技术领域technical field
本发明涉及催化剂领域，具体涉及一种用于CO2催化还原的异质结光催化剂及其制备。The invention relates to the field of catalysts, in particular to a heterojunction photocatalyst for catalytic reduction ofCO2 and its preparation.
背景技术Background technique
近年来，工业领域的不断发展和森林植被的严重破坏，导致CO2排放难以得到有效控制，严重威胁着人类的生存和发展。在众多应对方案中，光催化技术的发展是解决二氧化碳环境污染问题的一种有效途径。目前，光催化还原二氧化碳转化为CH4等有用物质的研究引起了世界各国研究团队的关注。许多光催化剂已被科学家研究和开发并应用于生产生活，其中g-C3N4由于具有适宜的禁带宽度(2.7eV)、制备简单方便、可见光响应性好、易与其他物质复合等优点而得到广泛应用。然而，我们应当注意到，由于单独的g-C3N4作为光催化剂，光生电子空穴对易于复合，所以催化活性不太好，导致CH4的产量偏低。因此，更好质量的光催化剂的开发是我们目前任务的重点。In recent years, the continuous development of the industrial field and the severe destruction of forest vegetation have made it difficult to effectively controlCO2 emissions, which seriously threatens the survival and development of human beings. Among many solutions, the development of photocatalytic technology is an effective way to solve the problem of carbon dioxide environmental pollution. At present, the research on photocatalytic reduction of carbon dioxide into useful substances such asCH4 has attracted the attention of research teams from all over the world. Many photocatalysts have been researched and developed by scientists and applied to production and life. Among them, gC3 N4 is obtained due to its suitable band gap (2.7eV), simple and convenient preparation, good response to visible light, and easy compounding with other substances. widely used. However, we should note that the photogenerated electron-hole pairs are easy to recombine because gC3 N4 alone acts as a photocatalyst, so the catalytic activity is not very good, resulting in low CH4 production. Therefore, the development of better quality photocatalysts is the focus of our current task.
发明内容Contents of the invention
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种用于CO2催化还原的异质结光催化剂及其制备。The object of the present invention is to provide a heterojunction photocatalyst for catalytic reduction ofCO2 and its preparation in order to overcome the defects of the above-mentioned prior art.
本发明的目的可以通过以下技术方案来实现：一种用于CO2催化还原的异质结光催化剂，该催化剂包括g-C3N4本体以及掺杂在g-C3N4内的Bi2O3，其中，所述Bi2O3的质量百分比为20％～80％。The purposeof the present invention can be achieved through the following technical solutions: a heterojunction photocatalyst forCO2 catalytic reduction, the catalyst includesgC3N4 body andBi2O3doped ingC3N4 , Wherein, the mass percentage of the Bi2 O3 is 20%-80%.
Bi2O3/g-C3N4复合物之间可以形成异质结结构产生内部电场，从而加快电子载流子的迁移、降低电子空穴复合率，因而提升光催化活性。Bi2 O3 /gC3 N4 complexes can form a heterojunction structure to generate an internal electric field, thereby accelerating the migration of electron carriers and reducing the electron-hole recombination rate, thus improving the photocatalytic activity.
一种如上所述用于CO2催化还原的异质结光催化剂的制备方法，包括以下步骤：A method for preparing a heterojunction photocatalyst forCO catalytic reduction as described above, comprising the following steps:
(1)将尿素以30～40r/min的速度研磨2～4h，然后烧结，冷却后研磨，得到g-C3N4；(1) Grinding urea at a speed of 30-40r/min for 2-4 hours, then sintering, cooling and grinding to obtain gC3 N4 ;
(2)将得到的g-C3N4置于乙二醇中并超声30min进行溶解，然后加入Bi(NO3)3·5H2O和尿素，以400～600r/min速率搅拌30min得到均匀溶液，然后热处理，洗涤、烘干，最后进行煅烧，即得所述用于CO2催化还原的异质结光催化剂。(2) Put the obtained gC3 N4 in ethylene glycol and ultrasonically dissolve it for 30 minutes, then add Bi(NO3 )3 5H2 O and urea, stir at 400-600 r/min for 30 minutes to obtain a uniform solution, Then heat treatment, washing, drying, and finally calcination to obtain the heterojunction photocatalyst for catalytic reduction of CO2 .
