p-Bromobenzaldehyde was electrochemical synthesized via indirect oxidation of p-bromotoluene by Mn3+ generated from electrolysis of MnSO4 in H2SO4.The electrolytic oxidation conditions were optimized based on orthogonal experiments of L9(33).The optimized electrolytic oxidation conditions were determined as concentration of sulphuric acid of 6.5 mol/L,molar ratio of p-bromotoluene to Mn3+ 1∶4,electrolysis time of 6 h,synthetic time of 3 h,and temperature of 65 ℃.Under the optimized experiment conditions,the current efficiency and yield of p-bromobenzaldehyde could reach 75.36% and 75.47%,respectively.The present indirect electrosynthesis process is simple in terms of operational path,and the used medium can be recycled without pollution,showing potential application for green production.
Sodium alpha-sulfonated polyethylene glycol (400) stearate was synthesized by the reaction of stearic acid with polyethylene glycol using phosphoric acid and p-Toluene sulfonic acid as catalysts, following by sulfonation with chlorosulfonic acid and neutralization. Effects of single factors such as temperature, time, material ratio on the esterification ratios were investigated. On this basis, employing the orthogonal design, the optimum synthetic conditions were studied. Experiment results: Stearic acid and polyethylene glycol reacted for 4 hours at 140-150 degrees C with the mole ratio 2.5:1.0 with 2.0% catalyst to give the product in 83% yield. Chlorosulfonic acid and Stearate reacted for 1 hour at 60-70 degrees C with mole ratio 2.4:1.0 to give the product in 96% yield. Total yield was 79.7%. Gemini surfactants demonstrated good suspension ability and cooperative effect of mixed system. Compared to conventional surfactants, Gemini surfactants have prior performance attributed to few change in suspension ratios at high temperature and in rate of viscosity change in impact experiments.
In this micro-scale experiment, new neraether (β-naphthalene aether) was synthesized by the dehydration of hydroxybenzene and ethanol under p-methyl phenyl sulfonic acid catalyzing with the materials of β-naphthol and ethanol. The best reaction condition is that the mole ratio of β-naphthol, ethanol and catalyzer is 1∶4∶0.021,the reaction time is 5h ,the reaction temperature is 84℃ and then the product ratio of new neraether is up to 80% .The technology of synthesis have high catalytic activity, relatively mild reaction conditions and simple operation, and then provide reference for micro-scale experiment of fine chemical.