铋酸钠基钙钛矿型功能材料的可见光催化/直接氧化降解典型有机水相染料研究
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摘要
可溶性有机染料的广泛生产和使用不可避免的导致了水体环境中的染料污染,对人类和生态健康产生潜在威胁。面对不断涌现的环境问题,当务之急是采取有效措施消除降解有机染料废水中的污染物。传统的降解技术处理有机水相染料污染效率较低,因此开发高效的处理技术正迅速成为一大研究热点。本论文建立了铋酸钠可见光光催化,铋银氧化物直接氧化与可见光催化/直接氧化联用降解水体有机染料等方法。这些基于铋酸钠型功能材料的降解方法成本低、简单易行,同时实现了对典型有机水相染料的高效、深度降解。
以罗丹明B作为模式染料研究铋酸钠的可见光催化活性以及罗丹明B的降解行为。1g/L铋酸钠在可见光照射下30分钟内将20mg/L罗丹明B溶液完全脱色,假一级反应速率常数为0.124min-1。染料溶液紫外可见吸收光谱在降解过程中有一定蓝移,最大吸收峰波长从554nm降至534nm。铋酸钠加热温度显著影响其光催化反应活性,未加热的铋酸钠样品活性最高。重复5次降解罗丹明B溶液结果显示铋酸钠有较高的光催化稳定性。检测出罗丹明B所有脱乙基产物与多种小分子产物。其中两种脱乙基同分异构体产物生成量区别很大,推测原因为降解过程中罗丹明B分子两侧电子密度不同所致。在铋酸钠可见光催化降解过程中罗丹明B主要有两种竞争性反应路径：破坏生色团与脱乙基过程。
利用二水铋酸钠与硝酸银采用水相共沉淀方法首次合成铋银氧化物(BSO),并基于BSO提出了快速直接氧化降解罗丹明B染料的方法。结果显示,在仅需混合BSO与罗丹明B溶液的条件下,20mg/L罗丹明B降解假一级反应速率常数k=0.5594min-1,同时形成多种小分子分解产物。该反应在常温常压下进行,无需任何外加能源。BSO能够被多次重复利用降解罗丹明B溶液而没有显著失活。当铋酸钠与硝酸银重量比为2/1的时候,合成的BSO活性最好。BSO表征结果显示在罗丹明B降解反应过程中银元素被还原为零价银；初始二水铋酸钠的主体钙钛矿结构变为Bi2O2CO3结构；晶格氧含量减少,活性/吸附氧含量增加。反应过程中有单重态氧生成,其作为主要活性物质直接导致了染料分子的降解。
开发了基于BSO直接氧化与基于铋酸钠可见光催化的联用方法,大幅提高了有机染料的降解效果。以结晶紫染料为目标化合物研究发现,在铋酸钠光催化降解过程中,染料溶液最大吸收波长由584nm蓝移至576nm；而在BSO直接氧化过程中,最大吸收波长由584nm红移至592nm。由于产生的自由基种类不同,结晶紫的降解路径差异很大。脱甲基过程在光催化反应中显著发生而在直接氧化反应中并不显著。另外,基于相同铋酸钠量的直接氧化对结晶紫溶液脱色效率比可见光催化效率高,并且染料浓度越大降解效率差别越大。通过对比联用的和单一使用的直接氧化与可见光催化方法降解效果发现,应用联用方法130mg/L结晶紫溶液在30分钟内矿化率达到37%,相同使用量的BSO或铋酸钠在相同时间内直接氧化或光催化降解相同浓度的结晶紫溶液,矿化率只有18%和15%。应用联用方法降解多种不同浓度不同类型染料都达到了更高的矿化率。在联用过程中,开始的直接氧化过程主要起快速脱色作用,使后续的可见光催化过程效率得到实质性提高,从而最终达到染料溶液矿化率提高100%的效果。该新型联用方法效率高,成本低特别适用于高浓度染料溶液的深度矿化。
此外,开发出铜掺杂铋酸钠(CSB)材料,并基于该材料发展了一种快速简单的染料降解方法。应用此方法降解孔雀石绿染料溶液发现,在0.2g二水铋酸钠合成的CSB作用下,15分钟内30mg/L孔雀石绿溶液脱色率达到95%,并生成多种小分子降解产物。当铋酸钠与硝酸铜两者重量比相同时,合成的CSB活性最好。该方法在常温常压下应用,无需任何外加能源。对CSB的表征研究结果表明铜元素主要分布于材料表面。该材料作用方式与BSO作用方式相似,可以进一步发展为更低成本的替代性材料。
The production and widespread use of soluble organic dyes inevitably results in their unintended release into the aqueous environment where they pose potential threats to human and ecological health. With the growing awareness and environmental concerns, it is imperative that the hierarchy of reduction and degradation be adopted and measures be taken to remove pollutants from the organic dye wastewater. The traditional treatment techniques prove to be ineffective in removing these pollutions. The desire to develop efficient water treatment techniques is quickly becoming a major focus in the environmental research community. This work presented novel, affordable and easy-operated organic dye wastewater control technologies based on sodium bismuthate-type functional material, viz. NaBiO3initiated visible light photocatalytic (PC) technique, silver bismuth oxide (BSO) initiated direct oxidation (DO) technique and combined DO/PC technique.
