| 曹小华.化学通报,2015,78(10):928-932. |
| Dawson结构磷钨酸银催化绿色合成阿司匹林 |
| Green Synthesis of Aspirin Catalyzed by Silver Salts of Tungstophosphoricwith Dawson Structure |
| 投稿时间：2015-02-08 修订日期：2015-03-21 |
| DOI： |
| 中文关键词: 磷钨酸银 Dawson结构 催化合成 阿司匹林 |
| 英文关键词:Silver salts of tungstophosphoric Dawson structure CatalyticSsynthesis Aspirin |
| 基金项目:国家自然科学基金项目(21161009)、江西省教育厅科技项目(GJJ13723)及九江学院科技项目(2013KJ005)资助。 |
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| 中文摘要: |
| 通过沉淀法制备出新型Dawson结构磷钨酸银(Ag3H3P2W18O62.nH2O)催化剂,采用FT-IR、EDX对催化剂进行了表征,并将其用于催化乙酸酐和水杨酸合成阿司匹林。研究了催化剂用量、水杨酸和乙酸酐摩尔比、反应温度、反应时间等因素对反应的影响。结果表明：自制磷钨酸银具有Dawson结构,并且在多次使用后仍保持Dawson结构不变。在优化条件下,即n(水杨酸):n(乙酸酐)=1:1.75,反应温度为90℃,催化剂用量为3.2%(以反应物质量计),反应时间为20min,阿司匹林收率为90.1%。催化剂重复使用5次,阿司匹林收率仍可保持为82.4%。 |
| 英文摘要: |
| Silver salts of tungstophosphoric with Dawson structure(Ag3H3P2W18O62.nH2O)was prepared by precipitation method and was characterized by FT-IR and EDX. Then it was employed as the catalyst for the synthesis of acetylsalicylic acid from salicylic acid and acetic anhydride. The effects of catalyst dosage, ratio of reactants, reaction temperature and reaction time on the yield of acetylsalicylic acid were investigated. The results showed that self-prepared silver tungstophoricSacidScatalyst kept primary Dawson structure andShad the structure of DawsonSafter reuseSforSseveral times. Under the optimum reaction conditions, i.e., the molar ratio of salicylic acid to acetic anhydride was 1:1.75, the weight ratio of Ag3H3P2W18O62 to reactants was 3.2%, the reaction temperature was 90℃ and the reaction time was 20 min, the yield of aspirin could reach 90.1%. The catalyst can be reused for 5 times with yield of aspirinSof 82.4%. |
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