CN108043457A - 高导电性石墨烯-曙红y复合气凝胶光催化剂的制备方法 - Google Patents
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Abstract
本发明公开了一种高导电性石墨烯‑曙红Y复合气凝胶光催化剂的制备方法。本发明在氧化石墨烯与曙红Y溶液中加入一定量的高导电性的Elicarb石墨烯，再经水热处理，冷冻干燥，即可得到高导电性的石墨烯‑曙红Y复合气凝胶光催化剂。在可见光光照下，高导电性的石墨烯‑曙红Y复合气凝胶在液相光催化还原硝基苯和Cr(VI)中体现更为优异的光催化活性；本发明操作简单有效，对制备更加高效的石墨烯气凝胶复合光催化剂具有广阔的实用价值和应用前景。
Description
技术领域
本发明属于材料技术领域，具体涉及一种高导电性石墨烯-曙红Y复合气凝胶光催化剂的制备方法。
背景技术
环境污染和能源短缺问题的日益加剧，极大的威胁着人类社会的可持续发展。染料敏化光催化技术由于其具有不产生二次污染、成本低、能耗少、反应条件温和、操作简易等优点已经成为近年来人们研究的热点。然而，至今为止，染料敏化光催化体系的效率依旧较低。此外，较低的光催化稳定性和在循环过程中催化剂的大量损失也严重影响了其在实际中的应用。三维石墨烯气凝胶凭借其独特的结构优势，大的比表面积，易回收重复利用等优势吸引了极大的关注。
然而，现阶段合成的三维石墨烯气凝胶都是以氧化石墨烯为前驱物制备而得到的。这种方法制备的石墨烯气凝胶不可避免地会残留含氧官能团和大量的结构缺陷，这极大地破坏了石墨烯二维π-共轭电子结构，降低了石墨烯的导电性，进而影响了石墨烯基复合光催化材料的光催化性能。因此为了充分有效地利用石墨烯，提高石墨烯的导电性变得十分必要。因此，发明一种高导电性的石墨烯气凝胶复合光催化材料十分必要。
发明内容
本发明的目的在于针对现阶段制备得到的石墨烯气凝胶复合光催化材料导电性较低等缺陷，提供一种高导电性的石墨烯-曙红Y复合气凝胶光催化剂的制备方法及其应用。本方面制备的石墨烯-曙红Y复合气凝胶光催化剂具有更高的导电性，其在可见光下液相降解还原对硝基苯和降解Cr(VI)体现出更优异的光催化活性。
为实现上述目的，本发明采用如下技术方案：将Elicarb石墨烯添加到氧化石墨烯分散液中，随后加入曙红Y混合搅拌均匀，然后通过水热还原，冷冻干燥，即可得到高导电性的石墨烯-曙红Y复合气凝胶光催化剂；具体步骤如下：
（1）氧化石墨烯（GO）的制备：
将P2O5和K2S2O8按1:1的质量比混合均匀，缓慢加入12 mL 98％浓H2SO4，加热到80 ℃，再加入石墨粉，恒温24 h；室温冷却，用水稀释后搅拌，然后静止；抽滤，得滤渣；所得滤渣干燥后溶于120 mL 98％浓H2SO4中，磁力搅拌下缓慢加入15 g KMnO4，并控制反应液的温度低于20 ℃，然后在35 ℃～40 ℃下搅拌反应2 h；边搅拌边缓慢加入250 mL水进行稀释并控制反应液的温度低于50 ℃；再加入1 L去离子水和20 mL 30％H2O2（逐滴加入），继续搅拌，放置过夜；过滤，滤渣用1:10盐酸:去离子水洗涤，离心分离，渗析洗涤，收集固体，干燥，然后最终获得的氧化石墨重新超声分散到去离子水里，获得氧化石墨烯分散液；
（2）高导电性石墨烯-曙红Y复合气凝胶光催化剂的制备：
将一定质量（2~4 mg）Elicarb石墨烯加入到步骤（1）超声分散好的10 mL氧化石墨烯分散液中(浓度为3 mg/mL)，后加入2mg的曙红Y混合搅拌均匀，接着180 ℃水热12 h，而后冷却、洗涤、真空冷冻干燥得到高导电性的石墨烯-曙红Y复合气凝胶光催化剂。
一种如上所述高导电性的石墨烯-曙红Y复合气凝胶光催化剂在波长>420 nm的可见光下照射40 min，光催化还原对硝基苯胺和Cr (VI)，具体步骤如下：
