明以乙氧基化三羟甲基丙烷三丙烯酸酯和3,6-二氧杂-1,8-辛二硫醇，制备的凝胶聚合物具有阻燃性，具有室温电导率高、锂离子迁移数高、电化学窗口宽优点。用本发明制备的阻燃凝胶聚合物电组装的锂电池安全性好，倍率性能好，循环寿命高且稳定。乙氧基化三羟甲基丙烷三丙烯酸酯和3,6-二氧杂-1,8-辛二硫醇的摩尔比影响阻燃凝胶聚合物的阻燃性和电导率。
作为本发明阻燃凝胶聚合物制备方法的优选实施方式，所述乙氧基化三羟甲基丙烷三丙烯酸酯和3,6-二氧杂-1,8-辛二硫醇的摩尔比为2:3。上述配比下制备的阻燃凝胶聚合物电解质的阻燃性更好，电导率更高。
作为本发明阻燃凝胶聚合物制备方法的优选实施方式，所述溶剂为碳酸丙烯酯。
作为本发明阻燃凝胶聚合物制备方法的优选实施方式，所述光引发剂为安息香二甲醚。
作为本发明阻燃凝胶聚合物制备方法的优选实施方式，所述电解液由锂盐和有机溶剂组成。
作为本发明阻燃凝胶聚合物制备方法的优选实施方式，所述锂盐由0.8M双氟黄酰亚胺锂和0.2M二氟草酸硼酸锂组成；所述有机溶剂由碳酸乙烯酯、氟代碳酸乙烯酯和乙氧基(五氟)环三磷腈按2:2:6体积配比制成。
第三方面，本发明提供了一种阻燃凝胶聚合物电解质在锂离子电池中的应用。
与现有技术相比，本发明的有益效果为：本发明制备的阻燃凝胶聚合物具有室温电导率高、锂离子迁移数高、电化学窗口宽的优点，其制备方法合成简单易行、原料便宜易得；用本发明制备的阻燃凝胶聚合物组装的锂电池安全性好，倍率性能好，循环寿命高且稳定。
附图说明
图1为实施例1阻燃凝胶聚合物、乙氧基化三羟甲基丙烷三丙烯酸酯的红外光谱图；
图2为实施例1阻燃凝胶聚合物的阻燃性能图；
图3为实施例1阻燃凝胶聚合物制备的磷酸铁锂电池性能图。
具体实施方式
为更好的说明本发明的目的、技术方案和优点，下面将结合具体实施例和附图对本发明作进一步的说明。
实施例1
本发明提供了一种阻燃凝胶聚合物，其化学结构如式1所示：
第二方面，本发明提供了一种阻燃凝胶聚合物的制备方法，包括以下步骤：
(1)前驱液的配制(ETT+DODT)：将1.0690g乙氧基化三羟甲基丙烷三丙烯酸酯和0.6829g 3,6-二氧杂-1,8-辛二硫醇溶解于3.612g碳酸丙烯酯中，配置成溶液，避光条件下将0.015g安息香二甲醚加入上述溶液中，搅拌溶解至溶液完全透明，即得前驱液，避光保存；其中，碳酸丙烯酯的含量为85％。
(2)浸泡液的配制：将0.5986g双(氟磺酰)亚胺锂，0.1150g二氟草酸硼酸锂置于容器中，加入0.8mL碳酸乙烯酯、1.2mL氟代碳酸乙烯酯、2.4mL三氟乙基甲基碳酸酯，搅拌溶解至浸泡液完全透明；
(3)将聚偏氟乙烯静电纺丝膜展开，平铺于聚四氟乙烯模具中，用移液枪吸取50uL前驱体溶液将聚偏氟乙烯静电纺丝膜润湿，然后用纸将聚偏氟乙烯静电纺丝膜压平，得到前处理的模具；
(4)将0.2mL前驱体溶液加入步骤(3)所得前处理的模具中，晃动模具，是前驱体溶液均匀铺满模具，然后将模具置于紫外灯下照射5min，得到聚合物膜；
(5)将步骤(4)所得聚合物膜置于浸泡液中浸泡，即得阻燃凝胶聚合物，记为ETT-DODT。
使用傅里叶红外光谱仪测试所得阻燃凝胶聚合物电解质，测试结果如图1所示，图1为实施例1阻燃凝胶聚合物、乙氧基化三羟甲基丙烷三丙烯酸酯的红外光谱图。从图1中可知，乙氧基化三羟甲基丙烷三丙烯酸酯(ETT)谱中1721cm-1处的强吸收峰对应C＝O的拉伸振动，双键对应的吸收峰为1635cm-1。ETT-DODT光谱中处的1635cm-1吸收峰已经完全消失，说明双键已经反应完全，证明已经合成阻燃凝胶聚合物。
将实施例1所得阻燃凝胶聚合物置于火焰上，测试其阻燃性，测试结果如图2所示，图2为实施例1阻燃凝胶聚合物的阻燃性能图。从图中可以看出，实施例1制备的阻燃凝胶聚合物具有优异的阻燃性能。
将实施例1所得阻燃凝胶聚合物夹在磷酸铁锂正极片与金属锂负极之间，组装成磷酸铁锂电池进行充放电实验，试验结果如图3所示。图3为实施例1阻燃凝胶聚合物制备的磷酸铁锂电池性能图，从图3中可以看出，由阻燃凝胶聚合物制备的磷酸铁锂电池循环寿命高、稳定性高。
最后所应当说明的是，以上实施例用以说明本发明的技术方案而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者同等替换，而不脱离本发明技术方案的实质和范围。

Claims (3)

1.一种阻燃凝胶聚合物，其特征在于，其化学结构如式1所示：
。
式1
2.一种如权利要求1所述阻燃凝胶聚合物的制备方法，其特征在于，包括以下步骤：
（1）将乙氧基化三羟甲基丙烷三丙烯酸酯和3,6-二氧杂-1,8-辛二硫醇溶解于溶剂中，配置成溶液，将光引发剂加入上述溶液中，搅拌均匀后得到前驱体溶液；
（2）将前驱体溶液置于聚偏氟乙烯纤维骨架中，然后在紫外光照射下进行反应，得到聚合物膜；
（3）将步骤（2）所得聚合物膜置于电解液中浸泡，即得阻燃凝胶聚合物；
其中，步骤（1）中乙氧基化三羟甲基丙烷三丙烯酸酯和3,6-二氧杂-1,8-辛二硫醇的摩尔比为2:3；所述溶剂为碳酸丙烯酯；所述光引发剂为安息香二甲醚；
所述步骤（3）中的电解液由锂盐和有机溶剂组成；所述锂盐由0.8M双氟黄酰亚胺锂和0.2M二氟草酸硼酸锂组成；所述有机溶剂由碳酸乙烯酯、氟代碳酸乙烯酯和乙氧基（五氟）环三磷腈按2:2:6体积配比制成。
3.一种权利要求1所述阻燃凝胶聚合物在锂离子电池中的应用。
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