Trinitroethyl energetic compound and preparation method thereof

A technology of trinitroethyl function and trinitroethyl, which is applied in the field of preparation of trinitroethyl energetic compounds, can solve the problems of high sensitivity, explosion hazard, explosion, etc., and meet environmental requirements, thermal Good stability and high oxygen content

Inactive Publication Date: 2012-10-24
HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0003]In recent years, a large number of different types of solid oxidants have been developed, but the availability of practical solid oxidants is still very limited
The practical application of ammonium dinitramide (ADN) still faces some challenges, such as hygroscopicity, low melting point, etc.; due to poor thermal stability and high sensitivity, the practical application of hydrazine nitrate (HNF) is very difficult
The disadvantage of this separation method is that the boiling point of trinitromethane is 48 ~ 50 ° C, and when the temperature reaches the boiling point when dealing with trinitromethane, it is easy to decompose or even explode, and it is difficult to obtain solid trinitromethane products by distillation. of
[0006] Trinitroethanol is an important intermediate for the preparation of trinitroethyl energetic compounds, N. S. Marans [J. Am. Chem. Soc, 1950, 72 ( 11), 5329] and others reported that trinitroethanol can be prepared by reacting trinitromethane and paraformaldehyde, but trinitroethanol needs to be distilled during the operation, which has the risk of explosion, and the melting point of the obtained product is only 30 °C , extremely unstable
[0007]Regarding the synthesis of trinitroethyl compounds, the reaction of substituting the H connected to the N atom with trinitroethyl, domestic researchers have conducted some research : Fang Yingao et al [Energetic Materials, 1997, 5(1): 10], prepared trinitroethyl compounds by first hydroxymethylation and then reacting with trinitromethane, the process operation is cumbersome ; Zhang Jiaoqiang et al [Energetic Materials, 1997, 5(4): 176] also reported a trinitroethyl compound 1- ( 2', 2', 2'-trinitroethyl)- The preparation method of 3, 3-dinitroazetidine, trinitroethanol is extremely unstable, but the method of preparing trinitroethanol is not mentioned in the article

Method used

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  • Trinitroethyl energetic compound and preparation method thereof
  • Trinitroethyl energetic compound and preparation method thereof
  • Trinitroethyl energetic compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Synthesis of trinitromethane, the specific method is as follows:

[0029] For ice bath reaction, a 500 mL four-necked flask was equipped with mechanical stirring, a condenser, and a thermometer, and 180 mL of concentrated sulfuric acid was added to the four-necked flask, and 22.4 g (0.2 mol) of 4,6-dihydroxy-pyrimidine was added in batches, mechanically Stir until completely dissolved. Slowly add 64 g (1 mol) of fuming nitric acid dropwise, and control the dropping rate so that the reaction temperature does not exceed 10 °C. After the dropwise addition, continue to react for 20 min, heat up to 10°C in a water bath, stir for 10 min, then raise the temperature to 20°C, stir for 30 min, and finally raise the temperature to 40°C, stir for 90 min, pour into 800 g of ice-water mixture after the reaction , stirred for 60 min, extracted the aqueous solution with dichloromethane three times (200 mL each time), combined the dichloromethane phases, dried with anhydrous magnesium ...

Embodiment 2

[0031] Synthesis of trinitromethane, the specific method is as follows:

[0032] For ice bath reaction, a 500 mL four-necked flask was equipped with mechanical stirring, a condenser, and a thermometer, and 150 mL of concentrated sulfuric acid was added to the four-necked flask, and 22.4 g (0.2 mol) of 4,6-dihydroxy-pyrimidine was added in batches, mechanically Stir until completely dissolved. Slowly add 51 g (0.8 mol) of fuming nitric acid dropwise, and control the dropping rate so that the reaction temperature does not exceed 10 °C. After the dropwise addition, continue to react for 20 min, heat up to 10°C in a water bath, stir for 10 min, then raise the temperature to 20°C, stir for 30 min, and finally raise the temperature to 40°C, stir for 90 min, pour into 800 g of ice-water mixture after the reaction , stirred for 60 min, extracted the aqueous solution with dichloromethane three times (200 mL each time), combined the dichloromethane phases, dried with anhydrous magnesium ...

Embodiment 3

[0034] Synthetic trinitroethanol, concrete method is as follows:

[0035] A 1000 mL four-neck flask was equipped with mechanical stirring, a condenser, and a thermometer, and 350 mL of carbon tetrachloride was added to it, and a dichloromethane solution of trinitromethane (containing 7.5 g of trinitromethane, 49.6 mmol) and polymer Formaldehyde 1.62 g (mass fraction 95%, containing 49.6 mmol formaldehyde), heated to 62 °C with mechanical stirring for 3 h, then heated to 75 °C and refluxed for 30 min. After the reaction solution was filtered, the filtrate was rotary evaporated to 100 mL under reduced pressure, and placed in a refrigerator to precipitate long needle-like crystals with a melting point of 72 °C and a yield of 85%.

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Abstract

The invention relates to a trinitroethyl energetic compound. According to a method for preparing the trinitroethyl energetic compound, low temperature vacuum distillation is combined based on an extraction method to obtain a trinitromethane solution, wherein the operation is simple and safe; the trinitromethane reacts with paraformaldehyde to synthesize trinitroethanol so as to avoid explosion danger due to trinitroethanol distillation, and provide advantages of high purity and high yield; the trinitroethanol and an amino group in an amine, an azole or an azine are subjected to a condensation reaction to synthesize the trinitroethyl energetic compound. The trinitroethyl energetic compound of the present invention has high explosion heat and high oxygen balance value, and is a candidate oxidizing agent variety, wherein the candidate oxidizing agent variety can replace commonly used components comprising AP and HMX of solid propellants, part of the trinitroethyl energetic compound provides significantly-lowered sensitivity and the same energy compared with the HMX, and the trinitroethyl energetic compound of the present invention is adopted as an excellent low sensitivity high energy compound, and provides wide application prospects in the field of solid propellants.

Description

technical field [0001] The invention relates to the technical field of research on energetic components of solid propellants, in particular to a preparation technology of trinitroethyl energetic compounds applied to solid propellants. Background technique [0002] At present, ammonium perchlorate (AP) is widely used as an oxidant in the field of solid propellants. However, AP is the source of high signal and environmental pollution smoke generated by solid propellant combustion, and it must be replaced in the future. For a long time, researchers have been trying to develop a new high-energy oxidant with higher density, enthalpy of formation, and effective oxygen content, and without halogen elements, to replace the widely used oxidant AP. [0003] In recent years, a large number of different kinds of solid oxidants have been developed, but the availability of practical solid oxidizers is still very limited. The practical application of ammonium dinitramide (ADN) still faces...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D257/08C07D257/06
Inventor 任晓婷何金选王亚卢艳华雷晴郭潆媛
Owner HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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