CN116253859A - 一种石墨烯改性聚氨酯电磁屏蔽材料的制备方法 - Google Patents
一种石墨烯改性聚氨酯电磁屏蔽材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种石墨烯改性聚氨酯电磁屏蔽材料的制备方法，该方法包括以下步骤：将氧化石墨烯粉体与水混合，得到氧化石墨烯分散液；将碳纳米管粉体溶于甲苯中，制成碳纳米管溶液；将碳纳米管溶液和聚[9‑(1‑辛基壬基)‑9H‑咔唑]混合；将氧化石墨烯溶液和碳纳米管‑聚[9‑(1‑辛基壬基)‑9H‑咔唑]溶液进行混合；将混合溶液、已二酸聚酯二元醇、二苯甲烷二异氰氨酯、丙三醇、硅油和水进行混合；将催化剂加入混合溶液中，搅拌后静置发泡，发泡后通过模具成型固化，得到石墨烯改性聚氨酯电磁屏蔽材料。通过本发明制备的石墨烯改性聚氨酯电磁屏蔽材料在厚度仅为0.1mm时也能有效地屏蔽外界电磁辐射，在X波段实现屏蔽效能大于55dB，电磁辐射屏蔽效果好。
Description
技术领域
本发明属于电磁屏蔽材料技术领域，具体地说是一种石墨烯改性聚氨酯电磁屏蔽材料的制备方法。
背景技术
聚氨酯材料广泛用于各个领域，其作为涂料、弹性体、泡沫等应用于建筑、家具、汽车等领域。作为聚氨酯应用形态中最重要的一类产品，聚氨酯泡沫在许多的精密仪器运输过程中用来进行包裹，质量轻、弹性，能起到明显的缓冲作用。然而对于精密仪器的保护除了减少震动以及冲击外，更需要减弱外界的电磁辐射对精密仪器的性能影响。另外，随着人类社会的快速发展，电磁污染对人类的危害也在日益加剧，正逐渐被人们熟知和关注，特别是在信息技术快速发展的时代，各类电子设备进入了人类的生产生活，带来便利的同时也带来了电磁污染和射频干扰，引发了危害身体健康等一系列问题，因此开发生产有效聚氨酯电磁屏蔽材料越来越受到研发人员的关注和广大的市场需求。
电磁屏蔽材料的屏蔽效能取决于材料的电导率、磁导率和结构，传统的电磁屏蔽材料以金属为主，如铜、铝等。金属作为电磁屏蔽材料存在诸多缺点，如密度较大、易被腐蚀、非柔性、成本高等。石墨烯是一种片状二维碳素材料，具有优异的物理化学性能，是目前世上最薄却也是最坚硬的纳米材料，也是目前世上电阻率最小的材料，常温下其电子迁移率超过15000cm2/V·s，比碳纳米管或硅晶体高，而电阻率只约10-6Ω·cm，比铜或银更低。通过将石墨烯作为导电添加剂形成立体网络导电结构可以很大程度增加材料的导电能力。
CN 110149790A提出一种制备石墨烯电磁屏蔽膜的方法，该专利将石墨烯导电油墨涂敷于经除油的柔性支撑基底上以形成石墨烯导电油墨墨层，并烘干、高温退火、电镀等操作以得到石墨烯电磁屏蔽膜。虽然在基体表面涂覆一层较薄的导电金属层或导电涂料，提高了导电率和磁导率，增强屏蔽效应，但其主要是以反射损耗为主，且屏蔽效果的大小取决于表面材料本身的屏蔽效果。虽然具有成本低、制备简单的优点，但表面导电材料层存在容易脱落、二次加工性能较差、使用寿命短的缺点。
ACS Applied Materials&Interfaces,2016,8,8050-8057使用溶液涂覆的技术制备了具有优异弹性且具有开孔结构的石墨烯涂层聚氨酯泡沫，并通过简单的机械压缩回复来改变多孔结构对电磁波的多重反射/散射衰减能力，从而实现了对泡沫材料屏蔽性能的有效调控。但是，上述复合泡沫材料的局限性在于当去除外力时材料的机械变形将恢复，无法固定屏蔽效能值。
发明内容
本发明的目的是克服现有技术中存在的不足，提供一种制备方法步骤简单、原料易得且无毒、制备过程绿色环保且产物电磁辐射屏蔽效果好的。
按照本发明提供的技术方案，所述石墨烯改性聚氨酯电磁屏蔽材料的制备方法，该方法包括以下步骤：
S1、将氧化石墨烯粉体50-100重量份与水混合，再经超声分散，得到4-10mg/ml浓度的氧化石墨烯分散液；
