H6P2Mo9W9O62/Cu3(BTC)2的制备及催化合成缩醛(酮)

doi:10.13218/j.cnki.csdc.2017.05.009

摘要/Abstract

摘要： 采用浸渍法制得H₆P₂Mo₉W₉O₆₂/Cu₃(BTC)₂,利用傅里叶变换红外光谱仪(FT-IR)、X射线衍射仪(XRD)、热重分析仪(TG)以及扫描电镜(SEM)表征其组成、结构、热稳定性以及形貌。以H₆P₂Mo₉W₉O₆₂/Cu₃(BTC)₂为催化剂,环己酮和乙二醇合成缩酮的反应为探针,探究出较佳反应条件:环己酮用量为0.2 mol,n(环己酮)∶n(乙二醇)=1∶1.3,催化剂用量占反应物总质量的0.3%,反应时间为60 min,带水剂用量为6 mL。在此条件下,环己酮乙二醇缩酮收率可达83.7%。且以上条件下催化合成苯甲醛乙二醇缩醛、丁酮乙二醇缩酮、丁酮1,2-丙二醇缩酮、苯甲醛1,2-丙二醇缩醛和环己酮1,2-丙二醇缩酮的收率分别为70.1%,66.0%,62.1%,66.3%和75.8%。与分子筛MCM-48负载硅钨酸、活性炭负载对甲苯磺酸和铝交联蒙脱土催化剂相比,H₆P₂Mo₉W₉O₆₂/Cu₃(BTC)₂是一种催化性能较好的催化剂。

关键词: 合成香料, 缩醛(酮), 催化合成, 金属有机骨架

Abstract: H₆P₂Mo₉W₉O₆₂/Cu₃(BTC)₂ as a new catalyst was prepared by impregnation method.Fourier transformation infrared spectrum (FT-IR),X-ray diffraction (XRD),thermal gravimetry (TG) and scanning electron microscope (SEM) were used for characterization and measurement of its composition,structure,thermal stability and morphology.The reaction,with H₆P₂Mo₉W₉O₆₂/Cu₃(BTC)₂ as catalyst,for synthesis of ketal from cyclohexanone and ethylene glycol as starting materials was used as probe reaction,and the optimized synthesis conditions were found by orthogonal experiments as follows:fixing the amount of cyclohexanone as 0.2 mol;molar ratio,n(cyclohexanone)∶n(ethylene glycol)=1∶1.3;mass ratio of the catalyst to total reactants,0.3%;the reaction time,60 min;and amount of water stripping agent,6 mL.The yield of the product reaches 83.7%.Under similar reaction conditions,the yield of benzaldehyde ethylene glycol acetal reaches 70.1%;butanone glycol ketal,66.0%;butanone 1,2-propylene glycol ketal,62.1%;benzaldehyde 1,2-propanediol acetal,66.3%;and cyclohexanone 1,2-propylene glycol ketal,75.8%.Compared with that of catalysts H₄SiW₁₂O₄₀/MCM-48,activated carbon supported p-toluene sulfonic acid and Al-cross linked montmorillonite,H₆P₂Mo₉W₉O₆₂/Cu₃(BTC)₂ shows better catalytic performance.

Key words: perfume, acetals and ketals, catalytic synthesis, metal-organic framework

中图分类号:

TQ655

向诗银, 杨水金. H₆P₂Mo₉W₉O₆₂/Cu₃(BTC)₂的制备及催化合成缩醛(酮)[J]. 日用化学工业, 2017, 47(5): 281-285.

XIANG Shi-yin, YANG Shui-jin. Preparation of H₆P₂Mo₉W₉O₆₂/Cu₃(BTC)₂ and its catalytic performance for synthesis of acetals and ketals[J]. China Surfactant Detergent & Cosmetics, 2017, 47(5): 281-285.

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H₆P₂Mo₉W₉O₆₂/Cu₃(BTC)₂的制备及催化合成缩醛(酮)

Preparation of H₆P₂Mo₉W₉O₆₂/Cu₃(BTC)₂ and its catalytic performance for synthesis of acetals and ketals

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