超声合成Cu(INA)_2·4H_2O纳米晶及催化氧化苯乙烯

Ultrasonic synthesis Cu(INA)_2 ·4H_2O nanocrystals and catalytic oxidation of styrene

以硝酸铜和异烟酸(HINA)为原料,采用超声辐射法,合成了具有一维结构的Cu(INA)2·4H2O纳米晶。采用x射线衍射、透射电镜、红外光谱等技术对该纳米晶的结构和形貌进行了表征。结果表明,超声10 min即可获目标产物;在超声辐射的条件下,通过控制反应时间,能够调控该纳米晶尺寸和形貌。以双氧水为氧化剂,考察不同纳米晶对苯乙烯的催化氧化活性,结果显示反应温度为60℃、反应时间为12 h,n(H2O2)∶n(苯乙烯)∶n(催化剂)=1800∶300∶1时,氧化产物以苯甲醛和环氧苯乙烷为主,苯乙烯的最大转化率达到85.5%,转化数(TON)为252,苯环氧乙烷的选择性为69.1%。

Nanocrystals of a one-dimensional（1-D）metal-organic framework（MOFs）of Cu（INA）2.4H2O were synthesized using ul-trasonic method at room temperature. The samples were characterized by XRD,FTIR,TEM. The results indicated that the product were obtained as expected of ultrasonic irradiation for 10 min gave Cu（INA）2.4H2O in 47. 0%yield. TEM revealed that size and shape of nanocrystals could be tuned by varying the reaction time. The nanocrystallines of as-synthesised were investigated on cata-lytic oxidation styrene with H2 O2 as the oxidant. The results suggested that benzaldehyde and styrene oxide were obtained as the ma-jor products. The conversion reached up to 85. 5%,turnover number was 252,and selectivity for 69. 1%under the reaction tempera-ture 60 ℃,reaction time 12 h and the molar ratio of n（ H2 O2 ）∶n（ styrene）∶n（ cat） was 1800∶300∶1.