对甲酚常压液相催化氧化制备对羟基苯甲醛  

Synthesis of p-hydroxybenzaldehyde by the liquid-phase catalytic oxidation of p-cresol under ambient pressure

作　　者：邵俊泉[1] 陈晓亚[1] 罗聪颖[1] 张斌[1] 章亚东[1] 

机构地区：[1]郑州大学化工与能源学院,河南郑州450001

出　　处：《现代化工》2017年第5期140-144,共5页Modern Chemical Industry

摘　　要：以钴铜为主催化剂,镍锆为助催化剂,TiO_2为载体,用浸渍法制备一系列负载型催化剂,并用XRD、IR对其进行表征。将催化剂用于对甲酚常压液相催化氧化制备对羟基苯甲醛(PHBA)的反应中,结果表明,n(Co^(2+))∶n(Cu^(2+))=3∶1,n(Co^(2+))∶n(Ni^(2+))=1∶0.06,n(Co^(2+))∶n(Zr^(2+))=1∶0.005时,催化剂的催化效果最佳。同时,考察了反应温度、氢氧化钠用量、反应时间、通氧量、甲醇用量对该反应的影响。在单因素实验基础上,采用正交实验优化出该反应较佳工艺:反应时间为5 h,反应温度为75℃,甲醇用量为30 m L,n(氢氧化钠)∶n(对甲酚)=5∶1,通氧量为50 m L/min。以对甲酚计,PHBA的收率为92.58%。所制备催化剂在常压下对于对甲酚的催化氧化反应具有较高的催化活性和重复性。A series of supported catalysts using Co and Cu as main catalysts,Ni and Zr as sub-catalysts and TiO2 as carrier are prepared by the impregnation method,and then are characterized by XRD and IR. The catalysts are used in the liquid-phase catalytic oxidation reaction of p-cresol to make p-hydroxybenzaldehyde（ PHBA） under ambient pressure,and results show that when n（ Co2＋） ∶ n（ Cu2＋） = 3∶ 1,n（ Co2＋） ∶ n（ Ni2＋） = 1∶ 0. 06,n（ Co2＋） ∶ n（ Zr2＋） = 1∶0. 005,the catalysts have the best catalytic effect. At the same time,the influences of reaction parameters such as reaction temperature,molar ratio of Na OH to p-cresol,reaction time,oxygen flow rate and methanol dosage on the reaction are studied. On the basis of single factor experiments,the orthogonal experimentis designed to optimize reaction conditions,i. e.,reaction time being 5 h,reaction temperature 75℃,methanol dosage 30 m L,n（ Na OH） ∶ n（ PHBA） = 5 ∶ 1,oxygen flow rate 50 m L/min,and then the yield of PHBA based on the amount of p-cresol is 92. 58%. The prepared catalyst under ambient pressure exhibits excellent catalytic activity and reusability in the catalytic oxidation reaction of p-cresol.

关 键 词：催化氧化 常压 液相 对甲酚 PHBA 

分 类 号：TQ452[化学工程—农药化工]