CN108043394A - 一种用于降解VOCs的银掺杂纳米棒复合薄膜的制备方法 - Google Patents
一种用于降解VOCs的银掺杂纳米棒复合薄膜的制备方法 Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/007—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by irradiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
本发明设计了一种用于降解VOCs的银掺杂纳米棒复合薄膜的制备方法，具体步骤如下：在ITO衬底(1)上滴涂一层石墨烯薄膜(2)，然后以四氯化钛和钛酸丁酯为前驱体，以乙酰丙酮银作为掺杂银离子，在反应釜中，用盐酸和去离子水作为导向剂，在石墨烯薄膜(2)上生长银掺杂二氧化钛纳米棒(3)，高温退火处理，得到银掺杂二氧化钛纳米棒(3)/石墨烯薄膜(2)。本发明操作方法简单、绿色、无污染，为制备光催化降解VOCs的复合薄膜奠定了一定基础。
Description
技术领域
本发明涉及一种用于降解VOCs的银掺杂纳米棒复合薄膜的制备方法，属于光催化降解技术领域。
背景技术
VOCs(volatile organic compounds)挥发性有机物，通常指在常温下容易挥发的有机物，危害人的身体健康以及对LCD显示行业的产品良率有一定的影响。在众多半导体光催化剂中，如TiO2、ZnO、CdS、WO3、SnO2，半导体TiO2因其催化活性高、稳定性好、无毒、价廉等优点而备受青睐，但是TiO2存在禁带宽度大、电子-空穴复合率高的缺点，限制其应用推广。而石墨烯是由单层碳原子构成的二维晶格平面薄膜，呈蜂窝状，具有比表面积大、电子迁移率高的优势，因而，在复合光催化材料方面具有很高的应用价值。
为了克服上述技术方面的困难，本发明使用了一种简单、绿色的水热方法，制备了一种银掺杂二氧化钛纳米棒(3)/石墨烯薄膜(2)，减小TiO2的禁带宽度、提高复合光催化剂的比表面积、降低电子-空穴对的再结合速率，进而提高光催化效率。
发明内容
本发明是一种用于降解VOCs的银掺杂纳米棒复合薄膜的制备方法，拟解决上述背景技术中存在的问题。即在ITO衬底(1)上滴涂石墨烯薄膜(2)，氮气环境干燥，转移至高温高压反应釜中，以四氯化钛和钛酸丁酯为前驱体，掺入乙酰丙酮银固体，在石墨烯薄膜(2)上生长银掺杂二氧化钛纳米棒(3)，经过高温退火之后，得到银掺杂二氧化钛纳米棒(3)/石墨烯薄膜(2)。
1.作为一种优选方案，以ITO衬底(1)为基板，用水浴加热90℃的食人鱼溶液下浸泡30～50min，进行预处理。
2.作为一种优选方案，采用滴涂的方法制备石墨烯薄膜(2)，在NaOH溶液中加入氧化石墨烯粉末，制备10～15mL的0.2～0.5g/L的氧化石墨烯溶液，磁力搅拌1～2h，加入0.2～0.5mL的水合肼，80～100℃恒温搅拌5～10h，得到石墨烯溶胶(4)，0.5～1μL石墨烯溶胶(4)滴涂在ITO衬底(1)上，氮气环境下干燥，再滴涂0.5～1μL石墨烯溶胶(4)，氮气环境干燥，得到石墨烯薄膜(2)。
3.作为一种优选方案，采用水热法制备银掺杂二氧化钛纳米棒(3)，10mL盐酸分散到10mL去离子水和20mL无水乙醇混合液中，形成混合溶剂。将1mL四氯化钛和1mL钛酸丁酯混合10mL冰醋酸，按摩尔质量n(Ag):n(Ti)＝0.3％～0.5％比例加入乙酰丙酮银固体，形成乙酰丙酮银前驱溶液。将乙酰丙酮银前驱溶液滴加到混合溶剂中，搅拌1～2h，形成均匀乙酰丙酮银溶液。将载有石墨烯薄膜(2)的ITO衬底(1)倾斜45°放置反应釜中，石墨烯薄膜(2)方向朝上，将乙酰丙酮银溶液倒入反应釜中，180～200℃条件下12～24h，取出样品，380～500℃下退火30min，得到银掺杂二氧化钛纳米棒(3)/石墨烯薄膜(2)。
附图说明
图1：银掺杂二氧化钛纳米棒(3)/石墨烯薄膜(2)结构图
图2：银掺杂二氧化钛纳米棒(3)/石墨烯薄膜(2)形成过程
具体实施方式