S2、将碳纳米管粉体10-100重量份溶于甲苯中，制成1-10mg/ml浓度的碳纳米管溶液；
S3、将S2制备的碳纳米管溶液和聚[9-(1-辛基壬基)-9H-咔唑]20-40重量份混合，然后进行搅拌，搅拌机转速控制在300-600rpm、搅拌时间控制在1-4h；
S4、将S1制备的氧化石墨烯溶液和S3制备的碳纳米管-聚[9-(1-辛基壬基)-9H-咔唑]溶液按体积比为(1-9):1进行混合；
S5、将S4制备的混合溶液、已二酸聚酯二元醇200-500重量份、二苯甲烷二异氰氨酯200-500重量份、丙三醇100-500重量份、硅油1-10重量份和水1-10重量份进行混合；
S6、将催化剂0.2-1重量份加入S5得到的混合溶液中，然后进行搅拌，搅拌机转速控制在1000-2000rpm、搅拌时间控制在15-60s，搅拌后静置发泡12-24h，发泡后通过模具成型固化，得到石墨烯改性聚氨酯电磁屏蔽材料。
作为优选，S1中，氧化石墨烯粉体通过Hummers法进行制备。
作为优选，S2中，碳纳米管粉体通过电弧法进行制备。
作为优选，S6中，催化剂为二月桂酸二丁基锡与三乙醇胺的混合物。进一步优选，催化剂为二月桂酸二丁基锡与三乙醇胺的等质量混合物。
本发明制备方法步骤简单、原料易得且无毒、制备过程绿色环保，通过本发明制备的石墨烯改性聚氨酯电磁屏蔽材料在厚度仅为0.1mm时也能有效地屏蔽外界电磁辐射，在X波段(8-12GHz)实现屏蔽效能大于55dB，电磁辐射屏蔽效果好。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1
一种石墨烯改性聚氨酯电磁屏蔽材料的制备方法，该方法包括以下步骤：
S1、将通过Hummers法制备的氧化石墨烯粉体50重量份与水混合，再经超声分散，得到10mg/ml浓度的氧化石墨烯分散液；
S2、将通过电弧法制备的碳纳米管粉体10重量份溶于甲苯中，制成2mg/ml浓度的碳纳米管溶液；
S3、将S2制备的碳纳米管溶液和聚[9-(1-辛基壬基)-9H-咔唑]20重量份混合，然后进行搅拌，搅拌机转速控制在600rpm、搅拌时间控制在1h；
S4、将S1制备的氧化石墨烯溶液和S3制备的碳纳米管-聚[9-(1-辛基壬基)-9H-咔唑]溶液按体积比为4:1进行混合；
S5、将S4制备的混合溶液、已二酸聚酯二元醇200重量份、二苯甲烷二异氰氨酯200重量份、丙三醇200重量份、硅油1重量份和水1重量份进行混合；
S6、将二月桂酸二丁基锡与三乙醇胺的等质量混合物催化剂0.2重量份加入S5得到的混合溶液中，然后进行搅拌，搅拌机转速控制在2000rpm、搅拌时间控制在15s，搅拌后静置发泡12h，发泡后通过模具成型固化，得到石墨烯改性聚氨酯电磁屏蔽材料。
实施例2
一种石墨烯改性聚氨酯电磁屏蔽材料的制备方法，该方法包括以下步骤：
S1、将通过Hummers法制备的氧化石墨烯粉体100重量份与水混合，再经超声分散，得到4mg/ml浓度的氧化石墨烯分散液；
S2、将通过电弧法制备的碳纳米管粉体100重量份溶于甲苯中，制成1mg/ml浓度的碳纳米管溶液；
S3、将S2制备的碳纳米管溶液和聚[9-(1-辛基壬基)-9H-咔唑]20重量份混合，然后进行搅拌，搅拌机转速控制在600rpm、搅拌时间控制在4h；
S4、将S1制备的氧化石墨烯溶液和S3制备的碳纳米管-聚[9-(1-辛基壬基)-9H-咔唑]溶液按体积比为1:1进行混合；
S5、将S4制备的混合溶液、已二酸聚酯二元醇500重量份、二苯甲烷二异氰氨酯500重量份、丙三醇100重量份、硅油5重量份和水5重量份进行混合；
