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Method for producing hexogen

A production method, the technology of RDX, which is applied in the field of improvement of the production method of RDX preparation by direct nitrification, can solve the problems of backward technology, high production cost, obsolete equipment, etc., and achieve the effect of high purity and improved yield

Inactive Publication Date: 2011-04-13
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The advantage of the direct nitrification method is that acetic anhydride is not consumed, but the disadvantage is that the theoretical yield is only 50% of that of the acetic anhydride method, and a large amount of nitric acid is consumed
[0010] Our country is rich in nitric acid, so the only few RDX production lines currently adopt the direct nitrification production process. The process equipment and process conditions are the technology of the former Soviet Union in the 1950s and 1960s. There has been no major change for decades, and the equipment is outdated. The technology is backward, the yield is only about 74%, and the annual production capacity is about 10,000 tons, which is less than one-twentieth of that of the United States.
At the same time, the production cost of Hexogen is very high, and the price is about 4 times that of TNT

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] After drying the urotropine, grind it to 70 mesh with a mortar and set it aside.

[0019] Add 75ml of concentrated nitric acid to a 500ml four-necked flask equipped with a stirrer, a thermometer and an addition funnel, place the four-necked flask in an ice-water bath, start stirring, cool to 13°C, and gradually uniformize the mixture through the two inlets of the four-necked flask Add 12g of refined urotropine, control the nitrification temperature at 12°C, and add all urotropine within 12 minutes. After the addition, continue to stir and keep warm at 15°C for 25min. Then the reaction solution was poured into a beaker filled with 300ml of ice water, stirred sufficiently to crystallize RDX, filtered and dried to obtain 13.54 g of RDX product with a yield of 85.4% and a melting point of 201°C.

Embodiment 2

[0021] After drying the urotropine, grind it to 60 mesh with a mortar and set it aside.

[0022] Add 70ml of concentrated nitric acid into a 500ml four-necked flask equipped with a stirrer, a thermometer and an addition funnel, place the four-necked flask in an ice-water bath, start stirring, cool to 12°C, and gradually uniformize the mixture through the two inlets of the four-necked flask Add 10 g of refined urotropine, control the nitrification temperature at 10°C, and add all urotropine within 15 minutes. After the addition, the stirring was continued at 12°C for 20 minutes. Then the reaction solution was poured into a beaker filled with 300ml of ice water, stirred sufficiently to crystallize dersogen, filtered, and dried to obtain 13.51 g of hexogen product with a yield of 85.2% and a melting point of 200°C.

Embodiment 3

[0024] After drying the urotropine, grind it to 80 mesh with a mortar and set it aside.

[0025] Add 73ml of concentrated nitric acid to a 500ml four-necked flask equipped with a stirrer, a thermometer and an addition funnel, place the four-necked flask in an ice-water bath, and start stirring. Cool to 10°C, gradually and uniformly add 11g of refined urotropine through the two inlets of the four-necked flask, control the nitrification temperature at 13°C, and add all the urotropine within 13 minutes. After the addition, the stirring was continued at 14°C for 30 minutes. Then the reaction solution was poured into a beaker filled with 300ml of ice water, stirred thoroughly to crystallize dersogen, filtered, and dried to obtain 13.64 g of hesogen product, with a yield of 86.0% and a melting point of 202°C.

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Abstract

The invention discloses a method for producing hexogen. In the method, urotropine and concentrated nitric acid are taken as reaction materials, and the weight ratio of the urotropine to the concentrated nitric acid is 1:9-11. On the basis of a conventional direct-nitrolysis production process, the method comprises the following steps of: simultaneously and uniformly feeding the raw material urotropine with the fineness of 60 to 80 meshes into a device containing the concentrated nitric acid from at least two feed inlets, and reacting the urotropine with the concentrated nitric acid under the condition of 10 to 15 DEG C to prepare the hexogen. The method remarkably increases the yield of the hexogen from original 78.4 percent to over 85.2 percent only by changing the feeding way and fineness of the reaction material without increasing any investment.

Description

technical field [0001] The present invention relates to a production method of RDX, in particular to a method for producing RDX by direct nitrolysis method, specifically, the present invention is an improvement on the production method of RDX by direct nitrolysis method. Background technique [0002] RDX, whose chemical name is cyclotrimethylenetrinitramine, or RDX for short, was produced by Henning in the synthesis of medicine in 1899. In 1921, Hertz first confirmed that it was a valuable explosive, and successfully prepared it by nitrating hexamethamine with nitric acid at low temperature. Due to its good explosive performance and rich sources of raw materials, RDX is increasingly important in the field of explosives. During and after the Second World War, many countries conducted research on the production method of Hexogen. Now Hexogen has developed into one of the main charges of modern weapons and ammunition after TNT. [0003] At present, the production methods of R...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/06
Inventor 李永祥郑志花徐春彦王建龙曹端林王艳红
Owner ZHONGBEI UNIV
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