Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for preparing CL-20 through two-step method

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

Active Publication Date: 2019-08-13
ZHONGBEI UNIV
View PDF5 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing CL-20 through two-step method
  • Method for preparing CL-20 through two-step method
  • Method for preparing CL-20 through two-step method

Examples

Experimental program
Comparison scheme
Effect test

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 100mL four-necked bottle and lower the temperature to below 10°C, and prepare the prepared ammonium nitrate-nitric acid solution Slowly add the 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 solution at 0°C for 8 hours, then pour it into 10...

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 100mL four-necked bottle and lower the temperature to below 10°C, and prepare the 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 nitration solution; react the nitration solution at 30°C for 4h, the...

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 100mL four-necked bottle and lower the temperature to below 10°C, and prepare the ammonium nitrate- Slowly add nitric acid solution into acetic anhydride, then add 3.0g HSIW in batches and at the same time add 15.0g acetic acid to the system to obtain a nitration solution; react the nitration solution at 30°C for 4h, then p...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for preparing CL-20 through a two-step method, and belongs to the technical field of energetic materials. The method includes the steps of firstly, adding a sulfamatewater solution and a 40% glyoxal water solution into a container, conducting the condensation reaction at a certain temperature, and then conducting filtering and drying to obtain white powder HSIW; secondly, conducting nitration reaction on the HSIW obtained in the first step through a nitrating agent, pouring nitration liquid into icy water, and conducting filtering, washing and drying to obtaina product containing CL-20, wherein the yield of the CL-20 can reach 1.78% at most. By means of the method, sulfamate replaces benzylamine, and the raw material cost is reduced; no catalytic hydrogenolysis is needed, and cost is reduced; the preparing process of the CL-20 is simplified, and the synthesis cycle of the CL-20 is shortened.

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, the 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 synthesize...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com