CN108456125A - A kind of CL-20 and CBNT cocrystallized explosives and preparation method thereof - Google Patents
A kind of CL-20 and CBNT cocrystallized explosives and preparation method thereof Download PDFInfo
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- CN108456125A CN108456125A CN201810192773.2A CN201810192773A CN108456125A CN 108456125 A CN108456125 A CN 108456125A CN 201810192773 A CN201810192773 A CN 201810192773A CN 108456125 A CN108456125 A CN 108456125A
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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
- C06B25/38—Compositions containing a nitrated organic compound the compound being a nitroparaffin with other nitrated organic compound
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Abstract
The present invention relates to a kind of CL 20 and CBNT cocrystallized explosives and preparation method thereof, belong to energetic material field.For raw material, CL 20/CBNT cocrystallized explosives are prepared using solvent/non-solvent method with Hexanitrohexaazaisowurtzitane (CL 20) and 5,5 ' dinitro amidos 3,3 ' connection triazole phosphinylidyne hydrazonium salt (CBNT) by the present invention.CL 20/CBNT cocrystallized explosives energy prepared by the present invention is suitable with CL 20, and sensitivity is greatly lowered compared with CL 20；CL 20/CBNT cocrystallized explosive manufacturing costs prepared by the present invention are less than CL 20；The preparation process of the present invention is simple, easy to operation, mild condition, is prepared suitable for extensive.The cocrystallized explosive is a kind of low sense explosive of novel high energy, can be used for manufacturing low rapid wear ammunition, there is good application prospect.
Description
Technical field
The present invention relates to low sense cocrystallized explosive of a kind of high energy and preparation method thereof, more particularly to a kind of CL-20 and CBNT is total
Brilliant explosive and preparation method thereof belongs to energetic material field.
Background technology
With the continuous development of new and high technology and increasingly complicated, requirement of the modern war to ammunition weapon of battlefield surroundings
It is more and more harsh.Warhead not only requires the feature that far firing range, power are big, energy is high, while to improve one's own side operation people
Member's viability, cartridge system must have the characteristics of insensitive (i.e. insensitiveness) again.Wherein desensitized explosive is 21 century energetic material
Research emphasis and hot spot.Eutectic technology provides a kind of new technological approaches to prepare insensitiveness high energy energetic material.
1987, the Nielsen of USN's weapons center synthesized Hexanitrohexaazaisowurtzitane (HNIW for the first time
Or CL-20).CL-20 density is 2.04g/cm3, and theoretical explosion velocity is 9500m/s, detonation pressure 43GPa, wherein density ratio HMX high
8%, explosion velocity is high by 6%, and detonation pressure is high by 8%, is the highest single chmical compound explosive of energy applied so far, is described as by international explosive wastewater circle
" high explosive of tomorrow ".But due to its higher mechanical sensitivity, drastically influence applications of the CL-20 in weaponry.
Drop sense is carried out as the research hotspot of recent domestic to CL-20 using eutectic technology.CL-20/TNT、CL-
20/DNP, CL-20/HMX, CL-20/RDX, CL-20/TATB, CL-20/LLM-105 etc. are using CL-20 as the cocrystallized explosive phase of base
After appearance.But due to ligand, for these cocrystallized explosives for preparing at present are with respect to CL-20, be not sensitivity it is relatively low and
Energy, which is also greatly lowered, simultaneously is exactly that the energy range of decrease is smaller and sensitivity remains in a relatively high level.
Invention content
The problem of can not balancing sensitivity and energy the purpose of the present invention is to solve the prior art, provide a kind of CL-20/
5,5 '-dinitro amido -3,3 '-connection-triazole phosphinylidyne hydrazonium salt (CBNT) cocrystallized explosive and preparation method thereof, the cocrystallized explosive belong to high
Can low sense explosive, the preparation method is simple for process and high income.
The purpose of the present invention is what is be achieved through the following technical solutions.
The molar ratio of the CL-20/CBNT cocrystallized explosives of the present invention, CL-20 and CBNT are 1:10-10:1.
