The Preparation, Purification Of Glycol Glucoside And Glycol Glucoside Caproate

The preparation, separation of glycol glucosides, the biological synthesis of glycol glucoside caproate, and the analysis of the configuration and character of glycol glucoside caproate were studied in this paper. The main contents are as follow:Glucose heated with ethylene glycol in the presence of an acid catalyst and forms a mixture of glycol glucoseds. In the process of synthesis glycol glucosides, the quantity of the glycol is superfluous, so it need to get rid of all the glycol from glycol glucosides. In the study, the mothod of molecular distillation was used to remove the excess glycol in the products, and had a comparison with the methods of solvent extraction and vacuum distillation. Experimental results showed that the method of molecular distillation was most effective when the conditions were as follows: feed flow rate 80～100mL/h,feed temperature 80℃, wiper rolling speed 200r/min, condensation temperature 25℃, evaporation temperature150℃and evaporation pressure 200Pa. Under this conditions, the residual glycol content can reduce to 1% and even less. So it enlarges the applications of the glycol glucoside.Glycol glucoside caproate were synthesized by glycol glucosides and caproic acid as reaction materials, Novozyme435 lipase as catalyst. The effect of solvent, concentration of glycol glucosedes and caproic acid, the quantity of lipase, reaction temperature, reaction time on the conversion of caproic acid were studied. The optium conditions were as follows: in the solvent of hexane, glycol glucosides 0.3 mol/L ,caproic acid 1.8 mol/L, enzyme concentration 80mg/mL, reaction tempreture 70℃, reaction time 24h, and the conversion of caproic acid 23.74% was obtained.The separation of esterification products were finished by the methods of solvent extraction and silica gel chromatography. The glycol glucoside caproic acid monoester was eluted by chloroform:methanol(v:v is 8:1) in the water phase and the glycol glucoside caproic acid diester was eluted by chloroform:methanol(v:v is 8:1) in the chloroform phase. The configurations of the products were identified by TLC, HPLC and MS.The character of the glycol glucoside caproate, the glycol glucoside caproic acid monoester and the glycol glucoside caproic acid diester were studied. The results showed that they have good emulsification by test the emulsification and the HLB value.