文章摘要
王玉斌,陈彤,王公应.固体碱KF/MgAl-LDO催化苯酚与碳酸二甲酯合成苯甲醚[J].精细化工,2021,(8):0
固体碱KF/MgAl-LDO催化苯酚与碳酸二甲酯合成苯甲醚
Synthesis of Anisole from Phenol and Dimethyl Carbonate catalyzed by solid base KF/MgAl-LDO
投稿时间:2021-02-06  修订日期:2021-04-17
DOI:
中文关键词: 固体碱  镁铝水滑石  氟化钾  碳酸二甲酯  苯甲醚  催化技术
英文关键词: Solid base  Magnesium aluminum hydrotalcites  potassium fluoride  dimethyl carbonate  anisole  catalysis technology
基金项目:四川省重点研发项目(2021YFG0109)
作者单位E-mail
王玉斌 中国科学院成都有机化学研究所 bywangyb@foxmail.com 
陈彤 中国科学院成都有机化学研究所 chentongw@sina.com.cn 
王公应 中国科学院成都有机化学研究所  
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中文摘要:
      共沉淀法制备了镁铝水滑石(MgAl-LDHs),以 MgAl-LDHs 为前驱体,高温焙烧得到类水滑石 MgAl-LDO和不同碱金属卤化物(MX)掺杂的固体碱催化剂MX/MgAl-LDO。对其进行XRD表征和Hammett 法碱性滴定,并考察了其催化苯酚与碳酸二甲酯合成苯甲醚的活性。结果显示,前驱体 MgAl-LDHs 的 Mg/Al 摩尔比、沉淀 pH 及焙烧温度均影响 KF/MgAl-LDO 的结构和碱性;KF 的掺杂大幅增加催化剂的碱量,且 碱强度(H0)在 11~15 区间强碱的碱量提升更为显著,增加的强碱性位主要是由 KMgF3 和 K2CO3提供。当 KF 质量分数为 KF/MgAl-LDO 的 33 %时,KF/MgAl-LDO 显示最好的催化性能:在 DMC/苯酚物质的量比 为 2:1,KF/MgAl-LDO 用量仅 1 wt%(以苯酚质量为基准),200 ℃下反应 4 h,苯甲醚收率为 95.2%。对催 化剂催化活性与碱性关系的分析发现,催化剂的活性与碱量正相关,而碱强度 H0在 11~15 区间的强碱性位 具有最高的催化效率。
英文摘要:
      The solid base catalysts MgAl-LDO and KF/MgAl-LDO doped with different alkali metal halides(MX) were prepared by MgAl-LDHs as precursor. XRD characterization and Hammett titration were carried out, and the catalytic activity for the synthesis of anisole from phenol and dimethyl carbonate was investigated. The results showed that the Mg/Al molar ratio, precipitation pH and calcination temperature of MgAl-LDHs all affect the structure and basicity of the catalyst, and the droping of KF greatly increases the base amount of the catalyst, especially the strong base amount of H0(11-15), which is mainly provided by KMgF3 and K2CO3. The catalyst of KF/MgAl-LDO with the KF mass fraction of 33% showed the best catalytic performance. When the molar ratio of DMC to phenol was 2:1, the catalyst dosage is only 1 wt%(based on the phenol mass), reaction temperature is 200 ℃, reaction time is 4 h, the yield of anisole was 95.2%. The research of the relation between the activity and the basicity showed that the activity of the catalyst was positively correlated with the total base amount, and the strong base site of H -(11~15) had the highest catalytic performance.
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