CN109621953A - 一种高效光催化氧化苯甲醇的三维有序大孔钒酸铋负载钌催化剂 - Google Patents
一种高效光催化氧化苯甲醇的三维有序大孔钒酸铋负载钌催化剂 Download PDFInfo
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Abstract
一种高效光催化氧化苯甲醇的三维有序大孔钒酸铋负载钌催化剂，属于催化化学与纳米科学领域。首先采用以Bi(NO3)3·5H2O和NH4VO3为前驱体溶液，以甲醇、乙二醇、硝酸和水为溶剂的聚甲基丙烯酸甲酯微球胶晶模板法制备3DOM BiVO4载体；然后采用以三氯化钌为金属前驱体和以含有氢氧化钠的乙二醇溶液为还原剂的制备Ru纳米粒子；最后采用物理吸附法将Ru纳米粒子负载到3DOM BiVO4载体上，得到xRu/3DOM BiVO4(x为Ru负载量，x＝0.3‑2.4wt％)复合光催化剂。本发明制备工艺简单，产物粒子形貌规整可控，所得光催化剂对苯甲醇氧化表现出优异的光催化活性和高选择性。
Description
技术领域
本发明涉及一种高效光催化氧化苯甲醇的三维有序大孔钒酸铋负载钌催化剂，其中以聚甲基丙烯酸甲酯(PMMA)为硬模板和以乙二醇为还原剂，采用胶晶模板法和乙二醇还原吸附法分别制备了三维有序大孔(3DOM)BiVO4和xRu/3DOM BiVO4(x＝0.3-2.4wt％)光催化剂，其中xRu/3DOM BiVO4对苯甲醇氧化具有优异的光催化活性和高选择性。属于催化化学与纳米科学领域。
背景技术
苯甲醛是一种重要的化工原料和中间体，因而被广泛应用于制药、染料、香料和农药的生产中。目前，工业上常以甲苯和苯为原料，在高温或高压条件下，利用有毒的氧化剂高锰酸和重铬酸盐来实现到苯甲醛的转化。尽管上述的方法取得了较高的收率，但由于反应条件苛刻，反应过程产生有毒物质，会造成环境污染，危害人体健康。因此，开发一种反应条件温和和反应过程无污染的技术势在必行。最近，研究报道以苯甲醇为原料，利用光催化氧化过程来合成苯甲醛。该过程只需在光催化剂和光照下，以空气或氧气为氧化剂即可由苯甲醇合成苯甲醛。该方法不仅反应条件温和，原料价格便宜，而且还可避免有毒物质的生成。光催化氧化的关键是设计一种具有高效稳定催化性能的光催化剂。之前我们课题组已成功制备了Fe2O3/3DOM BiVO4和Co-Pd/BiVO4催化剂并用于酚类的光催化氧化(K.F.Zhang,Appl.Catal.B 202(2017)569–579,K.F.Zhang,Appl.Catal.B.224(2018)350–359)。目前还没有将3DOM BiVO4及其负载贵金属光催化剂用于光催化苯甲醇氧化的报道。此外，相对于贵金属Au、Pd和Pt，金属Ru的价格相对便宜。我们最近的研究发现，1.0wt％Ru/3DOM BiVO4对苯甲醇氧化表现出最好的催化性能(可见光照8h，苯甲醇转化率为78％，选择性为100％，反应条件为:6mL乙腈+0.12mmol苯甲醇，1atm O2)。
发明内容
本发明的目的在于，利用PMMA胶晶硬模板法和乙二醇还原法分别制备3DOM BiVO4和xRu/3DOM BiVO4光催化剂，用于苯甲醇的光催化氧化。
一种高效光催化氧化苯甲醇的三维有序大孔钒酸铋负载钌催化剂，其特征在于，所述的催化剂为在三维有序大孔(3DOM)BiVO4上负载有Ru，形成xRu/3DOM BiVO4(x＝0.3-2.4wt％，x为Ru负载量)复合光催化剂。
上述所述高效光催化氧化苯甲醇的三维有序大孔钒酸铋负载钌催化剂的制备，其特征在于，包括以下步骤：
(1)制备3DOM BiVO4；
(2)采用乙二醇还原法制备Ru纳米粒子；
(3)采用物理吸附法，将步骤(2)的Ru纳米粒子吸附到步骤(1)制备3DOM BiVO4上，干燥即可得到Ru/3DOM BiVO4。
