以经H2SO4处理焙烧的高岭土为载体,制备了以其负载的SO4(2-)/ZrO2-TiO2固体酸催化剂.用FT-IR、XRD和NH3-TPD等测试技术表征了催化剂的微观结构及酸强度,考察了对环己酮乙二醇缩酮反应的催化活性及稳定性.结果表明,酸化处理使高岭土表面酸量增加,但酸强度变化不大,而其负载SO4(2-)/ZrO2-TiO2后,经500℃焙烧3 h其酸量及酸强度显著升高.环己酮用量为0.2 mol、乙二醇0.24 mol、催化剂1.2 g、带水剂环己烷15 mL,回流反应70 min后,缩酮收率可达96.8%,催化剂重复使用5次收率保持在90%以上.
参考文献
[1] | LI Shumin,GUO Haifu,YAN Peng,et al.Synthesis of Cyclohexanone 1,2-Propanediol Ketal Catalyzed by Solid Superacid S2O8(2-)/SnO2-SiO2[J].Petrochem Technol,2008,37(2):169-173(in Chinese).李淑敏,郭海福,闫鹏,等.固体超强酸S2O8(2-)/SnO2-SiO2催化合成环己酮1,2-丙二醇缩酮[J].石油化工,2008,37(2):169-173. |
[2] | LI Guixian,ZHAO Junlong,YU Hua,et al.Synthesis of Acetophenone Cylic Ethylic Ketal by the Keggin Type Multicomponent Heteropoly Acids[J].Chinese J Mol Catal,2010,24(2):129-135(in Chinese).李贵贤,赵军龙,余华,等.Keggin型多元杂多酸催化合成苯乙酮环乙二缩酮[J].分子催化,2010,24(2):129-135. |
[3] | LIANG Xuezheng,GAO Shan,YU Xinyu,et al.Catalytic Synthesis of Acetals(ketals)by FeCl3[J].Chem Ind Eng Prog,2006,25(6):684-686(in Chinese).梁学正,高珊,于心玉,等.FeCl3催化合成缩醛(酮)[J].化工进展,2006,25(6):684-686. |
[4] | SONG Xiaoliang,YIN Minghui,ZHANG Guoliang,et al.Synthesis of 1,4-Cyelohexanedione Mono-neopentylketal over NKC-9 Macroporous Resin[J].J Chem Eng Chinese Univ,2009,23(2):321-325(in Chinese).宋晓亮,尹明辉,张国亮,等.NKC-9型树脂催化合成单新戊二醇缩1,4-环己二酮[J].高校化学工程学报,2009,23(2):321-325. |
[5] | Thomas B,Sugunan S.Acetalization of Ketones on K-10 Clay and Rare Earth Exchanged HFAU-Y Zeolites:A Mild and Facile Procedure for the Synthesis of Dimethylacetals[J].J Porous Mater,2006,13(2):99-106. |
[6] | LI Caolong,DENG Zhangwu,HU Xianzhi,et al.Catalytic Synthesis of Cyclohexanone Ethylene Keta over Solid Superacid[J].Chinese J Mol Catal,2009,23(1):37-41(in Chinese).李曹龙,邓长戊,胡显智,等.钛基固体超强酸对环己酮乙二醇缩酮催化反应的特性[J].分子催化,2009,23(1):37-41. |
[7] | YANG Shuijin,BAI Aimin,Yu Xieqing,et al.Preparation and Catalytic Activity of SO4(2-)/TiO2-WO3[J].Chinese J Org Chem,2004,24(10):1262-1266(in Chinese).杨水金,白爱民,余协卿,等.固体超强酸催化剂SO4(2-)/TiO2-WO3的制备及其催化性能研究[J].有机化学,2004,24(10):1262-1266. |
[8] | REN Liguo,GAO Wenyi.Green Catalytic Synthesis of Acetophenone 1,3-Propandiol Ketal[J].Petrochem Technol,2006,35(3):264-267(in Chinese).任立国,高文艺.苯乙酮1,3-丙二醇缩酮的绿色催化合成[J].石油化工,2006,35(3):264-267.Preparation of Kaolinite Supported SO4(2-)/ZrO2-TiO2 |
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