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采用水热法制备了新型H6P2W9Mo9O62 ·24H2O催化剂,并用UV-Vis、FT-IR和TG-DTA等测试技术对催化剂进行了表征.以微波促进30%过氧化氢氧化环已酮制备己二酸合成反应为探针,考察了催化剂的催化性能.通过正交实验探讨了几种因素对反应的影响,确定了优化工艺条件为:n(环已酮)∶n(过氧化氢)∶n(草酸)∶n(催化剂)=100∶400∶1.25∶0.25,反应温度100℃,微波辐射功率400W,反应时间3.5h,己二酸产品的收率达87.33%,纯度可达99.7%.反应结束后,将反应后含催化剂的溶液浓缩至一定浓度,催化产率降 低,重复使用5次收率降低为45.89%.

参考文献

[1] REN Shuiying,XIE Zhengfeng,XIE Xiaopeng,et al.Environmental-Friendly Synthesis of Adipic Acid by Catalytic Oxidation[J].Prog Chem,2009,21(4):663-671(in Chinese).任水英,解正峰,谢晓鹏,等.催化氧化合成己二酸的清洁方法[J].化学进展,2009,21(4):663-671.
[2] JING Shubo,ZHU Wanchun,GUAN Jingqi,et al.Research Progress of Catalytic Oxidation Synthesis of Adipic Acid Using Clean Oxidant[J].Chem Ind Eng Prog,2009,28(1):62-66(in Chinese).井淑波,朱万春,管景奇,等.环境友好氧化剂催化氧化合成己二酸研究进展[J].化工进展,2009,28(1):62-66.
[3] Kozhevnikov I V.Catalysis by Polyoxometalates (Catalysis for Fine Chemical Synthesis[M].TANG Beikun,LI Xianggao,WANG Shirong Trans.Beijing:Chemical Industry Press,2005:159-174(in Chinese).Kozhevnikov I V.精细化学品的合成:多酸化合物及其催化[M].唐培堃,李祥高,王世荣,译.北京:化学工业出版社,2005:159-174.
[4] YU Hua.Synthesis,Characterization and Catalytic Performance of Keggin Type Multicomponent Hetero-poly Compounds[D].Lanzhou Univ Technol,2010(in Chinese).余华.Keggin型多元杂多化合物的合成-表征及催化性能研究[D].兰州理工大学,2010.
[5] CAO Xiaohua,LI Xiancai,ZHAO Wenjie,et al.Clear Oxidation of Cyclohexanone to Adipic Acid with H2O2 Using H3PW6Mo6O40 ·nH2O as Catalyst[J].China Tungsten Ind,2006,21(4):34-37(in Chinese).曹小华,黎先财,赵文杰,等.H3PW6Mo6O40 ·nH2O催化过氧化氢清洁氧化环己酮合成己二酸[J].中国钨业,2006,21(4):34-37.
[6] CAO Xiaohua,XIE Baohua,TANG Ming,et al.Oxidation of Cyclohexanol to Adipic Acid Catalyzed by Phosphptungstic Acid with Dawson Structure[J].Speciality Petrochem,2008,25 (3):26-29 (in Chinese).曹小华,谢宝华,汤明,等.Dawson结构磷钨杂多酸催化环己醇合成己二酸[J].精细石油化工,2008,25(3):26-29.
[7] Sato K,Aoki M,Noyori R.A Green Route to Adipic Acid:Direct Oxidation of Cyclohexenes with 30 Percent Hydrogen Peroxide[J].Science,1998,281:1646-1647.
[8] Ben S Y,Xie Z F,Cao L Q.Clean Synthesis of Adipic Acid Catalyzed by Complexes Derived from Heteropoly Acid and Glycine[J].Catal Commun,2009,10 (5):464-467.
[9] Chenga C-Y,Lina K-J,Prasad M R,et al.Synthesis of a Reusable Oxotungsten-containing SBA-15 Mesoporous Catalyst for the Organic Solvent-free Conversion of Cyclohexene to Adipic Acid[J].Catal Commun,2007,8 (7):1060-1064.
[10] WEI Li,CHEN Mei,LIU Na,et al.Catalytic Oxidation Cyclohexene to Adipic Acid over Tungtophosphoric Acid in Ionic Liquid[J].J Dalian Polytech Univ,2010,29(3):216-219(in Chinese).魏莉,陈梅,刘娜,等.清洁催化氧化合成己二酸[J].大连工业大学学报,2010,29(3):216-219.