For PC process, the photocatalytic degradation of Rhodamine B (RhB) over NaBiO3under visible light irradiation was investigated.20mg/L of RhB solution was completely decolorized in30min with1g/L of NaBiO3·2H2O at the pseudo first-order reaction constant k=0.124min-1. The dye solution absorption maximum shifted from554to534nm during the degradation reaction. NaBiO3heating temperature significantly influenced its photocatalytic activity. The original sample exhibited higher activity than the heated samples did. The stability of NaBiO3was evaluated by repeated degradation of RhB solution for five times. All N-deethylation intermediates and several small molecular products were separated and identified. The yield distinctness between two isomer intermediates was correlated with the changes in the electron density of the dye molecule. Then two possible competitive photodegradation pathways of RhB over NaBiO3were proposed:Chromophore cleavage and N-deethylation.
For DO process, the oxidative powder BSO was firstly prepared by simple coprecipitation of NaBiO3·2H2O and AgN03. The technique was evaluated for the decolorization and oxidative decomposition of RhB. The results demonstrated that mixing BSO with an aqueous solution of RhB (20mg/L) resulted in rapid decolorization (pseudo-first-order kinetic constant k=0.5594min-1) and formation of several small molecular weight products. The optimal starting weight for NaBiO3·2H2O to AgNO3is2to1for synthesizing the BSO. The reaction proceeded at ambient temperature and pressure, and required no external energy sources or light. An advantage of the technique is that BSO can be used to degrade sequential additions of dye without significant fouling or loss of activity. The characterization of BSO and its corrosion products revealed that Ag species were reduced to metallic silver and NaBiO3·2H2O was transformed into the Bi2O2CO3during the reaction process. Singlet oxygen (1O2) was identified as the major reactive species generated by BSO for the degradation of RhB.
For combined DO and PC process, extensive and much enhanced organic dye degradation was achieved. In single PC treatment process, the Crystal Violet (CV) dye solution absorption maximum blue-shifted from584to576nm; whereas in single DO treatment process, it red-shifted from584to592nm. CV dye decomposition by each reagent proceeded via two distinct pathways, each involving different active oxygen species. N-demethylation of CV significantly occurred in PC but not in DO process. Same amount of NaBiO3·2H2O based DO process exhibited a superior performance to PC process with respect to the CV decolorization, particularly when high concentration dye solution was treated. A comparison of each treatment method alone and in combination demonstrated that using the combined sequential methods37%of TOC removal was achieved in30min for130mg/L of CV solution whereas only18%and15%was obtained using DO and PC alone, respectively. The combined method also manifested significantly improved mineralization of several diverse groups of dyes. In the combined process DO acts as a pre-treatment to rapidly bleach the dye solution which substantially facilitates subsequent PC processes. The integrated sequential DO and PC are complementary manifesting a>100%increase in TOC removal, compared to either isolated method. The combined process is proposed as a novel and effective technology (especially with respect of TOC removal) for treating wastewaters contaminated by high concentrations of organic dyes.
