CN106479047B - 一种低逾渗值高力学性能聚丙烯导电薄膜的制备方法 - Google Patents
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Abstract
本发明公开了一种低逾渗值高力学性能聚丙烯导电薄膜的制备方法,步骤如下:将PP粒料放入熔喷机中熔喷制备PP纤维网;将导电粒子分散于二甲苯溶剂中超声震荡制得溶液A;将PP纤维网置于溶液A中超声震荡2~5 min后取出,洗涤、自然晾干得到导电纤维;将导电纤维网上下两层铺于压机模板上,纤维网中间放置一些PP粒料,于真空压机中热压10~15 min,得到具有综合力学性能较高和较低逾渗值的PP导电薄膜。本发明利用熔喷工艺制备PP超细纤维网,比表面积大,通过超声分散的方法将导电填料均匀修饰在纤维网表面,热压后在膜内形成均匀的导电网络结构,不仅工艺简单,制得的导电薄膜同时具有较高的力学性能和较低逾渗值。
Description
技术领域
本发明属于高分子材料加工领域,具体涉及一种具有较好力学性能和较低逾渗值PP导电薄膜的简单制备方法。
背景技术
炭黑、碳纳米管、石墨烯等粒子是制备聚合物导电复合材料常用的填料。如何在改善导电性能的同时能提高力学性能,怎样尽可能采用较低的导电填料来制备性能更加优越的材料,已经吸引导电材料领域越来越多的兴趣。然而,导电复合材料的制备往往采用将导电填料与基体共混的方法,不仅操作繁琐,导电填料用量大,而且在共混时导电粒子很容易发生团聚,严重制约高性能导电复合材料的制备及应用。
发明内容
针对现有技术中存在的问题,本发明提供一种具有较高力学性能和较低逾渗值的聚丙烯(PP)导电薄膜的制备方法,该制备工艺简单,设备要求低,所制备的PP导电薄膜具有较高的力学性能和较低的逾渗值。
为解决上述技术问题,本发明采用以下技术方案:
一种低逾渗值高力学性能聚丙烯导电薄膜的制备方法,步骤如下:
(1)纤维网的制备:采用熔喷机将聚丙烯粒料熔喷制备出均匀的聚丙烯纤维网;
(2)导电粒子分散:将导电粒子分散于二甲苯溶剂中超声震荡10~15min制得不同浓度的溶液A;
(3)超声震荡:将步骤(1)制得的聚丙烯纤维网分别置于不同浓度的溶液A中超声震荡2~5 min;
(4)洗涤:将步骤(3)中超声震荡后的聚丙烯纤维网取出,用无水乙醇洗涤、自然晾干得到导电纤维网;
(5)热压:将晾干后的导电纤维网上下两层铺于模板上,上、下两层导电纤维网中间放置一定质量的聚丙烯(PP)粒料,置于真空压机中热压后得到综合力学性能较高和较低逾渗值的“三明治结构”的聚丙烯导电薄膜。
所述步骤(1)中的纤维网是将熔喷级聚丙烯粒料放于熔喷机中在175~200℃的条件下制备得到厚度为60µm的聚丙烯纤维网,纤维直径为3~7 µm。
所述步骤(2)中导电粒子为炭黑、碳纳米管或石墨烯。
所述步骤(2)中溶液A的浓度分别为1,0.5,0.25,0.1,0.05,0.025,0.01 mg/mL。
所述步骤(5)中聚丙烯粒料与导电纤维网的质量比为5:3。
所述步骤(5)中热压的条件为在175~200℃、1~2MPa的条件下热压10~15min。
