物理化学学报
物理化學學報
물이화학학보
ACTA PHYSICO-CHIMICA SINICA
2012年
9期
2148-2154
,共7页
杨志旺%陈丽娜%洪伟%康瑞雪%王佳%贾娜%赵磊%马恒昌
楊誌旺%陳麗娜%洪偉%康瑞雪%王佳%賈娜%趙磊%馬恆昌
양지왕%진려나%홍위%강서설%왕가%가나%조뢰%마항창
固体酸%缩合反应%Baeyer-Villiger氧化%Fe2O3-掺杂%硫酸氧化锡
固體痠%縮閤反應%Baeyer-Villiger氧化%Fe2O3-摻雜%硫痠氧化錫
고체산%축합반응%Baeyer-Villiger양화%Fe2O3-참잡%류산양화석
Solid acid%Acetalization%Baeyer-Villigeroxidation%Fe2O3-doping%Sulfated tin oxide
采用共沉淀的方法制备了不同Fe掺杂量的SO2-4/SnO2-Fe2O3固体超强酸催化剂.利用傅里叶变换红外(FTIR)光谱,粉末X射线衍射(XRD),N2吸附-脱附实验(BET),热重(TG)分析和扫描电镜(SEM)等方法对样品进行了表征.考察了所得催化剂对4-叔丁基环己酮与乙二醇缩合反应的催化性能.实验结果表明,与未经过掺杂改性的SO;-/SnO2固体酸催化剂相比,改性后催化剂的催化性能得到了改善.研究了以Fe/Sn摩尔比为0.5的SO2-4/SnO2-Fe2O3固体酸为催化剂,部分醛酮类化合物与乙二醇及1,2-丙二醇的缩合反应.考察了反应时间、催化剂用量等因素对反应的影响.同时,将所得催化剂应用于环酮Baeyer-ViIIiger氧化反应中,催化剂表现出良好的催化活性,且催化剂具有一定的循环使用性.
採用共沉澱的方法製備瞭不同Fe摻雜量的SO2-4/SnO2-Fe2O3固體超彊痠催化劑.利用傅裏葉變換紅外(FTIR)光譜,粉末X射線衍射(XRD),N2吸附-脫附實驗(BET),熱重(TG)分析和掃描電鏡(SEM)等方法對樣品進行瞭錶徵.攷察瞭所得催化劑對4-叔丁基環己酮與乙二醇縮閤反應的催化性能.實驗結果錶明,與未經過摻雜改性的SO;-/SnO2固體痠催化劑相比,改性後催化劑的催化性能得到瞭改善.研究瞭以Fe/Sn摩爾比為0.5的SO2-4/SnO2-Fe2O3固體痠為催化劑,部分醛酮類化閤物與乙二醇及1,2-丙二醇的縮閤反應.攷察瞭反應時間、催化劑用量等因素對反應的影響.同時,將所得催化劑應用于環酮Baeyer-ViIIiger氧化反應中,催化劑錶現齣良好的催化活性,且催化劑具有一定的循環使用性.
채용공침정적방법제비료불동Fe참잡량적SO2-4/SnO2-Fe2O3고체초강산최화제.이용부리협변환홍외(FTIR)광보,분말X사선연사(XRD),N2흡부-탈부실험(BET),열중(TG)분석화소묘전경(SEM)등방법대양품진행료표정.고찰료소득최화제대4-숙정기배기동여을이순축합반응적최화성능.실험결과표명,여미경과참잡개성적SO;-/SnO2고체산최화제상비,개성후최화제적최화성능득도료개선.연구료이Fe/Sn마이비위0.5적SO2-4/SnO2-Fe2O3고체산위최화제,부분철동류화합물여을이순급1,2-병이순적축합반응.고찰료반응시간、최화제용량등인소대반응적영향.동시,장소득최화제응용우배동Baeyer-ViIIiger양화반응중,최화제표현출량호적최화활성,차최화제구유일정적순배사용성.
Fe-doped SO2-4/SnO2 (STF) solid acid catalysts with different amounts of iron were prepared via co-condensation,followed by sulfation and calcination.These materials were characterized by Fourier transform infrared (FTIR) spectroscopy,X-ray powder diffraction (XRD),N2 adsorption-desorption analysis (BET),thermogravimetric (TG) analysis,and scanning electron microscopy (SEM).The Fe-doped catalysts exhibited more activity than undoped catalysts in acetalization reactions of 4-tert-butylcyclohexanone and diols.The catalytic acetalization of several ketones and 1,2-diols with the SO2-4/SnO2-Fe2O3 catalysts (with the Fe/Sn molar ratio of 0.5) were studied.The influence of the reaction time and the amount of the catalysts on the acetalization were also investigated.In addition,the high performance of this Fe-modified catalyst was demonstrated in the Baeyer-Villiger oxidation of cyclic ketones.The catalyst can be recycled several times without any significant loss in catalytic activity.