将ITO衬底(1)在水浴加热90℃的食人鱼溶液下浸泡30min进行ITO衬底(1)预处理，取出后用去离子水清洗、浸泡并超声，再用丙酮、无水乙醇、去离子水清洗一遍，氮气吹干，烘干备用。在NaOH溶液中加入氧化石墨烯，制备0.2g/L的氧化石墨烯溶液10mL，磁力搅拌1h，然后加入0.2mL的水合肼，80℃恒温搅拌5h，得到石墨烯溶胶(4)，0.5μL石墨烯溶胶(4)滴涂在ITO衬底(1)上，氮气环境下干燥，再滴涂0.5μL石墨烯溶胶(4)，氮气环境下干燥，得到石墨烯薄膜(2)。20mL盐酸分散到10mL去离子水和20mL的无水乙醇混合液中，形成混合溶剂。1mL四氯化钛和1mL钛酸丁酯混合10mL的冰醋酸，按照摩尔质量n(Ag):n(Ti)＝0.3％的比例加入乙酰丙酮银固体，形成乙酰丙酮银前驱溶液。将乙酰丙酮银前驱溶液滴加到混合溶剂中，磁力搅拌1h，形成均匀乙酰丙酮银溶液。将载有石墨烯薄膜(2)的ITO衬底(1)，倾斜45°放置反应釜中，石墨烯薄膜(2)方向朝上，将均匀乙酰丙酮银溶液倒入反应釜中，180℃条件下水热反应12h，取出样品，380℃下退火30min，得到银掺杂二氧化钛纳米棒(3)/石墨烯薄膜(2)。
Claims (3)
1.一种用于降解VOCs的银掺杂纳米棒复合薄膜的制备方法，其特点在于：以ITO为衬底(1)，采用滴涂的方法制备石墨烯薄膜(2)，以四氯化钛和钛酸丁酯为前驱体，以乙酰丙酮银作为掺杂银离子，采用一步水热法，在石墨烯薄膜(2)上生长银掺杂二氧化钛纳米棒(3)。
2.根据权利要求1所述的一种用于降解VOCs的银掺杂纳米棒复合薄膜的制备方法，其特点在于：采用滴涂的方法制备石墨烯薄膜(2)，即配制10～15mL浓度为0.2～0.5g/L的氧化石墨烯与NaOH混合溶液，滴加0.2～0.5mL水合肼，80～100℃恒温搅拌5～10h，得到石墨烯溶胶(4)，0.5～1μL石墨烯溶胶(4)滴涂在ITO衬底(1)上，氮气环境干燥，得到石墨烯薄膜(2)。
3.根据权利要求1所述的一种用于降解VOCs的银掺杂纳米棒复合薄膜的制备方法，其特点在于：采用水热法制备银掺杂二氧化钛纳米棒(3)，按照摩尔质量n(Ag):n(Ti)＝0.3％～0.5％配比溶液，磁力搅拌1～2h。将载有石墨烯薄膜(2)的ITO衬底(1)放置反应釜中，倒入配比溶液，180～200℃下12～24h，取出样品，380～500℃下退火，得到银掺杂二氧化钛纳米棒(3)/石墨烯薄膜(2)。
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Citations (2)
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| CN102380364A (zh) * | 2011-09-02 | 2012-03-21 | 武汉大学 | 一种TiO2/石墨烯复合薄膜的制备方法 |
| CN105771980A (zh) * | 2016-04-27 | 2016-07-20 | 吉首大学 | 一种石墨烯/银/介孔二氧化钛纳米复合光催化剂及其制备工艺 |
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Patent Citations (2)
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|---|---|---|---|---|
| CN102380364A (zh) * | 2011-09-02 | 2012-03-21 | 武汉大学 | 一种TiO2/石墨烯复合薄膜的制备方法 |
| CN105771980A (zh) * | 2016-04-27 | 2016-07-20 | 吉首大学 | 一种石墨烯/银/介孔二氧化钛纳米复合光催化剂及其制备工艺 |
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| GAI LI等: "Preparation and photoelectrochemical performance of Ag/graphene/TiO2 composite film", 《APPLIED SURFACE SCIENCE》 * |
| HUNG JI HUANG等: "Confined migration of induced hot electrons in Ag/graphene/TiO2 composite nanorods for plasmonic photocatalytic reaction", 《OPTICS EXPRESS》 * |
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