Synthesis of Acetal With Solid Super Acid Catalyst S2O2-8/ZrO2

doi:10.3696/j.issn.1006-396X.2009.03.002

Journal of Petrochemical Universities ›› 2009, Vol. 22 ›› Issue (3): 5-8.DOI: 10.3696/j.issn.1006-396X.2009.03.002

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Synthesis of Acetal With Solid Super Acid Catalyst S₂O^2-₈/ZrO₂

1.School of Chemistry and Chemical Engineering, Shanxi Datong University, Datong Shanxi 037009,P.R. China;

2.Key Laboratory of Coal Science and Technology of Ministry of Education and Shanxi Province, Taiyuan University of Technology, Taiyuan Shanxi030024,P.R.China

Received:2008-08-30 Revised:2009-03-12 Published:2009-09-25 Online:2009-09-25

固体超强酸S₂O^2-₈/ZrO₂催化合成缩醛

王俊丽¹,孟双明¹,李忠²,郭永¹,赵强¹,樊月琴¹

1.山西大同大学化学与化工学院,山西大同037009;
2.太原理工大学煤科学与技术教育部和山西省重点实验室，山西太原030024

作者简介:王俊丽(1983 -), 女, 山西晋城市, 硕士
基金资助:
国家重点基础研究发展计划(2005CB221204);国家自然科学基金资助项目(20576085)

Abstract

Abstract:

The S₂O^2-₈/ZrO₂  solid acid catalyst was prepared from ZrOCl₂and (NH₄)₂S₂O₈ by precipitation, aging, filtering, washing, drying, impregnation and calcination processes. The characterization of the catalyst was performed using XRD, FT-IR and NH₃-TPD. The effect of calcination temperature on the acidic property, textural property and catalytic perfomance of S₂O^2-₈/ZrO₂ solid acid catalysts was studied. XRD patterns show that the catalyst present is higher tetragonal phase. FT-IR spectra shows that S₂O^2-₈ is strongly bind with the ZrO₂surface bidentately. With S₂O^2-₈/ZrO₂ as catalyst,the effects of molar ratio of glycol to aldehyde, quantity of catalyst, reaction time on the yield of acetalation was more systematically studied and the best reaction conditions were confirmed. The results show that the molar ratio of butyraldehyde to glycol is 1∶1.4, the quantity of catalyst is equal to 0.25% of feed stocks, the reaction time is 50 min, and the yield of butyraldehyde glycol acetal can reach 75.8%; the yield of benzaldehyde glycol acetal is 68.8% under the following conditions：molar ratio of benzaldehyde to glycol 1∶1.25, the quantity of catalyst 0.5% of feed stocks, the reaction time 50 min.

Key words: Butyraldehyde glycol acetal , Benzaldehyde glycol acetal , Solid superacid , Catalysis , Acetalization

摘要： 通过沉淀、老化、过滤、洗涤、干燥、浸渍和焙烧等过程，由 ZrOCl₂ 和(NH₄)₂S₂O₈制备了S₂O^2-₈ /ZrO₂催化剂。用XRD，FT-IR，NH₃-TPD对其进行了表征，研究了焙烧温度对其酸性、结构和催化性能的影响。XRD 结果表明具有较高T型晶相峰。FT-IR分析表明S₂O^2-₈ /ZrO₂ 表面以双桥鳌合状配位化合物形式结合。研究了醛醇物质的量比、催化剂用量、反应时间等因素对产品收率的影响。结果表明，在 n(丁醛) / n(乙二醇) =1:1 .4，催化剂质量分数为0 .25%,反应时间为 50 min的最佳条件下，丁醛乙二醇缩醛的收率可达95.8%；在n(苯甲醛)/ n(乙二醇)=1∶1 .25，催化剂质量分数为0 .5%，反应时间为50 min的最佳条件下，苯甲醛乙二醇缩醛的收率可达 88 .8%。

关键词: 丁醛乙二醇缩醛 , 苯甲醛乙二醇缩醛 , 固体超强酸 , 催化 , 缩醛反应

WANG Jun-li,MENG Shuang-ming,LI Zhong,et al. Synthesis of Acetal With Solid Super Acid Catalyst S₂O^2-₈/ZrO₂[J]. Journal of Petrochemical Universities, 2009, 22(3): 5-8.

王俊丽,孟双明,李忠. 固体超强酸S₂O^2-₈/ZrO₂催化合成缩醛[J]. 石油化工高等学校学报, 2009, 22(3): 5-8.

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Synthesis of Acetal With Solid Super Acid Catalyst S₂O^2-₈/ZrO₂

固体超强酸S₂O^2-₈/ZrO₂催化合成缩醛

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