CN109575363A - 一种2MgO·B2O3·H2O/RGO纳米复合阻燃剂 - Google Patents
一种2MgO·B2O3·H2O/RGO纳米复合阻燃剂 Download PDFInfo
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Abstract
本发明公开了一种2MgO·B2O3·H2O/RGO纳米复合阻燃剂,该复合阻燃剂是在还原氧化石墨烯(RGO)表面负载2MgO·B2O3·H2O纳米带,RGO的质量含量为5%~20%。本发明通过在水热法制备2MgO·B2O3·H2O纳米带的过程中添加GO,原位反应制备出了RGO负载2MgO·B2O3·H2O纳米带的纳米复合阻燃剂,制备方法简单,成本低廉,所制备的2MgO·B2O3·H2O/RGO纳米复合阻燃材料分散性好、粒径小,且具有较好的阻燃效果和力学性能,具有潜在的应用前景。
Description
技术领域
本发明属于阻燃技术领域,具体涉及一种阻燃和力学性能优良的2MgO·B2O3·H2O/RGO纳米复合阻燃材料。
背景技术
随着重大火灾次数的增多以及塑料焚烧造成的二次污染等问题的出现,阻燃剂的应用受到了广泛的关注。硼酸镁是一种新型高效无机阻燃剂,它具有热稳定性高、粒度细、体积质量小、易分散、无毒等显著特点,既能阻燃又能抑烟,并能消灭电弧,因此有着良好的市场前景,被广泛应用于各种纤维、树脂、橡胶制品、电器绝缘材料、电线、电缆、防锈漆等方面的阻燃。然而,硼酸镁相对大的粒径在基质中很难分散,限制了其在工业上的应用;由于纳米材料的形貌和尺寸对其阻燃性能有很大影响,对于等量的阻燃剂,其粒径愈小比表面积愈大,超细化、纳米化以后,增强了界面的相互作用,可以更均匀的分散于基质中,阻燃效果就愈好。
所以,开展硼酸镁纳米材料及其复合阻燃剂的制备和阻燃性能研究具有重要现实意义。发明人在研发过程中发现有关水合硼酸镁纳米结构的制备报道极少,虽然WanchengZhu等人提出采用水热法制备花状、纤维状纳米2MgO·B2O3·H2O,但是没有进行阻燃试验。本课题组最近报道了2MgO·B2O3·1.5H2O纳米短棒阻燃材料以及2MgO·B2O3·1.5H2O/Mg(OH)2纳米复合材料,其阻燃性能相比单一阻燃材料有了较大提升。
石墨烯(GO)作为一种高强度碳材料,由于其热稳定性高、阻隔性强、比表面吸附能力大等优点,有效地减少了传热传质,作为阻燃剂受到越来越多的关注。但是单一填充GO在聚合物中分散性并不好,其炭层不能有效形成防火体系,这说明GO的阻燃性能有待提高。为了解决这个问题,人们通常用GO作为佐剂结合其他传统无机阻燃剂如偏硼酸钠、羟基锡酸锌和硼酸锌,所有这些可以有效地提高GO在聚合物基质中的分散性和阻燃性能,而且有效地降低了填料的总体含量。本课题组大量阻燃实验表明,即使添加碱土金属硼酸盐纳米阻燃材料到聚丙烯基材中,虽然阻燃效果有了较大提高,但是材料的力学性能明显降低,仍然限制了其应用。
发明内容
本发明的目的是提供一种粒径小、分散性好、阻燃性能和力学性能优良的2MgO·B2O3·H2O/RGO纳米复合阻燃剂。
针对上述目的,本发明所采用的2MgO·B2O3·H2O/RGO纳米复合阻燃剂是表面负载2MgO·B2O3·H2O纳米带的还原氧化石墨烯,它由下述方法制备得到:
将Mg(NO3)2·6H2O、H3BO3、NaOH和石墨烯加入去离子水中,超声分散均匀,在180~260℃下水热反应12~36小时,自然冷却至室温,所得产物经抽滤、洗涤、干燥,得到2MgO·B2O3·H2O/RGO纳米复合阻燃剂。
上述Mg(NO3)2·6H2O与H3BO3、NaOH的摩尔比为1:1~4:1~5,优选Mg(NO3)2·6H2O与H3BO3、NaOH的摩尔比为1:1.5~3:2~4。
