CN112142890A - 一种环碳酸酯聚合物粘结剂及其制备方法和应用 - Google Patents
一种环碳酸酯聚合物粘结剂及其制备方法和应用 Download PDFInfo
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- CN112142890A CN112142890A CN202010824745.5A CN202010824745A CN112142890A CN 112142890 A CN112142890 A CN 112142890A CN 202010824745 A CN202010824745 A CN 202010824745A CN 112142890 A CN112142890 A CN 112142890A
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- cyclic carbonate
- polymer binder
- electrode
- unsaturated double
- double bonds
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- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 claims description 2
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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Abstract
本发明公开了一种环碳酸酯聚合物粘结剂及其制备方法和应用,本发明聚合物粘结剂由带有不饱和双键的环碳酸酯和带有不饱和双键的功能单体发生自由基聚合反应获得;且聚合物粘结剂在制备二次锂电池的电极中应用良好。且将环碳酸酯聚合物粘结剂制备的电极的制备方法如下:将电极活性材料、环碳酸酯聚合物粘结剂和导电剂加入至有机溶剂中,混合均匀得到粘稠的浆料,将其用刮刀涂布于导电集流体上置于60‑120℃烘箱干燥12h得到极片。本发明粘结剂用于锂二次电池,大幅度延长电池的循环寿命,提高容量保持率。有利于提高电极润湿性,加速离子传导。
Description
技术领域
本发明公开了一种环碳酸酯聚合物粘结剂的制备方法,并将其应用在锂二次电池。
背景技术
随着科技的进步,电子设备和电动汽车等行业快速发展,人们对高能量密度、可快速充电的电池系统需求越来越大。在过去的几十年中,锂离子电池由于其可快速充放电、充电效率高、工作温度范围宽、放电电压高、自放电率低、对环境友好和使用寿命长等众多优点得到了广泛的应用。
锂硫电池由于具有高达2600Whkg-1的理论能量密度,硫具有高达1675mAhg-1的理论容量,且硫价格低廉、储量丰富,是下一代电池体系的候选材料。然而,锂硫电池存在一些问题:活性物质硫的电导率低;电化学反应中间产物多硫化锂存在“穿梭效应”造成活性物质损失;充放电过程巨大的体积膨胀,造成电极粉化脱落,导致容量快速衰减,因此锂硫电池实际应用还面临着巨大的挑战。
为解决以上问题,电极中的粘结剂受到了广泛的关注,它将活性物质和导电剂粘合在集流体上,只需要使用相对较低的质量分数,就可以使电极保持完整性和具有良好的电连接性。虽然粘结剂属于电化学惰性组分,但其性能的好坏对电极材料的性能具有显著影响。传统锂电池电极以聚偏氟乙烯(PVDF)为粘结剂,其不具备离子电导性,仅依靠范德华力粘结集流体和活性物质难以克服硫的体积膨胀。
碳酸亚乙烯酯和碳酸乙烯亚乙酯是常见的电解液添加剂,在电池充放电过程中,可以在电极表面聚合成聚碳酸酯,是固体电解液界面层(SEI)的主要成分,改善了界面相容性和循环稳定性。受此启发,环状碳酸酯基聚合物有望作为锂电池粘结剂使用,以提高粘结剂离子电导率,改善电极润湿性,增强界面相容性。
发明内容