A kind of preparation method of CL-20/CBNT cocrystallized explosives, includes the following steps：
CL-20 and CBNT are added in solvent；The molar ratio of CL-20 and CBNT is 1:10-10:1；The additive amount of solvent
Related to CL-20, i.e., the CL-20 of 1g need to be dissolved in the solvent of 0.1~30ml；Be warming up to 40 DEG C -90 DEG C be completely dissolved after, cooling
To 20 DEG C -35 DEG C, it is then added non-solvent, the volume ratio of solvent and non-solvent is 1:1~6, it is obtained after stirring, filtering, drying
CL-20/CBNT cocrystallized explosives.
The solvent is dimethyl sulfoxide (DMSO) (DMSO), N,N-dimethylformamide (DMF), N-Methyl pyrrolidone (NMP)
One or both of or three kinds of mixtures.
The non-solvent is the mixture of water or ethyl alcohol or the two.
Advantageous effect
1, the CL-20/CBNT cocrystallized explosive energy (explosion velocity 9200-9400m/s) that prepared by the present invention is suitable with CL-20, sense
Degree (impact sensitivity 10-35cm) is greatly lowered compared with CL-20.
2, preparation process of the invention is simple, easy to operation, mild condition, is prepared suitable for extensive.
3, while CL-20/CBNT cocrystallized explosive comprehensive performances prepared by the present invention are better than CL-20, cost is also compared with CL-20
Significantly decline.
Description of the drawings
Fig. 1 is the preparation technology flow chart of one embodiment of the invention CL-20 and CBNT cocrystallized explosives；
Fig. 2 is the scanning electron microscope (SEM) photograph of CL-20, CBNT and 2CL-20 of the embodiment of the present invention and CBNT cocrystallized explosives；Wherein, a
The scanning electron microscope (SEM) photograph that figure is CL-20；The scanning electron microscope (SEM) photograph that b figures are CBNT；C, d, e figure are the scanning electron microscope of CL-20/CBNT eutectics
Figure；
Fig. 3 is the infrared spectrogram of CL-20, CBNT and 2CL-20 of the embodiment of the present invention and CBNT cocrystallized explosives；
Fig. 4 is the powder diagram of CL-20, CBNT and 2CL-20 of the embodiment of the present invention and CBNT cocrystallized explosives；
Fig. 5 is the Raman spectrogram of CL-20, CBNT and 2CL-20 of the embodiment of the present invention and CBNT cocrystallized explosives；
Fig. 6 is the thermogram of CL-20, CBNT and 2CL-20 of the embodiment of the present invention and CBNT cocrystallized explosives.
Specific implementation mode
Invention is described further with example below by way of attached drawing, but invention is not limited by the following sample.
Embodiment 1
The molar ratio of the CL-20/CBNT cocrystallized explosives of the present invention, CL-20 and CBNT are 1:10.
0.438g Cl-20,3.46g CBNT are added in 5mL DMSO, are warming up to 90 DEG C, waits for that two kinds of raw materials are all molten
Solution is cooled to 35 DEG C of addition 15ml non-solvent water, 0.5h is stirred after adding, is then filtered.Filter cake uses 20mL water washings primary again,
Obtain 3.5g CL-20/CBNT cocrystallized explosives.The explosion velocity of the cocrystallized explosive is 9300m/s, impact sensitivity (H50) it is 35cm.
Embodiment 2
The molar ratio of the CL-20/CBNT cocrystallized explosives of the present invention, CL-20 and CBNT are 1:1.
4.38g Cl-20,3.46g CBNT are added in 10mL DMSO, are warming up to 80 DEG C, waits for that two kinds of raw materials are all molten
Solution is cooled to 25 DEG C of addition 35ml non-solvent ethyl alcohol, 0.5h is stirred after adding, is then filtered.Filter cake uses 20mL water washings one again
It is secondary, obtain 7.05g CL-20/CBNT cocrystallized explosives.The explosion velocity of the cocrystallized explosive is 9350m/s, impact sensitivity (H50) it is 28cm.Its
The scanning electron microscope of middle raw material and the cocrystallized explosive is as shown in Figure 2；The infrared spectrum of raw material and the cocrystallized explosive is as shown in Figure 3；It is former
Material is as shown in Figure 4 with the powder diffraction of the cocrystallized explosive；The Raman spectrum of raw material and the cocrystallized explosive is as shown in Figure 5；Raw material with
The heat analysis of the cocrystallized explosive is as shown in Figure 6.
