摘要
以钛硅分子筛(Ts-1)为催化剂,过氧化氢和丙酮为原料,催化氨氧化合成丙酮肟。对影响合成反应的多个因素进行了考察,合成条件经正交实验优化后丙酮肟产率有了较为明显的提高。结果表明:在反应温度65℃,搅拌转速320 r/min,质量分数30%过氧化氢水溶液滴加3.5~4.5 h,催化剂用量为丙酮质量的40%,n(丙酮)∶n(H2O2)∶n(NH3)=1∶1.1∶3.5,溶剂V(水)∶V(异丙醇)=1∶1的混合溶剂,此时丙酮肟产率〉80%。向系统中充入惰性气体可减少副反应的发生,提高丙酮肟收率。
Acetone oxime was synthesized by catalytic ammoxidation using Ti-Si molecular sieve(TS-1) as catalyst,hydrogen peroxide and acetone as raw materials.Many factors affecting the synthesis reaction are studied.The yield of acetone oxime obviously increased through optimizing synthesis conditions by orthogonal experiments.The results show that the yield of acetone oxime can reach over 80% when reaction temperature is 65℃,stirring speed is 320r/min,dropping time of 30% hydrogen peroxide aqueous solution is 3.5~4.5h,catalyst mass fraction based on acetone is 40%,n(acetone):n(H2O2):n(NH3)=1:1.1: 3.5,V(water):V(isopropanol)=1:1 mixture is used as solvent.Feeding inert gas to system can decrease the side reactions,and increase the yield of acetone oxime.
出处
《化学推进剂与高分子材料》
CAS
2011年第2期67-69,共3页
Chemical Propellants & Polymeric Materials
关键词
钛硅分子筛
丙酮肟
催化氨氧化
过氧化氢
正交实验
Ti-Si molecular sieve
acetone oxime
catalytic ammoxidation
hydrogen peroxide
orthogonal experiment