CN112358370A - CL-20 and NTO eutectic explosive and preparation method thereof - Google Patents
CL-20 and NTO eutectic explosive and preparation method thereof Download PDFInfo
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- CN112358370A CN112358370A CN202010991284.0A CN202010991284A CN112358370A CN 112358370 A CN112358370 A CN 112358370A CN 202010991284 A CN202010991284 A CN 202010991284A CN 112358370 A CN112358370 A CN 112358370A
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- NDYLCHGXSQOGMS-UHFFFAOYSA-N CL-20 Chemical compound [O-][N+](=O)N1C2N([N+]([O-])=O)C3N([N+](=O)[O-])C2N([N+]([O-])=O)C2N([N+]([O-])=O)C3N([N+]([O-])=O)C21 NDYLCHGXSQOGMS-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000002360 explosive Substances 0.000 title claims abstract description 58
- 230000005496 eutectics Effects 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000013078 crystal Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000012047 saturated solution Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 20
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 14
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 238000005474 detonation Methods 0.000 abstract description 12
- 230000008018 melting Effects 0.000 abstract description 9
- 238000002844 melting Methods 0.000 abstract description 9
- 239000011159 matrix material Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 150000002576 ketones Chemical class 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000000935 solvent evaporation Methods 0.000 abstract 1
- QJTIRVUEVSKJTK-UHFFFAOYSA-N 5-nitro-1,2-dihydro-1,2,4-triazol-3-one Chemical compound [O-][N+](=O)C1=NC(=O)NN1 QJTIRVUEVSKJTK-UHFFFAOYSA-N 0.000 description 69
- 238000001914 filtration Methods 0.000 description 24
- 238000003756 stirring Methods 0.000 description 12
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 9
- 238000001035 drying Methods 0.000 description 8
- 230000035945 sensitivity Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- XTFIVUDBNACUBN-UHFFFAOYSA-N 1,3,5-trinitro-1,3,5-triazinane Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)C1 XTFIVUDBNACUBN-UHFFFAOYSA-N 0.000 description 2
- MNYFLTUIJHCVIQ-UHFFFAOYSA-N 1-methyl-2,4,5-trinitroimidazole Chemical compound CN1C([N+]([O-])=O)=NC([N+]([O-])=O)=C1[N+]([O-])=O MNYFLTUIJHCVIQ-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- ZCRYIJDAHIGPDQ-UHFFFAOYSA-N 1,3,3-trinitroazetidine Chemical compound [O-][N+](=O)N1CC([N+]([O-])=O)([N+]([O-])=O)C1 ZCRYIJDAHIGPDQ-UHFFFAOYSA-N 0.000 description 1
- SPSSULHKWOKEEL-UHFFFAOYSA-N 2,4,6-trinitrotoluene Chemical compound CC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O SPSSULHKWOKEEL-UHFFFAOYSA-N 0.000 description 1
- CVYZVNVPQRKDLW-UHFFFAOYSA-N 2,4-dinitroanisole Chemical compound COC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O CVYZVNVPQRKDLW-UHFFFAOYSA-N 0.000 description 1
- KIJCKNUNZABDBC-UHFFFAOYSA-N 3,4-dinitro-1,2,5-oxadiazole Chemical compound [O-][N+](=O)C1=NON=C1[N+]([O-])=O KIJCKNUNZABDBC-UHFFFAOYSA-N 0.000 description 1
- VXMCBBMNFIAYQD-UHFFFAOYSA-N 4,5-dinitro-1h-pyrazole Chemical compound [O-][N+](=O)C=1C=NNC=1[N+]([O-])=O VXMCBBMNFIAYQD-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- JKFAIQOWCVVSKC-UHFFFAOYSA-N furazan Chemical compound C=1C=NON=1 JKFAIQOWCVVSKC-UHFFFAOYSA-N 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
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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
- C06B25/34—Compositions containing a nitrated organic compound the compound being a nitrated acyclic, alicyclic or heterocyclic amine
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0008—Compounding the ingredient
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Nitrogen Condensed Heterocyclic Rings (AREA)
Abstract
本发明涉及一种CL‑20与NTO共晶炸药及其制备方法，具体涉及六硝基六氮杂异伍兹烷(CL‑20)与3‑硝基‑1,2,4‑三唑‑5‑酮(NTO)共晶炸药及其制备方法，属于含能材料领域。本发明以CL‑20与NTO为原料，采用溶剂挥发法制备了CL‑20/NTO共晶炸药。本发明制备的CL‑20/NTO共晶炸药，熔点大大降低，更加适合作为熔铸基体炸药；晶体密度显著提高(6.1％)；爆速提高了9.7％，表现出良好的爆轰性能。本发明的制备条件温和、工艺简单、便于操作。该共晶炸药是一种新型的高能低感熔铸基体炸药，有较好的应用前景。
The invention relates to a CL-20 and NTO eutectic explosive and a preparation method thereof, in particular to hexanitrohexaazaisowurtzitane (CL-20) and 3-nitro-1,2,4-triazole-5 A ketone (NTO) eutectic explosive and a preparation method thereof belong to the field of energetic materials. The invention uses CL-20 and NTO as raw materials, and adopts a solvent evaporation method to prepare CL-20/NTO eutectic explosives. The CL-20/NTO eutectic explosive prepared by the invention has a greatly reduced melting point and is more suitable as a molten-cast matrix explosive; the crystal density is significantly increased (6.1%); the detonation speed is increased by 9.7%, showing good detonation performance. The preparation condition of the invention is mild, the process is simple, and the operation is convenient. The eutectic explosive is a new type of high-energy and low-sensitivity fused-cast matrix explosive, which has good application prospects.
