Process Development Of Tert-butylamine

There exist disadvantages of serious corrosion of acid and alkali, highly toxic ofraw materials, high cost, strict process condition and seriously polluted. For this,Reactive Distillation(RD) was introduced to product the high purity of2-chloro-2-methylpropane used tert-butanol and hydrochloric acid as raw material.Reaction and distillation were integrated in the RD column. Distillation was improvedby reaction so that the conversion of tert-butanol was effectively improved, thus theload and energy consumption of the following refined section were reduced. we usedthe high purity of2-chloro-2-methylpropane and ammonia as raw material, methanolas solvent to product tert-butylamine. Therefore, the equipment investment and energyconsumption were significantly reduced. The process was studied systematicallythrough the method of combining experiment and Aspen Plus simulation together.The reaction between tert-butanol and hydrochloric acid was studied by smallscale experiment. The reaction kinetic equation were:RD pilot was constructed to carry out continuous production of2-chloro-2-methylpropane. Adjusting the process parameters to produce pure productof top of column. The suitable process parameters were the temperature of top ofcolumn50.5℃, the temperature of bottom of column100.9℃. The content of2-chloro-2-methylpropane was97%, the content of tert-butanol was0.322%, thecontent of water was1.678%in the top of column. In the bottom of column, thecontent of hydrochloric acid was4.93%, the content of tert-butanol was0.0037. Theproduct of top of column was refined to remove water. The best effect was calciumchloride. The content of water was reduced to0.365%.The effect of reaction factors was investigated for the reaction used2-chloro-2-methylpropane and ammonia as raw material. When used methanol assolvent, The reaction rate was quick, the conversion of2-chloro-2-methylpropane wasmost high. The suitable process parameters were temperature90℃, reaction time1h, the pressure10atm, feeding ratio ω(methanol)：ω(2-chloro-2-methylpropane)4:1. Onthe basis of these parameters, the conversion of2-chloro-2-methylpropane was95.3%,the yield of tert-butylamine88%. The content of ammonium chloride of solid productwas98%, the solid average particle size was1330nm, the sedimentation velocity was0.0837cm/s.The process was simulated by ASPEN PLUS and the good agreement betweensimulation result and the pilot experiment indicated that the software can be used forthis process simulation. Preliminary design of the continuous process for1000t/y2-chloro-2-methylpropane production was carried out, the process equipmentparameters and technological conditions were designed and optimized by the use ofcomputer simulation. The appropriate operating parameters were: total plate number18, with8for reaction,5for distillation,5for stripping; reflux ratio2; the flow rate oftert-butanol1.04t/h, the flow rate of hydrochloric acid1.894t/h. Simulated based onthis condition, the composition of2-chloro-2-methylpropane at the top of column was96.17%, the purity of tert-butanol at the bottom of column was3.6×10-4%.