Chromatographic Reactors:  Esterification of Glycerol with Acetic Acid Using Acidic Polymeric Resins

Abstract

Reactive chromatography is an attractive method for chemical synthesis because chemical reactions and product separation occur simultaneously in the same unit. In this work, the synthesis of triacetine, starting from glycerol and acetic acid, using reactive chromatography on acidic polymeric resins is investigated. The study proceeds first to the characterization of the adsorption equilibria of the involved multicomponent mixtures and then to the study of the kinetics of the relevant reactions using a batch reactor. Next, the separation−reaction process is investigated using a fixed-bed chromatographic column. The obtained data are compared with the predictions of a mathematical model, whose kinetic and equilibrium parameters were estimated from the batch experiments mentioned above. It is shown that, although this synthesis requires three steps in series, the chromatographic reactor can produce high-purity (i.e., food-grade) triacetine with high conversions. It is found that the presence of water in the resin at the end of the regeneration step has a strongly detrimental effect on the final triacetine purity.

Continuous Process of Reactive Distillation to Produce Bio-additive Triacetin From Glycerol

“…Traditionally, the reaction of glycerol and acetic acid is carried out using homogeneous catalysts, such as sulphuric acid (Gelosa et al, 2003;Mufrodi et al, 2010;Mufrodi et al, 2012) and acidic functional ionic liquid (Li et al, 2009), H 3 PO 4 , HCl, HNO 3 and H 2 SO 4 (Khayoon & Hameed, 2011). This process has advantages including high activity (complete conversion within short time) and mild reaction conditions (from 100 to 120 °C and atmospheric pressure).…”

Co-production of butyrate methyl ester and triacetylglycerol from tributyrin and methyl acetate

“…As a matter of fact the partially acetylated intermediates (MAG and DAG) tend to accumulate to some extent. This is not surprising because, as observed in the case of the esterification of glycerol with acetic acid, the reaction between the third acyl group and the di-acetyl glycerine has an equilibrium constant significantly lower than the first acylation step [7,17].…”

“…The direct esterification with organic acids (such as acetic acid) in the presence of acid catalysts (including sulphonic resin and zeolites) is one of the most used methodologies [7,8]. All these approaches are based on the availability of pure glycerol, which has to be independently isolated and purified from the FAME synthesis, a step that, actually, is a common side route of FAME industrial production.…”

Oxygenated Glycerol Derivatives as an Alternative Source of Energy: A Review

“…According to Gelosa (2003), conversion efficiency is widely influenced by the reaction mechanism and the equilibrium parameters, being strongly unfavorable to the dehydration of acetic acid 45 :…”

“…The reactor permitted to obtain high conversion rates of glycerol and high purity of the products 45 . Later, Mota et al (2008) 46 evaluated the performance of glycerol acetylation using different solid acid catalysts, whom proposed the kinetic mechanism for glycerol into mono-, di-and triacetin.…”