CN102698784B - Visible light response catalyst and preparation method thereof - Google Patents
Visible light response catalyst and preparation method thereof Download PDFInfo
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Abstract
Description
技术领域 technical field
本发明涉及一种可见光响应催化剂及其制备方法。The invention relates to a visible light responsive catalyst and a preparation method thereof.
背景技术 Background technique
环境污染是当前人类面临的重大挑战，它导致了人们生活的饮用水源，工业水源质量不断下降，大气污染不断加剧，造成生态环境的不断破坏，严重影响着人们的健康和生活质量。因此，如何经济有效地净化环境污染是我们必须应对与解决的重大科学挑战。与传统的物理吸附，化学催化等方法相比，光催化技术具有成本低，无二次污染，应用范围广的优点，是21世纪最具开发前途的绿色环境治理技术。Environmental pollution is a major challenge facing mankind at present. It has led to the continuous decline in the quality of drinking water and industrial water sources for people's lives, and the aggravation of air pollution, resulting in continuous destruction of the ecological environment, seriously affecting people's health and quality of life. Therefore, how to purify environmental pollution economically and effectively is a major scientific challenge that we must face and solve. Compared with traditional methods such as physical adsorption and chemical catalysis, photocatalytic technology has the advantages of low cost, no secondary pollution, and wide application range. It is the most promising green environmental treatment technology in the 21st century.
自1972年Fujishima和Honda发现TiO2电极在光照下能分解水这一现象从而揭开光催化研究序幕以来，已有众多的催化剂被报道。纳米TiO2是其中最具有应用潜力的光催化剂之一，它具有良好的化学稳定性、抗磨损性、耐光腐蚀、低成本和无毒等优点，因而被广泛地用于光解水、降解有机物、杀菌和敏化太阳能电池的制备等。但是由于二氧化钛的禁带（3.2ev）过宽，光吸收范围仅限于紫外光区，对太阳能的利用率过低（约4％），限制了它的大规模应用。因此，为了有效的利用太阳能，同时满足室内无紫外线环境光催化净化的需求，寻找可见光响应的光催化剂势在必行。Since Fujishima and Honda discovered in 1972 that TiO 2 electrodes can split water under light, which opened the prelude to photocatalytic research, many catalysts have been reported. Nano-TiO 2 is one of the photocatalysts with the most application potential. It has the advantages of good chemical stability, wear resistance, light corrosion resistance, low cost and non-toxicity, so it is widely used in photolysis of water and degradation of organic matter. , Sterilization and preparation of sensitized solar cells, etc. However, due to the wide band gap (3.2ev) of titanium dioxide, the light absorption range is limited to the ultraviolet region, and the utilization rate of solar energy is too low (about 4%), which limits its large-scale application. Therefore, in order to effectively utilize solar energy and meet the demand for photocatalytic purification in indoor UV-free environments, it is imperative to search for photocatalysts that respond to visible light.
目前开发新型可见光响应催化剂的方法主要有两条途径，对TiO2进行修饰使其具有可见光响应能力（如掺杂金属阳离子或非金属阴离子，染料敏化等）和直接开发具有可见光响应能力的新型光催化剂。从目前的研究成果看，TiO2改性催化剂在太阳光照射下降解有机物的活性并不是很高，稳定性方面也存在一些问题。因此，人们纷纷将注意力集中到后一种开发途径上，一大批新型的可见光催化剂被报道，如邹志刚等开发的Ag2ZO4型（Z代表Cr、Mo、W、Mn等）复合氧化物（CN1799691A）和AgTO2型（T代表Al、Ga、In、Cr、Fe、Co、Ni）复合氧化物（CN1799690A），CN1905940A公开的BaBixOy（0.5<x<2,2<y<4）复合氧化物等。由于V的3d轨道电子能被可见光激发，因而钒酸盐也是一类具有可见光响应性质的半导体材料，不仅可用作光敏化半导体修饰其他宽带隙半导体，本身也具有较好的光催化性能，近来受到了较多研究者的关注。石墨型氮化碳（g-C3N4）则是2009年新发现的一类聚合物型光催化材料，由于其性价比高，同时也具有较高的热稳定性和化学稳定性，迅速得到了研究者的重视。但受限于研究时间较短，相关的研究报道较少。