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Method for preparing cl-20 in two steps

A CL-20 and one-step technology, which is applied in the field of two-step preparation of CL-20, can solve the problems of long cycle, complex reaction route, and poor atom economy, and achieve the effects of shortening the synthesis cycle, simplifying the preparation process, and reducing costs

Active Publication Date: 2022-01-04
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Nevertheless, there are still some problems in this process: (1) atom economy is poor, only amino group is the effective group of benzylamine used, and benzyl occupies a large proportion of benzylamine as a leaving group; (2) the reaction route is complicated, The long cycle is essentially due to the fact that the benzyl group on HBIW is difficult to be nitrated directly and requires catalytic hydrogenolysis; (3) The debenzylation process requires the use of expensive metal catalysts, resulting in high production costs for CL-20

Method used

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  • Method for preparing cl-20 in two steps
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  • Method for preparing cl-20 in two steps

Examples

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Embodiment 1

[0046] A two-step method for preparing CL-20, comprising the following two steps:

[0047] 1) Dissolve 5.68g of ammonium sulfamate (50mmol) in 5.7mL of deionized water, add the solution to a 100mL four-neck flask, then add 2.9mL of 40% glyoxal (25mmol) aqueous solution at room temperature, and stir under 20 React at ℃ for 24 hours, filter, and dry to obtain 0.93 g of white powder HSIW; a sufficient amount of HSIW can be obtained by repeating the above steps.

[0048] 2) Dissolve 0.5g of ammonium nitrate in 5.0g of fuming nitric acid to prepare an ammonium nitrate-nitric acid solution; add 10.0g of acetic anhydride to a 100 mL four-necked bottle and lower the temperature to below 10°C, and prepare the prepared ammonium nitrate- Slowly add nitric acid solution into acetic anhydride, then add 3.0g HSIW in batches and at the same time add 10.0g acetic acid to the system to obtain a nitrating solution; react the nitrating solution at 0°C for 8 hours, pour it into 10 times the volum...

Embodiment 2

[0050] A two-step method for preparing CL-20, comprising the following two steps:

[0051] 1) Dissolve 7.10 g of ammonium sulfamate (62.5 mmol) in 5.7 mL of deionized water, add the solution to a 100 mL four-neck flask, then add 2.9 mL of 40% glyoxal (25 mmol) aqueous solution at room temperature, and place under stirring React at 10°C for 48 hours, filter, and dry to obtain 1.07 g of white powder, which is designated as HSIW; a sufficient amount of HSIW can be prepared by repeating the above steps.

[0052] 2) Dissolve 0.5g of ammonium nitrate in 5.0g of fuming nitric acid to prepare an ammonium nitrate-nitric acid solution; add 10.0g of acetic anhydride to a 100 mL four-necked bottle and lower the temperature to below 10°C, and prepare the ammonium nitrate prepared in advance -Slowly add nitric acid solution into acetic anhydride, then add 3.0g HSIW in batches and at the same time add 10.0g acetic acid to the system to obtain a nitration solution; react the nitration solutio...

Embodiment 3

[0054] A two-step method for preparing CL-20, comprising the following two steps:

[0055] 1) Dissolve 8.52g of ammonium sulfamate (75mmol) in 5.7mL of deionized water, add the solution to a 100mL four-neck flask, then add 2.9mL of 40% glyoxal (25mmol) aqueous solution at room temperature, and place under stirring in - React at 20°C for 24 hours, filter, and dry to obtain 1.03 g of white powder, which is designated as HSIW; a sufficient amount of HSIW can be prepared by repeating the above steps.

[0056] 2) Dissolve 0.5g of ammonium nitrate in 5.0g of fuming nitric acid to prepare an ammonium nitrate-nitric acid solution; add 10.0g of acetic anhydride to a 100 mL four-necked bottle and lower the temperature to below 10°C, and prepare the ammonium nitrate prepared in advance -Slowly add nitric acid solution to acetic anhydride, then add 3.0g HSIW in batches and add 15.0g acetic acid to the system at the same time to obtain a nitration solution; react the nitration solution at ...

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Abstract

The invention is a two-step method for preparing CL‑20, which belongs to the technical field of energetic materials. The method of the present invention includes: 1) adding aqueous sulfamic acid salt solution and 40% glyoxal aqueous solution to a container, carrying out condensation reaction at a certain temperature, then filtering and drying to obtain white powder HSIW; 2) using a nitrating agent for step 1 ) The obtained HSIW was subjected to nitration reaction, and then the nitration solution was poured into ice water, filtered, washed, and dried, and the product containing CL‑20 was obtained, and the yield of CL‑20 was as high as 1.78%. The method of the invention replaces benzylamine with sulfamate, which reduces the cost of raw materials; does not require catalytic hydrogenolysis, reduces the cost; simplifies the preparation process of CL-20, and shortens the synthesis period of CL-20.

Description

technical field [0001] The invention belongs to the technical field of energetic materials, in particular to a two-step method for preparing CL-20. Background technique [0002] CL-20, chemical name 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetracyclo[5.5.0.0 5 ,9 .0 3,11 ] Dodecane, referred to as hexanitrohexaazaisowurtzitane, English name is 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetracyclo[5.5.0.0 5,9 .0 3,11 ]dodecane, the molecular formula is C 6 h 6 N 12 o 12 , the structural formula is: The relative molecular mass is 438.28, white solid, and the crystal density of its ε-crystal form is 2.04g·cm -1 , the detonation speed can reach 9.5~9.6km·s -1 , the explosion pressure can reach 42~43GPa, and the standard enthalpy of formation is 980kJ·kg -1 , is currently reported the highest comprehensive performance single-substance explosives, can be used in solid propellants, weapons and ammunition. [0003] The preparation of CL-20 was first synthesized in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 王建龙李云路薛梅陈丽珍曹端林李永祥
Owner ZHONGBEI UNIV