S6、将二月桂酸二丁基锡与三乙醇胺的等质量混合物催化剂1重量份加入S5得到的混合溶液中，然后进行搅拌，搅拌机转速控制在1000rpm、搅拌时间控制在60s，搅拌后静置发泡24h，发泡后通过模具成型固化，得到石墨烯改性聚氨酯电磁屏蔽材料。
实施例3
一种石墨烯改性聚氨酯电磁屏蔽材料的制备方法，该方法包括以下步骤：
S1、将通过Hummers法制备的氧化石墨烯粉体50重量份与水混合，再经超声分散，得到10mg/ml浓度的氧化石墨烯分散液；
S2、将通过电弧法制备的碳纳米管粉体50重量份溶于甲苯中，制成10mg/ml浓度的碳纳米管溶液；
S3、将S2制备的碳纳米管溶液和聚[9-(1-辛基壬基)-9H-咔唑]40重量份混合，然后进行搅拌，搅拌机转速控制在300rpm、搅拌时间控制在2h；
S4、将S1制备的氧化石墨烯溶液和S3制备的碳纳米管-聚[9-(1-辛基壬基)-9H-咔唑]溶液按体积比为9:1进行混合；
S5、将S4制备的混合溶液、已二酸聚酯二元醇200重量份、二苯甲烷二异氰氨酯200重量份、丙三醇500重量份、硅油10重量份和水10重量份进行混合；
S6、将二月桂酸二丁基锡与三乙醇胺的等质量混合物催化剂0.5重量份加入S5得到的混合溶液中，然后进行搅拌，搅拌机转速控制在1000rpm、搅拌时间控制在30s，搅拌后静置发泡12h，发泡后通过模具成型固化，得到石墨烯改性聚氨酯电磁屏蔽材料。
将三个实施例固化成型的石墨烯改性聚氨酯材料放置常温干燥环境24h，每个实施例所得的石墨烯改性聚氨酯材料使用切片工具切取三块尺寸为10cm*10cm*0.1mm的成型材料，记为试样1-1、1-2、1-3、2-1、2-2、2-3、3-1、3-2、3-3，根据平面型电磁屏蔽材料的屏蔽效能测试方法(GB/T30142-2013)测试各试样的密度和X波段(8-12GHz)屏蔽性能，见表1。
表1
从表1可以看出，9个试样在X波段(8-12GHz)实现屏蔽效能大于55dB，电磁辐射屏蔽效果好。
Claims (5)
1.一种石墨烯改性聚氨酯电磁屏蔽材料的制备方法，其特征是该方法包括以下步骤：
S1、将氧化石墨烯粉体50-100重量份与水混合，再经超声分散，得到4-10mg/ml浓度的氧化石墨烯分散液；
S2、将碳纳米管粉体10-100重量份溶于甲苯中，制成1-10mg/ml浓度的碳纳米管溶液；
S3、将S2制备的碳纳米管溶液和聚[9-(1-辛基壬基)-9H-咔唑] 20-40重量份混合，然后进行搅拌，搅拌机转速控制在300-600rpm、搅拌时间控制在1-4h；
S4、将S1制备的氧化石墨烯溶液和S3制备的碳纳米管-聚[9-(1-辛基壬基)-9H-咔唑]溶液按体积比为 (1-9):1进行混合；
S5、将S4制备的混合溶液、已二酸聚酯二元醇200-500重量份、二苯甲烷二异氰氨酯200-500重量份、丙三醇100-500重量份、硅油1-10重量份和水1-10重量份进行混合；
S6、将催化剂0.2-1重量份加入S5得到的混合溶液中，然后进行搅拌，搅拌机转速控制在1000-2000rpm、搅拌时间控制在15-60s，搅拌后静置发泡12-24h，发泡后通过模具成型固化，得到石墨烯改性聚氨酯电磁屏蔽材料。
2.如权利要求1所述的石墨烯改性聚氨酯电磁屏蔽材料的制备方法，其特征是：S1中，氧化石墨烯粉体通过Hummers法进行制备。
3.如权利要求1所述的石墨烯改性聚氨酯电磁屏蔽材料的制备方法，其特征是：S2中，碳纳米管粉体通过电弧法进行制备。
4.如权利要求1所述的石墨烯改性聚氨酯电磁屏蔽材料的制备方法，其特征是：S6中，催化剂为二月桂酸二丁基锡与三乙醇胺的混合物。
5.如权利要求4所述的石墨烯改性聚氨酯电磁屏蔽材料的制备方法，其特征是：催化剂为二月桂酸二丁基锡与三乙醇胺的等质量混合物。
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