CN110124733A - 一种共轭聚合物光催化剂及制备方法和应用 - Google Patents
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Abstract
本发明涉及光催化剂，特指一种可见光下分解水产氢的共轭聚合物光催化剂。首先将尿素在120‑160℃下加热融化，随后加入三聚氰胺甲醛树脂，搅拌形成均一的混合溶液，冷却至室温后研磨，以3‑5℃/min的升温速率升温到550‑750℃，并在550‑750℃下煅烧2‑4h，得到多孔氮化碳基共轭聚合物光催化剂；并将制备好的多孔氮化碳基共轭聚合物光催化剂应用于可见光下分解水产氢性能研究。
Description
技术领域
本发明涉及光催化剂，特指一种可见光下分解水产氢的共轭聚合物光催化剂，利用简单的一步煅烧法合成了多孔氮化碳(g-C3N4)基共轭聚合物，并将制备好的多孔氮化碳基共轭聚合物应用于可见光下分解水产氢性能研究。
背景技术
氢能作为一种“零污染、零碳、能量高、环境友好、全能(既可发电、供热，也可用作交通燃料等)”的可持续清洁能源之一在全球能源分配中扮演着重要角色。世界氢能委员会认为,发展氢能对于实现能源转型、遏制全球气候变暖至关重要，同时可以利用氢能来转换和存储超过500太瓦时的电力，从而充分发挥可再生能源的替代作用，也可以作为发电的备用能源和战略储备能源。据预测，到 2040年氢能将占世界终端能源消费的18％，到2050年全球20％的CO2减排要靠氢能来完成。因此积极推进氢能源快速发展已成为世界各国所面临和亟待解决的重大课题。然而，传统工业上采用的裂解化石能源制氢、电解水制氢和生物制氢技术存在耗能高、污染大、效率低等缺点，极大地限制了氢能源的快速发展。光催化分解水制氢技术作为一种廉价、节能、绿色环保、可持续发展的制氢途径，由于反应体系简单、反应条件温和、清洁无污染、易实用化等优势，可以有效避免上述传统的工业制氢存在的缺点引起了学术界和工业界的广泛兴趣。
近年来，非金属聚合物类氮化碳(g-C3N4)由于原料低廉、制备简单、受可见光驱动(带隙约2.7eV)、无毒且具有良好的离子/电子传输性和种类多样性等优势，在催化、传感、能源存储等领域得到了广泛关注。尤其在光催化领域因具有如下的独特优势吸引了研究人员将其应用于催化分解水制氢：首先g-C3N4具有高效的电子传递、良好的稳定性以及丰富的表面暴露活性位点，表面拥有大量的亲水官能团，容易与其他材料复合；其次，由于电位梯度的存在，由能带结构相匹配的g-C3N4半导体构建的异质结光催化剂可以有效地加速光生电荷的分离和传输；再次，g-C3N4具有合适的禁带宽度，在拥有极大平面尺寸的同时还能保持原子厚度，赋予其极大的比表面积。然而，对于单纯、未经修饰的g-C3N4光催化剂仍然具有低的催化活性。因此，需要对单一的g-C3N4进行修饰或者改性，提高其比表面积、载流子分离效率及可见光吸收能力，从而进一步提高光催化活性。
发明内容
本发明的目的是提供一种多孔g-C3N4-MF共轭聚合物光催化剂及其制备方法，并考察引入不同含量的MF对可见光下光催化分解水制氢性能的影响。通过引入聚合物三聚氰胺甲醛树脂(MF)与g-C3N4构成共轭聚合物，并通过控制 MF的不同含量，使得制备的g-C3N4-MF共轭聚合物光催化剂具有大的比表面积、最大的可见光吸收能力、快速的载流子分离，并且具有最高的可见光分解水制氢性能。
一种多孔g-C3N4-MF共轭聚合物光催化剂的制备方法，包括如下步骤：
步骤S1：纯g-C3N4的制备
首先将尿素在120-160℃下加热融化，冷却至室温后研磨，以3-5℃/min的升温速率升温到550-750℃，并在550-750℃下煅烧2-4h。
步骤S2：多孔g-C3N4-MF共轭聚合物光催化剂的制备
首先将尿素在120-160℃下加热融化，随后加入三聚氰胺甲醛树脂，搅拌形成均一的混合溶液，冷却至室温后研磨，以3-5℃/min的升温速率升温到550-750℃，并在550-750℃下煅烧2-4h。
优选的，步骤S1中，尿素的含量为20g，煅烧温度为600℃，升温速率为 5℃/min，煅烧时间为3h。
步骤S2中，尿素与三聚氰胺甲醛树脂的比例为10-30g：25-200μL，优选比例为20g：100μL，搅拌时间为10-30min，优选20min，煅烧温度优选为600℃，升温速率优选为5℃/min，煅烧时间优选为3h。
本发明的有益效果
本发明的优点在于简便的合成了多孔g-C3N4-MF共轭聚合物光催化剂，并将其作为光催化剂分解水制氢具有很高的光催化产氢性能。本发明所提供的多孔 g-C3N4-MF共轭聚合物光催化剂具有大的比表面积，可提供的活性点更多，形成分子内供体-受体进一步提高载流子的分离效率，使得所制备的光催化剂高效的光催化活性得以发挥，该方法不会造成资源浪费，且操作简便，成本较低，是一种绿色环保的高效处理技术。
附图说明
图1a是所制备催化剂的X射线衍射图，从图1a中可以看出g-C3N4与g-C3N4-MF共轭聚合物光催化剂在2θ为13°与27°的衍射峰完全一致。在红外吸收光谱图1b中，g-C3N4-MF共轭聚合物的伸缩振动峰与纯的g-C3N4的衍射峰相同，证明MF的引入并没有改变g-C3N4本身的结构。
