CN109096286A - A kind of CL-20 and 1-AMTN cocrystallized explosive and preparation method thereof - Google Patents
A kind of CL-20 and 1-AMTN cocrystallized explosive and preparation method thereof Download PDFInfo
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- CN109096286A CN109096286A CN201810808919.1A CN201810808919A CN109096286A CN 109096286 A CN109096286 A CN 109096286A CN 201810808919 A CN201810808919 A CN 201810808919A CN 109096286 A CN109096286 A CN 109096286A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains four or more hetero rings
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B25/00—Compositions containing a nitrated organic compound
- C06B25/36—Compositions containing a nitrated organic compound the compound being a nitroparaffin
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
- C06D5/00—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
- C06D5/06—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets by reaction of two or more solids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D249/00—Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms
- C07D249/02—Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms not condensed with other rings
- C07D249/04—1,2,3-Triazoles; Hydrogenated 1,2,3-triazoles
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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- Nitrogen Condensed Heterocyclic Rings (AREA)
Abstract
The present invention relates to a kind of CL-20 and 1-AMTN cocrystallized explosive and preparation method thereof, specifically related to Hexanitrohexaazaisowurtzitane (CL-20) and 1- amino -3- methyl-1,2,3- triazole nitrate (1-AMTN) cocrystallized explosive and preparation method thereof, belongs to energetic material field.The present invention is prepared for CL-20/1-AMTN cocrystallized explosive using CL-20 and 1-AMTN as raw material, using solvent evaporation method.CL-20/1-AMTN cocrystallized explosive impact sensitivity prepared by the present invention is greatly lowered compared with CL-20, greatly improves its security performance.Compared with 1-AMTN, crystalline density, explosion velocity are significantly increased the cocrystallized explosive, show good detonation property.Preparation condition of the invention is mild, simple process, is convenient for operation.The cocrystallized explosive is a kind of novel low sense explosive of high energy, can be used for manufacturing low rapid wear ammunition, there is good application prospect.
Description
Technical field
The present invention relates to a kind of CL-20 and 1-AMTN cocrystallized explosive and preparation method thereof, and in particular to arrives six nitrogen of hexanitro
Miscellaneous different 5 hereby alkane (CL-20) and 1- amino -3- methyl-1,2,3- triazole nitrate (1-AMTN) cocrystallized explosive and its preparation sides
Method belongs to energetic material field.
Background technique
Hexanitrohexaazaisowurtzitane (HNIW or CL-20) density is 2.04g/cm3, theoretical explosion velocity is 9500m/s,
Detonation pressure is 43GPa, is the highest single chmical compound explosive of energy applied so far, but its impact sensitivity is 4J, friction sensitivity is
48N, sensitivity are in a higher level.Modern increasingly serious battlefield surroundings, propose the performance of weapons and ammunitions higher
Requirement, wherein security performance is the most important thing, develops the low sense energetic material of high energy and has become current research emphasis.Institute
With the emphasis of high explosive CL-20 application study first is that drop sense research.
Traditional drop sensing method such as recrystallizes, high molecular material cladding due to cannot change explosive molecules structure and
Composition, drop sense effect are often less obvious.Cocrystallized explosive is that two or more explosive molecules are passed through intermolecular interaction
The microcosmic combination of power forms the multicomponent molecular crystal with specific structure and performance in same lattice.Eutectic technology is as one
The new explosive modification approach of kind, can effectively adjust the performance of explosive, such as sensitivity, density, thermal decomposition performance, explosion property
Deng.In order to reduce CL-20 sensitivity, using eutectic technology, CL-20 and 1-AMTN cocrystallized explosive are prepared, CL-20 sensitivity is reduced, mentions
Its high security performance.Currently, cocrystallized explosive in relation to CL-20 and 1-AMTN and preparation method thereof is temporarily without open source literature data report
Road.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, a kind of Hexanitrohexaazaisowurtzitane (CL-20) and 1- ammonia are provided
Base -3- methyl-1,2,3- triazole nitrate (1-AMTN) cocrystallized explosives and preparation method thereof, solves CL-20 sensitivity height etc. and asks
Topic provides a kind of new method for energetic material is modified, and also the synthesis for the low sense energetic material of high energy provides a new plan
Slightly.
In order to solve the above technical problems, the present invention is achieved through the following technical solutions.
