CN111057360A - 一种石墨烯导电橡胶纤维复合材料及其制备方法和应用 - Google Patents
一种石墨烯导电橡胶纤维复合材料及其制备方法和应用 Download PDFInfo
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- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
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Abstract
本发明提供一种石墨烯导电橡胶纤维复合材料及其制备方法和应用,该石墨烯导电橡胶纤维复合材料的原料包括石墨烯1~2份;偶联剂0.8~1.5份;活性天然酶0.8~1.5份;聚乙二醇0.8份~1.5份;酚醛树脂0.8~1.5份;导电炭黑20~30份;碳纳米管1~2份;导电石墨3~6份;加工助剂4~7.5份;纤维5~10份;聚醚醚酮0.8~1.5份。该石墨烯导电橡胶纤维复合材料可用于与普通橡塑胶材料一起制作防静电鞋底,可提高鞋底弹性和耐磨性能,同时兼具优异的防静电功能。
Description
技术领域
本发明属于鞋底材料技术领域,尤其涉及一种石墨烯导电橡胶纤维复合材料及其制备方法和应用。
背景技术
在制药厂、食品厂、电子厂车间、实验室等场所对静电控制严格,需要严防静电对设备和产品产生干扰。为减少或消除静电危害往往需要穿着防静电鞋,防静电鞋用防静电防滑材料作鞋底,将人体的静电引入大地。
防静电鞋底原料一般在橡胶中加入导电填料,如炭黑、石墨烯,例如公开号为CN107266900A的中国专利申请公开一种由有机锡稳定剂、防滑剂、导电填料、羟基化聚丙烯、弹性填料、碳酸钙、粘合剂、增强无机纤维、抗静电剂、偶联剂和加工助剂等原料制成的防静电鞋底材料,其导电填料由炭黑、纳米氧化锌和石墨烯混合而成。公开号为CN103289044A的中国专利申请也公开一种导电聚氨酯鞋底材料,由多元醇、扩链剂、催化剂、发泡剂、增塑剂、预聚体、石墨和硼酸铝晶须等原料制成。不过由于导电材料均为无机材料,与聚合物兼容性差,加入导电材料后往往会导致鞋底材料的机械性能降低,如撕裂强度、拉伸能力、弹力降低。
发明内容
本发明的目的在于解决现有导电鞋底材料无法兼顾导电性和韧性的问题,提供一种石墨烯导电橡胶纤维复合材料及其制备方法。
本发明的石墨烯导电橡胶纤维复合材料包括如下质量份的原料:
石墨烯 1~2份;
偶联剂 0.8~1.5份;
活性天然酶 0.8~1.5份;
聚乙二醇 0.8份~1.5份;
酚醛树脂 0.8~1.5份;
导电炭黑 20~30份;
碳纳米管 1~2份;
导电石墨 3~6份;
加工助剂 4~7.5份;
纤维 5~10份;
聚醚醚酮 0.8~1.5份。
进一步,所述纤维选自细度在0.55~1.4dtex(0.5~1.3旦)的细旦丝超细纤维。
进一步,所述偶联剂选自硅烷偶联剂。硅烷偶联剂分子中的硅烷氧基对无机物具有反应性,同时硅烷偶联剂中的有机官能团对有机物具有反应性,因此当硅烷偶联剂介于无机和有机界面之间,可形成有机基体-硅烷偶联剂-无机基体的结合层,可以参与到聚乙二醇、酚醛树脂、聚醚醚酮、纤维的固化网络中提升石墨烯与聚乙二醇、酚醛树脂、改性聚醚醚酮、纤维等高分子材料的界面结合作用。
