CN101838382A - 石墨烯填充三聚氰胺-甲醛树脂抗静电材料的制备方法 - Google Patents
石墨烯填充三聚氰胺-甲醛树脂抗静电材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种新型纳米材料-石墨烯填充三聚氰胺-甲醛树脂抗静电材料的制备方法。其步骤为:经超声分散将氧化还原法制得石墨烯的水或有机溶剂分散液按一定比例均匀分散到甲醛溶液中,再与三聚氰胺发生缩聚反应,形成石墨烯改性的三聚氰胺-甲醛树脂预聚胶。将装饰板用纸在石墨烯-三聚氰胺-甲醛树脂预聚胶中充分浸渍、晾干、真空干燥,再在油压机中压制成石墨烯改性装饰贴面板。本发明的经石墨烯改性的三聚氰胺-甲醛树脂的面电阻由原来的(1012~1014)Ω下降到106Ω,消除了三聚氰胺-甲醛树脂使用过程中所带来的静电危害,扩大了三聚氰胺-甲醛树脂的应用范围,经石墨烯改性的三聚氰胺-甲醛树脂适于做电子电气产品的装饰材料。
Description
技术领域
本发明涉及新型纳米材料石墨烯在制备新型抗静电材料方面的应用,特指将它应用在制备抗静电的三聚氰胺-甲醛树脂材料方面。
背景技术
三聚氰胺-甲醛树脂具有耐水、耐热、耐磨、耐化学腐蚀和机械强度好等优异性能,已广泛应用于木材、塑料、涂料、造纸、纺织、皮革等行业。由于三聚氰胺-甲醛树脂独特的三嗪环与亚甲基形成的相互交错的刚性结构,可以将它用于制备纸质装饰板和装饰纸贴面板。但是,此树脂的面电阻很高,一般在(1012~1014)Ω之间。它们表面很容易因摩擦或碰撞产生和积累静电,从而限制了它在电子电气行业的应用,另外,静电作用还会导致所制品易吸附尘埃,所以对此类树脂材料的抗静电处理至关重要。要做到消除三聚氰胺-甲醛树脂的静电危害,必须对它进行改性,降低它的面电阻,从而扩大其应用范围。
但是,现有抗静电剂在某些方面存在不足,例如,炭黑和石墨颗粒或粉状抗静电剂在预聚体中分散不均匀,导致所制品表面的抗静电性能不均匀而影响使用效果;镍、铜和铬等导电金属材料与预聚体相容性较差,会导致制品的力学性能下降较明显,使用范围受限;表面活性剂型抗静电剂受空气湿度的影响较大,当空气湿度低于50%时抗静电效果很差,且所制品的抗静电寿命不长。因此,寻找高效导电材料,制得导电三聚氰胺-甲醛树脂材料,具有非常重要的工业应用价值。本发明人发现,近期发现的新型纳米材料----石墨烯,具有优异的电学性能,还具有和碳纳米管相似的优异力学性能,是目前已知世界上强度最高的材料,与昂贵的富勒烯和碳纳米管相比,它价格低廉、原料易得、添加量少,非常适合于开发大规模高性能三聚氰胺-甲醛树脂抗静电材料,这也是石墨烯纳米材料迈向实际应用的一个重要方向。
发明内容
本发明的目的在于提供一种用石墨烯来降低三聚氰胺-甲醛树脂的面电阻的方法,以消除此树脂应用过程中所带来的静电危害,从而扩大它的应用范围。
本发明的技术方案是:用氧化还原法制备石墨烯,经超声分散将石墨烯的水或有机溶剂分散液按一定比例均匀分散到甲醛溶液中,再与三聚氰胺发生缩聚反应,形成石墨烯-三聚氰胺-甲醛树脂预聚胶。将装饰板用纸在石墨烯-三聚氰胺-甲醛树脂预聚胶中充分浸渍、晾干、真空干燥,再在油压机中压制成石墨烯改性装饰贴面板。
本发明包括以下步骤:
(1)将石墨烯的水或有机溶剂均分散液按一定比例均匀分散到甲醛溶液中,其中石墨烯与甲醛溶液质量比范围为1/10000~1/100,经超声分散备用;所述的有机溶剂为DMF、丙酮、甲苯、甲醇或乙醇,所述的石墨烯均分散液的浓度范围为1g石墨烯/1000g溶剂~1g石墨烯/20g溶剂;所述的甲醛溶液的质量分数为37%;
(2)将占甲醛摩尔量40%的三聚氰胺加入步骤1所得溶液液中,缩聚形成石墨烯-三聚氰胺-甲醛树脂;
(3)将装饰贴面板用纸裁剪成一定尺寸大小,每次试验准备三张这类试验纸,并编号;所述的装饰贴面板用纸尺寸范围为2cm×2cm~1.0m×1.0m;
