Laboratory optimization of process variables in reductive ozonolysis of methyl soyate

Abstract

AbstractThe laboratory experiments for reductive ozonolysis of methyl soyate were divided into four statistically designed groups, according to ozonolysis medium (methanol or water) and ozone carrier gas (oxygen or air). Each group comprised 27 separate experiments, each a one‐third replicate of a 34 factorial. Significant independent variables were determined by a preliminary set of experiments. Besides ozonolysis medium (X) and carrier gas (Y), the following significant independent variables were studied: medium/ester ratio (A), reduction catalyst (B), reduction pressure by hydrogen (C), and reduction temperature (D).By gas‐liquid partition chromatography of the dimethyl acetals of the two products, which included methyl azelaaldehydate (MAZDA) and pelargonic aldehyde (PDA), aldehyde yields were determined for each experiment in the statistical groups.Analysis of variance of the data (F‐test) showed the following main effects and interactions for yield of MAZDA where oxygen carrier gas, water as the ozonolysis medium, and palladium‐on‐carbon catalyst were used for reduction: Y, YA, YB, YD, AD, BD, and AC. Data fit (regression analysis) provided regression equations. Computer solution of these equations indicated optimum process levels. Based on these optimum levels, the predicted over‐all yield of MAZDA is 89% of theoretical.