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A kind of synthetic method of 1-nitroso-3,5,7-trinitro-1,3,5,7-tetraazacyclooctane

A tetraazacyclooctane and synthesis method technology, which is applied in the field of energetic material preparation, can solve problems such as low product yield, difficult separation and purification, waste acid discharge, etc., to reduce equipment requirements, reduce costs, and reduce pollution Effect

Active Publication Date: 2022-03-18
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are many disadvantages in the acetic anhydride method: (1) acetic anhydride and acetic acid are used in a large amount, the product yield is low, and the production cost is high; (2) a large amount of waste acid is discharged, which pollutes the environment; The difference in material ratio of nitric acid, ammonium nitrate, acetic anhydride and acetic acid, the difference in feeding method and temperature lead to the production of many by-products, which are difficult to separate and purify.
However, this method must use ammonium nitrate and sodium nitrite solution or dinitrogen tetroxide which are difficult to handle and have explosion hazards, and the process steps are cumbersome

Method used

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  • A kind of synthetic method of 1-nitroso-3,5,7-trinitro-1,3,5,7-tetraazacyclooctane
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  • A kind of synthetic method of 1-nitroso-3,5,7-trinitro-1,3,5,7-tetraazacyclooctane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The optimized synthesis experiment of 1-nitroso-3,5,7-trinitro-1,3,5,7-tetraazacyclooctane was carried out according to the following steps:

[0016] (1) At -25°C, add 0.78g of methylamine hydrochloride solid to 8.0mL of 96% HNO 3 After it dissolves, add 1g of DPT and react for 5min at the changed temperature.

[0017] (2) Slowly add 20mL of water dropwise, control the temperature of the system not to exceed 0°C, filter, wash with water, and dry to obtain 1-nitroso-3,5,7-trinitro-1,3,5,7-tetraaza Cyclooctane 1.0g, the yield is 78.5% based on DPT.

Embodiment 2

[0019] Other operating conditions and steps are the same as in Example 1, and the influence of the hydrochloride of different amines on the reaction is checked, and the results are shown in Table 1.

[0020] Table 1. Effect of hydrochloride salts of different amines on MNX yield

[0021]

[0022] As can be seen from the above-mentioned results, methylamine hydrochloride is the most favorable to this reaction, and even other hydrochlorides of its close structural amines are far inferior to it (embodiment 1) to the promoting effect of reaction.

Embodiment 3

[0024] Other operating conditions and steps are the same as in Example 1, and the impact of the amount of methylamine hydrochloride added on the reaction is checked, and the results are shown in Table 2.

[0025] Table 2. The impact of the amount of methylamine hydrochloride added on the yield of MNX.

[0026]

[0027]

[0028] As can be seen from the above results, the methylamine hydrochloride add-on is preferably 0.78g (embodiment 1).

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Abstract

The invention discloses a method for synthesizing 1-nitroso-3,5,7-trinitro-1,3,5,7-tetraazacyclooctane. Its steps are: first at low temperature 3,7-dinitro-1,3,5,7-tetraazabicyclo [3.3.1] nonane in methylamine hydrochloride and mass fraction of 96% fume Carry out nitrolysis reaction and nitrolysis reaction in nitric acid system; slowly add water dropwise, filter, wash with water, and dry to obtain 1‑nitroso‑3,5,7‑trinitroso‑1,3,5,7‑tetraaza Cyclooctane. The method avoids the use of ammonium nitrate, the obtained product has high purity, and the yield reaches 78.5%; it also avoids the use of sodium nitrite or dinitrogen tetroxide, etc., which simplifies the production process, reduces production costs, and reduces environmental pollution; improves production safety .

Description

technical field [0001] The invention relates to a synthesis method of 1-nitroso-3,5,7-trinitro-1,3,5,7-tetraazacyclooctane, belonging to the field of energetic material preparation. Background technique [0002] Octojin (1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane, referred to as HMX) is currently the best single substance high energy dense compounds. The industrialized production of Octo today basically follows the improved Bachmann method, i.e. the acetic anhydride method (US2461582, 1949). With urotropine as raw material, it can be obtained by nitrification in nitric acid-ammonium nitrate-acetic anhydride system. However, there are many disadvantages in the acetic anhydride method: (1) acetic anhydride and acetic acid are used in a large amount, the product yield is low, and the production cost is high; (2) a large amount of waste acid is discharged, which pollutes the environment; The difference in material ratio of nitric acid, ammonium nitrate, acetic anhydride a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D257/02
CPCC07D257/02
Inventor 罗军张宇候天骄张健
Owner NANJING UNIV OF SCI & TECH
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