(4)将试验纸浸渍于石墨烯-三聚氰胺-甲醛树脂中,待每张纸都浸渍足够多树脂后取出,滴掉多余的树脂;
(5)将浸胶试验纸放入真空干燥箱内烘干,温度控制在(80~140)℃;
(6)将烘干的试验纸取出,再重复步骤(4)、(5)一次;
(7)将一张浸好石墨烯-三聚氰胺-甲醛树脂预聚胶的试验纸,置于光滑的铝合金板上,在油压机上于135℃,4~100大气压下加热15min,即制得石墨烯改性装饰贴面板;
(8)将石墨烯-三聚氰胺-甲醛树脂材料装饰贴面板进行面电阻测试。
本发明与现有技术相比,其显著优点是:经石墨烯改性的三聚氰胺-甲醛树脂的面电阻由原来的(1012~1014)Ω下降到106Ω,消除了此树脂在使用过程中所带来的静电危害,扩大了三聚氰胺-甲醛树脂的应用范围,经石墨烯改性的三聚氰胺-甲醛树脂适于做电子电气产品的装饰材料。
附图说明
附图是本发明的石墨烯填充三聚氰胺-甲醛树脂抗静电材料制备流程示意图。
具体实施方式
下面结合附图和具体实施例对本发明作进一步的说明。
本发明中面电阻的测试方法为绝缘电阻测试方法(参见GB-T4677.1-1984-印制板表层绝缘电阻测试方法)。
实施例1
将10.0g石墨烯的DMF均分散液(浓度为1g石墨烯/1000gDMF,石墨烯单片层的尺寸为100nm~5μm)均匀分散到50.0g甲醛溶液(为51.5ml)中,经超声分散后,加入31.1g(约0.2mol)三聚氰胺,在80℃发生缩聚反应,直至反应沉淀比达到2∶2,即制得石墨烯-三聚氰胺-甲醛树脂。
将一张2cm×2cm的装饰贴面板用纸浸渍于石墨烯-三聚氰胺-甲醛树脂中,待装饰贴面板用纸浸渍了足够多树脂后取出,滴掉多余的树脂,放入真空干燥箱内烘干,温度控制在(80~140)℃,烘干后,将该装饰贴面板用纸置于光滑的铝合金板上,在油压机上于135℃,10atm下加热15min,即制得石墨烯改性装饰贴面板,用绝缘电阻测试方法测其面电阻,实验结果见表1。
实施例2
将10.0g石墨烯的乙醇均分散液(浓度为1g石墨烯/1000g乙醇,石墨烯单片层的尺寸为50nm~30μm)均匀分散到50.0g甲醛溶液(为51.5ml)中,经超声分散后,加入31.1g(约0.2mol)三聚氰胺,在80℃发生缩聚反应,直至反应沉淀比达到2∶2,即制得石墨烯-三聚氰胺-甲醛树脂。
将一张20cm×20cm的装饰贴面板用纸浸渍于石墨烯-三聚氰胺-甲醛树脂中,待装饰贴面板用纸浸渍了足够多树脂后取出,滴掉多余的树脂,放入真空干燥箱内烘干,温度控制在(80~140)℃,烘干后,将该装饰贴面板用纸置于光滑的铝合金板上,在油压机上于135℃,10atm下加热15min,即制得石墨烯改性装饰贴面板,用绝缘电阻测试方法测其面电阻,实验结果见表1。
实施例3
将5.0g石墨烯的DMF均分散液(浓度为1g石墨烯/250gDMF,石墨烯单片层的尺寸为1μm~30μm)均匀分散到50.0g甲醛溶液(为51.5ml)中,经超声分散后,加入31.1g(约0.2mol)三聚氰胺,在80℃发生缩聚反应,直至反应沉淀比达到2∶2,即制得石墨烯-三聚氰胺-甲醛树脂。
将一张2cm×2cm的装饰贴面板用纸浸渍于石墨烯-三聚氰胺-甲醛树脂中,待装饰贴面板用纸浸渍了足够多树脂后取出,滴掉多余的树脂,放入真空干燥箱内烘干,温度控制在(80~140)℃,烘干后,将该装饰贴面板用纸置于光滑的铝合金板上,在油压机上于135℃,10atm下加热15min,即制得石墨烯改性装饰贴面板,用绝缘电阻测试方法测其面电阻,实验结果见表1。
实施例4
将15.0g石墨烯的丙酮均分散液(浓度为1g石墨烯/1000g丙酮,石墨烯单片层的尺寸为500nm~40μm)均匀分散到50.0g甲醛溶液(为51.5ml)中,经超声分散后,加入31.1g(约0.2mol)三聚氰胺,在80℃发生缩聚反应,直至反应沉淀比达到2∶2,即制得石墨烯-三聚氰胺-甲醛树脂。
