CN106590400B - 一种石墨烯改性水性导电涂料及其制备方法 - Google Patents
一种石墨烯改性水性导电涂料及其制备方法 Download PDFInfo
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- Polyurethanes Or Polyureas (AREA)
Abstract
本发明涉及一种石墨烯改性水性导电涂料，由石墨烯改性水性醇酸树脂、水性醇酸树脂、水性丙烯酸树脂、乙二醇单丁醚、流平剂、异丙醇、分散剂、纳米二氧化硅、润湿剂、铜粉、氧化锌和去离子水组成；其中，所述的石墨烯聚氨酯改性水性醇酸树脂由植物油类脂肪酸、有机酸酐、多元醇、多元酸、石墨烯、二羟甲基丙酸、多异氰酸酯、中和剂和去离子水组成通过反应制得；本发明还提供一种石墨烯改性水性醇酸树脂的制备方法；本发明制得的一种石墨烯改性水性导电涂料，特点是硬度高，附着力好、交联密度高、耐腐蚀性能好、无污染、导电性能好、屏蔽效果佳。
Description
技术领域
本发明涉及一种导电涂料的制备方法，特别涉及一种导电性能好、屏蔽效果佳的石墨烯改性水性导电涂料的制备方法，属于水性特种功能涂料技术领域。
背景技术
随着电子信息技术的不断发展，电子产品已经越来越广泛的应用于生活中的各个领域，它们的工作给人们带来极大便利的同时也释放出大量的电磁辐射，危害着人们的健康。音像器械、精密医疗器械、计算机、移动电话等设备的外壳大多采用塑壳体，而塑料壳体容易产生静电。因此，为了保证电子电气设备的正常工作，保护人体健生态自然环境，需要对这些设备和装置进行屏蔽以减少电磁辐射和电磁干扰。
常用的防止电磁辐射的方法是在底材的表面形成导电层，使底材具有传导电流和排除积累静电荷的能力，从而起到防止电磁辐射干扰的作用。而导电涂料具有优越的抗静电和电磁屏蔽性能，可以方便地喷涂或刷涂于各种形状的材料表面，形成电磁屏蔽导电层，从而使材料达到屏蔽电磁波的目的。目前，大多塑料表面的导电涂料采用溶剂型导电涂料，这对环境和人们的健康造成严重影响。
现有的水性导电涂料存在一些不足：水性涂层附着力低，容易脱落；银系导电性能虽然较好，但是价格贵且容易出现银迁移的现象；导电炭黑类价格极其低廉，化学稳定性好，分散性好，大多用于对导电性要求低的场合，在屏蔽涂料方面使用效果并不十分理想。
中国专利CN102850885A公开了一种塑料表面用导电涂料，该专利采用银粉作为导电填料，虽然其导电系数高，但是银粉价格贵很难适应市场需求。
中国专利CN102977742A公开了一种导电涂料，其采用单独的石墨烯作为导电涂料的导电填料，虽然其附着力较好，但存在分散难，与树脂相容性差，其在固化过程中需要加入固化剂，这对施工造成一定困扰。
中国专利CN103897461A公开了一种高性能的复合石墨烯导电涂料的制备方法,该复合石墨烯导电涂料以具有高效性能的石墨烯作为基本成分,并将无机的涂料复合起来,通过各种复合添加剂如分散剂、中和剂、流平剂、消泡剂、交联剂的综合作用,所制备的涂料具有优异的导电性能以及导涂层，可应用于电磁屏蔽、抗静电、防腐、散热、耐磨及电子线路等领域，具有广泛的应用价值。该专利中采用纳米石墨烯、纳米二氧化硅、纳米铜颗粒配制成导电涂料是一种掺杂型导电涂料，稳定性上不太理想。
