CN101745381A - Hydrothermal method for synthesizing visible light catalyst SnWO4 - Google Patents
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Abstract
一种可见光催化剂SnWO4(钨酸亚锡)的合成方法,它是将等物质的量的SnCl2·2H2O和Na2WO4·2H2O分别加到等量去离子水中溶解,溶解后将两溶液混合,充分搅拌得到淡黄色的乳状沉淀,得到的含有淡黄色的乳状沉淀的反应混合物在密封状态下120~200℃反应24h,将反应后得到的红褐色的沉淀进行过滤收集、洗涤、烘干、碾磨,得到可见光催化剂SnWO4。本发明中使用预超声处理,设备简单,通过超声空化作用,使得反应混合物均匀分散,减小催化剂的粒径,扩大比表面积,能够提高催化剂的光催化活性。水热法可直接得到结晶良好的粉体,无需经过高温煅烧晶化,水热法合成温度较低,对设备要求低。本发明的方法制得的光催化剂SnWO4(钨酸亚锡)活性高。A kind of synthetic method of visible photocatalyst SnWO 4 (stannous tungstate), it is that SnCl 2 2H 2 O and Na 2 WO 4 2H 2 O of the amount of equal substance are respectively added to the equal amount of deionized water for dissolving, dissolving Afterwards, the two solutions were mixed and stirred thoroughly to obtain a light yellow milky precipitate. The obtained reaction mixture containing the light yellow milky precipitate was reacted in a sealed state at 120-200°C for 24 hours, and the reddish-brown precipitate obtained after the reaction was collected by filtration. Washing, drying and grinding to obtain the visible light catalyst SnWO 4 . In the present invention, pre-ultrasonic treatment is used, the equipment is simple, and the reaction mixture is uniformly dispersed through ultrasonic cavitation, the particle size of the catalyst is reduced, the specific surface area is enlarged, and the photocatalytic activity of the catalyst can be improved. The hydrothermal method can directly obtain a well-crystallized powder without high-temperature calcination and crystallization. The synthesis temperature of the hydrothermal method is low and the requirements for equipment are low. The photocatalyst SnWO 4 (tin tungstate) prepared by the method of the invention has high activity.
Description
技术领域technical field
本发明涉及一种光催化剂的合成,尤其是可见光催化剂的合成,具体的说是一种可见光催化剂SnWO4(钨酸亚锡)的合成方法。The invention relates to the synthesis of a photocatalyst, especially the synthesis of a visible light catalyst, specifically a synthesis method of a visible light catalyst SnWO 4 (tin tungstate).
背景技术Background technique
光催化正式在环境保护与治理上的应用研究开始于20世纪70年代后期。Fank和Bard关于水中氰化物在TiO2上的光分解研究以及Carey等关于多氯联苯在TiO2/紫外光下的降解研究,为光催化的迅速发展起到了极大的推动作用。光催化技术利用半导体材料在光照下表面能激活化的特性,利用光能可有效地氧化分解有机物、还原重金属离子、杀灭细菌和消除异味。由于光催化技术可利用太阳能在室温下发生反应,比较经济;目前关于光催化剂对各种有机物氧化降解的普适性已经成为共识,虽然不同的有机物由于结构、组成上的差异在降解活性上有一些差别,但总体上看光催化基本上是一个没有选择性的化学过程。所以未来光催化研究应该集中在机理的深刻认识、光响应范围宽和量子效率高的催化剂的制备、光催化技术工程化和新型的光催化产品开发等四个方面。The formal research on the application of photocatalysis in environmental protection and governance began in the late 1970s. Fank and Bard's research on the photodecomposition of cyanide on TiO 2 in water and Carey et al.'s research on the degradation of polychlorinated biphenyls under TiO 2 /ultraviolet light have greatly promoted the rapid development of photocatalysis. Photocatalytic technology utilizes the surface energy activation characteristics of semiconductor materials under light, and uses light energy to effectively oxidize and decompose organic matter, reduce heavy metal ions, kill bacteria and eliminate odors. Because photocatalytic technology can use solar energy to react at room temperature, it is relatively economical; at present, it has become a consensus on the universality of photocatalysts for the oxidative degradation of various organic substances, although different organic substances have different degradation activities due to differences in structure and composition. There are some differences, but in general photocatalysis is basically a non-selective chemical process. Therefore, future photocatalytic research should focus on four aspects: deep understanding of the mechanism, preparation of catalysts with a wide range of photoresponse and high quantum efficiency, engineering of photocatalytic technology, and development of new photocatalytic products.