本发明要解决的技术问题是,克服现有技术中的不足,提供一种适用于锂二次电池的粘结剂制备方法。
为解决技术问题,本发明的解决方案是:
一种环碳酸酯聚合物粘结剂,其特征在于:该聚合物粘结剂由带有不饱和双键的环碳酸酯和带有不饱和双键的功能单体发生自由基聚合反应获得;其中自由基引发带有不饱和双键的环碳酸酯自聚,或与带有不饱和双键的功能单体共聚;带有不饱和双键的环碳酸酯占聚合物粘结剂总质量的10-100%;带有不饱和双键的功能单体占聚合物粘结剂总质量的0-90%;自由基聚合反应温度为30-150℃。
优选的,带有不饱和双键的环碳酸酯占聚合物粘结剂总质量的50-100%;带有不饱和双键的功能单体占聚合物粘结剂总质量的0-50%。
所述聚合物粘结剂由自由基引发,通过打开单体中的双键进行聚合,具有高离子电导率(1.2×10-6-7.9×10-4Scm-1)和良好的电解液润湿性(接触角测试仪显示电解液滴落后0.2s完全铺展)。
优选的,所述自由基聚合反应温度为50-80℃。
所述带有不饱和双键的环碳酸酯为碳酸亚乙烯酯、碳酸乙烯亚乙酯。
所述带有不饱和双键的功能单体为聚乙二醇二甲基丙烯酸酯、丙烯酸丁酯、丙烯酸、甲基丙烯酸甲酯、甲基丙烯酸缩水甘油酯、丙烯腈、丙烯酰胺、苯乙烯中的一种或几种。
所述自由基引发剂为偶氮二异丁氰、偶氮二异庚腈、过氧化二苯甲酰等。
所述聚合物粘结剂应用在制备二次锂电池的电极中。
所述的一种环碳酸酯聚合物粘结剂制备的电极,其特征在于:电极包括电极活性材料、环碳酸酯聚合物粘结剂和导电剂;其中电极活性材料在电极中的质量分数为50-95%;环碳酸酯聚合物粘结剂在电极中的质量分数为2.5-25%;导电剂在电极中的质量分数为2.5-25%。
优选的,活性材料在电极中的质量分数为70-90%;环碳酸酯聚合物粘结剂在电极中的质量分数为5-15%;导电剂在电极中质量分数为5-15%。
一种环碳酸酯聚合物粘结剂制备的电极的制备方法,将电极活性材料、环碳酸酯聚合物粘结剂和导电剂加入至有机溶剂中,混合均匀得到粘稠的浆料,将其用刮刀涂布于导电集流体上置于60-120℃烘箱干燥12h得到极片。
所述的电极活性材料为钴酸锂、磷酸铁锂、磷酸锰铁锂、锰酸锂、镍锰酸锂、三元材料、硫、硫复合物中的一种或几种。
所述的导电剂包括石墨、SuperP、科琴黑和乙炔黑的一种或几种。
所述的有机溶剂包括N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAC)、二甲基亚砜(DMSO)和N-甲基吡咯烷酮(NMP)中的一种或几种。
所述的导电集流体包括铜箔、铝箔、不锈钢、碳纸、泡沫镍、铜网和铝网中的一种。优选铝箔或铜箔。
本发明原理描述:
本发明粘结剂由带有不饱和双键的环碳酸酯和带有不饱和双键的功能单体发生自由基聚合反应,用于锂二次电池,大幅度延长电池的循环寿命,提高容量保持率。聚环碳酸酯与电解液结构相似,有利于提高电极润湿性,同时具有高离子电导率,有利于加速离子传导。功能单体具备柔性,可以克服体积膨胀或者含有氨基、羟基、环氧等官能团,可以固定多硫化锂,或者发生交联形成网络结构。
与现有技术相比,本发明的有益效果是:
1、本发明提出环碳酸酯聚合物用作锂二次电池粘结剂,其离子电导率高,电解液浸润性好,适应于多种电极材料体系,能够解决目前的锂电池存在的循环寿命短、容量保持低率等问题。
2、本发明中自由基聚合反应条件温和,无需无水无氧的苛刻条件,可以采用一锅法制备;
3、参与共聚的功能单体含有氨基、羟基等官能团,可以抑制锂硫电池中多硫化物的穿梭效应。
具体实施方式
下面结合实例对本发明作进一步的说明:
实施例1:
取10g碳酸亚乙烯酯(VC)、0.1g偶氮二异丁氰(AIBN),加入50mL的三口烧瓶中,三口烧瓶配有磁子搅拌、冷凝管和恒压漏斗,升高温度至60℃,反应4h,加入10gN,N-二甲基甲酰胺(DMF),继续反应8h,得到粘稠液体,记为PVCA。