At present, there are two main ways to develop new visible light responsive catalysts, modifying TiO2 to make it have visible light responsive ability (such as doping metal cations or nonmetallic anions, dye sensitization, etc.) and directly developing new visible light responsive catalysts. catalyst of light. Judging from the current research results, the activity of TiO 2 modified catalysts to degrade organic matter under sunlight irradiation is not very high, and there are also some problems in terms of stability. Therefore, people have focused their attention on the latter development approach, and a large number of new visible light catalysts have been reported, such as the Ag 2 ZO 4 type (Z represents Cr, Mo, W, Mn, etc.) developed by Zou Zhigang. (CN1799691A) and AgTO type 2 (T represents Al, Ga, In, Cr, Fe, Co, Ni) composite oxide (CN1799690A), BaBi x O y (0.5<x<2,2<y<4) disclosed in CN1905940A ) Composite oxides, etc. Since the 3d orbital electrons of V can be excited by visible light, vanadate is also a kind of semiconductor material with visible light response properties. It can not only be used as a photosensitive semiconductor to modify other wide bandgap semiconductors, but also has good photocatalytic performance. Recently, has attracted the attention of many researchers. Graphite carbon nitride (gC 3 N 4 ) is a new type of polymer photocatalytic material discovered in 2009. Due to its high cost performance and high thermal and chemical stability, it has been rapidly studied attention. However, due to the short research time, there are few relevant research reports.
发明内容 Contents of the invention
本发明的目的在于提供一种制备方法简单、成本低廉的非氧化钛高活性光催化剂及制备方法。The purpose of the present invention is to provide a non-titanium oxide high-activity photocatalyst with simple preparation method and low cost and a preparation method.
为实施该发明目的，采用的技术方案为：For implementing this invention purpose, the technical scheme that adopts is:
一种可见光响应催化剂，其特征在于：该催化剂为钒酸镝复合石墨相氮化碳，化学组成通式为xDyVO4/g-C3N4，x为钒酸镝在催化剂中的质量分数，石墨相氮化碳（g-C3N4）的质量分数为1-x，0.1≤x≤0.4。A visible light response catalyst, characterized in that: the catalyst is dysprosium vanadate composite graphite phase carbon nitride, the general chemical composition formula is xDyVO 4 /gC 3 N 4 , x is the mass fraction of dysprosium vanadate in the catalyst, graphite phase The mass fraction of carbon nitride (gC 3 N 4 ) is 1-x, 0.1≤x≤0.4.
较佳的是x为0.15。Preferably x is 0.15.
g-C3N4即石墨相氮化碳(graphitic carbon nitride)。gC 3 N 4 is graphitic carbon nitride.
该催化剂的制备方法，包括以下步骤：The preparation method of this catalyst comprises the following steps:
（1）硝酸镝的制备：(1) Preparation of dysprosium nitrate:
在搅拌的情况下，按钒镝化学计量比（nV/nDy＝1:1？）将偏钒酸铵与硝酸镝分别溶于去离子水中，再将这两种溶液混合，生成黄色沉淀物后往该溶液中滴加30%的氨水调节其pH值等于7，沉淀物经搅拌陈化后过滤，清洗，所得固体烘干后在500°C温度下焙烧2小时，冷却后即得DyVO4。Under the condition of stirring, according to the stoichiometric ratio of vanadium and dysprosium (n V /n Dy = 1:1?), ammonium metavanadate and dysprosium nitrate were dissolved in deionized water respectively, and then the two solutions were mixed to form a yellow precipitate Add 30% ammonia water dropwise to the solution to adjust its pH value to be equal to 7. The precipitate is filtered and washed after stirring and aging. The obtained solid is dried and roasted at 500 ° C for 2 hours. After cooling, DyVO 4 .
（2）石墨相氮化碳的制备：(2) Preparation of graphite phase carbon nitride:
将三聚氰胺放于马弗炉中520°C焙烧4小时，冷却后即得黄色的g-C3N4.Put the melamine in a muffle furnace and bake it at 520°C for 4 hours. After cooling, the yellow gC 3 N 4 .