A kind of CL-20 and 1-AMTN cocrystallized explosive, CL-20 molecule and 1-AMTN molecule are with molar ratio in the cocrystallized explosive
For 1:1, passing through N-O ..., H intermolecular interaction is formed.The molecular formula of eutectic is C9H13N17O15, belong to rhombic system, Pca21
Space group, crystalline density are up to 1.795g/cm3.Its molecular structure is as shown in Figure 2.
A kind of preparation method of CL-20 and 1-AMTN cocrystallized explosive, the specific steps are as follows:
Step 1: the preparation of CL-20 and 1-AMTN saturated solution
In the case where temperature is 20-50 DEG C, enough CL-20 are dissolved in the mixed solvent, dissolves, CL-20 saturation is obtained by filtration
Solution；Enough 1-AMTN are added in CL-20 saturated solution again dissolve, be obtained by filtration CL-20 and 1-AMTN saturation it is molten
Liquid；
Step 2: the preparation of CL-20 and 1-AMTN cocrystallized explosive
CL-20 made from step 1 and 1-AMTN saturated solution are transferred in container, the container is then statically placed in perseverance
In incubator, slow solvent flashing, slowly there is Crystallization at a temperature of 20-50 DEG C, is filtered, dries to obtain CL-20/1-AMTN
Cocrystallized explosive.
Mixed solvent described in step 1 is ethyl alcohol/ethyl acetate, ethanol/acetone, ethanol/acetonitrile, methanol/acetic acid second
Ester, methanol/acetone or methanol/acetonitrile mixed solvent.
The volume ratio of two kinds of solvents of in the mixed solvent is 1:1.
Beneficial effect
1, CL-20/1-AMTN cocrystallized explosive prepared by the present invention hits sense (impact sensitivity 48%) and significantly drops compared with CL-20
It is low, greatly improve its security performance.
2, compared with 1-AMTN, crystalline density significantly improves CL-20/1-AMTN cocrystallized explosive prepared by the present invention
(10.1%)；Explosion velocity improves 8%, shows good detonation property.
3, preparation condition of the invention is mild, simple process, is convenient for operation.
Detailed description of the invention
Fig. 1 is the preparation flow figure of CL-20/1-AMTN cocrystallized explosive of the present invention；
Fig. 2 is CL-20/1-AMTN cocrystallized explosive molecular structure.
Specific embodiment
It is clear in order to be more clear the objectives, technical solutions, and advantages of the present invention, with reference to the accompanying drawings and embodiments,
The present invention will be described in further detail.It should be appreciated that specific embodiment described herein is used only for explaining this hair
It is bright, it is not intended to limit the present invention.
Fig. 1 shows gone out Hexanitrohexaazaisowurtzitane of the present invention and 1- amino -3- methyl-1,2,3- triazole nitric acid
The preparation flow figure of salt (CL-20/1-AMTN) cocrystallized explosive.The preparation process of CL-20/1-AMTN cocrystallized explosive is as follows:
(1) preparation of CL-20 and 1-AMTN solution
Enough CL-20 are dissolved in a certain proportion of in the mixed solvent, dissolution, mistake at being 20-50 DEG C in temperature
Filter obtains CL-20 saturated solution；Enough 1-AMTN are added in CL-20 saturated solution dissolve, be obtained by filtration CL-20 with
1-AMTN saturated solution.Mixed solvent can be ethyl alcohol/ethyl acetate, ethanol/acetone, ethanol/acetonitrile, methanol/acetic acid second
Ester, methanol/acetone, methanol/acetonitrile mixed solvent, the volume ratio 1:1 of mixed solvent.
(2) preparation of CL-20 and 1-AMTN cocrystallized explosive
CL-20/1-AMTN solution is transferred in beaker, then the beaker is statically placed in insulating box, in certain temperature
Solvent is slowly shot down, filtered, dry to obtain CL-20/1-AMTN cocrystallized explosive.Calorstat temperature is 20-50 DEG C when crystallization,
Convenient for crystal generation and grow up.
Fig. 2 indicates that CL-20/1-AMTN cocrystallized explosive passes through the molecular structure of single crystal diffraction (SXRD) confirmation.From SXRD
Analyze known to result: CL-20 molecule and 1-AMTN molecule are 1:1 with molar ratio in the cocrystallized explosive, the molecules such as H that pass through N-O ...
