New Technology Of Synthesis And Separation Of DL-camphor Sulfonic Acid

Camphor sulfonic acid(CSA),an important organic intermediate,is widely used in pharmaceuticals,light industry and daily chemicals.However,since the synthetic camphor is a racemic mixture,the CSA synthesized from the sulfonating of synthetic camphor is always a mixture of enantiomer pairs.At present,in China,most of the pure enantiomers of CSA are imported from overseas while the price keeps on rising.Therefore,it is in priority to develop a process for synthesizing and isolating pure enantiomers of CSA from the sulfonation synthetic camphorAt present,the batch reactor is widely used in camphor sulfonation process,which is low efficiency and trivial for operating.To improve the efficiency of CSA synthesis process,a study was carried out to study the heat and mass transfer process of the oscillation reactor and the influence to the CSA synthesis process.Exciting outcomes are achieved that both reaction rate and yield of CSA are improved using oscillation reactors compard to the batch reactors.The solubility of D-CSA in a series organic solvents were measured under atmospheric pressure and the data were correlated carefully by Apelblat equation,?h equation,Wilson model and UNIQUAC model.In addition,the thermodynamic parameters,molar dissolution enthalpy and entropyof D-CSA,were calculated by Van't Hoff equation to explain its dissolving behavior in each solvent.Furthermore,DL-CSA in high level purity(99%)was obtained by recrystallization from acetic acid,which was guided by the solubility data above.The influences of the reaction time,molar ratio,solvents and volume on the yield and purity of pure enantiomers of CSA in the chiral resolution process were investigated as well in this study.To optimize the operating parameters and product quality,a partial equilibrium model was proposed in the thesis,which described the relationships among the reaction components in the precipitation process.