应用化学 ›› 2024, Vol. 41 ›› Issue (6): 839-850.DOI: 10.19894/j.issn.1000-0518.240018
陆志艳1, 陈雯轩1, 孙汪师诒1, 卓宁泽2, 魏潇1, 廖丽芳1, 许庆利1, 吴诗勇1()
收稿日期:
2024-01-18
接受日期:
2024-04-18
出版日期:
2024-06-01
发布日期:
2024-07-09
通讯作者:
吴诗勇
基金资助:
Zhi-Yan LU1, Wen-Xuan CHEN1, Wang-Shi-Yi SUN1, Ning-Ze ZHUO2, Xiao WEI1, Li-Fang LIAO1, Qing-Li XU1, Shi-Yong WU1()
Received:
2024-01-18
Accepted:
2024-04-18
Published:
2024-06-01
Online:
2024-07-09
Contact:
Shi-Yong WU
About author:
wsy@ecust.edu.cnSupported by:
摘要:
污泥焚烧过程中会产生SO2污染环境,通过添加钙基固硫剂可将硫固定在灰渣里,但是固硫效果受高温抑制。针对上述问题,采用共沉淀法制备了Ce-Mn/ZrO2复合催化剂,利用场发射扫描电子显微镜-能量色散X射线谱仪(FESEM-EDS)、透射电子显微镜(TEM)、X射线粉末衍射仪(XRD)和X射线光电子能谱仪(XPS)表征催化剂的组成和形貌。将催化剂与污泥、钙基固硫剂混合,在自动测硫仪上进行高温固硫实验,研究其固硫催化性能,借助热重分析和燃烧动力学参数拟合计算探究其催化机理。实验结果表明,催化剂中活性组分Ce、Mn在载体中高度分散,Ce-Mn之间的协同作用可以为催化剂表面提供更多的氧空位,促进SO2转变为SO3。当n(Ca)/n(S)=1.5时,Ce-Mn/ZrO2的质量分数为3.5%,燃烧温度为1000 ℃时,固硫率高达72.60%。Ce-Mn/ZrO2可以降低污泥燃烧着火点和反应活化能,促进污泥燃烧,稳定固硫产物。该催化剂具有优异的催化活性,在污泥焚烧脱硫领域具有十分广阔的应用前景。
中图分类号:
陆志艳, 陈雯轩, 孙汪师诒, 卓宁泽, 魏潇, 廖丽芳, 许庆利, 吴诗勇. Ce-Mn/ZrO2复合催化剂的制备及其固硫性能[J]. 应用化学, 2024, 41(6): 839-850.
Zhi-Yan LU, Wen-Xuan CHEN, Wang-Shi-Yi SUN, Ning-Ze ZHUO, Xiao WEI, Li-Fang LIAO, Qing-Li XU, Shi-Yong WU. Preparation of Ce-Mn/ZrO2 Composite Catalyst and Its Sulfur Fixation Performance[J]. Chinese Journal of Applied Chemistry, 2024, 41(6): 839-850.
Sample | Proximate analysis/%(mass percent) | Ultimate analysis/%(mass percent) | |||||||
---|---|---|---|---|---|---|---|---|---|
Mad | Aad | Vad | FCad | Cdaf | Hdaf | Odaf | Ndaf | Sdaf | |
Sludge | 3.78 | 49.23 | 42.84 | 4.15 | 50.00 | 9.17 | 29.74 | 6.48 | 4.61 |
表1 污泥工业分析和元素分析数据
Table 1 Proximate and ultimate analysis of sludge
Sample | Proximate analysis/%(mass percent) | Ultimate analysis/%(mass percent) | |||||||
---|---|---|---|---|---|---|---|---|---|
Mad | Aad | Vad | FCad | Cdaf | Hdaf | Odaf | Ndaf | Sdaf | |
Sludge | 3.78 | 49.23 | 42.84 | 4.15 | 50.00 | 9.17 | 29.74 | 6.48 | 4.61 |
图3 Ce-Mn/ZrO2的FESEM图像(A)、 TEM图像(B)、 FESEM放大图像(C)、 面扫描能谱图(D)及表面元素分布图(E)
Fig.3 FESEM images (A), TEM images (B), enlarged images by FESEM (C), EDS pattern(D) and surface elemental distribution diagram (E) of Ce-Mn/ZrO2
图4 Ce-Mn/ZrO2的XRD图谱(A)、 总XPS图谱(B)、 Ce3d图谱(C)和Mn2p图谱(D)
Fig.4 XRD pattern (A), XPS spectra (B), Ce3d XPS spectrum (C) and Mn2p XPS spectrum (D) of Ce-Mn/ZrO2
图8 不同n(Ca)/n(S)条件下,催化剂对固硫效果的影响A. 700 ℃; B. 800 ℃; C. 900 ℃; D. 1000 ℃
Fig.8 Effect of catalysts on sulfur-fixation efficiency under different n(Ca)/n(S) conditions with various tempetures
