Method for synthesizing nitramine azide through phase-transfer catalysis

A technology of phase transfer catalyst and synthesis method, which is applied in the field of energetic material synthesis, can solve problems such as environmental pollution, restrictions on large-scale production and popularization of DIANP, difficulties in recycling and processing DMSO aqueous solution, etc., and achieve good large-scale production effects

Pending Publication Date: 2021-10-29
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This post-processing method will produce a large amount of DMSO aqueous solution, which is very difficult to recover and treat DMSO aqueous solution, which will cause serious environmental pollution and limit the large-scale production and application of DIANP.

Method used

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  • Method for synthesizing nitramine azide through phase-transfer catalysis
  • Method for synthesizing nitramine azide through phase-transfer catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 2 g of Gena to a 250 mL flask, followed by 50 mL of CH 2 Cl 2 ; 1.19 g NaN 3 Add 50 mL of water and stir to dissolve, pour it into a flask together, and finally add 0.4 g of tetrabutylammonium bromide, and stir vigorously at room temperature for 6 h. After the reaction is finished, use a separatory funnel to separate the liquid. The lower liquid is the methylene chloride phase, the upper liquid is the water phase, and the tetrabutylammonium bromide in the water phase can be recycled. The lower layer liquid was dried with anhydrous sodium sulfate, rotary evaporated at 40 °C, and separated by column chromatography to obtain DIANP with a purity of 98.2% (HPLC, the same below).

Embodiment 2

[0024] Add 4 g of Gena to a 250 mL flask, followed by 50 mL of CH 2 Cl 2 ; 2.38 g NaN 3 Add 50 mL of water and stir to dissolve, pour it into a flask together, and finally add 0.35 g of tetraethylammonium bromide, pass it through a condensing reflux device at 40 °C, and stir vigorously for 10 h. After the reaction was completed, the liquid was separated with a separatory funnel, and the lower liquid was dried with anhydrous sodium sulfate, rotary evaporated at 40 °C, and separated by column chromatography to obtain DIANP with a purity of 98.7%.

Embodiment 3

[0026] Add 6 g of Gena to a 250 mL flask, followed by 50 mL of CHCl 3 ; 3.6 g NaN 3 Add 50 mL of water and stir to dissolve, pour them into the flask together, and finally add 0.57 g of benzyltriethylammonium bromide, at 60°C, pass through the condensing reflux device, and stir vigorously for 12 h. After the reaction, use a separatory funnel to separate the liquid, the lower layer is the chloroform phase, the upper layer is the water phase, and DIANP is dissolved in chloroform. The lower layer was dried with anhydrous sodium sulfate, concentrated by rotary evaporation at 40 °C, and separated by column chromatography to obtain DIANP with a purity of 99.6%.

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Abstract

The invention discloses a method for synthesizing nitramine azide through phase-transfer catalysis. According to the compound, 1, 5-dinitrate group-3-nitro-3-azapentane and sodium azide are used as raw materials, and in the presence of a phase transfer catalyst, an azidation reaction is carried out in an organic solvent-water two-phase system to synthesize DIANP. According to the method, DMSO (dimethylsulfoxide) and other organic solvents which are difficult to treat are avoided, the method is green and environment-friendly, the synthetic route is simple and feasible, and the product is simple to separate.

Description

technical field [0001] The invention relates to a method for synthesizing azide nitramine, which belongs to the field of synthesizing energetic materials. Background technique [0002] 1,5-diazido-3-nitro-3-azopentane or azidonitroamine (DIANP), as an azide energetic plasticizer, has high energy, high burning rate, low burning temperature, gas With the advantages of small molecular weight and large gas production capacity, it can be used in high-energy and low-ablation propellants, propellants, pyrotechnic agents and gas generating agents. It is a new type of energetic plasticizer with great application prospects. Azide nitramine has good compatibility with commonly used components of propellants, especially digested cellulose. When it is used in high-energy and low-ablation propellants, the detonation temperature is 200-400 K lower than that of propellants with the same energy level, and the propellant power can reach 1300 J / g, used in conjunction with RDX, its propellant ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C247/04
CPCC07C247/04
Inventor 蔡春肖凯
Owner NANJING UNIV OF SCI & TECH
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