通过烧结，将尿素转化成g-C3N4，然后通过溶解，使得g-C3N4与Bi(NO3)3·5H2O充分混合，经热处理将乙二醇除去，煅烧使得Bi(NO3)3·5H2O转化成Bi2O3并与g-C3N4形成异质结，从而提高光催化活性。Through sintering, urea is converted into gC3 N4 , and then gC3 N4 is fully mixed with Bi(NO3 )3 ·5H2 O through dissolution, ethylene glycol is removed by heat treatment, and Bi(NO3 ) is calcined.3 5H2 O is transformed into Bi2 O3 and forms a heterojunction with gC3 N4 , thereby enhancing the photocatalytic activity.
所述尿素研磨成粒径为100μm以下的粉末状尿素，该粒径下的尿素烧结更充分。The urea is ground into powdered urea with a particle size below 100 μm, and the urea with this particle size is more fully sintered.
所述烧结的工艺如下：以12～18℃/min的速率加热至380～420℃，然后保温2～3h，用相同的加热速率升高至550～580℃，然后再保温2～3h。The sintering process is as follows: heating to 380-420° C. at a rate of 12-18° C./min, then keeping it for 2-3 hours, raising it to 550-580° C. at the same heating rate, and then keeping it for 2-3 hours.
所述g-C3N4与Bi(NO3)3·5H2O及尿素的质量比为1：(0.2～0.8)：2。The mass ratio of gC3 N4 to Bi(NO3 )3 ·5H2 O and urea is 1:(0.2-0.8):2.
所述热处理为在高压釜内以180～200℃温度水热处理12～18h。The heat treatment is a hydrothermal treatment at a temperature of 180-200° C. for 12-18 hours in an autoclave.
所述洗涤采用去离子水，烘干温度为80～110℃，烘干时间为12～24h。The washing uses deionized water, the drying temperature is 80-110° C., and the drying time is 12-24 hours.
所述煅烧的温度为360～400℃，煅烧时间为2～3h。The calcination temperature is 360-400° C., and the calcination time is 2-3 hours.
与现有技术相比，本发明的有益效果体现在以下几方面：Compared with the prior art, the beneficial effects of the present invention are reflected in the following aspects:
(1)制备方法简单、成本低，适合大规模工业化生产；(1) The preparation method is simple, the cost is low, and it is suitable for large-scale industrial production;
(2)选择Bi2O3与g-C3N4构建异质结，有效降低了电子空穴对复合率，对于光催化剂的CO2还原能力有了很大的提高；(2) Selecting Bi2 O3 and gC3 N4 to build a heterojunction can effectively reduce the recombination rate of electron-hole pairs, and greatly improve the CO2 reduction ability of the photocatalyst;
(3)采用水热法形成异质结结构可以极大提高催化剂的比表面积进而提高催化剂的CO2催化还原性能。(3) The formation of the heterojunction structure by the hydrothermal method can greatly increase the specific surface area of the catalyst, thereby improving theCO2 catalytic reduction performance of the catalyst.
附图说明Description of drawings
图1为本发明不同质量分数的Bi2O3掺杂的g-C3N4的XRD图谱；Fig. 1 is the XRD spectrum of gC3 N4 doped with Bi2 O3 of different mass fractions of the present invention;
图2为本发明不同质量分数的Bi2O3掺杂的g-C3N4的活性图谱。Fig. 2 is the activity spectrum of gC3 N4 doped with Bi2 O3 in different mass fractions of the present invention.
具体实施方式Detailed ways
下面对本发明的实施例作详细说明，本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。The following is a detailed description of the embodiments of the present invention. This embodiment is implemented on the premise of the technical solution of the present invention, and detailed implementation methods and specific operating procedures are provided, but the protection scope of the present invention is not limited to the following implementation example.
实施例1Example 1
g-C3N4粉体的制备：称量25g的尿素放入玻璃研钵中，用力研磨2个小时，转移至氧化铝坩埚中用铝箔纸包裹密封，以16度/分钟的速率加热至400度然后保温2小时，用相同的加热速率升高至550度然后再保温2小时。将坩埚自然冷却至室温，研磨所得浅黄色粉末即g-C3N4。Preparation of gC3 N4 powder: Weigh 25g of urea into a glass mortar, grind vigorously for 2 hours, transfer to an alumina crucible, wrap and seal with aluminum foil, and heat to 400°C at a rate of 16°C/min Then hold for 2 hours, use the same heating rate to increase to 550 degrees and hold for another 2 hours. The crucible was naturally cooled to room temperature, and the obtained light yellow powder, gC3 N4 , was ground.
