CN112495445A - 一种Bi12SiO20-Bi2O2SiO3-多巴胺光催化剂的制备方法 - Google Patents
一种Bi12SiO20-Bi2O2SiO3-多巴胺光催化剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种Bi12SiO20‑Bi2O2SiO3‑多巴胺(BSO‑DA·HCl)光催化剂及其制备方法。以硝酸铋为铋源，正硅酸乙酯为硅源，采用溶胶‑凝胶法成功制备了Bi12SiO20‑Bi2O2SiO3‑多巴胺(BSO‑DA·HCl)粉体材料，同时利用双异质结的协同光催化作用，有效改善了Bi12SiO20‑Bi2O2SiO3光催化剂光生电子容易与光生空穴复合的问题。该方法工艺简单、周期短、设备简单、成本低廉，所得复合材料表现出高的光催化性能。
Description
技术领域
本发明属于材料技术领域，特别涉及一种Bi12SiO20-Bi2O2SiO3-多巴胺(BSO-DA·HCl)光催化剂的制备方法。
背景技术
随着纳米及相关技术的发展，铋系光催化剂将以其独特的结构功能应用于更宽广的领域。作为Bi2O3-SiO2二元系统中常见的两种化合物，亚稳相的Bi2SiO3和稳定相的Bi12SiO20具有优良的光催化活性。但是单相光催化剂往往不能实现快速迁移光电荷的分离，从而在某种程度上限制了它们的光催化活性。现有的制备技术难以控制BSO体系晶相的生成，特别是亚稳相的生成，同时，存在团聚严重、表面性能不利于催化的问题。
发明内容
为了克服上述现有技术的缺点，本发明的目的在于提供一种Bi12SiO20-Bi2O2SiO3-多巴胺(BSO-DA·HCl)光催化剂的制备方法，该方法工艺简单、操作方便、周期短，制得的材料分散性好。本发明利用异质结的协同光催化作用，有效改善了Bi12SiO20-Bi2O2SiO3光催化剂光生电子容易与光生空穴复合的问题，从而有效提高其吸附作用并进一步增强可见光光催化性能，对于新型可见光响应光催化剂的开发及性能的优化提高具有重要意义。
为了实现上述目的，本发明采用的技术方案是：
一种Bi12SiO20-Bi2O2SiO3-多巴胺光催化剂的制备方法，包括：
步骤1)，将体积比约为(1.6～2)：1的无水乙醇与去离子水混合，向其中加入柠檬酸，加入后柠檬酸的浓度为0.005～0.008mol/L，待溶解完成后加入硝酸铋，加入后硝酸铋的浓度为0.004～0.008mol/L，搅拌约1h至完全溶解得到溶液A；按硅铋质量比m正硅酸乙酯：m硝酸铋＝(5～7)：1的比例称取正硅酸乙酯溶于溶液A中，待充分溶解后，加入1.8g～2.5g聚乙二醇，搅拌至完全溶解得到前驱体溶液；
步骤2)，将前驱体溶液置于水浴锅中，85℃～90℃下水浴蒸发3h～4h，之后于150℃～160℃下干燥7～10h，得到Bi12SiO20-Bi2O2SiO3干凝胶，在600℃-650℃煅烧2h-5h，得到Bi12SiO20-Bi2O2SiO3复合粉体；
步骤3)，称取Bi12SiO20-Bi2O2SiO3复合粉体0.1g～0.35g，与100mL～120mL浓度为0.08mol/L～0.15mol/L的HCl溶液混合，加入浓度为20～120mg/mL的盐酸多巴胺，搅拌8h～12h，然后在75℃～85℃烘箱中烘干即获得Bi12SiO20-Bi2O2SiO3-多巴胺光催化剂。
与现有技术相比，本发明的有益效果是：
1、本发明采用溶液混合、水浴蒸发、机械搅拌、烘干等较易简便的操作过程，其工艺简单、操作方便。
2、本发明将微量盐酸多巴胺(DA·HCl)直接与Bi12SiO20-Bi2O2SiO3复合以制备Bi12SiO20-Bi2O2SiO3-多巴胺复合催化剂，促进了Bi12SiO20-Bi2O2SiO3的结合和线型排列，同时，由于多巴胺含有邻苯二酚基团，易与原粉体形成自由基团，利于BSO主链和自由基之间的分子内电荷转移，提升空穴传输。
3、由于多巴胺具有大量的酚羟基，可有效地与水结合形成氢键，大幅度改善其亲水性，减少团聚。
4、本发明利用异质结的协同光催化作用，有效改善了Bi12SiO20-Bi2O2SiO3光催化剂光生电子容易与光生空穴复合的问题。
5、本发明制备周期短，成本低，且不会产生二次污染。
附图说明
图1是实施例1制得的光催化剂BSO-DA1对10mg/L罗丹明B溶液的降解曲线图。
图2是实施例2制得的光催化剂BSO-DA2对10mg/L罗丹明B溶液的降解曲线图。
图3是实施例3制得的光催化剂BSO-DA3对10mg/L罗丹明B溶液的降解曲线图。
具体实施方式
下面结合附图和实施例详细说明本发明的实施方式。
本发明以硝酸铋为铋源，正硅酸乙酯为硅源，采用溶胶-凝胶法成功制备了Bi12SiO20-Bi2O2SiO3-多巴胺(BSO-DA·HCl)粉体材料，同时利用双异质结的协同光催化作用，有效改善了Bi12SiO20-Bi2O2SiO3光催化剂光生电子容易与光生空穴复合的问题。该方法工艺简单、周期短、设备简单、成本低廉，所得复合材料表现出高的光催化性能。以下是本发明的几个具体实施例。
实施例1
