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A kind of preparation method of n-(1-imino-2,2-dinitroethyl)-2,2-dinitroacetamide potassium salt

A technology of dinitroacetamide and dinitroethyl, which is applied in the field of preparation of N--2,2-dinitroacetamide potassium salt, can solve the problem of no N- and the like, and can ensure safety and good heat dissipation. effect, the effect of improving process safety

Active Publication Date: 2018-12-14
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After retrieval, there is no public literature report on the synthesis method of N-(1-imino-2,2-dinitroethyl)-2,2-dinitroacetamide potassium salt

Method used

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  • A kind of preparation method of n-(1-imino-2,2-dinitroethyl)-2,2-dinitroacetamide potassium salt
  • A kind of preparation method of n-(1-imino-2,2-dinitroethyl)-2,2-dinitroacetamide potassium salt
  • A kind of preparation method of n-(1-imino-2,2-dinitroethyl)-2,2-dinitroacetamide potassium salt

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Embodiment 1

[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 2 mm. Prepare nitric-sulfur mixed acid in advance according to the volume ratio of concentrated sulfuric acid and fuming nitric acid at 1:1, and cool to room temperature. Weigh 5.0g of 2-methyl-4,6-dihydroxypyrimidine and 3.0g of potassium nitrate into a 500ml three-neck flask, add dichloromethane 3 times the mass of 2-methyl-4,6-dihydroxypyrimidine , start the agitator, control the temperature of the reaction material to -5 ~ 5 ° C, add 50 ml of nitric acid mixed acid at a rate of 0.5 ml / min, monitor the temperature of the material during the dropwise addition, and prevent the temperature of the material from rising by reducing the rate of addition , to ensure that the temperature of the material does not exceed 15°C. After adding nitric sulfur mixed acid, continue to nitrate ...

Embodiment 2

[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 mixed nitric acid in advance according to the volume ratio of 98% concentrated sulfuric acid and fuming nitric acid at a volume ratio of 2:1, and cool to room temperature. Weigh 5.0g of 2-methyl-4,6-dihydroxypyrimidine and 1.8g of potassium sulfate into a 1000ml three-necked flask, add 10 times the mass of 2-methyl-4,6-dihydroxypyrimidine in chloroform , start the agitator, control the temperature of the reaction material to be 5-10°C, add 75ml of nitric-sulfur mixed acid at a rate of 0.5ml / min, monitor the temperature of the material during the dropwise addition, and prevent the temperature of the material from rising by reducing the rate of addition. Make sure that the temperature of the material does not exceed 15°C. After adding nitric sulfur mixed acid, conti...

Embodiment 3

[0032]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 mixed nitric acid in advance according to the volume ratio of 98% concentrated sulfuric acid and fuming nitric acid at a volume ratio of 1.5:1, and cool to room temperature. Weigh 5.0g of 2-methyl-4,6-dihydroxypyrimidine and 2.5g of potassium sulfate into a 1000ml three-neck flask, add tetrachloromethane 15 times the mass of 2-methyl-4,6-dihydroxypyrimidine , start the agitator, control the temperature of the reaction material to be 0-5°C, add 50ml of nitric-sulfur mixed acid at a rate of 0.5ml / min, monitor the temperature of the material during the dropwise addition, and prevent the temperature of the material from rising by reducing the rate of addition. Make sure that the temperature of the material does not exceed 10°C. After adding nitric sulfur mixed acid, co...

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Abstract

The invention discloses a method for preapring N-(1-imino-2,2-dinitroethyl)-2,2-binitroacetamide sylvite. The method comprises the following steps: dropwise adding nitric-sulfuric acid into a reactor which is pre-added with 2-methyl-4,6-dihydroxypyrimidine, sylvite and an inert solvent, and continuously stirring at -5-15 DEG C to complete a nitratlon reaction; then continuously adding water into the reaction system, and performing hydrolysis at 0-20 DEG C; and separating solid and liquid after the hydrolysis is completed, washing the separated solid with water and ethanol, and drying to obtain N-(1-imino-2,2-dinitroethyl)-2,2-binitroacetamide sylvite. The method is simple in operation, heat released in the reaction can be dissipated in time since the inert solvent is added into the reactant, and potential safety hazard caused by high temperature in local part can be eliminated.

Description

technical field [0001] The invention belongs to the synthesis technology of organic compounds, in particular to a preparation method of N-(1-imino-2,2-dinitroethyl)-2,2-dinitroacetamide potassium salt. Background technique [0002] Flame suppressant is one of the important additives in solid propellant. The commonly used flame suppressant is potassium nitrate, potassium sulfate and potassium salt of organic acid. help. As the energy levels of solid propellants increase, new demands are placed on the energy levels of all components. Traditional flame suppressants can no longer adapt to this change in demand, and the development of energetic flame suppressants has become an international research hotspot. N-(1-imino-2,2-dinitroethyl)-2,2-dinitroacetamide potassium salt is a new type of high-energy compound. Due to the high oxygen balance of this compound, the enthalpy of formation is much higher than that of nitric acid. Potassium or potassium organic acid has good comprehe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C257/20
CPCC07C257/20C07D239/553
Inventor 蔺向阳孙义龙邵闪李营黄海丰杨军潘仁明
Owner NANJING UNIV OF SCI & TECH