技术领域Technical field
本发明涉及光催化技术领域，具体涉及一种卤素掺杂的Bi2WO6/Bi3.84W0.16O6.24催化剂，还涉及该光催化剂的制备方法和在光还原CO2中的应用。The invention relates to the technical field of photocatalysis, specifically to a halogen-doped Bi2 WO6 /Bi3.84 W0.16 O6.24 catalyst, and also relates to a preparation method of the photocatalyst and its application in photoreduction of CO2 .
背景技术Background technique
近几十年来，现代社会一直严重依赖于化石燃料来发展生产力。然而，燃烧化石燃料会产生大量的二氧化碳排放到空气中，从而导致一系列的环境问题，如全球日渐变暖的气候、海平面升高、沙漠化日趋严重、海洋日趋酸化、物种多样性逐渐减少等。这将严重影响了人类的生产生活安全。因此，我们迫切需要找到绿色和可持续的方法来解决这一问题。由于是反应条件温和、利用清洁能源，光催化技术被认为是一种很有前途的方法。In recent decades, modern society has relied heavily on fossil fuels to develop its productivity. However, burning fossil fuels will produce large amounts of carbon dioxide and emit it into the air, leading to a series of environmental problems, such as a warming global climate, rising sea levels, increasing desertification, increasing ocean acidification, and a gradual reduction in species diversity. . This will seriously affect the safety of human production and life. Therefore, we urgently need to find green and sustainable ways to solve this problem. Photocatalytic technology is considered a promising method due to its mild reaction conditions and the use of clean energy.
Bi2WO6是一种很有前途的光催化剂，因其合适的带隙、结构稳定、无毒无害和低成本而引起了广泛的关注。目前，Bi2WO6光催化剂的制备通常采用水热反应。水热法不仅是一种温和、简便的工艺，而且产品结晶度高，粒径可控。大量的研究结果表明，水热反应的溶液pH值对产物的组成有显著影响。当前驱体溶液的pH值达到一定的碱性时，晶体产物为Bi3.84W0.16O6.24。对于Bi3.84W0.16O6.24的研究和应用仍然较少。同时Bi2WO6和Bi3.84W0.16O6.24由于严重的电荷重组和弱光吸收，导致二氧化碳光还原活性较差。Bi2 WO6 is a promising photocatalyst that has attracted widespread attention due to its suitable band gap, stable structure, nontoxicity and low cost. At present, the preparation of Bi2 WO6 photocatalyst usually adopts hydrothermal reaction. The hydrothermal method is not only a gentle and simple process, but also the product has high crystallinity and controllable particle size. A large number of research results show that the pH value of the hydrothermal reaction solution has a significant impact on the composition of the product. When the pH value of the precursor solution reaches a certain alkalinity, the crystal product is Bi3.84 W0.16 O6.24 . There are still few studies and applications on Bi3.84 W0.16 O6.24 . At the same time, Bi2 WO6 and Bi3.84 W0.16 O6.24 have poor carbon dioxide photoreduction activity due to severe charge recombination and weak light absorption.
发明内容Contents of the invention
有鉴于此，本发明的目的之一在于提供一种卤素掺杂的Bi2WO6/Bi3.84W0.16O6.24催化剂的制备方法；本发明的目的之二在于提供所述方法制备的卤素掺杂的Bi2WO6/Bi3.84W0.16O6.24催化剂；本发明的目的之三在于提供所述卤素掺杂的Bi2WO6/Bi3.84W0.16O6.24催化剂在光还原CO2中的应用。In view of this, one object of the present invention is to provide a method for preparing a halogen-doped Bi2 WO6 /Bi3.84 W0.16 O6.24 catalyst; the second object of the present invention is to provide a halogen-doped catalyst prepared by the method Bi2 WO6 /Bi3.84 W0.16 O6.24 catalyst; The third object of the present invention is to provide the application of the halogen-doped Bi2 WO6 /Bi3.84 W0.16 O6.24 catalyst in the photoreduction of CO2 .
