| 赵福桐,李成龙,高文艺,吕雪川,焦玉娟,高肖汉.化学通报,2018,81(10):924-928. |
| 铁改性的HMS分子筛催化苯酚羟基化反应合成二酚 |
| Hydroxylation of phenol to produce dihydroxybenzene catalyzed by iron modified HMS |
| 投稿时间：2018-05-12 修订日期：2018-07-02 |
| DOI： |
| 中文关键词: 苯酚羟基化 过氧化氢 Fe/HMS 绿色化学 改性分子筛 |
| 英文关键词:Hydroxylation of Phenol Hydrogen Peroxide Fe/HMS Green Chemistry Modified Molecular Sieve |
| 基金项目:国家自然科学基金项目（21003069，21103078） |
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| 中文摘要: |
| 邻苯二酚和对苯二酚都是重要的精细化工中间体,在各个行业中具有广泛的应用。苯酚与过氧化氢反应化合成苯二酚是一条反应条件温和、环境友好的合成路线。该合成路线的关键是催化剂的选择和反应条件的优化。以铁改性的HMS分子筛为催化剂,研究了金属负载量、催化剂使用量、反应温度、反应时间等因素对催化性能的影响,优化了反应条件。以水为溶剂,n(Fe)：n(Si)=0.04,n(苯酚)：n(H2O2)=2：1,反应温度50 ℃,催化剂用量0.1 g,反应4 h,苯酚的转化率达45.5%,苯二酚选择性为94.9%。循环实验结果证实该催化剂是可以重复使用的。从FT-IR、N2吸附脱附等温曲线的结果表明使用过的催化剂的骨架保持完整,具有良好的稳定性。N2吸附-脱附结果表明Fe/HMS具有良好的介孔结构,铁进入HMS材料的骨架中。 |
| 英文摘要: |
| Catechol and hydroquinone are very important fine chemical intermediate products. They have a wide range of applications in all industries. It is a mild and environment-friendly route to hydroxylate phenol with hydrogen peroxide to produce dihydroxybenzene. The choices of the catalyst and the optimization of the reaction conditions are very important to the route. HMS modified by iron (Fe/HMS) is used as a catalyst. Effects of Fe contents in Fe/HMS, catalyst amount, temperature and reaction time on the catalytic performances were examined. The conditions were optimized. Under the conditions of water solvent, n(Fe)/n(Si) of 0.04, ratio of phenol to H2O2 of 2:1, reaction temperature of 50 ℃, amount of catalyst of 0.1 g and reaction time of 4 hours, phenol conversion of 45.5% and the dihydroxybenzene selectivity of 94.9% are achieved. The recycling test confirms that the Fe/HMS catalyst is reusable. The used catalyst structure keeps completely from the results of the FT-IR spectra and N2 absorption-desorption isotherms, which revealed that the Fe/HMS stability is excellent. The results of the N2 absorption-desorption isotherms illustrates that Fe/HMS material had a uniform mesoporous structure and Fe was successfully incorporated into the framework of HMS. |
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