CN115302884A - 一种耐电解液性能的铝塑复合膜及其制备方法 - Google Patents
一种耐电解液性能的铝塑复合膜及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种耐电解液性能的铝塑复合膜，包括铝箔层，设于所述铝箔层一侧的保护层，设于所述铝箔层另一侧的密封层，所述密封层包括中间层、设于所述中间层一侧的热封层，设于所述中间层另一侧的粘接层，所述粘接层与所述铝箔层粘结，所述中间层的制备原料包含氟树脂。该铝塑复合膜在中间层的制备原料中引入氟树脂，氟树脂具有低摩擦系数、且耐腐蚀性好，是一种较好的绝缘材料，能够与聚丙烯较相容，且性能稳定不易从聚丙烯材料中析出，避免出现迁移情形，因此，既能提高聚丙烯膜的耐电解液性能，也不会影响其流延工艺和冲深性能。
Description
技术领域
本发明涉及锂电池包装技术领域，更具体地涉及一种耐电解液性能的铝塑复合膜及其制备方法。
背景技术
锂离子电池广泛应用于数码、交通工具、军事以及储能方面的新能源系统，目前锂电池软包装膜主要应用的是铝塑复合膜，铝铝塑复合膜(也简称铝塑膜)由外层的尼龙保护层、中间的铝层以及内层的CPP(聚丙烯)层组成。内层聚丙烯膜直接接触电解液，电解液主要由有机溶剂、六氟磷酸锂为主的锂盐组成，聚丙烯膜要承受溶剂的溶胀，以及要耐受六氟磷酸锂遇水分解的HF的腐蚀，这就要求与铝箔粘结的聚丙烯膜要具备优异的耐电解液性能。聚丙烯本身是不具备耐溶剂及酸腐蚀的性能，一般在聚丙烯中加入特定材料起到减轻来自电解液对铝箔和CPP复合界面的渗透腐蚀，在一定程度上起到提高耐电解液性能的功效，常规方式是在聚丙烯流延过程中加入酰胺类爽滑剂以降低摩擦系数，但是该材料的加入对流延工艺和冲深性能有影响，由于该类爽滑剂在存储及温度变化过程中容易析出及分布不均匀，进而出现冲深性能、耐电解液性能不佳。
因此，很有必要在聚丙烯流延过程中加入新材料，既能实现耐电解液性能优良的铝塑复合膜，又不会影响其流延工艺和冲深性能。
发明内容
为了克服现有技术的缺陷，本发明的目的是提供一种铝塑复合膜，既具有优良的耐电解液性能，也具有良好的冲深性能。
为了实现上述目的，本发明公开了一种耐电解液性能的铝塑复合膜，包括铝箔层，设于所述铝箔层一侧的保护层，设于所述铝箔层另一侧的密封层，所述密封层包括中间层、设于所述中间层一侧的热封层，设于所述中间层另一侧的粘接层，所述粘接层与所述铝箔层粘结，所述中间层的制备原料包含氟树脂。
与现有技术相比，该铝塑复合膜，在中间层的制备原料中引入氟树脂，氟树脂具有低摩擦系数、且耐腐蚀性好，是一种较好的绝缘材料，能够与聚丙烯较相容，且性能稳定不易从聚丙烯材料中析出，避免出现迁移情形，因此，既能提高聚丙烯膜的耐电解液性能，也不会影响其流延工艺和冲深性能。
较佳地，结合流延工艺的需求，通常聚丙烯的熔点在130-170℃，流延温度在220-250℃，引入熔点较高于聚丙烯的氟树脂，氟树脂的熔点为170-230℃，比如可为但不限于170℃、180℃、190℃、200℃、210℃、220℃、230℃。优选地，氟树脂的熔点为170-190℃，氟树脂熔点过高，会影响流延时的温度，需要调整流延工艺窗口，以及过高熔点氟树脂的引入会影响铝塑膜封装效果的传热效果，影响热封强度。
较佳地，所述氟树脂选自聚偏氟乙烯(熔点为170-180℃)、聚三氟氯乙烯(熔点为213℃)、聚全氟乙丙烯(熔点为200℃)及其衍生物中的至少一种。优选采用聚偏氟乙烯，因其熔点缘故，与聚丙烯进行挤出时，有利于流延工艺。
