Synthesis method and equipment of alkyl nitrite

Abstract

The invention discloses a synthesis method and equipment of alkyl nitrite. The method mainly includes the following points that: a) the alkyl nitrite regeneration raw materials are the NO in the tail gas generated in production of oxalic acid alkyl ester by coupling reaction of CO and alkyl nitrite, and O2, alkyl alcohol and other raw materials supplemented from the outside; b) the tail gas of the coupling reaction in step a) mainly are unreacted CO, alkyl nitrite, and the NO gas generated by alkyl nitrite decomposition in reaction, O2 is introduced to oxidize most of NO into N2O3; c) the gas mixture in step b) and alkyl alcohol are subjected to esterification regeneration reaction to obtain alkyl nitrite; and d) the by-product nitric acid is inevitably produced in step c), and is also applied to the regeneration process of alkyl nitrite to re-react with the synthesis tail gas so as to generate alkyl nitrite, thus realizing atom economy. The invention also provides equipment for carrying out the reaction. The equipment is composed of three sets of small towers in series connection, i.e. (1) a full mixing tower; (2) an esterification tower; and (3) a nitric acid treatment tower. The method and the equipment provided by the invention have the advantages of mild operation conditions, high regeneration efficiency, good adaptability, strong economical efficiency and the like.

Description

technical field [0001] The invention relates to a method for preparing alkyl nitrite by using tail gas produced by coupling reaction of CO and alkyl nitrite to prepare alkyl oxalate as raw material and reaction equipment thereof. Background technique [0002] Alkyl nitrite is traditionally used as chemical additives, such as: motor oil additives, unsaturated organic compound stabilizers, antispasmodics, etc. Synthetic intermediate use. In recent years, the technology of preparing ethylene glycol from coal-based syngas has attracted widespread attention in my country, and at the same time, the application of alkyl nitrite has been further extended to the field of coal chemical industry. The process is mainly divided into coupling reaction, regeneration reaction and hydrogenation reaction. Among them, alkyl nitrite, as one of the main raw materials of the coupling reaction, plays an important role in both the coupling reaction and the regeneration reaction, especially the re...

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Problems solved by technology

[0009] In recent years, with the upsurge of coal chemical industry and the success of coal-to-ethylene glycol industrialization, a large number of research reports on coal-to-ethylene glycol have emerged, and there have also been a large number of literature reports on synthetic reaction systems. The researchers Most of them focus on the first step of the coupling reaction and the catalysts used and the reaction mechanism. Researchers have made a lot of reports on this aspect, but there are relatively few research reports on the second step of the regeneration reaction. In this regard, East China University of Science and Technology, Tianjin University and other universities have carried out relevant research. Shanghai Pujing Engineering Technology Co., Ltd. and East China University of Science and Technology have cooperated to report the preparation method and equipment of dinitrogen trioxide in the patent CN101885479A, which discloses a kind of nitrous acid A method for preparing dinitrogen trioxide as a raw material for alkyl esters, and equipment used to implement the above-mentioned preparation method is provided

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