Method for synthesizing TNAD through catalytic nitration by using ionic liquid

An ionic liquid and catalyst technology, applied in the field of synthesizing TNAD, can solve the problems of potential safety hazard, increase production cost, and high reaction temperature, and achieve the effects of less equipment corrosion, increased safety, and simple reaction operation.

Active Publication Date: 2015-02-11
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method has only one-step reaction, it consumes a large amount of acetic anhydride, which increases the production cost, and the reaction temperature is relatively high, which has potential safety hazards

Method used

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  • Method for synthesizing TNAD through catalytic nitration by using ionic liquid
  • Method for synthesizing TNAD through catalytic nitration by using ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Under ice bath, add 30mmol N to the four-neck flask 2 o 5 And 30ml of dichloromethane solvent, add 5mmol of dipiperazine in batches, control the temperature not to exceed 5°C, after the addition, raise the temperature to 25°C for 60min, after the reaction, pour the mixture into 50g of ice water, there is a white solid Precipitated, washed with water, 5% NaHCO 3 washing, washing with water until neutral, and drying to obtain TNAD with a yield of 77.6%.

Embodiment 2

[0030] The process was the same as in Example 1, but the reaction time was changed to 30 min to obtain TNAD with a yield of 48.2%.

Embodiment 3

[0032] The process was the same as in Example 1, but the reaction time was changed to 70 min to obtain TNAD with a yield of 77.8%.

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Abstract

The invention discloses a method for synthesizing TNAD (trans-1,4,5,8-tetranitro-1,4,5,8-tetraazadecalin) through catalytic nitration by using an ionic liquid. According to the method, N2O5 is taken as a nitration agent, an inertia organic liquid is taken as a solvent, the ionic liquid is taken as a catalyst, and decahydro-pyrazino[2,3-b]pyrazine is directly nitrated, so that high-purity TNAD is prepared. Compared with the prior art, the method has the advantages of mild reaction conditions, operation easiness, high purity, good safety, low cost and the like.

Description

technical field [0001] The invention relates to a method for preparing explosives, in particular to a method for synthesizing TNAD by using dinitrogen pentoxide as a nitrating agent and catalyzing an ionic liquid. Background technique [0002] Nitrogen heterocyclic compounds play an important role in the field of energetic materials. The synthesis of nitrogen heterocyclic ammonium nitrate provides new materials for the development of new nitrogen heterocyclic explosives, plasticizers and energetic additives. As a component of mixed explosives and propellants, tetranitrodipiperazine (TNAD) is an ideal new material, its energy is equivalent to RDX, and its stability is better than RDX. As a component of composite propellants, it is not Crystallization will occur, which can effectively improve the performance of the ammonium nitrate propellant. Therefore, the synthesis of tetranitrodipiperazine has attracted the attention of foreign scholars. [0003] In the early 1980s, Wil...

Claims

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Application Information

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IPC IPC(8): C07D487/04
CPCC07D487/04
Inventor 李斌栋曹晓峰王敏常婷
Owner NANJING UNIV OF SCI & TECH
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