Synthetic method of diethanol nitramine dinitrate

A technology of diethanol nitramine dinitrate and diethanolamine hydrochloride, applied in the direction of organic chemistry and the like, can solve problems such as high explosion risk, and achieve the effects of improving reaction efficiency, easy control of synthesis process and fast reaction speed

Pending Publication Date: 2020-10-13
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of synthetic method of diethanol nitramine dinitrate in order to overcome the shortcoming of the high explosion risk of the existing synthetic method

Method used

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  • Synthetic method of diethanol nitramine dinitrate
  • Synthetic method of diethanol nitramine dinitrate
  • Synthetic method of diethanol nitramine dinitrate

Examples

Experimental program
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Effect test

Embodiment 1

[0029] The synthetic method of the diethanol nitramine dinitrate of present embodiment 1 comprises the following steps:

[0030] Add 345g of acetic anhydride containing a small amount of 40g of fuming nitric acid to the 1L reaction calorimeter RC1e reactor, adjust the temperature of the reactor to 10°C, and then add 137g of diethanolamine hydrochloride and 195g of fuming nitric acid at the same time. The molar ratio of diethanolamine hydrochloride to fuming nitric acid to acetic anhydride is 1:3.2:3.5. After the feeding is finished, wait for 30 minutes, raise the temperature of the system to 40°C, and keep the temperature for 30 minutes. After completion, the reaction solution was poured into ice water to precipitate crystals, and the target product diethanolamine dinitrate 1 was obtained by suction filtration and drying. Yield 72.5%.

[0031] Due to incomplete nitration, the product contains impurities and is not pure. Carry out DSC test and nuclear magnetic characterizati...

Embodiment 2

[0033] The synthetic method of the diethanol nitramine dinitrate of present embodiment 2 comprises the following steps:

[0034] Add 345g of acetic anhydride containing a small amount of 40g of fuming nitric acid to the 1L reaction calorimeter RC1e reactor, adjust the temperature of the reactor to 10°C, and then add 100g of diethanolamine hydrochloride and 200g of fuming nitric acid at the same time. The molar ratio of diethanolamine hydrochloride to fuming nitric acid to acetic anhydride is 1:4.5:4.8. After the feeding was finished, because the amount of solvent was too small, crystallization occurred immediately in the reactor, and the target product diethanolamine dinitrate 2 was separated out, and the experiment ended. The yield is 73.8%.

[0035] There were no impurities in the product. Carry out DSC test and nuclear magnetic characterization to the product, the result sees image 3 , 4 shown.

Embodiment 3

[0037] The synthetic method of the diethanol nitramine dinitrate of present embodiment 3 comprises the following steps:

[0038] Add 345g of acetic anhydride containing a small amount of 45g of fuming nitric acid to the 1L reaction calorimeter RC1e reactor, adjust the temperature of the reactor to 10°C, and then simultaneously add 80g of diethanolamine hydrochloride and 150g of fuming nitric acid. The molar ratio of diethanolamine hydrochloride to fuming nitric acid to acetic anhydride is 1:4.5:6. After the feeding is finished, wait for 60 minutes, raise the temperature of the system to 40°C, and keep the temperature for 30 minutes. After completion, the reaction solution was poured into ice water to precipitate crystals, and the target product diethanolamine dinitrate 3 was obtained by suction filtration and drying. Yield 82%.

[0039] There were no impurities in the product. The heat release rate q of the reaction process r , Reaction temperature T r curve see Figure ...

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Abstract

The invention relates to a synthetic method of diethanol nitramine dinitrate. The method comprises the following steps: adding acetic anhydride containing a small amount of fuming nitric acid I into areaction kettle as a backing material, simultaneously adding diethanol amine hydrochloride and fuming nitric acid II at a certain reaction temperature, heating to carry out heat preservation reactionafter the feeding is finished, and finally cooling and washing the reaction product, carrying out suction filtration and drying the reaction product to obtain the final product. The method is high inreaction speed and uniform in heat release, and the synthesis process is easy to control; the product diethanol nitramine dinitrate is synthesized in one step, so that the reaction efficiency is improved; in the product synthesis process, the existence time of the unstable intermediate in the reaction system is short, so that the unstable intermediate can be quickly converted into diethanol nitramine dinitrate, and compared with a magnesium nitrate synthesis method, the safety is obviously improved.

Description

technical field [0001] The invention relates to a method for synthesizing diethanol nitramine dinitrate, which belongs to the field of synthesizing energetic materials. Background technique [0002] Diethanol nitramine dinitrate is an ammonium nitrate explosive containing O-nitro and N-nitro groups. It is famous for its abbreviation, DINA for short. DINA is a non-volatile gel of nitrocellulose Agent, can replace nitroglycerin to make smokeless medicine. Nitrocellulose, nitroguanidine, and gener make a non-hygroscopic, flameless propellant. Gena is also used as the charge of the bomb booster or as the active plasticizer component of some mixed explosives. [0003] At present, the domestic preparation of diethanolamine dinitrate all adopts the magnesium nitrate method, which is based on diethanolamine as a raw material, magnesium oxide as a dehydrating agent, and sodium chloride as a catalyst. Several unstable intermediates will be formed in the process, and "" "wax hanging...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C243/02
CPCC07C243/02
Inventor 郭子超李伟陈利平陈网桦
Owner NANJING UNIV OF SCI & TECH
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