为了达到足够的导电性能、电磁波防护效果，导电涂料所使用的导电材料需要具有良好的导电性，一般是贵金属，其价格高，连带的会提高导电涂料的成本，使导电涂料无法大量的使用，导致使用范围受的限制。因此开发一种导电性能好，附着力优异、低成本的导电涂料具有重大意义。
发明内容
本发明结合石墨烯的优点，利用氧化石墨烯中的羟基与多异氰酸酯反应制得改性石墨烯，再与醇酸树脂反应制得石墨烯聚氨酯改性水性醇酸树脂，石墨烯通过化学键与树脂结合，这不仅具有良好的导电性能，也具有良好的分散性，聚氨酯具有高硬度，耐摩擦等性能，这解决了涂层在使用过程的易划伤等问题，引入醇酸树脂，能有效降低成本，适应市场化需求。
本发明的目的旨在提供一种石墨烯改性水性导电涂料及其制备方法。
为了解决上面所述的技术问题，本发明采取以下技术方案：本发明涉及一种石墨烯改性水性导电涂料，按重量百分比计，其组成为：石墨烯改性水性醇酸树脂35.0～60.0份、水性丙烯酸树脂15.0～30.0份、乙二醇单丁醚2.0～5.0份、流平剂0.5～1.5份、异丙醇3.0～6.0份、分散剂1.0～4.0份、纳米二氧化硅2.0～5.0份、润湿剂0.2～0.6份、铜粉2.0～6.0份、氧化锌1.0～7.0份、去离子水4.0～10.0份。
本发明所述的石墨烯改性水性醇酸树脂，基于申请的发明专利“一种石墨烯聚氨酯改性水性醇酸树脂”，主要由植物油类脂肪酸、有机酸酐、多元醇、多元酸、石墨烯、二羟甲基丙酸、多异氰酸酯、中和剂和去离子水组成。
所述的石墨烯改性水性醇酸树脂，其特征在于：按重量百分比计，其组成为：植物油脂肪酸4.0～15.0份、苯酐1.0～4.0份、三羟甲基丙烷0.5～3.0份、二甲苯2.0～6.0份、新戊二醇1.0～6.0份、间苯二甲酸2.0～6.0份、苯甲酸4.0～8.0份、二羟甲基丙酸1.5～4.5份、石墨烯1.0～4.0份、多异氰酸酯4.0～12.0份、中和剂1.0～4.0份、二月桂酸二丁基锡0.02～0.08份、丙酮3.0～8.0份、去离子水40.0～65.0份。
其中，所述的植物油脂肪酸为精制亚麻油、大豆油、蓖麻油、妥尔油、椰子油、菜籽油、油酸中的一种或几种的组合。
所述的中和剂为三乙胺、氨水、二甲基乙醇胺中的一种或几种的组合。
所述的石墨烯为含羟基的氧化石墨烯，由Hummers法、Staudemaier法、电化学法或Brodie法制备；进一步的由Hummers法制备的氧化石墨烯。
所述的多异氰酸酯为甲苯二异氰酸酯TDI、异佛尔酮二异氰酸酯IPDI、六亚甲基二异氰酸酯HDI、苯二亚甲基二异氰酸酯XDI、环己烷二亚甲基二异氰酸酯H6XDI、四甲基苯二亚甲基二异氰酸酯TMXDI中的一种或几种的组合。
所述的石墨烯改性水性醇酸树脂的制备方法，其制备工艺如下：
步骤1、制备石墨烯聚氨酯活性体：按配方的重量百分比，将干燥好的氧化石墨烯和二羟甲基丙酸装入带有温度计、冷凝管、搅拌器的四口反应器中升温至75～80℃，然后匀速滴加多异氰酸酯，滴加时间为1h，继续反应2h，即得到活性中间体，待用；
