CN105161723A - 聚吡咯-3-甲酸及其作为锂离子电池正极材料的应用 - Google Patents
聚吡咯-3-甲酸及其作为锂离子电池正极材料的应用 Download PDFInfo
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- 239000002033 PVDF binder Substances 0.000 claims description 5
- 239000006230 acetylene black Substances 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 5
- 229910013870 LiPF 6 Inorganic materials 0.000 claims description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
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- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 2
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- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000005227 gel permeation chromatography Methods 0.000 description 2
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- 102000004310 Ion Channels Human genes 0.000 description 1
- 229910012820 LiCoO Inorganic materials 0.000 description 1
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Abstract
聚吡咯-3-甲酸及其作为锂离子电池正极材料的应用。本发明提供了一种如式(I)所示的聚吡咯-3-甲酸,其按如下方法制备得到:将吡咯-3-甲酸溶于四氯化碳中得到吡咯-3-甲酸溶液,将FeCl3溶于硝基甲烷中得到FeCl3溶液,将所得FeCl3溶液滴加到吡咯-3-甲酸溶液中,于-10~0℃,N2保护的条件下反应20~24h,之后反应液经抽滤,滤饼用去离子水、乙醇洗涤,置于烘箱中于60~70℃真空干燥10~12h,即得聚吡咯-3-甲酸;式(I)中,n为100~1000的整数;所述的聚吡咯-3-甲酸锂离子可作为电池正极材料,放电比容量高,循环稳定性好;
Description
(一)技术领域
本发明涉及聚吡咯-3-甲酸及其作为锂离子电池正极材料的应用。
(二)技术背景
20世纪,人类依靠化石能源使全球经济得到了飞速发展,直到现在,化石等不可再生能源依然占到全球能源构成的80%。然而,大量不可再生能源的使用,使得未来的能源安全充满了诸多不确定因素。同时不合理的能源结构也造成了全球环境污染,生态破坏等问题。可以说,开发新能源,改变传统的能源结构已经是迫在眉睫了。而电能由于清洁、安全且便利等特点愈发显示出其优越性,也越来越受到人们的青睐。因此,能将化学能直接转变成电能的化学电源,也随之引起了人们的广泛关注。而便携式电子设备的飞速发展则迫使化学电源朝着轻型、小型、长使用寿命型发展。这也催生了具有高能量密度、灵巧轻便、循环使用寿命长的锂离子电池产业的产生和发展。锂离子电池由于其良好的能量存储和输出特性,已成为纯电动汽车储能设备的首选电源。但是,锂离子电池的正极材料通常比负极材料具有较低的比容量,因此正极材料的选用是影响锂电池性能的关键因素。
近些年来,研究者们主要将目光集中在无机过渡金属氧化物(例如LiCoO2、LiMn2O4、LiFePO4、V2O5等)上,但是,这些过渡金属氧化物作为正极材料时有很多缺点,如:成本高,矿物资源有限,生产过程中能量需求高以及会产生CO2等等,这些缺点限制了其在锂离子电池正极材料中的广泛应用。然而有机导电高分子作为正极材料,不仅可以避免上述无机材料的缺点还具有理论比容量高,容易制备,分子结构的灵活设计性等优点。目前已经报道的有机导电高分子作为正极材料的有:有机硫聚合物,聚吡咯,TEMPO自由基聚合物,聚苯胺衍生物类。这些类型的有机导电高分子正极材料的使用使锂离子电池的性能得到了提高。
(三)发明内容
本发明的目的是解决无机化合物作为正极材料所具有的成本高,矿物资源有限,生产过程中能量要求高以及会产生CO2等等缺点而提出具有良好电化学性能及稳定性的锂离子电池正极材料,即由聚合吡咯衍生物得到的导电高分子材料作为正极材料。
本发明采用的吡咯衍生物是吡咯-3-甲酸(简称P3C),将该单体进行聚合,将聚合得到的聚吡咯-3-甲酸(简称PP3C)作为锂离子电池正极材料。
为实现上述目的,本发明采用如下技术方案:
一种如式(I)所示的聚吡咯-3-甲酸,所述的聚吡咯-3-甲酸按如下方法制备得到:
将吡咯-3-甲酸溶于四氯化碳中得到吡咯-3-甲酸溶液,将FeCl3溶于硝基甲烷中得到FeCl3溶液,将所得FeCl3溶液滴加到吡咯-3-甲酸溶液中,于-10~0℃,N2保护的条件下反应20~24h,之后反应液经抽滤,滤饼用去离子水、乙醇洗涤,置于烘箱中于60~70℃真空干燥10~12h,即得聚吡咯-3-甲酸;
所述四氯化碳的体积用量以吡咯-3-甲酸的质量计为70~80mL/g;所述硝基甲烷的体积用量以FeCl3的质量计为20~25mL/g;所述吡咯-3-甲酸与FeCl3的物质的量之比为1:2.9~3.0;
