Catalytic synthesis of isooctyl chloroacetate with SO_4~(2-)/ZrO_2-Al_2O_3 solid superacid prepared by ageing at low temperature

SO2-4/ZrO2-Al2O3 Solid superacid catalyst was prepared by coprecipitation in ammonia with ZrOCl2·8H2O and Al(NO3)3·9H2O.Preparing conditions of the catalyst were molar ratio of ZrOCl2·8H2O and Al(NO3)3·9H2O 3 ∶1,-15 ℃ ageing time 24 h,drying at 120 ℃ for 12 h,concentration of sulfuric acid 0.5 mol/L,impregnation time 4 h,drying at 120 ℃ for 1 h,calcination at 650 ℃ for 4 h.As concerning synthesis of 2-ethylhexyl chloroacetate,effects of catalyst dosage,molar ratio of 2-ethylhexanol to chloroacetic acid,reaction time,dosage of water entrainer on esterification rate were studied.Under the optimal conditions of mole ratio of 2-ethylhexanol to chloroacetic acid 1.1 ∶1,cyclohexane of 46% 2-ethylhexanol volume as water entrainer and mass of catalyst for 1.7% of chloroacetic acid,esterification rate is 94.3% at reaction time 1.5 h.