石油化工
石油化工
석유화공
PETROCHEMICAL TECHNOLOGY
2009年
11期
1151-1157
,共7页
李占双%范美青%刘岩峰%张艳%王君%刘琦
李佔雙%範美青%劉巖峰%張豔%王君%劉琦
리점쌍%범미청%류암봉%장염%왕군%류기
化学共沉淀法%复合氧化物%磁性固体酸催化剂%酯化反应
化學共沉澱法%複閤氧化物%磁性固體痠催化劑%酯化反應
화학공침정법%복합양화물%자성고체산최화제%지화반응
chemical co precipitation%composite oxide%magnetic solid acid catalyst%esterification
采用化学共沉淀法制备了SO_4~(2-)/ZrO_2/Fe_3O_4/TiO_2磁性固体酸,利用X射线衍射、示差扫描量热、Mssbauer谱、透射电子显微镜、NH_3-程序升温脱附、N_2吸附-脱附、磁滞回线等手段对磁性固体酸的结构与性质进行了表征.表征结果显示,磁性基质Fe_3O_4及TiO_2的引入有利于四方晶相ZrO_2(t)的稳定;ZrO_2晶体生长取向于ZrO_2(t)的(101)方向,(101)晶面间距为0.293 nm;Mssbauer谱中双峰的存在表明磁性基质Fe_3O_4的存在;在室温下磁性固体酸具有超顺磁性.以乙酸乙酯的合成为探针反应,考察了SO_4~(2-)/ZrO_2/Fe_3O_4/TiO_2磁性固体酸催化剂的催化性能,实验结果表明,外加磁场使酯化反应的醋酸转化率提高到92%.
採用化學共沉澱法製備瞭SO_4~(2-)/ZrO_2/Fe_3O_4/TiO_2磁性固體痠,利用X射線衍射、示差掃描量熱、Mssbauer譜、透射電子顯微鏡、NH_3-程序升溫脫附、N_2吸附-脫附、磁滯迴線等手段對磁性固體痠的結構與性質進行瞭錶徵.錶徵結果顯示,磁性基質Fe_3O_4及TiO_2的引入有利于四方晶相ZrO_2(t)的穩定;ZrO_2晶體生長取嚮于ZrO_2(t)的(101)方嚮,(101)晶麵間距為0.293 nm;Mssbauer譜中雙峰的存在錶明磁性基質Fe_3O_4的存在;在室溫下磁性固體痠具有超順磁性.以乙痠乙酯的閤成為探針反應,攷察瞭SO_4~(2-)/ZrO_2/Fe_3O_4/TiO_2磁性固體痠催化劑的催化性能,實驗結果錶明,外加磁場使酯化反應的醋痠轉化率提高到92%.
채용화학공침정법제비료SO_4~(2-)/ZrO_2/Fe_3O_4/TiO_2자성고체산,이용X사선연사、시차소묘량열、Mssbauer보、투사전자현미경、NH_3-정서승온탈부、N_2흡부-탈부、자체회선등수단대자성고체산적결구여성질진행료표정.표정결과현시,자성기질Fe_3O_4급TiO_2적인입유리우사방정상ZrO_2(t)적은정;ZrO_2정체생장취향우ZrO_2(t)적(101)방향,(101)정면간거위0.293 nm;Mssbauer보중쌍봉적존재표명자성기질Fe_3O_4적존재;재실온하자성고체산구유초순자성.이을산을지적합성위탐침반응,고찰료SO_4~(2-)/ZrO_2/Fe_3O_4/TiO_2자성고체산최화제적최화성능,실험결과표명,외가자장사지화반응적작산전화솔제고도92%.
Nano magnetic solid acids SO_4~(2-)/ZrO_2/Fe_3O_4/TiO_2 were prepared by co precipitation. Obtained samples were characterized by XRD, DSC, Mssbauer, TEM, NH_3 TPD,N_2 adsorption desorption and magnetic hysteresis loop. The introduction of TiO_2 and magnetic substrate Fe_3O_4 were beneficial to keep tetragonal crystalline structure of ZrO_2 from transferring to monoclinic form in calcination, ZrO_2 crystals grew along the direction of (101) crystal plane. The interplanar distance of ZrO_2(t) (101) plane were 0.293 nm. Mssbauer results revealed the existence of magnetic substrate Fe_3O_4 particles. Magnetic measurement showed superparamagnetism of solid acid catalyst at ambient temperature. Taking synthesis of ethyl acetate as probe reaction for evaluating the activity of nano magnetic solid acid SO_4~(2-)/ZrO_2/Fe_3O_4/TiO_2 catalyst, the conversion of acetic acid in the esterification mounted to 92% in external magnetic field and aggregation of nano magnetic solid acid catalyst was avoided.