CN115260556A - 一种纳米银线抗静电聚酯薄膜的制备方法 - Google Patents
一种纳米银线抗静电聚酯薄膜的制备方法 Download PDFInfo
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Abstract
本发明公开了一种纳米银线抗静电聚酯薄膜的制备方法，包括如下步骤：步骤一：准备原料，原料的重量组分分别为聚对苯二甲酸丁二醇酯70份，聚对苯二甲酸乙二醇酯30份，相容剂7.5份，碳纳米管6.5份，Fe3O4纳米线7.5份，石墨烯4份，纳米银线3份，表面处理剂0.8份，抗氧剂0.75份；步骤二：将上述原料混合均匀后加入到双螺杆共混造粒机内进行熔融混合成颗粒状；步骤三：将混料送入至干燥塔内进行烘干结晶；步骤四：干燥后的混料通过熔融挤出设备中挤出成型后以冷却，将冷却后的固体进行纵向拉伸和横向拉伸，最后热定型，得到抗静电聚酯薄膜。本发明制备的抗静电聚酯薄膜通过四种填料实现了在聚合物基体中填料的低接触电阻、高导电网络的有效搭建。
Description
技术领域
本发明涉及聚酯薄膜的制备领域，具体是一种纳米银线抗静电聚酯薄膜的制备方法。
背景技术
传统的抗静电聚酯薄膜加工工艺为：将抗静电剂/液通过涂布法涂覆在片材基层表面上，形成抗静电层；在聚酯薄膜基层上直接涂覆的涂布法具有见效快、用料省、对抗静电剂的耐热性要求低等优点，但抗静电效果不能持久，经过摩擦、紫外线光照、较高温存放后，抗静层表面电阻在3-5年后可能会逐步变化至7-9次方欧姆或更高，导致抗静电功能减弱或丧失，抗静电持久性差。因此，需一种持久抗静电聚酯薄膜材料，扩展聚酯薄膜的应用。
发明内容
本发明的目的是提供一种纳米银线抗静电聚酯薄膜的制备方法，来解决实际使用中，遇到的问题。
为实现上述目的，本发明提供如下技术方案：
一种纳米银线抗静电聚酯薄膜的制备方法，包括如下步骤：
步骤一：准备原料，原料的重量组分分别为聚对苯二甲酸丁二醇酯60～80份，聚对苯二甲酸乙二醇酯20～40份，相容剂5～10份，碳纳米管5～8份，Fe3O4纳米线5～10份，石墨烯3～5份，纳米银线1～5份，表面处理剂0.6～1份，抗氧剂0.5～1份；
步骤二：将上述原料混合均匀后加入到双螺杆共混造粒机内，由双螺杆共混造粒机将组分进行熔融混合成颗粒状，双螺杆共混造粒机的加热温度为280度，真空度为100Pa；
步骤三：将混料送入至干燥塔内进行烘干结晶，干燥塔预热温度为175℃，干燥至含水率≤200ppm；
步骤四：干燥后的混料通过熔融挤出设备中挤出成型后以72℃/min速度冷却，将冷却后的固体在110-115℃条件下进行纵向拉伸，在130-145℃条件下进行横向拉伸，在200-235℃进行热定型，得到抗静电聚酯薄膜。
优选的：Fe3O4纳米线通过以下制备方法得到：
步骤一：称取硫代硫酸钠和硫酸亚铁加入PEG和水的混合溶液中，用NaOH调节pH为1l，然后倒入反应釜内衬中；
步骤二：密封反应釜，在180℃下保温8h，反应结束冷却至室温；
步骤三：将黑色沉淀物用去离子水洗涤，去除多余的离子杂质，用磁铁进行沉降收集，60℃真空干燥，得到Fe3O4纳米线。
优选的：所述石墨烯的制备方式为将氧化石墨在600-1000℃，0.5-3min条件下还原剥离。
优选的：所述纳米银线的制备步骤为：在10-400mL0.1-0.5mMFeCl3的乙二醇溶液中，加入0.15-0.75M的PVP，搅拌至PVP完全溶解后，再逐滴加入10-400mL0.1-0.5M的AgNO3溶液，搅拌10-20分钟。然后把混合液转移至水热合成反应釜内，在160℃下反应2-4小时。自然冷却，即得到纳米银线。
优选的：所述相容剂由马来酸酐接枝丙烯腈-丁二烯-苯乙烯三元共聚物、马来酸酐接枝乙烯-辛烯共聚物、苯乙烯-丙烯腈-甲基丙烯酸缩水甘油酯三元无规共聚物中的一种或多种按任意配比混合组成。
优选的：所述表面处理剂由硅烷偶联剂、甲基硅油、硅酮粉中的一种或多种按任意配比混合组成。
优选的：所述抗氧剂由抗氧剂1010、抗氧剂168中的一种或两种按任意配比混合组成。