步骤2、制备石墨烯聚氨酯改性水性醇酸树脂：在装有温度计、冷凝管、分水器、搅拌器的四口反应器中，按配方的重量百分比依次加入植物油脂肪酸、苯酐、三羟甲基丙烷、二甲苯、间苯二甲酸、苯甲酸和新戊二醇，缓慢加热升温至140℃，开慢速搅拌，1.5h后升温至180℃，保温约2h，并测定酸值，当出水很少时，继续缓慢升温至210℃，每隔20min测定其酸值，当酸值达到理论设计值时，除溶剂，降温至80℃，匀速加入上述活性中间体，并加入催化剂二月桂酸二丁基锡，继续反应2h，可试反应物粘度大小加丙酮降低粘度，测定NCO含量，当NCO含量接近理论设计值时，降温至45℃以下，匀速滴加中和剂中和，搅拌0.5h，加入适量的去离子水，过滤，脱丙酮，即得到石墨烯聚氨酯改性水性醇酸树脂。
本发明制得的一种石墨烯改性水性导电涂料，特点是硬度高，附着力好、交联密度高、耐腐蚀性能好、无污染、导电性能好、屏蔽效果佳等优点。
具体实施方式
本发明结合以下实例对石墨烯改性水性导电涂料做进一步的描述。
实施例1
一种石墨烯聚氨酯改性水性醇酸树脂，其制备工艺如下：
a、将干燥好的氧化石墨烯1.2份和二羟甲基丙酸2.5份装入带有温度计、冷凝管、搅拌器的四口反应器中升温至一定温度，然后匀速滴加多异氰酸酯8.0份，滴加时间为1h，继续反应2h，即得到活性中间体A，待用；
b、在装有温度计、冷凝管、分水器、搅拌器的四口反应器中，按配方的重量百分比依次加入植物油脂肪酸8.0份、苯酐2.0份、三羟甲基丙烷1.5份、二甲苯4.0份、间苯二甲酸3.0份、苯甲酸6.0份和新戊二醇3.0份，缓慢加热升温至140℃，开慢速搅拌，1.5h后升温至180℃，保温约2h，并测定酸值，当出水很少时，继续缓慢升温至210℃，每隔20min测定其酸值，当酸值达到理论设计值时，除溶剂，降温至80℃，匀速加入上述活性中间体A，并加入催化剂二月桂酸二丁基锡0.06份，丙酮4.0份，可试反应物粘度大小加丙酮降低粘度，继续反应2h，测定NCO含量，当NCO含量接近理论设计值时，降温至45℃以下，匀速滴加中和剂1.5份中和，搅拌0.5h，加入去离子水55.24份，过滤，脱丙酮，即得到石墨烯聚氨酯改性水性醇酸树脂Ⅰ。
实施例2
一种石墨烯聚氨酯改性水性醇酸树脂，其制备工艺如下：
a、将干燥好的氧化石墨烯1.4份和二羟甲基丙酸2.6份装入带有温度计、冷凝管、搅拌器的四口反应器中升温至一定温度，然后匀速滴加多异氰酸酯8.5份，滴加时间为1h，继续反应2h，即得到活性中间体B，待用；
b、在装有温度计、冷凝管、分水器、搅拌器的四口反应器中，按配方的重量百分比依次加入植物油脂肪酸8.0份、苯酐2.0份、三羟甲基丙烷1.0份、二甲苯3.0份、间苯二甲酸3.5份、苯甲酸5.0份和新戊二醇3.5份，缓慢加热升温至140℃，开慢速搅拌，1.5h后升温至180℃，保温约2h，并测定酸值，当出水很少时，继续缓慢升温至210℃，每隔20min测定其酸值，当酸值达到理论设计值时，除溶剂，降温至80℃，匀速加入上述活性中间体B，并加入催化剂二月桂酸二丁基锡0.08份，丙酮5.0份，可试反应物粘度大小加丙酮降低粘度，继续反应2h，测定NCO含量，当NCO含量接近理论设计值时，降温至45℃以下，匀速滴加中和剂1.6份中和，搅拌0.5h，加入去离子水54.82份，过滤，脱丙酮，即得到石墨烯聚氨酯改性水性醇酸树脂Ⅱ。
实施例3
一种石墨烯改性水性导电涂料，按重量百分比，其组成为：石墨烯聚氨酯改性水性醇酸树脂Ⅰ45.0份、水性丙烯酸树脂25.0份、乙二醇单丁醚3.0份、流平剂0.8份、异丙醇4.0份、分散剂2.0份、纳米二氧化硅3.0份、润湿剂0.4份、铜粉5.0份、氧化锌5.0份、去离子水6.8份。
