微波辐射改性可膨胀石墨催化合成苯甲醛乙二醇缩醛  

Synthesis of Benzaldehyde Glycol Acetal Catalyzed by Expandable Graphite Modified Under Microwave Irradiation

作　　者：陈小燕[1] 杨浩[2] 谢昊[1] 李和平[1] 刘万毅[1] 

机构地区：[1]宁夏大学化学化工学院,宁夏银川750021 [2]宁夏生产力促进中心,宁夏银川750001

出　　处：《精细化工》2011年第9期880-882,892,共4页Fine Chemicals

基　　金：宁夏自然科学基金(NZ1021);宁夏大学科学研究基金项目〔(E)ndzr09-32〕~~

摘　　要：以改性可膨胀石墨为催化剂,微波辐射下制备了苯甲醛乙二醇缩醛。通过正交实验考察了合成苯甲醛乙二醇缩醛的影响因素。结果表明,当n(苯甲醛)∶n(乙二醇)=1∶2.5,催化剂占反应物总质量的2.04%,微波辐射功率300 W,辐射时间20 min,带水剂环己烷6 mL时,缩醛的收率可达87.6%;并且催化剂重复使用4次后活性基本不变。通过对催化剂进行SEM和XRD测试表明,H2SO4分子已插入到石墨层中形成层间化合物。Expandable graphite modified under microwave irradiation was prepared and then used as catalyst in the synthesis of benzaldehyde glycol acetal. The influencing factors in the synthesis process were investigated through orthogonal experiment. The optimum conditions were as follows ： molar ratio of benzyladehyde to glycol 1 ： 2.5, mass ratio of the catalyst to the total reactants 2.04% , microwave irradiation power 300 W, irradiation time 20. 0 rain, and the amount of cyclohexane was 6 mL. Under such optimum conditions,the yield of acetal reached 87.6% , and the activity of the catalyst remained basically unchanged after being used for 4 times. The catalyst was studied by SEM and XRD, and the results show that an interlayer compound was instituted by sulfuric acid molecules inserted into the graphite＇s layers.

关 键 词：改性可膨胀石墨 微波辐射 苯甲醛乙二醇缩醛 香料 

分 类 号：TQ655[化学工程—精细化工]