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Synthesis method of 5-nitrotetrazole sodium salt dihydrate

A technology of sodium nitrotetrazolium and dihydrate, applied in organic chemistry methods, organic chemistry, etc., can solve the problems of cumbersome, complicated process operation, and low product yield, and achieve complex operation process, simple operation process, and high product yield. The effect of high yield

Active Publication Date: 2018-09-28
XIAN MODERN CHEM RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The synthesis method of 5-nitrotetrazolium sodium salt dihydrate reported in the above-mentioned literature, the main process operation is complex, loaded down with trivial details, and the product yield is low, only 69.0%

Method used

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  • Synthesis method of 5-nitrotetrazole sodium salt dihydrate
  • Synthesis method of 5-nitrotetrazole sodium salt dihydrate
  • Synthesis method of 5-nitrotetrazole sodium salt dihydrate

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Effect test

Embodiment 1

[0017] Under stirring, add 5.15g (60.6mmol) of 5-aminotetrazole, 80mL of distilled water, and 3g of concentrated sulfuric acid with a mass percentage of 95% to 98% into the reaction flask in sequence at 20°C to 25°C, heat up to 40°C, and stir Dissolve and set aside; under stirring, add 12.55g (181.8mmol) sodium nitrite into 80mL distilled water, stir to dissolve, add the above-mentioned sulfuric acid aqueous solution of 5-aminotetrazole dropwise, control the temperature of the system not higher than 30°C, add dropwise After completion, stir for 10 minutes, raise the temperature to 65°C to 70°C for 2 hours, add 3g of sodium hydroxide, stir to dissolve, distill off the water under reduced pressure, add 360mL acetone to the distillation bottle and reflux for 2 hours, remove insoluble matter by filtration, and evaporate the filtrate under reduced pressure Acetone and air-dried to obtain 10.13 g of 5-nitrotetrazole sodium salt dihydrate, with a yield of 96.7%.

[0018] Structure Id...

Embodiment 2

[0027] Under stirring, at 20°C to 25°C, 5.15g (60.6mmol) of 5-aminotetrazole, 80mL of distilled water, and 1.8g of concentrated sulfuric acid with a mass percentage of 95% to 98% were successively added to the reaction flask, and the temperature was raised to 40°C. Stir to dissolve and set aside; under stirring, add 10.46g (151.5mmol) sodium nitrite to 80mL distilled water, stir to dissolve, add the above-mentioned sulfuric acid aqueous solution of 5-aminotetrazole dropwise, control the temperature of the system not higher than 30°C, drop After the addition, stir for 10 minutes, raise the temperature to 65°C to 70°C for 2 hours, add 1.8g of sodium hydroxide, stir to dissolve, distill off the water under reduced pressure, add 206mL of acetone to the distillation bottle and reflux for 2 hours, filter to remove insoluble matter, and depressurize the filtrate The acetone was distilled off and air-dried to obtain 5.09 g of 5-nitrotetrazolium sodium salt dihydrate with a yield of 48....

Embodiment 3

[0029] Under stirring, at 20°C to 25°C, 5.15g (60.6mmol) of 5-aminotetrazole, 80mL of distilled water, and 4.12g of concentrated sulfuric acid with a mass percentage of 95% to 98% were successively added to the reaction flask, and the temperature was raised to 40°C. Stir to dissolve and set aside; under stirring, add 14.64g (212.1mmol) sodium nitrite into 80mL distilled water, stir to dissolve, add the above-mentioned sulfuric acid aqueous solution of 5-aminotetrazole dropwise, control the temperature of the system not higher than 30°C, drop After the addition, stir for 10 minutes, raise the temperature to 65°C-70°C for 2 hours, add 4.12g of sodium hydroxide, stir to dissolve, distill off water under reduced pressure, add 412mL of acetone to the distillation bottle and reflux for 2 hours, filter to remove insoluble matter, and depressurize the filtrate The acetone was distilled off and air-dried to obtain 8.68 g of 5-nitrotetrazolium sodium salt dihydrate with a yield of 82.8%....

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Abstract

The invention discloses a synthesis method of 5-nitrotetrazole sodium salt dihydrate, which includes the steps of: under stirring at 20-25 DEG C, successively adding 5-aminotetrazole, distilled waterand concentrated sulfuric acid with mass percentage being 95-98% into a reaction bottle, heating the components to 40 DEG C, stirring the components for dissolution for later use; under stirring, adding sodium nitrite to distilled water, stirring the liquid for dissolution, dropwise adding the sulfuric acid water solution of 5-aminotetrazole, controlling the temperature of the system to be not more than 30 DEG C, after the solution is added, stirring the mixture for 10 min, heating the mixture to 65-70 DEG C and performing a reaction for 2 h, adding NaOH, stirring the mixture for dissolution,performing pressure reduced evaporation to remove water, adding acetone to the distiller bottle for reflux, filtering the mixture to remove insoluble substances, performing pressure reduced evaporation to remove acetone, and naturally air-drying the product to obtain the 5-nitrotetrazole sodium salt dihydrate. The method is mainly used for synthesizing the 5-nitrotetrazole sodium salt dihydrate.

Description

technical field [0001] The invention belongs to the field of energetic materials, in particular to a method for synthesizing 5-nitrotetrazole sodium salt dihydrate. Background technique [0002] Because of the presence of more C-N, N-N, C=N and N=N bonds in the molecular structure of nitrogen-rich heterocyclic compounds, they have higher positive heat of formation, higher density and better oxygen balance value, and have high Due to the advantages of gas generation, low sensitivity and clean detonation products, tetrazole compounds are typical representatives of nitrogen-rich heterocyclic compounds, so they have attracted much attention in the field of energetic materials research. The detonation velocity and detonation pressure of 5-nitrotetrazole are comparable to those of HMX. It is a typical energetic structural unit and can be used to construct new high energy density materials. Energetic groups, in order to obtain 5-nitrotetrazole derivatives with excellent comprehens...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D257/06
CPCC07B2200/13C07D257/06
Inventor 李亚南常佩周群陈涛胡建建王彬张红武
Owner XIAN MODERN CHEM RES INST
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