摘要
为制备性能优异的非涂覆整体式催化剂载体,通过电化学抛光、阳极氧化法、水合热反应和焙烧制备了工业纯铝基γ-Al2O3整体式催化剂载体,利用掠入射XRD、EDS、BET对多孔γ-Al2O3薄膜进行了晶型、比表面积的评价,并利用光学显微镜、扫描电子显微镜对抛光表面和多孔γ-Al2O3形貌进行了分析和膜厚测量。以高氯酸和无水乙醇的混合溶液作为电解液,电化学抛光了工业纯铝表面。在此基础上进行一次阳极氧化和水合焙烧,工艺条件为电压25 V、电解液为0.3 mol/L硫酸、反应温度15℃、反应时间4.0 h、阴阳极间距4 cm、搅拌速率中速,水合温度95℃、水合时间1.5 h,焙烧温度550℃、焙烧时间4 h。所制备的多孔γ-Al2O3整体式催化剂载体的比表面积高达214.86 m2/g,孔径分布均匀。通过正交试验确定了最佳电压、电解液浓度、反应时间和温度,有效避免了金属基"烧穿"现象,所制备的多孔γ-Al2O3薄膜比表面积高,并克服了传统整体式催化剂载体涂层和活性组分易从载体上脱落的缺点。
The industrial pure aluminum-basedγ-Al2O3 monolithic catalyst carrier was prepared by electrochemical polishing,anodizing,hydration heat reaction and calcination.The crystal form and specific surface area of the porousγ-Al2O3 film were investigated by grazing incidence XRD,EDS and BET.The polished surface and the porousγ-Al2O3 morphology were evaluated and measured by optical microscopy and scanning electron microscopy.An industrial pure aluminum surface was electrochemically polished by using a mixed solution of perchloric acid and absolute ethanol as an electrolyte.On this basis,a single oxidation and hydration roasting were carried out under the following conditions:voltage of 25 V,0.3 mol/L dilute sulfuric acid as electrolyte,reaction temperature of 15℃,reaction time of 4.0 h,cathode-anode spacing of 4 cm,stirring speed of medium speed,hydration temperature of 95℃,hydration time of 1.5 h,calcination temperature of 550℃and time of 4.0 h,respectively.The prepared porousγ-Al2O3 monolithic catalyst carrier had a specific surface area of up to 214.86 m2/g and a uniform pore size distribution.The optimum voltage,electrolyte concentration,reaction time and temperature were determined by orthogonal experiment,which effectively avoided the phenomenon of"burn through"of metal.The prepared porousγ-Al2O3 film had high specific surface area,and overcame the disadvantage of easy peeling off for the conventional monolithic catalyst support coating and the active component from the carrier.
作者
梅哲跃
杜红伟
白志鹏
李科
MEI Zhe-yue;DU Hong-wei;BAI Zhi-peng;LI Ke(Key Laboratory of Green Extraction and Efficient Utilization of Light Rare Earth Resources,Ministry of Education,Baotou 014010,China;School of Energy and Environment,Inner Mongolia University of Science and Technology,Baotou 014010,China;School of Materials Science and Engineering,University of Shanghai for Science and Technology,Shanghai 200093,China)
出处
《材料保护》
CAS
CSCD
北大核心
2020年第4期121-126,152,共7页
Materials Protection
基金
国家自然科学基金(51776221)
内蒙古自治区自然科学基金(2018LH05012)资助。
关键词
工业纯铝
阳极氧化
γ-型氧化铝
水合
焙烧
非涂覆整体式催化剂载体
正交试验
industrial pure aluminum
anodic oxidation
γ-Al2O3
hydration
calcination
non-coated monolith catalyst support
orthogonal experiment