较佳地，所述氟树脂的加入量为所述中间层总质量的20-40％，可为但不限于20％、22％、24％、26％、28％、30％、32％、34％、36％、38％、40％。还应理解的是，当氟树脂的加入量过高时，聚丙烯含量下降，会影响封装效果，进而使得热封强度下降，且氟树脂加入量越大，对于流延工艺要求也越高，且耐电解液性能反而下降，而氟树脂加入量较小，则对耐电解液性能影响不大。
较佳地，所述中间层的制备材料还包括均聚聚丙烯、嵌段共聚聚丙烯、聚丙烯弹性体和增塑剂。
较佳地，所述中间层的制备材料，按质量百分数计，包括30-50％均聚聚丙烯、10-20％嵌段共聚聚丙烯、20-40％氟树脂、10-20％聚丙烯弹性体和0.5-2％增塑剂。优选地，均聚聚丙烯的含量可为但不限于30％、35％、40％、45％、50％；嵌段共聚聚丙烯的含量可为但不限于12％、14％、16％、18％、20％；聚丙烯弹性体的含量可为但不限于12％、14％、16％、18％、20％；增塑剂的含量可为但不限于0.5％、1％、1.5％、2％；
较佳地，所述热封层的制备材料包括无规共聚聚丙烯和抗粘连母料。进一步地，热封层的制备材料还包括硅酮类爽滑剂，提高爽滑性。
较佳地，所述粘结层包括马来酸酐改性聚丙烯和聚烯烃弹性体。
较佳地，较佳地，保护层选自尼龙膜和/或PET膜。
相应地，本发明还提供一种耐电解液性能的铝塑复合膜的制备方法，包括步骤：
(1)将包含氟树脂的中间层制备材料，粘接层制备材料和热封层制备材料挤出制得密封层；
(2)在铝箔的哑面复合保护层；
(3)在铝箔的亮面复合密封层，制得铝塑包装膜。
较佳地，步骤(1)中挤出温度为240-260℃。
较佳地，进行步骤(2)之前采用钝化液对铝箔进行双面钝化，钝化液包括硝酸铬、水性环氧树脂、磷酸。进一步地，硝酸铬、水性环氧树脂和水按照2：5：93质量比混合后，再用磷酸调节pH至3。
具体实施方式
为详细说明本发明的技术内容、构造特征、所实现目的及效果，以下结合实施方式详予说明。
实施例1
一种铝塑复合膜的制备方法，包括步骤：
(1)粘接层的制备原料为马来酸酐接枝改性聚丙烯(QE840)、聚丙烯弹性体(埃克森美孚)，按质量比为4:1混合均匀；
热封层的制备原料为无规共聚聚丙烯(沙特基础PPQF673K)、抗粘连母料(SAB-7203S)和硅酮类爽滑剂(道康宁MB25-381)，按照94:3:3质量比混合均匀；
中间层的制备原料为均聚聚丙烯(中海壳牌的HP510M)、嵌段共聚聚丙烯(JJP的WMG03X)、氟树脂聚偏氟乙烯、聚丙烯弹性体(埃克森美孚3000)、增塑剂磷酸三甲苯酯，按照40:15:30:14:1质量比混合均匀；
将粘接层的制备原料、中间层的制备原料和热封层的制备原料分别混合后吸入到对应的料斗中，三层厚度分别为7μm、26μm、7μm，通过三螺杆定量输送、挤出机挤出(挤出温度为240-260℃)及过滤、从T形模头流延经冷却辊冷却、切边、收卷、再分切，制得聚丙烯膜，即密封层，厚度40μm；
(2)将铝箔(河南明泰，厚度为40μm)的哑面和亮面均采用钝化液进行钝化处理，具体的，采用含硝酸铬、水性环氧树脂、磷酸的钝化液对铝箔进行双面钝化，然后在150℃烘干待用，其中，硝酸铬、水性环氧树脂和水按照2：5：93质量比混合后，再用磷酸调节pH至3，得到钝化液；
(3)将钝化处理后的铝箔哑面与保护层(长塑25μm尼龙膜)干式复合后，然后在60℃固化3天，制得半成品；
(4)将半成品中铝箔的亮面与密封层热法复合，即得铝塑复合膜。
实施例2
本实施例与实施例1基本相同，不同在于：
实施例2中间层的制备原料为均聚聚丙烯(中海壳牌的HP510M)、嵌段共聚聚丙烯(JJP的WMG03X)、氟树脂聚偏氟乙烯、聚丙烯弹性体(埃克森美孚3000)、增塑剂磷酸三甲苯酯，按照30:15:40:14:1质量比混合均匀。
其余与实施例1相同，在此不再阐述。
