化工进展
化工進展
화공진전
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2014年
1期
105-109
,共5页
刘彦丽%王福余%王崇%赵振波
劉彥麗%王福餘%王崇%趙振波
류언려%왕복여%왕숭%조진파
WO3/ZrO2%固体酸%果糖%5-羟甲基糠醛
WO3/ZrO2%固體痠%果糖%5-羥甲基糠醛
WO3/ZrO2%고체산%과당%5-간갑기강철
tungsten trioxide/zirconium dioxide%solid acid%fructose%5-hydroxymethylfurfural
用共沉淀-热回流处理法制备了系列WO3/ZrO2固体酸催化剂,通过调节W与Zr的摩尔比优化其对果糖脱水制备5-羟甲基糠醛(5-HMF)的催化活性。利用X射线衍射(XRD)、N2吸脱附、氨气程序升温脱附(NH3-TPD)对材料的结构和酸性质进行了表征,并在以二甲基亚砜(DMSO)为溶剂、果糖为原料的催化体系中,考察催化剂的用量、反应时间、反应温度等对5-HMF收率的影响。研究发现,热回流处理大大增加了样品的比表面积,增强了样品的酸强度,当n(W)∶n(Zr)=0.1∶1时,样品比表面积最大,催化活性最好,以其为催化剂,在130℃下反应3 h条件下,5-HMF收率最高可达80.29%。
用共沉澱-熱迴流處理法製備瞭繫列WO3/ZrO2固體痠催化劑,通過調節W與Zr的摩爾比優化其對果糖脫水製備5-羥甲基糠醛(5-HMF)的催化活性。利用X射線衍射(XRD)、N2吸脫附、氨氣程序升溫脫附(NH3-TPD)對材料的結構和痠性質進行瞭錶徵,併在以二甲基亞砜(DMSO)為溶劑、果糖為原料的催化體繫中,攷察催化劑的用量、反應時間、反應溫度等對5-HMF收率的影響。研究髮現,熱迴流處理大大增加瞭樣品的比錶麵積,增彊瞭樣品的痠彊度,噹n(W)∶n(Zr)=0.1∶1時,樣品比錶麵積最大,催化活性最好,以其為催化劑,在130℃下反應3 h條件下,5-HMF收率最高可達80.29%。
용공침정-열회류처리법제비료계렬WO3/ZrO2고체산최화제,통과조절W여Zr적마이비우화기대과당탈수제비5-간갑기강철(5-HMF)적최화활성。이용X사선연사(XRD)、N2흡탈부、안기정서승온탈부(NH3-TPD)대재료적결구화산성질진행료표정,병재이이갑기아풍(DMSO)위용제、과당위원료적최화체계중,고찰최화제적용량、반응시간、반응온도등대5-HMF수솔적영향。연구발현,열회류처리대대증가료양품적비표면적,증강료양품적산강도,당n(W)∶n(Zr)=0.1∶1시,양품비표면적최대,최화활성최호,이기위최화제,재130℃하반응3 h조건하,5-HMF수솔최고가체80.29%。
Catalytic dehydration of fructose to 5-hydroxymethylfurfural (5-HMF) was studied and improved by synthesizing series of solid acid catalyst WO3/ZrO2 with different mole ratio of W to Zr using co-precipitation with hot reflux method. The structure and properties of the catalysts thus synthesized were investigated by X-ray diffraction(XRD),N2 sorption,temperature -programmed desorption of (NH3-TPD),and then the influence of temperature,mass ration of fructose/catalyst and reaction time on the yield of 5-HMF from fructose were studied in dimethyl sulfoxide. These studies showed that specific surface area and acid strength of the catalysts were increased greatly by hot reflux method,and an optimized 5-HMF yield of 80.29%was obtained with 3 h at 130 ℃ in the presence of the sample WO3/ZrO2 with W-Zr mole ratio of 0.1∶1,which had a largest specific surface area and best catalytic activity.