（1）取一定量的去离子水、高导电性的石墨烯-曙红Y复合气凝胶光催化剂、对硝基苯胺以及三乙醇胺于反应瓶中，并通入氮气(60 mL/min)，在黑暗状态下吸附一定时间，对硝基苯胺在光催化剂表面达到吸附平衡；在氮气保护下，对上述体系进行光照，每隔一定时间后取适量液体，反应结束后，采用紫外可见吸收光谱对所取液体进行分析；
（2）取一定量的去离子水、高导电性的石墨烯-曙红Y复合气凝胶光催化剂、Cr (VI)溶液以及三乙醇胺于反应瓶中，并通入氮气(60 mL/min)，在黑暗状态下吸附一定时间，对硝基苯胺在光催化剂表面达到吸附平衡；在氮气保护下，对上述体系进行光照，每隔一定时间后取适量液体，反应结束后，采用紫外可见吸收光谱对所取液体进行分析。
本发明的显著优点在于：
（1）本发明通过在氧化石墨烯与曙红Y溶液中加入少量的Elicarb石墨烯即可实现提高石墨烯气凝胶曙红Y复合光催化剂的导电性，该方法实验操作简单，具有广泛的应用前景；
（2）高导电性的石墨烯-曙红Y气凝胶光催化性能更为优异，且其具有制备成本低、生产工艺简单、环境友好、易回收且可循环使用等优点。
附图说明
图1是实施例3制得的4EGR-EY复合气凝胶光催化剂的SEM图和实物照片；
图2是实施例3制得的4EGR-EY复合气凝胶光催化剂的XPS图；
图3是石墨烯-曙红Y复合气凝胶光催化剂的XRD图；
图4是石墨烯气凝胶-曙红Y复合气凝胶光催化剂可见光还原对硝基苯胺（A）和Cr (VI)（B）的活性测试图；
图5是对比例制得的GR-EY和实施例3制得的4EGR-EY复合气凝胶光催化剂的电阻值测试值。
具体实施方式
本发明用下列实施例来进一步说明本发明的内容，但本发明的保护范围并不限于下列实施例。
将P2O5和K2S2O8按1:1的质量比混合均匀，缓慢加入12 mL 98％浓H2SO4，加热到80℃，再加入石墨粉，恒温24 h；室温冷却，用水稀释后搅拌，然后静止；抽滤，得滤渣；所得滤渣干燥后溶于120 mL 98％浓H2SO4中，磁力搅拌下缓慢加入15 g KMnO4，并控制反应液的温度低于20 ℃，然后在35 ℃～40 ℃下搅拌反应2 h；边搅拌边缓慢加入250 mL水进行稀释并控制反应液的温度低于50 ℃；再加入1 L去离子水和20 mL 30％H2O2（逐滴加入），继续搅拌，放置过夜。过滤，滤渣用1:10盐酸:去离子水洗涤，离心分离，渗析洗涤，收集固体，干燥，然后最终获得氧化石墨重新超声分散到去离子水里，获得氧化石墨烯分散液。
对比例
在10mL氧化石墨烯分散液中(浓度为3 mg/mL)加入2 mg的曙红Y（EY），且超声混合搅拌均匀，接着180 ℃水热12 h，而后冷却、洗涤、真空冷冻干燥得到石墨烯-曙红Y复合气凝胶（GR-EY气凝胶）光催化剂。
实施例1
将2 mg的Elicarb石墨烯（EGR）加入到10 mL氧化石墨烯分散液中(浓度为3 mg/mL)，后加入2 mg的曙红Y（EY），且超声混合搅拌均匀，接着180 ℃水热12 h，而后冷却、洗涤、真空冷冻干燥得到高导电性的石墨烯-曙红Y复合气凝胶（2EGR-EY气凝胶）光催化剂。
实施例2
将3 mg的Elicarb石墨烯（EGR）加入到10 mL氧化石墨烯分散液中(浓度为3 mg/mL)，后加入2 mg的曙红Y（EY），且超声混合搅拌均匀，接着180 ℃水热12 h，而后冷却、洗涤、真空冷冻干燥得到高导电性的石墨烯-曙红Y复合气凝胶（3EGR-EY气凝胶）光催化剂。
实施例3
将4 mg的Elicarb石墨烯（EGR）加入到10 mL氧化石墨烯分散液中(浓度为3 mg/mL)，后加入2 mg的曙红Y（EY），且超声混合搅拌均匀，接着180 ℃水热12 h，而后冷却、洗涤、真空冷冻干燥得到高导电性的石墨烯-曙红Y复合气凝胶（4EGR-EY气凝胶）光催化剂。
应用例1