（3）钒酸镝复合石墨相氮化碳催化剂的制备：(3) Preparation of dysprosium vanadate composite graphite phase carbon nitride catalyst:
按DyVO4/g-C3N4质量比，将钒酸镝与石墨相氮化碳粉体混合研磨10min,最后于300-600°C下焙烧2小时即得该催化剂成品。According to the mass ratio of DyVO 4 /gC 3 N 4 , dysprosium vanadate and graphite phase carbon nitride powder were mixed and ground for 10 minutes, and finally calcined at 300-600°C for 2 hours to obtain the finished catalyst.
本发明采用半导体复合的方法来改性g-C3N4的思路，以g-C3N4为核心组分，通过修饰DyVO4以提高其光催化性能，从而开发出了一种高活性的钒酸镝复合石墨相氮化碳光催化剂。The present invention adopts the method of semiconductor compounding to modify gC 3 N 4 , takes gC 3 N 4 as the core component, and modifies DyVO 4 to improve its photocatalytic performance, thereby developing a highly active dysprosium vanadate Composite graphitic carbon nitride photocatalyst.
本发明制备的用于降解有机污染物的光催化剂具有以下两个特点：首先是催化剂的高可见光响应性，该催化剂禁带宽度为2.3eV左右，可以吸收波长小于560nm的可见光，这使得本发明制备的催化剂具有很高的吸收可见光的能力；其次，还表现在催化剂的光催化反应活性上：该催化剂对罗丹明B等多种有机染物都具有很高的可见光降解活性。此外，本发明制备的催化剂还有制备方法简单、适用条件不苛刻、光催化降解性能稳定，可长久使用等优点，因此，具有较高的商业化应用前景。The photocatalyst prepared by the present invention for degrading organic pollutants has the following two characteristics: first, the high visible light responsiveness of the catalyst, the catalyst band gap is about 2.3eV, and can absorb visible light with a wavelength less than 560nm, which makes the present invention The prepared catalyst has a high ability to absorb visible light; secondly, it is also manifested in the photocatalytic reactivity of the catalyst: the catalyst has a high visible light degradation activity for various organic dyes such as rhodamine B. In addition, the catalyst prepared by the present invention has the advantages of simple preparation method, not harsh application conditions, stable photocatalytic degradation performance, and long-term use. Therefore, it has a high commercial application prospect.
附图说明 Description of drawings
图1为实施例1~5及比较例1~3制备的催化剂在可见光下催化降解罗丹明B活性图。Fig. 1 is the catalytic degradation activity graph of Rhodamine B under visible light of the catalysts prepared in Examples 1-5 and Comparative Examples 1-3.
图2为实施例2、6~8制备的催化剂在可见光下催化降解罗丹明B活性图。Fig. 2 is the catalytic degradation activity diagram of rhodamine B under visible light of the catalysts prepared in Examples 2, 6-8.
图3为实施例3在可见光下降解罗丹明B反应的循环使用寿命图。Fig. 3 is the cycle service life diagram of the degradation reaction of Rhodamine B under visible light in Example 3.
图4为实施例3及比较例1~2制备的催化剂的X射线粉末衍射（XRD）。Fig. 4 is the X-ray powder diffraction (XRD) of the catalysts prepared in Example 3 and Comparative Examples 1-2.
图5为实施例3及比较例1~2制备的催化剂的紫外可见吸收（UV-vis）光谱。Fig. 5 is the ultraviolet-visible absorption (UV-vis) spectrum of the catalysts prepared in Example 3 and Comparative Examples 1-2.
具体实施方式 Detailed ways
以下用实施例进一步阐明本发明，但本发明不局限于以下实施例。The following examples further illustrate the present invention, but the present invention is not limited to the following examples.