为了更有效地利用太阳光,扩大光催化剂的光响应范围,研究在可见光下具有高效光催化活性的催化材料非常有意义,寻求廉价、环境友好并具有高性能的可见光光催化材料将是光催化发展进一步走向实用化的必然趋势。目前国内对于新型的可见光催化剂的研究较少,目前报道可见光催化剂的SnWO4的合成方法只有固相合成法。In order to make more effective use of sunlight and expand the photoresponse range of photocatalysts, it is very meaningful to study catalytic materials with high photocatalytic activity under visible light. Seeking cheap, environmentally friendly and high-performance visible light photocatalytic materials will be an important step in photocatalysis. The inevitable trend of further development towards practicality. At present, there are few domestic studies on new visible light catalysts, and the only reported synthesis method of visible light catalyst SnWO 4 is solid-phase synthesis.
固相合成法(参见:In-Sun Cho,Chae Hyun Kwak,Dong Wook Kim,Sangwook Lee,and Kug Sun Hong.Photophysical,Photoelectrochemical and Photocatalytic Properties ofNovel SnWO4 Oxide Semiconductors with Narrow Band Gaps·J Phys Chem C 2009(113):10647~10653),该法是以SnO和WO3机械混合后直接在800℃高温下烧结一定时间得到光催化剂SnWO4(钨酸亚锡),该方法合成条件苛刻,反应温度高,对设备要求高,能耗高,先驱材料的混合缺乏均匀性,合成催化剂产品颗粒粒径较大,分布不均匀,比表面积较小,需分解、降解的污染物在催化剂表面的吸附较小,从而可见光催化的活性不高。Solid phase synthesis (see: In-Sun Cho, Chae Hyun Kwak, Dong Wook Kim, Sangwook Lee, and Kug Sun Hong. Photophysical, Photoelectrochemical and Photocatalytic Properties of Novel SnWO 4 Oxide Semiconductors with Narrow Band Gaps J Phys Chem C 2009( 113): 10647~10653), this method is to obtain the photocatalyst SnWO 4 (tin tungstate) by mixing SnO and WO 3 mechanically and directly sintering at a high temperature of 800°C for a certain period of time. The synthesis conditions of this method are harsh and the reaction temperature is high. High requirements on equipment, high energy consumption, lack of uniformity in the mixing of precursor materials, large particle size of synthetic catalyst products, uneven distribution, small specific surface area, and small adsorption of pollutants that need to be decomposed and degraded on the surface of the catalyst. Therefore, the activity of visible light catalysis is not high.
综上所述,现有的方法对设备要求高、能耗高,操作复杂,条件苛刻,故需要开发简单低能耗的合成方法,能够合成具有高活性的可见光催化剂SnWO4(钨酸亚锡),能在可见光照射下分解降解有机物,长期发展具有较好的环境效益和经济效益。To sum up, the existing methods have high requirements for equipment, high energy consumption, complicated operation and harsh conditions. Therefore, it is necessary to develop a simple and low-energy synthesis method that can synthesize a highly active visible light catalyst SnWO 4 (stannous tungstate) , can decompose and degrade organic matter under visible light irradiation, and have good environmental and economic benefits in long-term development.
