CN116037214A - 一种Pt NPs@CTF-1复合光催化剂的制备及光催化产氢性能研究 - Google Patents
一种Pt NPs@CTF-1复合光催化剂的制备及光催化产氢性能研究 Download PDFInfo
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Abstract
本发明涉及一种CTFs复合光催化剂的制备方法及其应用。先通过高温快速成核法合成超小的Pt NPs；通过离子热法合成CTF‑1采用浸泡法将Pt NPs负载到合成的CTF‑1上，形成负载量为0.2 wt%的Pt NPs@CTF‑1复合光催化剂。超小的Pt NPs暴露出更多的活性位点大幅提高光催化产氢性能。载体CTF‑1具有良好的耐碱性，使复合材料有良好的稳定性。本发明的Pt NPs负载的CTF‑1复合光催化剂制备方法简单，成本低，可重复性好。
Description
技术领域
本发明涉及一种复合光催化剂的制备及其光催化性能研究。
背景技术
随着科技的发展，化石燃料早已无法实现地球的能源供应。化石燃料具有不可再生性并且燃烧产物污染大，为此人们迫切寻找新能源作为其代替品。氢能作为化石燃料的代替品之一，由于燃烧产物简单绿色一直是化石燃料最佳的替代品。光催化和电催化产氢是制备氢气的重要技术，相较于电催化产氢，光催化产氢技术直接利用太阳能，少一次能源转化，可以实现更低的能耗而更具竞争力。自1972年第一次报道TiO2上的光电化学水分裂以来，各种无机半导体和异质结等已被报道为可见光驱动光催化剂。可惜的是，第一代和第二代催化剂这些材料的主要问题是本身的毒性和腐蚀性，因此研究方向也开始向其他材料发生改变。共价有机骨架（COFs）材料作为一种新型半导体材料由于毒性小、耐腐蚀等优势得到了人们广泛的研究。
共价三嗪骨架（CTFs）材料作为二维COFs的一种，是通过共价和芳香三嗪键构建的，该骨架具有较高的孔密度、丰富的氮含量和较高的化学和热稳定性。即使在强酸和强碱的存在下，CTFs也表现出很高的稳定性，这使它们比其他多孔材料更加具有优势，并具有很强的工业应用的潜力。采用最传统的离子热合成方法得到的非晶态的黑色CTF-1具有较多的缺陷，可以为纳米粒子的负载提供位点。
铂作为贵金属，具有较低的析氢过电位和较高的电子转移能力，是光催化产氢反应最佳的催化活性物质之一。然而由于其稀缺性，使得催化制氢工艺成本变高不利于工业生产。例如，以1,4-二氰苯为原料，在氧化石墨烯存在下进行低温缩合，得到CTF-1/氧化石墨烯杂化材料，在3 wt% Pt的氯铂酸溶液作为助催化剂的条件下实现了高出纯CTF-1的9倍产氢速率。但是测试体系中的Pt并不能回收。为了实现贵金属Pt的回收再利用，合成Pt NPs并将其与载体半导体结合是目前常用的手段。金属纳米材料具有一系列块体材料所不具备的新效应，如小尺寸效应、界面效应和量子隧道效应等。将铂制成较小的纳米粒子可以大幅提升活性位点的利用率，从而在负载量较少的条件下实现高效产氢。最早人们采用光沉积的方法，在含有金属前体和还原剂的溶液中加入半导体材料，在光照下Pt NPs可以沉积到半导体材料表面，但这种方法合成的Pt NPs尺寸大小不一且容易团聚。为此，引入覆盖剂如聚乙烯吡咯烷酮（PVP）不仅可以调控纳米粒子的大小，还可以使其均匀分散阻碍纳米粒子间的团聚。
发明内容
本发明目的在于合成一种Pt NPs@CTF-1复合光催化剂，使Pt NPs负载在CTF-1表面，大幅提高光催化产氢性能。