优选地,所述硅烷偶联剂可采用A151(乙烯基三乙氧基硅烷)、A171(乙烯基三甲氧基硅烷)和A172(乙烯基三(β-甲氧乙氧基硅烷)中的一种或混合使用。
进一步,所述加工助剂包括稳定剂、乳化剂、分散剂、流平剂和表面活性剂。
进一步,所述稳定剂、乳化剂、分散剂、流平剂和表面活性剂用量均为0.8~1.5份。
进一步,所述稳定剂选自稀土稳定剂和/或有机锡稳定剂,可以减慢反应,保持化学平衡,降低表面张力,防止光、热分解或氧化分解。
进一步,所述乳化剂选自山梨酸醇脂肪酸酯类、磷脂类、糖脂类乳化剂等新型乳化剂的一种或二种配合。
进一步,所述分散剂选自石油磺酸盐类分散剂和/或脂肪酸类分散剂,用于减少完成分散过程所需要的时间和能量,稳定所分散的物料分散体,改性物料粒子表面性质,调整物料粒子的运动性。
进一步,所述流平剂选自以多元共聚物为基础的改性硅助剂(如ACR平滑流平剂)、非离子型表面活性剂和聚醚改性有机硅化合物中的任意一种,用于降低表面张力,控制表面流动的能力、增滑性、抗缩孔、抗粘连性。
进一步,所述表面活性剂为聚乙二醇(PEG)与二甘醇(DEG)的组合,且聚乙二醇(PEG)与二甘醇(DEG)的质量比为5:2。
本发明提供的上述石墨烯导电橡胶纤维复合材料的制备方法包括如下步骤:
(1)将石墨烯、偶联剂和活性天然酶混合均匀得到改性石墨烯浆料;
(2)取1/3~1/2步骤(1)的改性石墨烯浆料,向其中加入导电炭黑、碳纳米管、导电石墨、聚乙二醇和酚醛树脂,混合均匀后,得到石墨烯导电高分子浆料;
(3)在剩余的改性石墨烯浆料中加入纤维和聚醚醚酮,混合均匀得到橡塑/纤维聚合物;
(4)在90~135℃下,将步骤(2)制得的石墨烯导电高分子浆料和步骤(3)制得的橡塑/纤维聚合物混合均匀,得到石墨烯导电橡胶纤维复合材料。
其中,步骤(4)中将石墨烯导电高分子浆料与橡塑/纤维聚合物混合过程具体为:先在90~100℃下将石墨烯导电高分子浆料加入万马力混密炼机中,然后加入橡塑纤维聚合物,在螺杆转速35~30r/min下混合6~8min;混合均匀后,在135℃下料。
在实际操作中,步骤(1)中可将石墨烯、偶联剂和活性天然分散到溶剂中进行混合;步骤(2)可采用研磨分散进行混合均匀。
本发明利用上述石墨烯导电橡胶纤维复合材料制作一种防静电鞋底,该防静电鞋底的原料按重量份计包括如下组分:
橡塑胶材料60~70份;
石墨烯导电橡胶纤维复合材料30~40份;
硫化剂 1~1.5份;
促进剂 0.6~0.8份;
导电助剂 0.5~1份;
活性剂 0.5~1份。
其中橡塑胶材料由以下质量份的原料制备得到:橡胶和塑料100份、白炭黑40~50份、白矿油5~10份、硫磺1.5~2.5份、活性剂4~5份、促进剂1.8~2.5份、纳米氧化锌2~3份、硬脂酸1.0~1.5份、防老剂1.0~1.5份。其中橡胶可选择天然橡胶和/或合成橡胶,合成橡胶选自丁腈橡胶和/或顺丁橡胶,塑料选自PVC塑料。
进一步,所述硫化剂选自硫、硒、碲、含硫化合物、过氧化物、醌类化合物、胺类化合物、树脂类化合物、金属氧化物、异氰酸酯中的至少一种,优选硫和含硫化合物。
