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A kind of continuous preparation method of 1,1-diamino-2,2-dinitroethylene

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 large amount of materials in production, cumbersome operations, accidental explosions, etc., and achieve reduction The effect of improving online volume, improving purity and improving production efficiency

Active Publication Date: 2017-06-27
NANJING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, the disadvantage of this method is that the process is long, and the intermediate product (3) needs to be separated and washed with concentrated sulfuric acid before being hydrolyzed. The operation is cumbersome and dangerous.
The batch reaction preparation method has a relatively large amount of materials in production. Once the heat released by the reaction cannot be dissipated in time, the accumulation of heat may cause accidental explosion accidents.

Method used

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  • A kind of continuous preparation method of 1,1-diamino-2,2-dinitroethylene
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  • A kind of continuous preparation method of 1,1-diamino-2,2-dinitroethylene

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preparation example Construction

[0023] A kind of continuous preparation method of 1,1-diamino-2,2-dinitroethylene of the present invention, comprises the following steps:

[0024] Step 1, dissolving 2-methyl-4,6-dihydroxypyrimidine in concentrated sulfuric acid to obtain a sulfuric acid solution of 2-methyl-4,6-dihydroxypyrimidine; the 2-methyl-4,6- The sulfuric acid solution of dihydroxypyrimidine refers to the solution obtained by dissolving solid 2-methyl-4,6-dihydroxypyrimidine into sulfuric acid with a concentration of 95%-100%. In the above solution, 2-methyl-4,6- The concentration range of dihydroxypyrimidine is 0.05g / ml-0.2g / ml.

[0025] Step 2. Use continuous conveying equipment to convey the sulfuric acid solution of 2-methyl-4,6-dihydroxypyrimidine, the inert solvent and the main nitrating agent in parallel, and the above three liquid materials are mixed through the first mixer and conveyed through the pipeline , the above-mentioned mixed material in the pipeline is continuously treated with ultr...

Embodiment 1

[0036] The peristaltic pump is used as the continuous conveying equipment for liquid materials. Both the first mixer and the second mixer use static mixers. The liquid material conveying pipeline adopts polytetrafluoroethylene pipes with an inner diameter of 2mm. The solid-liquid separation of materials adopts vacuum filtration device , The pipeline after the liquid material is mixed is immersed in a constant temperature water bath for heat dissipation, and an ultrasonic generator is installed inside the constant temperature water bath.

[0037]Using 99.0% 1,1-diamino-2,2-dinitroethylene (MDP) as raw material, first weigh 40 grams of MDP and dissolve 98% of the concentrated sulfuric acid to obtain 200ml of MDP solution for subsequent use, MDP The concentration of the solution is 0.2g / ml; prepare 200ml of 98% fuming nitric acid and 1000ml of inert solvent dichloromethane.

[0038] Three peristaltic pumps are used to control the volume flow of MDP solution, main nitrating agent ...

Embodiment 2

[0044] The plunger pump is used as the continuous conveying equipment for liquid materials. Using the same raw materials and continuous reaction process as in Example 1 to prepare 1,1-diamino-2,2-dinitroethylene, only double the volume flow rate of material delivery, that is, the volume flow rate of the MDP solution is set to 0.4ml / min, the volume flow rate of the main nitrating agent is 0.4ml / min, the volume flow rate of the inert solvent is 1.0ml / min, that is, the volume flow rate of the main nitrating agent is 1 time of the volume flow rate of the MDP solution, and the volume flow rate of the inert solvent is the volume of the MDP solution 2.5 times the traffic. The feed temperature of the main nitrating agent and the MDP solution are both 15°C. After passing through the mixer, the material flows through a pipeline with an inner diameter of 4 mm and a length of 60 meters. After mixing, the material stays in the pipeline for about 27 minutes, that is, 0.45 hours, and then ...

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Abstract

The present invention discloses a method for continuous preparation of 1,1-diamino-2,2-dinitroethylene. The method comprises: using a continuous transport device to transport a sulphuric acid solution, an inert solvent and a main nitrating agent of 2-methyl-4,6-dihydroxy pyrimidine in parallel; mixing the materials in a first blender and transporting the mixture by using a heat dissipation pipeline; carrying out nitrification reaction during mixing and transportation, and meanwhile carrying out ultrasonic treatment on the mixed materials; continuously mixing the mixed materials with water by using a second blender, and transporting the mixture by using a heat dissipation pipeline; carrying out hydrolysis reaction in the transport pipeline; then subjecting the resultant product to solid-liquid separation, washing, and drying to obtain 1,1-diamino-2,2-dinitroethylene. This method significantly improves reaction efficiency and simplifies the operation. During continuous feeding and mixing, the inert solvent is introduced, so that heat released from the reaction is more promptly and uniformly diffused, thereby removing potential accidents that may be caused by untimely heat dissipation of a batch reactor, and improving intrinsic safety of the preparation method.

Description

technical field [0001] The invention belongs to the synthesis technology of organic compounds, in particular to a continuous 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 Energetic materials have good compatibility, so this compound has attracted extensive attention, and it is very necessary to improve the synthesis efficiency and process safety of this compound. The traditional synthesis method is carried out by batch process. Due to the large amount of heat released during the synthesis reaction of this compound, once the reaction temperature is out of control, there is a greater risk of explosion accidents, especially in the industrial production process. The risk is increased, so the intermittent reaction equipment sys...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/24C07C209/62
Inventor 蔺向阳邵闪李营黄海丰杨军潘仁明
Owner NANJING UNIV OF SCI & TECH