本发明Pt NPs@CTF-1复合光催化剂制备方法，其特征在于该方法包括以下步骤：
一、制备CTF-1：将对苯二腈和干燥的氯化锌按照1:1的摩尔比加入玻璃管中，抽真空，在马弗炉中加热至400 ℃，恒温40小时。取出样品，研磨，洗涤，抽滤，干燥。
二、制备Pt NPs：将H2PtCl6 H2O和NaOH溶解在7.5 mL乙二醇中，抽真空，通氮气，160 ℃恒温2小时。待冷却后加入10 mL含PVP的乙醇溶液，离心，洗涤，最后保存在乙醇中。
三、制备Pt NPs@CTF-1：取CTF-1投入10 mL Pt NPs乙醇溶液中，搅拌24小时。抽滤，洗涤，干燥，得到Pt NPs@CTF-1复合光催化剂。
进一步的，步骤一称取药品在手套箱中进行。
进一步的，步骤一盐酸溶液和蒸馏水分别洗涤三次，每次不少于6小时。
进一步的，步骤一干燥过程不能鼓风，干燥条件为70 ℃，12小时。
进一步的，步骤二油浴先加热后放入反应器继续加热至160 ℃。
进一步的，步骤二用丙酮和三氯甲烷交替洗涤三次。
进一步的，步骤三用乙醇洗涤三次。
进一步的，步骤三干燥过程不能鼓风，干燥条件为60 ℃，6小时。
本发明具备优点：
（1）本发明制备的Pt NPs@CTF-1较纯CTF-1的产氢速率提升了44倍，具有更高的光催化产氢性能；
（2）尺寸小且均一的1.8 nm的Pt NPs 具有很高的比表面积，处于表面的原子数较多，大幅提升参与反应的活性位点数目；
（3）采用传统的离子热法合成CTF-1操作简单、成本低，产生的缺陷给Pt NPs提供了负载位点，使得Pt NPs均匀负载在CTF-1上，在Pt负载量为0.2 wt%的条件下实现高效产氢；
附图说明：
图1为实施得到的Pt NPs@CTF-1的TEM图。
图2为实施得到的CTF-1的热重图。
图3为实施得到的CTF-1、Pt NPs@CTF-1的光催化产氢图。
图4为实施得到的CTF-1、Pt NPs@CTF-1的光催化循环稳定图。
图5为实施得到的光催化前后Pt NPs@CTF-1的红外光谱图（FT-IR）。
具体实施方式
为能进一步了解本发明的发明内容、特征及其优点，通过以下实施例来进一步阐述：
实施例1
本实施例的Pt NPs@CTF-1复合光催化剂制备方法如下：
步骤一：CTF-1的制备方法：将对苯二腈和干燥的氯化锌按照1:1的摩尔比加入玻璃管中，抽真空，在马弗炉中加热至400 ℃，恒温40小时，取出样品，研磨，用盐酸溶液和蒸馏水洗涤，抽滤，70 ℃干燥过夜得到黑色固体。
步骤二：Pt NPs的制备方法：将0.1 g H2PtCl6 H2O和3.5 mmol NaOH溶解在7.5 mL乙二醇中，抽真空，通氮气，160 ℃恒温2小时，待冷却后加入10 mL含过量PVP的乙醇溶液，离心分离，丙酮和三氯甲烷交替洗涤，最后超声溶解并保存在10 mL乙醇中，形成均匀分散深褐色的Pt NPs乙醇溶液。
步骤三：Pt NPs@CTF-1的制备方法：取1 mL Pt NPs乙醇溶液稀释到10 mL，超声分散后，加入适量CTF-1搅拌24小时，边抽滤边用乙醇洗涤，在60 ℃下干燥过夜，即可得到黑色的Pt NPs@CTF-1复合光催化剂。
实施例2
本实施例的Pt NPs@CTF-1复合材料的制备方法如下：
步骤一同具体实施方式1中步骤一
步骤二同具体实施方式1中步骤二
