Study On 1,1,1,3-Tetrachloropropane Synthesis And Industrization

1,1,1,3-tetrachloropropane is an important fine chemical,the new application of cut CTC,so the study on 1,1,1-3-tetrachloropropane synthesis process and its industrialization has significant practical impacts.Through laboratory test,pilot and amplified production,the author studies and finds solutions to the uncertainty and problems that occur during the industrial production of tetrachloropropane.During laboratory test,the author chose different production routes,raw materials and processes aiming to study the following variables’ impacts on the reaction,namely,different catalysts,operating pressure,temperature,contact time and catalyst ratio.In addition,the author proved the reaction reliability through reaction stability tests.During pilot phase,the author studied the general rules and conditions of tetrachloropropane synthesis to cast insights into the impacts of catalyst volume,operating pressure,temperature,CTC recovery and other elements on the production process.He also attempted to explore the product purification methods.Furthermore,reasonability of designed process and applicability of equipment specifications calculated through emulation were also proved.The commercial tests involve commercial production with scaled-up manufacturing facility to verify the performance of amplified tetrachloropropane production.Emphasizing synthesis reaction and separation processes,the author delved deep into the optimal process conditions and equipment bottleneck problems to achieve reaction safety,processes simplification and product economy.Through all the tests and researches above,it can be concluded that the optimal conditions for kettle-type telomerization synthesis reaction are as follows:composite catalyst:consisting of iron powder and triethyl phosphate with the 9:1 wt%;reaction pressure:0.7～1.0MPa;temperature:110～135℃;reaction time:5-8h.As one of the raw materials,ethylene yield reaches 98～99.9%and tetrachloropropane selectivity is 91～98%.Besides,product purification and by-product treatment processes are optimized.Operating methods and conditions are finally determined.