Between interact formed.The molecular formula of eutectic is C9H13N17O15, belong to rhombic system, Pca21Space group, crystalline density are high
Up to 1.795g/cm3, compared with 1-AMTN (1.63 g/cm3) significantly improve 10.1%.
Table 1 is the explosion property of CL-20/1-AMTN cocrystallized explosive of the present invention.CL-20/1-AMTN as can be seen from the table
The explosion velocity of cocrystallized explosive has been respectively increased 8% compared with 1-AMTN, shows good detonation property.From table 1 it can also be seen that by altogether
Brilliant mode can effectively adjust the physical and chemical performance of explosive.
Table 2 is the impact sensitivity of CL-20/1-AMTN cocrystallized explosive of the present invention.As shown in Table 2, the CL-20 of high sensitivity
Eutectic is formed by intermolecular force with the 1-AMTN of low sensitivity, significantly reduces the impact sensitivity of pure component CL-20, significantly
Improve its security performance.
The explosion property of 1 CL-20/1-AMTN cocrystallized explosive of table and component sample
The impact sensitivity of 2 CL-20/1-AMTN cocrystallized explosive of table and component sample
The specific embodiment of CL-20/1-AMTN cocrystallized explosive preparation of the present invention is explained in detail below.
Embodiment 1
At 20 DEG C, 10ml ethyl alcohol and 10ml ethyl acetate are added in there-necked flask, enough CL-20 are added, unlatching is stirred
It mixes, the CL-20 solution for dissolving, filtering to be saturated.Then enough 1-AMTN, stirring, dissolution, mistake are added in the above solution
Filter CL-20 and 1-AMTN saturated solution.CL-20 and 1-AMTN saturated solution are transferred in beaker, in 20 DEG C of constant temperature
Slow solvent flashing, precipitates crystal in case, filters, dries to obtain CL-20/1-AMTN cocrystallized explosive.
Embodiment 2
At 30 DEG C, 20ml ethyl alcohol and 20ml acetone are added in there-necked flask, enough CL-20 are added, opens stirring,
The CL-20 solution for dissolving, filtering to be saturated.Then enough 1-AMTN are added in the above solution, stirs, dissolve, filter
The saturated solution of CL-20 and 1-AMTN.CL-20 and 1-AMTN saturated solution are transferred in beaker, in 30 DEG C of insulating box
Slow solvent flashing, precipitates crystal, and filters, dries to obtain CL-20/1-AMTN cocrystallized explosive.
Embodiment 3
At 40 DEG C, 50ml ethyl alcohol and 50ml acetonitrile are added in there-necked flask, enough CL-20 are added, opens stirring,
The CL-20 solution for dissolving, filtering to be saturated.Then enough 1-AMTN are added in the above solution, stirs, dissolve, filter
The saturated solution of CL-20 and 1-AMTN.CL-20 and 1-AMTN saturated solution are transferred in beaker, in 50 DEG C of insulating box
Slow solvent flashing, precipitates crystal, and filters, dries to obtain CL-20/1-AMTN cocrystallized explosive.
Embodiment 4
At 50 DEG C, 50ml methanol and 50ml ethyl acetate are added in there-necked flask, enough CL-20 are added, unlatching is stirred
It mixes, the CL-20 solution for dissolving, filtering to be saturated.Then enough 1-AMTN, stirring, dissolution, mistake are added in the above solution
Filter CL-20 and 1-AMTN saturated solution.CL-20 and 1-AMTN saturated solution are transferred in beaker, in 50 DEG C of constant temperature
Slow solvent flashing, precipitates crystal in case, filters, dries to obtain CL-20/1-AMTN cocrystallized explosive.
Embodiment 5
At 25 DEG C, 20ml methanol and 20ml acetonitrile are added in there-necked flask, enough CL-20 are added, opens stirring,
The CL-20 solution for dissolving, filtering to be saturated.Then enough 1-AMTN are added in the above solution, stirs, dissolve, filter
The saturated solution of CL-20 and 1-AMTN.CL-20 and 1-AMTN saturated solution are transferred in beaker, in 25 DEG C of insulating box
Slow solvent flashing, precipitates crystal, and filters, dries to obtain CL-20/1-AMTN cocrystallized explosive.