进一步,所述促进剂选自噻唑类促进剂、秋兰姆类促进剂、次磺酰胺类促进剂、胍类促进剂、二硫代氨基甲酸盐类促进剂、醛胺类促进剂、黄原酸盐类促进剂和硫脲中的至少两种的组合,优选其中任意两种或三种的组合。
进一步,所述活性剂选自PEG聚乙二醇和DEG二甘醇的组合。
相对于现有技术,本发明首先利用偶联剂对石墨烯进行改性,使石墨烯表面连接上含氧活性基团;然后将一部分改性石墨烯浆料与导电炭黑、碳纳米管、导电石墨等其他导电填料混合,并加入聚乙二醇和酚醛树脂两种高分子有机聚合物,改性石墨烯浆料中的偶联剂同时与聚乙二醇和酚醛树脂中的基团连接,从而将石墨烯与聚乙二醇、酚醛树脂结合在一起,形成均匀的石墨烯导电高分子浆料;同理,另一部分改性石墨烯浆料也通过相同的作用与纤维、聚醚醚酮形成均匀的橡塑/纤维聚合物;最后石墨烯导电高分子浆料与橡塑纤维聚合物混合后形成交叉网状结构,各物料交叉紧密连接,使得最终的石墨烯导电橡胶纤维复合材料内部无机物料与有机物料紧密、均匀交织在一起,提高材料的韧性,同时兼具防静电功能。在整个制备过程中,硅烷偶联剂都在发生作用,可降低合成熔体的粘度,改善各种原料的分散度以提高加工性能,进而使制品获得良好的表面质量及机械、热和电性能。
具体实施方式
发明人发现,石墨烯、导电炭黑、碳纳米管和导电炭黑等无机材料与高分子有机聚合物在特定的制备条件下可以均匀、紧密结合在一起,其中石墨烯具有优异的耐热性、机械性能、电性能、传输性能、气体屏障性能及热电性能,其水溶液经改性后可以与聚乙二醇、酚醛树脂、聚醚醚酮、纤维进行复合,从而大幅度地提升材料的拉伸强度,抗冲击性能以及导热导电性能,形成一种兼具高韧性和防静电功能的石墨烯导电橡胶纤维复合材料。以下结合具体实施例详细说明本发明的技术方案。
实施例1
本实施例提供一种石墨烯导电橡胶纤维复合材料,包括如下百分比的原料:
石墨烯 1~2份;
偶联剂 0.8~1.5份;
活性天然酶 0.8~1.5份;
聚乙二醇 0.8份~1.5份;
酚醛树脂 0.8~1.5份;
导电炭黑 20~30份;
碳纳米管 1~2份;
导电石墨 3~6份;
加工助剂 4~7.5份;
纤维 5~10份;
聚醚醚酮 0.8~1.5份;
其中纤维选自细度在0.55~1.4dtex(0.5~1.3旦)的细旦丝超细纤维。加工助剂包括用量均为0.8~1.5份的稳定剂、乳化剂、分散剂、流平剂和表面活性剂,所述稳定剂选自稀土稳定剂和/或有机锡稳定剂,乳化剂选自山梨酸醇脂肪酸酯类、磷脂类、糖脂类乳化剂等新型乳化剂的一种或二种配合,分散剂选自石油磺酸盐类分散剂和/或脂肪酸类分散剂,流平剂选自以多元共聚物为基础的改性硅助剂(如ACR平滑流平剂)、非离子型表面活性剂和聚醚改性有机硅化合物中的任意一种;表面活性剂为聚乙二醇(PEG)与二甘醇(DEG)的组合,且聚乙二醇(PEG)与二甘醇(DEG)的质量比为5:2。
在实际制备石墨烯导电橡胶纤维复合材料过程中,在上述原料基础上增加0.1~0.2份N,N-二甲基甲酰胺和/或环己酮等溶剂,或者添加0.8~1.5份分散树脂和/或树脂引发剂对物料进行乳化。具体配比参见表1。
表1.石墨烯导电橡胶纤维复合材料的原料及用量
本发明的石墨烯导电橡胶纤维复合材料的制备方法包括如下步骤:
(1)将石墨烯、偶联剂和活性天然酶混合均匀得到改性石墨烯浆料。
