化学研究与应用
化學研究與應用
화학연구여응용
CHEMICAL RESEARCH AND APPLICATION
2014年
1期
13-17
,共5页
李宗群%邰燕芳%张敏%裘灵光
李宗群%邰燕芳%張敏%裘靈光
리종군%태연방%장민%구령광
金属-有机骨架%纳米晶%超声合成%催化氧化
金屬-有機骨架%納米晶%超聲閤成%催化氧化
금속-유궤골가%납미정%초성합성%최화양화
metal-organic framework%nanocrystals%ultrasonic synthesis%catalytic oxidation
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( H2 O2)∶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%。
以硝痠銅和異煙痠(HINA)為原料,採用超聲輻射法,閤成瞭具有一維結構的Cu(INA)2·4H2O納米晶。採用x射線衍射、透射電鏡、紅外光譜等技術對該納米晶的結構和形貌進行瞭錶徵。結果錶明,超聲10 min即可穫目標產物;在超聲輻射的條件下,通過控製反應時間,能夠調控該納米晶呎吋和形貌。以雙氧水為氧化劑,攷察不同納米晶對苯乙烯的催化氧化活性,結果顯示反應溫度為60℃、反應時間為12 h,n( H2 O2)∶n(苯乙烯)∶n(催化劑)=1800∶300∶1時,氧化產物以苯甲醛和環氧苯乙烷為主,苯乙烯的最大轉化率達到85.5%,轉化數(TON)為252,苯環氧乙烷的選擇性為69.1%。
이초산동화이연산(HINA)위원료,채용초성복사법,합성료구유일유결구적Cu(INA)2·4H2O납미정。채용x사선연사、투사전경、홍외광보등기술대해납미정적결구화형모진행료표정。결과표명,초성10 min즉가획목표산물;재초성복사적조건하,통과공제반응시간,능구조공해납미정척촌화형모。이쌍양수위양화제,고찰불동납미정대분을희적최화양화활성,결과현시반응온도위60℃、반응시간위12 h,n( H2 O2)∶n(분을희)∶n(최화제)=1800∶300∶1시,양화산물이분갑철화배양분을완위주,분을희적최대전화솔체도85.5%,전화수(TON)위252,분배양을완적선택성위69.1%。
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.