| 孙 悦,李 雪,任铁强，等.磷钼钒杂多酸的制备及其催化合成油酸甲酯[J].中国油脂,2015,40(4):.[SUN Yue,LI Xue,REN Tieqiang，etc.Preparation of molybdovanadophosphoric heteropoly acid and its catalysis in esterification synthesis of methyl oleate[J].China Oils and Fats,2015,40(4):.] |
| 磷钼钒杂多酸的制备及其催化合成油酸甲酯 |
| Preparation of molybdovanadophosphoric heteropoly acid and its catalysis in esterification synthesis of methyl oleate |
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| DOI： |
| 中文关键词: 磷钼钒杂多酸 酯化反应 油酸甲酯 |
| 英文关键词:molybdovanadophosphoric heteropoly acid esterification reaction methyl oleate |
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| 中文摘要: |
| 采用二水钼酸钠、十二水磷酸氢二钠和偏钒酸钠为原料，制备了磷钼钒杂多酸(H4PMo11VO40)催化剂。利用紫外可见吸收光谱、红外光谱和热重分析方法对H4PMo11VO40的化学结构和化学热稳定性进行了表征，并将H4PMo11VO40作为催化剂用于油酸与甲醇的酯化反应中。结果表明:H4PMo11VO40红外谱图含有明显P—O键、Mo—O键和Mo—O—Mo桥键特征吸收峰；该杂多酸在308 nm处有明显紫外吸收峰；该杂多酸热稳定性在209℃以上。在酸醇摩尔比1∶6、反应时间7 h、催化剂用量为油酸质量9%的条件下，油酸酯化率为90.7%；H4PMo11VO40催化剂循环使用5次后，油酸酯化率仍在85%以上。因此，该磷钼钒杂多酸可循环使用，且易与产物分离。 |
| 英文摘要: |
| Molybdovanadophosphoric heteropoly acid (H4PMo11VO40) catalyst was synthesized using Na2MoO4·2H2O, Na2HPO4·12H2O and NaVO3 as raw materials. The chemical structure and thermal stability of H4PMo11VO40were characterized by UV-Vis, FTIR and TG-DTG and it was used as catalyst in the esterification of oleic acid and methanol. The results showed that the characteristic absorption peaks of P—O bond, Mo—O bond and Mo—O—Mo bridge bond could be observed obviously in FTIR spectra of H4PMo11VO40; H4PMo11VO40 had a clear ultraviolet absorption peak at 308 nm; it was provided with high thermal stability above 209℃. When the molar ratio of oleic acid to methanol was 1∶6, the dosage of catalyst was 9% (based on the mass of oleic acid) and the reaction time was 7 h, the esterification rate of oleic acid reached 90.7%. After the catalyst was reused for five times, the esterification rate of oleic acid was still above 85%. Therefore, heteropoly acid H4PMo11VO40 could be repeatedly used and easily separated from the product. |
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