2589-57-3Relevant articles and documents
Method for continuously preparing dimethyl azodiisobutyrate by using micro-channel reactor
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Paragraph 0031-0037, (2020/11/23)
The invention discloses a method for continuously preparing dimethyl azodiisobutyrate by using a micro-channel reactor, which comprises the following steps: 1, heating butyronitrile, and dissolving the butyronitrile in a benzene solvent to obtain a mixed solution with the mass concentration of butyronitrile of 5-30%; inputting the mixed solution and methanol into a first mixing zone of a micro-channel reactor for mixing to obtain a first mixed material; 2, mixing the mixed material and hydrogen chloride gas in a second mixing zone of a micro-channel reactor, and introducing the mixture into the micro-channel reactor for primary reaction; and 3, mixing the reaction solution after the heat preservation reaction with water, introducing the mixture into a micro-channel reactor, carrying out asecondary reaction, standing, performing centrifuging to obtain a crude product of dimethyl azobisisobutyrate after the reaction is finished, and performing recrystallizing to obtain dimethyl azobisisobutyrate. According to the method, the reaction rate and the raw material utilization rate are increased, the batch quality difference caused by reaction temperature fluctuation is avoided, the reaction is easy to control, the production period is short, and the total yield can reach 75% or above.
2,2'-azo(2-methyl-N-(2-hydroxyethyl)propionamide) preparation method
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Paragraph 0014; 0032-0060, (2019/10/04)
The invention discloses a 2,2'-azo(2-methyl-N-(2-hydroxyethyl)propionamide) preparation method, which comprises: adding 2,2'-azobisisobutyronitrile, methanol and toluene to a reactor having a stirring and reflux device, starting stirring, slowly introducing hydrogen chloride gas under cooling, and controlling the temperature of the material and carrying out a thermal insulation reaction; after completing the reaction, adding the reaction liquid into water in a dropwise manner, carrying out a hydrolysis reaction, layering after completing the hydrolysis, adding a small amount of methanol to the organic phase, and carrying out pressure reducing distillation for a certain time; after completing the distillation, slowly adding the organic phase into a mixed solution of sodium methoxide and monoethanolamine in a dropwise manner, and carrying out thermal insulation; after completing the thermal insulation, carrying out solid-liquid separation by a centrifuge, continuously washing the solid with water, crystallizing, carrying out centrifugation until the material is dried, placing the material in a drying device, and drying; and after the drying, cooling the material to a normal temperature to obtain the 2,2'-azo(2-methyl-N-(2-hydroxyethyl)propionamide) product, wherein the product content (HPLC) is more than 98%, and the yield is 55-75%.
METHOD FOR PRODUCING AZO COMPOUNDS
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Paragraph 0048; 0062, (2018/05/03)
PROBLEM TO BE SOLVED: To provide a method that can produce azo compounds at good yields by making oxygen or an oxygen-containing gas act on hydrazo groups of hydrazo compounds when oxidatively dehydrogenating them. SOLUTION: Azo compounds are produced by making oxygen or an oxygen-containing gas act on hydrazo compounds in the presence of vanadium or cerium compounds, and a solvent. SELECTED DRAWING: None COPYRIGHT: (C)2018,JPOandINPIT