CN108043379A - 石墨烯/TiO2复合柔性光催化膜及其制备方法 - Google Patents
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Abstract
本发明公开了一种石墨烯/TiO2复合柔性光催化膜及其制备方法,将氧化石墨烯分散于水中得到质量浓度为0.5mg/mL的氧化石墨烯分散液,将0.003‑0.019g TiO2超声分散于10mL氧化石墨烯分散液中得到石墨烯/TiO2分散液,将石墨烯/TiO2分散液在抽滤膜上抽滤得到石墨烯/TiO2复合膜,再将得到的石墨烯/TiO2复合膜自然晾干、还原得到石墨烯/TiO2复合柔性光催化膜。本发明采用简单的抽滤法制备出易于回收利用的石墨烯/TiO2复合柔性光催化膜,该光催化膜在可见光照射下对有机污染物的降解效率较高。
Description
技术领域
本发明属于自然可见光光催化剂的合成技术领域,具体涉及一种石墨烯/TiO2复合柔性光催化膜及其制备方法。
背景技术
光催化氧化技术(photocatalytic oxidation)是一种新型的绿色高级氧化技术,可直接利用太阳光在常温常压条件下催化降解废水及空气中的有机污染物,具有工艺简单、操作方便的优点,降解彻底且无二次污染,在环保领域具有广泛的应用前景。光催化氧化技术的核心是高效光催化剂的研发。TiO2具有催化效率高、化学性质稳定、廉价无毒等优点,被认为是较为理想的光催化剂。但是TiO2的禁带宽度较大(锐钛矿型TiO2的禁带Eg=3.2eV),只能被波长较短的紫外线所激发,而这部分的紫外光仅占太阳光的3%-5%,对太阳能的利用率较低。
在光催化降解过程中,粉末类样品易流失,且光激发产生的电子-空穴对易复合,使得光催化反应的量子效率很低。如何减小TiO2的禁带宽度和电子-空穴对的复合率,提高可见光催化活性和重复利用性能有望推动TiO2光催化材料的工业化应用。研究者为此做了大量的改性研究如金属离子掺杂、贵金属沉积、半导体复合、表面光敏化等来提高TiO2的可见光催化活性。近年来的研究发现,TiO2与活性炭、碳纳米管、石墨烯等碳类材料复合能大幅提高其光催化性能。其中石墨烯因其具有优异的 导电性,容易捕获光生电子并充当电子转移的媒介,从而有效阻止了载流子的复合,是光催化材料的理想载体。此外,石墨烯内部的芳香结构可与污染物形成π-π共轭作用从而表现出对污染物强烈的吸附作用,其较高的机械强度为催化剂的沉积提供了一个二维面结构。从应用角度看,光催化剂存在诸如光催化量子效率低、吸收利用波长范围窄、粉末回收困难等问题,与实际应用之间存在着不小的差距。以环境净化技术为例,如果将石墨烯/TiO2复合光催化剂用于废水处理领域,就可能结合石墨烯膜较高载流子迁移率与TiO2高催化活性的双重优势,制备性能更加优良的光催化剂。
发明内容
本发明解决的技术问题是提供了一种易于回收利用且具有高效可见光光催化活性的石墨烯/TiO2复合柔性光催化膜及其制备方法,该方法将纳米TiO2负载于石墨烯薄膜上制备出性能优异且易于回收利用的可见光复合光催化剂。
本发明为解决上述技术问题采用如下技术方案,石墨烯/TiO2复合柔性光催化膜的制备方法,其特征在于具体步骤为:将氧化石墨烯分散于水中得到质量浓度为0.5mg/mL的氧化石墨烯分散液,将0.003-0.019g TiO2超声分散于10mL氧化石墨烯分散液中得到石墨烯/TiO2分散液,将石墨烯/TiO2分散液在抽滤膜上抽滤得到石墨烯/TiO2复合膜,再将得到的石墨烯/TiO2复合膜自然晾干、还原得到石墨烯/TiO2复合柔性光催化膜。
进一步优选,所述TiO2的质量优选为0.011-0.015g。
进一步优选,所述TiO2优选为商业P25。