Significant change has occurred with two kinds of raw material comparisons in the crystalline form crystalline substance looks of the cocrystallized explosive as can be seen from Figure 2；From figure
3, as can be seen that apparent offset or intensity has occurred compared to two kinds of raw materials in the characteristic peak of the cocrystallized explosive in Fig. 4 and Fig. 5
It changes；From fig. 6 it can be seen that decomposition peak's temperature of cocrystallized explosive is between two raw material decomposes peak temperature.Described in synthesis,
It may determine that CL-20 and CBNT forms eutectic.Other embodiments have carried out corresponding series of tests, in text no longer one by one
It lists.
Embodiment 3
The molar ratio of the CL-20/CBNT cocrystallized explosives of the present invention, CL-20 and CBNT are 2:1.
4.38g Cl-20,1.73g CBNT are added in 10mL NMP, are warming up to 60 DEG C, waits for that two kinds of raw materials are all molten
Solution is cooled to 20 DEG C and 30ml non-solvents water and alcohol mixeding liquid (volume ratio 1 is added:1) 1h is stirred after, adding, and is then filtered.
Filter cake uses 20mL water washings primary again, obtains 5.50g CL-20/CBNT cocrystallized explosives.The explosion velocity of the cocrystallized explosive is 9270m/s,
Impact sensitivity (H50) it is 15cm.
Embodiment 4
The molar ratio of the CL-20/CBNT cocrystallized explosives of the present invention, CL-20 and CBNT are 1:2.
2.19g Cl-20,3.46g CBNT are added to 10mL mixed solvents, and (DMF and DMSO volume ratios are 1:1) it in, rises
Temperature waits for that two kinds of raw materials all dissolve to 85 DEG C, is cooled to 20 DEG C of addition 40ml non-solvent water, 0.5h is stirred after adding, then mistake
Filter.Filter cake uses 20mL water washings primary again, obtains 5.08g CL-20/CBNT cocrystallized explosives.The explosion velocity of the cocrystallized explosive is 9250m/
S, impact sensitivity (H50) it is 30cm.
Embodiment 5
The molar ratio of the CL-20/CBNT cocrystallized explosives of the present invention, CL-20 and CBNT are 5:3.
5.48g Cl-20,2.6g CBNT are added to 10mL mixed solvents, and (DMF and NMP volume ratios are 1:1) in, heating
To 70 DEG C, wait for that two kinds of raw materials all dissolve, being cooled to 30 DEG C of addition 60ml non-solvents, (water is 2 with ethyl alcohol volume ratio:1) it, adds
After stir 0.5h, then filter.Filter cake uses 20mL water washings primary again, obtains 7.27g CL-20/CBNT cocrystallized explosives.The eutectic
The explosion velocity of explosive is 9200m/s, impact sensitivity (H50) it is 20cm.
Embodiment 6
The molar ratio of the CL-20/CBNT cocrystallized explosives of the present invention, CL-20 and CBNT are 10:1.
4.38g Cl-20,0.346g CBNT are added to 3mL mixed solvents, and (DMF, NMP, DMSO volume ratio are 1:1:1)
In, 40 DEG C are warming up to, waits for that two kinds of raw materials all dissolve, being cooled to 25 DEG C of addition 8ml non-solvents, (water is 1 with ethyl alcohol volume ratio:
2) 2h is stirred after, adding, and is then filtered.Filter cake uses 20mL water washings primary again, obtains 4.25g CL-20/CBNT cocrystallized explosives.It should
The explosion velocity of cocrystallized explosive is 9220m/s, impact sensitivity (H50) it is 10cm.
Table 1
The cocrystallized explosive formed as can be seen from Table 1 is while guarantee ability is hardly reduced, impact sensitivity (characteristic
The bigger H of drop height50It is lower to hit sense) significantly decline.
