水热合成一锅法制备FePO4-SBA-15及其水热稳定性能

doi:10.1016/S1872-2067(14)60202-3

催化学报 ›› 2015, Vol. 36 ›› Issue (3): 446-453.DOI: 10.1016/S1872-2067(14)60202-3

• 论文 • 上一篇

水热合成一锅法制备FePO₄-SBA-15及其水热稳定性能

王润琴^a,c, 林荣和^a, 丁云杰^a,b, 刘佳^a,c, 罗文婷^a,c, 杜虹^a,c, 吕元^a

a 中国科学院大连化学物理研究所洁净能源国家实验室(筹), 辽宁大连116023;
b 中国科学院大连化学物理研究所催化基础国家重点实验室, 辽宁大连116023;
c 中国科学院大学, 北京100049

收稿日期:2014-10-09 修回日期:2014-11-18 出版日期:2015-02-14 发布日期:2015-02-14
通讯作者: 丁云杰
基金资助:
国家自然科学基金(21103170).

Highly hydrothermally stable FePO₄-SBA-15 synthesized using a novel one-pot hydrothermal method

Runqin Wang^a,c, Ronghe Lin^a, Yunjie Ding^a,b, Jia Liu^a,c, Wenting Luo^a,c, Hong Du^a,c, Yuan Lü^a

a Dalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China;
b State Key Laboratory of Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China;
c University of Chinese Academy of Sciences, Beijing 100049, China

Received:2014-10-09 Revised:2014-11-18 Online:2015-02-14 Published:2015-02-14
Supported by:
This work was supported by the National Natural Science Foundation of China (21103170).

摘要/Abstract

摘要：

通过两种水热处理方式, 即800 ℃水汽条件和100 ℃沸水处理, 考察了一锅法制备的FePO₄-SBA-15 (OP)的水热稳定性.水热处理前后样品的结构变化通过小角X射线衍射和N₂物理吸附表征.研究发现, 经水热条件下原位生成FePO₄修饰后的OP样品具有良好的水热稳定性, 并且FePO₄的担载量(5%和40%)对OP样品的水热稳定性几乎没有影响.这与文献报道的金属担载量会影响介孔材料水热稳定性的结果不同.此外, 还对比研究了浸渍法制备的FePO₄/SBA-15 (IMP)和商品SBA-15的水热稳定性.结果表明, 各样品水热稳定性由强到弱的顺序是OP > IMP >> SBA-15.OP和IMP样品水热稳定性优于纯硅分子筛SBA-15的原因可能是FePO₄保护层能抑制介孔材料在水热环境下的结构塌陷.OP样品水热稳定性较IMP样品好的原因可能主要是由于OP样品中存在稳定的Si-O-Fe键和较多的微孔.

关键词: 磷酸铁, SBA-15, 介孔材料, 水热稳定性, 水蒸气, 金属担载量

Abstract:

The hydrothermal stability of FePO₄-SBA-15 synthesized using a novel one-pot hydrothermal method (OP) was systematically investigated using two methods: treatment with pure steam at 800 ℃ or with boiling water at 100 ℃. The structural changes in the samples were monitored using small angle X-ray diffraction and N₂-physisorption methods. It was found that the hydrothermal stabilities of OP samples remained high and showed little difference over the FePO₄-doping range 5-40 wt%. These results differ from previous reports that the loading of heterogeneous metal atoms significantly influences the hydrothermal stability of the host ordered mesoporous material. For comparison, the hydrothermal stabilities of FePO₄-SBA-15 synthesized using an impregnation method (IMP) and commercially obtained SBA-15 were also studied. The order of the sample hydrothermal stabilities was OP > IMP >> SBA-15. The formed FePO₄ protective layers helped to prevent mesostructure degradation during hydrothermal treatment, therefore modified samples showed superior hydrothermal stabilities compared with pure SBA-15. The superior performance of OP samples over IMP samples is mainly attributed to the formation of stable Si-O-Fe bonds and more micropores in OP samples.

Key words: Iron phosphate, SBA-15, Mesoporous material, Hydrothermal stability, Steam, Metal loading

王润琴, 林荣和, 丁云杰, 刘佳, 罗文婷, 杜虹, 吕元 . 水热合成一锅法制备FePO₄-SBA-15及其水热稳定性能[J]. 催化学报, 2015, 36(3): 446-453.

Runqin Wang, Ronghe Lin, Yunjie Ding, Jia Liu, Wenting Luo, Hong Du, Yuan Lü. Highly hydrothermally stable FePO₄-SBA-15 synthesized using a novel one-pot hydrothermal method[J]. Chinese Journal of Catalysis, 2015, 36(3): 446-453.

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水热合成一锅法制备FePO₄-SBA-15及其水热稳定性能

Highly hydrothermally stable FePO₄-SBA-15 synthesized using a novel one-pot hydrothermal method

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