CN109053987A - 一种石墨烯/镍复合物改性水性聚氨酯材料的制备方法 - Google Patents
一种石墨烯/镍复合物改性水性聚氨酯材料的制备方法 Download PDFInfo
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Abstract
本发明公开一种石墨烯/镍复合物改性水性聚氨酯材料的制备方法,本发明通过原位聚合法将石墨烯/镍复合物引入聚氨酯中,一方面石墨烯/镍复合物可以使聚氨酯复合材料具有比单纯石墨烯更好的防电磁辐射效能,另一方面石墨烯/镍复合物可以提高聚氨酯的力学性能。本发明制备的水性聚氨酯复合材料可以广泛地应用于电磁辐射防护领域。
Description
技术领域
本发明属于复合材料制备技术领域,涉及改性水性聚氨酯材料的制备,尤其涉及一种用石墨烯/镍复合物改性的水性聚氨酯材料的制备方法。
背景技术
电磁辐射不仅对一些高精尖电子设备极易形成干扰,影响数据和信号的准确性,而且能够引发人体的病变反应。长期、过量的电磁辐射会导致生殖,神经的直接损伤,人体免疫系统破坏等严重的健康问题。防电磁辐射材料的发展是解决此类问题的有效途径之一。随着微波电子技术的快速发展,防电磁辐射材料在民用领域的应用越来越广。防电磁辐射材料在减弱,消除由电子产品如计算机、微波炉、移动电话等产生的有害电磁辐射方面有着良好的效果。在军事领域,防电磁辐射材料用于隐身技术更是各军事强国关注的热点之一。厚度薄、质量轻、吸收强、频段宽、性能高的防电磁辐射材料的研究和开发无论在改善民用电磁环境抑或军事隐身材料领域都具有重大意义。
石墨烯是一种新的二维碳材料,与传统碳材料相比,它具有更加优异的物理、化学和机械性能。石墨烯对电磁波响应的研究表明石墨烯对X 波段电磁波有良好的吸收特性,而且石墨烯对该频率电磁波的吸收具有非线性响应的特点。石墨烯复合材料具有对电磁辐射吸收频带宽、兼容性好、质量轻和厚度薄等特点。(Liang J J, Yan W, Yi H.Electromagnetic interference shielding of graphene/epoxy composites. Carbon,2009, 47(3): 922-925.; Mikhailov S A. Electromagnetic response of electronsin graphene: non-linear effects. Physica E: Low-dimensional Systems andstructures, 2008, 40(7): 2626−2629. )但是,对于除X波段之外的其他电磁波,石墨烯的吸收效果较差,无法满足军用的需求。
石墨烯与磁性金属复合有利于拓宽对电磁波的吸收频带,相关研究逐渐引起人们的重视。其中镍和石墨的润湿性好,同时它也不易与碳元素反应生成稳定的碳化物相,所以石墨烯/镍复合物的研究备受关注。例如,文献报道碳材料的反射率损耗通常位于高频区,与纳米镍的复合有利于吸收频带的拓宽(Li X L, Wang X R, et.al. Chemicallyderived ultrasmsmoothgraphenenanoribbon semiconductors [J].Science,2008,3 19,1229-1232.; Yan Q M, Huang B,Yu J, et. al. Intrinsic current-voltagecharacteristics of graphenenanoribbon transistors and effect of edge doping[J]. NanoLett, 2007, 7, 1469-1473.)。方建军等以石墨烯为原料,采用化学镀镍法在石墨烯上沉积纳米镍颗粒,并在2~18GHz频段范围内的电磁参数进行测试。结果表明,复合材料的微波吸收峰随着样品厚度的增加向低频移动,材料的电磁损耗机制主要为电损耗,未镀镍石墨烯的吸波层厚度为1mm 时,在 7GHz左右最大衰减值为−6.5dB,镀镍石墨烯的吸波层厚度为1.5mm 时,在约12GHz时最大值为−16.5d 2011, B,并且在频带 9.5~14.6 GHz 的范围内达到−10dB的吸收 (方建军,李素芳,查文珂等,镀镍石墨烯的微波吸收性能[J]. 无机材料学报2011,26 (5) :467-471.)。