Description
Technical Field
The invention relates to a hexanitrohexaazaisowurtzitane (CL-20) and 3-nitro-1, 2, 4-triazole-5-ketone (NTO) eutectic explosive and a preparation method thereof, belonging to the technical field of energetic materials.
Background
The existing fusion-cast matrix explosives have inherent defects, such as low charge density of 2,4, 6-trinitrotoluene (TNT), unsatisfactory detonation performance and easy oil leakage in long-term storage; 2, 4-Dinitroanisole (DNAN) has poor detonation performance; the melting point of 3, 4-dinitrofurazan-based furazan (DNTF) is too high, and the DNTF is volatile when a fused cast medicine is prepared; 1,3, 3-Trinitroazetidine (TNAZ) is too costly to be produced in large quantities; the synthetic route of 1-methyl-2, 4, 5-trinitroimidazole (MTNI) is complicated, and the cost is high. The traditional fusion-cast matrix explosive cannot meet the requirements of modern weapons on the performance of energetic materials. Therefore, the research on the preparation of the novel fusion-cast matrix explosive is not slow enough.
The eutectic technology is a new technology developed in recent years, is widely applied to the field of energetic materials, and can essentially and effectively improve the properties of the energetic materials, such as melting point, sensitivity, thermal stability, solubility, hygroscopicity and the like from a molecular level. The CL-20 explosive name hexanitrohexaazaisowurtzitane is a newly developed high explosive for military use. The explosion energy and mechanical sensitivity of the CL-20 explosive are higher than that of HMX, and the heat resistance is similar to that of RDX. NTO (chemical name is 3-nitro-1, 2, 4-triazole-5-ketone) is a high-energy low-sensitivity single-substance explosive with excellent performance, the crystal density is 1.93g/cm3, and the theoretical detonation velocity is 8670 m/s; the degree of friction sensitivity was 8% (3.92MPa, 90 ℃ swing angle), the characteristic drop height H50 was 102.3cm (5kg drop weight), and the degree of impact sensitivity was 16% (10kg drop weight, 25cm drop height). The NTO energy is close to that of hexogen, has higher thermal stability and chemical stability, has excellent X-ray and ultraviolet radiation resistance, and can be used as a insensitive coating agent of sensitive explosives. At present, there is no report on a literature disclosing a cocrystal explosive of hexanitrohexaazaisowurtzitane (CL-20) and 3-nitro-1, 2, 4-triazol-5-one (NTO) and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a CL-20 and NTO eutectic explosive and a preparation method thereof, wherein the crystal density of the eutectic explosive is obviously improved (6.1%); the detonation velocity is improved by 9.7 percent, and good detonation performance is shown.
In order to solve the technical problems, the invention is realized by the following technical scheme.
CL-20 and NTO eutectic explosive, wherein CL-20 molecules, NTO molecules and H in the eutectic explosive2The molar ratio of O molecules is 1:1: 1. The molecular formula of the eutectic is C5H8N8O6Belonging to the orthorhombic system, P212121Space group with crystal density up to 1.909g/cm3。
A preparation method of a CL-20 and NTO eutectic explosive comprises the following specific steps:
step one, preparation of CL-20 and NTO saturated solution
Dissolving sufficient CL-20 in a solvent at the temperature of 35-65 ℃, and dissolving and filtering to obtain a saturated CL-20 solution; adding sufficient NTO into the NTO saturated solution for dissolving and filtering to obtain CL-20 and NTO saturated solution;
step two, preparation of CL-20 and NTO eutectic explosive
And (3) transferring the CL-20 and NTO saturated solution prepared in the step one into a container, standing the container in a thermostat, slowly volatilizing the solvent at the temperature of 35-65 ℃, slowly forming crystals, filtering and drying to obtain the CL-20/NTO eutectic explosive.
