CN106189578A - 一种高分散型油系碳纳米管导电浆料 - Google Patents
一种高分散型油系碳纳米管导电浆料 Download PDFInfo
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Abstract
本发明公开了一种高分散型油系碳纳米管导电浆料，包括以下重量份的组分：有机树脂10～60质量份、活性碳纳米管5～40质量份、有机溶剂B 20～70质量份；所述活性碳纳米管是将碳纳米管进行高速搅拌，同时将油性分散剂溶于液体中通过喷雾的方式将其喷入搅拌中的碳纳米管粉体中，使得碳纳米管表面活化，得到的活性碳纳米管。本发明提供的高分散型油系碳纳米管导电浆料导电性能良好，抗静电性能良好，分散性佳，可长期保存。
Description
一、技术领域
本发明涉及一种高分散型油系碳纳米管导电浆料。
二、背景技术
导电涂料是涂于高电阻率的高分子材料上,使之具有传导电流和排除积累静电荷能力的特种涂料,可涂覆于任何形状基材的表面或内部。导电涂料按组成及导电机理可分为两大类:结构型(亦称本征型)导电涂料与复合型(亦称添加型)导电涂料。本征型导电涂料的导电材料是高聚物自身。添加型导电涂料的导电材料是在绝缘高聚物中添加的导电物质(金属、石墨等),利用导电物质的导电作用,使高聚物具有导电性能。
目前实际应用得较多的是复合型导电涂料,它是利用导电填料来实现导电的,其导电机理比较复杂,目前比较一致的看法主要是导电填料相互接触形成连续网链,载流子可在网链上运动,从而使涂层导电。导电涂料的主要用途是抗静电(ESD)、电磁波屏蔽(EMI)和作为电加热体,其中抗静电涂料是目前所有导电涂料中应用最为广泛的一类。导电填料是添加型导电涂料的重要组成部分,也是导电涂料所需研究的重点,能用作导电涂料的导电材料通常为金属系填料,金属微粒的形状、用量、稳定性、表面效应等均会影响涂层的导电性能.一般来讲,选择薄片状或树枝状金属填充的涂料比球状金属填充的涂料导电性能好.导电填料的用量达到临界浓度时才会形成空间导电网络,涂层的导电性能才会显著提高.对一些易氧化的金属(如Cu)必须在涂料中添加相应的抗氧化剂。另外为了使导电填料和基体树脂应具有一定的亲和性和润湿性,还需加入一定的分散剂和偶联剂等。但填料的分散性也不能太好,否则使粒子间的连接与基料聚合物先析出同时进行,形成均一构造的涂膜,电导率下降。另外，常用的导电填料还包括包括碳系填料、金属氧化物系填料和复合系填料。
碳纳米管自1991年被发现以来,短短十几年之间,这种纳米尺寸的炭质管状物就引起了全球性物理、化学和材料等科学界的广泛兴趣。由于碳纳米管的特殊结构和优异的力学、电学和光学性能以及其潜在的工业价值,使其逐渐成为化学、物理和材料等学科领域的研究热点。由于碳纳米管具有很好的导电性,同时又拥有较大的长径比,因而很适合做导电填料,相对于其它金属颗粒和石墨颗粒,用很少的量就能形成导电网链,且其密度比金属颗粒小得多,不易因重力的作用而聚沉。
然而，由于碳纳米管是一种高度极化、表面光滑的无机高分子化合物，表面缺陷少、缺乏活性基团，同时碳纳米管之间存在较强的范德华力和它巨大的比表面积、非常高的长径比，导致在一般情况下，碳纳米管易缠绕团聚成束。要发挥碳纳米管游戏性能使其广泛应用，如何解决碳纳米管的分散是关键性问题。目前，分散碳纳米管的方法有研磨与搅拌、高能球磨、超声波处理、强酸强碱洗涤、添加表面活性剂、原位生长合成、多种方法综合处理等。
三、发明内容
本发明提供了一种高分散型油系碳纳米管导电浆料，将碳纳米管经预处理改性后，作为导电填料加入有机溶剂中，从而制备出高分散型油系碳纳米管导电浆料。
本发明采用的技术方案是：
一种高分散型油系碳纳米管导电浆料，所述高分散型油系碳纳米管导电浆料包括以下重量份的组分：
有机树脂10～60质量份、活性碳纳米管5～40质量份、有机溶剂B 20～70质量份；
所述活性碳纳米管按以下方法制得：
将油性分散剂溶于有机溶剂A中，得到分散剂溶液，然后将分散剂溶液通过高压喷淋法喷入高速搅拌的碳纳米管中，高速搅拌混合后，制得活性碳纳米管。
