Performance study on visible-light catalytic conversion of low concentration coalmine gas to methanol with Z-type heterojunction Ag2S/AgVO3
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摘要:
因缺乏合理有效的利用途径，大量低浓度瓦斯（${C_{{\rm{C}}{{\rm{H}}_{\rm{4}}}}} $< 30%）被直接排放，研究开发低浓度瓦斯高值转化利用方法和技术对保障煤矿安全生产与减缓温室效应具有重要意义，也是实现我国“双碳”战略目标必不可缺少的部分。以低浓度瓦斯为碳源制取液体燃料甲醇被认为是其理想的利用途径之一，以清洁太阳能为驱动力的光催化技术可在室温常压下活化转化甲烷，为低浓度瓦斯低碳利用提供新途径。首先采用水热法制备AgVO3，以硫代乙酰胺为硫源，通过阴离子交换策略在AgVO3表面原位复合Ag2S，构筑出Ag2S/AgVO3异质结，改变硫代乙酰胺的用量可调控Ag2S复合比例。利用XRD、SEM、TEM和紫外可见漫反射光谱等对复合催化剂的微观结构进行表征分析，以体积比为1∶12的甲烷/空气混合物模拟低浓度瓦斯，系统研究了Ag2S复合比例、氧化剂用量、光照强度等对甲烷转化、甲醇产生及其选择性的影响规律，借助瞬态光电流响应谱和电子顺磁共振谱（EPR）探究了Z型异质结构Ag2S/AgVO3对增强模拟瓦斯转化性能的内在机理。研究结果表明：所制AgVO3呈纤维状形貌，其晶相结构为单斜相，原位复合的Ag2S呈纳米颗粒形态，其平均粒径为60 nm，且Ag2S颗粒均匀分布于AgVO3纤维表面。与单一AgVO3和Ag2S相比，复合材料Ag2S/AgVO3具有更强的光吸收性能，AgVO3的带隙能、价带与导带电势分别为2.08 eV、2.21 V和0.13 V，Ag2S的带隙能、价带与导带电势分别为0.91 eV、0.34 V和−0.57 V。与AgVO3相比，复合催化剂Ag2S/AgVO3具有显著增强的瓦斯转化性能，可见光照射1 h最优催化剂20% Ag2S/AgVO3的甲烷转化和甲醇产生量为3.10 mmol/g和2.45 mmol/g，分别为单一AgVO3的1.72倍与2.63倍，且其甲醇选择性高达78.9%；6次循环试验结果表明：Ag2S/AgVO3具有优异的催化稳定性。能带结构分析与EPR测试结果表明：Ag2S/AgVO3异质结遵循Z型电荷迁移机制，这不仅增强了光生电荷的空间分离，同时使其具有较强的氧化/还原能力，显著提升低浓度瓦斯定向转化制取甲醇的催化性能，为低浓度瓦斯低碳高效利用提供新思路。
Abstract:Large number of low-concentration gas (${C_{{\rm{C}}{{\rm{H}}_{\rm{4}}}}} $< 30%) is discharged directly due to the lack of reasonable and effective utilization pathways. Research and development of high-value conversion and utilization methods and technologies for low-concentration gas is of great significance to ensure the safe production in coal seams and mitigate the greenhouse effect, and it is also an indispensable part of realizing China’s “double carbon” strategic goal. The production of liquid fuel methanol from low-concentration gas as a carbon source is considered to be one of the ideal utilization pathways. Photocatalytic technology driven by clean solar energy can activate and convert methane at room temperature and atmospheric pressure, providing a novel approach for low-carbon utilization of low-concentration gas. AgVO3 was firstly prepared by hydrothermal method. Ag2S/AgVO3 heterojunction was constructed by in-situ decoration of Ag2S on the surface of AgVO3 via ion exchange strategy using thioacetamide as a sulfur source. Molar ratio of Ag2S could be regulated by varying the amount of thioacetamide. The microstructure of composite catalysts was characterized using XRD, SEM, TEM and UV-Vis diffuse reflectance spectroscopy. A methane-air mixture with a volume ratio of 1∶12 was used as the simulated low-concentration gas, and the effects of Ag2S compound ratio, oxidant concentration and light intensity on methane conversion, methanol productivity and selectivity were systematically investigated. The intrinsic mechanism of Z-type heterojunction Ag2S/AgVO3 for enhancing the conversion performance of simulated gas was explored by means of transient photocurrent response spectroscopy and electron paramagnetic resonance (EPR) spectroscopy. The results indicated that, the prepared AgVO3 shown a fibrous morphology with monoclinic crystalline phase structure. The in-situ composite Ag2S was in the form of nanoparticles with an average particle size of 60 nm, and the Ag2S particles were uniformly distributed on the surface of AgVO3 fibers. Composite Ag2S/AgVO3 exhibited enhanced light absorption compared to single AgVO3 and Ag2S. The bandgap energy, valence band and conduction band potentials of AgVO3 were 2.08 eV, 2.21 V and 0.13 V, and those of Ag2S were 0.91 eV, 0.34 V and −0.57 V, respectively. The composite catalyst Ag2S/AgVO3 shown significantly enhanced gas conversion performance compared to AgVO3. The methane conversion and methanol production of the optimal catalyst 20% Ag2S/AgVO3 irradiated with visible light for 1 h was 3.10 mmol/g and 2.45 mmol/g, which was 1.72 times and 2.63 times higher than that of the single AgVO3, respectively, and the methanol selectivity was up to 78.9%. The result of 6 cyclic tests shown the excellent catalytic stability of Ag2S/AgVO3. The results of energy band structure analysis and EPR test shown that, the Ag2S/AgVO3 heterojunction followed the Z-type charge transfer mechanism, which not only enhanced the spatial separation of photogenerated charges, but also maintained strong oxidation-reduction ability, which significantly improved the catalytic performance in the directional conversion of low concentration gas to methanol, and provided a novel idea for the high-efficiency utilization of low-concentration gas in a low-carbon way.
