CN107952489A - 一种有机无机杂化光催化剂的合成方法 - Google Patents
一种有机无机杂化光催化剂的合成方法 Download PDFInfo
- Publication number
- CN107952489A CN107952489A CN201711317024.XA CN201711317024A CN107952489A CN 107952489 A CN107952489 A CN 107952489A CN 201711317024 A CN201711317024 A CN 201711317024A CN 107952489 A CN107952489 A CN 107952489A
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- Prior art keywords
- inorganic hybridization
- photochemical catalyst
- organic inorganic
- synthetic method
- organic
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- 239000010931 gold Substances 0.000 claims abstract description 23
- 229910052737 gold Inorganic materials 0.000 claims abstract description 23
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 16
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- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
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- GEZAUFNYMZVOFV-UHFFFAOYSA-J 2-[(2-oxo-1,3,2$l^{5},4$l^{2}-dioxaphosphastannetan-2-yl)oxy]-1,3,2$l^{5},4$l^{2}-dioxaphosphastannetane 2-oxide Chemical compound [Sn+2].[Sn+2].[O-]P([O-])(=O)OP([O-])([O-])=O GEZAUFNYMZVOFV-UHFFFAOYSA-J 0.000 claims description 4
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- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 3
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- BRWIZMBXBAOCCF-UHFFFAOYSA-N hydrazinecarbothioamide Chemical compound NNC(N)=S BRWIZMBXBAOCCF-UHFFFAOYSA-N 0.000 claims description 2
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- 229960002447 thiram Drugs 0.000 claims 1
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Classifications
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
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- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
- C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
- C07C1/12—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon from carbon dioxide with hydrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2531/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- C07C2531/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups C07C2531/02 - C07C2531/24
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
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Abstract
