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Preparation method of ethylenediamine dinitrate

A technology of ethylenediamine dinitrate and ethylenediamine, which is applied in the field of explosive production, can solve the problems of affecting product quality, complicated operation, increasing material cost, etc. The effect of utilization

Pending Publication Date: 2020-09-01
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses > 98% nitric acid and ethylenediamine, the reaction is too violent, and the stability is poor. In addition, the reactants are all highly dangerous chemicals, which are highly toxic and seriously harmful to the environment.
In 2002, Zhao Xingxiang et al. used the saturated filtrate of ethylenediamine dinitrate as the reaction dilution medium to improve the process, using a mixture of ethanol and water as the reaction medium, but ethanol has poor thermal conductivity and the reaction temperature is not easy to control; in addition , Ethanol is prone to side reactions such as oxidative esterification under high concentration of nitric acid, which affects product quality
As mentioned above, the preparation method of ethylenediamine dinitrate not only has harsh conditions and complicated operation, but also produces a large amount of waste acid, which is easy to pollute the environment and increases the material cost, time cost and maintenance cost of production at the same time.

Method used

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  • Preparation method of ethylenediamine dinitrate
  • Preparation method of ethylenediamine dinitrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Put the 250mL three-necked flask in the water tank, add 12.0g of anhydrous ethylenediamine into the three-necked flask, and then add 80mL of solvent (V 水 :V 甲醇 =1:3), stirring, the speed is set to 300r / min. Slowly raise the temperature to 45°C, and at the same time slowly add 37.6g of nitric acid with a mass fraction of 66.0~68.0% dropwise, the dropwise addition is completed within 15 minutes, and the reaction is continued for 10 minutes, and the reaction is completed. Pour all the liquid in the three-neck flask into the beaker prepared in advance, and let it stand for a while until the temperature of the liquid in the beaker is consistent with room temperature, and crystals appear. Filter, wash with anhydrous methanol, dry at 60° C. for 4 hours, and weigh to obtain 31.1 g of ethylenediamine dinitrate, with a yield of 81.1%. Collect the mother liquor filtered in the above steps, replace it with 80mL of solvent and repeat the above steps to obtain 31.6g of ethylenediam...

Embodiment 2

[0022] Put the 250mL three-necked flask in the water tank, add 12.0g of anhydrous ethylenediamine into the three-necked flask, and then add 80mL of solvent (V 水 :V 甲醇 =1:3), stirring, the speed is set to 300r / min. Slowly raise the temperature to 40°C, and at the same time slowly add 37.6g of nitric acid with a mass fraction of 66.0~68.0% dropwise, the dropwise addition is completed within 10 minutes, and the reaction is continued for 10 minutes, and the reaction is completed. Pour all the liquid in the three-neck flask into the prepared beaker and let it stand until it is consistent with room temperature and crystals appear. Filter, wash with anhydrous methanol, dry at 60° C. for 4 hours, and weigh to obtain 30.8 g of ethylenediamine dinitrate, with a yield of 80.4%. The mother liquor filtered in the above steps was collected and replaced with 80 mL of solvent to repeat the above steps to obtain 31.0 g of ethylenediamine dinitrate with a yield of 80.8%.

Embodiment 3

[0024] Put the 250mL three-necked flask in the water tank, add 12.0g of anhydrous ethylenediamine into the three-necked flask, and then add 80mL of solvent (V 水 :V 甲醇 =1:3), stirring, the speed is set to 300r / min. Slowly raise the temperature to 40°C, and at the same time slowly add 37.6g of nitric acid with a mass fraction of 66.0~68.0% dropwise, the dropwise addition is completed within 10 minutes, and the reaction is continued for 10 minutes, and the reaction is completed. Pour all the liquid in the three-neck flask into the prepared beaker and let it stand until it is consistent with room temperature and crystals appear. Filter, wash with anhydrous methanol, dry at 60° C. for 8 hours, and weigh to obtain 30.6 g of ethylenediamine dinitrate, with a yield of 79.8%. The mother liquor filtered in the above steps was collected and replaced with 80 mL of solvent to repeat the above steps to obtain 30.9 g of ethylenediamine dinitrate with a yield of 80.6%.

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Abstract

The invention discloses a preparation method of ethylenediamine dinitrate and belongs to the technical field of explosive production. The preparation method comprises the following steps of: dissolving ethylenediamine in a mixed solvent of methanol and water in a volume ratio of 3: 1; dropwise adding concentrated nitric acid to perform reaction, making an obtained mixed solution stand still afterdropwise adding the concentrated nitric acid, performing filtering, washing and drying. The prepared ethylenediamine dinitrate is high in yield, good in crystal form and high in purity; mother liquorcan be recycled; and the preparation method is simple in technological process, convenient to operate, is performed under mild conditions, is easy in large-scale preparation and is environmentally friendly.

Description

technical field [0001] The invention belongs to the technical field of explosive production, and in particular relates to a simplified preparation method of ethylenediamine dinitrate. Background technique [0002] Ethylenediamine dinitrate is a stable elemental explosive, easily soluble in water, insoluble in organic phase, does not decompose at 270°C, and does not explode at 360°C. It can be used as a component of press-packed or cast-packed high-energy explosives, especially as a eutectic component in eutectic intermolecular explosives, and acts as a combustible agent. At the same time, it has excellent properties such as good oxygen balance, high energy, low combustion flame temperature, less solid residue, large gas production, and non-toxic and non-corrosive combustion products. As an energetic material with great development potential, ethylenediamine dinitrate has a good application prospect. [0003] In the early stage of the preparation of ethylenediamine dinitrat...

Claims

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Application Information

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IPC IPC(8): C07C209/00C07C211/10C07C209/82
CPCC07C209/00C07C209/82C07B2200/13C07C211/10
Inventor 张琳兰林朱顺官李燕牟景艳易镇鑫刘庆安曹亚清任刚
Owner NANJING UNIV OF SCI & TECH
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