【摘要】 以纳米钛硅分子筛TS-1为催化剂,采用三口玻璃反应器研究了甲乙酮(MEK)氨氧化的反应性能。采用SEM、TEM和XRD等分析手段表征了TS-1的晶粒尺寸。考察了TS-1的晶粒尺寸、反应物的加料方式、溶剂、催化剂用量、反应温度和反应物料配比对甲乙酮氨氧化反应性能的影响。结果表明,甲乙酮氨氧化反应的最佳反应条件为:75℃,n(NH3)∶n(H2O2)∶n(MEK)=4.0∶1.5∶1.0,TS-1用量21.6g(以1molMEK计);H2O2和氨水连续进料,最佳溶剂为叔丁醇或叔丁醇和水的混和液。在最佳反应条件下,甲乙酮的转化率和甲乙酮肟的选择性可分别达到99.4%和99.8%。更多还原

【Abstract】 The ammoxidation of methyl ethyl ketone （MEK） to methyl ethyl ketoxime （MEKO） over nano-scale TS-1 was studied with a three-neck glass reactor. The effects of crystal size of TS-1 characterized by SEM, TEM, XRD, the addition modes of H₂O₂ and ammonia, the type of solvent, the amount of catalyst used, reaction temperature, the molar ratio of H₂O₂ or NH₃ to MEK were investigated. The results showed that the optimal reaction conditions were as follows: H₂O₂ and ammonia were added slowly and continuously in 1 h, t-butanol or the mixture of t-butanol and water as the solvent, reaction temperature 75℃, 21.6 g of TS-1 for 1 mol MEK, n（NH₃）∶n（H₂O₂）∶n（MEK）=4.0∶1.5∶1.0. Under the optimal reaction conditions, conversion of MEK was up to 99.4%, selectivity of MEKO was up to 99.8%.更多还原