进一步优选步骤(1)：在室温下，将4.8507g Bi(NO3)3·5H2O溶解于3.5mL乙二醇和5.5mL甲醇中，磁力搅拌0.5h，得到透明前驱体溶液A；将1.1698g NH4VO3和1.7613g溶解于6mL去离子水和1mL硝酸的混合溶液中，将其置于70℃水浴锅中搅拌15min，得到深绿色溶液B；将溶液A和B混合搅拌0.5h后，将3.0g PMMA模板浸渍在上述溶液中3.0h，抽滤去除多余溶液后，将得到的固体样品在室温条件下干燥过夜，然后将样品置于马弗炉中进行焙烧。焙烧程序为：以1℃/min的速率由室温升至300℃并在该温度下保持2h，随后以1℃/min的速率由300℃升至450℃并在该温度下保持4h，然后冷却到室温即得到催化剂3DOM BiVO4。
进一步优选步骤(2)采用乙二醇还原法制备Ru纳米粒子，具体步骤如下：0.5gRuCl3·xH2O溶解在25mL乙二醇中，在N2气氛下，将含有0.26g NaOH的25mL乙二醇溶液逐滴加入上述溶液中，剧烈搅拌30min后，将溶液升至160℃，保持3h后，自然冷却到室温后收集得到Ru纳米粒子溶液。
进一步优选步骤(3):分别取Ru纳米粒子溶液，将其分散在去离子水中，搅拌，然后分别加入制备好的3DOM BiVO4催化剂，搅拌6h后，抽滤、洗涤、干燥，即得到各催化剂。
本发明所制得的催化剂用于苯甲醇的光催化氧化制备苯甲醛，xRu/3DOM BiVO4光催化剂对苯甲醇表现出良好的光催化活性和高的选择性。
本发明具有制备工艺简单，原料价格便宜，产量较高和产物粒子形貌规整及晶体结构可控等特征。本发明制得的xRu/3DOM BiVO4光催化剂对苯甲醇氧化反应表现出优异的催化性能，其中苯甲醇(反应溶液组成为:6mL乙腈+0.12mmol苯甲醇)在1.0wt％Ru/3DOMBiVO4催化剂上光照和1atm O2条件下，反应8h后，苯甲醇转化率为78％。
附图说明
图1为所制得样品的XRD谱图。其中曲线(a)、(b)、(c)、(d)分别为实施例1和实施例3的3DOM BiVO4、0.3wt％Ru/3DOM BiVO4、1.0wt％Ru/3DOM BiVO4和2.4wt％Ru/3DOM BiVO4催化剂的XRD谱图。
图2为所制得样品的SEM照片。图中依次为(a,b)3DOM BiVO4 0.3wt％Ru/3DOMBiVO4,(c,d)1.0wt％Ru/3DOM BiVO4和(e,f)2.4wt％Ru/3DOM BiVO4催化剂的SEM照片。
图3为3DOM BiVO4和xRu/3DOM BiVO4催化剂对苯甲醇氧化的光催化活性。测试条件为：可见光照射8h，反应溶液组成为：6mL乙腈+0.12mmol苯甲醇，1atm O2。
具体实施方式
为了进一步阐述本发明，下面以实施例作详细说明，并给出附图描述本发明得到的各催化剂材料。
实施例1：采用PMMA胶晶模板法制备3DOM BiVO4。具体过程为：在室温下，将4.8507g Bi(NO3)3·5H2O溶解于3.5mL乙二醇和5.5mL甲醇中，磁力搅拌0.5h，得到透明前驱体溶液A；将1.1698g NH4VO3和1.7613g溶解于6mL去离子水和1mL硝酸的混合溶液中，将其置于70℃水浴锅中搅拌15min，得到深绿色溶液B；将溶液A和B混合搅拌0.5h后，将3.0g PMMA模板浸渍在上述溶液中3.0h，抽滤去除多余溶液后，将得到的固体样品在室温条件下干燥过夜，然后将样品置于马弗炉中进行焙烧。焙烧程序为：以1℃/min的速率由室温升至300℃并在该温度下保持2h，随后以1℃/min的速率由300℃升至450℃并在该温度下保持4h，然后冷却到室温即得到催化剂3DOM BiVO4。
