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Method for preparing 1,1-diamido-2,2-binitroethylene at normal temperature

A dinitroethylene and diamino technology, which is applied in the preparation of amino compounds, organic compounds, chemical instruments and methods, etc., can solve the problems of difficult automatic feeding, difficult heat diffusion, safety hazards and side reactions, etc., to achieve Reduce the probability of explosion accidents and side reactions, improve heat dissipation, and simplify the operation process

Inactive Publication Date: 2015-03-04
NANJING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] But the disadvantage of this method is that directly dissolving 2-methyl-4,6-dihydroxypyrimidine in concentrated sulfuric acid is easy to cause agglomeration, because these agglomerates are not easy to be broken, the heat generated by dissolution is difficult to diffuse out, Not only are there potential safety hazards but also side effects
Solid feeding needs to be manually added on site in the reactor, and it is not easy to realize automatic feeding
In addition, concentrated sulfuric acid and fuming nitric acid are added in batches, and the intermediate (3) needs to be washed with concentrated sulfuric acid before being hydrolyzed, and the operation is cumbersome.

Method used

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  • Method for preparing 1,1-diamido-2,2-binitroethylene at normal temperature
  • Method for preparing 1,1-diamido-2,2-binitroethylene at normal temperature
  • Method for preparing 1,1-diamido-2,2-binitroethylene at normal temperature

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Embodiment 1

[0026] The peristaltic pump is used as the continuous conveying equipment for liquid materials, and the liquid material conveying pipeline adopts polytetrafluoroethylene pipes with an inner diameter of 2 mm. Prepare a mixed acid nitrating agent in advance according to the volume ratio of 20% oleum to fuming nitric acid at a volume ratio of 1:1, and cool to room temperature. Weigh 5.0 g of 2-methyl-4,6-dihydroxypyrimidine and add it to a 500ml three-neck flask, add dichloromethane 3 times the mass of 2-methyl-4,6-dihydroxypyrimidine, start the stirrer, The temperature of the reaction material is 22°C, which is basically the same as the room temperature. Add 30ml of mixed acid nitrating agent at a rate of 0.5ml / min, monitor the temperature of the material during the dropping process, and prevent the temperature of the material from rising by reducing the rate of addition to ensure the stability of the material. The temperature does not exceed 35°C. After adding the mixed acid n...

Embodiment 2

[0028] The peristaltic pump is used as the continuous conveying equipment for liquid materials, and the liquid material conveying pipeline adopts polytetrafluoroethylene pipes with an inner diameter of 3 mm. Pre-prepared mixed acid nitrating agent according to the volume ratio of 98% concentrated sulfuric acid and fuming nitric acid as 1:1, and cooled to room temperature. Weigh 5.0 g of 2-methyl-4,6-dihydroxypyrimidine and add it to a 500ml three-neck flask, add chloroform 10 times the mass of 2-methyl-4,6-dihydroxypyrimidine, start the stirrer, The temperature of the reaction material is 22°C, which is basically the same as the room temperature. Add 30ml of mixed acid nitrating agent at a rate of 0.5ml / min, monitor the temperature of the material during the dropping process, and prevent the temperature of the material from rising by reducing the rate of addition to ensure the stability of the material. The temperature does not exceed 35°C. After adding the mixed acid nitrati...

Embodiment 3

[0030]The peristaltic pump is used as the continuous conveying equipment for liquid materials, and the liquid material conveying pipeline adopts polytetrafluoroethylene pipes with an inner diameter of 3 mm. Prepare a mixed acid nitrating agent in advance according to the volume ratio of 98% concentrated sulfuric acid and fuming nitric acid at a volume ratio of 3:1, and cool to room temperature. Weigh 5.0 g of 2-methyl-4,6-dihydroxypyrimidine and add it to a 1000ml three-neck flask, add tetrachloromethane 20 times the mass of 2-methyl-4,6-dihydroxypyrimidine, start the stirrer, The temperature of the reaction material is 25°C, which is basically the same as the room temperature. Add 30ml of mixed acid nitrating agent at a rate of 0.5ml / min, monitor the temperature of the material during the dropping process, and prevent the temperature of the material from rising by reducing the rate of addition to ensure the stability of the material. The temperature does not exceed 35°C. Aft...

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Abstract

The invention discloses a simple preparation method of 1,1-diamido-2,2-binitroethylene (FOX-7). The preparation method comprises the following steps: continuously adding a mixed acid nitrating agent into a reactor in which 2-methyl-4-6-dyhydroxyl pyridine and an inert solvent are added in advance and continuously stirring at normal temperature till the end of reaction; then continuously adding water into the reaction system to realize hydrolysis; and recycling the solvent and byproducts, carrying out solid-liquid separation, washing and drying to obtain a solid product of 1,1-diamido-2,2-binitroethylene. The preparation method has the advantages that the reaction efficiency is improved remarkably; the operation is simplified; since the nitrating agent is added into the reactant continuously and the inert solvent is also added to the reactant, heat released during reaction can be dissipated uniformly in time, potential safety hazards caused by local heating can be avoided, requirement for reaction temperature control is reduced, the possibility of occurrence of side reactions can be lowered and the essential safety of the preparation method is improved further.

Description

technical field [0001] The invention belongs to the synthesis technology of organic compounds, in particular to a normal-temperature preparation method of 1,1-diamino-2,2-dinitroethylene. Background technique [0002] 1,1-diamino-2,2-dinitroethylene (FOX-7) is a new type of high-energy insensitive explosive. It has good heat resistance, energy density is better than RDX, and sensitivity is close to TATB. It is compatible with many The compatibility of energetic materials is good, so this compound has attracted extensive attention. It is very important to improve the synthesis efficiency and process safety of 1,1-diamino-2,2-dinitroethylene. [0003] There are many ways to synthesize 1,1-diamino-2,2-dinitroethylene reported in the literature, the most direct method is to use 2-methyl-4,6-dihydroxypyrimidine or 2-methyl-4, Synthetic method of 6-dipyrimidinone as raw material. When using 2-methyl-4,6-dihydroxypyrimidine as raw material, first dissolve 2-methyl-4,6-dihydroxyp...

Claims

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Application Information

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IPC IPC(8): C07C211/24C07C209/62
Inventor 蔺向阳邵闪郑文芳李权威潘仁明黄振亚孙义龙
Owner NANJING UNIV OF SCI & TECH
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