所述碳纳米管、油性分散剂、有机溶剂A的质量份数比为85～95：0.1～5：5～10。
所述高分散型油系碳纳米管导电浆料还可以包括助剂，所述助剂为抗沉降剂和消泡剂，所述有机树脂、活性碳纳米管、有机溶剂B、抗沉降剂、消泡剂的质量份数为10～60质量份、5～40质量份、20～70质量份、0.01～10质量份、0.01～10质量份，优选为20～40质量份、10～40质量份、30～60质量份、0.1～5质量份、0.1～5质量份。
所述油性分散剂为聚乙烯吡咯烷酮、聚乙烯醇、聚乙二醇辛基苯基醚、烷基酚环氧乙烷缩合物乳化剂、聚偏氟乙烯中的一种或两种以上的混合物。
所述有机溶剂A或有机溶剂B各自独立为N,N-二甲基甲酰胺、N-甲基吡咯烷酮、二甲基甲酰胺、二甲基亚砜、氯仿、石油醚、乙酸乙酯、乙酸丁酯、丙酮、环己酮中的一种或两种以上的混合物。
所述碳纳米管为多壁碳纳米管、单壁碳纳米管中的一种或两种的混合物，优选多壁碳纳米管。
所述方法中，有机溶剂A和有机溶剂B用于区分不同步骤中所使用的有机溶剂，A、B不具有化学意义。
所述有机树脂选自环氧树脂、聚氨酯树脂、聚酯树脂、丙烯酸树脂、硅氧烷树脂或聚醚多元醇树脂中的一种或两种以上的混合物，优选为环氧树脂、丙烯酸树脂、聚酯树脂中的任意一种或者两种以上的的混合物。所述有机树脂可以商购得到。
所述的抗沉降剂为有机改性的硼润土、聚酰胺防沉蜡浆、气相二氧化硅中的一种或两种以上的混合，可以购自德谦化学、德固萨公司和ROCKWOOD公司等。
所述消泡剂具有较低表面张力和较高表面活性，能抑制或消除在超声或砂磨的加工过程中液体中产生的泡沫，所述消泡剂优选为矿物油、聚硅氧烷聚醚共聚物、聚醚化合物、改性有机硅混合物中的一种或两种以上的混合。如BYK公司生产的BYK-065消泡剂、BYK-066N消泡剂、TEGO公司生产的TEGO-940消泡剂，EFKA公司生产的EFKA-2022消泡剂等。
在制备活性碳纳米管时，所用的高压喷淋法是将分散剂溶液通过高压喷淋装置以喷雾的形式喷入高速搅拌的碳纳米管，所述高压喷淋装置可采用高压喷淋机，通过高压水泵将分散剂溶液经高压喷头成喷雾状喷入物料中。所述高压喷淋机用于碳纳米管预处理尚属首次。高压喷淋法将分散剂溶液雾化，雾化后得到大量微小液滴，大大增大了溶液与碳纳米管的接触面积，有利于碳纳米管颗粒被助剂包覆，增强其分散性。
所述高压喷淋法中，喷雾速率一般为10～100ml/min；
雾化细度为0.1～1um。
所述高速搅拌的转速一般为300～1500转/min。
所述高速搅拌混合的时间一般为1分钟～1小时，优选5～40分钟。
本发明提供的高分散型油系碳纳米管导电浆料可通过将活性碳纳米管与有机树脂、有机溶剂B、抗沉降剂、消泡剂按组方量混合，经超声或砂磨工艺混合均匀制得。
本发明对碳纳米管进行高速搅拌，对其表面表面预处理，同时将分散剂溶于液体中通过喷雾的方式将其喷入搅拌中的碳纳米管粉体中，使得碳纳米管表面活化，同时被分散剂均匀润湿，造成碳纳米管之间形成排斥，提高了碳纳米管在溶剂中的分散性，并能同时提高碳纳米管的堆积密度，以得到最佳的分散效果与良好的加工性。
本发明将碳纳米管经预处理改性后，再将活性碳纳米管与有机树脂、有机溶剂、抗沉降剂、消泡剂等混合，通过超声、砂磨工艺将其混合均匀，制备出高效分散型油系碳纳米管导电浆料。制备出的导电浆料降低了碳纳米管的团聚程度，使其更好的分散于溶剂中，形成网状结构，提高其导电能力，同时大大降低了碳纳米管的沉降速度，延长了产品的保存及使用周期，浆料的分散性好，储存稳定性优秀。
本发明提供的高分散型油系碳纳米管导电浆料可应用作为电磁屏蔽涂料、抗静电涂料、导电涂料。
四、具体实施方式
下面以具体实施例来对本发明的技术方案做进一步说明，但本发明的保护内容不限于此。
实施例1～16
按下表1取各原料，将油性分散剂溶于有机溶剂中，得到分散剂溶液，然后将分散剂溶液通过高压喷淋法喷入高速搅拌的碳纳米管(直径1～30nm，长度1～100μm，堆积密度0.02g/mL)中，工艺参数如表1所示，高速搅拌混合后，制得活性碳纳米管；
表1
制得的活性碳纳米管的性能检测结果如下表2
表2