上述Mg(NO3)2·6H2O与石墨烯的质量比为1:0.003~0.1,优选Mg(NO3)2·6H2O与石墨烯的质量比为1:0.01~0.05。
上述制备方法中,进一步优选在200~240℃下水热反应18~26小时。
本发明的2MgO·B2O3·H2O/RGO纳米复合阻燃剂中,2MgO·B2O3·H2O纳米带的厚度5~15nm、宽度为30~50nm。
本发明的有益效果如下:
1、本发明考虑到石墨烯的高强度特点结合其可以作为阻燃剂,采用原位水热反应方法,制备了首例碱土金属硼酸盐2MgO·B2O3·H2O/RGO纳米复合材料。所制备的2MgO·B2O3·H2O/RGO纳米复合阻燃材料分散性好、粒径小,不但提高了阻燃性能,而且2MgO·B2O3·H2O/RGO纳米复合阻燃剂与单一2MgO·B2O3·H2O纳米带相比,抗拉强度增大,力学性能显著提高。结果表明添加10%2MgO·B2O3·H2O/RGO纳米复合材料的聚丙烯的阻燃性能比单一组分的强,表现出协同阻燃作用,特别是其保持了与聚丙烯接近的力学性能,很好地抵消了如果只添加2MgO·B2O3·H2O纳米带导致的材料力学性能的恶化。
2、本发明纳米复合阻燃剂的制备方法简单,成本低廉,且具有较好的阻燃效果和优良的力学性能,在阻燃领域具有广阔的应用前景。
附图说明
图1是实施例1制备的样品的X射线粉末衍射谱。
图2是实施例1制备的样品的EDS能谱图。
图3是实施例1制备的样品的SEM图。
图4是实施例1制备的样品的TEM图。
图5是2MgO·B2O3·H2O纳米带(曲线a)、RGO(曲线b)及2MgO·B2O3·H2O/RGO纳米复合阻燃剂(曲线c)的热重分析图。
图6是实施例2制备的样品的X射线粉末衍射谱。
图7是实施例2制备的样品的SEM图。
图8是实施例3制备的样品的X射线粉末衍射谱。
图9是实施例3制备的样品的SEM图。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明,但本发明的保护范围不仅限于这些实施例。
实施例1
将3.71g(14mmol)Mg(NO3)2·6H2O、1.73g(28mmol)H3BO3、1.60g(40mmol)NaOH和0.1g GO加入10mL去离子水中,用超声清洗器在功率为100W、频率为60kHz下室温超声分散30分钟,然后转入容积为50mL的聚四氟乙烯内衬的不锈钢反应釜内,将反应釜置于烘箱中240℃保温24小时,将反应釜取出,在空气中自然冷却至室温,所得产物经抽滤、80℃的二次蒸馏水及无水乙醇洗涤、60℃干燥12小时,得到2MgO·B2O3·H2O/RGO纳米复合阻燃剂。
发明人采用X射线衍射仪、扫描电镜及透射电镜分别对实施例1所得样品进行结构和形貌表征,结果见图1~4。由图1可见,样品的XRD图谱含有2MgO·B2O3·H2O和RGO的衍射峰;从图2的EDS能谱可以看出,样品中含有B、C、O、Mg四种元素,所以样品可以被指认为2MgO·B2O3·H2O与RGO复合物;从图3、4中可以看出,2MgO·B2O3·H2O纳米带(宽度约35nm)因具有吸附作用而原位沉积在RGO表面。
对比例1
在实施例1中,不添加GO,其他步骤与实施例1相同,得到2MgO·B2O3·H2O纳米带。
发明人采用热重分析仪对RGO、对比例1制备的2MgO·B2O3·H2O纳米带、实施例1制备的2MgO·B2O3·H2O/RGO纳米复合阻燃剂进行热重分析,结果见图5。可以计算出RGO在实施例1制备的2MgO·B2O3·H2O/RGO纳米复合阻燃剂中的质量分数约为8.18%,2MgO·B2O3·H2O所占质量分数约为91.82%。
实施例2
