CN111549385A - 一种导电纤维制备装置 - Google Patents
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Abstract
本发明属于纳米纤维技术领域,具体涉及一种导电纤维制备装置,主体结构包括供料机构、储液仓、喷头、接收机构、电源和接地导线,通过一次法利用静电纺丝技术实现碳纳米管/天然橡胶导电纤维和石墨烯/天然橡胶导电纤维的制备,制备的导电纤维在水浴溶剂的作用下纤维交联,经过导电性测试表明,添加了碳纳米管的导电纤维的导电性提高了5个数量级,添加了石墨烯的导电纤维的导电性提高了8个数量级;其结构简单,制备的导电纤维比表面积大、纤维尺寸均匀、更易实现表面功能化、克服了橡胶纤维的粘连问题,大幅度提高了物理机械性能,在天然橡胶产业化生产和增强增韧材料等方面具有更加广泛的应用。
Description
技术领域:
本发明属于纳米纤维技术领域,具体涉及一种导电纤维制备装置,能够通过一次法制备碳纳米管/天然橡胶导电纤维和石墨烯/天然橡胶导电纤维。
背景技术:
导电纤维是指在聚合物中混入导电介质所纺制成的化学纤维或金属纤维、碳纤维等,具有远高于抗静电纤维的优异的消除和防止静电的性能,且比电阻值持久不变并基本上不受湿度影响。按导电成分分布状态,分为均匀型、被覆型和复合型三类。一般采用混溶、蒸镀、电镀和复合纺丝等方法,在纤维中添加炭黑、石墨、金属粉或金属化合物等导电介质制得。其制晶可用予静电感应屏蔽,混有少量导电纤维的织物还可用作特种工作服、防尘刷等。
橡胶之所以被称为战略物资,是因为橡胶是国民生产中非常重要的物资。橡胶因其具有很强的弹性和良好的绝缘性,可塑性,隔水隔气,抗拉和耐磨等特点,广泛地运用于工业,农业,国防,交通,运输,机械制造,医药卫生领域和日常生活等方面。随着科学技术的不断发展对于橡胶制品也提出了越来越高的要求,高性能橡胶制品已成为橡胶工业的发展趋势。为适应这种发展趋势,需要不断开发橡胶制品的应用潜力。
碳系填料中的碳纳米管为碳的一种同素异形体,管间缝隙与石墨碳原子层的间隙相近,组成碳纳米管的碳原子的杂化类型主要是sp2,通过碳碳键与周围碳原子结合,形成圆柱形。碳纳米管特殊的结构使其具有其它材料不具备的优异性能,高强度、高韧性、高导电、高导热等性能,成为应用潜力广泛的纳米材料之一,可有效提高基体的综合性能,作为具有优越电学、力学性能的一维纳米材料,碳纳米管引起了世界范围的广泛关注。
碳系填料中二维结构的石墨烯被认为是能够有效改善复合材料导电性能的纳米级填料。石墨烯与其他材料结合形成复合材料或杂化结构后,可以改变宿主材料的电性能和力学性能。研究发现石墨烯在常温下电子迁移率高达15000cm2·V-1·S-1,是目前已知的在常温下导电性能最好的材料。石墨烯中每个碳原子都通过键与周边三个碳原子相互连接,键与键之间的夹角为120°,除键与其他碳原子链接成六角环的蜂窝式层状结构外,每个碳原子都垂直于层面的轨道形成贯穿全层的多原子的大π键,具有优良的导电性能。
静电纺丝技术是目前制备纳米纤维最为简单有效的技术工艺,目前已成功制备出聚乙烯醇(PVA)、聚丙烯腈(PAN)、聚乳酸(PLA)等聚合物基体。静电纺丝的原理是在高压静电场的作用下聚合物溶液克服表面张力形成喷射细流,经过在空中的不稳定流动溶剂得以挥发,最终在接收装置上得到聚合物纤维。目前通过静电纺丝制造的纳米纤维已广泛应用于空气过滤、水处理、异相催化、环境保护、智能织物、表面涂层、能量的收集转化和存储、封装生物活性材料、药物缓释、组织工程、再生医学等。