本发明公开了一种有机无机杂化光催化剂的合成方法，首先将含有或者不含结晶水的锡盐放入反应釜中，加入硫源和水，而后加入胺类有机表面活性剂，充分搅拌均匀，水热反应获得有机无机杂化硫化锡光催化剂沉淀，将沉淀用酒精和去离子水洗涤数次，取出冷冻干燥后研磨，制得有机无机杂化硫化锡光催化剂粉末。本发明合成的有机无机杂化硫化锡光催化剂具有更小的晶粒尺寸和大的比表面，为载流子的分离提供极大的便利；恰当的带隙很好地提高了对可见光的利用，实现了二氧化碳向甲烷和甲醇的转换，并且提高了光催化剂的稳定性；材料合成工艺简单，成本低廉，稳定性良好，可以大规模生产，具有工业化前景。
Description
技术领域
本发明涉及一种有机无机杂化光催化剂的合成方法，属于能源环境与纳米材料技术领域。
背景技术
能源短缺和环境恶化是21世纪人类面临的越来越严峻的问题，给人们的生存带来了极大的挑战。其中，全球气候变暖是我们亟待缓解的环境问题之一，二氧化碳是致使“温室效应”的主要气体，同时是一种丰富的碳资源，如何减少及利用二氧化碳成为研究者们的主题。太阳能是一种洁净、丰富、可再生的能源，利用太阳能转化二氧化碳不仅能够缓解给环境带来的压力，而且是实现碳循环、应对能源短缺问题的一条较有发展前景的途径。例如在光催化剂的作用，利用太阳能将二氧化碳还原成甲烷，甲醇，一氧化碳等碳氢或者碳氢氧燃料。开发二氧化碳还原技术不仅能够节约煤，石油，天然气等化石能源，而且可以还原化石燃料燃烧所产生的的二氧化碳，有效降低温室气体排放，对于未来新能源材料领域具有很大的应用前景。
然而，现在很多的光催化剂还原二氧化碳的效率很低，远远不能满足当前的需要。例如中国专利 CN107175097A公开了名称为一种二硫化锡包裹二氧化钛复合光催化剂及其制备方法，这种方法是以五水四氯化锡、钛酸丁酯、硫脲为原料,无水乙醇为溶剂,采用一步溶剂热法制得的复合光催化剂。但是这种方法制得的硫化锡性质并不稳定，因为锡离子易水解产生副产物导致光催化性能不稳定，而且由于该方法合成催化剂的比表面和晶粒尺寸较大这项技术光催化性能并不高。
除此之外还有中国专利CN106732719A公开了一种氮化碳/二硫化锡量子点复合光催化剂的制备方法，制备方法为以三聚氰胺为原料,经过煅烧,制备氮化碳纳米片；将制得的氮化碳纳米片超声分散在乙二醇中,依次加入二硫化锡前驱体和硫源,进行水热反应制得氮化碳/二硫化锡复合光催化剂。但是由于三聚氰胺制得的氮化碳带隙较大不利于对可见光的吸收，并且氮化碳是粒径较大的大块材料而不是多孔的氮化碳，且以乙二醇为溶剂并不利于对复合光催化剂形貌的调控导致制得的催化剂比表面较大，所以光催化效率并不高，不利于实际工业化生产。
发明内容
为了解决现有技术中存在的不足，本发明的目的在于提供一种简单便捷制备有机无机杂化光催化剂的合成方法。这种有机无机杂化的光催化剂由于使用了胺类有机表面活性剂很好地调控了产品的形貌，使得产品晶粒细化比表面增大，有效地促进了电子空穴对的产生和分离，增强了在可见光下对二氧化碳还原成甲烷，甲醇等碳氢或碳氢氧化合物的能力和效率。此外，这种催化剂合适的带隙促进了对可见光的吸收和利用选择性地将二氧化碳转换成甲烷和甲醇，并且也大大提高了催化剂在使用中的稳定性。
为了达到上述目的，本发明采用的技术手段是：一种有机无机杂化光催化剂的合成方法，首先将含有或者不含结晶水的锡盐放入反应釜中，加入硫源和水，而后加入胺类有机表面活性剂，充分搅拌均匀，水热反应获得有机无机杂化硫化锡光催化剂沉淀，将沉淀用酒精和去离子水洗涤数次，取出冷冻干燥、研磨，制得有机无机杂化硫化锡光催化剂粉末。
进一步的，所述锡盐为无水四氯化锡，四氯化锡，二氯化锡，草酸亚锡，丙烷磺酸锡，锡酸钠，氢氧化锡，硫酸亚锡，醋酸亚锡，锌酸亚锡，焦磷酸锡，焦磷酸亚锡和硫酸锡的一种或几种组合。
进一步的，所述硫源为硫代乙酰胺，硫粉，硫脲氨基酸，硫醇，噻唑，二硫化四甲基秋兰姆，硫醚，硫代荃，四硫代钼酸铵，硫代水杨酸，硫代氨基脲，硫代苯甲酰胺，硫代硫酸钠，吩噻嗪，双硫腙和L-胱氨酸中的一种或者几种组合。
进一步的，所述胺类有机表面活性剂为三乙烯四胺，三乙烯二胺，三乙胺，二甘醇胺，乙醇胺，二甲胺，六甲基三乙烯四胺，四乙烯五胺，乙二胺和十六烷基三甲基溴化铵中的一种或几种组合。
更进一步的，所述水和胺类有机表面活性剂的比例0.2～4:1。
进一步的，所述水热反应温度为60～180℃，反应时间为2～48 h。
进一步的，所述锡源和硫源的质量比为0.2～5:1。
本发明具有以下优点：有机无机杂化硫化锡光催化剂具有更小的晶粒尺寸和大的比表面，为载流子的分离提供极大的便利。第二，恰当的带隙很好地提高了对可见光的利用，实现了二氧化碳向甲烷和甲醇的转换，并且提高了光催化剂的稳定性。第三，材料合成工艺简单，成本低廉，稳定性良好，可以大规模生产，具有工业化前景。
附图说明
下面结合附图和实施例对本发明做进一步的阐述。
图1为本发明实施例2中制备的有机无机杂化硫化锡的FESEM图像。
具体实施方式
实施例1
首先将1 mmol无水四氯化锡放入反应釜中，然后加入4 mmol 硫代乙酰胺，加入15 ml水和25ml四乙烯五胺，置于搅拌器上搅拌，搅拌均匀后通过在160℃水热48小时，制备有机无机杂化硫化锡光催化剂沉淀。然后将沉淀用酒精和去离子水洗涤数次，最后冷冻干燥后研磨，制得有机无机杂化硫化锡光催化剂粉末。
经测试，其二氧化碳转化甲烷性能在2 h后可达到152 μmol。
实施例2
首先将1 mmol无水四氯化锡放入反应釜中，然后加入4 mmol 硫代乙酰胺，加入20 ml水和15 ml二乙烯三胺，混合溶液在80 ℃水热24小时，制备有机无机杂化硫化锡光催化剂沉淀。然后将沉淀用酒精和去离子水洗涤数次，最后冷冻干燥后研磨，制得有机无机杂化硫化锡光催化剂粉末。