水性聚氨酯具有优异的性能,是一类被广泛应用的高分子材料。随着功能聚氨酯材料的蓬勃发展,各种新型的功能水性聚氨酯材料不断出现。但是尚未见具有宽吸波性能的聚氨酯复合材料的报道。
本发明将石墨烯与镍通过一定的工艺步骤制备成的石墨烯/镍复合物,通过原位聚合法来改性水性聚氨酯,一方面石墨烯负载的镍可以使聚氨酯复合材料具有宽吸波功能,另一方面石墨烯可以改善聚氨酯的力学性能。通过综合镍和石墨烯各自的优点,从而使合成的水性聚氨酯在力学性能和防电磁辐射性能两方面都达到更高的水平。
发明内容
本发明的目的是提供一种既具有防电磁辐射功能,又具有良好机械性能的水性聚氨酯复合材料的制备方法。
为达到上述目的,本发明所公开的一种石墨烯/镍复合物改性水性聚氨酯材料的制备方法,包括如下步骤:
1. 制备石墨烯/镍复合物
石墨烯/镍复合物采用文献(方建军,李素芳,查文珂等,镀镍石墨烯的微波吸收性能[J]. 无机材料学报2011, 26 (5) :467-471.) 报道的方法制备。
2. 制备石墨烯/镍复合物改性的水性聚氨酯材料
将计量的聚酯多元醇或聚醚多元醇装入带有温度计、氮气保护装置的三口瓶中,在110℃条件下真空脱水2h,降温后加入一定量的二异氰酸酯和丁酮,在71℃~85℃之间反应90~110分钟得到预聚体,在预聚体中加入一定量的丁酮、2,2-二羟甲基丙酸(DMPA)和步骤1制备的石墨烯/镍复合物,在50℃~90℃(优选70℃)下反应3h,将反应液冷却至室温,加入一定量的三乙胺搅拌1h,将反应液倒入一定量的去离子水中,机械搅拌1h得到石墨烯/镍复合物改性的水性聚氨酯乳液,将乳液均匀地涂在离型纸上,并使得涂敷过程中不产生气泡,水平放置一天,成膜后在干燥箱中 80℃下烘5小时,从离型纸上剥离得到薄膜。
所述步骤2中聚酯多元醇可以是本领域常规的,优选聚己二酸丁二醇酯二醇(PBA)。
所述步骤2中聚醚多元醇可以是本领域常规的,优选至少有一种选自聚氧乙烯二醇(PEG)、聚氧丙烯二醇(PPG)、聚四氢呋喃二醇(PTHF)。
所述步骤2中二异氰酸酯可以是本领域常规的,优选至少有一种选自甲苯二异氰酸酯(TDI)、二苯基甲烷二异氰酸酯(MDI)、苯二亚甲基二异氰酸酯(XDI)、甲基环已基二异氰酸酯(HTDI)、二环已基甲烷二异氰酸酯(HMDI)、已二异氰酸酯(HDI)和异佛尔酮二异氰酸酯(IPDI)。
所述步骤2中二异氰酸酯与聚酯多元醇或聚醚多元醇、2,2-二羟甲基丙酸(DMPA)的质量比为20~39:100: 5~9。
所述步骤2中二异氰酸酯与石墨烯/镍复合物的质量比为180~280:1。
本发明的有益效果是:
本发明通过原位聚合法将石墨烯/镍复合物引入聚氨酯高分子链中,一方面石墨烯负载的镍可以使聚氨酯复合材料具有较宽的吸波功能,另一方面石墨烯可以改善聚氨酯的力学性能。因此该墨烯/镍复合物改性水性聚氨酯材料在力学性能和防电磁辐射性能两方面都达到更高的水平。
具体实施方式
本发明石墨烯/镍复合物改性水性聚氨酯材料的制备方法的具体实施方法如下。但是应该指出,本发明的实施不限于以下实施方式。
实施例1
采用文献(方建军,李素芳,查文珂等,镀镍石墨烯的微波吸收性能[J]. 无机材料学报2011, 26 (5) :467-471.)报道的方法制备石墨烯/镍复合物21mg。
在100mL三颈烧瓶中加入10g聚己二酸丁二醇酯二醇,在110℃条件下真空脱水2h。降温后将6g丁酮和3.9g甲苯二异氰酸酯加入烧瓶中,在75℃条件下反应110分钟得到预聚体。将6g丁酮、9g 2,2二羟甲基丙酸和21mg石墨烯/镍复合物加入烧瓶中,在70℃下反应3h,冷却至室温,加入6g三乙胺保温搅拌1h。将反应液倒入40g去离子水中,机械搅拌1h得到石墨烯/镍复合物改性的水性聚氨酯乳液。将乳液均匀地涂在离型纸上,并使得涂敷过程中不产生气泡。水平放置一天,成膜后在干燥箱中 80℃下烘5小时,从离型纸上剥离得到薄膜。
实施例2
采用文献(方建军,李素芳,查文珂等,镀镍石墨烯的微波吸收性能[J]. 无机材料学报2011, 26 (5) :467-471.)报道的方法制备石墨烯/镍复合物7mg。
在100mL三颈烧瓶中加入10g聚氧乙烯二醇,在110℃条件下真空脱水2h。降温后将6g丁酮和2g二苯基甲烷二异氰酸酯加入烧瓶中,在85℃条件下反应90分钟得到预聚体。将6g丁酮、5g 2,2二羟甲基丙酸和7mg石墨烯/镍复合物加入烧瓶中,在50℃下反应3h,冷却至室温,加入3g三乙胺保温搅拌1h。将反应液倒入40g去离子水中,机械搅拌1h得到乳液。薄膜的制备方法同实施例 1。