实施例4
一种石墨烯改性水性导电涂料，按重量百分比，其组成为：石墨烯聚氨酯改性水性醇酸树脂Ⅱ50.0份、水性丙烯酸树脂22.0份、乙二醇单丁醚3.5份、流平剂1.2份、异丙醇4.0份、分散剂3.0份、纳米二氧化硅3.5份、润湿剂0.3份、铜粉3.0份、氧化锌4.0份、去离子水5.5份。
按照相关标准，对本发明的实施例中的石墨烯改性水性导电涂料性能进行检测，其性能技术指标如表1所示。
其中，干燥速度：按照GB1728的规定进行检测；
附着力：按照GB/T1720-1988的规定，使用划格法进行测试；
硬度：按照GB/T6739-2006色漆和清铅笔法测定漆膜硬度；
柔韧性：按照GB/T1731-1993的规定进行检测；
漆膜外观：按照GB/T1727-1992的规定进行检测；
耐水性：按照GB/T1733-93的规定进行检测；
耐盐雾性：按照GB/T1771-1991的规定进行检测；
表面电阻率：按照SJ/T 11294—2003的规定进行检测。
表1石墨烯改性水性导电涂料性能技术指标
| 检测项目 | 实施例3 | 实施例4 |
| 漆膜外观 | 平整光滑 | 平整光滑 |
| 耐水性 | 漆膜正常 | 漆膜正常 |
| 附着力 | 0级 | 0级 |
| 表干 | ≤1.5h | ≤1.5h |
| 实干 | ≤10h | ≤12h |
| 硬度 | H | H |
| 柔韧性mm | 1 | 1 |
| 耐盐雾性96h | 漆膜正常 | 漆膜正常 |
| 表面电阻率Ω/cm<sup>2</sup> | ≤0.08 | ≤0.1 |
尽管本发明已作了详细说明并引证了实施例，但对于本领域的普通技术人员，显然可以按照上述说明而做出的各种方案、修改和改动，都应该包括在权利要求的范围之内。
Claims (3)
1.一种石墨烯改性水性导电涂料，其特征在于：所述的石墨烯改性水性导电涂料，按重量份计，其组成为：石墨烯聚氨酯改性水性醇酸树脂Ⅰ45.0份、水性丙烯酸树脂25.0份、乙二醇单丁醚3.0份、流平剂0.8份、异丙醇4.0份、分散剂2.0份、纳米二氧化硅3.0份、润湿剂0.4份、铜粉5.0份、氧化锌5.0份、去离子水6.8份；
所述的石墨烯聚氨酯改性水性醇酸树脂Ⅰ，其制备步骤如下：
a)、制备石墨烯聚氨酯活性中间体A：将干燥好的氧化石墨烯1.2份和二羟甲基丙酸2.5份加入到带有温度计、冷凝管、搅拌器的四口反应器中，升温至一定温度，然后匀速滴加多异氰酸酯8.0份，滴加时间为1h，继续反应2h，得到的活性中间体A，待用；
b)、制备石墨烯聚氨酯改性水性醇酸树脂Ⅰ：在装有温度计、冷凝管、分水器、搅拌器的四口反应器中，依次加入植物油脂肪酸8.0份、苯酐2.0份、三羟甲基丙烷1.5份、二甲苯4.0份、间苯二甲酸3.0份、苯甲酸6.0份和新戊二醇3.0份，缓慢加热升温至140℃，开慢速搅拌，1.5h后升温至180℃，保温2h，并测定酸值，当出水量很少时，继续缓慢升温至210℃，每隔20min测定其酸值，当检测的酸值达到理论设计值时，除溶剂，降温至80℃，匀速加入活性中间体A，并加入催化剂二月桂酸二丁基锡0.06份，加丙酮4.0份降低粘度，继续反应2h，测定NCO含量，当检测的NCO含量接近理论设计值时，降温至45℃以下，匀速滴加中和剂1.5份，搅拌0.5h，加入去离子水55.24份，过滤，脱丙酮，得到石墨烯聚氨酯改性水性醇酸树脂Ⅰ；