为达到上述目的，本发明提供如下技术方案：In order to achieve the above objects, the present invention provides the following technical solutions:
1、一种卤素掺杂的Bi2WO6/Bi3.84W0.16O6.24催化剂的制备方法，包含如下制备步骤：1. A method for preparing a halogen-doped Bi2 WO6 /Bi3.84 W0.16 O6.24 catalyst, including the following preparation steps:
1)将Bi(NO3)3·5H2O和Na2WO4·2H2O加入去离子水中；1) Add Bi(NO3 )3 ·5H2 O and Na2 WO4 ·2H2 O into deionized water;
2)加入NaCl，超声一定时间后搅拌得到不透明白色分散体；2) Add NaCl, ultrasonic for a certain period of time and then stir to obtain an opaque white dispersion;
3)用1M氢氧化钠溶液调节pH，搅拌一段时间；3) Adjust the pH with 1M sodium hydroxide solution and stir for a period of time;
4)将步骤3)中所得的溶液，转移到不锈钢高压釜中反应，洗涤、干燥得到Cl掺杂的Bi2WO6/Bi3.84W0.16O6.24，根据NaCl与Bi2WO6的重量比将所得样品分别命名为BWO/FBWO-Cl-1、BWO/FBWO-Cl-5、BWO/FBWO-Cl-10。4) Transfer the solution obtained in step 3) to a stainless steel autoclave for reaction, wash and dry to obtain Cl-doped Bi2 WO6 /Bi3.84 W0.16 O6.24 . According to the weight ratio of NaCl to Bi2 WO6 The obtained samples were named BWO/FBWO-Cl-1, BWO/FBWO-Cl-5, and BWO/FBWO-Cl-10.
本发明优选的，所述Bi(NO3)3·5H2O和Na2WO4·2H2O的摩尔比为2︰1。Preferably, the molar ratio of Bi(NO3 )3 ·5H2 O and Na2 WO4 ·2H2 O is 2:1.
本发明优选的，步骤3)中，所述pH为11-12。Preferably, in step 3) of the present invention, the pH is 11-12.
本发明优选的，步骤3)中，所述搅拌的时间为20-30min。Preferably, in step 3) of the present invention, the stirring time is 20-30 minutes.
本发明优选的，步骤4)中，所述反应的温度为150～180℃，时间为15-25h。Preferably, in step 4) of the present invention, the reaction temperature is 150-180°C and the reaction time is 15-25h.
2、权利要求1～5任一项所述方法制备的卤素掺杂的Bi2WO6/Bi3.84W0.16O6.24催化剂。2. The halogen-doped Bi2 WO6 /Bi3.84 W0.16 O6.24 catalyst prepared by the method of any one of claims 1 to 5.
3、权利要求6所述卤素掺杂的Bi2WO6/Bi3.84W0.16O6.24催化剂在光还原CO2中的应用。3. Application of the halogen-doped Bi2 WO6 /Bi3.84 W0.16 O6.24 catalyst described in claim 6 in the photoreduction of CO2 .
本发明的有益效果在于：The beneficial effects of the present invention are:
(1)本发明将Cl掺杂的Bi2WO6/Bi3.84W0.16O6.24光催化剂用于光催化CO2还原，具有较高的光催化二氧化碳还原能力，所制备的Cl掺杂的Bi2WO6/Bi3.84W0.16O6.24光催化剂具有比Bi2WO6和Bi3.84W0.16O6.24光催化剂更高的光催化CO2还原性能。(1) In the present invention, the Cl-doped Bi2 WO6 /Bi3.84 W0.16 O6.24 photocatalyst is used for photocatalytic CO2 reduction and has high photocatalytic carbon dioxide reduction ability. The prepared Cl-doped Bi2 WO6 /Bi3.84 W0.16 O6.24 photocatalyst has higher photocatalytic CO2 reduction performance than Bi2WO6 and Bi3.84W0.16O6.24 photocatalysts.