In the step one, the solvent is one or a mixture of industrial ethyl acetate, industrial isopropanol and industrial dimethyl sulfoxide.
Advantageous effects
1. Compared with CL-20, the CL-20/NTO eutectic explosive prepared by the invention has greatly reduced DSC melting peak and is more suitable for being used as a fusion casting matrix explosive.
2. Compared with NTO, the crystal density of the CL-20/NTO eutectic explosive prepared by the invention is obviously improved (6.1%); the detonation velocity is improved by 9.7 percent, and good detonation performance is shown.
3. The preparation method has the advantages of mild preparation conditions, simple process and convenient operation.
Drawings
FIG. 1 is a flow chart of the preparation of the CL-20/NTO eutectic explosive of the invention.
FIG. 2 is a CL-20/NTO eutectic explosive through infrared (FT-IR) diagram
FIG. 3 is a powder diffraction graph of CL-20/NTO eutectic explosive passing PXRD test
FIG. 4 is an SEM image of CL-20 (non-transcrystallized, a), NTO, and CL-20/NTO eutectic (c, d, e)
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly apparent, the present invention will be described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
FIG. 1 shows a preparation flow chart of a hexa-3, 4-diaminofurazan and 3, 4-dinitropyrazole (CL-20/NTO) eutectic explosive. The preparation process of the CL-20/NTO eutectic explosive is as follows:
(1) preparation of CL-20 and NTO solution
Dissolving sufficient CL-20 in a solvent, dissolving at 35-65 ℃, and filtering to obtain a saturated CL-20 solution; adding sufficient NTO into the saturated CL-20 solution, and filtering to obtain saturated CL-20 and NTO solution.
(2) Preparation of CL-20 and NTO eutectic explosive
Transferring the CL-20/NTO solution into a beaker, standing the beaker in a thermostat, slowly volatilizing the solvent at a certain temperature, filtering and drying to obtain the CL-20/NTO eutectic explosive.
FIGS. 2, 3 and 4 show the molecular structure diagrams of CL-20/NTO eutectic explosive confirmed by FT-IR and PXRD tests. From the analysis results of the above figures, it can be seen that: CL-20 molecules, NTO molecules and H in the eutectic explosive2The molar ratio of O molecules is 1:1: 1. The molecular formula of the eutectic is C5H8N8O6Belonging to the orthorhombic system, P212121Space group with crystal density up to 1.909g/cm3And the improvement is remarkably higher than NTO (6.1%).
Table 1 shows the explosive properties of the CL-20/NTO eutectic explosive of the invention. The table shows that the detonation velocity of the CL-20/NTO eutectic explosive is respectively improved by 9.7 percent compared with NTO, and the CL-20/NTO eutectic explosive shows good detonation performance. From table 1, it can also be seen that the physicochemical properties of the explosive can be effectively adjusted by means of eutectic.
Table 2 shows the DSC melting peak temperature (the temperature rise rate is 10 k/min) of the CL-20/NTO eutectic explosive of the invention. As can be seen from Table 2, the high melting point of CL-20 forms a eutectic with the low melting point of NTO through intermolecular forces, significantly lowering the melting point of the pure component CL-20.
TABLE 1 detonation performance of CL-20/NTO eutectic explosives and component samples
TABLE 2 DSC melting peak temperatures of CL-20/NTO eutectic explosives and component samples
Specific examples of the preparation of the CL-20/NTO eutectic explosive of the invention are described in detail below.
Example 1
Adding 10ml of industrial ethyl acetate into a three-neck flask at 20 ℃, adding enough CL-20, starting stirring, dissolving and filtering to obtain a saturated CL-20 solution. Then adding sufficient NTO into the solution, stirring, dissolving, and filtering to obtain saturated solution of CL-20 and NTO. And transferring the CL-20 and NTO saturated solution into a beaker, slowly volatilizing the solvent in a constant temperature box at 20 ℃, separating out crystals, filtering and drying to obtain the CL-20/NTO eutectic explosive.
Example 2
At 30 ℃, 20ml of industrial acetonitrile is added into a three-mouth bottle, sufficient CL-20 is added, stirring is started, and saturated CL-20 solution is obtained through dissolution and filtration. Then adding sufficient NTO into the solution, stirring, dissolving, and filtering to obtain saturated solution of CL-20 and NTO. And transferring the CL-20 and NTO saturated solution into a beaker, slowly volatilizing the solvent in a constant temperature box at 30 ℃, separating out crystals, filtering and drying to obtain the CL-20/NTO eutectic explosive.