中国专利201910417828.X公开的一种制备金属/聚合物复合导电纤维的装置,包括储液池、高频信号发生器、电源、收集板,其中:所述储液池用于盛放含金属纳米线的静电纺丝前驱液,储液池一端连接有喷射部件,储液池中设置有推进部件,用于将储液池中的静电纺丝前驱液推进至喷射部件,并通过喷射部件喷出;所述高频信号发生器的输出端通过导线连接有第一金属极板,第一金属极板放置于储液池内部,高频信号发生器的输入端通过导线连接有第二金属极板,第二金属极板固定在储液池外部与喷射部件的连接处;第一金属极板与第二金属极板平行;所述电源的一端通过导线与喷射部件连接,另一端接地;所述收集板对向置于喷射部件前方,收集板接地;中国专利201520083823.5公开的一种凹凸棒石杂化导电纤维的制备装置,包括母粒制备装置:纳米粉体进行反应的杂化反应器、单螺杆挤出机、真空干燥器、双螺杆挤出机、在线注射器、吹风机、切粒机;所述的纳米杂化反应器与单螺杆挤出机相通;所述的单螺杆挤出机通过真空干燥器与双螺杆挤出机相通;所述的注射器与双螺杆挤出机相通;所述的双螺杆挤出机通过管路与吹风机相通;所述的吹风机通过管路与切粒机相通;以及现有技术中均无基于静电纺丝技术通过一次法制备碳纳米管/天然橡胶导电纤维和石墨烯/天然橡胶导电纤维的记载。
发明内容:
本发明的目的在于克服现有技术存在的缺点,寻求设计一种导电纤维制备装置,通过简捷快速有效的导电纤维制备方法,制备机械性能优良的导线纤维,实现导电纤维的产业化生产。
为了实现上述目的,本发明涉及的导电纤维制备装置的主体结构包括供料机构、储液仓、喷头、接收机构、电源和接地导线;供料机构与储液仓连接,储液仓的底端与喷头连接,喷头的下方设置有接收机构,电源分别与喷头和接收机构连接后与接地导线连接。
本发明涉及的供料机构1能够按照设定的速度将纺丝溶液输送进储液仓;储液仓的容量大于等于5mL;喷头为纺丝喷头,包括单针喷头,喷头的直径为0.5-2.5mm;接收机构包括旋转滚筒、旋转框架、旋转圆盘和金属铝箔,制备单向有序排列的纤维时,选用旋转滚筒、旋转框架或旋转圆盘,制备无序排列的纤维时,选用金属铝箔;电源为高压直流电源;喷头与接收机构之间的垂直距离为10-25cm。
本发明涉及的导电纤维制备装置能够通过一次法制备碳纳米管/天然橡胶导电纤维和石墨烯/天然橡胶导电纤维,具体工艺过程包括配制纺丝溶液、静电纺丝和硫化共三个步骤:
(一)配制纺丝溶液:将天然橡胶破碎后溶于有机溶剂中配制重量百分比为0.5-4wt%的橡胶溶液,在温度为50℃的水浴条件下使用高速搅拌机对橡胶溶液进行溶解,并达到均一状态,向橡胶溶液中加入硫化剂、硫化助剂和碳纳米管或石墨烯,形成纺丝溶液,将纺丝溶液置于超声细胞粉碎仪超声20min,备用;
(二)静电纺丝:设定给料机构以0.03-0.2ml/min的速度将纺丝溶液输送进储液仓,待纺丝溶液从喷头稳定流出后,打开电源,施加静电,在温度为23-27℃,湿度为50-65%的条件下开始静电纺丝,喷头与接收机构之间形成聚合物射流,落到接收机构上,干燥后形成天然橡胶纳米纤维;
(三)硫化:将天然橡胶纳米纤维静置于水浴溶剂中,5-10min后取出,在温度为90-175℃的条件下硫化7-60min,冷却至室温,得到导电纤维。
本发明步骤(一)涉及的有机溶剂为环己烷、苯、甲苯、二甲苯、N,N-二甲基甲酰胺、四氢呋喃中的一种或几种的混合物;天然橡胶、硫化剂、硫化助剂和碳纳米管或石墨烯的质量份数分别为100、0.05-30、0.05-30和0.01-5;硫化剂为纳米级硫磺、金属氧化物、有机过氧化物、树脂类和胺类中的一种或几种的混合物,优先选择纳米级硫磺和有机过氧化物中的一种或两种的混合物;硫化助剂为促进剂、活性剂、防老剂、补强剂和填充剂中的一种或几种的混合物,硫化助剂中促进剂、活性剂、防老剂、补强剂和填充剂的质量份数分别为0.01-5、0-5、0-5、0-5和0-5;步骤(二)涉及的静电的电压为10-30kv;步骤(三)涉及的水浴溶剂为液体石蜡或乙醇硬脂酸锌溶液。
