CN116675645B - 一种含磷、氮离子液体及其制备方法和应用 - Google Patents
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Abstract
一种含磷、氮离子液体及其制备方法和应用,涉及离子液体技术领域,可作为电解质应用于离子电池中。室温下将溶解在溶剂中;在磁力搅拌下将逐滴加入步骤S1中的溶液中进行反应;对反应后的溶液旋转蒸发除去溶剂,然后在真空烘箱中干燥,得到含磷、氮离子液体,命名为PIL。将该离子液体作为电解液制备的电池,优异的电化学稳定性。
Description
技术领域
本发明涉及导电材料技术领域,具体涉及一种含磷、氮离子液体及其制备方法和应用。
背景技术
随着工业化进程的加速,环境污染和能源危机问题成为全球关注的焦点。在这个背景下,绿色环保高效的能源技术、污染控制和治理技术得到了广泛的应用和发展。
离子液体作为一种独特的液态材料,具有低挥发性、无毒性以及高稳定性等优点,可通过设计特定的离子组分以及物理和化学性质来实现多种功能。因此,在化学科研、新材料开发、环境治理和能源领域等方面,离子液体已经受到广泛的关注和研究。具体地,离子液体作为一种优秀的电解质、电极材料和催化剂,已被广泛应用于锂离子电池、超级电容器、燃料电池、太阳能电池等能源储存和转换设备中。离子液体的高离子电导率、热稳定性和高安全性等特点使其成为了代替传统溶液的一种理想的电解质和电极材料。
在离子液体的设计和合成方面,本领域技术人员越来越注重探索更高效、更环保的方法来制备特定性质的离子液体。例如,通过改变离子液体阳离子和阴离子的结构以及它们之间的比例,设计出具有特殊功能和性质的离子液体。
发明内容
本发明提出了一种含磷、氮离子液体及其制备方法和应用。
本发明的技术方案如下:
一种含磷、氮离子液体,具有如下结构通式:
,命名为PIL,
其中,R1和R2均选自含碳原子的基团。
优选地,R1和R2选自烷基、乙烯基或苯基。
优选地,所述烷基中的碳原子个数为1~20中的任一整数。
本发明还提供一种上述含磷、氮离子液体的制备方法,包括如下步骤:
S1、室温下将溶解在溶剂中;
S2、在磁力搅拌下将逐滴加入步骤S1中的溶液中进行反应;
S3、对反应后的溶液旋转蒸发除去溶剂,然后在真空烘箱中干燥,得到含磷、氮离子液体,命名为PIL。
优选地,步骤S1中所述溶剂为无水乙醇、甲醇或N,N-二甲基甲酰胺。
优选地,所述和/>的摩尔比为1:2。
优选地,所述旋转蒸发的温度为30℃~120℃。
优选地,所述干燥的温度为20℃~60℃。
优选地,步骤S2中所述反应的时间为0.5h~12h。
本发明还提供一种上述含磷、氮离子液体的应用,作为电解质应用于离子电池中。
与现有技术相比,本发明的具体有益效果为:
1.本发明提供了一种含磷、氮离子液体,具备优异的导电性能,将该离子液体作为电解液制备的电池,优异的电化学稳定性;
2.本发明提供的含磷、氮离子液体制备方法,制备工艺简单,过程便于操作,适合工业生产。
附图说明
图1为实施例1制得的离子液体的红外光谱图;
图2为实施例1制得的离子液体的核磁共振氢谱图;
图3为实施例1制得的离子液体的XPS图;
图4为实施例1制得的离子液体循环伏安曲线图;
图5为实施例1制得的离子液体不同电流密度下的充放电(GCD)图;
图6为实施例1制得的离子液体恒流连续充放电图;
图7为实施例1制得的离子液体电化学阻抗(EIS)图。
具体实施方式
为使本发明的技术方案更加清楚,下面将结合本发明的说明书附图,对本发明实施例中的技术方案进行清楚、完整地描述,需要说明的是,以下实施例仅用于更好地理解本发明的技术方案,而不应理解为对本发明的限制。
实施例1.