步骤三：Pt NPs@CTF-1的制备方法：取3 mL Pt NPs乙醇溶液稀释到10 mL，超声分散后，加入适量CTF-1搅拌24小时，边抽滤边用乙醇洗涤，在60 ℃下干燥过夜，即可得到黑色的Pt NPs@CTF-1复合光催化剂。
实施例3
本实施例的Pt NPs@CTF-1复合材料的制备方法如下：
步骤一同具体实施方式1中步骤一
步骤二同具体实施方式1中步骤二
步骤三：Pt NPs@CTF-1的制备方法：取5 mL Pt NPs乙醇溶液稀释到10 mL，超声分散后，加入适量CTF-1搅拌24小时，边抽滤边用乙醇洗涤，在60 ℃下干燥过夜，即可得到黑色的Pt NPs@CTF-1复合光催化剂。
试样表征及性能测试
图1为具体实施例2步骤三制备的Pt NPs@CTF-1的TEM图，结果表明Pt NPs成功的负载到CTF-1表面并且分散均匀。Pt NPs的粒径大概在1.8 nm左右，超小的Pt NPs为产氢性能的提升提供了条件。
图2为具体实施例2步骤一制备的CTF-1的热重图，结果表明CTF-1具有良好的热稳定性，在600 ℃才开始分解。
图3为具体实施例2步骤一制备的CTF-1和步骤三制备的Pt NPs@CTF-1的光催化产氢性能对比图，结果表明负载Pt NPs后材料的光催化性能提升了44倍。
图4为具体实施例2步骤三制备的Pt NPs@CTF-1的产氢循环稳定性测试图，结果表明经过四次循环后产氢性能仍然能保持80%以上。
图5为具体实施例2步骤一制备的CTF-1和步骤三制备的Pt NPs@CTF-1以及测完产氢之后Pt NPs@CTF-1的FT-IR光谱图，结果表明，Pt NPs@CTF-1材料的谱图与CTF-1的基本一致，负载Pt NPs后CTF-1的结构没有发生改变，测完产氢后的Pt NPs@CTF-1谱图也没有明显变化，说明材料具有良好的稳定性。
Claims (8)
1.一种Pt NPs@CTF-1复合光催化剂的制备方法，其特征在于，制备方法包括以下步骤：一、制备CTF-1：将对苯二腈和干燥的氯化锌按照1:1的摩尔比加入玻璃管中，抽真空，在马弗炉中加热至400 ℃，恒温40小时，取出样品，研磨，洗涤，抽滤，干燥；二、制备Pt NPs：将H2PtCl6 H2O和NaOH溶解在7.5 mL乙二醇中，抽真空，通氮气，160 ℃恒温2小时，待冷却后加入10 mL含PVP的乙醇溶液，离心，洗涤，最后保存在乙醇中；三、制备Pt NPs@CTF-1：取CTF-1投入10 mL Pt NPs乙醇溶液中，搅拌24小时，抽滤，洗涤，干燥，得到Pt NPs@CTF-1复合光催化剂。
2.根据权利要求书1所述的CTF-1材料的制备方法，其特征在于：称取药品在手套箱中进行。
3.根据权利要求书1所述的CTF-1材料的制备方法，其特征在于：盐酸溶液和蒸馏水分别洗涤三次，每次不少于6小时。
4.根据权利要求书1所述的CTF-1材料的制备方法，其特征在于：干燥过程不能鼓风，干燥条件为70 ℃，12小时。
5.根据权利要求书1所述的Pt NPs材料的制备方法，其特征在于：油浴先加热后再放入反应器继续加热至160 ℃。
6.根据权利要求书1所述的Pt NPs材料的制备方法，其特征在于：用丙酮和三氯甲烷交替洗涤三次。
7.根据权利要求书1所述的Pt NPs@CTF-1材料的制备方法，其特征在于：用乙醇洗涤三次。
8.根据权利要求书1所述的Pt NPs@CTF-1材料的制备方法，其特征在于：干燥过程不能鼓风，干燥条件60 ℃，6小时。
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