In addition, as an extension of the study, copper doped sodium bismuthate (CSB) was firstly synthesized through aqueous ion exchange reaction and a simple and efficient method based on it for degrading organic dye is proposed. The Malachite Green dye degradation experiments demonstrated that mixing0.2g NaBiO3·2H2O based CSB in the dye solution (30mg/L) for15min resulted in95%of decolorization and formation of several small molecular weight products. The sodium bismuthate starting weight equivalent to that of copper nitrate is optimal to synthesize CSB. The reaction proceeded at ambient temperature and pressure, and required no external energy sources or light. The characterization suggested copper species were distributed through the external surface of CSB. CSB performed in a similar functional mode as BSO did and it could be further developed as an optional material for BSO at lower cost.
以罗丹明B作为模式染料研究铋酸钠的可见光催化活性以及罗丹明B的降解行为。1g/L铋酸钠在可见光照射下30分钟内将20mg/L罗丹明B溶液完全脱色,假一级反应速率常数为0.124min-1。染料溶液紫外可见吸收光谱在降解过程中有一定蓝移,最大吸收峰波长从554nm降至534nm。铋酸钠加热温度显著影响其光催化反应活性,未加热的铋酸钠样品活性最高。重复5次降解罗丹明B溶液结果显示铋酸钠有较高的光催化稳定性。检测出罗丹明B所有脱乙基产物与多种小分子产物。其中两种脱乙基同分异构体产物生成量区别很大,推测原因为降解过程中罗丹明B分子两侧电子密度不同所致。在铋酸钠可见光催化降解过程中罗丹明B主要有两种竞争性反应路径：破坏生色团与脱乙基过程。
利用二水铋酸钠与硝酸银采用水相共沉淀方法首次合成铋银氧化物(BSO),并基于BSO提出了快速直接氧化降解罗丹明B染料的方法。结果显示,在仅需混合BSO与罗丹明B溶液的条件下,20mg/L罗丹明B降解假一级反应速率常数k=0.5594min-1,同时形成多种小分子分解产物。该反应在常温常压下进行,无需任何外加能源。BSO能够被多次重复利用降解罗丹明B溶液而没有显著失活。当铋酸钠与硝酸银重量比为2/1的时候,合成的BSO活性最好。BSO表征结果显示在罗丹明B降解反应过程中银元素被还原为零价银；初始二水铋酸钠的主体钙钛矿结构变为Bi2O2CO3结构；晶格氧含量减少,活性/吸附氧含量增加。反应过程中有单重态氧生成,其作为主要活性物质直接导致了染料分子的降解。
开发了基于BSO直接氧化与基于铋酸钠可见光催化的联用方法,大幅提高了有机染料的降解效果。以结晶紫染料为目标化合物研究发现,在铋酸钠光催化降解过程中,染料溶液最大吸收波长由584nm蓝移至576nm；而在BSO直接氧化过程中,最大吸收波长由584nm红移至592nm。由于产生的自由基种类不同,结晶紫的降解路径差异很大。脱甲基过程在光催化反应中显著发生而在直接氧化反应中并不显著。另外,基于相同铋酸钠量的直接氧化对结晶紫溶液脱色效率比可见光催化效率高,并且染料浓度越大降解效率差别越大。通过对比联用的和单一使用的直接氧化与可见光催化方法降解效果发现,应用联用方法130mg/L结晶紫溶液在30分钟内矿化率达到37%,相同使用量的BSO或铋酸钠在相同时间内直接氧化或光催化降解相同浓度的结晶紫溶液,矿化率只有18%和15%。应用联用方法降解多种不同浓度不同类型染料都达到了更高的矿化率。在联用过程中,开始的直接氧化过程主要起快速脱色作用,使后续的可见光催化过程效率得到实质性提高,从而最终达到染料溶液矿化率提高100%的效果。该新型联用方法效率高,成本低特别适用于高浓度染料溶液的深度矿化。
此外,开发出铜掺杂铋酸钠(CSB)材料,并基于该材料发展了一种快速简单的染料降解方法。应用此方法降解孔雀石绿染料溶液发现,在0.2g二水铋酸钠合成的CSB作用下,15分钟内30mg/L孔雀石绿溶液脱色率达到95%,并生成多种小分子降解产物。当铋酸钠与硝酸铜两者重量比相同时,合成的CSB活性最好。该方法在常温常压下应用,无需任何外加能源。对CSB的表征研究结果表明铜元素主要分布于材料表面。该材料作用方式与BSO作用方式相似,可以进一步发展为更低成本的替代性材料。
The production and widespread use of soluble organic dyes inevitably results in their unintended release into the aqueous environment where they pose potential threats to human and ecological health. With the growing awareness and environmental concerns, it is imperative that the hierarchy of reduction and degradation be adopted and measures be taken to remove pollutants from the organic dye wastewater. The traditional treatment techniques prove to be ineffective in removing these pollutions. The desire to develop efficient water treatment techniques is quickly becoming a major focus in the environmental research community. This work presented novel, affordable and easy-operated organic dye wastewater control technologies based on sodium bismuthate-type functional material, viz. NaBiO3initiated visible light photocatalytic (PC) technique, silver bismuth oxide (BSO) initiated direct oxidation (DO) technique and combined DO/PC technique.
