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Preparation method for hexogon

A technology of nitrolysis and time control, which is applied to the improvement of the production method of nitrolysis by direct nitrification method. The field of production of dermine by direct nitration method can solve the problems of backward technology, high production cost, and large consumption of nitric acid, etc., and achieve Effect of high purity and improved yield

Inactive Publication Date: 2009-12-09
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 relatively 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 There has been no major change for decades, and the equipment is outdated.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] Add 66mL 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 10°C, and gradually and evenly add urotropine to the four-necked In the flask, and control the nitrification temperature at 10-15 ° C, add all 10 g of urotropine in 12 minutes. After the feeding is completed, add the remaining 4mL of concentrated nitric acid to make the total amount of concentrated nitric acid 70mL, and continue to stir and keep warm for 20min at a temperature of 10-15°C. After the reaction is completed, the reaction liquid is dropped into another 500mL four-necked flask equipped with a stirrer and a thermometer, and an equivalent amount of water is added dropwise at the same time to carry out oxidation crystallization. Cool the oxidized and crystallized material to below 35°C, pour it into a beaker filled with 300mL of ice water, crystallize, filter, ...

Embodiment 2

[0020] Add 68mL 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 10°C, and gradually and evenly add urotropine to the four-necked In the flask, and control the nitrification temperature at 10-15°C, add all 11g of urotropine in 15 minutes. After the feeding is complete, add the remaining 5mL of concentrated nitric acid to make the total amount of concentrated nitric acid 73mL, and continue to stir and keep warm for 25min at a temperature of 10-15°C. After the reaction is completed, the reaction liquid is dropped into another 500mL four-necked flask equipped with a stirrer and a thermometer, and an equivalent amount of water is added dropwise at the same time to carry out oxidation crystallization. Cool the oxidized and crystallized material to below 35°C, pour it into a beaker filled with 300mL of ice water, crystallize, filter, and ...

Embodiment 3

[0022] Add 69 mL of concentrated nitric acid to a 500 mL 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, add urotropine gradually and evenly into the four-neck flask, and control the nitrification temperature at 10-15°C, and add all 12g of urotropine in 14 minutes. After the feeding is completed, add the remaining 6mL of concentrated nitric acid to make the total amount of concentrated nitric acid 75mL, and continue to stir and keep warm for 23min at a temperature of 10-15°C. After the reaction is completed, the reaction liquid is dropped into another 500mL four-necked flask equipped with a stirrer and a thermometer, and an equivalent amount of water is added dropwise at the same time to carry out oxidation crystallization. The oxidized and crystallized material was cooled to below 35°C, poured into a beaker filled with 300mL of ice water, crystallized, filtered...

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Abstract

The present invention relates to a method for producing hexocyanine by utilizing a direct nitrification method, which is improved on the basis of an existing direct nitrification method production process, so that concentrated nitric acid is reacted with urotropine in stages, and Lotropine is added to 90-95% by weight of concentrated nitric acid for reaction, and then the remaining 5-10% by weight of concentrated nitric acid is added for reaction. In the present invention, by changing the feeding mode of the reaction materials, the concentrated nitric acid is added in two steps, so that the yield of the hexogen is significantly improved, from the original 78.4% to more than 81.7%.

Description

technical field [0001] The invention relates to a method for preparing dersogen, in particular to a method for producing dersogen by using a direct nitrolysis method. Specifically, the present invention is an improvement on the direct nitrolysis method for producing rysogen. 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 1922, Hertz first confirmed that it was a valuable explosive, and successfully nitrated urotropine 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 RDX in industry ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/04
Inventor 李永祥张巧玲王建龙曹端林郑志花
Owner ZHONGBEI UNIV