Optimization of reaction conditions for acetone ammoxidation over titanium silicalite-1

The reaction conditions of acetone ammoxidation with NH3 and H2O2 as ammoxidation agents over titanium silicalite-1(TS-1) toward acetone oxime were investigated by single factor experiments.Results showed that the catalyst amount,n(NH3)/n(acetone),n(H2O2)/n(acetone),the addition time of NH3·H2O and H2O2,the ways to introduce NH3·H2O and H2O2,V(tert-butyl alcohol)/V(H2O),and the reaction temperature have a remarkable influence on the reaction.The conversion of the acetone and the selectivity to acetone oxime can reach 95% and 98% under the optimized operation conditions as follows:m(catalyst)/n(acetone) was larger than 4 g/mol,n(NH3)/n(acetone) was above 2.0,n(H2O2)/n(acetone) was at 1.0～1.4,the addition time of NH3·H2O and H2O2 was larger than 1 h,and the dropwise of NH3·H2O and H2O2 at one time,and the following reaction time longer than 1 h,the V(tert-butyl alcohol)/V(H2O) at about 2.3,and the reaction temperature at about 70 ℃.