Process Synthesis Glycol Ether Carboxylate

Binary alcohol ether carboxylic acid esters compound molecule contains different alkyl(-CnH2n+1), further contains a carbonyl group(>C=O), ester(-COO-), ether bond(-COC-),such as different functional group,therefore, is a kind of multifunctional compound of solven that both can dissolve alkyl compounds and can dissolve carbonyl class, esters, ethers. Since the molecular weight of binary alcohol ether carboxylic acid esters compound molecule is greater than the corresponding units of alcohol, so it is a high-boiling solvent; meanwhile it contained more than the corresponding unit of alcohol contained in the functional group, so it is solvents with more functional groups. With high boiling point and more functional groups,therefore binary alcohol ether carboxylic acid esters compound has the general performance that the organic solvent does not have.This thesis mainly take direct esterification method as the research method. Paper first chapter for the review, the main development trends at home and abroad are briefly discussed and the main kinds of catalysts are introduced, meanwhile points out the basic research ideas and innovations. The second chapter is the main equipment, reagents and reaction apparatus sketch medicines required for the experiment instruments. The third chapter is based on homogeneous catalysis, by single factor experiment and orthogonal test to determine the p-toluene sulfonic acid as catalyst for synthesis of ethylene glycol butyl ether acetate catalyzed with best reaction process conditions, and has carried on the analysis of the kinetics and thermodynamics. The fourth chapter introduces the preparation of new solid acid catalyst by impregnation, the active component p-toluene sulfonic acid is loaded on the pumice carrier, so as to solve the problem that the active component can not be reused for p-toluene sulfonic acid,catalyst reused after five times still has high activity. The fifth chapter put HSiW acid in the heteropoly acid as catalyst for catalytic synthesis of ethylene glycol butyl ether acetate.Homogeneous reaction optimum conditions are as follows: the molar ratio of reactant glycol butyl ether and ice acetic acid is 1:1.3, dosage of p-toluene sulfonic acid as catalyst is2.5% more than the doseage of ethylene glycol butyl ether and ice acetic acid as reactant,the dosage of cyclohexane as water-carrying agent is 30 ml, the reaction time need 70 min.Heterogeneous reaction optimum conditions are as follows: the dosage of cyclohexane as water-carrying agent is 25 ml, the molar ratio of reactant glycol butyl ether and ice acetic acid is 1:1.3, the dosage of load type catalyst is 4g, reaction time is130 min. False liquid phase reaction optimum conditions is as follow: the dosage of cyclohexane as water-carrying agent is30 ml, the molar ratio of reactant glycol butyl ether and ice acetic acid is 1:1.4, the dosage of HSiW acid as catalyst is 2% more than the quality of reactant ethylene glycol butyl ether and glacial acetic acid, the reaction time is 60 min.Homogeneous reaction kinetics linear equation is Y=-0.975+0.0935 X, Thermodynamics linear equation is Y=-6.43421X+15.24682, Reaction apparent activation energy is Ea=53.49 KJ mol-1. Heterogeneous reaction kinetics linear equation is Y=0.03807X+0.08.Thermodynamics linear equation is Y=9.09211+21.67199 X, the apparent activation energy is Ea=75.59KJ·mol-1. False liquid phase reaction kinetics linear equation is Y=0.06248X+0.5332,thermodynamic linear equation is Y=-4.98649X+10.94946, The apparent activation energy of the reaction obtained Ea=41.45KJ·mol-1. Apparent activation energy of false liquid phase reaction is less than homogeneous reaction activation energy and is less than the heterogeneous reaction activation energy. The smaller the activation energy, the more activated molecules, the reaction is faster.The product ethylene glycol butyl ether acetate has been analyzed in test and its purity is over 99% through gas chromatography test. The boiling point is 192℃, the density is0.942g/cm3, the refractive index is between 1.4000~1.4200, it has the same physical and chemical properties as pure glycol butyl ether acetate basically.