具体地,将石墨烯、硅烷偶联剂和活性天然酶分散到溶剂N,N-二甲基甲酰胺中,在超声或搅拌条件下再加入分散树脂或树脂引发剂或乳化剂或分散剂,对混合溶液进行乳化,使石墨烯与偶联剂、活性天然酶混合均匀,从而对石墨烯进行改性。搅拌约10min后,得到改性石墨烯浆料。
(2)取1/3~1/2(优选1/2)步骤(1)的改性石墨烯浆料,向其中加入导电炭黑、碳纳米管、导电石墨、聚乙二醇和酚醛树脂,混合均匀后得到石墨烯导电高分子浆料。
具体地,取1/2步骤(1)的改性石墨烯浆料,向其中加入聚乙二醇和酚醛树脂组成的混合液,然后再加入导电炭黑、碳纳米管和导电石墨,最后加入环己酮调整混合物的粘稠度,搅拌、碾磨均匀后再加入稳定剂、乳化剂、分散剂、流平剂和表面活性剂,混合均匀即得石墨烯导电高分子浆料。
(3)在剩余的改性石墨烯浆料中加入纤维和聚醚醚酮,混合均匀得到橡塑/纤维聚合物。
具体地,在磁力搅拌下,将经过有机溶剂浸泡以及有机酸处理的的纤维加入剩余的改性石墨烯浆料中,然后加入聚醚醚酮和偶联剂,超声分散均匀后冷却至室温(约4h),得到橡塑/纤维聚合物。
(4)在90~135℃下,将步骤(2)制得的石墨烯导电高分子浆料和步骤(3)制得的橡塑/纤维聚合物混合均匀后得到石墨烯导电橡胶纤维复合材料。
具体地,在90~100℃下将步骤(2)制得的石墨烯导电高分子浆料加入万马力混密炼机中,进行物理分散,直至石墨烯导电高分子浆料分散均匀,不出现分层或沉淀现象,然后加入步骤(3)制得的橡塑/纤维聚合物,在螺杆转速35~30r/min下混合6~8min;混合均匀后,在135℃下料,得到复合材料母料胶浆。
实施例2
本实施例利用实施例1制得的石墨烯导电橡胶纤维复合材料制备一种防静电鞋底,
该防静电鞋底按重量份计包括如下原料:
橡塑胶材料 60~70份;
石墨烯导电橡胶纤维复合材料 30~40份;
硫化剂 1~1.5份;
促进剂 0.6~0.8份;
导电助剂 0.5~1份;
活性剂 0.5~1份。
其中橡塑胶材料由以下质量份的原料制备得到:橡胶和塑料100份、白炭黑40~50份、白矿油5~10份、硫磺1.5~2.5份、活性剂4~5份、促进剂1.8~2.5份、纳米氧化锌2~3份、硬脂酸1.0~1.5份、防老剂1.0~1.5份。其中橡胶可选择天然橡胶和/或合成橡胶,合成橡胶选自丁腈橡胶和/或顺丁橡胶,塑料选自PVC塑料。
硫化剂选自硫、硒、碲、含硫化合物、过氧化物、醌类化合物、胺类化合物、树脂类化合物、金属氧化物、异氰酸酯中的至少一种,优选硫和含硫化合物。促进剂选自噻唑类促进剂、秋兰姆类促进剂、次磺酰胺类促进剂、胍类促进剂、二硫代氨基甲酸盐类促进剂、醛胺类促进剂、黄原酸盐类促进剂和硫脲中的至少一种。活性剂选自PEG聚乙二醇和DEG二甘醇的组合。
具体配比见表2。
作为对比,同时制备一种原料仅包括普通橡塑胶材料和硫化剂、促进剂、导电助剂和活性剂,不添加石墨烯导电橡胶纤维复合材料的鞋底,具体原料和用量见表2对比例。
表2.防静电鞋底原料和用量
注:实施例2-1、2-2和2-3的石墨烯导电橡胶纤维复合材料分别选自实施例1-4、1-5和1-6。
该防静电鞋底的制备方法为:
按表2的用量配比将所有原料输入密闭式炼胶机中,在130℃下混炼5min成团后送入开放式炼胶机中拉片束薄2次后下料冷却放置24h得到混炼坯料;