This patent is prepared for CL-20/CBNT cocrystallized explosives by solvent/non-solvent method.Using scanning electron microscope, infrared light
The methods of spectrum, powder diffraction, Raman spectrum and heat analysis have carried out structural characterization to it.And calculate the quick-fried of the cocrystallized explosive
Speed, the sensitivity for testing the cocrystallized explosive.The result shows that this method is practical, and the balance of energy and sensitivity is reached.
Above-described specific descriptions have carried out further specifically the purpose, technical solution and advantageous effect of invention
It is bright, it should be understood that the above is only a specific embodiment of the present invention, the protection model being not intended to limit the present invention
It encloses, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the present invention
Protection domain within.
Claims (4)
1. a kind of CL-20 and CBNT cocrystallized explosives and preparation method thereof, it is characterised in that：The molar ratio of CL-20 and CBNT is 1:
10-10:1。
2. a kind of CL-20 and CBNT cocrystallized explosives and preparation method thereof, it is characterised in that：CL-20 and CBNT are added to solvent
In；The molar ratio of CL-20 and CBNT is 1:10-10:1；The additive amount of solvent is related to CL-20, i.e., the CL-20 of 1g need to be dissolved in
In the solvent of 0.1~30ml；Be warming up to 40 DEG C -90 DEG C be completely dissolved after, be cooled to 20 DEG C -35 DEG C, non-solvent be then added, it is molten
The volume ratio of agent and non-solvent is 1:1~6, obtain CL-20/CBNT cocrystallized explosives after stirring, filtering, drying.
3. a kind of CL-20 as claimed in claim 2 and CBNT cocrystallized explosives and preparation method thereof, it is characterised in that：It is described molten
Agent is one or both of dimethyl sulfoxide (DMSO), N,N-dimethylformamide, N-Methyl pyrrolidone or three kinds of mixtures.
4. a kind of CL-20 as claimed in claim 2 and CBNT cocrystallized explosives and preparation method thereof, it is characterised in that：It is described non-
Solvent is the mixture of water or ethyl alcohol or the two.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110156545A (en) * | 2019-05-13 | 2019-08-23 | 南京理工大学 | A kind of CL-20/TKX-50 cocrystallized explosive and preparation method thereof |
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| CN103524444A (en) * | 2013-09-27 | 2014-01-22 | 北京理工大学 | Synthetic method of 5, 5'-bistetrazole-1, 1'-dioxo hydroxyl ammonium salt (TKX-50) |
| CN104016932A (en) * | 2014-06-19 | 2014-09-03 | 西安近代化学研究所 | Method for synthesizing 5,5'-dinitroamino-3,3'-co-1,2,4-triazole carbohydrazide |
| US20150361056A1 (en) * | 2014-03-31 | 2015-12-17 | Nalas Engineering Services Inc. | Cl-20:dnmt cocrystal crystal structure |
| CN106831278A (en) * | 2017-01-24 | 2017-06-13 | 中国工程物理研究院化工材料研究所 | A kind of Subjective and Objective explosive with crystalline density high and preparation method thereof |
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Patent Citations (4)
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| CN103524444A (en) * | 2013-09-27 | 2014-01-22 | 北京理工大学 | Synthetic method of 5, 5'-bistetrazole-1, 1'-dioxo hydroxyl ammonium salt (TKX-50) |
| US20150361056A1 (en) * | 2014-03-31 | 2015-12-17 | Nalas Engineering Services Inc. | Cl-20:dnmt cocrystal crystal structure |
| CN104016932A (en) * | 2014-06-19 | 2014-09-03 | 西安近代化学研究所 | Method for synthesizing 5,5'-dinitroamino-3,3'-co-1,2,4-triazole carbohydrazide |
| CN106831278A (en) * | 2017-01-24 | 2017-06-13 | 中国工程物理研究院化工材料研究所 | A kind of Subjective and Objective explosive with crystalline density high and preparation method thereof |
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| CN110156545A (en) * | 2019-05-13 | 2019-08-23 | 南京理工大学 | A kind of CL-20/TKX-50 cocrystallized explosive and preparation method thereof |
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