Embodiment 6
At 35 DEG C, 15ml methanol and 15ml acetone are added in there-necked flask, enough CL-20 are added, opens stirring,
The CL-20 solution for dissolving, filtering to be saturated.Then enough 1-AMTN are added in the above solution, stirs, dissolve, filter
The saturated solution of CL-20 and 1-AMTN.CL-20 and 1-AMTN saturated solution are transferred in beaker, in 50 DEG C of insulating box
Slow solvent flashing, precipitates crystal, and filters, dries to obtain CL-20/1-AMTN cocrystallized explosive.
Above-described specific descriptions have carried out further specifically the purpose of invention, technical scheme and beneficial effects
It is bright, it should be understood that the above is only a specific embodiment of the present invention, the protection being not intended to limit the present invention
Range, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in this
Within the protection scope of invention.
Claims (4)
1. a kind of CL-20 and 1-AMTN cocrystallized explosive, it is characterised in that: CL-20 molecule and 1-AMTN molecule in the cocrystallized explosive
It is 1:1 with molar ratio, passing through N-O ..., H intermolecular interaction is formed；The molecular formula of eutectic is C9H13N17O15, belong to orthorhombic
System, Pca21Space group, crystalline density are up to 1.795g/cm3；Its molecular structure is as shown in Figure 2.
2. the preparation method of a kind of CL-20 and 1-AMTN cocrystallized explosive, it is characterised in that: specific step is as follows:
Step 1: the preparation of CL-20 and 1-AMTN saturated solution；
In the case where temperature is 20-50 DEG C, enough CL-20 are dissolved in the mixed solvent, dissolves, CL-20 saturated solution is obtained by filtration；
Enough 1-AMTN are added in CL-20 saturated solution again and dissolves, CL-20 and 1-AMTN saturated solution is obtained by filtration；
Step 2: the preparation of CL-20 and 1-AMTN cocrystallized explosive；
CL-20 made from step 1 and 1-AMTN saturated solution are transferred in container, the container is then statically placed in insulating box
In, slow solvent flashing, slowly there is Crystallization at a temperature of 20-50 DEG C, filtered, dry CL-20/1-AMTN eutectic is fried
Medicine.
3. a kind of preparation method of CL-20 and 1-AMTN cocrystallized explosive as claimed in claim 2, it is characterised in that: step 1
Described in mixed solvent be ethyl alcohol/ethyl acetate, ethanol/acetone, ethanol/acetonitrile, methanol/ethyl acetate, methanol/acetone or first
Alcohol/acetonitrile mixed solvent.
4. a kind of preparation method of CL-20 and 1-AMTN cocrystallized explosive as claimed in claim 3, it is characterised in that: described mixed
The volume ratio of two kinds of solvents is 1:1 in bonding solvent.
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| CN201810808919.1A CN109096286A (en) | 2018-07-23 | 2018-07-23 | A kind of CL-20 and 1-AMTN cocrystallized explosive and preparation method thereof |
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| CN201810808919.1A CN109096286A (en) | 2018-07-23 | 2018-07-23 | A kind of CL-20 and 1-AMTN cocrystallized explosive and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111056885A (en) * | 2019-11-12 | 2020-04-24 | 北京理工大学 | DAF and DNP eutectic explosive and preparation method thereof |
| CN113912614A (en) * | 2021-11-19 | 2022-01-11 | 中国工程物理研究院化工材料研究所 | CL-20 and 1,3-DNP polymorphic supermolecular explosive and preparation method thereof |
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| US7645883B1 (en) * | 2006-03-30 | 2010-01-12 | The United States Of America As Represented By The Secretary Of The Air Force | Energetic ionic liquids |
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2018
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| US7645883B1 (en) * | 2006-03-30 | 2010-01-12 | The United States Of America As Represented By The Secretary Of The Air Force | Energetic ionic liquids |
| CN102992925A (en) * | 2012-11-01 | 2013-03-27 | 中国工程物理研究院化工材料研究所 | Method for preparing BTF-HNIW (benzotrifuroxan- hexanitrohexaazaisowurtzitane) eutectic explosive |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111056885A (en) * | 2019-11-12 | 2020-04-24 | 北京理工大学 | DAF and DNP eutectic explosive and preparation method thereof |
| CN113912614A (en) * | 2021-11-19 | 2022-01-11 | 中国工程物理研究院化工材料研究所 | CL-20 and 1,3-DNP polymorphic supermolecular explosive and preparation method thereof |
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Application publication date: 20181228 |