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目的:研究Strandberg型磷钼氧酸盐[Co(en)3]2[P2Mo5O23]·3H2O单晶体催化合成阿司匹林的催化性能。方法:采用水热合成法制备[Co(en)3]2[P2Mo5O23]·3H2O单晶体化合物;以阿司匹林产率为考察指标,选用L25(53)表进行正交试验其催化合成阿司匹林的性能进行研究;利用显色法、熔点法、核磁共振氢谱法对催化产物进行结构鉴定。结果:确定了[Co(en)3]2[P2Mo5O23]·3H2O单晶体化合物催化合成阿司匹林的最佳工艺条件为:催化剂用量0.15g,反应时间30min,反应温度90℃。结论:[Co(en)3]2[P2Mo5O23]·3H2O单晶体化合物能够高效地催化合成阿司匹林,并且具有无污染、低成本、可循环再生使用等优点。
OBJECTIVE: To study the catalytic performance of strandberg-type phosphomolybdic acid [Co (en) 3] 2 [P2Mo5O23] · 3H2O single crystals for the synthesis of aspirin. Methods: The [Co (en) 3] 2 [P2Mo5O23] · 3H2O single crystal compound was prepared by hydrothermal synthesis method. The yield of aspirin was taken as the index, and the performance of the synthesis of aspirin catalyzed by L25 (53) The structure of the catalytic product was identified by chromogenic method, melting point method and nuclear magnetic resonance spectroscopy. Results: The optimal conditions for the synthesis of [Co (en) 3] 2 [P2Mo5O23] · 3H2O monocrystal were found to be as follows: the amount of catalyst 0.15g, the reaction time 30min, the reaction temperature 90 ℃. CONCLUSION: The [Co (en) 3] 2 [P2Mo5O23] · 3H2O monocrystal compound can catalyze the synthesis of aspirin with high efficiency and has the advantages of no pollution, low cost and recyclable.