本发明的有益效果:(1)该发明中通过熔喷工艺制备超细聚丙烯纤维网,比表面积大,纤维粗细均匀,通过超声分散的方法将导电填料均匀修饰在纤维表面,热压后可以在膜内形成一层均匀的导电网络结构,制得的PP导电薄膜具有更低的逾渗值。(2)本发明提供的PP导电薄膜的制备方法,主要采用超声波分散的方法将导电粒子均匀修饰在PP纤维网表面,与传统共混的方法相比,不仅工艺简单,设备要求低,而且避免碳纳米管在共混过程中的团聚现象。(3)采用本发明制备的PP导电薄膜同时力学性能也得到较大提高。主要原因有两方面:一方面,超声波分散的方法有利于导电粒子在纤维网表面的均匀修饰,有效避免了碳纳米管的团聚;另一方面,PP导电纤维网和PP基体通过热压的方法界面结合紧密,在PP导电膜内部形成一个网络结构,促进碳纳米管和聚合物基体的应力传递,从而使导电复合薄膜的力学性能得到提高。与现有技术相比,不仅工艺简单,而且可以获得一种同时具有较高力学性能和较低逾渗值的导电薄膜。
附图说明
图1为实施例1制备得到的PP导电薄膜的电性能测试曲线。
图2为实施例1制备得到的PP导电薄膜的力学性能测试曲线。
具体实施方式
下面结合具体实施例,进一步阐述本发明。
实施例1
本实施例的低逾渗值高力学性能聚丙烯(PP)导电薄膜的制备方法,步骤如下:
(1)将PP粒料放于熔喷机中于180℃的条件下制备得到厚度约为60 µm的PP纤维网,纤维直径为3~7 µm;
(2)称取一定质量的MWCNTs 分散于40 mL的二甲苯溶剂中超声震荡10 min,配置MWCNTs浓度分别为1,0.5,0.25,0.1,0.05,0.025,0.01 mg/mL的溶液;
(3)将步骤(1)制得的PP纤维网置于步骤(2)制得的碳纳米管的二甲苯溶液中超声波震荡2 min,取出PP纤维网,用无水乙醇洗涤、自然晾干,得到导电纤维网;
(4)将晾干后的导电纤维网上下铺两层于压机模板上,上、下两层纤维网中间放置一定质量的PP粒料(导电纤维网与PP的质量比为3:5),于真空压机中在185℃、2 MPa的条件下热压10 min,得到具有综合力学性能较高和较低逾渗值的PP导电薄膜。
本实施例制备得到的PP导电薄膜的电性能测试如图1所示,由图1可以看出,随MWCNTs的浓度增加,PP膜的电阻率显著降低,当MWCNTs的浓度仅为0.1 mg/mL时,PP导电膜的电阻率与纯PP膜相比降低了高达8个数量级。基于TG分析,导电膜的逾渗值仅为0.08%。与文献中报道的结果相比,本发明中PP导电膜的逾渗值显著降低。
本实施例制备得到的PP导电薄膜的力学性能测试曲线如图2所示。由图2可知,PP导电薄膜的拉伸强度与纯PP薄膜相比得到较大提高,其中,MWCNTs的浓度仅为0.1 mg/mL时,拉伸强度提高了76%。同时,PP导电薄膜的断裂伸长率也提高了56%。与文献中报道的导电薄膜的力学性能结果相比,本发明的优点在于断裂伸长率和拉伸强度都得到较大提高,导电膜的综合力学性能较好。
实施例2
本实施例的低逾渗值高力学性能聚丙烯(PP)导电薄膜的制备方法,步骤如下:
(1)将PP粒料放于熔喷机中于185℃的条件下制备得到厚度约为60 µm的PP纤维网,纤维直径为3~7 µm;
(2)称取一定质量的MWCNTs分散于40 mL的二甲苯溶剂中超声震荡10 min,配置MWCNTs浓度分别为1,0.5,0.25,0.1,0.05,0.025,0.01 mg/mL的溶液;
(3)将步骤(1)制得的PP纤维网置于步骤(2)制得的碳纳米管的二甲苯溶液中超声波震荡2 min,取出PP纤维网,用无水乙醇洗涤、自然晾干,得到导电纤维网;
(4)将晾干后的导电纤维网上下铺两层于压机模板上,上、下两层纤维网中间放置一定质量的PP粒料(导电纤维网与PP的质量比为3:5),于真空压机中在175℃、2 MPa的条件下热压12 min,得到具有综合力学性能较高和较低逾渗值的PP导电薄膜。
实施例3
本实施例的低逾渗值高力学性能聚丙烯(PP)导电薄膜的制备方法,步骤如下:
(1)将PP粒料放于熔喷机中于185℃的条件下制备得到厚度约为60 µm的PP纤维网,纤维直径为3~7 µm;