将3.71g(14mmol)Mg(NO3)2·6H2O、1.73g(28mmol)H3BO3、1.60g(40mmol)NaOH和0.1g GO加入10mL去离子水中,用超声清洗器在功率为100W、频率为60kHz下室温超声分散30分钟,然后转入容积为50mL的聚四氟乙烯内衬的不锈钢反应釜内,将反应釜置于烘箱中200℃保温18小时,将反应釜取出,在空气中自然冷却至室温,所得产物经抽滤、80℃的二次蒸馏水及无水乙醇洗涤、60℃干燥12小时,得到2MgO·B2O3·H2O/RGO纳米复合阻燃剂。由图6和图7可见,所得样品可以被指认为2MgO·B2O3·H2O与RGO的复合物。
实施例3
将3.71g(14mmol)Mg(NO3)2·6H2O、1.20g(19mmol)H3BO3、0.95g(24mmol)NaOH和0.2g GO加入10mL去离子水中,用超声清洗器在功率为100W、频率为60kHz下室温超声分散30分钟,然后转入容积为50mL的聚四氟乙烯内衬的不锈钢反应釜内,将反应釜置于烘箱中240℃保温24小时,将反应釜取出,在空气中自然冷却至室温,所得产物经抽滤、80℃的二次蒸馏水及无水乙醇洗涤、60℃干燥12小时,得到2MgO·B2O3·H2O/RGO纳米复合阻燃剂。由图8和图9可见,所得样品可以被指认为2MgO·B2O3·H2O与RGO的复合物。
为了证明本发明的有益效果,发明人以聚丙烯(PP)为研究对象,分别向PP中添加10%(PP的质量分数为90%)实施例1制备的2MgO·B2O3·H2O/RGO纳米复合阻燃剂、2MgO·B2O3·H2O纳米带以及RGO,然后采用JF-3氧指数测定仪(南京炯雷仪器设备有限公司提供)和万能材料试验机(RGT-10)分别进行了阻燃性能和力学性能的测试,结果见表1。
表1不同阻燃剂的氧指数值和拉伸性能
由表1可见,聚丙烯中添加RGO,在不改变聚丙烯力学性能的同时也能提高样品的阻燃性能,但样品的阻燃性能提高不是很明显;在聚丙烯中添加2MgO·B2O3·H2O纳米带虽能明显提高样品的阻燃性能,但是样品的力学性能确显著降低;而添加本发明实施例1制备的2MgO·B2O3·H2O/RGO纳米复合阻燃剂,不但提高了样品的阻燃性能,而且样品的抗拉强度增大,力学性能显著提高,与纯的聚丙烯材料的力学性几乎接近。
Claims (5)
1.一种2MgO·B2O3·H2O/RGO纳米复合阻燃剂,其特征在于:该复合阻燃剂是表面负载2MgO·B2O3·H2O纳米带的还原氧化石墨烯,它由下述方法制备得到:
将Mg(NO3)2·6H2O、H3BO3、NaOH和石墨烯加入去离子水中,超声分散均匀,在180~260℃下水热反应12~36小时,自然冷却至室温,所得产物经抽滤、洗涤、干燥,得到2MgO·B2O3·H2O/RGO纳米复合阻燃剂;
上述Mg(NO3)2·6H2O与H3BO3、NaOH的摩尔比为1:1~4:1~5;所述Mg(NO3)2·6H2O与石墨烯的质量比为1:0.003~0.1。
2.根据权利要求1所述的2MgO·B2O3·H2O/RGO纳米复合阻燃剂,其特征在于:所述的Mg(NO3)2·6H2O与H3BO3、NaOH的摩尔比为1:1.5~3:2~4。
3.根据权利要求1所述的2MgO·B2O3·H2O/RGO纳米复合阻燃剂,其特征在于:所述的Mg(NO3)2·6H2O与石墨烯的质量比为1:0.01~0.05。
4.根据权利要求1~3任意一项所述的2MgO·B2O3·H2O/RGO纳米复合阻燃剂,其特征在于:在200~240℃下水热反应18~26小时。
5.根据权利要求1所述的2MgO·B2O3·H2O/RGO纳米复合阻燃剂,其特征在于:所述2MgO·B2O3·H2O纳米带的厚度5~15nm、宽度为30~50nm。
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