优选的：所述碳纳米管直径10-15nm，长度1-10μm；Fe3O4纳米线直径20-50nm，长度10-50μm。
优选的：所述石墨烯的厚度为0.35～20nm，直径为1～20μm。
优选的：所述纳米银线的直径为40～500nm，长度为5～50μm。
与现有技术相比，本发明的有益效果是：
本发明中纳米银线有很高的长径比，在体系中起桥梁作用，可以有效降低银填料的含量。有研究报道通过模板法制备纳米银线，并以此合成了各向同性导电胶，与传统导电胶相比，这种各向同性导电胶在纳米银线含量较低时就能具有更低的体积电阻率和较高的剪切强度，并利用场隧道效应发射理论解释了此体系的导电机理。石墨烯是当前最受瞩目的新型材料。自2004年Novoselov和Geim制备出石墨烯后，石墨烯的出现立刻引起了科学界的广泛关注，这种新型碳材料成为继富勒烯、碳纳米管后材料和物理学领域的又一个研究热点，各国学者都对石墨烯结构和性能展开大量研究。石墨烯是一种结晶度高并且能够稳定存在的单原子厚度碳膜，由碳原子六元环紧密构成的两维晶体，具有重复周期的蜂窝状点阵结构，可以翘曲成零维的富勒烯，卷成一维的碳纳米管或者堆积成三维的石墨。由于这种特殊的结构，石墨烯具备许多优异性能。通过碳纳米管、Fe3O4纳米线和石墨烯、纳米银线构筑形成复合抗静电材料，四种填料实现了在聚合物基体中填料的低接触电阻、高导电网络的有效搭建。突破性的采用二维和一维的金属纳米材料协同改性聚酯薄膜的抗静电性能，利用两者各自的优异性能的同时，也利用到它们一起产生的协同效应，因此使制备的复合材料具有优异的抗静电性能。通过检测，本发明申请制备的抗静电材料表面电阻率低至105～6Ω，同时抗静电能力持久。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述。
实施例1
本发明实施例中，一种纳米银线抗静电聚酯薄膜的制备方法，包括如下步骤：
步骤一：准备原料，原料的重量组分分别为聚对苯二甲酸丁二醇酯60份，聚对苯二甲酸乙二醇酯20份，相容剂5份，碳纳米管5份，Fe3O4纳米线5份，石墨烯3份，纳米银线1份，表面处理剂0.6份，抗氧剂0.5份；
步骤二：将上述原料混合均匀后加入到双螺杆共混造粒机内，由双螺杆共混造粒机将组分进行熔融混合成颗粒状，双螺杆共混造粒机的加热温度为280度，真空度为100Pa；
步骤三：将混料送入至干燥塔内进行烘干结晶，干燥塔预热温度为175℃，干燥至含水率≤200ppm；
步骤四：干燥后的混料通过熔融挤出设备中挤出成型后以72℃/min速度冷却，将冷却后的固体在110-115℃条件下进行纵向拉伸，在130-145℃条件下进行横向拉伸，在200-235℃进行热定型，得到抗静电聚酯薄膜。
需要说明的是，Fe3O4纳米线通过模板剂诱导从而控制各向异性生长最终形成线性结构，Fe3O4纳米线通过以下制备方法得到：
步骤一：称取硫代硫酸钠和硫酸亚铁加入PEG和水的混合溶液中，用NaOH调节pH为1l，然后倒入反应釜内衬中；
步骤二：密封反应釜，在180℃下保温8h，反应结束冷却至室温；
步骤三：将黑色沉淀物用去离子水洗涤，去除多余的离子杂质，用磁铁进行沉降收集，60℃真空干燥，得到Fe3O4纳米线。
所述石墨烯的制备方式为将氧化石墨在600-1000℃，0.5-3min条件下还原剥离。
所述纳米银线的制备步骤为：在10-400mL0.1-0.5mMFeCl3的乙二醇溶液中，加入0.15-0.75M的PVP，搅拌至PVP完全溶解后，再逐滴加入10-400mL0.1-0.5M的AgNO3溶液，搅拌10-20分钟。然后把混合液转移至水热合成反应釜内，在160℃下反应2-4小时。自然冷却，即得到纳米银线。
所述相容剂由马来酸酐接枝丙烯腈-丁二烯-苯乙烯三元共聚物、马来酸酐接枝乙烯-辛烯共聚物、苯乙烯-丙烯腈-甲基丙烯酸缩水甘油酯三元无规共聚物中的一种或多种按任意配比混合组成。
所述表面处理剂由硅烷偶联剂、甲基硅油、硅酮粉中的一种或多种按任意配比混合组成。
所述抗氧剂由抗氧剂1010、抗氧剂168中的一种或两种按任意配比混合组成。
