焙烧温度对Silicalite-1催化环己酮肟气相Beckmann重排反应的影响  

EFFECT OF CALCINATION TEMPERATURE ON PERFORMANCE OF SILICALITE-1 FOR VAPOR PHASE BECKMANN REARRANGEMENT OF CYCLOHEXANONE OXIME

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作  者:张帆[1] 魏会娟[1] 窦晓勇 王向宇[1] 

机构地区:[1]郑州大学化学与分子工程学院工业催化研究所,郑州450001 [2]中国平煤神马集团

出  处:《石油炼制与化工》2014年第10期52-56,共5页Petroleum Processing and Petrochemicals

基  金:河南省杰出人才创新基金(No.0221001200);河南省重大科技专项(No.131100210900)

摘  要:采用水热方法合成Silicalite-1分子筛,考察不同焙烧温度处理后用于催化环己酮肟气相Beckmann重排反应的催化性能。利用XRD,IR,BET和热分析方法对分子筛进行表征。结果表明,焙烧温度对环己酮肟的转化率和分子筛稳定性的影响较大,而对己内酰胺的选择性影响不明显。随着焙烧温度的升高,分子筛的比表面积变化不明显,而外表面积先增大后减小,微孔体积占总孔体积的比例呈下降趋势。最佳的焙烧温度为400℃,在该焙烧温度下的分子筛用于气相Beckmann重排反应中的活性和稳定性最佳。Silicalite-1 was synthesized by hydrothermal method. The catalytic performance of Sili- calite-1 treated by different calcination temperatures in vapor phase Beckmann rearrangement of cyclo- hexanone oxime was investigated. Silicalite-1 catalysts were characterized by XRD, IR, BET and ther- mal analysis. The results show that the calcination temperature has an important effect on the conver- sion of cyclohexanone oxime and the stability of the Silicalite-1 catalyst, but no obvious influence on the selectivity of caprolactam. With the increase of calcination temperature, BET surface area of molecular sieve does not change significantly, while external surface area first increases and then decreases. The ratio of micropore volume to the total volume is on the decline. The Silicalite-1 calcinated at 400 ℃ ex- hibits an excellent activity and stability in vapor phase Beckmann rearrangement reaction.

关 键 词:SILICALITE-1 环己酮肟 贝克曼重排 焙烧温度 

分 类 号:TQ225.261[化学工程—有机化工]

 

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