发明内容Contents of the invention
本发明的目的是使用新的合成方法,合成具有高可见光催化活性的SnWO4(钨酸亚锡),实现难降解有机物的可见光降解。The purpose of the present invention is to use a new synthesis method to synthesize SnWO 4 (stannous tungstate) with high visible light catalytic activity, so as to realize visible light degradation of refractory organic matter.
本发明目的可以通过以下技术方案达到:The object of the invention can be achieved through the following technical solutions:
一种可见光催化剂SnWO4(钨酸亚锡)的合成方法,其步骤如下:A kind of synthetic method of visible light catalyst SnWO 4 (tin tungstate), its steps are as follows:
(A)按物质的量的理论比例为1∶1,分别称取SnCl2·2H2O和Na2WO4·2H2O固体;(A) The theoretical ratio of the amount of substances is 1:1, respectively weigh the solids of SnCl 2 ·2H 2 O and Na 2 WO 4 ·2H 2 O;
(B)将SnCl2·2H2O和Na2WO4·2H2O分别加入到等量去离子水中溶解,溶解后将两溶液混合,充分搅拌得到淡黄色的乳状沉淀;(B) Add SnCl 2 ·2H 2 O and Na 2 WO 4 ·2H 2 O to an equal amount of deionized water to dissolve, mix the two solutions after dissolution, and stir well to obtain a light yellow milky precipitate;
(C)将步骤B得到的含有淡黄色的乳状沉淀的反应混合物在密封状态下120~180℃反应24h。(C) React the reaction mixture containing the light yellow milky precipitate obtained in step B at 120-180° C. for 24 hours in a sealed state.
(D)将反应后得到的红褐色的沉淀进行过滤收集、洗涤、烘干、碾磨,得到可见光催化剂SnWO4。(D) The reddish-brown precipitate obtained after the reaction is collected by filtration, washed, dried and milled to obtain the visible light catalyst SnWO 4 .
上述的可见光催化剂SnWO4的合成方法,其特征是:所述的步骤(B)中,去离子水的用量为每毫摩尔的SnCl2·2H2O固体和每毫摩尔的Na2WO4·2H2O固体各用去离子水10ml~12ml溶解。The synthesis method of the above-mentioned visible light catalyst SnWO 4 is characterized in that: in the step (B), the amount of deionized water is per millimole of SnCl 2 .2H 2 O solid and per millimole of Na 2 WO 4 . 2H 2 O solids were dissolved in 10ml-12ml of deionized water.
上述的可见光催化剂SnWO4的合成方法,其特征是:所述的步骤(B)中充分搅拌是将混合物在常温磁力搅拌30min,再置于超声反应器中超声30min使其充分混合。The synthesis method of the above-mentioned visible light catalyst SnWO 4 is characterized in that: the sufficient stirring in the step (B) is to magnetically stir the mixture at room temperature for 30 minutes, and then place it in an ultrasonic reactor for 30 minutes to make it fully mixed.
可以将上述制得的SnWO4(钨酸亚锡)光催化剂以一定量加入到目标污染物溶液中,先暗反应30min,然后在可见光照射下反应,进行目标污染物可见光降解。A certain amount of the above-prepared SnWO 4 (stannous tungstate) photocatalyst can be added to the target pollutant solution, reacted in the dark for 30 minutes, and then reacted under visible light irradiation to degrade the target pollutant with visible light.
本发明方法合成可见光催化剂SnWO4(钨酸亚锡)相对现有方法而言具有以下优点:Synthetic visible light catalyst SnWO 4 (tin tungstate) of the present invention has the following advantages relative to existing methods:
(1)通过改变水热反应环境,可得到不同结构和形貌的纳米粉体,通过控制水热反应条件(前驱物形式、反应温度、反应时间等),可得到不同粒度的产物。(1) Nano-powders with different structures and shapes can be obtained by changing the hydrothermal reaction environment, and products with different particle sizes can be obtained by controlling the hydrothermal reaction conditions (precursor form, reaction temperature, reaction time, etc.).