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图 1 Ag2S/AgVO3异质结光催化剂的制备流程
Figure 1. Preparation of Ag2S/AgVO3 heterojunction photocatalysts
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图 2 低浓度瓦斯光催化转化制甲醇试验系统示意
Figure 2. Experimental system for photocatalytic conversion of low-concentration coal mine gas to methanol
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图 3 单一AgVO3和复合材料Ag2S/AgVO3的XRD图
Figure 3. XRD patterns of AgVO3 and Ag2S/AgVO3 composites
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图 4 单一AgVO3、Ag2S和复合材料Ag2S/AgVO3的SEM图
Figure 4. SEM images of single AgVO3, Ag2S and composites Ag2S/AgVO3
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图 5 复合材料20% Ag2S/AgVO3的TEM图、HRTEM图和EDS元素mapping图
Figure 5. TEM, HRTEM and EDS elemental mapping images of 20% Ag2S/AgVO3 composite
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图 6 催化材料的紫外−可见漫反射光谱、Tauc曲线和莫特−肖特基曲线
Figure 6. UV-Vis DRS, Tauc plots and Mott-Schottky curves of catalyst materials
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图 7 复合光催化剂Ag2S/AgVO3的低浓度瓦斯转化性能
Figure 7. Conversion performance of low-concentration coalmine gas over Ag2S/AgVO3 photocatalyst
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图 8 H2O2浓度和光照强度对20% Ag2S/AgVO3瓦斯转化性能的影响
Figure 8. Effects of H2O2 concentration and light intensity on conversion performance of simulated gas over 20% Ag2S/AgVO3 catalyst
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图 9 复合催化剂20% Ag2S/AgVO3的循环稳定性试验
Figure 9. Cyclic stability test of 20% Ag2S/AgVO3 photocatalyst
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图 10 不同波长光源照射下20% Ag2S/AgVO3的表观量子效率和甲醇产生速率
Figure 10. Apparent quantum efficiency and CH3OH production rate of 20% Ag2S/AgVO3 under irradiation of different wavelength incident light
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图 11 AgVO3、Ag2S和20% Ag2S/AgVO3的瞬态光电流响应谱
Figure 11. Transient photocurrent response spectra of AgVO3、Ag2S和20% Ag2S/AgVO3
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图 12 AgVO3、Ag2S和20% Ag2S/AgVO3悬浮液光照3 min的EPR谱图
Figure 12. EPR spectra of AgVO3、Ag2S和20% Ag2S/AgVO3 suspension with irradiation for 3 min
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图 13 Ag2S/AgVO3异质结的能带结构和性能增强机理
Figure 13. Band structure and performance enhancement mechanism of Ag2S/AgVO3 heterojunction
表 1 用于光催化转化甲烷制甲醇的各种催化剂性能比较
Table 1 Performance comparison of various catalysts for photocatalytic conversion of methane to methanol
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表 2 复合催化剂Ag2S/AgVO3的反应活性中心物质的量
Table 2 Molar number of reaction active center of the composite catalysts Ag2S/AgVO3
复合催化剂 Ag2S还原活性中心
物质的量/μmolAgVO3氧化活性中心
物质的量/μmol5% Ag2S/AgVO3 2.49 45.36 10% Ag2S/AgVO3 5.01 42.29 20% Ag2S/AgVO3 10.05 36.27 30% Ag2S/AgVO3 14.50 30.95
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