Preparation method of 1-methyl-3,5-binitro-1,2,4-triazole

A technology of dinitro and methyl groups, applied in the direction of organic chemistry, etc., can solve the problems of difficult treatment of wastewater components, low yield of final products, potential safety hazards, etc., and achieve the effects of saving raw materials, low prices, and reducing emissions

Inactive Publication Date: 2017-06-13
ZHONGBEI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The present invention provides a 1-methyl-3,5- The preparation method of dinitro-1,2,4-triazole

Method used

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  • Preparation method of 1-methyl-3,5-binitro-1,2,4-triazole

Examples

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Embodiment 1

[0044] Embodiment 1, a kind of preparation method of 1-methyl-3,5-dinitro-1,2,4-triazole comprises the following steps:

[0045] The first step, the preparation of 1-methyl-3,5-diamino-1,2,4-triazole nitrate (DAMT)

[0046] Put the three-neck flask equipped with a stirrer in an ice-water bath, and after fixing, pour 300mL of water and 260mL of methylhydrazine solution (40%) into the reaction vessel slowly in sequence, stir, cool to -10°C, and then prepare the 310mL of concentrated nitric acid (65%) solution was slowly added dropwise to the aqueous solution of methylhydrazine. The entire feeding process of concentrated nitric acid took 30 minutes, and the temperature was controlled at -10°C, and stirred until completely mixed. After the concentrated nitric acid is added dropwise, 225g of dicyandiamide is added to obtain a mixed solution; the mixed solution is placed at 10°C and stirred for 0.5h. At this time, the dicyandiamide is not completely dissolved, and then the temperatu...

Embodiment 2

[0049] Example 2, in the first step of this example, the amount of water is 350mL, the amount of methylhydrazine is 220mL, cooled to -5°C, the amount of concentrated nitric acid is 250mL, the entire nitration process is 45min, and the temperature is controlled at -5°C, The dosage of dicyandiamide is 260g, the mixed solution is placed at 15°C and stirred for 0.8h, then heated to 85°C and stirred for 3h4h, and then placed at 0°C for 10h after the reaction is completed, and the rest is the same as in Example 1. The obtained product 1 was 324.7g, the yield of the first step reaction was 82.0%, the total reaction yield was 41.18%, and the purity of the target product was 98.40%.

Embodiment 3

[0050] Example 3, in the first step of this example, the amount of water is 400mL, the amount of methylhydrazine is 300mL, cooled to 0°C, the amount of concentrated nitric acid is 350mL, the entire nitration process is 60min, and the temperature is controlled at 0°C, dicyandiamide The amount of amine used was 300g. The mixed solution was placed at 20°C and stirred for 1 hour, then heated to 95°C and stirred for 5 hours. After the reaction was completed, it was placed at 5°C for 11 hours. The rest was the same as in Example 1. The obtained product 1 was 340.55g, the yield of the first step reaction was 86.0%, the total yield of the reaction was 43.19%, and the purity of the target product was 98.63%.

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Abstract

The invention discloses a preparation method of 1-methyl-3,5-binitro-1,2,4-triazole, belongs to the technical field of organic energetic materials and aims at solving the problems in the prior art that a two-step method for preparing DNMT is relatively high in cost, a potential safety hazard exists, wastewater ingredients are complicated and difficult to treat and the final product is low in yield and low in purity. The method comprises the steps of preparing a product 1 of which the main ingredient is 1-methyl-3,5-binitro-1,2,4-triazole nitrate (DAMT) from methylhydrazine and dicyandiamide as reaction raw materials through condensation and cyclization; and carrying out oxidation reaction on the product 1 and hydrogen peroxide to prepare a product 2 DNMT. The 1-methyl-3,5-binitro-1,2,4-triazole is high in yield and high in purity, and the risk of thermal runaway of reaction in the reaction process is avoided.

Description

technical field [0001] The invention belongs to the technical field of organic energetic materials, and in particular relates to a preparation method of 1-methyl-3,5-dinitro-1,2,4-triazole. Background technique [0002] 1-Methyl-3,5-dinitro-1,2,4-triazole (DNMT) is a new type of energetic material with a low melting point. It has excellent comprehensive detonation performance and low impact sensitivity before and after melting. The research on casting explosives with DNMT as the casting agent meets the standards of new casting carriers, and is expected to replace TNT as a new generation of liquid phase carriers, with extremely high potential application value. It was first seen in 2007 by Rao. Surapaneni et al. using DAT as a raw material to synthesize DNT through diazotization, denitrogenation, and nitration, and finally using acetonitrile as a solvent to obtain DNMT through methylation. The synthetic method is complicated, the route is long, the yield is low, and the raw ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D249/14
CPCC07D249/14
Inventor 刘玉存罗进刘燕李阳柴涛王建华袁俊明于雁武
Owner ZHONGBEI UNIV
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