| 高洪成,王秀艳,张晓飞,刘云鹤,祁强,宋晓静.PW11M(M=Cu、Co)@TiO2多相催化剂的制备及氧化脱硫性能[J].分子催化,2019,33(5):438-446 |
| PW11M(M=Cu、Co)@TiO2多相催化剂的制备及氧化脱硫性能 |
| Preparation of PW11M(M=Cu, Co)@TiO2 Heterogeneous Catalysts and Oxidative Desulfurization Performance |
| 投稿时间：2019-08-16 修订日期：2019-09-21 |
| DOI： |
| 中文关键词: 过渡金属 多金属氧酸盐 TiO2 多相催化 氧化脱硫 |
| 英文关键词:transition metal polyoxometalate TiO2 heterogeneous catalysis oxidative desulfurization |
| 基金项目:河北省自然科学青年基金（B2017411009） |
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| 中文摘要: |
| 以过渡金属（Cu，Co）取代磷钨酸为模板剂，硫酸钛为钛源，通过一步模板法合成出一类多酸基PW11M（M=Cu、Co）@TiO2材料，采用FT-IR、XRD、XPS、Raman、SEM和TEM表征手段对材料进行了结构表征.结果表明，PW11M（M=Cu、Co）被引入到TiO2中，形成了球形核壳结构.N2吸附-脱附测试表明，PW11Co@TiO2具有介孔结构：孔径大小为3.3 nm，比表面积为72.4 m2/g.在以H2O2为氧化剂，乙腈为溶剂的氧化脱硫反应体系中考察了其催化活性，结果表明：复合材料PW11M（M=Cu、Co）@TiO2表现出良好的催化性能.其中催化剂PW11Co@TiO2在投入量为40 mg，反应底物为500 ppm，反应温度60℃，反应40 min后，DBT的脱硫率达到99.7%.中断和循环实验表明，催化剂PW11Co@TiO2具有良好的稳定性，在相同的反应条件下，循环反应5次后，催化剂的催化活性没有明显下降. |
| 英文摘要: |
| A polyoxometalate-based materials has been synthesized though the one-step template using transition metal (Cu, Co) substituted phosphotungstic acid as template and titanium sulfate as titanium source, denoted as PW11M (M=Cu, Co)@TiO2. Multiple characterization methods namely FT-IR, XRD, XPS, Raman, SEM and TEM were used to characterize the resultant materials, and results indicated that PW11M (M=Cu, Co) is introduced into TiO2, forming core-shell spherical structure. N2 adsorption-desorption test showed that PW11Co@TiO2 was mesoporous material with pore size of 3.3 nm and specific surface area of 72.4 m2/g. The catalytic properties of these materials were investigated in the oxidative desulfurization reaction system with H2O2 as oxidant and acetonitrile as solvent. The results showed that the PW11M (M=Cu, Co)@TiO2 exhibited good catalytic performance. The S-removal of DBT reached 99.7% after 40 min reaction at a temperature of 60℃ when dosage of catalyst PW11Co@TiO2 was 40 mg and reaction substrate was 500 mg/kg. Leaching and recycling experiments revealed that catalyst PW11Co@TiO2 had excellent stability, and there was no significant decrease in S-removal after five cycles under same reaction conditions. |
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