Study On Synthesis Of Double-chain Esterquat

Esterquats are favored to many advanced countries because of its biodegradation and softening property.Technics conditions of esterification reaction were optimized through Single factor experiment and orthogonal experiment,so the ideal reaction conditions are the reaction temperature170℃,the reaction time4h/2h,the molar ratio1:3:0.8(MDEA:stearic acid:TEA), catalyst 0.5%wt(the total weight of the stearic acid,MDEA and TEA).Using the mixture of V(chloroform):V(methanol)=25:1 as mobile phase,the Rf value of triesteramine, diesteramine,and monoesteramine are 0.60,0.47 and 0.38 respectively.The three factions isolated by column chromatography were qualitatively detected and verified by high performance liquid chromatography,infrared spectrum and mass spectrometry.The results indicated that the three fractions were triesteramine,diesteramine and monoesteramine. Besides this,the percentage of the three factions were 93.26%,94.39% and 92.85% respectively.Comparisons were made between the mass percentage obtained by column chromatography and high performance liquid chromatography which indicates that their results were cosistent.In quaternized response,we investigated the reaction conditions about epichlorohydrin diethyl sulfate which as a quaternary ammonium reagent respectively with the ester amine.The results indicate that epichlorohydrin can occur chemical reaction with ester quaternary ammonium amine,but because of epoxy ring and long chains of ester amine, the large steric effect requires a higher reaction conditions. When the reaction temperature is high, one hand ester amine is easy to be carbonized, and the other hand the epoxy ring may be cracked, so epichlorohydrin is not suitable as a quaternary ester amine reagent. Diethyl sulfate can also occur chemical reaction with ester quaternary ammonium amine, but its reaction conditions is higher than dimethyl sulfate as a quaternary ammonium reagent,and we have not yet find a suitable solvent or catalyst at present,so that resulting a low volume product.