(2)称取一定质量的MWCNTs分散于40 mL的二甲苯溶剂中超声震荡10 min,配置MWCNTs浓度分别为1,0.5,0.25,0.1,0.05,0.025,0.01 mg/mL的溶液;
(3)将步骤(1)制得的PP纤维网置于步骤(2)制得的碳纳米管的二甲苯溶液中超声波震荡5min,取出PP纤维网,用无水乙醇洗涤、自然晾干,得到导电纤维网;
(4)将晾干后的导电纤维网上下铺两层于压机模板上,上、下两层纤维网中间放置一定质量的PP粒料(导电纤维网与PP的质量比为3:5),于真空压机中在175℃、2 MPa的条件下热压12 min,得到具有综合力学性能较高和较低逾渗值的PP导电薄膜。
实施例4
本实施例的低逾渗值高力学性能聚丙烯(PP)导电薄膜的制备方法,步骤如下:
(1)将PP粒料放于熔喷机中于190℃的条件下制备得到厚度约为60 µm的PP纤维网,纤维直径为3~7 µm;
(2)称取一定质量的石墨烯分散于40 mL的二甲苯溶剂中超声震荡10 min,配置石墨烯浓度分别为1,0.5,0.25,0.1,0.05,0.025,0.01 mg/mL的溶液;
(3)将步骤(1)制得的PP纤维网置于步骤(2)制得的碳纳米管的二甲苯溶液中超声波震荡5min,取出PP纤维网,用无水乙醇洗涤、自然晾干,得到导电纤维网;
(4)将晾干后的导电纤维网上下铺两层于压机模板上,上、下两层纤维网中间放置一定质量的PP粒料(导电纤维网与PP的质量比为3:5),于真空压机中在200℃、2 MPa的条件下热压10min,得到具有综合力学性能较高和较低逾渗值的PP导电薄膜。
实施例5
本实施例的低逾渗值高力学性能聚丙烯(PP)导电薄膜的制备方法,步骤如下:
(1)将PP粒料放于熔喷机中于195℃的条件下制备得到厚度约为60 µm的PP纤维网,纤维直径为3~7 µm;
(2)称取一定质量的石墨烯分散于40 mL的二甲苯溶剂中超声震荡15min,配置石墨烯浓度分别为1,0.5,0.25,0.1,0.05,0.025,0.01 mg/mL的溶液;
(3)将步骤(1)制得的PP纤维网置于步骤(2)制得的碳纳米管的二甲苯溶液中超声波震荡2 min,取出PP纤维网,用无水乙醇洗涤、自然晾干,得到导电纤维网;
(4)将晾干后的导电纤维网上下铺两层于压机模板上,上、下两层纤维网中间放置一定质量的PP粒料(导电纤维网与PP的质量比为3:5),于真空压机中在190℃、2 MPa的条件下热压10min,得到具有综合力学性能较高和较低逾渗值的PP导电薄膜。
实施例6
本实施例的低逾渗值高力学性能聚丙烯(PP)导电薄膜的制备方法,步骤如下:
(1)将PP粒料放于熔喷机中于195℃的条件下制备得到厚度约为60 µm的PP纤维网,纤维直径为3~7 µm;
(2)称取一定质量的炭黑分散于40 mL的二甲苯溶剂中超声震荡15min,配置炭黑浓度分别为1,0.5,0.25,0.1,0.05,0.025,0.01 mg/mL的溶液;
(3)将步骤(1)制得的PP纤维网置于步骤(2)制得的碳纳米管的二甲苯溶液中超声波震荡5 min,取出PP纤维网,用无水乙醇洗涤、自然晾干,得到导电纤维网;
(4)将晾干后的导电纤维网上下铺两层于压机模板上,上、下两层纤维网中间放置一定质量的PP粒料(导电纤维网与PP的质量比为3:5),于真空压机中在180℃、2 MPa的条件下热压10min,得到具有综合力学性能较高和较低逾渗值的PP导电薄膜。
实施例7
本实施例的低逾渗值高力学性能聚丙烯(PP)导电薄膜的制备方法,步骤如下:
(1)将PP粒料放于熔喷机中于200℃的条件下制备得到厚度约为60 µm的PP纤维网,纤维直径为3~7 µm;
(2)称取一定质量的炭黑分散于40 mL的二甲苯溶剂中超声震荡15min,配置炭黑浓度分别为1,0.5,0.25,0.1,0.05,0.025,0.01 mg/mL的溶液;
(3)将步骤(1)制得的PP纤维网置于步骤(2)制得的碳纳米管的二甲苯溶液中超声波震荡5min,取出PP纤维网,用无水乙醇洗涤、自然晾干,得到导电纤维网;
(4)将晾干后的导电纤维网上下铺两层于压机模板上,上、下两层纤维网中间放置一些PP粒料(导电纤维网与PP的质量比为3:5),于真空压机中在180℃、1MPa的条件下热压15min,得到具有综合力学性能较高和较低逾渗值的PP导电薄膜。
实施例8
本实施例的低逾渗值高力学性能聚丙烯(PP)导电薄膜的制备方法,步骤如下:
(1)将PP粒料放于熔喷机中于180℃的条件下制备得到厚度约为60 µm的PP纤维网,纤维直径为3~7 µm;
(2)称取一定质量的石墨烯分散于40 mL的二甲苯溶剂中超声震荡10 min,配置石墨烯浓度分别为1,0.5,0.25,0.1,0.05,0.025,0.01 mg/mL的溶液;
(3)将步骤(1)制得的PP纤维网置于步骤(2)制得的碳纳米管的二甲苯溶液中超声波震荡2 min,取出PP纤维网,用无水乙醇洗涤、自然晾干,得到导电纤维网;
(4)将晾干后的导电纤维网上下铺两层于压机模板上,上、下两层纤维网中间放置一定质量的PP粒料(导电纤维网与PP的质量比为3:5),于真空压机中在185℃、2 MPa的条件下热压10 min,得到具有综合力学性能较高和较低逾渗值的PP导电薄膜。
以上显示和描述了本发明的基本原理和主要特征以及本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (5)
1.一种低逾渗值高力学性能聚丙烯导电薄膜的制备方法,其特征在于步骤如下:
(1)纤维网的制备:采用熔喷机将聚丙烯粒料熔喷制备出均匀的聚丙烯纤维网;
(2)导电粒子分散:将导电粒子分散于二甲苯溶剂中超声震荡10~15min制得一定浓度的溶液A;
(3)超声震荡:将步骤(1)制得的聚丙烯纤维网置于一定浓度的溶液A中超声震荡2~5min;
(4)洗涤:将步骤(3)中超声震荡后的聚丙烯纤维网取出,用无水乙醇洗涤、自然晾干得到导电纤维网;
(5)热压:将晾干后的导电纤维网上下两层铺于模板上,上、下两层导电纤维网中间放置一定质量的聚丙烯粒料,置于真空压机中热压后得到聚丙烯导电薄膜;
所述步骤(2)中导电粒子为炭黑、碳纳米管或石墨烯。
2.根据权利要求1所述的低逾渗值高力学性能聚丙烯导电薄膜的制备方法,其特征在于:所述步骤(1)中的纤维网是将熔喷级聚丙烯粒料放于熔喷机中在175~200℃的条件下制备得到厚度为60µm的聚丙烯纤维网,纤维直径为3~7 µm。
3.根据权利要求1所述的低逾渗值高力学性能聚丙烯导电薄膜的制备方法,其特征在于:所述步骤(2)中溶液A的浓度为1,0.5,0.25,0.1,0.05,0.025或0.01 mg/mL。
4.根据权利要求1所述的低逾渗值高力学性能聚丙烯导电薄膜的制备方法,其特征在于:所述步骤(5)中聚丙烯粒料与导电纤维网的质量比为5:3。
5.根据权利要求1所述的低逾渗值高力学性能聚丙烯导电薄膜的制备方法,其特征在于:所述步骤(5)中热压的条件为在175~200℃、1~2MPa的条件下热压10~15min。
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