实施例1：Example 1:
（1）称取1.254g偏钒酸铵，加入50ml去离子水，80°C水浴搅拌溶解，得到偏钒酸铵溶液。称取2.0g氧化镝，加入3ml浓硝酸和7ml去离子水，80°C水浴搅拌溶解，得到硝酸镝溶液。然后在搅拌的情况下将硝酸镝溶液缓慢滴加到偏钒酸铵溶液中，生成黄色沉淀，搅拌陈化2小时后过滤，用去离子水清洗三次，所得固体在烘箱中90°C下烘干，最后在马福炉中500°C下焙烧4小时。自然冷却后即得沉淀法制备的DyVO4。(1) Weigh 1.254g of ammonium metavanadate, add 50ml of deionized water, stir and dissolve in an 80°C water bath, and obtain an ammonium metavanadate solution. Weigh 2.0g of dysprosium oxide, add 3ml of concentrated nitric acid and 7ml of deionized water, stir and dissolve in an 80°C water bath to obtain a dysprosium nitrate solution. Then slowly add the dysprosium nitrate solution dropwise into the ammonium metavanadate solution under the condition of stirring, generate a yellow precipitate, filter after stirring and aging for 2 hours, wash three times with deionized water, and dry the obtained solid at 90°C in an oven Dry and finally bake in a muffle furnace at 500°C for 4 hours. After natural cooling, DyVO 4 prepared by precipitation method was obtained.
（2）称取5g三聚氰胺，放入有盖的坩埚中，再将该坩埚放于马弗炉中520°C焙烧3小时。自然冷却后即得黄色的g-C3N4。(2) Weigh 5g of melamine, put it into a covered crucible, and put the crucible in a muffle furnace for 3 hours at 520°C for roasting. After natural cooling that is yellow gC 3 N 4 .
（3）分别称取0.10g的钒酸镝和0.90g的石墨型氮化碳，将其混合研磨10min,最后于450°C温度下焙烧2小时，自然冷却后即得450°C焙烧的钒酸镝质量分数为0.1的DyVO4/g-C3N4复合催化剂。(3) Weigh 0.10g of dysprosium vanadate and 0.90g of graphite-type carbon nitride, mix and grind them for 10min, and finally roast at 450°C for 2 hours, and cool naturally to obtain vanadium roasted at 450°C A DyVO 4 /gC 3 N 4 composite catalyst with a dysprosium acid mass fraction of 0.1.
实施例2：Example 2:
（1）同实施例1中（1）的步骤。(1) Same as the step in (1) in Example 1.
（2）同实施例1中（2）的步骤。(2) Same as the step in (2) in Example 1.
（3）分别称取0.15g的钒酸镝和0.85g的石墨型氮化碳，将其混合研磨10min,最后于450°C温度下焙烧2小时，自然冷却后即得450°C焙烧的钒酸镝质量分数为0.15的DyVO4/g-C3N4复合催化剂。(3) Weigh 0.15g of dysprosium vanadate and 0.85g of graphite-type carbon nitride, mix and grind them for 10min, and finally roast at 450°C for 2 hours, and cool naturally to obtain vanadium roasted at 450°C DyVO 4 /gC 3 N 4 composite catalyst with dysprosium acid mass fraction of 0.15.
实施例3：Example 3:
（1）同实施例1中（1）的步骤。(1) Same as the step in (1) in Example 1.
（2）同实施例1中（2）的步骤。(2) Same as the step in (2) in Example 1.
（3）分别称取0.20g的钒酸镝和0.80g的石墨型氮化碳，将其混合研磨10min,最后于450°C温度下焙烧2小时，自然冷却后即得450°C焙烧的钒酸镝质量分数为0.2的DyVO4/g-C3N4复合催化剂。(3) Weigh 0.20g of dysprosium vanadate and 0.80g of graphite-type carbon nitride, mix and grind them for 10min, and finally roast at 450°C for 2 hours, and cool naturally to obtain vanadium roasted at 450°C DyVO 4 /gC 3 N 4 composite catalyst with dysprosium acid mass fraction of 0.2.
实施例4：Example 4:
（1）同实施例1中（1）的步骤。(1) Same as the step in (1) in Example 1.
（2）同实施例1中（2）的步骤。(2) Same as the step in (2) in Example 1.
（3）分别称取0.30g的钒酸镝和0.70g的石墨型氮化碳，将其混合研磨10min,最后于450°C温度下焙烧2小时，自然冷却后即得450°C焙烧的钒酸镝质量分数为0.3的DyVO4/g-C3N4复合催化剂。(3) Weigh 0.30g of dysprosium vanadate and 0.70g of graphite-type carbon nitride, mix and grind them for 10min, and finally roast at 450°C for 2 hours, and cool naturally to obtain vanadium roasted at 450°C A DyVO 4 /gC 3 N 4 composite catalyst with a dysprosium acid mass fraction of 0.3.