将GR-EY气凝胶、2EGR-EY气凝胶、3EGR-EY气凝胶、4EGR-EY气凝胶光催化剂分别添加到4组完全相同的60 ml 10 ppm的对硝基苯胺溶液中，随后分别添加60 μL三乙醇胺，并通入氮气(60 mL/min)，室温暗吸附1 h后，置于可见光(>420 nm)下，每隔10 min取出3 mL样品溶液，光照40 min之后关闭氙灯光源，将所取的溶液离心处理，所得到的上层清液进一步转移到石英比色皿中，在紫外-可见分光光度计上测定不同光催化时间下的吸光度，从而得到各个时间段下催化剂在可见光照射下光催化还原对硝基苯胺溶液的曲线图（图3）。
应用例2
将GR-EY气凝胶、2EGR-EY气凝胶、3EGR-EY气凝胶、4EGR-EY气凝胶光催化剂分别添加到4组完全相同的60 ml 10 ppm 的Cr (VI)溶液中，随后分别添加60 μL三乙醇胺，并通入氮气(60 mL/min)，室温暗吸附1 h后，置于可见光(>420 nm)下光照40 min，每隔10 min后取适量液体，反应结束后，采用紫外可见吸收光谱对所取液体进行分析（结果如图4）。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。
Claims (6)
1.一种高导电性石墨烯-曙红Y复合气凝胶光催化剂的制备方法，其特征在于：包括以下步骤：
（1）将氧化石墨烯溶于去离子水中超声分散，得到氧化石墨烯分散液；
（2）将Elicarb石墨烯加入到步骤（1）得到的氧化石墨烯分散液中，随后加入曙红Y混合搅拌均匀，接着水热处理，而后冷却、洗涤和真空冷冻干燥得到所述石墨烯-曙红Y气凝胶复合光催化剂。
2.根据权利要求1所述的高导电性石墨烯-曙红Y复合气凝胶光催化剂的制备方法，其特征在于：步骤（2）中，Elicarb石墨烯的添加量为2~4 mg，曙红Y的添加量为2 mg，氧化石墨烯分散液的体积为10 mL。
3.根据权利要求1所述的高导电性石墨烯-曙红Y复合气凝胶光催化剂的制备方法，其特征在于：所述氧化石墨烯分散液的浓度为3 mg/mL。
4.根据权利要求1所述的高导电性石墨烯-曙红Y复合气凝胶光催化剂的制备方法，其特征在于：水热处理的工艺参数为：水热温度为180 ℃，水热时间为12 h。
5.一种如权利要求1~4中任一项所述的制备方法制得的高导电性石墨烯-曙红Y复合气凝胶光催化剂的应用，其特征在于：所述高导电性石墨烯-曙红Y复合气凝胶光催化剂用于液相可见光光催化还原对硝基苯胺。
6.一种如权利要求1~4中任一项所述的制备方法制得的高导电性石墨烯-曙红Y复合气凝胶光催化剂的应用，其特征在于：所述高导电性石墨烯-曙红Y复合气凝胶光催化剂用于液相可见光光催化还原去除污染物Cr (VI)。
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| CN110261450A (zh) * | 2019-05-20 | 2019-09-20 | 安徽科技学院 | 一种同时检测多巴胺和肾上腺素修饰玻碳电极、制备方法及应用 |
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| CN104437453A (zh) * | 2014-11-28 | 2015-03-25 | 浙江大学 | 一种碳气凝胶催化剂及其制备方法和用途 |
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| CN110261450A (zh) * | 2019-05-20 | 2019-09-20 | 安徽科技学院 | 一种同时检测多巴胺和肾上腺素修饰玻碳电极、制备方法及应用 |
| CN110261450B (zh) * | 2019-05-20 | 2021-11-30 | 安徽科技学院 | 一种同时检测多巴胺和肾上腺素修饰玻碳电极、制备方法及应用 |
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