实施例3
采用文献(方建军,李素芳,查文珂等,镀镍石墨烯的微波吸收性能[J]. 无机材料学报2011, 26 (5) :467-471.)报道的方法制备石墨烯/镍复合物12mg。
在100mL三颈烧瓶中加入10g聚氧乙烯二醇,在110℃条件下真空脱水2h。降温后将6g丁酮和3.5g异佛尔酮二异氰酸酯加入烧瓶中,在78℃条件下反应100分钟得到预聚体。将6g丁酮、6g 2,2二羟甲基丙酸和12mg石墨烯/镍复合物加入烧瓶中,在50℃下反应3h,冷却至室温,加入3.2g三乙胺保温搅拌1h。将反应液倒入40g去离子水中,机械搅拌1h得到乳液。薄膜的制备方法同实施例 1。
实施例4
采用文献(方建军,李素芳,查文珂等,镀镍石墨烯的微波吸收性能[J]. 无机材料学报2011, 26 (5) :467-471.)报道的方法制备石墨烯/镍复合物18mg。
在100mL三颈烧瓶中加入10g聚四氢呋喃二醇,在110℃条件下真空脱水2h。降温后将6g丁酮和3.6g二环已基甲烷二异氰酸酯加入烧瓶中,在80℃条件下反应110分钟得到预聚体。将6g丁酮、6g 2,2二羟甲基丙酸和18mg石墨烯/镍复合物加入烧瓶中,在60℃下反应3h,冷却至室温,加入3.2g三乙胺保温搅拌1h。将反应液倒入40g去离子水中,机械搅拌1h得到乳液。薄膜的制备方法同实施例1。
实施例5
采用美国AgilentE83262B型矢量网络分析仪测定实施例1中所制备的薄膜的电磁屏蔽效能。在室温,样品尺寸为长2.2cm、宽1.0cm、厚3 mm时,测定在频率范围:8.2-12.6GHz,薄膜的屏蔽效能为15dB,在频率范围:5.4-8.0 GHz,薄膜的屏蔽效能为9dB。
Claims (7)
1.一种石墨烯/镍复合物改性水性聚氨酯材料的制备方法,具体步骤如下:
将计量的聚酯多元醇或聚醚多元醇装入带有温度计、氮气保护装置的三口瓶中,在110℃条件下真空脱水2h,降温后加入一定量的二异氰酸酯和丁酮,在71℃~85℃之间反应90~110分钟得到预聚体,在预聚体中加入一定量的丁酮、2,2-二羟甲基丙酸(DMPA)和石墨烯/镍复合物,在50℃~90℃下反应3h,将反应液冷却至室温,加入一定量的三乙胺搅拌1h,将反应液倒入一定量的去离子水中,机械搅拌1h得到石墨烯/镍复合物改性的水性聚氨酯乳液,将乳液均匀地涂在离型纸上,并使得涂敷过程中不产生气泡,水平放置一天,成膜后在干燥箱中 80℃下烘5小时,从离型纸上剥离得到薄膜。
2.根据权利要求1所述的石墨烯/镍复合物改性水性聚氨酯材料的制备方法,其特征在于所述聚酯多元醇优选聚己二酸丁二醇酯二醇(PBA)。
3.根据权利要求1所述的石墨烯/镍复合物改性水性聚氨酯材料的制备方法,其特征在于所述聚醚多元醇至少有一种选自聚氧乙烯二醇(PEG)、聚氧丙烯二醇(PPG)或聚四氢呋喃二醇(PTHF)。
4.根据权利要求1所述的石墨烯/镍复合物改性水性聚氨酯材料的制备方法,其特征在于所述二异氰酸酯至少有一种选自甲苯二异氰酸酯(TDI)、二苯基甲烷二异氰酸酯(MDI)、苯二亚甲基二异氰酸酯(XDI)、甲基环已基二异氰酸酯(HTDI)、二环已基甲烷二异氰酸酯(HMDI)、已二异氰酸酯(HDI)或异佛尔酮二异氰酸酯(IPDI)。
5.根据权利要求1所述的石墨烯/镍复合物改性水性聚氨酯材料的制备方法,其特征在于所述二异氰酸酯与聚酯多元醇或聚醚多元醇、2,2-二羟甲基丙酸(DMPA)的质量比为20~39:100: 5~9。
6.根据权利要求1所述的石墨烯/镍复合物改性水性聚氨酯材料的制备方法,其特征在于所述二异氰酸酯与石墨烯/镍复合物的质量比为180~280:1。
7.根据权利要求1-6任一所述的石墨烯/镍复合物改性水性聚氨酯材料的制备方法,其特征在于所述在预聚体中加入一定量的丁酮、2,2-二羟甲基丙酸(DMPA)和石墨烯/镍复合物,在70℃下反应3h。
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CN106046287A (zh) * | 2016-06-17 | 2016-10-26 | 杭州吉华高分子材料股份有限公司 | 一种石墨烯改性水性聚氨酯的制备方法 |
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