本发明所述的石墨烯/TiO2复合柔性光催化膜,其特征在于是由上述方法制得的。
本发明与现有技术相比具有以下有益效果:本发明采用简单的抽滤法制备出易于回收利用的石墨烯/TiO2复合柔性光催化膜,该光催化膜在可见光照射下对有机污染物的降解效率较高,提供一种能够通过较简单制备工艺获得回收型石墨烯/TiO2复合柔性光催化膜的方法。
附图说明
图1为实施例1制得氧化石墨烯膜、石墨烯膜及实施例4制得石墨烯/TiO2复合柔性光催化膜的XRD图。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明,但不应该将此理解为本发明上述主题的范围仅限于以下的实施例,凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
采用改进的Hummers’法以石墨粉为原料制备氧化石墨烯,将氧化石墨烯分散于水中得到质量浓度为0.5mg/mL的氧化石墨烯分散液,将氧化石墨烯分散液在抽滤膜上抽滤得到氧化石墨烯膜,再将得到的氧化石墨烯膜自然晾干、还原得到柔性石墨烯光催化膜。经过紫外光照射30min对15mg/L的亚甲基蓝溶液去除率为23%,随后取出柔性石墨烯光催化膜放入10mg/L的亚甲基蓝溶液中,经过可见光照射80min对10mg/L的亚甲基蓝溶液去除率为16%。该柔性石墨烯光催化膜在光催化降解过程中受水流冲击不会有变化,机械稳定性较好,且可以直接用玻璃棒挑出转移,便于循环利用。
实施例2
采用改进的Hummers’法以石墨粉为原料制备氧化石墨烯,将氧化石墨烯分散于水中得到质量浓度为0.5mg/mL的氧化石墨烯分散液,将0.003g TiO2(商业P25)超声分散于10mL氧化石墨烯分散液中得到石墨烯/TiO2分散液,将石墨烯/TiO2分散液在抽滤膜上抽滤得到石墨烯/TiO2复合膜,再将得到的石墨烯/TiO2复合膜自然晾干、还原得到石墨烯/TiO2复合柔性光催化膜。经过紫外光照射30min对15mg/L的亚甲基蓝溶液去除率为91%,随后取出石墨烯/TiO2复合柔性光催化膜放入10mg/L的亚甲基蓝溶液中,经过可见光照射80min对10mg/L的亚甲基蓝溶液去除率为95%。该石墨烯/TiO2复合柔性光催化膜在光催化降解过程中受水流冲击不会有变化,机械稳定性较好,且可以直接用玻璃棒挑出转移,便于循环利用。
实施例3
采用改进的Hummers’法以石墨粉为原料制备氧化石墨烯,将氧化石墨烯分散于水中得到质量浓度为0.5mg/mL的氧化石墨烯分散液,将0.007g TiO2(商业P25)超声分散于10mL氧化石墨烯分散液中得到石墨烯/TiO2分散液,将石墨烯/TiO2分散液在抽滤膜上抽滤得到石墨烯/TiO2复合膜,再将得到的石墨烯/TiO2复合膜自然晾干、还原得到石墨烯/TiO2复合柔性光催化膜。经过紫外光照射30min对15mg/L的亚甲基蓝溶液去除率为95%,随后取出石墨烯/TiO2复合柔性光催化膜放入10mg/L的亚甲基蓝溶液中,经过可见光照射80min对10mg/L的亚甲基蓝溶液去除率为82%。该石墨烯/TiO2复合柔性光催化膜在光催化降解过程中受水流冲击不会有变化,机械稳定性较好,且可以直接用玻璃棒挑出转移,便于循环利用。
实施例4
采用改进的Hummers’法以石墨粉为原料制备氧化石墨烯,将氧化石墨烯分散于水中得到质量浓度为0.5mg/mL的氧化石墨烯分散液,将0.011g TiO2(商业P25)超声分散于10mL氧化石墨烯分散液中得到石墨烯/TiO2分散液,将石墨烯/TiO2分散液在抽滤膜上抽滤得到石墨烯/TiO2复合膜,再将得到的石墨烯/TiO2复合膜自然晾干、还原得到石墨烯/TiO2复合柔性光催化膜。经过紫外光照射30min对15mg/L的亚甲基蓝溶液去除率为96%,随后取出石墨烯/TiO2复合柔性光催化膜放入10mg/L的亚甲基蓝溶液中,经过可见光照射80min对10mg/L的亚甲基蓝溶液去除率为96%。该石墨烯/TiO2复合柔性光催化膜在光催化降解过程中受水流冲击不会有变化,机械稳定性较好,且可以直接用玻璃棒挑出转移,便于循环利用。