Example 3
Adding 3ml of industrial product dimethyl sulfoxide into a three-neck flask at 40 ℃, adding enough CL-20, starting stirring, dissolving and filtering to obtain a saturated CL-20 solution. Then adding sufficient NTO into the solution, stirring, dissolving, and filtering to obtain saturated solution of CL-20 and NTO. And transferring the CL-20 and NTO saturated solution into a beaker, slowly volatilizing the solvent in a constant temperature box at 50 ℃, separating out crystals, filtering and drying to obtain the CL-20/NTO eutectic explosive.
Example 4
Adding enough CL-20 into a bottle of 20ml industrial ethyl acetate and acetonitrile (volume ratio is 1:1) at 50 ℃, starting stirring, dissolving and filtering to obtain a saturated CL-20 solution. Then adding sufficient NTO into the solution, stirring, dissolving, and filtering to obtain saturated solution of CL-20 and NTO. And transferring the CL-20 and NTO saturated solution into a beaker, slowly volatilizing the solvent in a constant temperature box at 50 ℃, separating out crystals, filtering and drying to obtain the CL-20/NTO eutectic explosive.
Example 5
At 25 ℃, 20ml of industrial dimethyl sulfoxide and acetonitrile (volume ratio is 1:1) are added into a three-mouth bottle, sufficient CL-20 is added, stirring is started, and the saturated CL-20 solution is obtained by dissolution and filtration. Then adding sufficient NTO into the solution, stirring, dissolving, and filtering to obtain saturated solution of CL-20 and NTO. And transferring the CL-20 and NTO saturated solution into a beaker, slowly volatilizing the solvent in a constant temperature box at 25 ℃, separating out crystals, filtering and drying to obtain the CL-20/NTO eutectic explosive.
Example 6
Adding 15ml of industrial ethyl acetate and dimethyl sulfoxide (volume ratio is 1:1) into a three-necked bottle at 35 ℃, adding enough CL-20, stirring, dissolving, and filtering to obtain a saturated CL-20 solution. Then adding sufficient NTO into the solution, stirring, dissolving, and filtering to obtain saturated solution of CL-20 and NTO. And transferring the CL-20 and NTO saturated solution into a beaker, slowly volatilizing the solvent in a constant temperature box at 50 ℃, separating out crystals, filtering and drying to obtain the CL-20/NTO eutectic explosive.
The above detailed description is intended to illustrate the objects, aspects and advantages of the present invention, and it should be understood that the above detailed description is only exemplary of the present invention and is not intended to limit the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113121294A (en) * | 2021-04-19 | 2021-07-16 | 北京理工大学 | NTO and ATO eutectic explosive and preparation method thereof |
| CN113443948A (en) * | 2021-07-08 | 2021-09-28 | 北京理工大学 | Porous aromatic skeleton EPAF-6 material, NTO composite salt energetic material 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 |
| CN114031473A (en) * | 2021-11-19 | 2022-02-11 | 中国工程物理研究院化工材料研究所 | CL-20 and 3,5-MDNP supramolecular explosive and preparation method thereof |
| CN114133306A (en) * | 2021-11-19 | 2022-03-04 | 中国工程物理研究院化工材料研究所 | CL-20 and 3,4-MDNP supramolecular explosive and preparation method thereof |
| CN114539010A (en) * | 2022-03-09 | 2022-05-27 | 中北大学 | A kind of preparation method of MTNP/DNTF/DNAN eutectic |
| CN115677436A (en) * | 2021-07-28 | 2023-02-03 | 北京理工大学 | A kind of hexanitrohexaazaisowurtzitane and nitroimidazole eutectic energetic material and its preparation method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113121294A (en) * | 2021-04-19 | 2021-07-16 | 北京理工大学 | NTO and ATO eutectic explosive and preparation method thereof |
| CN113443948A (en) * | 2021-07-08 | 2021-09-28 | 北京理工大学 | Porous aromatic skeleton EPAF-6 material, NTO composite salt energetic material and preparation method thereof |
| CN115677436A (en) * | 2021-07-28 | 2023-02-03 | 北京理工大学 | A kind of hexanitrohexaazaisowurtzitane and nitroimidazole eutectic energetic material and its preparation method |
| 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 |
| CN114031473A (en) * | 2021-11-19 | 2022-02-11 | 中国工程物理研究院化工材料研究所 | CL-20 and 3,5-MDNP supramolecular explosive and preparation method thereof |
| CN114133306A (en) * | 2021-11-19 | 2022-03-04 | 中国工程物理研究院化工材料研究所 | CL-20 and 3,4-MDNP supramolecular explosive and preparation method thereof |
| CN114539010A (en) * | 2022-03-09 | 2022-05-27 | 中北大学 | A kind of preparation method of MTNP/DNTF/DNAN eutectic |
| CN114539010B (en) * | 2022-03-09 | 2022-11-11 | 中北大学 | A kind of preparation method of MTNP/DNTF/DNAN eutectic |
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Application publication date: 20210212 |