Study On Conntinuous Coupling Reaction And Sulfonation Reaction In Microchannel Reactor

Micro-chemical technology is a new technology to realize green synthesis through strengthening process,compared with traditional batch reactor,micro-channel reactor has advantages as follows: high heat efficiency and mass transfer property,small probability of back mixing,better controlled in reaction temperature and resident time,and continuous production can be achieved.in the dissertation,the PTFE microchannel reactor and 316 L stainless steel microchannel reactor were designed for the application of micro-chemical technology in coupling reaction and sulfonation reaction.The coupling reaction and sulfonation reaction in microchannel reactor were studied.A model study was initiated with C.I.acid blue 29 and C.I.reactive red 195 as substrate,the effects of the reaction flow,the residence time,the pipe inner diameter and the reaction temperature on the single-pass conversion and selectivity were evaluated.The optimum process parameters of C.I.reactive red 195 were selected as follows: at room temperature,flow rate 0.55 m/min,residence time 3.63 min,tube diameter 0.8 mm,the yield reached to 91.0%.The optimum process parameters of the acid coupling about the C.I.acid blue 29 was selected as follows: at room temperature,flow rate 0.12 m/s,residence time 17.2 s,tube diameter 0.8 mm.The optimum process parameters of the alkaline coupling about the C.I.acid blue 29 was selected as follows: at room temperature,flow rate 0.30 m/s,residence time 5.1 s,tube diameter 1.2 mm,The total yield reached to 91.9%.The synthesis of azo dyes such as C.I.acid black 10 B,C.I.acid red 1 and C.I.reactive black 5 were studied according to the synthesis process about C.I.acid blue 29 and C.I.reactive red 195.The yield was above 90%,especially C.I.reactive black 5 because of its large solubility,so in particular the C.I.reactive black 5 alkaline coupling was amplified study,C.I.reactive black 5 alkaline coupling better process conditions: the concentration of 0.03 mol/L,the temperature 20℃,flow rate 0.13 m/s,residence time75.4 s,pipe diameter 4 mm,the target product yield reached 95.6%.The sulfonation reaction of toluene in microchannels was studied by the synthesis of CLT acid.The effects of temperature,residence time,flow rate and molar ratio(concentrated sulfuric acid / toluene)on the sulfonation reaction The optimum conditions were as follows: temperature 100 ℃,flow rate 0.01 m/s,n(concentrated sulfuric acid / toluene)2.8,residence time 600 s,p-toluenesulfonic acid selectivity reached 89.5%,one-way conversion rate of 66%,single-way yield of 59.1%.The results show that the process has the advantages of high efficiency,mild condition and continuous process.