CN105772096A - 一种应用于太阳光催化的纳米复合材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种全光谱吸收可以应用于太阳光催化的纳米复合材料及其制备方法，该复合材料具有较高的催化效率。本发明采用正负电吸附的方法，将带正电的两亲高分子与带负电的氧化石墨烯通过静电作用结合，得到两亲的GO/polymer复合物，并通过超声乳化的方法，利用复合物将疏水的Cu7S4纳米晶包覆，得到Cu7S4@GO纳米复合材料，即为应用于太阳光催化的纳米复合材料。其中含有3‑5mg Cu7S4的纳米复合材料在模拟太阳光1W/cm2的照射下，光催化效果高达94.7％，具有较高的应用前景。
Description
技术领域
本发明属于纳米材料制备技术领域，特别涉及一种全光谱吸收具有较高光催化效率的Cu7S4@GO纳米复合物，可以应用于太阳光催化降解有机物。
技术背景
由于半导体是一个可以将太阳光能转化为化学能的高效的光催化剂，因此，半导体光催化剂材料的设计、合成及应用引起了广泛的关注。人们探索了大量的半导体。例如常用的N型半导体TiO2，由于具有较大的带隙，只能吸收占有整个太阳光5％的紫外光。再者α-Fe2O3虽是有相对较小的带隙可以利用可见光，但是传递电子的能力较差。而具有不错电子传递性能的Si、GaN等具有较弱的催化能力。
光催化剂的首要条件就是能够产生电子空穴对以及有较好的电子传递介质，阻止电子和空穴的快速结合。因此，需要理性的设计光催剂的结构以及组成。由于很好的设计和控制金属与碳材料的界面并且石墨烯及其衍生物氧化石墨烯，具有较好的导电性和机械性，这使得石墨烯类物质称为很好的电子传递桥梁。因此，发展可以产生电子空穴对的半导体和可以传递电子的石墨烯的纳米复合结构，是太阳光直接利用与催化领域的重要需求。
发明内容
本发明为满足太阳能转化为化学能需求，特别设计一种全光谱吸收具有比较高光转换效率的Cu7S4纳米复合材料，可以应用于光催化。
本发明采用正负电吸附的方法，将带正电的高分子与带负电的氧化石墨烯通过静电作用结合，得到两亲的GO/polymer复合物，并通过超声乳化的方法，利用复合物将疏水的Cu7S4纳米晶包覆，得到Cu7S4@GO纳米复合材料，即为应用于太阳光催化的纳米复合材料。
本发明所述的一种应用于太阳光催化的纳米复合材料的制备方法，其具体步骤如下：
a.将10-30mg带正电的两亲高分子分散在1-5mL氯仿中，然后加入到3-8mL的DMSO中，混匀；随后加入浓度为3-8mg/mL的氧化石墨烯溶液，其中氧化石墨烯加入量为10-20mg，摇晃振荡混合均匀；
b.向步骤a的混合液中加入乙醇沉淀并离心，沉淀用0.5-2mL氯仿分散得到功能化的高分子-氧化石墨烯复合物分散液；
c.将有机相分散的Cu7S4纳米颗粒加入到步骤b得到的分散液中，Cu7S4纳米颗粒含量为2-10mg，然后转入10mL的0.3-1mM的NaOH溶液中，在功率为100-500W的超声下得到稳定乳液；
d.30-60℃下搅拌蒸掉步骤c的乳液中的有机溶剂，5000-15000转/分离心5-20min得到应用于太阳光催化的纳米复合材料，最后将其重新分散到去离子水中。
所述的带正电的两亲高分子为聚苯乙烯-甲基丙烯酸-丙烯基甲基氯代咪唑，其中丙烯基甲基氯代咪唑质量含量为5-8％，甲基丙烯酸质量含量为2-5％。
所述的带正电的两亲高分子为聚苯乙烯-甲基丙烯酸-丙烯酰胺，其中甲基丙烯酸质量含量为2-5％，丙烯酰胺质量含量为5-8％。
所述的带正电的两亲高分子分子量范围为5000-10000。
将上述制备得到的纳米复合材料在太阳光条件下催化降解有机物的应用。
