Method for synthesizing O-methyl-N-nitroisourea by microchannel reactor

Abstract

The invention relates to the technical field of fine chemical engineering, and provides a method for synthesizing O-methyl-N-nitroisourea by a micro-channel reactor, which comprises the following specific steps: adding nitric acid into a four-neck bottle for cooling, dropwise adding fuming sulfuric acid, controlling the temperature of a mixed solution, adding sulfuric acid into the four-neck bottle, and reacting for 2-4 hours; stirring and a low-temperature constant-temperature reaction bath are started to cool sulfuric acid, disulfate is put into a four-opening bottle to prepare a disulfate sulfuric acid solution, a mixed acid metering pump is started, a disulfate sulfuric acid solution metering pump is started, the disulfate sulfuric acid solution is mixed and enters a nitration micro-channel reaction device, and after heat preservation of nitration liquid is completed, the nitration liquid is dropwise added till the temperature is lowered to 0 DEG C in advance; the preparation method comprises the following steps: adding water into a reaction kettle, dropwise adding while stirring, continuously cooling and preserving heat after dropwise adding, carrying out suction filtration on eluted feed liquid, and washing a filter cake with chilled water to obtain an O-methyl-N-nitroisourea wet product, so that the defects of long production period, low effective productivity, lower safety coefficient and relatively higher safety risk of a traditional method for synthesizing O-methyl-N-nitroisourea are overcome.

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