Research Of Glycidyl Butyrate:Synthesis, Bioresolution, VLE And Liquid-solid Reaction Kinetic

Glycidyl butyrate is a very important pharmaceuticals compound. It is applied in many field and it is necessary research the new method and the technology of the synthesis.This paper studied the new the method, with tetrabutyl ammonium bromide (TBAB) as phase transfer catalyst synthesised glycidyl butyrate with epichlorohydrin and sodium butyrate. And studied the synthesised factor of the sodium butyrate3h, the synthesised factor of glycidyl butyrate was1:7mole,110℃and4.5h。Using quick analysis of gas chromatography ditect glycidyl butyrate of epichlorohydrin reaction system. The SE-30(Φ3x1.5mm) column was used,3μL inlet with the gas flate of48.86mL/min.The column temperature was at100℃and185℃of the gas room and185℃of the thermal conductivity detector.The good linear relationship between the peak area and the quantity of the glycidyl butyrate (R2=0.9993,n=6) with the regression equation y=1.5578x106χ+1.3805x103and minimum detection limit (S/N=3) is0.1778mg/ml with the precision0.19%and the accuracy0.014%and the recovery99.3%in average.The vapour-liquid equilibria (VLE) date for the binary system of glycidyl butyrate (1) and epichlorohydrin (2) was studied at100,88.66and56kPa. An azeotropic behavior has not been found in this work. The activity coefficients were obtained by the nonlinear least squares method based on minimization from the equilibrium data. Average relative deviations between calculated values and the experimental data of temperature are all lower than0.99%for the three models at the three different pressures investigated. The root mean square deviations (RMSD) of gas phase compositions y1and tempertures are all lower than0.0099and1.1K for100kPa,0.0094and4.5K for88.66kPa and0.0095and3.7K for56kPa. Thermodynamic consistency of the calculated data are checked by the Herrington method. The experimental VLE data are compared with the correlated values obtained by means of the NRTL, UNIQUAC and Wilson models. Isobaric (vapour+liquid) equilibrium experiments have been reported for the binary mixtures of glycidyl butyrate (1)+acetone (2), glycidyl butyrate (1)+carbon tetrachloride (2) and glycidyl butyrate (1)+chloroform (2) at100kPa. The thermodynamic consistency of the correlation were checked using Herrington’s area test. The experimental correlated satisfactory by means of the Wilson, NRTL and UNIQUAC models.This paper described the catalytic fluid-solid reaction of epichlorohydrin and sodium butyrate with tetrabutyl ammonium bromide (TBAB) as phase transfer catalyst. The shrinking core model was applied. The analysis of the reaction based on the kinetic model showed a reaction-controlled regime at temperature varying from90to100℃. The exterior diffusivity was removed between300r/min and400r/min.The internal diffusivity was removed when the particle size was2x10-4m. Reaction rate constants were calculated at the different temperature.Two mixed strains of microorganism capable of optically resolving racemic glycidyl butyrate has been isolated from soil and identified to be Alkaline lipase, which one strain of lipase has no ideal result from tens of lipase. The suitable carbon source of the condition was starch and the nitrogen source was beaf extract. The fitted temperature and initial pH for enzme formation were30℃and pH=8.0,respectively. Rotating rate was200r/min.Under2days fementation, it can get1.5U/mL. The technology of the two Alkaline lipase in the optical resolution of glycidyl butyrate were studied. The condition was pH=6.0,28℃,200r/min,0.50g substrate added in the Alkaline lipase liquid,when the glycidyl butyrate was transformed83.2%, the optical purity of (R)-glycidyl butyrate was92.8%ee(enantiomeric excess).