所述碳纳米管直径10-15nm，长度1-10μm；Fe3O4纳米线直径20-50nm，长度10-50μm。
所述石墨烯的厚度为0.35～20nm，直径为1～20μm。
所述纳米银线的直径为40～500nm，长度为5～50μm。
所述碳纳米管直径10-15nm，长度1-10μm；Fe3O4纳米线直径20-50nm，长度10-50μm。
实施例2
一种纳米银线抗静电聚酯薄膜的制备方法，包括如下步骤：
步骤一：准备原料，原料的重量组分分别为聚对苯二甲酸丁二醇酯70份，聚对苯二甲酸乙二醇酯30份，相容剂7.5份，碳纳米管6.5份，Fe3O4纳米线7.5份，石墨烯4份，纳米银线3份，表面处理剂0.8份，抗氧剂0.75份；
步骤二：将上述原料混合均匀后加入到双螺杆共混造粒机内，由双螺杆共混造粒机将组分进行熔融混合成颗粒状，双螺杆共混造粒机的加热温度为280度，真空度为100Pa；
步骤三：将混料送入至干燥塔内进行烘干结晶，干燥塔预热温度为175℃，干燥至含水率≤200ppm；
步骤四：干燥后的混料通过熔融挤出设备中挤出成型后以72℃/min速度冷却，将冷却后的固体在110-115℃条件下进行纵向拉伸，在130-145℃条件下进行横向拉伸，在200-235℃进行热定型，得到抗静电聚酯薄膜。
实施例3
一种纳米银线抗静电聚酯薄膜的制备方法，包括如下步骤：
步骤一：准备原料，原料的重量组分分别为聚对苯二甲酸丁二醇酯80份，聚对苯二甲酸乙二醇酯40份，相容剂10份，碳纳米管8份，Fe3O4纳米线10份，石墨烯5份，纳米银线5份，表面处理剂1份，抗氧剂1份；
步骤二：将上述原料混合均匀后加入到双螺杆共混造粒机内，由双螺杆共混造粒机将组分进行熔融混合成颗粒状，双螺杆共混造粒机的加热温度为280度，真空度为100Pa；
步骤三：将混料送入至干燥塔内进行烘干结晶，干燥塔预热温度为175℃，干燥至含水率≤200ppm；
步骤四：干燥后的混料通过熔融挤出设备中挤出成型后以72℃/min速度冷却，将冷却后的固体在110-115℃条件下进行纵向拉伸，在130-145℃条件下进行横向拉伸，在200-235℃进行热定型，得到抗静电聚酯薄膜。
对比例1
步骤一中准备的原料重量组分分别为聚对苯二甲酸丁二醇酯60份，聚对苯二甲酸乙二醇酯20份，相容剂5份，碳纳米管5份，Fe3O4纳米线5份，石墨烯3份，纳米银线0份，表面处理剂0.6份，抗氧剂0.5份。
对比例2
步骤一中准备的原料重量组分分别为聚对苯二甲酸丁二醇酯60份，聚对苯二甲酸乙二醇酯20份，相容剂5份，碳纳米管5份，Fe3O4纳米线5份，石墨烯0份，纳米银线1份，表面处理剂0.6份，抗氧剂0.5份。
对比例3
步骤一中准备的原料重量组分分别为聚对苯二甲酸丁二醇酯60份，聚对苯二甲酸乙二醇酯20份，相容剂5份，碳纳米管5份，Fe3O4纳米线0份，石墨烯3份，纳米银线1份，表面处理剂0.6份，抗氧剂0.5份。
对比例4
步骤一中准备的原料重量组分分别为聚对苯二甲酸丁二醇酯60份，聚对苯二甲酸乙二醇酯20份，相容剂5份，碳纳米管0份，Fe3O4纳米线5份，石墨烯0份，纳米银线1份，表面处理剂0.6份，抗氧剂0.5份。
对比例5
步骤一中准备的原料重量组分分别为聚对苯二甲酸丁二醇酯60份，聚对苯二甲酸乙二醇酯20份，相容剂5份，碳纳米管5份，Fe3O4纳米线5份，石墨烯0份，纳米银线1份，表面处理剂0.6份，抗氧剂0.5份。
性能检测
将实施例1-5中制备的抗静电聚酯薄膜：用GB/T1410-2006进行表面电阻率测定。
表1性能检测结果
| 实施例1 | 10<sup>6～7</sup>Ω |
| 实施例2 | 10<sup>5～6</sup>Ω |
| 实施例3 | 10<sup>6～7</sup>Ω |
| 对比例1 | 10<sup>8～9</sup>Ω |
| 对比例2 | 10<sup>8～9</sup>Ω |
| 对比例3 | 10<sup>8～9</sup>Ω |
| 对比例4 | 10<sup>8～9</sup>Ω |