采用乙二醇还原法制备Ru纳米粒子。具体步骤如下：0.5g RuCl3·xH2O溶解在25mL乙二醇中，在N2气氛下，将含有0.26g NaOH的25mL乙二醇溶液逐滴加入上述溶液中，剧烈搅拌30min后，将溶液升至160℃，保持3h后，自然冷却到室温后收集得到浓度为3.7mg/mL的Ru纳米粒子溶液。
采用物理吸附法制备0.3wt％Ru/3DOM BiVO4、1.0wt％Ru/3DOM BiVO4和2.4wt％Ru/3DOM BiVO4催化剂。具体步骤如下：分别取0.32mL、1.62mL和2.70mL的Ru纳米粒子溶液，将其分散在50mL去离子水中，搅拌10min，然后分别加入0.4g制备好的3DOM BiVO4催化剂，搅拌6h后，抽滤、洗涤、干燥，即得到各催化剂。此外，将1.0wt％Ru/3DOM BiVO4催化剂在Ar气氛下300℃处理4h得到1.0wt％Ru/3DOM BiVO4-Ar-300催化剂。
本发明具有制备工艺简单，原料价格便宜，产量较高和产物粒子形貌规整可控，本发明制备得到的xRu/3DOM BiVO4光催化剂对苯甲醇氧化反应表现出优异的光催化性能。
Claims (6)
1.一种高效光催化氧化苯甲醇的三维有序大孔钒酸铋负载钌催化剂，其特征在于，所述的催化剂为在三维有序大孔(3DOM)BiVO4上负载有Ru，形成xRu/3DOM BiVO4复合光催化剂，x＝0.3-2.4wt％，x为Ru负载量。
2.制备权利要求1所述的一种高效光催化氧化苯甲醇的三维有序大孔钒酸铋负载钌催化剂的方法，其特征在于，包括以下步骤：
(1)制备3DOM BiVO4；
(2)采用乙二醇还原法制备Ru纳米粒子；
(3)采用物理吸附法，将步骤(2)的Ru纳米粒子吸附到步骤(1)制备3DOM BiVO4上，干燥即可得到Ru/3DOM BiVO4。
3.按照权利要求2所述的方法，其特征在于，步骤(1)：在室温下，将4.8507g Bi(NO3)3·5H2O溶解于3.5mL乙二醇和5.5mL甲醇中，磁力搅拌0.5h，得到透明前驱体溶液A；将1.1698gNH4VO3和1.7613g溶解于6mL去离子水和1mL硝酸的混合溶液中，将其置于70℃水浴锅中搅拌15min，得到色溶液B；将溶液A和B混合搅拌0.5h后，将3.0g PMMA模板浸渍在上述溶液中3.0h，抽滤去除多余溶液后，将得到的固体样品在室温条件下干燥过夜，然后将样品置于马弗炉中进行焙烧；焙烧程序为：以1℃/min的速率由室温升至300℃并在该温度下保持2h，随后以1℃/min的速率由300℃升至450℃并在该温度下保持4h，然后冷却到室温即得到催化剂3DOM BiVO4。
4.按照权利要求2所述的方法，其特征在于，步骤(2)采用乙二醇还原法制备Ru纳米粒子，具体步骤如下：0.5g RuCl3·xH2O溶解在25mL乙二醇中，在N2气氛下，将含有0.26g NaOH的25mL乙二醇溶液逐滴加入上述溶液中，剧烈搅拌30min后，将溶液升至160℃，保持3h后，自然冷却到室温后收集得到Ru纳米粒子溶液。
5.按照权利要求2所述的方法，其特征在于，步骤(3):分别取Ru纳米粒子溶液，将其分散在去离子水中，搅拌，然后分别加入制备好的3DOM BiVO4催化剂，搅拌6h后，抽滤、洗涤、干燥，即得到各催化剂。
6.权利要求1所述的一种高效光催化氧化苯甲醇的三维有序大孔钒酸铋负载钌催化剂的应用，用于苯甲醇的光催化氧化制备苯甲醛。
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| CN114870827A (zh) * | 2022-05-13 | 2022-08-09 | 南开大学 | 铈镧复合氧化物载体的制备方法及其负载铂的催化剂与应用 |
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