20wt％Bi2O3掺杂g-C3N4异质结光催化剂的制备：称量0.5g的g-C3N4，将其溶解在60ml乙二醇中并超声处理30分钟，获得片状g-C3N4。随后向该溶液中加入0.104g的Bi(NO3)3·5H2O和1g的尿素，剧烈搅拌30分钟以获得均匀溶液。将该溶液在聚四氟乙烯衬里的高压釜中以180度水热处理12小时。所得产物用去离子水洗涤数次并在80～100℃下烘干。然后将该水热产物在380℃的空气中煅烧2小时，最终获得20wt％Bi2O3掺杂的g-C3N4异质结光催化剂。Preparation of 20wt%Bi2O3- dopedgC3N4 heterojunction photocatalyst: 0.5 gofgC3N4 was weighed, dissolved in 60 ml of ethylene glycol and sonicated for30 min to obtain flakegC3 N4 . Then 0.104 g of Bi(NO3 )3 ·5H2 O and 1 g of urea were added to the solution, and stirred vigorously for 30 minutes to obtain a homogeneous solution. The solution was hydrothermally treated at 180°C for 12 hours in a Teflon-lined autoclave. The obtained product was washed several times with deionized water and dried at 80-100°C. The hydrothermal product was then calcined in air at 380 °C for2 h to finally obtain a 20 wt%Bi2O3- dopedgC3N4 heterojunction photocatalyst.
实施例2Example 2
采用于是实施例1相同的g-C3N4制备方法，不同之处在于：Adopt then embodiment 1 same gC3 N4 preparation method, difference is:
40wt％Bi2O3掺杂g-C3N4异质结光催化剂的制备：称量0.5g的g-C3N4，将其溶解在60ml乙二醇中并超声处理30分钟，获得片状g-C3N4。随后向该溶液中加入0.208g的Bi(NO3)3·5H2O和1g的尿素，剧烈搅拌30分钟以获得均匀溶液。将该溶液在聚四氟乙烯衬里的高压釜中以180℃水热处理12小时。所得产物用去离子水洗涤数次并在80～100℃下烘干。然后将该水热产物在380℃的空气中煅烧2小时，最终获得40wt％Bi2O3掺杂的g-C3N4异质结光催化剂。Preparation of 40wt%Bi2O3- dopedgC3N4 heterojunction photocatalyst: 0.5 gofgC3N4 was weighed, dissolved in 60 ml of ethylene glycol and sonicated for30 min to obtain flakegC3 N4 . Then 0.208 g of Bi(NO3 )3 ·5H2 O and 1 g of urea were added to the solution, and vigorously stirred for 30 minutes to obtain a homogeneous solution. The solution was hydrothermally treated at 180°C for 12 hours in a Teflon-lined autoclave. The obtained product was washed several times with deionized water and dried at 80-100°C. The hydrothermal product was then calcined in air at 380 °C for 2 h to finally obtain a40 wt%Bi2O3- dopedgC3N4 heterojunction photocatalyst.
实施例3Example 3
采用于是实施例1相同的g-C3N4制备方法，不同之处在于：Adopt then embodiment 1 same gC3 N4 preparation method, difference is:
60wt％Bi2O3掺杂g-C3N4异质结光催化剂的制备：称量0.5g的g-C3N4，将其溶解在60ml乙二醇中并超声处理30分钟，获得片状g-C3N4。随后向该溶液中加入0.312g的Bi(NO3)3·5H2O和1g的尿素，剧烈搅拌30分钟以获得均匀溶液。将该溶液在聚四氟乙烯衬里的高压釜中以180度水热处理12小时。所得产物用去离子水洗涤数次并在80～100℃下烘干。然后将该水热产物在380℃的空气中煅烧2小时，最终获得60wt％Bi2O3掺杂的g-C3N4异质结光催化剂。Preparation of 60 wt%Bi2O3 dopedgC3N4heterojunction photocatalyst: Weigh 0.5 gofgC3N4 , dissolve it in 60 ml of ethylene glycol and sonicate for30 min to obtain flakegC3 N4 . Then 0.312 g of Bi(NO3 )3 ·5H2 O and 1 g of urea were added to the solution, and vigorously stirred for 30 minutes to obtain a homogeneous solution. The solution was hydrothermally treated at 180°C for 12 hours in a Teflon-lined autoclave. The obtained product was washed several times with deionized water and dried at 80-100°C. The hydrothermal product was then calcined in air at 380 °C for2 h to finally obtain a 60 wt%Bi2O3- dopedgC3N4 heterojunction photocatalyst.