其中，所述的植物油脂肪酸为精制亚麻油脂肪酸、大豆油脂肪酸、蓖麻油脂肪酸、妥尔油脂肪酸、椰子油脂肪酸或菜籽油脂肪酸中的一种或几种的组合；
所述的氧化石墨烯为Hummers法、Staudenmaier法或Brodie法制备的含羟基氧化石墨烯；
所述的多异氰酸酯为甲苯二异氰酸酯、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、苯二亚甲基二异氰酸酯、环己烷二亚甲基二异氰酸酯或四甲基苯二亚甲基二异氰酸酯中的一种或几种的组合；所述的中和剂为三乙胺、氨水或二甲基乙醇胺中的一种或几种的组合。
2.一种石墨烯改性水性导电涂料，其特征在于：所述的石墨烯改性水性导电涂料，按重量份计，其组成为：石墨烯聚氨酯改性水性醇酸树脂Ⅱ50.0份、水性丙烯酸树脂22.0份、乙二醇单丁醚3.5份、流平剂1.2份、异丙醇4.0份、分散剂3.0份、纳米二氧化硅3.5份、润湿剂0.3份、铜粉3.0份、氧化锌4.0份、去离子水5.5份；
所述的石墨烯聚氨酯改性水性醇酸树脂Ⅱ，其制备步骤如下：
a)、制备石墨烯聚氨酯活性中间体B：将干燥好的氧化石墨烯1.4份和二羟甲基丙酸2.6份加入到带有温度计、冷凝管、搅拌器的四口反应器中，升温至一定温度，然后匀速滴加多异氰酸酯8.5份，滴加时间为1h，继续反应2h，得到的活性中间体A，待用；
b)、制备石墨烯聚氨酯改性水性醇酸树脂Ⅰ：在装有温度计、冷凝管、分水器、搅拌器的四口反应器中，依次加入植物油脂肪酸8.0份、苯酐2.0份、三羟甲基丙烷1.0份、二甲苯3.0份、间苯二甲酸3.5份、苯甲酸5.0份和新戊二醇3.5份，缓慢加热升温至140℃，开慢速搅拌，1.5h后升温至180℃，保温2h，并测定酸值，当出水量很少时，继续缓慢升温至210℃，每隔20min测定其酸值，当检测的酸值达到理论设计值时，除溶剂，降温至80℃，匀速加入活性中间体B，并加入催化剂二月桂酸二丁基锡0.08份，加丙酮5.0份降低粘度，继续反应2h，测定NCO含量，当检测的NCO含量接近理论设计值时，降温至45℃以下，匀速滴加中和剂1.6份，搅拌0.5h，加入去离子水54.82份，过滤，脱丙酮，得到石墨烯聚氨酯改性水性醇酸树脂Ⅱ；
其中，所述的植物油脂肪酸为精制亚麻油脂肪酸、大豆油脂肪酸、蓖麻油脂肪酸、妥尔油脂肪酸、椰子油脂肪酸或菜籽油脂肪酸中的一种或几种的组合；
所述的氧化石墨烯为Hummers法、Staudenmaier法或Brodie法制备的含羟基氧化石墨烯；
所述的多异氰酸酯为甲苯二异氰酸酯、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、苯二亚甲基二异氰酸酯、环己烷二亚甲基二异氰酸酯或四甲基苯二亚甲基二异氰酸酯中的一种或几种的组合；所述的中和剂为三乙胺、氨水或二甲基乙醇胺中的一种或几种的组合。
3.根据权利要求1或2所述的石墨烯改性水性导电涂料，其特征在于：所述的氧化石墨烯为Hummers法制备的含羟基氧化石墨烯。
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