Continuous preparing technology for dimethyl dicarbonate

Abstract

The invention discloses a continuous preparing technology for dimethyl dicarbonate. The continuous preparing technology comprises the first step of material selection, the second step of caustic soda solution pumping and reacting, the third step of layering, the fourth step of extraction, the fifth step of neutralizing dissolving, the sixth step of distillation, the seventh step of rectifying and packaging and the eighth step of treatment standard reaching and discharging. In the first step, selected materials are organic solvent methylbenzene, a phase transfer catalyst and methylclhlorofonmate, and the charging molar ratio catalyst: methylbenzene: methylclhlorofonmate of the organic solvent methylbenzene to the phase transfer catalyst to the methylclhlorofonmate is 1:(50-150):(100-260). In the second step, the continuously-pumped 14%-20% caustic soda solution is subjected to the reaction at the constant temperature ranging from 0 DEG C to 20 DEG C under the situation of outer cooling. The continuous preparing technology is short in reaction time, low in cost, safe, environmentally friendly and suitable for continuous industrial production.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a continuous preparation process of dimethyl dicarbonate. Background technique [0002] Dimethyl dicarbonate is mainly used for cold sterilization of the following types of beverages: fruity beverages, high-energy beverages (with or without carbon dioxide), tea beverages (with or without carbon dioxide), fruit juice beverages (with or without carbon dioxide, fruit juices) content to 100%). [0003] 1. Dimethyl dicarbonate (also known as Vigoline), which has the chemical structure of the following formula, is a food additive for sterilizing beverages. [0004] [0005] American Journal of Organic Chemistry J.Org.Chem., 2000, 65 (24), 8224-8228 DOI: 10.1021 / jo000820u discloses a kind of synthetic method for preparing dimethyl dicarbonate, by triphosgene and methanol reagent The reaction forms phosgene, which is then substituted with methanol and condensed to obtain dime...

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Problems solved by technology

[0011] For the deficiencies in the above-mentioned prior art, the purpose of this invention is to provide a kind of continuous preparation process of dimethyl dicarbonate, it in the water-insoluble organic solvent, with phase-transfer catalyst, with methyl chloroformate and The lye is used as the raw material, and the reaction is carried out at 0-20°C under the condition of continuous feeding, and the organic phase after the reaction is continuously subjected to layering, extraction, toluene vacuum distillation, and product vacuum distillation to obtain the product dimethyl di carbonate

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