实施例4Example 4
采用于是实施例1相同的g-C3N4制备方法，不同之处在于：Adopt then embodiment 1 same gC3 N4 preparation method, difference is:
80wt％Bi2O3掺杂g-C3N4异质结光催化剂的制备：称量0.5g的g-C3N4，将其溶解在60ml乙二醇中并超声处理30分钟，获得片状g-C3N4。随后向该溶液中加入0.416g的Bi(NO3)3·5H2O和1g的尿素，剧烈搅拌30分钟以获得均匀溶液。将该溶液在聚四氟乙烯衬里的高压釜中以180度水热处理12小时。所得产物用去离子水洗涤数次并在80～100℃下烘干。然后将该水热产物在380℃的空气中煅烧2小时，最终获得80wt％Bi2O3掺杂的g-C3N4异质结光催化剂。Preparation of 80wt%Bi2O3- dopedgC3N4 heterojunction photocatalyst: 0.5 gofgC3N4 was weighed, dissolved in 60 ml of ethylene glycol and sonicated for30 min to obtain flakegC3 N4 . Then 0.416 g of Bi(NO3 )3 ·5H2 O and 1 g of urea were added to the solution, and vigorously stirred for 30 minutes to obtain a homogeneous solution. The solution was hydrothermally treated at 180°C for 12 hours in a Teflon-lined autoclave. The obtained product was washed several times with deionized water and dried at 80-100°C. The hydrothermal product was then calcined in air at 380 °C for2 h to finally obtain 80 wt%Bi2O3- dopedgC3N4 heterojunction photocatalyst.
将上述实施例得到的催化剂以及g-C3N4进行XRD衍射，得到结果如图1所示，我们可以观察到27.3°处的衍射峰，归属于g-C3N4(JCPDS 87-1526)的(002)峰面。在12.7°处的衍射峰代表(100)峰，其与g-C3N4的报道结果非常吻合。制备的Bi2O3在2θ＝27.8°，31.7°，32.6°，46.2°，55.4°和74.4°处对应于(201)，(002)，(220)，(222)，(421)和(423)六个主峰。这与粉末衍射标准联合委员会数据(JCPDS 65-1209)一致。可以看出，随着复合光催化材料中Bi2O3含量的增加，g-C3N4的峰值强度变弱，而Bi2O3的峰值则随着掺杂量的增加变得更强。可以发现，27.8°处的衍射峰明显随着掺杂量的增加而变强，同时，由于Bi2O3和g-C3N4之间形成了异质结结构，因而峰面发生一定程度的偏移。The catalyst and gC3 N4 obtained in the above examples were subjected to XRD diffraction, and the obtained results are shown in Figure 1. We can observe the diffraction peak at 27.3°, which belongs to the( 002 ) peak surface.The diffraction peak at 12.7° represents the (100) peak, which is in good agreement with the reported results forgC3N4 .The as-preparedBi2O3 corresponds to (201), (002), (220), (222), (421) and ( 423) six main peaks. This is consistent with the Joint Committee on Powder Diffraction Standards data (JCPDS 65-1209). It can be seen that with the increaseofBi2O3 content in the composite photocatalytic material, the peak intensity ofgC3N4 becomesweaker , while the peakofBi2O3 becomes stronger with the increase of doping amount. It can be found that the diffraction peak at 27.8° becomes stronger with the increase of doping amount, and at the same time, due to the formation of a heterojunction structure between Bi2 O3 and gC3 N4 , the peak surface is deviated to a certain extent. shift.
