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Preparation method of HMX

A technology of tetraazacyclooctane and tetraazabicyclo, which is applied in the field of energetic material synthesis and green nitration, can solve the problems of low yield and impractical application, and overcome the extremely low yield and low post-processing cost , The effect of high process atom economy

Inactive Publication Date: 2017-10-24
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Dinitrogen pentoxide / organic solvent system is used for the preparation of HMX without adding nitric acid, the product is easy to separate, and has the advantages of environmental protection, but the yield of this system is very low, and it is almost impossible for practical application

Method used

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  • Preparation method of HMX

Examples

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Embodiment 1

[0024] Example 1,3,5,7-tetranitro-1,3,5,7-tetraazacycloctane preparation method of the present invention, the method comprises: dissolving dinitrogen pentoxide in an organic solvent to form a nitrated agent, ammonium salt is slowly added to the nitrating agent, and 3,7-dinitro-1,3,5,7-tetraazabicyclo[3,3,1]nonane (DPT) is added in batches to obtain For the reactant, the temperature of the material is controlled at 0-10°C during the feeding process, the temperature of the reactant is raised to 20-35°C, and the reaction is carried out at a constant temperature for 20-60min; after the reaction is completed, the solid-liquid is separated to obtain a solid, and the solid is washed. Dried, purified to obtain 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane (HMX);

[0025] The organic solvent is selected from acetonitrile and dichloromethane, and the ammonium salt is selected from tetramethylammonium chloride, ammonium carbonate, ammonium acetate and ammonium oxalate.

[0026] The raw...

Embodiment 2

[0041] The preparation method of 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane in Example 2 of the present invention comprises the following steps:

[0042] Step 1, the preparation of nitrourea

[0043] Add 540ml of concentrated sulfuric acid with a concentration of 98% to a 1000ml three-necked flask under an ice-salt bath, weigh 175g of dry urea, and slowly add it into the three-necked flask under vigorous stirring. Concentration is slowly added dropwise in the flask and is the concentrated nitric acid 130ml of 68% (whole process control temperature is under 10 ℃). After the concentrated nitric acid is added, the temperature is lowered to below 5°C, and the reaction is kept for 90 minutes. After the reaction is completed, slowly add the reaction solution in the three-neck flask to two beakers with 500g of ice water under stirring conditions, and control the temperature not to exceed 15°C. During this period, white solids will be precipitated, and then suction filtered A wh...

Embodiment 3

[0049] The preparation method of 1,3,5,7-tetranitro-1,3,5,7-tetraazacycloctane in Example 3 of the present invention comprises the following steps:

[0050] Step 1, the preparation of nitrourea

[0051] Add 540ml of concentrated sulfuric acid with a concentration of 98% to a 1000ml three-necked flask under an ice-salt bath, weigh 185g of dry urea, and slowly add it to the three-necked flask under vigorous stirring. Concentration is slowly added dropwise in the flask and is the concentrated nitric acid 140ml of 68% (whole process control temperature is under 10 ℃). After adding the concentrated nitric acid, lower the temperature to below 5°C and keep the reaction for 60 minutes. After the reaction is completed, slowly add the reaction solution in the three-neck flask to two beakers with 500g of ice water under stirring conditions, and control the temperature not to exceed 15°C. During this period, white solids will be precipitated, and then suction filtered A white solid - ni...

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Abstract

The invention discloses a preparation method of HMX. The preparation method comprises the steps of dissolving dinitrogen pentoxide into an organic solvent to form a nitrating agent; slowly adding ammonium salt into the nitrating agent, and adding DPT in batches to obtain reactants; controlling the temperature of the materials to be 0-10 DEG C in a feeding process, heating the reactants up to 20-35 DEG C, and carrying out a reaction at the constant temperature for 20-60min; after the reaction is finished, carrying out solid-liquid separation to obtain solid; washing the obtained solid, drying in the air, and purifying to obtain the HMX, wherein the organic solvent is selected from acetonitrile and dichloromethane, and the ammonium salt is selected from tetramethyl ammonium chloride, ammonium carbonate, ammonium acetate and ammonium oxalate. The preparation method provided by the invention is mild in reaction conditions and easy in separation of products, and needs a less amount of acid; the system does not produce waste acid, thus being low in treatment cost; furthermore, the preparation method greatly increases the yield of the HMX.

Description

technical field [0001] The invention belongs to the technical field of energetic material synthesis and green nitration, and in particular relates to a preparation method of 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane. Background technique [0002] Nitrification is one of the classic organic reactions. At present, the nitrating agents widely used in industry include nitric acid mixed acid, nitric acid-acetic anhydride, etc. The corresponding process not only has low atomic economy, but also produces a large amount of waste acid and organic acid wastewater in the production process, which is not suitable for the requirements of today's green chemistry. The strong corrosiveness of the mixed acid will also seriously damage the equipment, and the side reactions such as multi-nitration and oxidation that occur during the reaction will cause serious safety hazards. With the improvement of people's awareness of environmental protection, people pay more and more attention to th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/08C07D257/02
CPCC07D487/08C07D257/02
Inventor 唐月娇吕早生
Owner WUHAN UNIV OF SCI & TECH
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