(2)本发明中使用的预超声处理,设备简单,效果明显。通过超声空化作用,使得反应混合物均匀分散,减小催化剂的粒径,扩大比表面积,能够提高催化剂的光催化活性。(2) The pre-ultrasonic treatment used in the present invention has simple equipment and obvious effect. Through ultrasonic cavitation, the reaction mixture is uniformly dispersed, the particle size of the catalyst is reduced, the specific surface area is enlarged, and the photocatalytic activity of the catalyst can be improved.
(3)水热法可直接得到结晶良好的粉体,无需经过高温煅烧晶化,减少了在煅烧过程中难以避免的粉体硬团聚,并且降低了能耗。(3) The hydrothermal method can directly obtain a well-crystallized powder without high-temperature calcination and crystallization, which reduces the unavoidable hard agglomeration of the powder during the calcination process and reduces energy consumption.
(4)水热法合成温度较低,对设备要求低。(4) The synthesis temperature of the hydrothermal method is low, and the requirements for equipment are low.
(5)本发明的方法制得的光催化剂SnWO4(钨酸亚锡)活性高。(5) The photocatalyst SnWO 4 (tin tungstate) prepared by the method of the present invention has high activity.
具体实施方式Detailed ways
实施例一Embodiment one
首先称取2mmol的SnCl2·2H2O和2mmol的Na2WO4·2H2O固体,分别加入20ml的去离子水,在磁力搅拌下,将钨酸钠溶液慢慢加入到氯化亚锡溶液中,磁力搅拌30min,再置于超声反应器中超声反应30min使混合物充分混合,将处理后的混合物移入到聚四氟乙烯的反应罐中,置于不锈钢反应釜中,密封放入烘箱中,溶剂热反应温度120℃,水热反应24h后,从烘箱中取出反应釜,待冷却到室温后,取出聚四氟乙烯反应罐,得到红褐色沉淀,将沉淀通过装有0.45μm滤膜的滤斗过滤,并用蒸馏水和无水乙醇反复洗涤沉淀,然后将沉淀连同滤斗一起放入烘箱中80℃恒温干燥6h,待烘干后用玛瑙钵研细后备用,称取0.300g上述催化剂,加入到200ml初始浓度为20.66mg/l的甲基橙溶液中,暗反应30min后浓度为20.57mg/l,然后用日光镝灯照射,光源功率400w,离液面15cm,定时取样,用752-N型紫外-可见分光度计测量样品的吸光度,根据甲基橙的标准曲线,计算光催化反应后不同时间的溶液浓度,光催化反应120min后,染料甲基橙的浓度为4.45mg/l,甲基橙总去除率达到了78.45%。First weigh 2mmol of SnCl 2 ·2H 2 O and 2mmol of Na 2 WO 4 ·2H 2 O solids, add 20ml of deionized water respectively, and slowly add sodium tungstate solution to stannous chloride under magnetic stirring solution, magnetically stirred for 30 minutes, then placed in an ultrasonic reactor for ultrasonic reaction for 30 minutes to fully mix the mixture, and moved the treated mixture into a polytetrafluoroethylene reaction tank, placed in a stainless steel reaction kettle, sealed and placed in an oven , solvothermal reaction temperature 120°C, after hydrothermal reaction for 24 hours, take out the reaction vessel from the oven, after cooling to room temperature, take out the polytetrafluoroethylene reaction vessel to obtain a reddish-brown precipitate, pass the precipitate through a filter equipped with a 0.45μm filter membrane Filter through the filter funnel, and repeatedly wash the precipitate with distilled water and absolute ethanol, then put the precipitate together with the filter funnel into an oven and dry at a constant temperature of 80°C for 6 hours. Add it to 200ml of methyl orange solution with an initial concentration of 20.66mg/l. After dark reaction for 30 minutes, the concentration will be 20.57mg/l. Then, it will be irradiated with a daylight dysprosium lamp. The power of the light source is 400w. N-type ultraviolet-visible spectrometer measures the absorbance of sample, according to the standard curve of methyl orange, calculates the solution concentration of different time after photocatalytic reaction, after photocatalytic reaction 120min, the concentration of dyestuff methyl orange is 4.45mg/l, The total removal rate of methyl orange reached 78.45%.
