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Preparation method of perdeuterated tetrol

A technology of deuterated and deuterated nitric acid, which is applied in the field of synthesis of deuterated energetic materials, can solve the problems of poor quality of tequier products, failure to meet production needs, complicated operation process, etc., and achieve simple post-processing and temperature change Effects with small amplitude and simple compositing paths

Active Publication Date: 2020-09-22
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is easy to produce meta-nitro tequil in the production process, and this impurity has this very bad influence on tequil product quality, and this method operation process is too complicated, and productive rate is lower
Therefore if only the raw material of above-mentioned method is replaced with deuterated raw material to prepare deuterated tequil, the purity of gained product is relatively low, and productive rate is not high, can't satisfy production needs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Place a four-mouth pressure-resistant container with a volume of 50 mL and 7.1 g of phosphorus pentoxide in a high-precision medium-temperature circulating bath at -5 ° C, and add 19.6 g of phosphorus pentoxide to the concentration of phosphorus pentoxide through a constant pressure dropping funnel. For 98% deuterated nitric acid, stir the solution at a rate of 150rpm. After the phosphorus pentoxide is dissolved, slowly add 8.1g of deuterated p-chloronitrobenzene into the nitric acid solution in 4 equal parts, and keep mixing during the addition process. The temperature of the liquid is not higher than 5°C. After the deuterated p-chloronitrobenzene is dissolved, seal the reaction device, raise the temperature to 55°C, keep it for 2 hours and let it stand for stratification. Pour the upper organic phase into 10ml and the temperature is 5°C. In deionized water, stirred at a rate of 50rpm for 30 minutes, suction filtered, and the filtrate was washed with deionized water at ...

Embodiment 2

[0025] Place a four-mouth pressure-resistant container with a volume of 100mL and 21.8g of phosphorus pentoxide in a high-precision medium-temperature circulating bath at -5°C, and add 50.3g of phosphorus pentoxide at a concentration of For 98% deuterated nitric acid, stir the solution at a rate of 150rpm. After the phosphorus pentoxide is dissolved, slowly add 17.8g of deuterated p-chloronitrobenzene into the nitric acid solution in 6 equal parts, and keep mixing during the addition process. The temperature of the liquid is not higher than 5°C. After the deuterated p-chloronitrobenzene is dissolved, seal the reaction device, raise the temperature to 45°C, keep it for 4 hours and let it stand for stratification. Pour the upper organic phase into 30ml and the temperature is 5°C. In deionized water, stirred at a rate of 70rpm for 30 minutes, suction filtered, and the filtrate was washed with deionized water at 5°C until the pH of the filtrate was neutral, and then the filtrate wa...

Embodiment 3

[0030] Place a four-mouth pressure-resistant container with a volume of 100mL and 11.3g of phosphorus pentoxide in a high-precision medium-temperature circulating bath at -5°C, and add 39.8g of phosphorus pentoxide at a concentration of For 90% deuterated nitric acid, stir the solution at a rate of 150rpm. After the phosphorus pentoxide is dissolved, slowly add 12.9g of deuterated p-chloronitrobenzene into the nitric acid solution in 4 equal parts, and keep mixing during the addition process. The temperature of the liquid is not higher than 5°C. After the deuterated p-chloronitrobenzene is dissolved, seal the reaction device, raise the temperature to 50°C, keep it for 3 hours and let it stand for stratification. Pour the upper organic phase into 18ml and the temperature is 5°C. In deionized water, stirred at a rate of 70rpm for 30 minutes, suction filtered, and the filtrate was washed with deionized water at 5°C until the pH of the filtrate was neutral, and then the filtrate wa...

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Abstract

The invention relates to a preparation method of perdeuterated tetrol, and belongs to a synthesis technology of a deuterated energetic material. The preparation method comprises the following steps: completely dissolving phosphorus pentoxide and deuterated nitric acid, adding deuterated parachloronitrobenzene to obtain deuterated 2, 4-dinitrochlorobenzene, and dissolving the deuterated 2, 4-dinitrochlorobenzene in a substance A; sequentially adding a deuterated methylamine solution and a sodium deuterium oxide solution, heating, filtering and the like to obtain deuterated 2, 4-dinitro-N-methylaniline; treating to obtain the deuterated tetrol; the method has the advantages of simple synthesis path, no violent oxidation effect in the nitrification process, stable reaction and small temperature change amplitude. Because no violent oxidation reaction exists in the reaction process, the consumption of raw materials is low, meanwhile, the use of deuterated sulfuric acid is avoided due to theuse of phosphorus pentoxide, and the production cost is reduced. No meta-position nitro-tetrol is generated in the nitration process, aftertreatment is simple, refining is not needed, and the productpurity is high. The preparation of the perdeuterated tetrol is realized, and a reference is provided for the industrial production of the perdeuterated tetrol.

Description

technical field [0001] The invention relates to a method for preparing all-deuterated tequil, which belongs to the synthesis technology of deuterated energetic materials. Background technique [0002] 2,4,6-Trinitrobenzyl nitramine, also known as tequier, is an explosive with excellent comprehensive performance, and its specific gravity can reach 1.73. Its detonation sensitivity is good, it is easy to be detonated by the primer, and its own detonation velocity is also high, which can reach 7860m / s. [0003] As early as 1877, Mertens et al. reacted fuming nitric acid with a sulfuric acid solution of dimethylaniline to synthesize tequil first. Nearly three decades later, in 1906, Tequel began to be used as a dynamite. Because of its good explosive power and detonation sensitivity, it was used to fill detonators (as a booster charge) and as a booster charge for shells in World War I. Tequel was also used as a component of high explosives during World War II. Tequel has cert...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C243/02C07C241/00C07B59/00
CPCC07B59/001C07B2200/05C07C201/08C07C209/10C07C241/00C07C243/02C07C211/52C07C205/12
Inventor 刘吉平方祝青
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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