取0.08g磷酸铁锂(LiFePO4)、0.01g碳粉(SuperP)、0.01gPVCA(干物质)、450微升N-甲基吡咯烷酮(NMP),研磨均匀涂覆在涂碳铝箔上,80℃烘干12h。切成直径为14mm的电极片,以锂片为对电极,PP/PE/PP(Celgard2325)复合隔膜为电池隔膜,碳酸乙烯酯/碳酸二甲酯/碳酸甲乙酯(体积比1:1:1)、1MLiPF6为电解液,装备扣式电池。
取0.08g硫碳复合材料(S:C质量比7:3)、0.01g碳粉(SuperP)、0.01gPVCA(干物质)、450微升N-甲基吡咯烷酮(NMP),研磨均匀涂覆在涂碳铝箔上,60℃烘干12h。切成直径为14mm的电极片,以锂片为对电极,PP/PE/PP(Celgard2325)复合隔膜为电池隔膜,1,3-二氧戊环/乙二醇二甲醚(体积比1:1)、1MLiTFSI和1wt.%LiNO3为电解液,装备扣式电池。采用深圳新威电子有限公司的BTS-5V/50mA型充放电循环测试仪对电池的循环性能进行测试。
实施例2:
取10g碳酸乙烯亚乙酯(VEC)、0.1g偶氮二异丁氰(AIBN),加入50mL的三口烧瓶中,三口烧瓶配有磁子搅拌和冷凝管,升高温度至80℃,反应24h,得到粘稠液体,记为PVEC。
以PVEC作为粘结剂,按实施例1的方法制备扣式电池,进行测试。
实施例3:
取10g碳酸亚乙烯酯(VC)、3g聚乙二醇二甲基丙烯酸酯(PEGMA)、0.13g偶氮二异丁氰(AIBN),加入50mL的三口烧瓶中,三口烧瓶配有磁子搅拌、冷凝管和恒压漏斗,升高温度至50℃,反应4h,加入13gN,N-二甲基甲酰胺(DMF),继续反应8h,得到粘稠液体,记为PVCAPEG。
以PVCAPEG作为粘结剂,按实施例1的方法制备扣式电池,进行测试。
实施例4:
取10g碳酸乙烯亚乙酯(VEC)、3g聚乙二醇二甲基丙烯酸酯(PEGMA)、0.13g偶氮二异丁氰(AIBN),加入50mL的三口烧瓶中,三口烧瓶配有磁子搅拌、冷凝管和恒压漏斗,升高温度至50℃,反应4h,加入13gN,N-二甲基甲酰胺(DMF),继续反应8h,得到粘稠液体,记为PVECPEG。
以PVECPEG作为粘结剂,按实施例1的方法制备扣式电池,进行测试。
实施例5:
取5g碳酸亚乙烯酯(VC)、5g碳酸乙烯亚乙酯(VEC)、0.1g过氧化二苯甲酰(BPO),加入50mL的三口烧瓶中,三口烧瓶配有磁子搅拌、冷凝管和恒压漏斗,升高温度至80℃,反应4h,加入10gN,N-二甲基甲酰胺(DMF),继续反应8h,得到粘稠液体,记为PVCAVEC。
以PVCAVEC作为粘结剂,按实施例1的方法制备扣式电池,进行测试。
实施例6:
取7g碳酸乙烯亚乙酯(VEC)、1.97g丙烯酸丁酯(BA)、0.09g偶氮二异丁氰(AIBN),加入50mL的三口烧瓶中,三口烧瓶配有磁子搅拌和冷凝管,升高温度至80℃,反应12h,得到粘稠液体,记为PVECBA。
以PVECBA作为粘结剂,按实施例1的方法制备扣式电池,进行测试。
实施例7:
取7g碳酸亚乙烯酯(VC)、1.47g丙烯酸(AA)、0.085g偶氮二异丁氰(AIBN),加入50mL的三口烧瓶中,三口烧瓶配有磁子搅拌、冷凝管和恒压漏斗,升高温度至60℃,反应2h,加入20gN,N-二甲基甲酰胺(DMF),继续反应8h,得到粘稠液体,记为PVCAAA。
取0.08g磷酸铁锂(LiFePO4)、0.01g碳粉(SuperP)、0.01gPVCAAA(干物质)、350微升N,N-二甲基甲酰胺(DMF),研磨均匀涂覆在涂碳铝箔上,80℃烘干12h。切成直径为14mm的电极片,以锂片为对电极,PP/PE/PP(Celgard2325)复合隔膜为电池隔膜,碳酸乙烯酯/碳酸二甲酯/碳酸甲乙酯(体积比1:1:1)、1MLiPF6为电解液,装备扣式电池,采用深圳新威电子有限公司的BTS-5V/50mA型充放电循环测试仪对电池的循环性能进行测试。
