CN105907259A - 一种耐高温环氧树脂基散热粉末涂料及其制作方法 - Google Patents

一种耐高温环氧树脂基散热粉末涂料及其制作方法 Download PDF

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CN105907259A
CN105907259A CN201610529826.6A CN201610529826A CN105907259A CN 105907259 A CN105907259 A CN 105907259A CN 201610529826 A CN201610529826 A CN 201610529826A CN 105907259 A CN105907259 A CN 105907259A
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陈俊
刘学涛
赵遵刚
霍柏林
李正
孙红兴
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Yan Mei Powdery Paints Co Ltd Of Hefei City
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Abstract

本发明公开了一种耐高温环氧树脂基散热粉末涂料，以双酚Ａ和环氧氯丙烷为原料，纳米碳管为导热填料，通过原位聚合法得到改性环氧树脂，使碳纳米管与环氧基团形成远大于范德华力的作用力，有利于两者之间的应力传递，提高了两者之间的界面结合力和相容性，改善了涂料存储稳定性；同时添加壳聚糖、改性助料等为增强填料，复合材料中碳氯键的伸缩振动强度减弱，C、Cl原子与周围原子的结合力增强，改善了各组分在涂料中的分散性，促使碳纳米管与涂料充分接触并起到额外的物理交联点的作用，形成散热通道，有利于热量的散发，制得的涂料具有抗菌、耐高温低温、耐化学腐蚀等性能，并且应用领域广。

Description

一种耐高温环氧树脂基散热粉末涂料及其制作方法
技术领域
本发明涉及粉末涂料技术领域，尤其涉及一种耐高温环氧树脂基散热粉末涂料及其制作方法。
背景技术
随着现代科技的快速发展，电子器件的高频、高速以及集成电路的密集和小型化，使得单位容积电子器件的总功率密度和发热量大幅度地增长，从而使电子器件的冷却问题变得越来越突出。而常规的冷却系统所能达到的冷却能力受到极大挑战，尤其在能源、汽车、空调、农业、化工、采暖、航空航天、微电子、信息等领域，对强化传热、提高散热效率等技术提出了更高的要求。而散热涂料是一种提高物体表面散热效率，降低体系温度的特种涂料。粉末涂料是一种新型的不含溶剂100%固体粉末状涂料，具有高利用率、易涂装、耐腐蚀、环保等优点，在现代喷涂和防腐散热领域中得到了广泛应用，将散热粉末涂料涂在电子器件上可以显著提高电子器件的散热效率。
环氧树脂是非常重要的热固性高分子材料之一，具有粘结强度高，电绝缘性能好，收缩率低，加工性能好等优点，被广泛应用于电子、机械、建筑等各领域。纳米碳管具有较高的热导率，因此将纳米碳管作为填充材料填充到环氧树脂中作为一种散热材料具有很好的应用前景，但是由于纳米碳管的纳米效应，纳米碳管在环氧树脂中较难分散。为了提高纳米碳管在环氧树脂中的分散性，大都是将纳米碳管接枝改性，破坏了纳米碳管的结构，使其产生缺陷，这些缺陷有利于声子的散射，降低了碳纳米管的导热性能。因而需要改进现有方法改善纳米碳管在环氧树脂中的分散性。原位聚合法由于单体的分子量较小，粘度低，有利于纳米粒子在单体聚合过程中在基质中的的分散，而且原位聚合法并不破坏碳纳米管的结构。
《碳纳米管/环氧树脂复合粉末涂料的制备及其性能研究》一文采用双酚Ａ和环氧氯丙烷为原料，纳米碳管作为增强和导热填料，通过原位聚合法制备了碳纳米管/环氧树脂复合材料。结果表明：随着碳纳米管含量的增多，粉末涂料的各项性能逐渐变好。然而由于碳纳米管在复合粉末涂料中的分散性差易团聚，当碳纳米管含量继续增加时，复合材料的各项性能又变差，且利用文中的生产工艺和配方制备出的复合粉末涂料的功能较为单一，产品结构单一无特色，无法满足特殊环境中要求，需要加以改进。
发明内容
本发明目的就是为了弥补已有技术的缺陷，提供一种耐高温环氧树脂基散热粉末涂料及其制作方法。
本发明是通过以下技术方案实现的：
一种耐高温环氧树脂基散热粉末涂料，由下列重量份的原料制成：双酚A34-37、环氧氯丙烷18-23、碳纳米管2.5-3.5、壳聚糖3-4、脲丙基三乙氧基硅烷2.1-2.6、氧化锌4-6、六次甲基四胺2-4、椴木皮15-17、竹纤维6-8、硫黄1-2、烯基丁二酸酯3-5、松香季戊四醇乳液10-11、造纸黑泥9-11、颜料7-9。
所述的一种耐高温环氧树脂基散热粉末涂料的制作方法，包括以下步骤：
（1）将椴木皮烘干、粉碎研磨过200目筛，加入松香季戊四醇乳液搅拌混匀静置12-14小时，造粒，在氮气保护下于800-1000℃烧结20-30分钟得预混料；
（2）将造纸黑泥在740-820℃下煅烧2-3小时，出料冷却至60℃-80℃，加入脲丙基三乙氧基硅烷、竹纤维超声分散20-30分钟，加入步骤（1）预混料、氧化锌充分球磨，造粒，粒径为2-4μm，得改性助料；
（3）将双酚A放入10%的氢氧化钠溶液中加热至60℃搅拌混匀，降温至55℃加入碳纳米管超声分散30分钟，升温至80℃加入环氧氯丙烷、烯基丁二酸酯保持温度超声分散4小时，用冷水和80℃热水反复交替洗至中性，50℃低温烘干得改性环氧树脂；
（4）将步骤（3）制得的改性环氧树脂、壳聚糖及其他剩余成分投入高速混合机中搅拌混匀，经双螺杆挤出机熔融挤出，冷却磨粉，过250-300目筛，出料。
本发明的优点是：本发明以双酚Ａ和环氧氯丙烷为原料，纳米碳管为导热填料，通过原位聚合法得到改性环氧树脂，使碳纳米管与环氧基团形成远大于范德华力的作用力，有利于两者之间的应力传递，提高了两者之间的界面结合力和相容性，改善了涂料存储稳定性；同时添加壳聚糖、改性助料等为增强填料，复合材料中碳氯键的伸缩振动强度减弱，C、Cl原子与周围原子的结合力增强，改善了各组分在涂料中的分散性，促使碳纳米管与涂料充分接触并起到额外的物理交联点的作用，形成散热通道，有利于热量的散发，制得的涂料具有抗菌、耐高温低温、耐化学腐蚀等性能，并且应用领域广，不仅适用于LED相关的设备，还可用于CPU、电器、机柜、电线电缆、暖气片、风机风扇、热力管道、真空炉、真空暖气片等的散热器件上。
具体实施方式
一种耐高温环氧树脂基散热粉末涂料，由下列重量份的原料制成：双酚A34、环氧氯丙烷18、碳纳米管2.5、壳聚糖3、脲丙基三乙氧基硅烷2.1、氧化锌4、六次甲基四胺2、椴木皮15、竹纤维6、硫黄1、烯基丁二酸酯3、松香季戊四醇乳液10、造纸黑泥9、颜料7。
所述的一种耐高温环氧树脂基散热粉末涂料的制作方法，包括以下步骤：
（1）将椴木皮烘干、粉碎研磨过200目筛，加入松香季戊四醇乳液搅拌混匀静置12-14小时，造粒，在氮气保护下于800-1000℃烧结20-30分钟得预混料；
（2）将造纸黑泥在740-820℃下煅烧2-3小时，出料冷却至60℃-80℃，加入脲丙基三乙氧基硅烷、竹纤维超声分散20-30分钟，加入步骤（1）预混料、氧化锌充分球磨，造粒，粒径为2-4μm，得改性助料；
（3）将双酚A放入10%的氢氧化钠溶液中加热至60℃搅拌混匀，降温至55℃加入碳纳米管超声分散30分钟，升温至80℃加入环氧氯丙烷、烯基丁二酸酯保持温度超声分散4小时，用冷水和80℃热水反复交替洗至中性，50℃低温烘干得改性环氧树脂；
（4）将步骤（3）制得的改性环氧树脂、壳聚糖及其他剩余成分投入高速混合机中搅拌混匀，经双螺杆挤出机熔融挤出，冷却磨粉，过250-300目筛，出料。
利用本发明制得的散热粉末涂料的存储稳定性比纯环氧树脂的提高了1倍；抗冲击能力为39kg•cm；附着力和耐中性盐雾腐蚀等级为２级；热导率为0.591W/mK。