将混炼坯料在开放式炼胶机上进行翻炼并拉薄下片(5~6mm厚),取样进行硫变测试。硫变测试通过后,进行裁条、裁片、成型;然后在平板硫化机上进行硫化,同时热压、冷却、定型、修边加工制作,即得一种一体成型的防静电鞋底。
对上述防静电鞋底进行性能测试,结果如表3所示。
表3.鞋底性能
根据表3可知,利用本发明的石墨烯导电橡胶纤维复合材料制备的鞋底具有良好的弹性和耐磨性能,同时具有较好的导电能力,可有效起到传导电荷、防静电作用;而未添加石墨烯导电橡胶纤维复合材料的鞋底的导电性能差,无法达到标准(GB4385-1995)的要求。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (10)
1.一种石墨烯导电橡胶纤维复合材料,其特征在于:包括如下质量份的原料:
石墨烯1~2份;
偶联剂0.8~1.5份;
活性天然酶0.8~1.5份;
聚乙二醇0.8份~1.5份;
酚醛树脂0.8~1.5份;
导电炭黑20~30份;
碳纳米管1~2份;
导电石墨3~6份;
加工助剂4~7.5份;
纤维5~10份;
聚醚醚酮0.8~1.5份。
2.根据权利要求1所述石墨烯导电橡胶纤维复合材料,其特征在于:所述纤维细度为0.55~1.4dtex。
3.根据权利要求1所述石墨烯导电橡胶纤维复合材料,其特征在于:所述偶联剂选自硅烷偶联剂。
4.根据权利要求1所述石墨烯导电橡胶纤维复合材料,其特征在于:所述加工助剂包括稳定剂、乳化剂、分散剂、流平剂和表面活性剂。
5.根据权利要求4所述石墨烯导电橡胶纤维复合材料,其特征在于:所述稳定剂、乳化剂、分散剂、流平剂和表面活性剂用量均为0.8~1.5份。
6.一种如权利要求1~5任一项所述石墨烯导电橡胶纤维复合材料的制备方法,其特征在于:包括如下步骤:
(1)将石墨烯、偶联剂和活性天然酶混合均匀得到改性石墨烯浆料;
(2)取1/3~1/2步骤(1)的改性石墨烯浆料,向其中加入导电炭黑、碳纳米管、导电石墨、聚乙二醇和酚醛树脂,混合均匀后得到石墨烯导电高分子浆料;
(3)在剩余的改性石墨烯浆料中加入纤维和聚醚醚酮,混合均匀得到橡塑/纤维聚合物;
(4)在90~135℃下,将步骤(2)制得的石墨烯导电高分子浆料和步骤(3)制得的橡塑/纤维聚合物混合均匀后得到石墨烯导电橡胶纤维复合材料。
7.一种防静电鞋底,其特征在于:包括如下质量份的原料:
橡塑胶材料60~70份;
权利要求1~5任一项所述石墨烯导电橡胶纤维复合材料30~40份;
硫化剂1~1.5份;
促进剂0.6~0.8份;
导电助剂0.5~1份;
活性剂0.5~1份。
8.根据权利要求7所述防静电鞋底,其特征在于:所述硫化剂选自硫、硒、碲、含硫化合物、过氧化物、醌类化合物、胺类化合物、树脂类化合物、金属氧化物和异氰酸酯中的至少两种。
9.根据权利要求8所述防静电鞋底,其特征在于:所述促进剂选自噻唑类促进剂、秋兰姆类促进剂、次磺酰胺类促进剂、胍类促进剂、二硫代氨基甲酸盐类促进剂、醛胺类促进剂、黄原酸盐类促进剂和硫脲中的至少两种的组合。
10.根据权利要求9所述防静电鞋底,其特征在于:所述活性剂选自聚乙二醇和二甘醇的组合。
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