取0.08g硫碳复合材料(S:C质量比7:3)、0.01g碳粉(SuperP)、0.01gPVCA(干物质)、400微升N,N-二甲基甲酰胺(DMF),研磨均匀涂覆在涂碳铝箔上,60℃烘干12h。切成直径为14mm的电极片,以锂片为对电极,PP/PE/PP(Celgard2325)复合隔膜为电池隔膜,1,3-二氧戊环/乙二醇二甲醚(体积比1:1)、1MLiTFSI和1wt.%LiNO3为电解液,装备扣式电池。采用深圳新威电子有限公司的BTS-5V/50mA型充放电循环测试仪对电池的循环性能进行测试。
实施例8:
取7g碳酸亚乙烯酯(VC)、2.04g甲基丙烯酸甲酯(MMA)、0.091g偶氮二异丁氰(AIBN),加入50mL的三口烧瓶中,三口烧瓶配有磁子搅拌、冷凝管和恒压漏斗,升高温度至75℃,反应12h,得到粘稠液体,记为PVCAMMA。
取0.08g磷酸铁锂(LiFePO4)、0.01g碳粉(SuperP)、0.01gPVCAMMA(干物质)、500微升二甲基亚砜(DMSO),研磨均匀涂覆在涂碳铝箔上,80℃烘干12h。切成直径为14mm的电极片,以锂片为对电极,PP/PE/PP(Celgard2325)复合隔膜为电池隔膜,碳酸乙烯酯/碳酸二甲酯/碳酸甲乙酯(体积比1:1:1)、1MLiPF6为电解液,装备扣式电池,采用深圳新威电子有限公司的BTS-5V/50mA型充放电循环测试仪对电池的循环性能进行测试。
取0.08g硫碳复合材料(S:C质量比7:3)、0.01g碳粉(SuperP)、0.01gPVCAMMA(干物质)、400微升二甲基亚砜(DMSO),研磨均匀涂覆在涂碳铝箔上,60℃烘干12h。切成直径为14mm的电极片,以锂片为对电极,PP/PE/PP(Celgard2325)复合隔膜为电池隔膜,1,3-二氧戊环/乙二醇二甲醚(体积比1:1)、1MLiTFSI和1wt.%LiNO3为电解液,装备扣式电池。采用深圳新威电子有限公司的BTS-5V/50mA型充放电循环测试仪对电池的循环性能进行测试。
实施例9:
取7g碳酸亚乙烯酯(VC)、2.89g甲基丙烯酸缩水甘油酯(GMA)、0.099g过氧化二苯甲酰(BPO),加入50mL的三口烧瓶中,三口烧瓶配有磁子搅拌、冷凝管和恒压漏斗,升高温度至70℃,反应4h,加入20gN,N-二甲基甲酰胺(DMF),继续反应8h,得到粘稠液体,记为PVCAGMA。
以PVCAGMA作为粘结剂,按实施例1的方法制备扣式电池,进行测试。
对比例1:
以市售商品聚偏二氟乙烯粉末(简称:PVDF,型号:KynarHSV900厂家:阿科玛PVDF)作为粘结剂乳液。按实施例1的方法制备扣式电池,进行测试。
对比例2:
以市售商品羧甲基纤维素II-丁苯橡胶乳液(简称CMC-SBR,其中,羧甲基纤维素II(CMC)型号为平均分子量250000Da,粘度1500~3100mPa·s,购买自阿拉丁试剂。丁苯胶乳质量固含量50%,购买自NIPPONA&L株式会社)。
取0.08g磷酸铁锂(LiFePO4)、0.01g碳粉(SuperP)、0.01gCMC-SBR(干物质)、500微升去离子水,研磨均匀涂覆在涂碳铝箔上,80℃烘干12h。切成直径为14mm的电极片,以锂片为对电极,PP/PE/PP(Celgard2325)复合隔膜为电池隔膜,碳酸乙烯酯/碳酸二甲酯/碳酸甲乙酯(体积比1:1:1)、1MLiPF6为电解液,装备扣式电池,采用深圳新威电子有限公司的BTS-5V/50mA型充放电循环测试仪对电池的循环性能进行测试。
取0.08g硫碳复合材料(S:C质量比7:3)、0.01g碳粉(SuperP)、0.01gCMC-SBR(干物质)、450微升去离子水,研磨均匀涂覆在涂碳铝箔上,60℃烘干12h。切成直径为14mm的电极片,以锂片为对电极,PP/PE/PP(Celgard2325)复合隔膜为电池隔膜,1,3-二氧戊环/乙二醇二甲醚(体积比1:1)、1MLiTFSI和1wt.%LiNO3为电解液,装备扣式电池。采用深圳新威电子有限公司的BTS-5V/50mA型充放电循环测试仪对电池的循环性能进行测试。
表1磷酸铁锂电池性能测试
表2锂硫电池性能测试
