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苯甲醇和苯甲酸制备实验的改进与创新设计 被引量:2
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作者 全晓塞 门秀琴 +2 位作者 王军旗 周颖 姚俊 《大学化学》 CAS 2020年第4期103-111,共9页
以苯甲醛为原料,通过Cannizarro反应制备苯甲醇和苯甲酸是有机化学实验教学中的经典内容。鉴于现有实验方案已难满足日益提升的教学要求,对其进行了改进与创新设计:采用微波辐射法合成,引入正交设计优化条件;采用紫外分光光度法定量测... 以苯甲醛为原料,通过Cannizarro反应制备苯甲醇和苯甲酸是有机化学实验教学中的经典内容。鉴于现有实验方案已难满足日益提升的教学要求,对其进行了改进与创新设计:采用微波辐射法合成,引入正交设计优化条件;采用紫外分光光度法定量测定粗产品中苯甲醇的含量;采用柱层析法分离得到苯甲醇。改进结果表明:KOH溶液浓度50%(质量百分比),微波功率500 W时,反应15 min完成。光度法定量显示苯甲醇产率可达82.0%。萃取分离后的粗产品用50:1和15:1石油醚/乙酸乙酯(体积比)梯度洗脱,柱层析分离后可得苯甲醇纯品,水相酸化重结晶后得到苯甲酸。产物的相关测试与表征结果与文献吻合良好。与传统方案相比,新方案时间锐减99%,产率提高约15%,萃取剂更安全,产率测定快速准确,产物纯化方法优化。将之用于教学,可通过各要点功能的分别承载,综合实现研究性思维与方法的培养目标。 展开更多
关键词 微波辐射 正交试验 分光光度法 改进与创新
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La_(2)O_(3)-promoted Ni/H-ZSM-5 catalyzed aqueous-phase guaiacol hydrodeoxygenation to cyclohexanol 被引量:1
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作者 Feng Lin Yudan Zhong +3 位作者 Yulong Ma Yonggang Sun xiuqin men Yingbo Zhu 《Journal of Rare Earths》 SCIE EI CAS CSCD 2023年第2期224-232,共9页
Hydrodeoxygenation(HDO)of renewable lignin-derived biomass in aqueous-phase to produce high value-added products is of great significance.However,developing new catalysts with high activity and excellent stability in ... Hydrodeoxygenation(HDO)of renewable lignin-derived biomass in aqueous-phase to produce high value-added products is of great significance.However,developing new catalysts with high activity and excellent stability in an aqueous phase faces considerable challenges.Rare earth doping can effectively regulate the water exchange rate constant(WERC)value of the catalyst and play an important role in promoting the hydrolysis of ether bonds.Therefore,in this paper the bimetallic supported catalyst Ni-La_(2)O_(3)/H-ZSM-5 doped with rare earth metal La_(2)O_(3)was prepared,and used to catalyze the conversion of the lignin model co mpound guaiacol to cyclohexanol in the aqueous phase.The co nversion of guaiacol catalyzed by 10Ni-3La_(2)O_(3)/H-ZSM-5 reaches 100%,and the selectivity of the product cyclohexanol is 85%.A series of characterizations illustrate that the doping of La_(2)O_(3)causes the electron transfer between La_(2)O_(3)-Ni and changes the distribution of Ni,and a strong metal carrier interaction occurs between the bimetallic Ni-La_(2)O_(3)and H-ZSM-5.This can effectively promote the hydrolysis of the C-O ether bond in guaiacol and significantly improve the activity of the catalyst.The possible catalytic reaction mechanism of Ni-La_(2)O_(3)/H-ZSM-5 catalytic conversion of guaiacol was proposed. 展开更多
关键词 La_(2)O_(3) GUAIACOL Catalysis H-ZSM-5 Rare earths
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