(2)本发明采用简单的水热法，通过调节前驱体的pH一步制备了Cl掺杂的Bi2WO6/Bi3.84W0.16O6.24光催化剂。该材料的光催化选择性高、制作成本低、生产工艺简单。(2) The present invention adopts a simple hydrothermal method to prepare the Cl-doped Bi2 WO6 /Bi3.84 W0.16 O6.24 photocatalyst in one step by adjusting the pH of the precursor. The material has high photocatalytic selectivity, low production cost and simple production process.
附图说明Description of the drawings
为了使本发明的目的、技术方案和有益效果更加清楚，本发明提供如下附图进行说明：In order to make the purpose, technical solutions and beneficial effects of the present invention clearer, the present invention provides the following drawings for illustration:
图1为制备得到的BWO、FBWO、BWO/FBWO、BWO/FBWO-Cl的XRD图；Figure 1 is the XRD pattern of the prepared BWO, FBWO, BWO/FBWO, and BWO/FBWO-Cl;
图2为制备得到的BWO/FBWO-Cl的TEM图；Figure 2 is a TEM image of the prepared BWO/FBWO-Cl;
图3为制备得到的BWO、FBWO、BWO/FBWO和BWO/FBWO-Cl催化剂的EDX图；Figure 3 is the EDX pattern of the prepared BWO, FBWO, BWO/FBWO and BWO/FBWO-Cl catalysts;
图4为所制备BWO、FBWO、BWO/FBWO和BWO/FBWO-Cl催化剂的紫外可见光吸收(UV-vis)图谱；Figure 4 shows the ultraviolet-visible light absorption (UV-vis) spectra of the prepared BWO, FBWO, BWO/FBWO and BWO/FBWO-Cl catalysts;
图5为制备得到的BWO/FBWO-Cl的光致发光光谱图；Figure 5 is the photoluminescence spectrum of the prepared BWO/FBWO-Cl;
图6为模拟太阳光照射下制备的BWO、FBWO、BWO/FBWO和BWO/FBWO-Cl催化剂还原CO2产生CO的产率。Figure 6 shows the yield of CO produced by reducing CO2 using BWO, FBWO, BWO/FBWO and BWO/FBWO-Cl catalysts prepared under simulated sunlight irradiation.
具体实施方式Detailed ways
下面结合附图和具体实施例对本发明作进一步说明，以使本领域的技术人员可以更好的理解本发明并能予以实施，但所举实施例不作为对本发明的限定。The present invention will be further described below in conjunction with the accompanying drawings and specific examples, so that those skilled in the art can better understand the present invention and implement it, but the examples are not intended to limit the present invention.
实施例1Example 1
Cl掺杂的Bi2WO6/Bi3.84W0.16O6.24催化剂的制备，具体方法如下：Preparation of Cl-doped Bi2 WO6 /Bi3.84 W0.16 O6.24 catalyst, the specific method is as follows:
(1)称取2mmol Bi(NO3)3·5H2O和1mmol Na2WO4·2H2O加入到75ml去离子水中；(1) Weigh 2mmol Bi(NO3 )3 ·5H2 O and 1mmol Na2 WO4 ·2H2 O and add them to 75ml of deionized water;
(2)然后加入NaCl，超声一定时间后搅拌得到不透明白色分散体；(2) Then add NaCl, ultrasonic for a certain period of time and then stir to obtain an opaque white dispersion;
(3)然后用1M氢氧化钠溶液调节pH＝11-12，搅拌30min；(3) Then adjust pH = 11-12 with 1M sodium hydroxide solution and stir for 30 minutes;
将步骤3)中所得的溶液，转移到不锈钢高压釜中，160℃下反应20h，洗涤、干燥得到Cl掺杂的Bi2WO6/Bi3.84W0.16O6.24，根据NaCl添加量占步骤1理论产物Bi2WO6的重量比1％、5％、10％，分别将制得的样品分别命名为BWO/FBWO-Cl-1、BWO/FBWO-Cl-5、BWO/FBWO-Cl-10。Transfer the solution obtained in step 3) to a stainless steel autoclave, react at 160°C for 20 hours, wash and dry to obtain Cl-doped Bi2 WO6 /Bi3.84 W0.16 O6.24 . According to the amount of NaCl added accounts for the theory in step 1 The weight ratio of the product Bi2 WO6 is 1%, 5%, and 10%, and the prepared samples are named BWO/FBWO-Cl-1, BWO/FBWO-Cl-5, and BWO/FBWO-Cl-10 respectively.