本发明涉及的导电纤维的形貌通过调节包括纺丝溶液的浓度、有机溶剂挥发性、静电电压、纺丝溶液的输送速度、喷头与接收机构之间的垂直距离、喷头的直径、环境温度和湿度的静电纺丝参数调节。
本发明与现有技术相比,通过一次法利用静电纺丝技术实现碳纳米管/天然橡胶导电纤维和石墨烯/天然橡胶导电纤维的制备,具体过程是在纺丝溶液中加入硫化体系等进行静电纺丝,然后在纺丝过程中添加设定的温度场,提高溶剂挥发速率,采用水浴接收,保持水浴溶剂温度为60-70℃,水浴溶剂能够有效避免橡胶纤维的流动粘连,很好的保持纤维的形貌,制备的导电纤维在水浴溶剂的作用下纤维交联,经过导电性测试表明,添加了碳纳米管的导电纤维的导电性提高了5个数量级,添加了石墨烯的导电纤维的导电性提高了8个数量级;其结构简单,制备的导电纤维比表面积大、纤维尺寸均匀、更易实现表面功能化、克服了橡胶纤维的粘连问题,大幅度提高了物理机械性能,在天然橡胶产业化生产和增强增韧材料等方面具有更加广泛的应用。
附图说明:
图1为本发明的主体结构原理示意图。
图2为本发明实施例2涉及的天然橡胶纳米纤维的三维形貌照片。
图3为本发明实施例3涉及的天然橡胶纳米纤维的三维形貌照片。
具体实施方式:
下面通过实施实例并结合附图对本发明做进一步描述。
实施例1:
本实施例涉及的导电纤维制备装置的主体结构如图1所示,包括供料机构1、储液仓2、喷头3、接收机构4、电源5和接地导线6;供料机构1与储液仓2连接,储液仓2的底端与喷头3连接,喷头3的下方设置有接收机构4,电源5分别与喷头3和接收机构4连接后与接地导线6连接;喷头3为单针喷头;接收机构4为金属铝箔;喷头3与接收机构4之间的垂直距离为15cm。
实施例2:
本实施例涉及的导电纤维制备装置的主体结构与实施例1相同,其制备碳纳米管/天然橡胶导电纤维的具体工艺过程包括配制纺丝溶液、静电纺丝和硫化共三个步骤:
(一)配制纺丝溶液:将天然橡胶破碎后溶于有机溶剂中配制300ml重量百分比为3wt%的橡胶溶液,其中有机溶剂是质量比为10:1的环己烷和N,N-二甲基甲酰胺的混合溶剂,在温度为50℃的水浴条件下使用高速搅拌机对橡胶溶液进行溶解,并达到均一状态,向橡胶溶液中加入硫化剂、硫化助剂和碳纳米管,其中,天然橡胶100重量份,硫磺1.5份,氧化锌5重量份,硬脂酸2重量份,促进剂CZ1.5重量份,碳纳米管1重量份,形成纺丝溶液,将纺丝溶液置于超声细胞粉碎仪超声20min,备用;
(二)静电纺丝:设定给料机构1以0.05ml/min的速度将纺丝溶液输送进储液仓2,待纺丝溶液从喷头3稳定流出后,打开电源5,施加电压为17kV的静电,在温度为23-27℃,湿度为50-65%的条件下开始静电纺丝,喷头3与接收机构4之间形成聚合物射流10,落到接收机构4上,干燥后形成无序排列结构的天然橡胶纳米纤维;
(三)硫化:将天然橡胶纳米纤维静置于水浴溶剂中5-10min后取出,在温度为90-175℃的条件下硫化7-60min,冷却至室温,得到导电纤维。
本实施例步骤(二)制备的天然橡胶纳米纤维的三维形貌照片如图2所示。
实施例3:
本实施例涉及的导电纤维制备装置的主体结构与实施例1相同,其制备石墨烯/天然橡胶导电纤维的具体工艺过程包括配制纺丝溶液、静电纺丝和硫化共三个步骤:
(一)配制纺丝溶液:将天然橡胶破碎后溶于有机溶剂中配制300ml重量百分比为3wt%的橡胶溶液,其中有机溶剂是质量比为10:1的环己烷和N,N-二甲基甲酰胺的混合溶剂,在温度为50℃的水浴条件下使用高速搅拌机对橡胶溶液进行溶解,并达到均一状态,向橡胶溶液中加入硫化剂、硫化助剂和石墨烯,其中,天然橡胶100重量份,硫磺1.5份,氧化锌5重量份,硬脂酸2重量份,促进剂CZ1.5重量份,石墨烯1重量份,形成纺丝溶液,将纺丝溶液置于超声细胞粉碎仪超声20min,备用;
