CN107317049B - 一种单离子导电聚合物电解质及其制备方法和用途 - Google Patents
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Abstract
本发明公开了一种单离子导电聚合物电解质及其制备方法和用途。将4‑苯乙烯磺酰全氟烷基磺酰亚胺锂盐,和烯丙基聚醚通过硅氢加成反应接枝在含氢硅油上。得到单离子导体通过交联剂交联成膜。本发明主要是提高聚合物电解质的锂离子迁移数以及电导率,获得的电解具有较低的玻璃化温度,较高的稳定性,以及较高的锂离子迁移数,较高的电化学窗口,在锂离子电池聚合物固体电解质由很大的应用前景。
Description
技术领域
本发明公布了一种单离子导电聚合物电解质及其制备方法和用途。
背景技术
锂离子电池具有能量密度和输出电压高、无记忆效应、环境友好等优点,已经被广泛地应用于电子、航天、电动车辆等领域。电解质是制造锂电池所需的四大关键材料之一,其性能很大程度上决定了电池的功率密度、循环稳定性、安全性能、高低温性能以及使用寿命。目前常用的是液体电解质,但液体电解质由于含有低沸点的有机溶剂,很容易造成燃烧、***、漏液等安全事故。
固体聚合物电解质由于不含有有机溶剂,因此不存在安全隐患。而且,采用固体聚合物电解质会有效的抑制锂枝晶的形成,且易于加工。固体聚合物电解质一般是将导电锂盐和聚合物基体复合形成聚合/锂盐熔盐体系,常见的聚合物基体是PEO。通过醚氧键与锂离子的弱配位以及PEO的链段运动来实现锂离子的迁移。
由于PEO的结晶性,固体电解质在常温下的电导率只有10-5S/cm左右,不能满足商业要求的10-3S/cm,目前采用加入纳米粒子,共聚,增塑剂等方法来降低PEO的结晶性.
目前的固体电解质很多是双离子导电体系,即直接加入锂盐,比如LiPF6,LiClO4,LiTFSI等锂盐,这些外加电场下,阴阳离子都会移动,由于阴离子不参加电极反应,在电极与电解质的界面会形成浓度梯度,产生浓差极化,这样会与外加电场形成相反的电动势,降低电池的能量密度,严重影响电池的使用寿命。
目前常见的单离子导电聚合物电解质是将含双键的阴离子与PEGMA共聚,但由于玻璃化温度较高,常温下电导率较低。而聚硅氧烷类电解质则会有效的解决这个问题。
发明内容
本发明旨在解决目前的固体聚合物电解质存在的迁移数低以及电导率低等问题,提出了一种单离子导电聚合物电解质及其制备方法和用途。
本发明首先公开了一种式(I)结构的单离子导电聚合物电解质,
式(I)中:x是1-4的整数,y是4-7的整数,I是6-10的整数,m是整数的整数,p也是整数。
该单离子导电聚合物电解质可以交联成膜在锂离子电池中进行应用。
本发明还公开了一种基于式(1)所述的单离子导电聚合物电解质的固体电解质膜的制备方法,按以下的步骤进行(1)将烯丙基聚醚溶于甲苯中,加入100ppm的0.01mol/LH2PtCl6,其中烯丙基聚醚与甲苯的质量比是1:1,得到混合物A;(2)将含氢硅油溶于甲苯中,含氢硅油与甲苯的质量比是1:1,得到混合物B;(3)将混合物A滴加到混合物B中,其中烯丙基聚醚与含氢硅油的质量比为2:1,80℃反应24h,反应后将甲苯溶剂蒸掉,将得到的聚醚改性含氢硅油溶解在乙腈中,得到混合物C;(4)将4-苯乙烯磺酰全氟烷基磺酰亚胺锂溶于乙腈中,其中锂盐单体与乙腈的质量比例是1:10,在手套箱内搅拌5h,得到混合物D;(5)将含有锂盐单体的混合物D滴加到混合物C中,80℃反应24h,得到单离子导电聚合物;(6)将单离子导电聚合物与双烯丙基封端的聚醚反应,交联成固体电解质膜。
本发明采用硅氢加成的方法将4-苯乙烯磺酰全氟烷基磺酰亚胺锂和烯丙基聚醚接枝到聚硅氧烷主链上,然后通过交联剂双烯丙基聚醚交联成固体电解质膜。由于聚硅氧烷具有较高的柔韧性,玻璃化温度比较低,且采用聚醚类交联剂,最终所获得的聚合物在常温下电导率达到3.7×10-5S·cm-1。将阴离子接枝到聚硅氧烷上,可以降低阴离子的移动性,减少浓差极化现象,最终所获得的迁移数达到0.8,且电化学窗口高于5.0V(vs Li+/Li)。
具体实施方式
本发明技术方案不局限于以下的实施方式,还包括各实施方案之间的任意组合。
实施实例1-4为单离子导电聚合物电解质的制备。
实施实例1单离子导电聚合物电解质的制备(EO:Li=10:1)。
在25ml的三口烧瓶中加入含有1gPMHS的甲苯溶液(质量分数为50%),然后在通N2的条件下缓慢滴加2g烯丙基聚醚的甲苯溶液(质量分数为50%)。50℃反应3h,然后升温至80℃,反应一段时间后溶液变澄清,当C=C双键消失的时候,停止反应,旋蒸除去甲苯,然后在正己烷中沉淀三次,得到粘稠的聚合物。