Claims (2)

1.一种耐高温环氧树脂基散热粉末涂料，其特征在于，由下列重量份的原料制成：双酚A34-37、环氧氯丙烷18-23、碳纳米管2.5-3.5、壳聚糖3-4、脲丙基三乙氧基硅烷2.1-2.6、氧化锌4-6、六次甲基四胺2-4、椴木皮15-17、竹纤维6-8、硫黄1-2、烯基丁二酸酯3-5、松香季戊四醇乳液10-11、造纸黑泥9-11、颜料7-9。
2.根据权利要求1所述的一种耐高温环氧树脂基散热粉末涂料的制作方法，其特征在于包括以下步骤：
（1）将椴木皮烘干、粉碎研磨过200目筛，加入松香季戊四醇乳液搅拌混匀静置12-14小时，造粒，在氮气保护下于800-1000℃烧结20-30分钟得预混料；
（2）将造纸黑泥在740-820℃下煅烧2-3小时，出料冷却至60℃-80℃，加入脲丙基三乙氧基硅烷、竹纤维超声分散20-30分钟，加入步骤（1）预混料、氧化锌充分球磨，造粒，粒径为2-4μm，得改性助料；
（3）将双酚A放入10%的氢氧化钠溶液中加热至60℃搅拌混匀，降温至55℃加入碳纳米管超声分散30分钟，升温至80℃加入环氧氯丙烷、烯基丁二酸酯保持温度超声分散4小时，用冷水和80℃热水反复交替洗至中性，50℃低温烘干得改性环氧树脂；
（4）将步骤（3）制得的改性环氧树脂、壳聚糖及其他剩余成分投入高速混合机中搅拌混匀，经双螺杆挤出机熔融挤出，冷却磨粉，过250-300目筛，出料。
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CN105585934A (zh) * 2014-10-29 2016-05-18 西安优信机电工程有限公司 一种碳纳米管填充环氧树脂复合粉末涂料的制备方法

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袭肖光等: "碳纳米管/环氧树脂复合粉末涂料的制备及其性能研究", 《浙江理工大学学报》 *

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