(二)静电纺丝:设定给料机构1以0.03ml/min的速度将纺丝溶液输送进储液仓2,待纺丝溶液从喷头3稳定流出后,打开电源5,施加电压为17kV的静电,在温度为23-27℃,湿度为50-65%的条件下开始静电纺丝,喷头3与接收机构4之间形成聚合物射流10,落到接收机构4上,干燥后形成无序排列结构的天然橡胶纳米纤维;
(三)硫化:将天然橡胶纳米纤维静置于水浴溶剂中5-10min后取出,在温度为90-175℃的条件下硫化7-60min,冷却至室温,得到导电纤维。
本实施例步骤(二)制备的天然橡胶纳米纤维的三维形貌照片如图3所示。
Claims (8)
1.一种导电纤维制备装置,其特征在于主体结构包括供料机构、储液仓、喷头、接收机构、电源和接地导线;供料机构与储液仓连接,储液仓的底端与喷头连接,喷头的下方设置有接收机构,电源分别与喷头和接收机构连接后与接地导线连接。
2.根据权利要求1所述的导电纤维制备装置,其特征在于供料机构能够按照设定的速度将纺丝溶液输送进储液仓;储液仓的容量大于等于5mL;喷头为纺丝喷头,包括单针喷头,喷头的直径为0.5-2.5mm;接收机构包括旋转滚筒、旋转框架、旋转圆盘和金属铝箔,制备单向有序排列的纤维时,选用旋转滚筒、旋转框架或旋转圆盘,制备无序排列的纤维时,选用金属铝箔;电源为高压直流电源。
3.根据权利要求1或2所述的导电纤维制备装置,其特征在于喷头3与接收机构4之间的垂直距离为10-25cm。
4.根据权利要求3所述的导电纤维制备装置,其特征在于能够通过一次法制备碳纳米管/天然橡胶导电纤维和石墨烯/天然橡胶导电纤维,具体工艺过程包括配制纺丝溶液、静电纺丝和硫化共三个步骤:
(一)配制纺丝溶液:将天然橡胶破碎后溶于有机溶剂中配制重量百分比为0.5-4wt%的橡胶溶液,在温度为50℃的水浴条件下使用高速搅拌机对橡胶溶液进行溶解,并达到均一状态,向橡胶溶液中加入硫化剂、硫化助剂和碳纳米管或石墨烯,形成纺丝溶液,将纺丝溶液置于超声细胞粉碎仪超声20min,备用;
(二)静电纺丝:设定给料机构以0.03-0.2ml/min的速度将纺丝溶液输送进储液仓,待纺丝溶液从喷头稳定流出后,打开电源,施加静电,在温度为23-27℃,湿度为50-65%的条件下开始静电纺丝,喷头与接收机构之间形成聚合物射流,落到接收机构上,干燥后形成天然橡胶纳米纤维;
(三)硫化:将天然橡胶纳米纤维静置于水浴溶剂中,5-10min后取出,在温度为90-175℃的条件下硫化7-60min,冷却至室温,得到导电纤维。
5.根据权利要求4所述的导电纤维制备装置,其特征在于步骤(一)涉及的有机溶剂为环己烷、苯、甲苯、二甲苯、N,N-二甲基甲酰胺、四氢呋喃中的一种或几种的混合物;天然橡胶、硫化剂、硫化助剂和碳纳米管或石墨烯的质量份数分别为100、0.05-30、0.05-30和0.01-5;硫化剂为纳米级硫磺、金属氧化物、有机过氧化物、树脂类和胺类中的一种或几种的混合物,优先选择纳米级硫磺和有机过氧化物中的一种或两种的混合物;硫化助剂为促进剂、活性剂、防老剂、补强剂和填充剂中的一种或几种的混合物,硫化助剂中促进剂、活性剂、防老剂、补强剂和填充剂的质量份数分别为0.01-5、0-5、0-5、0-5和0-5。
6.根据权利要求4所述的导电纤维制备装置,其特征在于步骤(二)涉及的静电的电压为10-30kv。
7.根据权利要求4所述的导电纤维制备装置,其特征在于步骤(三)涉及的水浴溶剂为液体石蜡或乙醇硬脂酸锌溶液。
8.根据权利要求4-7中任一项所述的导电纤维制备装置,其特征在于制备的导电纤维的形貌通过调节包括纺丝溶液的浓度、有机溶剂挥发性、静电电压、纺丝溶液的输送速度、喷头与接收机构之间的垂直距离、喷头的直径、环境温度和湿度的静电纺丝参数调节。
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