上述制备的2.8g的产物溶于乙腈中,缓慢滴加到含有0.4g4-苯乙烯磺酰全氟烷基磺酰亚胺锂的乙腈溶液中,80℃的条件下反应一段时间,当C=C双键消失的时候,停止反应,除去乙腈,在正己烷中沉淀三次得到粘稠的聚合物。
将上述制备的3.0g聚合物加入到THF中,然后加入0.3g交联剂双烯丙基聚醚,70摄氏度反应一段时间后,涂在聚四氟乙烯模具上成膜。
实施实例2单离子导电聚合物电解质的制备(EO:Li=20:1)。
在25ml的三口烧瓶中加入含有1gPMHS的甲苯溶液(质量分数为50%),然后在通N2的条件下缓慢滴加2g烯丙基聚醚的甲苯溶液(质量分数为50%)。50℃反应3h,然后升温至80℃,反应一段时间后溶液变澄清,当C=C双键消失的时候,停止反应,旋蒸除去甲苯,然后在正己烷中沉淀三次,得到粘稠的聚合物。
上述制备的2.8g的产物溶于乙腈中,缓慢滴加到含有0.35g4-苯乙烯磺酰全氟烷基磺酰亚胺锂的乙腈溶液中,80℃的条件下反应一段时间,当C=C双键消失的时候,停止反应,除去乙腈,在正己烷中沉淀三次得到粘稠的聚合物。
将上述制备的3.0g聚合物加入到THF中,然后加入0.3g交联剂双烯丙基聚醚,70摄氏度反应一段时间后,涂在聚四氟乙烯模具上成膜。
实施实例3单离子导电聚合物电解质的制备(EO:Li=28:1)。
在25ml的三口烧瓶中加入含有1g PMHS的甲苯溶液(质量分数为50%),然后在通N2的条件下缓慢滴加2g烯丙基聚醚的甲苯溶液(质量分数为50%)。50℃反应3h,然后升温至80℃,反应一段时间后溶液变澄清,当C=C双键消失的时候,停止反应,旋蒸除去甲苯,然后在正己烷中沉淀三次,得到粘稠的聚合物。
上述制备的2.8g的产物溶于乙腈中,缓慢滴加到含有0.20g4-苯乙烯磺酰全氟烷基磺酰亚胺锂的乙腈溶液中,80℃的条件下反应一段时间,当C=C双键消失的时候,停止反应,除去乙腈,在正己烷中沉淀三次得到粘稠的聚合物。
将上述制备的3.0g聚合物加入到THF中,然后加入0.3g交联剂双烯丙基聚醚,70摄氏度反应一段时间后,涂在聚四氟乙烯模具上成膜。
实施实例4单离子导电聚合物电解质的制备(EO:Li=40:1)。
在25ml的三口烧瓶中加入含有1gPMHS的甲苯溶液(质量分数为50%),然后在通N2的条件下缓慢滴加2g烯丙基聚醚的甲苯溶液(质量分数为50%)。50℃反应3h,然后升温至80℃,反应一段时间后溶液变澄清,当C=C双键消失的时候,停止反应,旋蒸除去甲苯,然后在正己烷中沉淀三次,得到粘稠的聚合物。
上述制备的2.8g的产物溶于乙腈中,缓慢滴加到含有0.2g4-苯乙烯磺酰全氟烷基磺酰亚胺锂的乙腈溶液中,80℃的条件下反应一段时间,当C=C双键消失的时候,停止反应,除去乙腈,在正己烷中沉淀三次得到粘稠的聚合物。
将上述制备的3.0g聚合物加入到THF中,然后加入0.3g交联剂双烯丙基聚醚,70摄氏度反应一段时间后,涂在聚四氟乙烯模具上成膜。
单离子聚合物导电体的性能测试。
(1)电导率的测定:本发明使用上海辰华的CHI660D电化学工作站,采用电化学交流阻抗谱来测定聚合物电解质的电导率。测定时组装成不锈钢/聚合物电解质膜/不锈钢体系进行测量。
(2)离子迁移数的测定:本发明采用的是Bruce等和Abraham等改进的交流阻抗直流极化法测定锂离子迁移数。组装成Li/聚合物/Li体系进行测量,测试温度常温,极化电压10mV。
(3)电化学窗口的测定:采用线性扫描伏安法(LSV)测定电解质的电化学窗口,扫描速率1mv/s,测试温度为30℃。
性能测试见表1。
表1为电解质测试结果所示(30℃):
Claims (1)
1.一种基于下式(I)结构的单离子导电聚合物电解质的固体电解质膜的制备方法,
式(I)结构如下:
式(I)中:x是1-4的整数,y是4-7的整数,I是6-10的整数,m、p为整数;
其特征在于具体包括以下步骤:
(1)将烯丙基聚醚溶于甲苯中,加入100ppm的0.01mol/L H2PtCl6,其中烯丙基聚醚与甲苯的质量比是1:1,得到混合物A;
(2)将含氢硅油溶于甲苯中,含氢硅油与甲苯的质量比是1:1,得到混合物B;
(3)将混合物A滴加到混合物B中,其中烯丙基聚醚与含氢硅油的质量比为2:1,80℃反应24h,反应后将甲苯溶剂蒸掉,将得到的聚醚改性含氢硅油溶解在乙腈中,得到混合物C;
(4)将4-苯乙烯磺酰全氟烷基磺酰亚胺锂溶于乙腈中,其中锂盐单体与乙腈的质量比例是1:10,在手套箱内搅拌5h,得到混合物D;
(5)将含有锂盐单体的混合物D滴加到混合物C中,80℃反应24h,得到单离子导电聚合物电解质;
(6)将单离子导电聚合物与双烯丙基封端的聚醚反应,交联成固体电解质膜。
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