实施例2Example 2
Bi2WO6催化剂的制备，具体方法如下：Preparation of Bi2 WO6 catalyst, the specific method is as follows:
(1)称取2mmol Bi(NO3)3·5H2O和1mmol Na2WO4·2H2O加入到75ml去离子水中；(1) Weigh 2mmol Bi(NO3 )3 ·5H2 O and 1mmol Na2 WO4 ·2H2 O and add them to 75ml of deionized water;
(2)超声一定时间后搅拌得到不透明白色分散体；(2) Ultrasound for a certain period of time and then stir to obtain an opaque white dispersion;
(3)然后用1M氢氧化钠溶液调节pH＝9-11，搅拌30min；(3) Then adjust pH=9-11 with 1M sodium hydroxide solution and stir for 30 minutes;
(4)将步骤3)中所得的溶液，转移到不锈钢高压釜中，160℃下反应20h，洗涤、干燥得到Bi2WO6，制得的产品命名为BWO。(4) Transfer the solution obtained in step 3) to a stainless steel autoclave, react at 160°C for 20 hours, wash and dry to obtain Bi2 WO6 , and the obtained product is named BWO.
实施例3Example 3
Bi3.84W0.16O6.24催化剂的制备，具体方法如下：Preparation of Bi3.84 W0.16 O6.24 catalyst, the specific method is as follows:
(1)称取2mmol Bi(NO3)3·5H2O和1mmol Na2WO4·2H2O加入到75ml去离子水中；(1) Weigh 2mmol Bi(NO3 )3 ·5H2 O and 1mmol Na2 WO4 ·2H2 O and add them to 75ml of deionized water;
(2)然后超声一定时间后搅拌得到不透明白色分散体；(2) Then ultrasonic for a certain period of time and then stir to obtain an opaque white dispersion;
(3)然后用1M氢氧化钠溶液调节pH＝12-13，搅拌30min；(3) Then adjust the pH=12-13 with 1M sodium hydroxide solution and stir for 30 minutes;
(4)将步骤3)中所得的溶液，转移到不锈钢高压釜中，160℃下反应20h，洗涤、干燥得到Bi3.84W0.16O6.24，制得的产品命名为FBWO。(4) Transfer the solution obtained in step 3) to a stainless steel autoclave, react at 160°C for 20 hours, wash and dry to obtain Bi3.84 W0.16 O6.24 . The obtained product is named FBWO.
实施例4Example 4
Bi2WO6/Bi3.84W0.16O6.24催化剂的制备，具体方法如下：Preparation of Bi2 WO6 /Bi3.84 W0.16 O6.24 catalyst, the specific method is as follows:
(1)称取2mmol Bi(NO3)3·5H2O和1mmol Na2WO4·2H2O加入到75ml去离子水中；(1) Weigh 2mmol Bi(NO3 )3 ·5H2 O and 1mmol Na2 WO4 ·2H2 O and add them to 75ml of deionized water;
(2)超声一定时间后搅拌得到不透明白色分散体；(2) Ultrasound for a certain period of time and then stir to obtain an opaque white dispersion;
(3)然后用1M氢氧化钠溶液调节pH＝11-12，搅拌30min；(3) Then adjust pH = 11-12 with 1M sodium hydroxide solution and stir for 30 minutes;
(4)将步骤3)中所得的溶液，转移到不锈钢高压釜中，160℃下反应20h，洗涤、干燥得到Bi2WO6/Bi3.84W0.16O6.24，制得的产品命名为BWO/FBWO。(4) Transfer the solution obtained in step 3) to a stainless steel autoclave, react at 160°C for 20 hours, wash and dry to obtain Bi2 WO6 /Bi3.84 W0.16 O6.24 . The obtained product is named BWO/FBWO .