从上表中可以看出,用环碳酸酯聚合物粘结剂制备的电极容量保持率高于传统商用粘结剂。利用碳酸亚乙烯酯(VC)和丙烯酸(AA)共聚得到的PVCAAA粘结剂,其所制备的磷酸铁锂电池具有最高的容量保持率,聚碳酸亚乙烯酯与电解液结构相似,有利于电极充分润湿,聚丙烯酸的胶水状结构充分包覆电极材料,使电极材料牢固附着在集流体上。利用碳酸乙烯亚乙酯(VEC)和聚乙二醇二甲基丙烯酸酯(PEGMA)共聚得到的PVECPEG粘结剂,其所制备的锂硫电池具有最高的初始容量和容量保持率,聚碳酸乙烯亚乙酯和聚乙二醇具有高离子电导率,有利于加速离子传导,同时聚乙二醇二甲基丙烯酸酯玻璃化转变温度低,链段具有柔性,可以缓解充放电过程中硫的体积膨胀,避免电极粉化脱落。
Claims (10)
1.一种环碳酸酯聚合物粘结剂,其特征在于:该聚合物粘结剂由带有不饱和双键的环碳酸酯和带有不饱和双键的功能单体发生自由基聚合反应获得;其中自由基引发带有不饱和双键的环碳酸酯自聚,或与带有不饱和双键的功能单体共聚;带有不饱和双键的环碳酸酯占聚合物粘结剂总质量的10-100%;带有不饱和双键的功能单体占聚合物粘结剂总质量的0-90%;自由基聚合反应温度为30-150℃。
2.根据权利要求1所述的一种环碳酸酯聚合物粘结剂,其特征在于:自由基聚合反应温度为50-80℃;带有不饱和双键的环碳酸酯占聚合物粘结剂总质量的50-100%;带有不饱和双键的功能单体占聚合物粘结剂总质量的0-50%。
3.根据权利要求1或2所述的一种环碳酸酯聚合物粘结剂,其特征在于:带有不饱和双键的环碳酸酯为碳酸亚乙烯酯和碳酸乙烯亚乙酯。
4.根据权利要求3所述的一种环碳酸酯聚合物粘结剂,其特征在于:带有不饱和双键的功能单体为聚乙二醇二甲基丙烯酸酯、丙烯酸丁酯、丙烯酸、甲基丙烯酸甲酯、甲基丙烯酸缩水甘油酯、丙烯腈、丙烯酰胺、苯乙烯中的一种或几种。
5.根据权利要求4所述的一种环碳酸酯聚合物粘结剂的应用,其特征在于所述聚合物粘结剂应用在制备二次锂电池的电极中。
6.根据权利要求4所述的一种环碳酸酯聚合物粘结剂制备的电极,其特征在于:电极包括电极活性材料、环碳酸酯聚合物粘结剂和导电剂;其中电极活性材料在电极中的质量分数为50-95%;环碳酸酯聚合物粘结剂在电极中的质量分数为2.5-25%;导电剂在电极中的质量分数为2.5-25%。
7.根据权利要求6所述的一种环碳酸酯聚合物粘结剂制备的电极的制备方法,其特征在于:将电极活性材料、环碳酸酯聚合物粘结剂和导电剂加入至有机溶剂中,混合均匀,将其用刮刀涂布于导电集流体上置于60-120℃烘箱干燥12h得到极片。
8.根据权利要求7所述的一种环碳酸酯聚合物粘结剂制备的电极的制备方法,其特征在于:所述的电极活性材料为钴酸锂、磷酸铁锂、磷酸锰铁锂、锰酸锂、镍锰酸锂、三元材料、硫、硫复合物中的一种或几种。所述的导电剂包括石墨、SuperP、科琴黑和乙炔黑的一种或几种。
9.根据权利要求7所述的一种环碳酸酯聚合物粘结剂制备的电极的制备方法,其特征在于:所述的有机溶剂包括N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、二甲基亚砜和N-甲基吡咯烷酮中的一种或几种。
10.根据权利要求7所述的一种环碳酸酯聚合物粘结剂制备的电极的制备方法,其特征在于所述的导电集流体包括铜箔、铝箔、不锈钢、碳纸、泡沫镍、铜网和铝网中的一种。
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CN114349893A (zh) * | 2021-12-27 | 2022-04-15 | 新纶电子材料(常州)有限公司 | 一种光学薄膜及其制备方法和应用 |
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CN114106501B (zh) * | 2021-12-16 | 2023-08-11 | 新纶电子材料(常州)有限公司 | 光学薄膜及共混树脂、制备方法、应用 |
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