Centrifugal extraction separation method and separation device in preparation process of nitro-azide compounds

Abstract

The invention relates to a centrifugal extraction separation method and a separation device in a preparation process of nitro-azide compounds in a formula of explosives and powders. The method comprises the following steps: collecting a reaction solution of a desalting unit after an azidation reaction of a nitro-azide compound to obtain a mixed solution containing the nitro-azide compound, dichloromethane, a reaction solvent and a small amount of sodium salt; performing four-stage centrifugal extraction on the mixed solution, injecting fresh water into a light-phase inlet of a third-stage centrifugal extraction machine through a peristaltic pump, and returning separated wastewater flowing out of light-phase outlets of the third-stage centrifugal extraction machine and the second-stage centrifugal extraction machine to a previous-stage centrifugal extraction system to form a countercurrent series circulating washing process; and carrying out fourth-stage centrifugal extraction, adding alkali liquor, and carrying out alkali washing separation, so as to obtain a product mixed solution of the nitryl azide and dichloromethane. The invention further provides a centrifugal extraction separation device, and internal components of a centrifugal extraction machine are optimized and improved.

Description

technical field [0001] The invention specifically relates to a centrifugal extraction and separation method and a separation device in the preparation process of a novel azide energetic material of a propellant formula - nitro azide compound. It belongs to the application field of chemical separation. Background technique [0002] Nitroazide compounds such as 1,5-diazido-3-nitro-3-azopentane (DIANP), 2-azidoethylbutynitroamine (BuAENE), 3-azido-1 , 3-dinitroazetidine (AzDNAZ), 3-nitro-5-azido-3-azopentyl nitrate (PNAN), etc., are a new type of liquid azides with great application prospects. The nitriding reaction product has the advantages of high energy, high burning rate, low burning temperature, small relative molecular weight of gas, and large gas production. It can be used in the development of propellant formulations and propellants. The synthesis process of this type of compound usually includes azidation, extraction, washing, decolorization, filtration and vacuum d...

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Problems solved by technology

[0005] The invention provides a novel centrifugal extraction separation method and separation device in the preparation process of nitroazide compounds, thereby solving some problems existing in the existing production process

[0006] The technical problems to be solved by the present invention are: (1) problems such as intermittent operation, low mass transfer efficiency, and long standing time in the extraction and washing process after the azidation reaction in the original production process have seriously affected the production of nitroazide compounds. Preparation quality and production efficiency, at the same time, due to the instability of energetic materials caused by multi-phase long-term mixing, the production equipment brings safety hazards; (2) As the core equipment of this separation method, a general-purpose centrifugal extractor is used for extraction and separation , because the two-phase density difference between the liquid to be extracted (continuous phase) and the extractant (dispersed phase) in most heterogeneous systems is small, the particle size distribution is uneven, and the circumferential shear force of the original drum design structure The impact is small, resulting in serious emulsification of the liquid to be extracted and the extractant after mixing in the annulus area, which affects the separation efficiency in the drum

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