Synthesis of Benzaldehyde Glycerol Acetals Catalyzed by CuSO4/SiO2

doi:10.3696/j.issn.1672-6952.2011.03.005

Abstract

Abstract:

CuSO₄/SiO₂ solid acid catalysts were prepared using sol-gel technique and impregnation method, and then characterized by XRD, low temperature N₂-adsorption and NH₃-TPD. The effects of calcination temperature of catalysts, CuSO₄ loading, the molar ratio of benzaldehyde to glycerol, reaction time and amount of deaquation reagent on the synthesis yield were discussed. The results show that CuSO₄ is highly dispersed over surface of SiO₂ to form mesoporous solid acid catalysts with medium acid strength and high specific surface. CuSO₄/SiO₂ showed good catalytic activities and stabilities in the condensation of benzaldehyde with glycerol to produce benzaldehyde glycerol acetals. The optimum preparation conditions are as follows: CuSO₄loadings 15%, and calcination temperature 550 ℃. The optimum reaction conditions are as follows: molar ratio of benzaldehyde to glycerol is 1∶1.1, the weight percentage of catalyst in reaction mixture is 1%, and volume of cyclohexane is 10 mL and reaction time 2 h. Under the optimum reaction conditions, the yield of benzaldehyde glycerol acetal can reach 92.5%.

Key words: Sol-gel, Impregnation , , Solid acid , , Condensation reaction , Benzaldehyde glycerol acetal

摘要： 通过溶胶—胶凝法和浸渍法制备了CuSO ₄/SiO₂ 催化剂,用XRD、低温N₂-吸附和 NH₃-TPD进行
了表征,研究了CuSO₄/SiO₂ 在合成苯甲醛甘油缩醛上的催化性能,考察了催化剂的焙烧温度、CuSO₄ 负载量、原料
物质的量比、反应时间、环己烷体积等因素对产品收率的影响。结果表明:CuSO₄高度分散在SiO2 表面上形成中等
酸强度、高表面积的中孔固体酸催化剂,并在苯甲醛和甘油的缩合反应中具有良好的催化活性和稳定性。催化剂制
备的最佳条件为:焙烧温度550℃,CuSO₄ 的负载量为15%,反应的最佳条件为:n(苯甲醛)∶n(甘油)=1∶1.1,催
化剂质量为反应物总质量的1%,环己烷体积为10mL,反应时间2.0h。在最佳条件下,苯甲醛甘油缩醛的收率可达
92.5%。

关键词: 溶胶—胶凝, , 浸渍 , 固体酸 , , 缩合反应 , , 苯甲醛甘油缩醛

LI Guo-jun.

Synthesis of Benzaldehyde Glycerol Acetals Catalyzed by CuSO_4/SiO₂

[J]. Journal of Liaoning Petrochemical University, 2011, 31(3): 16-19.

李国军. CuSO₄/SiO₂在合成苯甲醛甘油缩醛中的应用[J]. 辽宁石油化工大学学报, 2011, 31(3): 16-19.

[1]	Liang Jiling，Wang Liqun，Liu Lijuan，Tian Li，Zhang Lunqiu，Wang Weiqiang. The Modification of Fe3O4@SiO2 by Silane Coupling Agent and Performance [J]. Journal of Liaoning Petrochemical University, 2019, 39(6): 21-26.
[2]	Wang Yan， Nie Hong. Synchronous H _∞ Stabilization of TimeDelay Switched Systems under Partially DelayDependent Controllers [J]. Journal of Liaoning Petrochemical University, 2018, 38(04): 93-100.
[3]	Yang Fan, Li Yongfeng. Research Progress in Preparation and Catalytic Performance of the Carbon-Based Non Noble Metal Catalysts [J]. Journal of Liaoning Petrochemical University, 2018, 38(02): 1-8.
[4]	Wang Guoliang， Yi Chenglong. Fault Dependency Detection Method Based on Random Occurrence of Fault Signal [J]. Journal of Liaoning Petrochemical University, 2018, 38(02): 71-79.
[5]	. Removal of Sulfides from Simulated Oil by CH₃CONH₂/ZnCl₂ Deep Eutectic Solvent [J]. Journal of Liaoning Petrochemical University, 2017, 37(5): 1-7.
[6]	LiuYujuan,XuJi,TongYufei,et al. Progress in Research of the Synthesis Methods of Nanometer Ceria [J]. Journal of Liaoning Petrochemical University, 2017, 37(5): 8-12.
[7]	Liu Jindong,He Xin,Xin Dingye,et al. Change Law of Four Fractions in Residue Hydrotreating Catalyst Grading System [J]. Journal of Liaoning Petrochemical University, 2017, 37(5): 13-16.
[8]	Fu Yu,Li Xiaoou,Li Heming,et al. Enhanced Removal of the Mechanical Impurities in OilSandsOil  from Indonesia by UltrasoundSedimentation Method [J]. Journal of Liaoning Petrochemical University, 2017, 37(5): 17-21.
[9]	Wu Hao， Ma Guiyang， Xiang Nan，et al. The Effect Analysis of Settlement of Soil on Stress Fields of  Horizontal Section of Crossing Pipeline Structure [J]. Journal of Liaoning Petrochemical University, 2017, 37(5): 22-25.
[10]	Yan Rongju， Wang Weiqiang， Li Zimeng，et al. Progress of Severe Slugging in Marine Riser System [J]. Journal of Liaoning Petrochemical University, 2017, 37(5): 26-30.
[11]	Wang Long. Application of Seismic Reconstruction Inversion in Prediction of River  Channel of X Development Zone in Daqing Placantieline [J]. Journal of Liaoning Petrochemical University, 2017, 37(5): 31-37.
[12]	Zhu Bomin. Optimization of Well Spacing in Gaotaizi Reservoir  of Sazhong Development Zone [J]. Journal of Liaoning Petrochemical University, 2017, 37(5): 38-43.
[13]	Ma Jing,Jin Kejun,Liang Yufeng,et al. Study on Comprehensive Evaluation for Engineering  Mode of Offshore Oil and Gas Fields [J]. Journal of Liaoning Petrochemical University, 2017, 37(5): 44-48.
[14]	Fan Dengshuai,Gao Peng, Liu Zhihui，et al. A Method of Connection Reliability Analysis of Bolted Flange Systems [J]. Journal of Liaoning Petrochemical University, 2017, 37(5): 49-52.
[15]	Wu Zhiyong,Liu Yang,Gao Yang,et al. An Investigation on the Time Relaxation Parameter Used in Boiling  Simulation of Helical Coil Heat Exchanger ShellSide [J]. Journal of Liaoning Petrochemical University, 2017, 37(5): 53-60.

Synthesis of Benzaldehyde Glycerol Acetals Catalyzed by CuSO_4/SiO₂

CuSO₄/SiO₂在合成苯甲醛甘油缩醛中的应用

PDF

Knowledge

Abstract

Cite this article

share this article

References

Related Articles 15

Recommended Articles

Metrics