For PC process, the photocatalytic degradation of Rhodamine B (RhB) over NaBiO3under visible light irradiation was investigated.20mg/L of RhB solution was completely decolorized in30min with1g/L of NaBiO3·2H2O at the pseudo first-order reaction constant k=0.124min-1. The dye solution absorption maximum shifted from554to534nm during the degradation reaction. NaBiO3heating temperature significantly influenced its photocatalytic activity. The original sample exhibited higher activity than the heated samples did. The stability of NaBiO3was evaluated by repeated degradation of RhB solution for five times. All N-deethylation intermediates and several small molecular products were separated and identified. The yield distinctness between two isomer intermediates was correlated with the changes in the electron density of the dye molecule. Then two possible competitive photodegradation pathways of RhB over NaBiO3were proposed:Chromophore cleavage and N-deethylation.
For DO process, the oxidative powder BSO was firstly prepared by simple coprecipitation of NaBiO3·2H2O and AgN03. The technique was evaluated for the decolorization and oxidative decomposition of RhB. The results demonstrated that mixing BSO with an aqueous solution of RhB (20mg/L) resulted in rapid decolorization (pseudo-first-order kinetic constant k=0.5594min-1) and formation of several small molecular weight products. The optimal starting weight for NaBiO3·2H2O to AgNO3is2to1for synthesizing the BSO. The reaction proceeded at ambient temperature and pressure, and required no external energy sources or light. An advantage of the technique is that BSO can be used to degrade sequential additions of dye without significant fouling or loss of activity. The characterization of BSO and its corrosion products revealed that Ag species were reduced to metallic silver and NaBiO3·2H2O was transformed into the Bi2O2CO3during the reaction process. Singlet oxygen (1O2) was identified as the major reactive species generated by BSO for the degradation of RhB.
For combined DO and PC process, extensive and much enhanced organic dye degradation was achieved. In single PC treatment process, the Crystal Violet (CV) dye solution absorption maximum blue-shifted from584to576nm; whereas in single DO treatment process, it red-shifted from584to592nm. CV dye decomposition by each reagent proceeded via two distinct pathways, each involving different active oxygen species. N-demethylation of CV significantly occurred in PC but not in DO process. Same amount of NaBiO3·2H2O based DO process exhibited a superior performance to PC process with respect to the CV decolorization, particularly when high concentration dye solution was treated. A comparison of each treatment method alone and in combination demonstrated that using the combined sequential methods37%of TOC removal was achieved in30min for130mg/L of CV solution whereas only18%and15%was obtained using DO and PC alone, respectively. The combined method also manifested significantly improved mineralization of several diverse groups of dyes. In the combined process DO acts as a pre-treatment to rapidly bleach the dye solution which substantially facilitates subsequent PC processes. The integrated sequential DO and PC are complementary manifesting a>100%increase in TOC removal, compared to either isolated method. The combined process is proposed as a novel and effective technology (especially with respect of TOC removal) for treating wastewaters contaminated by high concentrations of organic dyes.
In addition, as an extension of the study, copper doped sodium bismuthate (CSB) was firstly synthesized through aqueous ion exchange reaction and a simple and efficient method based on it for degrading organic dye is proposed. The Malachite Green dye degradation experiments demonstrated that mixing0.2g NaBiO3·2H2O based CSB in the dye solution (30mg/L) for15min resulted in95%of decolorization and formation of several small molecular weight products. The sodium bismuthate starting weight equivalent to that of copper nitrate is optimal to synthesize CSB. The reaction proceeded at ambient temperature and pressure, and required no external energy sources or light. The characterization suggested copper species were distributed through the external surface of CSB. CSB performed in a similar functional mode as BSO did and it could be further developed as an optional material for BSO at lower cost.
引文
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