| 对比例5 | 10<sup>8～9</sup>Ω |
表1
由表1可知本发明申请制备的纳米银线复合抗静电聚酯薄膜表面电阻率最低可达105～6Ω，具有良好的抗静电性能。
本发明制备的抗静电聚酯薄膜通过碳纳米管、Fe3O4纳米线和石墨烯、纳米银线构筑形成复合抗静电材料，四种填料实现了在聚合物基体中填料的低接触电阻、高导电网络的有效搭建。突破性的采用二维和一维的金属纳米材料协同改性聚酯薄膜的抗静电性能，利用两者各自的优异性能的同时，也利用到它们一起产生的协同效应，因此使制备的复合材料具有优异的抗静电性能。通过检测，本发明申请制备的抗静电材料表面电阻率低至105 -6Ω，同时抗静电能力持久。
Claims (10)
1.一种纳米银线抗静电聚酯薄膜的制备方法，其特征在于，包括如下步骤：
步骤一：准备原料，原料的重量组分分别为聚对苯二甲酸丁二醇酯60～80份，聚对苯二甲酸乙二醇酯20～40份，相容剂5～10份，碳纳米管5～8份，Fe3O4纳米线5～10份，石墨烯3～5份，纳米银线1～5份，表面处理剂0.6～1份，抗氧剂0.5～1份；
步骤二：将上述原料混合均匀后加入到双螺杆共混造粒机内，由双螺杆共混造粒机将组分进行熔融混合成颗粒状，双螺杆共混造粒机的加热温度为280度，真空度为100Pa；
步骤三：将混料送入至干燥塔内进行烘干结晶，干燥塔预热温度为175℃，干燥至含水率≤200ppm；
步骤四：干燥后的混料通过熔融挤出设备中挤出成型后以72℃/min速度冷却，将冷却后的固体在110-115℃条件下进行纵向拉伸，在130-145℃条件下进行横向拉伸，在200-235℃进行热定型，得到抗静电聚酯薄膜。
2.根据权利要求1所述的一种纳米银线抗静电聚酯薄膜的制备方法，其特征在于，Fe3O4纳米线通过以下制备方法得到：
步骤一：称取硫代硫酸钠和硫酸亚铁加入PEG和水的混合溶液中，用NaOH调节pH为1l，然后倒入反应釜内衬中；
步骤二：密封反应釜，在180℃下保温8h，反应结束冷却至室温；
步骤三：将黑色沉淀物用去离子水洗涤，去除多余的离子杂质，用磁铁进行沉降收集，60℃真空干燥，得到Fe3O4纳米线。
3.根据权利要求1所述的一种纳米银线抗静电聚酯薄膜的制备方法，其特征在于，所述石墨烯的制备方式为将氧化石墨在600-1000℃，0.5-3min条件下还原剥离。
4.根据权利要求1所述的一种纳米银线抗静电聚酯薄膜的制备方法，其特征在于，所述纳米银线的制备步骤为：在10-400mL0.1-0.5mMFeCl3的乙二醇溶液中，加入0.15-0.75M的PVP，搅拌至PVP完全溶解后，再逐滴加入10-400mL0.1-0.5M的AgNO3溶液，搅拌10-20分钟，然后把混合液转移至水热合成反应釜内，在160℃下反应2-4小时，自然冷却，即得到纳米银线。
5.根据权利要求1所述的一种纳米银线抗静电聚酯薄膜的制备方法，其特征在于，所述相容剂由马来酸酐接枝丙烯腈-丁二烯-苯乙烯三元共聚物、马来酸酐接枝乙烯-辛烯共聚物、苯乙烯-丙烯腈-甲基丙烯酸缩水甘油酯三元无规共聚物中的一种或多种按任意配比混合组成。
6.根据权利要求1所述的一种纳米银线抗静电聚酯薄膜的制备方法，其特征在于，所述表面处理剂由硅烷偶联剂、甲基硅油、硅酮粉中的一种或多种按任意配比混合组成。
7.根据权利要求1所述的一种纳米银线抗静电聚酯薄膜的制备方法，其特征在于，所述抗氧剂由抗氧剂1010、抗氧剂168中的一种或两种按任意配比混合组成。
8.根据权利要求1所述的一种纳米银线抗静电聚酯薄膜的制备方法，其特征在于，所述碳纳米管直径10-15nm，长度1-10μm；Fe3O4纳米线直径20-50nm，长度10-50μm。
9.根据权利要求1所述的一种纳米银线抗静电聚酯薄膜的制备方法，其特征在于，所述石墨烯的厚度为0.35～20nm，直径为1～20μm。
10.根据权利要求1所述的一种纳米银线抗静电聚酯薄膜的制备方法，其特征在于，所述纳米银线的直径为40～500nm，长度为5～50μm。
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