Prepare For Polyglycerol Middle Carbon Chain Fatty Acid Ester

In this paper, I use camphor tree seed oil as experimental materials, to prepare polyglycerol middle carbon chain fatty acid ester. In this paper, the method of preparing this kind of ester can divide into two parts, first step is to make polyglycerol; secondly, using polyglycerol and middle carbon chain fatty acid together to make esterification, and finally, make the polyglycerol middle carbon chain fatty acid ester. In this paper, I use solid base catalysts catalyze the esterification, and I mainly study the technological parameter of making solid base catalysts, and the optimization of reaction condition of esterification.In this paper, when I papered the polyglycerol, I use the homogenous catalyst (ratio of quality 5% NaOH) to catalytic polymerization of polyglycerol. Choose the reaction condition as follows:temperature 260℃,when the color of reaction system turn to light brown, it is the time to stop the reaction, it is about 3.5h.The produce is light, no pungent smell. After I determined the hydroxyl value and count its degree of polymerization is 5.6, after MS analysis, there are mainly linear chain polyglycerol, little ringlike polyglycerol, and the degree of polymerization mainly contain 2-9. The quality of the product is good.In this paper, I use immersion method to make the solid base catalysts. Fistly,choose the same preparation conditions (specific of active constituent and carrier 1:4, bakery temperature 600℃, bakery time 6h) to prepare four different kinds of solid base catalysts (KOH/MgO,NaOH/MgO,KOH/Al2O3,NaOH/Al2O3), choose the esterification rate as reference index; secondly, screen the best solid base catalysts. The result of experiments show that the best catalytic effect is KOH/Al2O3,and its esterification rate is 78.28%. And then, determine the scope of strength of alkalis of the four kind of solid base catalysts, the result of experiments show that the most strong catalyst is KOH/Al2O3, NaOH/Al2O3,KOH/MgO,NaOH/MgO is ordinal abate.Choose KOH/Al2O3 as goal catalyst,and optimize the preparing conditions. Using the single factor analysis to analyse to the effect of specific of active constituent and carrier,bakery temperature,bakery time. The result of experiments show that the bakery time is longer,the esterification rate is up first and then steady, the best time is 6.5h, and the esterification rate is 82.32%; the bakery temperature is higher, the esterification rate is up first and then sharp decline, the best temperature is 650℃,and the esterification rate is 83.65%;specific of active constituent and carrier is higher, the esterification rate is up first and then steady,the best ratio is 4:10,and the esterification rate is 82.88%. At the base of single factor analysis,I make the response surface analysis to optimize the preparing conditions, devise 17 experiments of 3 factors and 3 levels, and the result of experiments show that,when the ratio is 0.5, bakery temperature is 645.32℃, bakery time is 6.63h, the esterification rate is 83.96%, it is very similar with number of analog computer 84.64%. After then, I analyse the best solid base catalysts in IR, and there is the especial absorption peak of KAlO2, it shows there are active centres in the solid base catalysts.In this paper, I choose the direct esterifiable method to paper the polyglycerol middle carbon chain fatty acid ester. Using the single factor analysis to analyse to the effect of the ratio of polyglycerol and middle carbon chain fatty acid, the dosage of catalysts time,temperate. The result of experiments show that the four factors is higher, the esterification rate is up first and then down, and the best parameter values separately is 70:40,5%,2.5h,220℃, and the esterification rate separately is 88.41%,89.74%,88.37%,92.58%. At the base of single factor analysis,I make the response surface analysis to optimize the preparing conditions, devise 29 experiments of 4 factors and 3 levels, the result of experiments show that when the ratio of polyglycerol and middle carbon chain fatty acid is 1.77, the dosage of catalyst is 5.05%, time is 2.45h,temperate is 219.44℃, the esterification rate is 91.89%, it is very similar with number of analog computer 92.778%. After then, I analyse the product in IR, and there is the especial absorption peak of ester group, it shows the product is polyglycerol middle carbon chain fatty acid ester.