摘要
通过外部磁场来分离粉状非均相催化剂,可以有效地提高分离效率。以具有超顺磁性的磁性纳米Fe_(3)O_(4)为载体,通过硅烷偶联剂,将对羟基苯乙酮肟锚合在Fe_(3)O_(4)表面,然后再用Pd(OAc)_(2)配合制备出磁性可回收的对羟基苯乙酮肟钯配体催化剂(Fe_(3)O_(4)@oxime)-Pd)。采用XRD、TG、振动样品磁强分析(VSM)等分析方法对所制备催化剂的结构、负载量和磁性进行了表征。考察了反应条件对Fe_(3)O_(4)@oxime)-Pd催化Suzuki反应性能的影响。实验结果表明,在水/乙醇混合溶剂中、碳酸钾作碱、反应温度为40℃、反应时间为30 min、催化剂用量为0.34 mol%的钯含量时,催化对溴苯乙酮与苯硼酸的Suzuki反应产物收率大于96%。Fe_(3)O_(4)@oxime)-Pd催化剂对含吸电基团和供电基团的溴代苯具有良好的普适性。
The separation efficiency can be effectively improved by using external magnetic field to separate the heterogeneous powder catalysts.The p-hydroxyacetophenone oxime is anchored on the magnetic nano Fe_(3)O_(4) which has a superparamagnetic property by silane coupling agent,and then it is complexed with Pd(OAc)2 to prepare magnetic recyclablep-hydroxyacetophenone oxime palladium complex catalyst(Fe_(3)O_(4)@oxime)-Pd).The structure,loading amount and magnetic properties of the prepared catalyst are characterized by means of XRD,TG and VSM.The effects of reaction conditions on the catalytic performance of Fe_(3)O_(4)@oxime)-Pd for Suzuki reaction are investigated.The experimental results show that the Suzuki reac-tion product's yield is more than 96%when the reaction temperature is 40℃,the reaction time is 30 min,the amount of catalyst is 0.34 mol%of palladium and the potassium carbonate is used as the base in a water/ethanol mixture.The Fe_(3)O_(4)@oxime-Pd catalyst has an excellent adaptability for the bromobenzene containing electron-withdrawing group and electron-donating group.
作者
单雯妍
樊惠娟
白雪峰
SHAN Wenyan;FAN Huijuan;BAI Xuefeng(Institute of Petrochemistry,Heilongjiang Academy of Sciences,Harbin 150040,China)
出处
《化学与粘合》
CAS
2023年第3期205-208,共4页
Chemistry and Adhesion
基金
黑龙江省科学院科研基金项目。