图1为本发明实施例实施例1～4所制备材料的XRD图。可以清楚的看出，实施例2所制备BWO材料的XRD衍射峰与标准卡片JCPDS No.73-2020相一致，表明所制备的样品是纯的Bi2WO6材料。实施例3所制备的FBWO的XRD衍射峰与标准卡片JCPDS No.43-0447相一致，表明所制备的样品是纯的Bi3.84W0.16O6.24材料。同时实施例1和4所制备的催化剂的XRD图中即观察到Bi2WO6衍射峰的同时也观察到Bi3.84W0.16O6.24的衍射峰。这证明成功制备了Bi2WO6和Bi3.84W0.16O6.24的复合催化剂。Figure 1 is an XRD pattern of the materials prepared in Examples 1 to 4 of the present invention. It can be clearly seen that the XRD diffraction peak of the BWO material prepared in Example 2 is consistent with the standard card JCPDS No. 73-2020, indicating that the prepared sample is a pure Bi2 WO6 material. The XRD diffraction peak of the FBWO prepared in Example 3 is consistent with the standard card JCPDS No. 43-0447, indicating that the prepared sample is a pure Bi3.84 W0.16 O6.24 material. At the same time, in the XRD patterns of the catalysts prepared in Examples 1 and 4, the diffraction peaks of Bi2 WO6 and Bi3.84 W0.16 O6.24 were also observed. This proves that the composite catalyst of Bi2 WO6 and Bi3.84 W0.16 O6.24 was successfully prepared.
图2是BWO/FBWO-Cl-5的TEM(图2，a-b)。图2，b的TEM图不仅发现了Bi2WO6的晶格条纹，还发现了Bi3.84W0.16O6.24的晶格条纹，并且在图中观察到了明显的界面接触。Figure 2 is the TEM of BWO/FBWO-Cl-5 (Figure 2, ab). In the TEM image of Figure 2, b, not only the lattice fringes of Bi2 WO6 were found, but also the lattice fringes of Bi3.84 W0.16 O6.24 were found, and obvious interface contact was observed in the picture.
图3是BWO/FBWO-Cl-5的EDX(图3，a-d)。EDX证明Cl元素均匀分布在BWO/FBWO-Cl中，证实Cl原子成功掺杂到材料里面，这进一步证明成功制备Cl掺杂BWO/FBWO复合催化剂。Figure 3 is the EDX of BWO/FBWO-Cl-5 (Figure 3, a-d). EDX proved that the Cl element was uniformly distributed in BWO/FBWO-Cl, confirming that Cl atoms were successfully doped into the material, which further proved the successful preparation of Cl-doped BWO/FBWO composite catalyst.
图4是将本发明实施例1～4制得的光催化剂进行紫外可见光吸收(UV-vis)测试分析。本发明实施例1制得的BWO/FBWO-Cl-5光催化剂具备更好的光吸收能力，有较高的光利用率。Figure 4 is an ultraviolet-visible light absorption (UV-vis) test and analysis of the photocatalysts prepared in Examples 1 to 4 of the present invention. The BWO/FBWO-Cl-5 photocatalyst prepared in Example 1 of the present invention has better light absorption capacity and higher light utilization rate.
图5是将本发明实施例1～4制得的光催化剂的光致发光光谱图。BWO/FBWO-Cl-5光催化剂的PL光谱发射峰的强度最弱，表明该光催化剂样品的电子-空穴对的复合速率低。这是由于异质结和Cl掺杂的协同作用，抑制了光生电子-空穴对的复合，从而提高了材料的光催化性能。Figure 5 is a photoluminescence spectrum chart of the photocatalyst prepared in Examples 1 to 4 of the present invention. The intensity of the PL spectrum emission peak of the BWO/FBWO-Cl-5 photocatalyst is the weakest, indicating that the recombination rate of electron-hole pairs of this photocatalyst sample is low. This is due to the synergistic effect of heterojunction and Cl doping, which inhibits the recombination of photogenerated electron-hole pairs, thereby improving the photocatalytic performance of the material.
