Research On Phase Transfer Catalyzed Synthesis Of The New Food Preservative Dmdc

The spoiling of food will lead to great economic loss, accede to food preservative is a common mean to solve this problem. Although this may achieve their goals, at the same time they caused food contamination, and some food additives even have very strong side effects on the human body. With the importance of healthy, people pay more and more attention to the safe and efficient preservatives.New preservative dimethyl dicarbonate (DMDC) is a safe, efficient and easy to use preservative, which have attracted much attention. But so far there have been no report about the synthesis of DMDC in the home. A series of explorations of the synthesis of DMDC were carried on in this paper, aiming at identifying the best synthetic process.In this paper, we study the phase transfer catalysis and put forward a new synthetic method, we use phase transfer catalyst synthesis of DMDC. With the inorganic alkali and the presence of phase transfer catalyst, nine synthetic conditions were studied: reaction time, solvent, temperature, inorganic alkali, catalyst, amount of catalyst, amount of Methyl chloroformate, amount of solvents. At the optimum conditions, the reaction time is 40-60min, the best solvent is toluene, reaction temperature is 15℃, sodium hydroxide is the best inorganic alkali, Tridodecyl methyl ammonium chloride is the best catalyst, ratio of n(Tridodecyl methyl ammonium chloride): n(Methyl chloroformate)is 0.0022: 1, molar ratio of n(Methyl chloroformate): n(sodium hydroxide)is 1:1, mass ratio of and m(water):m(toluene)is 3:1, The Mass yield of DMDC is about30%.According to the latest data provided by the United States patent, we found that this process show a very low yield of DMDC and unable to repeat the test of the patent, there is still a considerable difference.In this paper, the optimal conditions show a higher mass yield than this patent and better repeatability.After the whole reaction the experiment data was studied, we put forward a new synthesis method:nonaqueous phase transfer catalytic synthesis of DMDC. Use Tridodecyl methyl ammonium chloride as catalyst, methyl chloroformate and sodium hydroxide as raw material, reaction temperature is 15℃, reaction time is 40min, The Mass yield of DMDC is about 10%. Such nonaqueous phase transfer catalysis of DMDC will be more favorable, and simplifying the treatment process, preliminary experiment shows a lot of feasibility, which worth further study.