| Because of its high photon quantum yield and good stability,polyfluorene(PF)is chosen as an excellent polymer blue light material.The Suzuki reaction is a typical method for manufacturing polyfluorene materials.It involves the synthesis of dibromo monomers and diboronic acid monomers.Before the Suzuki reaction,monomer purification is essential,and high-purity reaction monomers are advantageous to the Suzuki reaction.Because of its ease of use and excellent purification effectiveness,the solvent anti-solvent precipitation method is one of the most extensively used monomer purification methods.Due to a decrease in monomer concentration in the later stages of the Suzuki reaction,the reaction rate reduced and the reaction time increased.The rotating packed bed(RPB)is a device that improves micro-mixing and mass transfer,whether it’s for the increased solvent anti-solvent precipitation method’s two-phase mixing or the enhanced Suzuki reaction.All of them have a strong promotional effect.To improve the efficiency of monomer purification,the RPB enhanced solvent anti-solvent precipitation method is utilized in this study,and the Suzuki reaction is moved to the RPB reactor to minimize the Suzuki reaction time and improve the reaction efficiency.The following are the specifics:(1)The solubility of 9,9-dihexyl-2,7-dibromofluorene(F6-Br)and9,9-dihexylfluorene-2,7-diboronic acid(F6-B)was determined in 12solvents and 9 solvents.The modified Apelblat equation was used to correlate the measured solubility data,resulting in a solubility model with a maximum mean square error of 4.42×10-3.The experimental results were mostly in line with what was predicted.(2)The appropriate solvent and anti-solvent for the two monomers were chosen for precipitation and purification based on the solubility data,and the best reaction conditions were investigated.Purity after purification can achieve 99.42%and 99.01%when the temperature is10°C,the solvent-anti-solvent ratio is 1:20,the solution concentration is1 mg/m L,and the shift duration is 1min.Purification purity can reach99.88%and 99.87%when using the high gravity method to boost the solvent anti-solvent purification process.The scale-up trials of the two approaches reveal that the high gravity method’s increased solvent anti-solvent purification is unaffected by the scale-up effect.(3)To synthesize poly(9,9-dihexylfluorene)luminous materials,the Suzuki reaction was utilized,and the ideal reaction conditions were investigated to find the best reaction time,temperature,alkali,and catalyst dose.The RPB reactor was used to improve the reaction process and figure out what the best reaction time and rotation speed were.The RPB reactor significantly raised the Suzuki reaction rate,shortened reaction time,increased the molecular weight of the polymer product,and decreased the dispersibility index,according to the findings. |