分散性实验按以下方法检测：将实施例1～16制得的活性碳纳米管10mg分别加入10mL制备该活性碳纳米管所用的溶剂(参见表1)中，超声分散30分钟，得到悬浮液，静置，出现明显分层时，记录时间为保存时间，所得结果详见表2。保存时间越长，表明其分散性越好。未经预处理的碳纳米管无法形成稳定的悬浮液。
上述实验结果表明，经预处理后，碳纳米管的堆积密度提高了10倍左右(未处理的碳纳米管的堆积密度为0.02g/mL左右)，分散性均有显著提高。
实施例17～32
将实施例1～16制备的活性碳纳米管与有机树脂、有机溶剂、抗沉降剂、消泡剂混合，经超声或砂磨工艺混合均匀，制得所述高分散型油系碳纳米管导电浆料；各原料用量见表3。实施例17～24采用超声工艺，实施例25～32采用砂磨工艺。
制备得到的高分散型油系碳纳米管导电浆料的固含量和性能数据如表4所示。其中储存稳定性(一年)按照标准《GB6753.3》检测。
将实施例17～32制备的高分散型油系碳纳米管导电浆料喷涂于PET基材上，按照《GB/T1410-2006固体绝缘材料体积电阻率和表面电阻率试验方法》测试涂层的表面电阻率，结果如表4所示。
表3
表4
实施例数据表明，本发明制备的高分散型油系碳纳米管导电浆料的制备的抗静电涂层的表面电阻率较好，表面电阻率在106～108Ω左右，抗静电性能良好，而且所用的抗静电剂(即碳纳米管)的用量比现有技术要达到同样性能的抗静电剂的用量要显著降低。分散性优良，长期保存性能表现优秀。
Claims (10)
1.一种高分散型油系碳纳米管导电浆料，其特征在于所述高分散型油系碳纳米管导电浆料包括以下重量份的组分：
有机树脂10～60质量份、活性碳纳米管5～40质量份、有机溶剂B 20～70质量份；
所述活性碳纳米管按以下方法制得：
将油性分散剂溶于有机溶剂A中，得到分散剂溶液，然后将分散剂溶液通过高压喷淋法喷入高速搅拌的碳纳米管中，高速搅拌混合后，制得活性碳纳米管。
2.如权利要求1所述的高分散型油系碳纳米管导电浆料，其特征在于所述碳纳米管、油性分散剂、有机溶剂A的质量份数比为85～95：0.1～5：5～10。
3.如权利要求1所述的高分散型油系碳纳米管导电浆料，其特征在于所述高分散型油系碳纳米管导电浆料还包括助剂，所述助剂为抗沉降剂和消泡剂，所述有机树脂、活性碳纳米管、有机溶剂B、抗沉降剂、消泡剂的质量份数为10～60质量份、5～40质量份、20～70质量份、0.01～10质量份、0.01～10质量份。
4.如权利要求1所述的高分散型油系碳纳米管导电浆料，其特征在于所述高分散型油系碳纳米管导电浆料由以下重量份的组分组成：有机树脂、活性碳纳米管、有机溶剂B、抗沉降剂、消泡剂的质量份数为20～40质量份、10～40质量份、30～60质量份、0.1～5质量份、0.1～5质量份。
5.如权利要求1所述的高分散型油系碳纳米管导电浆料，其特征在于所述油性分散剂为聚乙烯吡咯烷酮、聚乙烯醇、聚乙二醇辛基苯基醚、烷基酚环氧乙烷缩合物乳化剂、聚偏氟乙烯中的一种或两种以上的混合物。
6.如权利要求1所述的高分散型油系碳纳米管导电浆料，其特征在于所述有机溶剂A或有机溶剂B各自独立为N,N-二甲基甲酰胺、N-甲基吡咯烷酮、二甲基甲酰胺、二甲基亚砜、氯仿、石油醚、乙酸乙酯、乙酸丁酯、丙酮、环己酮中的一种或两种以上的混合物。
7.如权利要求1所述的高分散型油系碳纳米管导电浆料，其特征在于所述有机树脂选自环氧树脂、聚氨酯树脂、聚酯树脂、丙烯酸树脂、硅氧烷树脂或聚醚多元醇树脂中的一种或两种以上的混合物。
8.如权利要求3所述的高分散型油系碳纳米管导电浆料，其特征在于所述的抗沉降剂为有机改性的硼润土、聚酰胺防沉蜡浆、气相二氧化硅中的一种或两种以上的混合。
9.如权利要求3所述的高分散型油系碳纳米管导电浆料，其特征在于所述消泡剂为矿物油、聚硅氧烷聚醚共聚物、聚醚化合物、改性有机硅混合物中的一种或两种以上的混合。
10.如权利要求1～9之一所述的高分散型油系碳纳米管导电浆料作为电磁屏蔽涂料、抗静电涂料、导电涂料的应用。
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