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Preparation method of perdeuterated 1, 5-diaminotetrazole

A technology of diaminotetrazole and deuteration, which is applied in the field of synthesis of deuterated energetic materials, can solve the problems of high sensitivity of cyanogen azide and the danger of direct use, and achieve short operation process, safe and controllable operation process, and safe sex high effect

Inactive Publication Date: 2020-09-29
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2008, Joo et al. synthesized DAT with cyanogen azide and hydrazine, and increased its yield to 79%. However, the dry cyanogen azide used in this reaction is highly sensitive and it is very dangerous to use directly
In addition, the products obtained by the above method are all non-deuterated 1,5-diaminotetrazoles, and we cannot achieve efficient production of fully deuterated 1,5-diaminotetrazoles by replacing raw materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Place a three-port pressure-resistant device with a volume of 100mL and 0.92g of cyanogen chloride in a high-precision medium-temperature circulating bath at -15°C, seal the device, replace the air in the device with nitrogen for three times, and then pass constant pressure dripping Add 14.3g of anhydrous acetonitrile dropwise into the device through the funnel at a rate of 1mL / min. After the dropwise addition, start stirring at a rate of 50rpm and stir for 15 minutes. After the cyanogen chloride is completely dissolved, slowly add 0.8g of acetonitrile into the device. For sodium nitride, keep the temperature of the solution not higher than -5°C during the addition process. After the addition is complete, seal the reaction device, replace the air in the device with nitrogen, replace three times, raise the temperature to 5°C, and heat the solution for 6 hours. The temperature was lowered to -3°C, followed by suction filtration to obtain filtrate C;

[0017] The filtrate ...

Embodiment 2

[0020] Place a three-port pressure-resistant device with a volume of 100mL and 1.66g of cyanogen chloride in a high-precision medium-temperature circulating bath at -15°C, seal the device, replace the air in the device with nitrogen for three times, and then pass constant pressure dripping Add 27.2g of anhydrous acetonitrile dropwise into the device through the funnel at a rate of 2mL / min. After the dropwise addition, start stirring at a rate of 70rpm and stir for 17 minutes. After the cyanogen chloride is completely dissolved, slowly add 1.7g of acetonitrile into the device. Potassium nitride, keep the solution temperature not higher than -5°C during the addition process, after the addition is complete, seal the reaction device, replace the air in the device with nitrogen, replace three times, raise the temperature to 10°C, keep stirring for 5 hours, and dissolve the solution The temperature was lowered to -3°C, followed by suction filtration to obtain filtrate C;

[0021] Th...

Embodiment 3

[0024] Place a three-port pressure-resistant device with a volume of 200mL and 4.77g of cyanogen bromide in a high-precision medium-temperature circulating bath at -10°C, seal the device, replace the air in the device with nitrogen for three times, and then pass constant pressure dripping Add 84.8g of anhydrous acetonitrile dropwise into the device through the funnel at a rate of 4mL / min. After the dropwise addition, start stirring at a rate of 80rpm and stir for 17 minutes. After the cyanogen bromide is completely dissolved, slowly add 2.2g of acetonitrile into the device. For sodium nitride, keep the temperature of the solution not higher than -5°C during the addition process. After the addition is complete, seal the reaction device, replace the air in the device with nitrogen, replace three times, raise the temperature to 10°C, keep stirring for 5 hours, and dissolve the solution The temperature was lowered to -4°C, followed by suction filtration to obtain filtrate C;

[00...

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Abstract

The invention discloses a preparation method of perdeuterated 1, 5-diaminotetrazole, and belongs to a synthesis technology of a deuterated energetic material. Relatively safe sodium (potassium) azideis used as the raw material, cyanogen azide with high sensitivity is not used as the raw material, the operation process is safe and controllable, the safety is high, and the operation process is short. According to the method, the preparation of the perdeuterated 1, 5-diaminotetrazole is realized, the purity of the obtained product is 99.4% or above, the yield is relatively high, and no obvious by-product is generated. Compared with common 1, 5-diaminotetrazole, the crystal density of perdeuterated 1, 5-diaminotetrazole is increased by 4.1%, the detonation velocity is increased to about 5945m / s from 5765 m / s, meanwhile, the initial decomposition temperature of perdeuterated 1, 5-diaminotetrazole is increased, the thermal stability is improved, and the application range of perdeuterated 1, 5-diaminotetrazole is widened. According to the invention, reference can be provided for industrial production of perdeuterated 1, 5-diaminotetrazole.

Description

technical field [0001] The invention relates to a preparation method of fully deuterated 1,5-diaminotetrazole, which belongs to the synthesis technology of deuterated energetic materials. Background technique [0002] 1,5-diaminotetrazole, also known as DTA, has a high nitrogen content (84%) and good thermal stability (melting point is 183°C, initial decomposition temperature is 210°C), and can be reacted with strong acid to obtain 1, 5-diaminotetrazole hydrochloride, nitrate and perchlorate, DTA salts and complexes have good explosive properties, and are expected to be potential energetic materials with high energy density. [0003] Neutron diffraction technology is a new method developed in recent decades to study the internal structure of matter and crystal defects. The use of neutron single crystal diffraction can be used to study the occupancy of hydrogen atoms in materials, and the use of perdeuterated 1,5-diaminotetrazole helps to avoid the influence of hydrogen on t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D257/06C06B43/00
CPCC06B43/00C07B2200/05C07D257/06
Inventor 刘吉平方祝青
Owner BEIJING INSTITUTE OF TECHNOLOGYGY