实施例5：Example 5:
（1）同实施例1中（1）的步骤。(1) Same as the step in (1) in Example 1.
（2）同实施例1中（2）的步骤。(2) Same as the step in (2) in Example 1.
（3）分别称取0.40g的钒酸镝和0.60g的石墨型氮化碳，将其混合研磨10min,最后于450°C温度下焙烧2小时，自然冷却后即得450°C焙烧的钒酸镝质量分数为0.4的DyVO4/g-C3N4复合催化剂。(3) Weigh 0.40g of dysprosium vanadate and 0.60g of graphite carbon nitride respectively, mix and grind them for 10min, and finally roast them at 450°C for 2 hours, and cool naturally to obtain vanadium roasted at 450°C A DyVO 4 /gC 3 N 4 composite catalyst with a dysprosium acid mass fraction of 0.4.
实施例6：Embodiment 6:
（1）同实施例1中（1）的步骤。(1) Same as the step in (1) in Example 1.
（2）同实施例1中（2）的步骤。(2) Same as the step in (2) in Example 1.
（3）分别称取0.15g的钒酸镝和0.85g的石墨型氮化碳，将其混合研磨10min,最后于300°C温度下焙烧2小时，自然冷却后即得400°C焙烧的钒酸镝质量分数为0.15的DyVO4/g-C3N4复合催化剂。(3) Weigh 0.15g of dysprosium vanadate and 0.85g of graphite-type carbon nitride, mix and grind them for 10min, and finally roast at 300°C for 2 hours, and cool naturally to obtain vanadium roasted at 400°C DyVO 4 /gC 3 N 4 composite catalyst with dysprosium acid mass fraction of 0.15.
实施例7：Embodiment 7:
（1）同实施例1中（1）的步骤。(1) Same as the step in (1) in Example 1.
（2）同实施例1中（2）的步骤。(2) Same as the step in (2) in Example 1.
（3）分别称取0.15g的钒酸镝和0.85g的石墨型氮化碳，将其混合研磨10min,最后于400°C温度下焙烧2小时，自然冷却后即得500°C焙烧的钒酸镝质量分数为0.15的DyVO4/g-C3N4复合催化剂。(3) Weigh 0.15g of dysprosium vanadate and 0.85g of graphite-type carbon nitride, mix and grind them for 10min, and finally roast them at 400°C for 2 hours, and cool naturally to obtain vanadium roasted at 500°C DyVO 4 /gC 3 N 4 composite catalyst with dysprosium acid mass fraction of 0.15.
比较例1：Comparative example 1:
钒酸镝，制备方法同实施例1中步骤（1）。Dysprosium vanadate, the preparation method is the same as step (1) in embodiment 1.
比较例2：Comparative example 2:
g-C3N4，制备方法同实施例1中步骤（2）。gC 3 N 4 , the preparation method is the same as step (2) in Example 1.
比较例3：Comparative example 3:
N掺杂TiO2（N–TiO2）。该光催化剂的制备方法如下：取钛酸四丁酯10ml,加入5ml冰乙酸，保持溶液温度在25°C左右，磁力搅拌10min后，缓慢滴加30%的浓氨水，至反应液pH值为9。将白色沉淀物用去离子水冲洗5次，85°C下烘干、研细，最后在400°C温度下焙烧2小时，冷却后即得到黄色的N–TiO2粉体催化剂。N-doped TiO 2 (N—TiO 2 ). The preparation method of the photocatalyst is as follows: take 10ml of tetrabutyl titanate, add 5ml of glacial acetic acid, keep the solution temperature at about 25°C, and after magnetic stirring for 10min, slowly add 30% concentrated ammonia water dropwise until the pH of the reaction solution is 9. Wash the white precipitate with deionized water 5 times, dry it at 85°C, grind it finely, and finally roast it at 400°C for 2 hours, and obtain a yellow N—TiO 2 powder catalyst after cooling.