将上述实施例得到的催化剂以及g-C3N4进行CO2的催化电解反应，CO2光催化还原反应在从Perfect Light Company(中国，北京)购买的500mL反应器的气体封闭循环系统中进行。在反应过程中，用300W氙弧灯用作光源，在充分搅拌下将50mg光催化剂均匀分散至100mL去离子水中。照明前，将悬浮液进行真空处理，然后将CO2(99.999％)用质量流量计控制流量，均匀通入悬浮液中，压力为100kPa，并保持30分钟以达到吸附-解吸平衡。然后放上光源进行实验。反应器温度和压力分别保持在25℃和100kPa。在反应过程中，每小时从玻璃室采样0.15mL气体，以通过气相色谱(GC-2010Plus，SHIMADZU，日本)检测碳基气体产物。考察5中产品的火星，其结果如图2所示，我们可以看到，掺杂Bi2O3的g-C3N4的活性比g-C3N4高，且掺杂量为405％时最高。The catalyst obtained in the above examples and gC3 N4 were subjected to the catalytic electrolysis reaction of CO2 , and the photocatalytic reduction reaction of CO2 was carried out in a gas closed circulation system of a 500 mL reactor purchased from Perfect Light Company (China, Beijing). During the reaction process, a 300W xenon arc lamp was used as a light source, and 50 mg of the photocatalyst was uniformly dispersed into 100 mL of deionized water with sufficient stirring. Before lighting, the suspension was subjected to vacuum treatment, and then CO2 (99.999%) was uniformly passed into the suspension with a mass flow meter to control the flow rate, and the pressure was 100kPa, and kept for 30 minutes to achieve adsorption-desorption equilibrium. Then put on the light source to experiment. The reactor temperature and pressure were maintained at 25 °C and 100 kPa, respectively. During the reaction, 0.15 mL of gas was sampled from the glass chamber every hour to detect carbon-based gas products by gas chromatography (GC-2010Plus, SHIMADZU, Japan). Investigating the Mars of the product in 5, the results are shown in Figure 2. We can see that the activity of gC3 N 4 doped with Bi 2 O 3 is higher than that of gC 3N 4,andtheactivity is the highest when the doping amount is 405%.
实施例5Example 5
采用与实施例2相同的原料及配比，采用类似的制备方法，不同之处在于：Adopt the raw material identical with embodiment 2 and proportioning, adopt similar preparation method, difference is:
(1)烧结条件不同：以12℃/min的速率加热至380℃，然后保温3h，用相同的加热速率升高至580℃，然后再保温2h；(1) The sintering conditions are different: heat to 380°C at a rate of 12°C/min, then hold for 3h, raise to 580°C with the same heating rate, and then hold for 2h;
(2)热处理条件不同：以180℃温度水热处理18h；(2) Different heat treatment conditions: hydrothermal treatment at 180°C for 18 hours;
(3)烘干条件不同：烘干温度为80℃，烘干时间为24h；(3) The drying conditions are different: the drying temperature is 80°C, and the drying time is 24 hours;
(4)煅烧条件不同：煅烧的温度为360℃，煅烧时间为3h。(4) The calcination conditions are different: the calcination temperature is 360°C, and the calcination time is 3h.
得到的40wt％Bi2O3掺杂的g-C3N4异质结光催化剂，经检验，具有良好的催化活性。The obtained 40wt% Bi2 O3 doped gC3 N4 heterojunction photocatalyst has good catalytic activity after inspection.
实施例6Example 6
采用与实施例2相同的原料及配比，采用类似的制备方法，不同之处在于：Adopt the raw material identical with embodiment 2 and proportioning, adopt similar preparation method, difference is:
(1)烧结条件不同：以18℃/min的速率加热至420℃，然后保温2h，用相同的加热速率升高至550℃，然后再保温3h；(1) The sintering conditions are different: heating to 420°C at a rate of 18°C/min, then holding for 2h, increasing to 550°C at the same heating rate, and then holding for 3h;
(2)热处理条件不同：以200℃温度水热处理12h；(2) Different heat treatment conditions: hydrothermal treatment at 200°C for 12 hours;
(3)烘干条件不同：烘干温度为110℃，烘干时间为12h；(3) The drying conditions are different: the drying temperature is 110°C, and the drying time is 12h;
(4)煅烧条件不同：煅烧的温度为400℃，煅烧时间为2h。(4) The calcination conditions are different: the calcination temperature is 400°C, and the calcination time is 2h.
得到的40wt％Bi2O3掺杂的g-C3N4异质结光催化剂，经检验，具有良好的催化活性。The obtained 40wt% Bi2 O3 doped gC3 N4 heterojunction photocatalyst has good catalytic activity after inspection.
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| CN111036223A (en)* | 2019-12-19 | 2020-04-21 | 江南大学 | A kind of Bi2O3/BiFeO3 nanofiber composite photocatalyst and preparation method thereof |
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| CN114452989A (en)* | 2022-01-30 | 2022-05-10 | 江苏大学 | A kind of porous structure carbon nitride composite catalyst and its preparation method and application |
| CN115364874A (en)* | 2022-04-20 | 2022-11-22 | 南昌航空大学 | A method for preparing composite photocatalytic materials by one-pot hydrothermal construction of heterojunction |
| CN116371447A (en)* | 2023-04-21 | 2023-07-04 | 上海电力大学 | double-Z heterojunction photocatalyst and preparation method and application thereof |
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