实施例3
本实施例与实施例1基本相同，不同在于：
实施例3中间层的制备原料为均聚聚丙烯(中海壳牌的HP510M)、嵌段共聚聚丙烯(JJP的WMG03X)、聚全氟乙丙烯、聚丙烯弹性体(埃克森美孚3000)、增塑剂磷酸三甲苯酯，按照45:20:20:13:2质量比混合均匀。
其余与实施例1相同，在此不再阐述。
实施例4
本实施例与实施例1基本相同，不同在于：
实施例4中间层的制备原料氟树脂为聚三氟乙烯，而实施例1中氟树脂为氟树脂聚偏氟乙烯，其余与实施例1相同，在此不再阐述。
实施例5
本实施例与实施例1基本相同，不同在于：
实施例5中间层的制备原料为均聚聚丙烯(中海壳牌的HP510M)、嵌段共聚聚丙烯(JJP的WMG03X)、氟树脂聚偏氟乙烯、聚丙烯弹性体(埃克森美孚3000)、增塑剂磷酸三甲苯酯，按照10:15:60:14:1质量比混合均匀。
其余与实施例1相同，在此不再阐述。
对比例1
本对比例与实施例1基本相同，不同在于：
对比例1中间层的制备原料为均聚聚丙烯(中海壳牌的HP510M)、嵌段共聚聚丙烯(JJP的WMG03X)、聚丙烯弹性体(埃克森美孚3000)、增塑剂磷酸三甲苯酯，按照70:15:14:1质量比混合均匀。
其余与实施例1相同，在此不再阐述。
将实施例1-5和对比例1制得铝塑复合膜进行性能检测：
耐电解液性能：将样条裁切为15mm宽，150mm长，测得CPP/Al初始剥离力，放入1mol/L六氟磷酸锂电解液中，并加入1％水，然后放在85度烘箱烘烤24h后测试CPP与铝箔的末期剥离力(即测得耐电解液性能)，结果如表1所示。
流延时加工难度在现场通过观察得到，并通过放慢流延速度进行一定的缓解。
热封强度：将铝塑膜裁切为(15±0.1)mm宽的长样条，按照QB/T 2358-1998的规定进行试验，热封条件如下：热封温度180℃，压力0.5MPa，时间3s，封装后用拉力试验机测试其封装强度。
冲深深度：将铝塑膜裁切120*150mm大小的样片，用冲壳机进行冲深，坑位尺寸55*60mm，设定冲壳深度Xmm，连续冲壳40个，在暗箱中用强光电筒对着坑位观察有无透光判定是否破损，如未破损则在X基础上增加0.2mm深度，如Xmm概率性破损，则在X基础上降低0.2mm深度，按上述方法继续冲深及观察破损情况。冲深深度H最终以某个深度不破，同时增加0.2mm出现概率性破损，以此时的不破值作为冲深深度的结果。
表1性能测试结果
注释：☆数量越多代表工艺难度越大。
由表1的数据可知，实施例1与对比例1相比，当中间层中加入氟树脂后，其流延工艺虽然增加难度，但难度增加不大，却能够有效提高其耐电解液性能，且冲深性能优良。这是由于在中间层的制备原料中引入氟树脂，氟树脂具有低摩擦系数、且耐腐蚀性好，是一种较好的绝缘材料，能够与聚丙烯较相容，且性能稳定不易从聚丙烯材料中析出，避免出现迁移情形，因此，既能提高聚丙烯膜的耐电解液性能，也不会影响其流延工艺和冲深性能。
实施例2与实施例1，氟树脂含量的增加流延工艺难度增加，性能并未同比呈正相关，氟树脂含量超过40％后铝塑膜性能可能呈下降趋势，实施例2同比优于对比例1的耐腐性性能，但是需要克服流延加工工艺难度，需要配合温度提升或者流延速度放慢给予足够热的热量，保证流延的稳定性。
实施例3中聚全氟乙丙烯的熔点较实施例2中聚偏氟乙烯高了20℃左右，加入的比例在控制范围的中间范围，流延难度与实施例2差不多，耐腐性性能和冲深性能也是明显优于对比例1。
实施例4加入的氟树脂聚三氟乙烯熔点较实施例1聚偏氟乙烯高出35℃左右，流延工艺难度更大，同时由于流延效果不是最佳的，影响了材料的相容性、以及可能影响了稳定挤出，造成材料未能发挥最佳效果，冲深深度同比实施例1、2、3偏低了0.2mm。