实施例5
采用改进的Hummers’法以石墨粉为原料制备氧化石墨烯,将氧化石墨烯分散于水中得到质量浓度为0.5mg/mL的氧化石墨烯分散液,将0.015g TiO2(商业P25)超声分散于10mL氧化石墨烯分散液中得到石墨烯/TiO2分散液,将石墨烯/TiO2分散液在抽滤膜上抽滤得到石墨烯/TiO2复合膜,再将得到的石墨烯/TiO2复合膜自然晾干、还原得到石墨烯/TiO2复合柔性光催化膜。经过紫外光照射30min对15mg/L的亚甲基蓝溶液去除率为96%,随后取出石墨烯/TiO2复合柔性光催化膜放入10mg/L的亚甲基蓝溶液中,经过可见光照射80min对10mg/L的亚甲基蓝溶液去除率为98%。该石墨烯/TiO2复合柔性光催化膜在光催化降解过程中受水流冲击不会有变化,机械稳定性较好,且可以直接用玻璃棒挑出转移,便于循环利用。
实施例6
采用改进的Hummers’法以石墨粉为原料制备氧化石墨烯,将氧化石墨烯分散于水中得到质量浓度为0.5mg/mL的氧化石墨烯分散液,将0.019g TiO2(商业P25)超声分散于10mL氧化石墨烯分散液中得到石墨烯/TiO2分散液,将石墨烯/TiO2分散液在抽滤膜上抽滤得到石墨烯/TiO2复合膜,再将得到的石墨烯/TiO2复合膜自然晾干、还原得到石墨烯/TiO2复合柔性光催化膜。经过紫外光照射30min对15mg/L的亚甲基蓝溶液去除率为91%,随后取出石墨烯/TiO2复合柔性光催化膜放入10mg/L的亚甲基蓝溶液中,经过可见光照射80min对10mg/L的亚甲基蓝溶液去除率为94%。该石墨烯/TiO2复合柔性光催化膜在光催化降解过程中受水流冲击不会有变化,机械稳定性较好,且可以直接用玻璃棒挑出转移,便于循环利用。
基于以上实施例选取添加0.011g TiO2(商业P25)制备的石墨烯/TiO2复合柔性光催化膜进一步研究其稳定性,经过5次循环降解实验,光催化活性无明显降低,且整体完整性良好,表明制得的石墨烯/TiO2复合柔性光催化膜具有较好的可见光催化活性,且回收利用性能好,有望用于实际废水的处理。
以上实施例描述了本发明的基本原理、主要特征及优点,本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明原理的范围下,本发明还会有各种变化和改进,这些变化和改进均落入本发明保护的范围内。
Claims (4)
1. 石墨烯/TiO2复合柔性光催化膜的制备方法,其特征在于具体步骤为:将氧化石墨烯分散于水中得到质量浓度为0.5mg/mL的氧化石墨烯分散液,将0.003-0.019g TiO2超声分散于10mL氧化石墨烯分散液中得到石墨烯/TiO2分散液,将石墨烯/TiO2分散液在抽滤膜上抽滤得到石墨烯/TiO2复合膜,再将得到的石墨烯/TiO2复合膜自然晾干、还原得到石墨烯/TiO2复合柔性光催化膜。
2.根据权利要求1所述的石墨烯/TiO2复合柔性光催化膜的制备方法,其特征在于:所述TiO2的质量优选为0.011-0.015g。
3.根据权利要求1所述的石墨烯/TiO2复合柔性光催化膜的制备方法,其特征在于:所述TiO2优选为商业P25。
4.石墨烯/TiO2复合柔性光催化膜,其特征在于是由权利要求1-3中任意一项所述的方法制得的。
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