(1)将无水乙醇与去离子水混合(体积比约为1.8:1)，向其中加入一定量的柠檬酸(浓度为0.007mol/L)，待溶解完成后加入一定量的硝酸铋(浓度为0.007mol/L)，搅拌约1h至完全溶解得到溶液A。同时按硅铋比为5:1称取一定量的正硅酸乙酯溶于上述溶液A中，待充分溶解后，加入1.8g聚乙二醇，搅拌至完全溶解得到前驱体溶液；
(2)将前驱体溶液置于水浴锅中，在85℃下水浴蒸发3h，之后于150℃下干燥约8h，得到Bi12SiO20-Bi2O2SiO3干凝胶，将其在600℃煅烧5h，得到Bi12SiO20-Bi2O2SiO3复合粉体；
(3)称取Bi12SiO20-Bi2O2SiO3复合粉体0.15g，加入一定量的盐酸多巴胺(浓度为40mg/mL)，与浓度为0.08mol/L的HCl溶液100mL混合搅拌8h，然后在80℃烘箱中烘干即获得Bi12SiO20-Bi2O2SiO3-多巴胺光催化剂。
图1是由实施例1制得的光催化剂BSO-DA1对10mg/L罗丹明B溶液的降解曲线，可看出其具有较好的吸附催化性能，30mg BSO-DA1对于30mL10mg/L RhB溶液能够做到60min内吸附超过60％，30min催化超过90％的吸附/催化效果。
实施例2
(1)将无水乙醇与去离子水混合(体积比约为2:1)，向其中加入一定量的柠檬酸(浓度为0.005mol/L)，待溶解完成后加入一定量的硝酸铋(浓度为0.006mol/L)，搅拌约1h至完全溶解得到溶液A。同时按硅铋比为6:1称取一定量的正硅酸乙酯溶于上述溶液A中，待充分溶解后，加入2.3g聚乙二醇，搅拌至完全溶解得到前驱体溶液；
(2)将前驱体溶液置于水浴锅中，在90℃下水浴蒸发4h，之后于160℃下干燥约10h，得到Bi12SiO20-Bi2O2SiO3干凝胶，将其在620℃煅烧3h，得到Bi12SiO20-Bi2O2SiO3复合粉体；
(3)称取Bi12SiO20-Bi2O2SiO3复合粉体0.2g，加入一定量的盐酸多巴胺(浓度为60mg/mL)，与浓度为0.12mol/L的HCl溶液120mL混合搅拌12h，然后在85℃烘箱中烘干即获得Bi12SiO20-Bi2O2SiO3-多巴胺光催化剂。
图2是由实施例2制得的光催化剂BSO-DA2对10mg/L罗丹明B溶液的降解曲线，可看出其具有较好的吸附催化性能，30mg BSO-DA2对于30mL 10mg/L RhB溶液能够做到60min内吸附超过70％，25min催化超过90％的吸附/催化效果。
实施例3：
(1)将无水乙醇与去离子水混合(体积比约为2:1)，向其中加入一定量的柠檬酸(浓度为0.008mol/L)，待溶解完成后加入一定量的硝酸铋(浓度为0.005mol/L)，搅拌约1h至完全溶解。同时按硅铋比为5:1称取一定量的正硅酸乙酯溶于上述溶液A中，待充分溶解后，加入2.0g聚乙二醇，搅拌至完全溶解得到前驱体溶液；
(2)将前驱体溶液置于水浴锅中，在90℃下水浴蒸发4h，之后于150℃下干燥约8h，得到Bi12SiO20-Bi2O2SiO3干凝胶，将其在650℃煅烧4h，得到Bi12SiO20-Bi2O2SiO3复合粉体；
(3)称取Bi12SiO20-Bi2O2SiO3复合粉体0.30g，加入一定量的盐酸多巴胺(浓度为120mg/mL)，与浓度为0.15mol/L的HCl溶液120mL混合搅拌12h，然后在85℃烘箱中烘干即获得Bi12SiO20-Bi2O2SiO3-多巴胺光催化剂。
图3是由实施例3制得的光催化剂BSO-DA3，可看出其具有较好的吸附催化性能，30mg BSO-DA3对于30mL 10mg/L RhB溶液能够做到60min内吸附超过60％，25min催化超过90％的吸附/催化效果。
Claims (1)
1.一种Bi12SiO20-Bi2O2SiO3-多巴胺光催化剂的制备方法，其特征在于，包括：
步骤1)，将体积比约为(1.6～2)：1的无水乙醇与去离子水混合，向其中加入柠檬酸，加入后柠檬酸的浓度为0.005～0.008mol/L，待溶解完成后加入硝酸铋，加入后硝酸铋的浓度为0.004～0.008mol/L，搅拌约1h至完全溶解得到溶液A；按硅铋质量比m正硅酸乙酯：m硝酸铋＝(5～7)：1的比例称取正硅酸乙酯溶于溶液A中，待充分溶解后，加入1.8g～2.5g聚乙二醇，搅拌至完全溶解得到前驱体溶液；
步骤2)，将前驱体溶液置于水浴锅中，85℃～90℃下水浴蒸发3h～4h，之后于150℃～160℃下干燥7～10h，得到Bi12SiO20-Bi2O2SiO3干凝胶，在600℃-650℃煅烧2h-5h，得到Bi12SiO20-Bi2O2SiO3复合粉体；
步骤3)，称取Bi12SiO20-Bi2O2SiO3复合粉体0.1g～0.35g，与100mL～120mL浓度为0.08mol/L～0.15mol/L的HCl溶液混合，加入浓度为20～120mg/mL的盐酸多巴胺，搅拌8h～12h，然后在75℃～85℃烘箱中烘干即获得Bi12SiO20-Bi2O2SiO3-多巴胺光催化剂。
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