光催化活性的评价采用自制光催化反应装置。光源灯为350W球形氙灯，由上往下照光，光源灯与液面间距15cm，侧面风扇吹风降温，光强约为15mW/cm2，反应时温度为室温。催化剂用量200mg，溶液体积100mL，罗丹明B染料浓度为1×10-5mol/L。反应前反应液均于黑暗条件下搅拌1h,以达到吸脱附平衡。反应后每隔30min抽取5ml左右的反应液，通过离心分离，然后用紫外可见分光光度计测定上层清液的吸光度，再根据朗伯－比尔定律换算出罗丹明B的浓度，以染料的脱色率来衡量催化剂的活性。The photocatalytic activity was evaluated using a self-made photocatalytic reaction device. The light source lamp is a 350W spherical xenon lamp, illuminated from top to bottom, the distance between the light source lamp and the liquid surface is 15cm, the side fan blows the air to cool down, the light intensity is about 15mW/cm 2 , and the reaction temperature is room temperature. The dosage of the catalyst is 200 mg, the volume of the solution is 100 mL, and the concentration of rhodamine B dye is 1×10 -5 mol/L. Before the reaction, the reaction solution was stirred for 1 h in the dark to achieve adsorption-desorption equilibrium. After the reaction, extract about 5ml of the reaction solution every 30 minutes, separate by centrifugation, and then measure the absorbance of the supernatant with a UV-visible spectrophotometer, and then convert the concentration of rhodamine B according to the Lambert-Beer law, and use the decolorization rate of the dye to measure catalyst activity.
以上实施例1~5以及对比例1，3所述的催化剂的光催化降解罗丹明B的活性见图1。实施例2和实施例6~7，比较例2制得的催化剂的可见光催化降解罗丹明B的活性见图2。实施例2在可见光下降解罗丹明B反应的循环使用寿命见图3。a1~a7分别对应实施例1~7制得的催化剂,b1~b3则分别对应比较例1~3制得的催化剂。由评价结果可知，采用本发明的制备方法制备的用于可见光下降解染料废水中有机污染物的光催化剂具有很高的光催化活性和使用寿命。在可见光照射下实施例2制得的催化剂降解罗丹明B染料的降解率几乎为100％。The activity of photocatalytic degradation of rhodamine B of the catalysts described in Examples 1-5 and Comparative Examples 1 and 3 above is shown in FIG. 1 . The visible light catalytic degradation activity of rhodamine B of the catalyst prepared in Example 2 and Examples 6-7 and Comparative Example 2 is shown in FIG. 2 . The cycle life of the degradation reaction of Rhodamine B under visible light in Example 2 is shown in FIG. 3 . a1~a7 respectively correspond to the catalysts prepared in Examples 1~7, and b1~b3 respectively correspond to the catalysts prepared in Comparative Examples 1~3. It can be seen from the evaluation results that the photocatalyst prepared by the preparation method of the present invention for degrading organic pollutants in dye wastewater under visible light has high photocatalytic activity and service life. The degradation rate of the catalyst prepared in Example 2 to degrade Rhodamine B dye under visible light irradiation is almost 100%.
实施例2和比较例1~2制得的催化剂的X射线粉末衍射（XRD）表征结果见图4，实施例2和比较例1~2制得的催化剂的紫外可见漫反射吸收（UV-vis）表征结果见图5。从图4中可以看出，催化剂中只存在DyVO4和g-C3N4相，由于两半导体间的协同耦作用，使得光生电子-空穴对在这两相间能够定向迁移，从而有效的促进了电子空穴对的分离，因此大大提高了其光催化活性。紫外可见漫反射吸收光谱表征结果表明实施例2在小于467nm可见光区范围内具有很强的吸收能力。这与上述的催化性能评价结果是一致的，即实施例2制得的催化剂具有很高的可见光降解废水染料有机污染物性能。The X-ray powder diffraction (XRD) characterization result of the catalyst that embodiment 2 and comparative examples 1～2 make is shown in Fig. ) characterization results are shown in Figure 5. It can be seen from Figure 4 that there are only DyVO 4 and gC 3 N 4 phases in the catalyst, and due to the synergistic coupling between the two semiconductors, the photogenerated electron-hole pairs can migrate directionally between the two phases, thus effectively promoting the The separation of electron-hole pairs thus greatly enhances its photocatalytic activity. The ultraviolet-visible diffuse reflectance absorption spectrum characterization results show that Example 2 has a strong absorption capacity in the range of visible light less than 467nm. This is consistent with the above-mentioned catalytic performance evaluation results, that is, the catalyst prepared in Example 2 has a very high performance of visible light degradation of organic pollutants in wastewater dyes.
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