实施例5的试验数据可知，氟树脂由于本身熔点高，粘度大，流延工艺会增加一定的难度，因此，其添加量不宜过多，氟树脂的加入量超过中间层总质量的50％后，可能会影响材料的相容性、以及稳定挤出，造成材料未能发挥最佳效果，耐电解液性能反而下降，同时聚丙烯含量下降，会影响封装效果，进而使得热封强度下降。
以上所揭露的仅为本发明的优选实施例而已，当然不能以此来限定本发明之权利范围，因此依本发明申请专利范围所作的等同变化，仍属本发明所涵盖的范围。
Claims (10)
1.一种耐电解液性能的铝塑复合膜，其特征在于，包括铝箔层，设于所述铝箔层一侧的保护层，设于所述铝箔层另一侧的密封层，
所述密封层包括中间层、设于所述中间层一侧的热封层，设于所述中间层另一侧的粘接层，所述粘接层与所述铝箔层粘结，
所述中间层的制备原料包含氟树脂。
2.如权利要求1所述的耐电解液性能的铝塑复合膜，其特征在于，所述氟树脂的熔点为170-230℃。
3.如权利要求1所述的耐电解液性能的铝塑复合膜，其特征在于，所述氟树脂选自聚三氟氯乙烯、聚全氟乙丙烯、聚偏氟乙烯及其衍生物中的至少一种。
4.如权利要求1所述的耐电解液性能的铝塑复合膜，其特征在于，所述氟树脂的加入量为所述中间层总质量的20-40％。
5.如权利要求1所述的耐电解液性能的铝塑复合膜，其特征在于，所述中间层的制备材料还包括均聚聚丙烯、嵌段共聚聚丙烯、聚丙烯弹性体和增塑剂。
6.如权利要求5所述的耐电解液性能的铝塑复合膜，其特征在于，所述中间层的制备材料，按质量百分数计，包括30-50％均聚聚丙烯、10-20％嵌段共聚聚丙烯、20-40％氟树脂、10-20％聚丙烯弹性体和0.5-2％增塑剂。
7.如权利要求1所述的耐电解液性能的铝塑复合膜，其特征在于，所述热封层的制备材料包括无规共聚聚丙烯和抗粘连母料。
8.如权利要求1所述的耐电解液性能的铝塑复合膜，其特征在于，所述粘结层包括马来酸酐改性聚丙烯和聚烯烃弹性体。
9.一种如权利要求1-8任一项所述的耐电解液性能的铝塑复合膜的制备方法，其特征在于，包括步骤：
(1)将包含氟树脂的中间层制备材料，粘接层制备材料和热封层制备材料挤出制得密封层；
(2)在铝箔的哑面复合保护层；
(3)在铝箔的亮面复合密封层，制得铝塑包装膜。
10.如权利要求9所述的耐电解液性能的铝塑复合膜的制备方法，其特征在于，步骤(1)中，挤出温度为240-260℃。
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| CN109378410A (zh) * | 2018-09-26 | 2019-02-22 | 成都新柯力化工科技有限公司 | 一种锂电池用防腐蚀铝塑膜 |
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| CN109378410A (zh) * | 2018-09-26 | 2019-02-22 | 成都新柯力化工科技有限公司 | 一种锂电池用防腐蚀铝塑膜 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116001399A (zh) * | 2022-12-08 | 2023-04-25 | 江西省盛纬材料有限公司 | 一种耐腐蚀的铝塑复合膜及其制备方法 |
| WO2024119738A1 (zh) * | 2022-12-08 | 2024-06-13 | 江西省盛纬材料有限公司 | 一种耐腐蚀的铝塑复合膜及其制备方法 |
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