实施例5Example 5
评估本发明制备材料的光催化性能通过Labsolar-6A设备((BeijingPerfectlight，中国)。所制备的材料在模拟太阳光照射下进行了光催化二氧化碳还原实验。首先我们需要制备测试样品，称取10mg样品放入玻璃瓶中，再加入1.0mL的去离子水，然后将含有样品的去离子水均匀地滴到玻璃纤维滤膜上面，在60℃下干燥。实验在250mL玻璃反应器中进行，使用300W Xe灯(PLS-300，Beijing Perfectlight，中国)。实验过程中，开启循环水使温度保持在20±0.03℃。开灯前，将反应器密封，然后用高纯度二氧化碳(≥99.999％)进行三次洗气，来去除O2和其他外来气体。洗气后，向反应器中充入91kPa压力的二氧化碳，随后将少量的水(100μL)注入反应器中。在反应过程中，每1小时用气相色谱(GC2002，CeChuang)和火焰电离检测器(FID)和热导检测器(TCD)进行分析。The photocatalytic performance of the materials prepared in the present invention was evaluated through Labsolar-6A equipment (BeijingPerfectlight, China). The prepared materials were subjected to photocatalytic carbon dioxide reduction experiments under simulated sunlight irradiation. First, we need to prepare test samples and weigh 10mg samples Put it into a glass bottle, then add 1.0mL of deionized water, and then drop the deionized water containing the sample evenly onto the glass fiber filter membrane, and dry it at 60°C. The experiment was carried out in a 250mL glass reactor, using 300W A Gas scrubbing to remove O2 and other external gases. After gas scrubbing, fill the reactor with carbon dioxide at a pressure of 91kPa, and then inject a small amount of water (100 μL) into the reactor. During the reaction, use the gas phase every 1 hour Chromatography (GC2002, CeChuang) and flame ionization detector (FID) and thermal conductivity detector (TCD) were used for analysis.
图6是本发明实施例1～4制得的光催化剂在模拟太阳光的照射5h后生成CO的产率。通过图片可以发现，Cl掺杂和异质结协同作用可以有效提高催化剂的催化性能。其中，BWO/FBWO-Cl-5有着最优异的光催化还原CO2转化性能，其光照5小时的CO产率约为6.27μmol·g-1。Figure 6 shows the yield of CO generated by the photocatalysts prepared in Examples 1 to 4 of the present invention after irradiation with simulated sunlight for 5 hours. It can be found from the pictures that the synergistic effect of Cl doping and heterojunction can effectively improve the catalytic performance of the catalyst. Among them, BWO/FBWO-Cl-5 has the most excellent photocatalytic reduction of CO2 conversion performance, and its CO yield after 5 hours of illumination is approximately 6.27 μmol·g-1 .
以上所述实施例仅是为充分说明本发明而所举的较佳的实施例，本发明的保护范围不限于此。本技术领域的技术人员在本发明基础上所作的等同替代或变换，均在本发明的保护范围之内。本发明的保护范围以权利要求书为准。The above-described embodiments are only preferred embodiments to fully illustrate the present invention, and the protection scope of the present invention is not limited thereto. Equivalent substitutions or transformations made by those skilled in the art on the basis of the present invention are within the protection scope of the present invention. The protection scope of the present invention shall be determined by the claims.
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| CN202311055086.3ACN117085711A (en) | 2023-08-21 | 2023-08-21 | A halogen-doped Bi2WO6/Bi3.84W0.16O6.24 catalyst and its preparation method and application |
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| CN202311055086.3ACN117085711A (en) | 2023-08-21 | 2023-08-21 | A halogen-doped Bi2WO6/Bi3.84W0.16O6.24 catalyst and its preparation method and application |
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|---|---|---|---|---|
| WO2001046208A2 (en)* | 1999-12-21 | 2001-06-28 | Monsanto Technology Llc | Use of a supplemental promoter in conjunction with a carbon-supported, noble-metal-containing catalyst in liquid phase oxidation reactions |
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