式(I)中,n为100~1000的整数。
本发明还提供了聚吡咯-3-甲酸作为锂离子电池正极材料的应用。
进一步,本发明还提供了聚吡咯-3-甲酸作为锂离子电池正极材料在组装锂离子电池中的应用。
所述组装锂离子电池的方法为:
(1)制备正极极片:将聚吡咯-3-甲酸研磨至300~400目的粉末,然后将聚吡咯-3-甲酸粉末与乙炔黑、PVDF混合,滴加N-甲基吡咯烷酮,搅拌形成正极浆料,将所得正极浆料涂布在铝箔上,然后将涂布有正极浆料的铝箔置于60~70℃恒温烘箱中真空干燥10~12h,即得正极极片;
所述聚吡咯-3-甲酸粉末与乙炔黑、PVDF的质量比为50:40:10;所述N-甲基吡咯烷酮的体积用量以聚吡咯-3-甲酸粉末的质量计为20mL/g;所述正极浆料在铝箔上的涂布厚度为90μm;
(2)组装锂离子电池:取步骤(1)制备的正极极片,以锂片为负极极片,以含有LiPF6的EC/DMC溶液为电解液,装配成扣式电池,即得所述的锂离子电池;所述电解液中,LiPF6的含量为1M,EC/DMC体积比为1:1。
本发明的有益效果在于:本发明提供了一种锂离子电池正极材料——聚吡咯-3-甲酸,由于吡咯环上含有羧基,羧基具有亲水亲电解液的性质,因此有助于活性物质与电解液之间的接触,在电极的氧化还原反应中具有更多的离子通道有利于锂离子的嵌入和脱出。与目前已报导的聚吡咯作为正极材料中的活性物质相比,聚吡咯-3-甲酸作为活性物质具有更高的放电比容量,更好的循环稳定性。聚吡咯-3-甲酸作为锂离子电池正极材料,在20mA·g-1充放电速率下进行充放电,充放电电压范围为2.5~4.0V,最大放电比容量达到54.4mAh·g-1,并且具有良好的循环稳定性。
(四)附图说明
图1是以20mA·g-1恒定充放电速率下测试的首次充放电曲线,如图所示PP3C电极的首次放电比容量达到54.4mAh·g-1,是文献中报导的聚吡咯的首次放电比容量16.5mAh·g-1的3.3倍。
图2是PP3C电极的充放电循环性能测试图,放电比容量变化幅度很小。
(五)具体实施方式
下面通过具体实施例对本发明进行进一步的说明,但本发明的保护范围并不仅限于此。
实施例1制备PP3C
化学氧化法聚合P3C:称取P3C(1.0953g,9.8587mmol)于250ml的单口圆底烧瓶中,然后用量筒量取四氯化碳(80ml)加到烧瓶中。称取FeCl3(4.6844g,28.88mmol)溶解到硝基甲烷(100ml)中,将该氧化体系至于恒压滴液漏斗中逐滴滴加到反应体系中。体系温度控制在0℃,在N2保护下反应24小时。反应结束后,抽滤,滤饼分别用去离子水和乙醇洗涤,最后置于烘箱中于65℃真空干燥11小时,得到PP3C0.4109g,GPC凝胶渗透色谱测得聚合度为950。
实施例2锂离子电池的组装
(1)制备正极极片:将聚吡咯-3-甲酸研磨至300~400目的粉末,然后称取聚吡咯-3-甲酸粉末(0.05g)、乙炔黑(0.04g)、PVDF(0.01g)混合,滴加N-甲基吡咯烷酮(1mL),搅拌形成正极浆料,将所得正极浆料用刀片涂布在铝箔(铝箔在使用前,用沾有丙酮的滤纸擦拭,直至滤纸上没有黑色物质即可)上,涂布厚度为90μm,然后将涂布有正极浆料的铝箔置于70℃恒温烘箱中真空干燥12h,即得正极极片,将所得正极极片用切片机切成直径为1.2cm的圆片,用分析天平称量,质量为7.69mg;
(2)组装锂离子电池:采用CR2032型扣式电池体系,取步骤(1)制备的正极极片,以锂片(购自天津中能锂业有限公司,直径15.8mm*0.58mm)为负极极片,以含有1MLiPF6的EC/DMC(EC/DMC体积比1:1)溶液为电解液,装配成扣式电池,即得所述的锂离子电池。
Claims (4)
1.一种如式(I)所示的聚吡咯-3-甲酸,其特征在于,所述的聚吡咯-3-甲酸按如下方法制备得到:
将吡咯-3-甲酸溶于四氯化碳中得到吡咯-3-甲酸溶液,将FeCl3溶于硝基甲烷中得到FeCl3溶液,将所得FeCl3溶液滴加到吡咯-3-甲酸溶液中,于-10~0℃,N2保护的条件下反应20~24h,之后反应液经抽滤,滤饼用去离子水、乙醇洗涤,置于烘箱中于60~70℃真空干燥10~12h,即得聚吡咯-3-甲酸;
所述四氯化碳的体积用量以吡咯-3-甲酸的质量计为70~80mL/g;所述硝基甲烷的体积用量以FeCl3的质量计为20~25mL/g;所述吡咯-3-甲酸与FeCl3的物质的量之比为1:2.9~3.0;
式(I)中,n为100~1000的整数。
2.如式(I)所示的聚吡咯-3-甲酸作为锂离子电池正极材料的应用。
3.如式(I)所示的聚吡咯-3-甲酸作为锂离子电池正极材料在组装锂离子电池中的应用。
4.如权利要求3所述的应用,其特征在于,所述组装锂离子电池的方法为:
(1)制备正极极片:将聚吡咯-3-甲酸研磨至300~400目的粉末,然后将聚吡咯-3-甲酸粉末与乙炔黑、PVDF混合,滴加N-甲基吡咯烷酮,搅拌形成正极浆料,将所得正极浆料涂布在铝箔上,然后将涂布有正极浆料的铝箔置于60~70℃恒温烘箱中真空干燥10~12h,即得正极极片;
所述聚吡咯-3-甲酸粉末与乙炔黑、PVDF的质量比为50:40:10;所述N-甲基吡咯烷酮的体积用量以聚吡咯-3-甲酸粉末的质量计为20mL/g;所述正极浆料在铝箔上的涂布厚度为90μm;
(2)组装锂离子电池:取步骤(1)制备的正极极片,以锂片为负极极片,以含有LiPF6的EC/DMC溶液为电解液,装配成扣式电池,即得所述的锂离子电池;所述电解液中,LiPF6的含量为1M,EC/DMC体积比为1:1。
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