Using self-made solid-phase reaction complete sets of equipment(model SRE-1000), Solid-state dehydroacetic acid , sodium hydroxide and sodium carbonate were grinded together then Leading to solid-phase reaction producing food preventive sodium dehydroacetate. Orthogonal experiment results showed that the dehydroacetic acid reaction with molar ratio of 3∶7 NaOH and Na2CO3 mixture was the optimal ratio, Adding solid base twice could accelerate the solid-state reaction smoothly. Response surface experimental design was used to optimize the grinding media ratio of alumina ball, as a result, when different diameter alumina ball were 18 = 254 kg, 27 = 368 kg, 35 = 252 kg, the time for solid-phase reaction was shortest which was 444.7 minutes.