图2a和图2b分别为g-C3N4和g-C3N4-MF共轭聚合物光催化剂的扫描电镜图。通过图2a我们发现，纯的g-C3N4是由边缘卷曲的纳米片组成的体相材料，而g-C3N4-MF共轭聚合物光催化剂(图2b)相比于纯的g-C3N4具有明显的孔结构。为了进一步证明多孔结构的存在，对纯的g-C3N4和g-C3N4-MF共轭聚合物光催化剂进行了透射电镜分析。通过图2c我们发现纯的g-C3N4呈现纳米片结构。值得注意的是，g-C3N4-MF共轭聚合物光催化剂通过图2d可以明显的观察到多孔结构。有利于比表面积的增大，进而提高光催化产氢活性。
图3a为所制备催化剂的固体紫外吸收图。通过图3a我们发现相比于纯的 g-C3N4，g-C3N4-MF共轭聚合物光催化剂的可将光吸收能力明显增强。通过图3b 可以确定，相比于纯的g-C3N4(2.63eV),g-C3N4-MF共轭聚合物光催化剂的禁带(2.57eV)宽度变窄，更有利于可见光吸收。为了进一步确定价导带位置，我们进行了价带谱测试，图3c显示g-C3N4与g-C3N4-MF共轭聚合物光催化剂的价带位置分别为1.82eV和1.53eV。根据公式Eg＝EVB–ECB，最终我们确定了 g-C3N4与g-C3N4-MF共轭聚合物光催化剂的价导带位置。通过图3d我们发现， g-C3N4-MF共轭聚合物光催化剂的导带位置上移，更有利于电子与H+发生还原反应产生H2。
图4a-d分别为所合成催化剂的光催化产氢性能图、循环实验图、循环前后的X射线衍射图和量子效率图。通过图4a可以说明我们优化出的最佳条件 g-C3N4-MF100在可见光下具有最高的光催化产氢活性。图4b表示g-C3N4-MF100共轭聚合物光催化剂在经过六次循环之后仍具有良好的稳定性。通过观察反应前后样品的X射线衍射(图4b)说明经过六次循环之后样品得晶相并没有发生明显的改变。图4d说明光催化产氢活性主要取决于紫外-可见光吸收能力而不是入射光的波长。
图5a-d分别为荧光、衰减、光电流及阻抗图。图5a-b说明，g-C3N4-MF100共轭聚合物光催化剂相比于纯的g-C3N4具有很好的光生载流子分离效率。图5c 中，在所有制备的催化剂中，g-C3N4-MF100共轭聚合物光催化剂具有最大的光电流响应，与之相对于的是图5d中g-C3N4-MF100共轭聚合物光催化剂具有最小的阻抗，说明g-C3N4-MF100共轭聚合物光催化剂有效的抑制了载流子的重组，更有利于电子转移发生还原反应产生氢气。
具体实施方式
实施例1
多孔g-C3N4-MF25共轭聚合物光催化剂的制备
首先将20g尿素在140℃下加热融化，随后加入25μL的三聚氰胺甲醛树脂，搅拌20min形成均一的混合溶液，冷却至室温后研磨，以5℃/min的升温速率升温到600℃，并在600℃下煅烧3h。
实施例2
多孔g-C3N4-MF75共轭聚合物光催化剂的制备
首先将20g尿素在140℃下加热融化，随后加入75μL的三聚氰胺甲醛树脂，搅拌20min形成均一的混合溶液，冷却至室温后研磨，以5℃/min的升温速率升温到600℃，并在600℃下煅烧3h。
实施例3
多孔g-C3N4-MF100共轭聚合物光催化剂的制备
首先将20g尿素在140℃下加热融化，随后加入100μL的三聚氰胺甲醛树脂，搅拌20min形成均一的混合溶液，冷却至室温后研磨，以5℃/min的升温速率升温到600℃，并在600℃下煅烧3h。
实施例4
多孔g-C3N4-MF150共轭聚合物光催化剂的制备
首先将20g尿素在140℃下加热融化，随后加入150μL的三聚氰胺甲醛树脂，搅拌20min形成均一的混合溶液，冷却至室温后研磨，以5℃/min的升温速率升温到600℃，并在600℃下煅烧3h。
Claims (7)
1.一种共轭聚合物光催化剂的制备方法，其特征在于，具体步骤如下：首先将尿素在120-160℃下加热融化，随后加入三聚氰胺甲醛树脂，搅拌形成均一的混合溶液，冷却至室温后研磨，以3-5℃/min的升温速率升温到550-750℃，并在550-750℃下煅烧2-4h。
2.如权利要求1所述的一种共轭聚合物光催化剂的制备方法，其特征在于，尿素与三聚氰胺甲醛树脂的比例为10-30g：25-200μL。
3.如权利要求2所述的一种共轭聚合物光催化剂的制备方法，其特征在于，尿素与三聚氰胺甲醛树脂的比例为20g：100μL。
4.如权利要求1所述的一种共轭聚合物光催化剂的制备方法，其特征在于，搅拌时间为10-30min。
5.如权利要求4所述的一种共轭聚合物光催化剂的制备方法，其特征在于，搅拌时间为20min。
6.如权利要求1所述的一种共轭聚合物光催化剂的制备方法，其特征在于，煅烧温度为600℃，升温速率为5℃/min，煅烧时间为3h。
7.如权利要求1-6任一所述方法制备的共轭聚合物光催化剂的用途，其特征在于，应用于可见光下分解水产氢。
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