在单颈圆底烧瓶中,室温下将0.01mol苯基磷酸(PPA)溶解在无水乙醇中,随后通过磁力搅拌将0.02mol1-乙基咪唑逐滴添加到苯基磷酸溶液中反应10h,最后将溶液在60℃下旋转蒸发除去溶剂,并在30℃真空烘箱中干燥1h,获得淡黄色透明的离子液体(PIL)。
图1为本实施例中所述PPA、MZ和PIL的红外光谱图,可以看到,PPA在1439cm-1,1144cm-1,938cm-1处出现特征峰,分别归属于P-Ph,P=O和P-OH的伸缩振动;MZ在1647cm-1和1512cm-1出现的特征峰归属于咪唑环的拉伸振动;在合成的PIL红外图谱中,原本的P-OH消失以及新出现了1545处的NH+,这证明了PIL的成功合成。图2为本实施例制得的PIL的核磁共振氢谱图,图中约8.07ppm处的信号峰为NH+的信号峰,除此之外,其他所有信号峰的化学位移和积分面积与PIL的化学结构的质子对应。根据以上的结果和分析,可以表明成功合成了目标化合物。图3为本实施例制得的PIL的X射线光电子能谱图,光谱揭示了PIL中存在C、N、O、P元素;对于XPS C1s光谱,PIL在285.1、283.8eV处显示两个峰,分别对应于C-N/C=N和C-C的键;对于XPS N1s光谱,PIL在400.5eV处显示一个峰,对应于C-N/C=N的键;对于XPSP1s光谱,PIL在531.6和530.3eV处显示两个峰,分别对应于P-O和P=O的键。这也表明了PIL的成功合成。以上可以证明,本实施例成功合成了结构式如下的离子液体:
。
以304不锈钢作为正负极材料,以本实施例制得的离子液体作为电解质,组装成2032型号的对称纽扣电池,并对该纽扣电池进行循环伏安法(CV)测试,扫描速率为0.1mVs-1,结果见图4所示,在循环三圈过后,第三圈的形状与初始形状基本保持一致,表明了它具有良好的电化学稳定性。对该纽扣电池进行不同电流密度下的充放电(GCD)测试,电流密度测试范围0.01mAcm-2~0.1mAcm-2,结果见图5所示,在不同电流密度下,均展示出了较好较长的放电时间,表明PIL具有较好的电化学性能。对该纽扣电池进行恒流连续充放电测试,电流密度为0.1mAcm-2,结果见图6,经过5500圈的连续充放电测试之后,可以看到依然可以平稳运行,表明具有良好的电化学稳定性;通过电化学阻抗谱法(EIS)评估离子电导率(σ),频率范围为0.01Hz~1MHz,振幅为5mV,得到的测试结果见图7,在高频区有较小的半圆,阻抗值较小;在低频区表现出平稳的直线,说明了具有较快的离子穿梭速率。同时,利用ZView软件拟合实验阻抗数据,得到PIL的离子转移电阻(Rb),根据公式,计算得到离子电导率σ=1.19×10-3S/m,这证明了PIL具有优异的导电性。可以看出,本实施例制备的离子液体具有优异的电化学稳定性。
实施例2.
在单颈圆底烧瓶中,室温下将0.01mol乙烯基磷酸溶解在甲醇中,随后通过磁力搅拌将0.02molN-甲基咪唑逐滴添加到苯基磷酸溶液中反应6h,最后将溶液在40℃下旋转蒸发除去溶剂,并在40℃真空烘箱中干燥1h,获得淡黄色透明的离子液体(PIL)。
实施例3.
在单颈圆底烧瓶中,室温下将0.01mol苯基磷酸(PPA)溶解在N,N-二甲基甲酰胺溶液中,随后通过磁力搅拌将0.02mol乙烯基咪唑逐滴添加到苯基磷酸溶液中反应2h,最后将溶液在110℃下旋转蒸发除去溶剂,并在60℃真空烘箱中干燥1h,获得淡黄色透明的离子液体(PIL)。
显然,上述实施例仅仅是为了清楚的说明所作的举例,在上述说明的基础上还可以做出其他形式的变动或变化。因此,由此所引申出的显而易见的变化或变动仍属于本发明的保护范围之内。
Claims (7)
1.一种含磷、氮离子液体,其特征在于,具有如下结构通式:
,
其中, R1为苯基,R2为乙基。
2.一种如权利要求1所述的含磷、氮离子液体的制备方法,其特征在于,包括如下步骤:
S1、室温下将苯基磷酸溶解在无水乙醇中;
S2、在磁力搅拌下将1-乙基咪唑逐滴加入步骤S1中的溶液中进行反应;
S3、对反应后的溶液旋转蒸发除去溶剂,然后在真空烘箱中干燥,得到含磷、氮离子液体。
3.根据权利要求2所述的含磷、氮离子液体的制备方法,其特征在于,所述苯基磷酸和1-乙基咪唑的摩尔比为1:2。
4.根据权利要求2所述的含磷、氮离子液体的制备方法,其特征在于,所述旋转蒸发的温度为30℃~120℃。
5.根据权利要求2所述的含磷、氮离子液体的制备方法,其特征在于,所述干燥的温度为20℃~60℃。
6.根据权利要求2所述的含磷、氮离子液体的制备方法,其特征在于,步骤S2中所述反应的时间为0.5h~12h。
7.一种如权利要求1所述的含磷、氮离子液体的应用,其特征在于,作为电解质应用于离子电池中。
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