图10 污泥的TG/DTG图(A)、 各组试样的TG图(B)和各组试样的DTG图(C)
Fig.10 TG/DTG curves of sludge (A), TG curves of each group of samples (B) and DTG curves of each group of samples (C)
Sample | Ignition point/℃ | Combustion stage | Corresponding temperature range/℃ | Reaction order n | Fitting equation | Coefficient of determination R2 | E/ (kJ·mol-1) |
---|---|---|---|---|---|---|---|
Sludge | 218.00 | Before volatile peak 1 | 217.66~264.91 | 0.5 | y=-4 054.5x-6.071 9 | 0.963 4 | 33.71 |
After volatile peak 1 | 272.09~300.28 | 2 | y=-4 478.1x-4.757 4 | 0.975 6 | 37.23 | ||
After fixed carbon peak 2 | 400.72~467.43 | 2 | y=-6 627.9x-1.815 2 | 0.995 9 | 55.10 | ||
Sludge-Ca | 212.06 | Before volatile peak 1 | 220.92~263.66 | 0.5 | y=-3 358.7x-7.380 9 | 0.964 0 | 27.92 |
After volatile peak 1 | 275.01~305.03 | 2 | y=-4 358.9x-5.022 9 | 0.985 2 | 36.24 | ||
After fixed carbon peak 2 | 402.13~471.85 | 2 | y=-5 172.6x-4.066 5 | 0.987 3 | 43.01 | ||
Sludge-Ca-C | 206.21 | Before volatile peak 1 | 227.08~261.98 | 0.5 | y=-2 759.5x-8.640 5 | 0.981 0 | 22.94 |
After volatile peak 1 | 286.34~324.70 | 2 | y=-4 025.9x-5.875 0 | 0.993 2 | 33.47 | ||
After fixed carbon peak 2 | 396.46~457.86 | 2 | y=-3596.6x-6.6980 | 0.988 3 | 29.90 |
表2 试样燃烧动力学参数
Table 2 Kinetic parameters for combustion of sludge
Sample | Ignition point/℃ | Combustion stage | Corresponding temperature range/℃ | Reaction order n | Fitting equation | Coefficient of determination R2 | E/ (kJ·mol-1) |
---|---|---|---|---|---|---|---|
Sludge | 218.00 | Before volatile peak 1 | 217.66~264.91 | 0.5 | y=-4 054.5x-6.071 9 | 0.963 4 | 33.71 |
After volatile peak 1 | 272.09~300.28 | 2 | y=-4 478.1x-4.757 4 | 0.975 6 | 37.23 | ||
After fixed carbon peak 2 | 400.72~467.43 | 2 | y=-6 627.9x-1.815 2 | 0.995 9 | 55.10 | ||
Sludge-Ca | 212.06 | Before volatile peak 1 | 220.92~263.66 | 0.5 | y=-3 358.7x-7.380 9 | 0.964 0 | 27.92 |
After volatile peak 1 | 275.01~305.03 | 2 | y=-4 358.9x-5.022 9 | 0.985 2 | 36.24 | ||
After fixed carbon peak 2 | 402.13~471.85 | 2 | y=-5 172.6x-4.066 5 | 0.987 3 | 43.01 | ||
Sludge-Ca-C | 206.21 | Before volatile peak 1 | 227.08~261.98 | 0.5 | y=-2 759.5x-8.640 5 | 0.981 0 | 22.94 |
After volatile peak 1 | 286.34~324.70 | 2 | y=-4 025.9x-5.875 0 | 0.993 2 | 33.47 | ||
After fixed carbon peak 2 | 396.46~457.86 | 2 | y=-3596.6x-6.6980 | 0.988 3 | 29.90 |
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