将一张2cm×2cm的装饰贴面板用纸浸渍于石墨烯-三聚氰胺-甲醛树脂中,待装饰贴面板用纸浸渍了足够多树脂后取出,滴掉多余的树脂,放入真空干燥箱内烘干,温度控制在(80~140)℃,烘干后,将该装饰贴面板用纸置于光滑的铝合金板上,在油压机上于135℃,10atm下加热15min,即制得石墨烯改性装饰贴面板,用绝缘电阻测试方法测其面电阻,实验结果见表1。
实施例5
将10.0g石墨烯的甲苯均分散液(浓度为1g石墨烯/1000g甲苯,石墨烯单片层的尺寸为500nm~45μm)均匀分散到50.0g甲醛溶液(为51.5ml)中,经超声分散后,加入31.1g(约0.2mol)三聚氰胺,在80℃发生缩聚反应,直至反应沉淀比达到2∶2,即制得石墨烯-三聚氰胺-甲醛树脂。
将一张2cm×2cm的装饰贴面板用纸浸渍于石墨烯-三聚氰胺-甲醛树脂中,待装饰贴面板用纸浸渍了足够多树脂后取出,滴掉多余的树脂,放入真空干燥箱内烘干,温度控制在(80~140)℃,烘干后,将该装饰贴面板用纸置于光滑的铝合金板上,在油压机上于135℃,15atm下加热15min,即制得石墨烯改性装饰贴面板,用绝缘电阻测试方法测其面电阻,实验结果见表1。
实施例6
将20.0g石墨烯的乙醇均分散液(浓度为1g石墨烯/500g乙醇,石墨烯单片层的尺寸为10μm~30μm)均匀分散到50.0g甲醛溶液(为51.5ml)中,经超声分散后,加入31.1g(约0.2mol)三聚氰胺,在80℃发生缩聚反应,直至反应沉淀比达到2∶2,即制得石墨烯-三聚氰胺-甲醛树脂。
将一张2cm×2cm的装饰贴面板用纸浸渍于石墨烯-三聚氰胺-甲醛树脂中,待装饰贴面板用纸浸渍了足够多树脂后取出,滴掉多余的树脂,放入真空干燥箱内烘干,温度控制在(80~140)℃,烘干后,将该装饰贴面板用纸置于光滑的铝合金板上,在油压机上于135℃,10atm下加热15min,即制得石墨烯改性装饰贴面板,用绝缘电阻测试方法测其面电阻,实验结果见表1。
对照例1
将10.0gDMF均匀分散到50.0g甲醛溶液(为51.5ml)中,经超声分散后,加入31.1g(约0.2mol)三聚氰胺,在80℃发生缩聚反应,直至反应沉淀比达到2∶2,即制得三聚氰胺-甲醛树脂。
将一张2cm×2cm的装饰贴面板用纸浸渍于三聚氰胺-甲醛树脂中,待装饰贴面板用纸浸渍了足够多树脂后取出,滴掉多余的树脂,放入真空干燥箱内烘干,温度控制在(80~140)℃,烘干后,将该装饰贴面板用纸置于光滑的铝合金板上,在油压机上于135℃,10atm下加热15min,即制得三聚氰胺-甲醛树脂贴面板,用绝缘电阻测试方法测其面电阻,实验结果见表1。
表1
Claims (1)
1.石墨烯填充三聚氰胺-甲醛树脂抗静电材料的制备方法,其特征在于包括以下步骤:
(1)将石墨烯的水或有机溶剂均分散液按一定比例均匀分散到甲醛溶液中,其中石墨烯与甲醛溶液质量比范围为1/10000~1/100,经超声分散备用;所述的有机溶剂为DMF、丙酮、甲苯、甲醇或乙醇,所述的石墨烯均分散液的浓度范围为1g石墨烯/1000g溶剂~1g石墨烯/20g溶剂;所述的甲醛溶液的质量分数为37%;
(2)将占甲醛摩尔量40%的三聚氰胺加入步骤1所得溶液液中,缩聚形成石墨烯-三聚氰胺-甲醛树脂;
(3)将装饰贴面板用纸裁剪成一定尺寸大小,每次试验准备三张这类试验纸,并编号;所述的装饰贴面板用纸尺寸范围为2cm×2cm~1.0m×1.0m;
(4)将试验纸浸渍于石墨烯-三聚氰胺-甲醛树脂中,待每张纸都浸渍足够多树脂后取出,滴掉多余的树脂;
(5)将浸胶试验纸放入真空干燥箱内烘干,温度控制在(80~140)℃;
(6)将烘干的试验纸取出,再重复步骤(4)、(5)一次;
(7)将一张浸好石墨烯-三聚氰胺-甲醛树脂预聚胶的试验纸,置于光滑的铝合金板上,在油压机上于135℃,4~100大气压下加热15min,即制得石墨烯改性装饰贴面板;
(8)将石墨烯-三聚氰胺-甲醛树脂材料装饰贴面板进行面电阻测试。
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