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Method of preparing 1,5-diazido-3-nitryl azapentane

A nitroazopentane and diazide-based technology, applied in the field of new energetic plasticizer 1, can solve problems such as increased process risk, difficult recycling, and potential safety hazards

Inactive Publication Date: 2015-01-07
LIMING RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] (1) The DINA preparation process is a strong exothermic nitration reaction, and the temperature is not easy to control, which increases the risk of the process;
[0009] (2) DINA itself is an explosive with high energy. It is solid at room temperature and has high sensitivity. The impact sensitivity is H 50 = 31cm (2kg drop hammer), there are great safety hazards in its use and transfer process;
[0010] (3) DINA and NaN 3 The reaction is carried out in an organic solvent such as DMF or DMSO. After the reaction, add water to precipitate the product. The organic solvent is used in a large amount and is not easy to recycle.

Method used

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  • Method of preparing 1,5-diazido-3-nitryl azapentane
  • Method of preparing 1,5-diazido-3-nitryl azapentane

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Experimental program
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Effect test

Embodiment 1

[0023] Add 35.7g of bis(2-chloroethyl)amine hydrochloride and 35ml of 98% nitric acid in a 500ml reaction flask, add 86ml of acetic anhydride dropwise to the reaction solution under stirring, and raise the temperature of the reaction solution to 75 ℃, and continue to keep warm for 3h. Add 100ml dichloromethane and 200ml water at the end of the reaction, and wash the organic phase with water-5%Na 2 CO 3 Washing - washing with water, drying with anhydrous magnesium sulfate, and concentrating the organic phase to obtain 24.9 g of light yellow oily liquid BCENA with a yield of 67% and a purity of 97.6% as measured by liquid chromatography.

Embodiment 2

[0025] In the 500ml reaction flask, add 35.7g of bis(2-chloroethyl)amine hydrochloride, 50ml of carbon tetrachloride, 18ml of 98% nitric acid, add 45ml of acetic anhydride dropwise to the reaction solution under stirring, after the dropwise addition, add The temperature of the reaction solution was raised to 60° C. and kept warm for 2 h. At the end of the reaction, add water for liquid separation, and wash the organic phase with water - 5% Na 2 CO 3 Washing with aqueous solution - washing with water, drying with anhydrous magnesium sulfate, and concentrating the organic phase to obtain 24.5 g of light yellow oily liquid BCENA with a yield of 66% and a purity of 97.2% as determined by liquid chromatography.

Embodiment 3

[0027] In the 500ml reaction flask, add 35.7g of bis(2-chloroethyl)amine hydrochloride, 60ml of dichloroethane, 26ml of 98% nitric acid, 70ml of acetic anhydride is added dropwise to the reaction solution under stirring, after the dropwise addition, the The temperature of the reaction solution was raised to 80° C. and kept warm for 4 h. After the reaction, add water solution, and the organic phase is washed with water - 5% Na 2 CO 3 Washing with aqueous solution - washing with water, drying with anhydrous magnesium sulfate, and concentrating the organic phase to obtain 25.2 g of light yellow oily liquid BCENA with a yield of 67% and a purity of 98.0% as measured by liquid chromatography.

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Abstract

The invention discloses a method of preparing 1,5-diazido-3-nitryl azapentane. The method comprises the following steps: firstly, nitrifying by virtue of a nitric acid-acetic anhydride system to synthesize an intermediate 1,5-di chlorethyl-3-nitryl azapentane (BCENA) by taking di(2-chlorethyl) amine hydrochloride as a raw material; then, synthesizing the 1,5-diazido-3-nitryl azapentane (DIANP) in an aqueous liquid in the presence of a phase transfer catalyst. According to the method, 1,5- dinitrate yl-3-nitryl azapentane is not used, so that the safety of the preparation process is greatly improved. Besides, the azidation reaction of the method is carried out in the aqueous liquid, and thus, the method is environmentally friendly.

Description

technical field [0001] The invention relates to a synthesis method of novel energy-containing plasticizer 1,5-diazido-3-nitroazopentane. Background technique [0002] 1,5-diazido-3-nitroazopentane (DIANP) is a new type of energetic plasticizer, which not only has excellent plasticizing properties, but also has high energy, high burning rate, low burning temperature, Gas has the advantages of small relative molecular weight and large gas production. Because of its low freezing point, low sensitivity, low volatility, good thermal stability, and good compatibility with common components of propellants and explosives, especially digested cellulose, when it is used in high-energy and low-ablation propellants, the explosion temperature ratio is the same as The energy-grade propellant is 200-400K lower, and the propellant power can reach 1300J / g. When used in conjunction with RDX, the propellant power exceeds 1400J / g, and at the same time, a higher burning rate can be obtained. W...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C247/04
Inventor 薛金强王伟徐琰璐韩世民刘飞张得亮尚丙坤
Owner LIMING RES INST OF CHEM IND