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摘要
以正硅酸四乙酯(TEOS)为硅源、十二胺(DDA)为模板剂、偏钒酸铵为金属活性组分,通过溶胶-凝胶法合成钒改性HMS(V-HMS)介孔材料,利用SEM、小角XRD、BET、FT-IR和TG-DTA对V-HMS进行表征。以30%的H2O2为氧化剂,催化2-萘酚氧化合成2-羟基-1,4-萘醌。分别探究了反应温度、反应时间、金属的负载量、催化剂的质量以及物料摩尔比对该反应的影响。结果表明,反应温度为50℃、反应时间为3 h、催化剂质量为0.04 g、催化剂金属负载量为4%、n(2-萘酚)∶n(H2O2)=1∶48时,2-羟基-1,4-萘醌的收率最高达到95.5%。催化剂可以重复使用。
Abstract
Vanadium modified HMS (V-HMS) mesoporous materials are synthesized by sol-gel method using tetraethyl orthosilicate (TEOS) as silicon source, dodecylamine (DDA) as template and ammonium metasvanate as metal active component. The prepared V-HMS is characterized by scanning electron microscope (SEM), small angle XRD, N2 adsorption desorption (BET), Fourier transform infrared (FT-IR) and thermal analysis (TG-DTA). 2-Hydroxy-1, 4-naphthoquinone is synthesized through oxidation of 2-naphthol by using 30% H2O2 as oxidant and V-HMS as catalyst. Influences of reaction temperature, reaction time, loading amount of metal, catalyst dosage and materials ratio on the reaction are investigated. The results indicate that the yield of 2-hydroxy-1, 4-naphthoquinone is the highest, reaching 95.5% when reaction temperature remains at 50℃, the reaction lasts for 3 h, catalyst dosage is 0.04 g, the loading amount of metal in the catalyst is 4%, and the molar ratio between 2-naphthol and H2O2 is 1∶48. The catalyst can be reused.
关键词
V-HMS
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2-羟基-1,4-萘醌
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氧化
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2-萘酚
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介孔材料
Key words
V-HMS
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2-hydroxy-1,4-naphthoquinone
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oxidation
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2-naphthol
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mesoporous material
Author summay
卢虹竹(1995-),女,硕士研究生,研究方向为绿色有机催化,954043501@qq.com
V-HMS催化氧化2-萘酚合成2-羟基-1,4-萘醌的研究[J].
现代化工, 2021, 41(8): 193-197 DOI:10.16606/j.cnki.issn0253-4320.2021.08.038