其FESEM图像如图1所示。我们可以发现有机无机杂化硫化锡光催化剂颗粒直径约为50~100nm,粒径分布均匀。
经测试，其二氧化碳转化甲烷性能在4 h后可达到311 μmol。
实施例3
首先将1 mmol 2.5水和二氯化锡放入反应釜中，然后加入4 mmol 双硫腙，加入20 ml水和12 ml乙二胺混合溶液在60 ℃水热48小时，制备有机无机杂化硫化锡光催化剂沉淀。然后将沉淀用酒精和去离子水洗涤数次，最后冷冻干燥后研磨，制得有机无机杂化硫化锡光催化剂粉末。
经测试，其苯酚降解率达94%。
实施例4
首先将1 mmol醋酸亚锡放入反应釜中，然后加入4 mmol半胱氨酸，加入20 ml水和12ml三乙烯四胺在180 ℃水热2小时，制备有机无机杂化硫化锡光催化剂沉淀。然后将沉淀用酒精和去离子水洗涤数次，最后冷冻干燥后研磨，制得有机无机杂化硫化锡光催化剂粉末。
经测试，其甲醛降解率达96%。
实施例5
首先将3 mmol锡酸钠放入反应釜中，然后加入4 mmol硫粉，加入20 ml水和15 ml二甲胺在140℃水热20小时，制备有机无机杂化硫化锡光催化剂沉淀。然后将沉淀用酒精和去离子水洗涤数次，最后冷冻干燥后研磨，制得有机无机杂化硫化锡光催化剂粉末。
经测试，其杀菌率达99%。
从上述实施例子中可以看出，选择锡盐和硫源材料加上胺类表面活性剂在一定温度下即可制成有机无机杂化材料。有机无机杂化硫化锡的合成方法十分快捷简单，制作成本低廉且材料易得，锡源和硫源的选择多样。这种有机无机杂化的硫化锡不同于常规无机光催化材料，能够提高材料的光学、电学、催化性能，还能够很好地控制样品形貌，使得目标产物的合成更加灵活容易控制并且富有多样性。化学性质更加稳定，不易变质，其恰当的带隙能够充分有效地利用可见光，促进半导体载流子的分离，提高该催化剂在液相及气相有机污染物降解、杀菌和二氧化碳还原方面的能力。
这种有机无机杂化材料由于有机分子和无机组分之间的协同作用使得具有与传统无机光催化材料所不可比拟的光催化性能。这种有机无机光催化材料能够在二氧化碳还原过程中选择性地将其转换为甲烷，并且能够有效阻止反应过程中副产物的产生。此外，合成方法简单快捷，原料易得且成本低廉，二氧化碳还原成甲烷甲醇等效率高，催化能力强，循环稳定性良好且使用寿命长。
本发明通过严格的化学计量比选用锡源和硫源，锡源和硫源的质量比控制在0.2～5:1，当高于或低于上述比例时后续反应无法实现。加入胺类表面活性剂和水充分搅拌均匀，其中水和胺类有机表面活性剂的比例0.2～4:1。再通过水热制得有机无机杂化硫化锡光催化剂。这种通过加入胺类表面活性剂的有机无机杂化材料形貌得到了很好地调控，有着较大的比表面和材料本身合适的带隙，一定程度上促进了光生电子空穴对的产生和分离由此增强了光催化能力,可用于光催化产氢,有机废水和有毒有害废气的降解处理。此外，这种有机无机杂化材料的循环稳定性较好。本发明合成方法简单便捷，原料易得且成本低廉，光催化性能，在未来新型能源环境材料领域有着较好的前景。
本发明所公开的实例只针对本发明的技术方案的解释，不能作为对本发明的内容的限制，本领域技术人员在本发明基础上的变更依然在本发明的保护范围内。
Claims (7)
1.一种有机无机杂化光催化剂的合成方法，其特征在于：首先将含有或者不含结晶水的锡盐放入反应釜中，加入硫源和水，而后加入胺类有机表面活性剂，充分搅拌均匀，水热反应获得有机无机杂化硫化锡光催化剂沉淀，将沉淀用酒精和去离子水洗涤数次，取出冷冻干燥后研磨，制得有机无机杂化硫化锡光催化剂粉末。
2.根据权利要求1所述的有机无机杂化光催化剂的合成方法，其特征在于：所述锡盐为无水四氯化锡，四氯化锡，二氯化锡，草酸亚锡，丙烷磺酸锡，锡酸钠，氢氧化锡，硫酸亚锡，醋酸亚锡，锌酸亚锡，焦磷酸锡，焦磷酸亚锡和硫酸锡的一种或几种组合。
3.根据权利要求1所述的有机无机杂化光催化剂的合成方法，其特征在于：所述硫源为硫代乙酰胺，硫粉，硫脲氨基酸，硫醇，噻唑，二硫化四甲基秋兰姆，硫醚，硫代荃，四硫代钼酸铵，硫代水杨酸，硫代氨基脲，硫代苯甲酰胺，硫代硫酸钠，吩噻嗪，双硫腙和L-胱氨酸中的一种或者几种组合。
4.根据权利要求1所述的有机无机杂化光催化剂的合成方法，其特征在于：所述胺类有机表面活性剂为三乙烯四胺，三乙烯二胺，三乙胺，二甘醇胺，乙醇胺，二甲胺，六甲基三乙烯四胺，四乙烯五胺，乙二胺和十六烷基三甲基溴化铵中的一种或几种组合。
5.根据权利要求4所述的有机无机杂化光催化剂的合成方法，特征在于：所述水和胺类有机表面活性剂的比例0.2～4:1。
6.根据权利要求1所述的有机无机杂化光催化剂的合成方法，特征在于：所述水热反应温度为60～180℃，反应时间为2～48 h。
7.根据权利要求1所述的有机无机杂化光催化剂的合成方法，其特征在于：所述锡源和硫源的质量比为0.2～5:1。
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| CN114195184A (zh) * | 2021-10-27 | 2022-03-18 | 苏州大学 | 一种二维硫属化合物的制备方法及其应用 |
| CN114195184B (zh) * | 2021-10-27 | 2023-02-10 | 苏州大学 | 一种二维硫属化合物的制备方法及其应用 |
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