实施例二:Embodiment two:
溶剂热反应在140℃下进行,其它合成条件同实施例一,称取0.300g制得的催化剂,加入到200ml初始浓度为20.63mg/l的甲基橙溶液中,其它反应条件相同,暗反应30min后,染料甲基橙的浓度为20.43mg/l,光催化反应120min后,染料甲基橙的浓度为2.40mg/l,染料总去除率达到了88.37%。The solvothermal reaction was carried out at 140°C. Other synthesis conditions were the same as in Example 1. Weighed 0.300g of the prepared catalyst and added it to 200ml of methyl orange solution with an initial concentration of 20.63mg/l. Other reaction conditions were the same. After 30min, the concentration of methyl orange dye was 20.43mg/l, and after 120min of photocatalytic reaction, the concentration of methyl orange dye was 2.40mg/l, and the total removal rate of dye reached 88.37%.
实施例三:Embodiment three:
溶剂热反应在160℃下进行,其他合成条件通实施例一,取0.300g制得的催化剂,加入到200ml初始浓度为20.55mg/l的甲基橙溶液中,其他反应条件相同,暗反应后30min,甲基橙的浓度为21.17mg/l,光催化反应120min后,染料甲基橙的浓度为0.96mg/l,甲基橙的总去除率达到了95.33%。The solvothermal reaction is carried out at 160°C. Other synthesis conditions are the same as in Example 1. Take 0.300 g of the prepared catalyst and add it to 200 ml of methyl orange solution with an initial concentration of 20.55 mg/l. Other reaction conditions are the same. After dark reaction After 30min, the concentration of methyl orange was 21.17mg/l. After 120min of photocatalytic reaction, the concentration of dye methyl orange was 0.96mg/l, and the total removal rate of methyl orange reached 95.33%.
实施例四:Embodiment four:
溶剂热反应在180℃下进行,其他合成条件同实施例一,称取0.300g制得的催化剂,加入到200ml初始浓度为21.33mg/l的甲基橙溶液中,其他反应条件相同,暗反应30min后,甲基橙的浓度为21.17mg/l,光催化反应120min后,染料甲基橙的浓度为6.18mg/l,甲基橙的总去除率达到了71.05%。The solvothermal reaction was carried out at 180°C. Other synthesis conditions were the same as in Example 1. Weighed 0.300 g of the prepared catalyst and added it to 200 ml of methyl orange solution with an initial concentration of 21.33 mg/l. The other reaction conditions were the same. Dark reaction After 30min, the concentration of methyl orange was 21.17mg/l, and after 120min of photocatalytic reaction, the concentration of dye methyl orange was 6.18mg/l, and the total removal rate of methyl orange reached 71.05%.
不同温度下合成的光催化剂对目标污染物甲基橙的光照降解120min后的去除率达70%以上,其中在160℃下合成的催化剂,对目标污染物甲基橙的去除率达95.33%,见下表1,因而,该发明具有良好的环境效益。Photocatalysts synthesized at different temperatures have a removal rate of more than 70% of the target pollutant methyl orange after 120 minutes of photodegradation. Among them, the catalyst synthesized at 160°C has a removal rate of 95.33% of the target pollutant methyl orange. See table 1 below, thus, this invention has good environmental benefits.
表1Table 1
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CN112745854B (en) * | 2020-11-30 | 2021-10-26 | 河南省中农嘉吉化工有限公司 | Soil remediation agent |
CN114471620A (en) * | 2022-03-09 | 2022-05-13 | 淮北师范大学 | a-SnWO4/In2S3Composite photocatalyst |
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