[11] XIE Baohua,CAO Xiaohua,XU Changlong,et al.Green Synthesis of Adipic Acid Catalyzed with Phosphotungstic Acid with Dawson Structure[J].China Synth Fiber Ind,2010,33 (2):21-23 (in Chinese).谢宝华,曹小华,徐常龙,等.Dawson结构磷钨酸催化绿色合成己二酸[J].合成纤维工业,2010,33(2):21-23.
[12] ZHOU Cairong,SHI Xiaohua,NAN Huifang,et al.Study on Process of Preparing Adipic Acid by Catalytic Oxidation of Cyclohexene[J].Fine Chem,2010,27(5):437-441(in Chinese).周彩荣,石晓华,南慧芳,等.催化氧化环己烯制备己二酸[J].精细化工,2010,27(5):437-441.
[13] GONG Hong,YANG Zhonghua,JIANG Heng,et al.Role of Acidic Ligand for Clean Synthesis of Adipic Acid via Catalytic Oxidation of Cyclohexene[J].Chinese J Catal,2002,23 (2):182-184 (in Chinese).宫红,杨中华,姜恒,等.清洁催化氧化环己烯合成己二酸反应中酸性配体的作用[J].催化学报,2002,23(2):182-184.
[14] Usui Y,Sato K.A Green Method of Adipic Acid Synthesis:Organic Solvent and Halide Free Oxidation of Cycloalkanones with 30% Hydrogen Peroxide[J].Green Chem,2003,5(4):373-375.
[15] CHEN Danyun,YANG Xiaoke,ZHOU Hui,et al.Green Catalytic Oxidation of Cyclohexanone with H2O2 to Adipic Acid Using a Monovacant Dawson Heteropolytungstate as Catalyst[J].Petrochem Technol,2010,39(6):656-660(in Chinese).陈丹云,杨晓珂,周慧,等.单缺位Dawson结构杂多钨酸盐绿色催化H2O2氧化环己酮合成己二酸[J].石油化工,2010,39(6):656-660.
[16] WANG Xiaodan,WU Wenyuan,TU Ganfeng,et al.Oxidation of Cyclohexanone to Adipic Acid Catalyzed by Lactam-Based Ionic Liquid[J].Chinese J Org Chem,2010,30(12):1935-1938 (in Chinese).王晓丹,吴文远,涂赣峰,等.内酰胺型离子液体催化环己酮氧化合成己二酸[J].有机化学,2010,30(12):1935-1938.
[17] ZHOU Hui,HE Hongju,HE Jianying,et al.Preparation of Supported Phosphotungstic Acid Catalyst with Multi-carriers and Using It to Green Synthesis of Adipic Acid[J].Sci Technol Food Ind,2011,32(1):256-257,334(in Chinese).周慧,贺红举,何建英,等.多元载体固载磷钨酸催化剂的研制及绿色合成已二酸[J].食品工业科技,2011,32(1):256-257,334.
[18] CAI Lei,LIU Wanyi.Oxidation of Cyclohexanone to Adipic Acid Catalyzed by Heteropoly Complex with Dawson Structure[J].Chinese J Appl Chem,2006,23(1):26-29(in Chinese).蔡磊,刘万毅.Dawson结构杂多盐催化氧化环己酮合成己二酸[J].应用化学,2006,23(1):26-29.
[19] CHEN Xinxiu,XU Pan,XIA Zhining.Methods for Non-thermal Microwave Effects in Microwave Assisted Organic Synthesis[J].Chemistry,2009,(8):674-679(in Chinese).陈新秀,徐盼,夏之宁.微波辅助有机合成中“非热效应”的研究方法[J].化学通报,2009,(8):674-679.
[20] WU Tonghao,LI Jianqing,YANG Hongmao,et al.The Synthesis and Characterization of Molybdophosphoric Acid with Dawson Structure[J].Chem Res Chinese Univ,1991,12(10):1373-1377(in Chinese).吴通好,李建庆,杨洪茂,等.Dawson结构钼磷酸的合成与表征[J].高等学校化学学报,1991,12(10):1373-1377.
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