本发明的有益效果：本发明制备了一种全光谱吸收可以应用于太阳光催化的纳米复合材料，该复合材料具有较高的催化效率。其中含有3-5mg Cu7S4的纳米复合材料在模拟太阳光1W/cm2的照射下，光催化效果高达94.7％，具有较高的应用前景。
附图说明
图1：实施例1制备的应用于太阳光催化的纳米复合材料的电镜图。
图2：实施例1制备的应用于太阳光催化的纳米复合材料与带正电的两亲高分子聚苯乙烯-甲基丙烯酸-丙烯基甲基氯代咪唑光催化降解罗丹明B的降解曲线对比图。
具体实施方式
实施例1
a.将10mg聚苯乙烯-甲基丙烯酸-丙烯基甲基氯代咪唑(分子量6000，丙烯基甲基氯代咪唑质量含量为5％，甲基丙烯酸质量含量为5％)分散在1mL氯仿中，然后加入到3mL的DMSO中，混匀；随后加入浓度为5mg/mL的氧化石墨烯溶液，其中氧化石墨烯加入量为20mg，摇晃振荡1分钟；
b.向步骤a的混合液中加入乙醇沉淀并离心，沉淀用0.6mL氯仿分散得到功能化的高分子-氧化石墨烯复合物分散液；
c.将0.4mL的氯仿分散的Cu7S4纳米颗粒加入到步骤b得到的分散液中，Cu7S4纳米颗粒含量为3.2mg，然后转入10mL的1mM的NaOH溶液中，在功率为300W的超声下得到稳定乳液；
d.50℃下搅拌蒸掉步骤c的乳液中的氯仿，7000转/分离心10min得到应用于太阳光催化的纳米复合材料，最后将其重新分散到去离子水中。
将上述制备的应用于太阳光催化的纳米复合材料进行光催化降解罗丹明B，反应条件：光功率密度为1W/cm2，纳米复合材料浓度为7.5mg/mL，罗丹明B浓度为10ppm，降解总体积为2mL。
以不加纳米复合材料光降解罗丹明B溶液为对比，结果如图2所示。
Claims (4)
1.一种应用于太阳光催化的纳米复合材料的制备方法，其特征在于，其具体步骤如下：
a.将10-30mg带正电的两亲高分子分散在1-5mL氯仿中，然后加入到3-8mL的DMSO中，混匀；随后加入浓度为3-8mg/mL的氧化石墨烯溶液，其中氧化石墨烯加入量为10-20mg，摇晃振荡混合均匀；
b.向步骤a的混合液中加入乙醇沉淀并离心，沉淀用0.5-2mL氯仿分散得到功能化的高分子-氧化石墨烯复合物分散液；
c.将有机相分散的Cu7S4纳米颗粒加入到步骤b得到的分散液中，Cu7S4纳米颗粒含量为2-10mg，然后转入10mL的0.3-1mM的NaOH溶液中，在功率为100-500W的超声下得到稳定乳液；
d.30-60℃下搅拌蒸掉步骤c的乳液中的有机溶剂，5000-15000转/分离心5-20min得到应用于太阳光催化的纳米复合材料，最后将其重新分散到去离子水中。
2.根据权利要求1所述的制备方法，其特征在于，所述的带正电的两亲高分子为聚苯乙烯-甲基丙烯酸-丙烯基甲基氯代咪唑，其中丙烯基甲基氯代咪唑质量含量为5-8％，甲基丙烯酸质量含量为2-5％。
3.根据权利要求1所述的制备方法，其特征在于，所述的带正电的两亲高分子为聚苯乙烯-甲基丙烯酸-丙烯酰胺，其中甲基丙烯酸质量含量为2-5％，丙烯酰胺质量含量为5-8％。
4.根据权利要求1-3任一所述的方法制备得到的纳米复合材料在太阳光条件下催化降解有机物的应用。
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| WO2010061212A1 (en) * | 2008-11-25 | 2010-06-03 | Johnson Matthey Plc | Reduced copper sulphide sorbent for removing heavy metals |
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